#Makefile for thesis
+
+all :
+ make clean
+ make thesis.pdf
+ evince thesis.pdf &
+
thesis.pdf : thesis.tex
rm -f *.aux *.bbl *.log *.toc *.lof *.blg *.lot
rm -f *.bbl *.log *.toc *.lof *.blg *.lot
+ pdftk thesis.pdf proposal/proposal.pdf cat output out.pdf
+ mv out.pdf thesis.pdf
+
clean :
- rm thesis.pdf
+ rm -f thesis.pdf
#Makefile for thesis
+
+all :
+ make clean
+ make thesis.pdf
+ evince thesis.pdf &
+
thesis.pdf : thesis.tex
rm -f *.aux *.bbl *.log *.toc *.lof *.blg *.lot
pdflatex --shell-escape thesis
bibtex thesis
- pdflatex thesis
- pdflatex thesis
+ pdflatex --shell-escape thesis
+ pdflatex --shell-escape thesis
rm -f *.bbl *.log *.toc *.lof *.blg *.lot
+ pdftk thesis.pdf proposal/proposal.pdf cat output out.pdf
+ #mv out.pdf thesis.pdf
+
clean :
- rm thesis.pdf
+ rm -f thesis.pdf
--- /dev/null
+[LATEX]
+master-filename = ../thesis.tex
+
\relax
+\citation{pfund1930}
+\citation{harris1952}
+\citation{panjwani2011}
\@setckpt{abstract/Abstract}{
\setcounter{page}{1}
\setcounter{equation}{0}
\begin{abstract}
+\section*{Preparation and Characterisation of Nanostructured metal films}
+
+
+{\bf \emph{Keywords:}} plasmonics, thin films, silver, gold, nanostructures, optical transmission spectroscopy, ellipsometry, total current secondary electron spectroscopy, scanning electron microscopy
+
+Black metal films have been used for a wide range of optical applications for many decades due to their unusual absorbsion properties \cite{pfund1930} \cite{harris1952}. Black metal films have recently been shown to increase the efficiency of thin film solar cells \cite{panjwani2011}. %Advances in nano fabrication technologies have allowed for the creation of ``artificially'' blackened metal surfaces which suppress reflection via surface plasmon scattering of light in nano-grooves \cite{sondergaard2012}. Considering these recent developements, it seems possible that ``traditional'' black metal films may support plasmonic behaviour.
+
+In this project we have produced a range of silver and gold nanostructured films for study using optical and electronic spectroscopic techniques. Scanning electron microscopy images have been used to study the structural differences between black and non-black metal films. A Total Current Spectroscopy experiment has been designed and integrated with sample preparation technology; this allowed us to perform analysis of surfaces in situ. Optical transmission spectroscopy has been used to compare the transmissive behaviour of black and non-black films under visible wavelengths. Variable Angle Spectroscopic Ellipsometry (VASE) has been employed for detailed measurements and modelling of samples.
+
+SEM images confirm that the structure of black metal films is extremely complicated when compared to a non-black film. With Total Current Spectroscopy, we have demonstrated a change in surface potential when a Black Ag film was deposited onto an existing Ag film. Ellipsometric modelling for very thin Ag and Black Ag films shows a notable difference in optical constants of the two films.
+
+
+
+
\end{abstract}
+\begin{abstract}
+
+\section*{Preparation and Characterisation of Nanostructured metal films}
+
+
+{\bf \emph{Keywords:}} plasmonics, thin films, silver, gold, nanostructures, optical transmission spectroscopy, ellipsometry, total current secondary electron spectroscopy, scanning electron microscopy
+
+Black metal films have been used for a wide range of optical applications for many decades due to their unusual absorbsion properties \cite{pfund1930} \cite{harris1952}. Black metal films have recently been shown to increase the efficiency of thin film solar cells \cite{panjwani2011}. Advances in nano fabrication technologies have allowed for the creation of ``artificially'' blackened metal surfaces which suppress reflection via surface plasmon scattering of light in nano-grooves \cite{sondergaard2012}. Considering these recent developements, it seems possible that ``traditional'' black metal films may support plasmonic behaviour.
+
+In this project we have produced a range of silver and gold nanostructured films for study using optical and electronic spectroscopic techniques. Scanning electron microscopy images have been used to study the structural differences between black and non-black metal films. A Total Current Spectroscopy experiment has been designed and integrated with sample preparation technology; this allowed us to perform analysis of surfaces in situ. Optical transmission spectroscopy has been used to compare the transmissive behaviour of black and non-black films under visible wavelengths. Variable Angle Spectroscopic Ellipsometry (VASE) has been employed for detailed measurements and modelling of samples.
+
+SEM images confirm that the structure of black metal films is extremely complicated when compared to a non-black film. With Total Current Spectroscopy, we have demonstrated a change in surface potential when a Black Ag film was deposited onto an existing Ag film. Ellipsometric modelling for very thin Ag and Black Ag films shows a notable difference in optical constants of the two films.
+
+
+
+
+\end{abstract}
\relax
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-%\\
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-%\\
-%\\
-%Joe Citizen
-%\newpage
-\chapter*{Acknowledgments}
+\chapter*{Declaration}
\thispagestyle{empty}
+{I declare that this thesis contains less than 40 pages, excluding: the title page, this declaration, acknowledgements, the table of contents, and references.}
+\chapter*{Acknowledgments}
+
I am extremely grateful for the support offered to me by many individuals during this project. There aren't many synonyms for ``Thanks'', so I'm afraid this section may be a little repetitive.
Thanks to my supervisors Prof Sergey Samarin and W/Prof Jim Williams for envisioning the project, and their invaluable support throughout the year. I would also like to thank staff members at CAMSP for assisting with the supervision of this project. In particular I am extremely grateful for the help and advice given by Dr Paul Gualiardo during the construction and testing of the Total Current Spectroscopy experiment.
-Thanks to the Centre for Microscopy Characterisation and Analysis (CMCA) for producing the SEM images which proved a invaluable aid for discussing the structure of the metallic-black films. Thanks to Nikita Kostylev for helping me learn the art of operating the ellipsometer. Thanks to both Prof Mikhail Kostylev and Jeremy Hughes for lending me some samples for ellipsometric analysis. I would also like to endorse the team at J.A Woolam, who provided replacement pins for the ellipsometer alignment detector at no charge after one of the original pins became mysteriously damaged.
+Thanks to CMCA for producing the SEM images which proved a invaluable aid for discussing the structure of the metallic-black films. Thanks to Jeremy Hughes for lending me some samples for ellipsometric analysis (even though I did not get around to studying those samples). I would also like to endorse the team at J.A Woolam, who provided replacement pins for the ellipsometer alignment detector at no charge after one of the original pins became mysteriously damaged.
Congratulations to Jeremy Hughes who successfully predicted that the emission current of the electron gun was varying periodically less than a quarter of the way through the first period. Condolences to Alexander Mazur, whose theory that the vacuum chamber contained a pulsar proved unfounded.
Thanks to all my family and friends for their support and for continuing to put up with my slow descent into madness during the last 12 months.
-Finally, perhaps as a result of the aforementioned madness, I would also like to thank the various pieces of equipment and inanimate objects which have been crucial to the success of this project. This includes the ellipsometer, the ADC/DAC box, my laptop computer ``Cerberus'', and the two ammeters upon which I relied upon so heavily. Rest in peace Keithly 610B. Your death was not in vain.
+Finally, perhaps as a result of the aforementioned madness, I would also like to thank the various pieces of equipment and inanimate objects which have been crucial to the success of this project. This includes the ellipsometer, the ADC/DAC box, my laptop computer ``Cerberus'', and the two electrometers that I relied upon so heavily. Rest in peace Keithly 610B. Your death was not in vain.
+\chapter*{Declaration}
+\thispagestyle{empty}
+{I declare that this thesis contains less than 40 pages, excluding: the title page, this declaration, acknowledgements, the table of contents, and references.}
+\chapter*{Acknowledgments}
+
+
+I am extremely grateful for the support offered to me by many individuals during this project. There aren't many synonyms for ``Thanks'', so I'm afraid this section may be a little repetitive.
+
+Thanks to my supervisors Prof Sergey Samarin and W/Prof Jim Williams for envisioning the project, and their invaluable support throughout the year. I would also like to thank staff members at CAMSP for assisting with the supervision of this project. In particular I am extremely grateful for the help and advice given by Dr Paul Gualiardo during the construction and testing of the Total Current Spectroscopy experiment.
+
+Thanks to CMCA for producing the SEM images which proved a invaluable aid for discussing the structure of the metallic-black films. Thanks to Jeremy Hughes for lending me some samples for ellipsometric analysis (even though I did not get around to studying those samples). I would also like to endorse the team at J.A Woolam, who provided replacement pins for the ellipsometer alignment detector at no charge after one of the original pins became mysteriously damaged.
+
+Congratulations to Jeremy Hughes who successfully predicted that the emission current of the electron gun was varying periodically less than a quarter of the way through the first period. Condolences to Alexander Mazur, whose theory that the vacuum chamber contained a pulsar proved unfounded.
+
+Thanks to all my family and friends for their support and for continuing to put up with my slow descent into madness during the last 12 months.
+
+Finally, perhaps as a result of the aforementioned madness, I would also like to thank the various pieces of equipment and inanimate objects which have been crucial to the success of this project. This includes the ellipsometer, the ADC/DAC box, my laptop computer ``Cerberus'', and the two electrometers that I relied upon so heavily. Rest in peace Keithly 610B. Your death was not in vain.
+
--- /dev/null
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+\section*{Summary of Student Achievements}
+
+
+\begin{enumerate}
+ \item Implementation of a low energy Total Current Spectroscopy experiment, involving:
+ \begin{itemize}
+ \item Design and construction of the sample holder
+ \item Design and construction of the electron gun control circuit
+ \item Design and construction of an automated data aquisition system (both hardware and software). This system was used to produce over 2GB in data files during the project.
+ \item Attaching cable plugs for use with the TCS experiment (also, reattaching existing damaged plugs)
+ \item Implementation of a webcam based system for automatic monitoring of chamber pressure
+ \item Focusing the electron gun
+ \item Design and implementation of custom software which assisted in troubleshooting the electron gun
+ \item Modifications to the electron gun to reduce charging problems
+ \item Developement of software for analysis and processing of TCS data
+ \end{itemize}
+ \item Preparation of black and non-black nanostructured metal surfaces on both Si and glass substrates
+ \item Obtaining all ellipsometric measurements for samples
+ \item Construction of models within the WVASE32 software
+ \item Design and construction of a sample holder for the transmission spectroscopy experiments
+ \item Analysis of SEM images prepared by CMCA
+\end{enumerate}
--- /dev/null
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+
+\section*{Summary of Student Achievements}
+
+
+\begin{enumerate}
+ \item Implementation of a low energy Total Current Spectroscopy experiment, involving:
+ \begin{itemize}
+ \item Design and construction of the sample holder
+ \item Design and construction of the electron gun control circuit
+ \item Design and construction of an automated data aquisition system (both hardware and software). This system was used to produce over 2GB in data files during the project.
+ \item Attaching cable plugs for use with the TCS experiment (also, reattaching damaged existing plugs)
+ \item Implementation of a webcam based system for automatic monitoring of chamber pressure
+ \item Focusing the electron gun
+ \item Design and implementation of custom software which assisted in troubleshooting the electron gun
+ \item Modifications to the electron gun to reduce charging problems
+ \item Developement of software for analysis and processing of TCS data
+ \end{itemize}
+ \item Preparation of black and non-black nanostructured metal surfaces on both Si and glass substrates
+ \item Obtaining all ellipsometric measurements for samples
+ \item Construction of models within the WVASE32 software
+ \item Design and construction of a sample holder for the transmission spectroscopy experiments
+ \item Analysis of SEM images prepared by CMCA
+\end{enumerate}
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\section{Data Aquisition Hardware}
-{\bf NOTE:} This is slightly out of date, since when the 610B ammeter mysteriously broke, I just used ADC5 for everything. So I can probably leave out all the stuff about the differences between ADC5 and the other ADC's. Then again, it's the appendix. I can probably leave \emph{all} of it out.
-
\subsection{Overview}
+During this project, more than 6000 total current spectra were recorded. This would not have been possible without automation.
+
In order to automate TCS experiments, both Digital to Analogue and Analogue to Digital Convertors were required (DAC and ADC). To provide these, a custom DAC/ADC Box was designed and constructed. The box can be controlled by any conventional computer with available RS-232 serial communication (COM) ports. Most modern computers no longer feature COM ports; a commercially available convertor can be used to interface between the box's RS-232 output and a standard Universal Serial Bus (USB) port.
\label{adc5.pdf}
\end{center}
-asdfa
The instrumentation amplifier consists of two stages of operational amplifiers (op-amps); input buffers, and a difference amplifier.
The difference amplifier can be shown using the ideal op-amp model to produce an output voltage proportional to the difference between its inputs:
The low pass filters were added to the inputs of ADC5 after it was found that an unacceptable level of AC noise was being output by the electrometer. The level of noise was too high to be filtered in software, for reasons that will be discussed in Appendix D.
-\subsection{Temperature Measurement}
-
-The AVR Butterfly features an onboard thermistor connected to ADC0. Reading ADC0 and applying the formula given in the AVR Butterfly User's Guide \cite{} results in a temperature measurement. This was useful in establishing a link between the changing chamber pressure and the temperature of the laboratory (see Appendix C).
-
\subsection{Power Supplies}
Due to the presence of both analogue and digital electronics in the DAC/ADC box, three seperate supply voltages were required:
\begin{enumerate}
The buffer amplifier ensures that negligable current can flow from the power supply into the logic and ADC circuits, whilst the capacitor removes high frequency fluctuations of the power supply relative to ground.
\subsection{DAC Output}
-A commercial DAC board was used to produce the DAC output. The Microchip MCP4922 ET-Mini DAC is controlled by the AVR Butterfly using Motorola's Serial Peripheral Interface (SPI) Bus. The software used to implement SPI between the MCP4922 and the AVR Butterfly is discussed in Appendix D.
+A commercial DAC board was used to produce the DAC output. The Microchip MCP4922 ET-Mini DAC is controlled by the AVR Butterfly using Motorola's Serial Peripheral Interface (SPI) Bus.
The ET-Mini DAC can only be powered off $3V$ to $5V$. Using $V_{cc} = 3.3V$ means that the DAC output cannot exceed $V_{cc} = 3.3V$. For TCS, energies of up to $15eV$ are required, so amplification of the DAC output was clearly necessary. A simple non-inverting amplifier with a manually adjustable gain was used to amplify the DAC output by a factor of three. This output was then used to control a laboratory power supply to produce the full range of initial energies.
Although the RS-232 is relatively simple to implement, which makes it ideal for non-proprietry microprocessor applications, most modern computers no longer feature RS-232 COM ports. Although a computer with COM ports was available at CAMSP, due to the extreme unreliability of this computer, it was quickly replaced with a laptop that did not possess COM ports, and a commercial RS-232 to USB converter was used to interface with the laptop.
+\subsection{Software}
+
+The data aquistion system required software to be written for both the AVR Butterfly and the attached processing computer. The AVR Butterfly software has been written in C, and is based upon open source examples provided by Atmel. The interface for the attached computer was written in python. We will not include any detailed description of the software here. More information is available on request.
+
\section{Data Aquisition Hardware}
-{\bf NOTE:} This is slightly out of date, since when the 610B ammeter mysteriously broke, I just used ADC5 for everything. So I can probably leave out all the stuff about the differences between ADC5 and the other ADC's.
-
\subsection{Overview}
+During this project, more than 6000 total current spectra were recorded. This would not have been possible without automation.
+
In order to automate TCS experiments, both Digital to Analogue and Analogue to Digital Convertors were required (DAC and ADC). To provide these, a custom DAC/ADC Box was designed and constructed. The box can be controlled by any conventional computer with available RS-232 serial communication (COM) ports. Most modern computers no longer feature COM ports; a commercially available convertor can be used to interface between the box's RS-232 output and a standard Universal Serial Bus (USB) port.
\label{adc5.pdf}
\end{center}
-asdfa
The instrumentation amplifier consists of two stages of operational amplifiers (op-amps); input buffers, and a difference amplifier.
The difference amplifier can be shown using the ideal op-amp model to produce an output voltage proportional to the difference between its inputs:
The low pass filters were added to the inputs of ADC5 after it was found that an unacceptable level of AC noise was being output by the electrometer. The level of noise was too high to be filtered in software, for reasons that will be discussed in Appendix D.
-\subsection{Temperature Measurement}
-
-The AVR Butterfly features an onboard thermistor connected to ADC0. Reading ADC0 and applying the formula given in the AVR Butterfly User's Guide \cite{} results in a temperature measurement. This was useful in establishing a link between the changing chamber pressure and the temperature of the laboratory (see Appendix C).
-
\subsection{Power Supplies}
Due to the presence of both analogue and digital electronics in the DAC/ADC box, three seperate supply voltages were required:
\begin{enumerate}
The buffer amplifier ensures that negligable current can flow from the power supply into the logic and ADC circuits, whilst the capacitor removes high frequency fluctuations of the power supply relative to ground.
\subsection{DAC Output}
-A commercial DAC board was used to produce the DAC output. The Microchip MCP4922 ET-Mini DAC is controlled by the AVR Butterfly using Motorola's Serial Peripheral Interface (SPI) Bus. The software used to implement SPI between the MCP4922 and the AVR Butterfly is discussed in Appendix D.
+A commercial DAC board was used to produce the DAC output. The Microchip MCP4922 ET-Mini DAC is controlled by the AVR Butterfly using Motorola's Serial Peripheral Interface (SPI) Bus.
The ET-Mini DAC can only be powered off $3V$ to $5V$. Using $V_{cc} = 3.3V$ means that the DAC output cannot exceed $V_{cc} = 3.3V$. For TCS, energies of up to $15eV$ are required, so amplification of the DAC output was clearly necessary. A simple non-inverting amplifier with a manually adjustable gain was used to amplify the DAC output by a factor of three. This output was then used to control a laboratory power supply to produce the full range of initial energies.
Although the RS-232 is relatively simple to implement, which makes it ideal for non-proprietry microprocessor applications, most modern computers no longer feature RS-232 COM ports. Although a computer with COM ports was available at CAMSP, due to the extreme unreliability of this computer, it was quickly replaced with a laptop that did not possess COM ports, and a commercial RS-232 to USB converter was used to interface with the laptop.
+\subsection{Software}
+
+The data aquistion system required software to be written for both the AVR Butterfly and the attached processing computer. The AVR Butterfly software has been written in C, and is based upon open source examples provided by Atmel. The interface for the attached computer was written in python.
+
+We will not include any detailed description of the software here. More information is available on request.
+
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\section{Electron Optics}
-The electron gun used for this study contains a total of ten electrodes, with six independently adjustable groups. Figure \ref{egun_simulation1.pdf} illustrates a cross section of the gun, using colour coding to indicate groups of electrodes which are kept at the same potential.
-
-
The important electrode groups are, in order from left to right:
\begin{enumerate}
- \item {\bf Wenhalt Cylindar}
+ \item {\bf Wenhalt Cylindar} $Vw$
- The first electrode, which houses the cathode, providing a narrow apparture for electrons to exit. A positive potential (of the order of $10V$ applied to the Wenhalt causes electrons leaving the cathode to be accelerated into a narrow beam.
- It is difficult to control the focusing properties of the gun using the Wenhalt alone; the main purpose of the Wenhalt is to create a high current, narrow beam of electrons, which can be focused by the other electrodes in the gun. If the potential applied to the Wenhalt is too high, electrons will be drawn into its surface. If the Wenhalt potential is too low, then fewer electrons are able to leave the aparture.
+ The first electrode, which houses the cathode, providing a narrow apparture for electrons to exit. A positive potential (of the order of $10V$) applied to the Wenhalt causes electrons leaving the cathode to be accelerated into a narrow beam.
- \item {\bf Einzel Lens }
+ The main purpose of the Wenhalt is to create a high current, narrow beam of electrons. If the potential applied to the Wenhalt is too high, electrons will be drawn into its surface. If the Wenhalt potential is too low, then fewer electrons are able to leave the aparture.
+
+ \item {\bf Accelerating Electrodes } $V_a$
+
+ The first and
The six central electrodes are an example of an Einzel lens, used for acceleration and focusing of the electron beam.
The first and last pair of electrodes are held at a large positive potential, causing electrons to accelerate. A smaller potential (often negative, but not necessarily) applied to the central pair of electrodes has the effect of altering the angular dispersion of the beam.
In preparation for Total Current Spectroscopy experiments, the effect of each of the controllable potentials was investigated by focusing the electron gun on its original flurescent screen. However, when repurposed for total current spectroscopy, the gun needed to be refocused several times (with changing sample holder design).
-The gun was focused using an iterative process, by which each potential was altered in turn to maximise the current.
-
\pagebreak
\subsection{A two dimensional electron gun simulation}
-The below figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} are the results of a simplistic electron gun simulation. The results of this simulation were not used to focus the actual electron gun; the images shown here are purely presented as a visual aid.
+The below figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} are the results of a simplistic electron gun simulation. The results of this simulation were not used to focus the actual electron gun; however Figure \ref{egun_simulation1.pdf} was extremely useful, as it shows the possibility for electrons to strike the insulating posts holding the gun together. When these posts were covered with Ta strips connected to the final electrode, the stability of the electron gun was improved.
-\begin{center}
+\begin{figure}[H]
+ \centering
\includegraphics[scale=0.45, angle=270]{figures/egun/egun_simulation1.pdf}
-
- \captionof{figure}{{\bf 2D Simulation of trajectories of electrons accelerated through an electron gun}}
+ \caption{Simulated electron trajectories}
\label{egun_simulation1.pdf}
+\end{figure}
+
+\begin{figure}[H]
+ \centering
\includegraphics[scale=0.45, angle=270]{figures/egun/egun_simulation2.pdf}
\captionof{figure}{{\bf 2D Simulation of the electrostatic potential produced by the electron gun}}\label{egun_simulation2.pdf}
-
-\end{center}
+\end{figure}
+
\pagebreak
\section{Electron Optics}
-The electron gun used for this study contains a total of ten electrodes, with six independently adjustable groups. Figure \ref{egun_simulation1.pdf} illustrates a cross section of the gun, using colour coding to indicate groups of electrodes which are kept at the same potential.
-
-
The important electrode groups are, in order from left to right:
\begin{enumerate}
- \item {\bf Wenhalt Cylindar}
+ \item {\bf Wenhalt Cylindar} $Vw$
- The first electrode, which houses the cathode, providing a narrow apparture for electrons to exit. A positive potential (of the order of $10V$ applied to the Wenhalt causes electrons leaving the cathode to be accelerated into a narrow beam.
- It is difficult to control the focusing properties of the gun using the Wenhalt alone; the main purpose of the Wenhalt is to create a high current, narrow beam of electrons, which can be focused by the other electrodes in the gun. If the potential applied to the Wenhalt is too high, electrons will be drawn into its surface. If the Wenhalt potential is too low, then fewer electrons are able to leave the aparture.
+ The first electrode, which houses the cathode, providing a narrow apparture for electrons to exit. A positive potential (of the order of $10V$) applied to the Wenhalt causes electrons leaving the cathode to be accelerated into a narrow beam.
- \item {\bf Einzel Lens }
+ The main purpose of the Wenhalt is to create a high current, narrow beam of electrons. If the potential applied to the Wenhalt is too high, electrons will be drawn into its surface. If the Wenhalt potential is too low, then fewer electrons are able to leave the aparture.
+
+ \item {\bf Accelerating Electrodes } $V_a$
+
The six central electrodes are an example of an Einzel lens, used for acceleration and focusing of the electron beam.
The first and last pair of electrodes are held at a large positive potential, causing electrons to accelerate. A smaller potential (often negative, but not necessarily) applied to the central pair of electrodes has the effect of altering the angular dispersion of the beam.
In preparation for Total Current Spectroscopy experiments, the effect of each of the controllable potentials was investigated by focusing the electron gun on its original flurescent screen. However, when repurposed for total current spectroscopy, the gun needed to be refocused several times (with changing sample holder design).
-The gun was focused using an iterative process, by which each potential was altered in turn to maximise the current.
-
\pagebreak
\subsection{A two dimensional electron gun simulation}
-The below figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} are the results of a simplistic electron gun simulation. The results of this simulation were not used to focus the actual electron gun; the images shown here are purely presented as a visual aid.
+The below figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} are the results of a simplistic electron gun simulation. The results of this simulation were not used to focus the actual electron gun; however Figure \ref{egun_simulation1.pdf} was extremely useful, as it shows the possibility for electrons to strike the insulating posts holding the gun together. When these posts were covered with Ta strips connected to the final electrode, the stability of the electron gun was improved.
-\begin{center}
+\begin{figure}[H]
+ \centering
\includegraphics[scale=0.45, angle=270]{figures/egun/egun_simulation1.pdf}
-
- \captionof{figure}{{\bf 2D Simulation of trajectories of electrons accelerated through an electron gun}}
+ \caption{Simulated electron trajectories}
\label{egun_simulation1.pdf}
+\end{figure}
+
+\begin{figure}[H]
+ \centering
\includegraphics[scale=0.45, angle=270]{figures/egun/egun_simulation2.pdf}
\captionof{figure}{{\bf 2D Simulation of the electrostatic potential produced by the electron gun}}\label{egun_simulation2.pdf}
-
-\end{center}
+\end{figure}
+
\pagebreak
--- /dev/null
+\subsection{Fourier Analysis of SEM Images}
+
+The two dimensional Discrete Fourier Transform is given by:
+\begin{align}
+ F(k_x, k_y) &= \displaystyle\sum_{x=0}^{N-1}\displaystyle\sum_{y=0}^{N-1} f(x, y) e^{\frac{-2 \pi i}{N}\left(k_x x + k_y y\right)} \label{dft}
+\end{align}
+
+Where $f(x, y)$ is a discrete data value (in this case the pixel intensity of the image) co-ordinates $(x, y)$, $N \times N$ are the dimensions of the image, and $F(k_x, k_y)$ gives the Fourier Coefficient. If the image represents a region with dimensions of $L \times L$, then the largest frequency components that can be contained in $F$ are $\frac{N}{L}$ \cite{}.
+
+
+Equation \eqref{dft} actually gives the Fourier coefficients of the infinite periodic extension of $f(x, y)$. If $f(x, y)$ is not periodic, then applying \eqref{dft} introduces extra high frequency components due to sharp discontinuities at the boundaries. These components are revealed as sharp lines running through the centre of the DFT images. Because the Black Au image has a greater contrast in intensity levels and therefore larger discontinuities are the boundaries, these lines are sharper in the Black Au DFT images.
+
+
+Windowing techniques may be used to reduce these high frequency components, however since this comes at a cost of reduced resolution we have not employed windowing here.
+
+\pagebreak
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_abs.png}
+ \caption{Amplitude density plot of DFT for Black Au SEM image}
+
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_abs.png}
+ \caption{Amplitude density plot of DFT for Au-Bright SEM image}
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_phase.png}
+ \caption{Phase density plot of DFT for Black Au SEM image}
+ \captionof[figure]{Amplitude density plot of DFT for Black Au}
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_phase.png}
+ \caption{Phase density plot of DFT for Au-Bright SEM image}
+\end{figure}
+
+
+
+
--- /dev/null
+\subsection{Fourier Analysis of SEM Images}
+
+The two dimensional Discrete Fourier Transform is given by:
+\begin{align}
+ F(k_x, k_y) &= \displaystyle\sum_{x=0}^{N-1}\displaystyle\sum_{y=0}^{N-1} f(x, y) e^{\frac{-2 \pi i}{N}\left(k_x x + k_y y\right)} \label{dft}
+\end{align}
+
+Where $f(x, y)$ is a discrete data value (in this case the pixel intensity of the image) co-ordinates $(x, y)$, $N \times N$ are the dimensions of the image, and $F(k_x, k_y)$ gives the Fourier Coefficient. If the image represents a region with dimensions of $L \times L$, then the largest frequency components that can be contained in $F$ are $\frac{N}{L}$ \cite{}.
+
+
+Equation \eqref{dft} actually gives the Fourier coefficients of the infinite periodic extension of $f(x, y)$. If $f(x, y)$ is not periodic, then applying \eqref{dft} introduces extra high frequency components due to sharp discontinuities at the boundaries. These components are revealed as sharp lines running through the centre of the DFT images. Because the Black Au image has a greater contrast in intensity levels, these lines are sharper in the Black Au DFT images.
+
+
+Windowing techniques may be used to reduce these high frequency components, however since this comes at a cost of reduced resolution we have not employed windowing here.
+
+\pagebreak
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_abs.png}
+ \caption{Amplitude density plot of DFT for Black Au SEM image}
+
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_abs.png}
+ \caption{Amplitude density plot of DFT for Au-Bright SEM image}
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_phase.png}
+ \caption{Phase density plot of DFT for Black Au SEM image}
+ \captionof[figure]{Amplitude density plot of DFT for Black Au}
+\end{figure}
+\begin{figure}[H]
+ \centering
+ \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_phase.png}
+ \caption{Phase density plot of DFT for Au-Bright SEM image}
+\end{figure}
+
+
+
+
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+
+
+
+
\label{siI_tcs.eps}
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+\section{Sources of Noise}
+
+
+
--- /dev/null
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+master-filename = ../thesis.tex
+
--- /dev/null
+[LATEX]
+master-filename = ../thesis.tex
+
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-\chapter{Conclusion}
+\chapter{Conclusions} \label{chapter_conclusion}
-We have demonstrated the use of multiple techniques for characterisation and analysis of metallic thin films\footnote{(We have?)}. In particular we have found measurable differences in the properties of metallic-black thin films in comparison with bright metallic thin films. We just don't know what to say about them yet.
+\begin{enumerate}
+
+\item We fabricated a range of nanostructured metallic thin films on both Si and glass substrates using evaporative techniques. These films have been characterised using a combination of electronic and optical spectroscopy techniques.
+
+\item Secondary electron microscopy analysis reveals striking differences in the structure of Au and Black Au films; Au films have been shown to consist of a regular periodic array of nanoparticles, whilst Black Au appears to consist of a highly randomised, porous mix of strand like structures.
+
+\item A Total Current Spectroscopy experiment for characterisation of samples in situ has been integrated with the technology for sample preparation. We used this setup to investigate elastic scattering of electrons as a function of film deposition.
+\begin{itemize}
+ \item Results for Black metal films deposited on existing layers of metal films suggest that the Black metal films present a sharper, more step like potential barrier to the primary electrons.
+ \item Further improvements may be made to the Total Current Specroscopy experiment with a possibility to investigate inelastic scattering processes occuring in the metallic thin films.
+\end{itemize}
+
+\item
+The optical properties of Black Au have been investigated and compared with those of Au.
+\begin{itemize}
+ \item Transmission spectroscopy experiments support existing evidence for a plateau in the infra-red.
+ \item We found a minima in the transmission spectrum of a Black Au film at around $370$nm; this minima is absent in the spectrum of a similar thickness Au film.
+\end{itemize}
+
+\item Ellipsometry has been used to determine the optical constants of thin films of Ag and Black Ag. These results show a significant peak in both the refractive index and extinction coefficient of the Black Ag film in the region of $350$ to $400$nm. These peaks are absent for the Ag sample.
+
+\end{enumerate}
-\chapter{Conclusion}
+\chapter{Conclusions} \label{chapter_conclusion}
-We have demonstrated the use of multiple techniques for characterisation and analysis of metallic thin films\footnote{(We have?)}. In particular we have found measurable differences in the properties of metallic-black thin films in comparison with bright metallic thin films. We just don't know what to say about them yet.
+\begin{enumerate}
+
+\item We fabricated a range of nanostructured metallic thin films on both Si and glass substrates using evaporative techniques. These films have been characterised using a combination of electronic and optical spectroscopy techniques.
+
+\item Secondary electron microscopy analysis reveals striking differences in the structure of Au and Black Au films; Au films have been shown to consist of a regular periodic array of nanoparticles, whilst Black Au appears to consist of a highly randomised, porous mix of strand like structures.
+
+\item A Total Current Spectroscopy experiment for characterisation of samples in situ has been integrated with the technology for sample preparation. We used this setup to investigate elastic scattering of electrons as a function of film deposition.
+\begin{itemize}
+ \item Results for Black metal films deposited on existing layers of metal films suggest that the Black metal films present a sharper, more step like potential barrier to the primary electrons.
+ \item Further improvements may be made to the Total Current Specroscopy experiment with a possibility to investigate inelastic scattering processes occuring in the metallic thin films.
+\end{itemize}
+
+\item
+The optical properties of Black Au have been investigated and compared with those of Au.
+\begin{itemize}
+ \item Transmission spectroscopy experiments support existing evidence for a plateau in the infra-red.
+ \item We found a minima in the transmission spectrum of a Black Au film at around $370$nm; this minima is absent in the spectrum of a similar thickness Au film.
+\end{itemize}
+
+\item Ellipsometry has been used to determine the optical constants of thin films of Ag and Black Ag. These results show a significant peak in both the refractive index and extinction coefficient of the Black Ag film in the region of $350$ to $400$nm. These peaks are absent for the Ag sample.
+
+\end{enumerate}
\relax
+\citation{faraday1857}
+\citation{garnet1904}
+\citation{mei1908}
+\citation{wriedt2008}
+\citation{atwater2010}
+\citation{linic2011}
+\citation{maksymov2011}
+\citation{maksymov2010}
\citation{pfund1930}
-\citation{pfund1933}
\citation{pfund1930}
-\citation{pfund1933}
\citation{harris1948}
\citation{harris1952}
\citation{harris1953}
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-\citation{sondergaard2012}
+\newlabel{chapter_introduction}{{1}{1}{Introduction\relax }{chapter.1}{}}
+\citation{panjwani2011}
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+\chapter{Introduction} \label{chapter_introduction}
-% TODO: Broad general sweeping statements about thin films
+Interest in the optical properties of nanostructured thin films can be traced back to the 19th century. In the 1857 Bakerian Lecture, Michael Faraday discussed a range of unusual optical effects exhibited by thin films of Au and other metals subjected to different treatements \cite{faraday1857}. The role of metallic nanoparticles of gold in producing the colours of stained glass was first investigated by Garnet in 1904 \cite{garnet1904} using Rayleigh's theory for scattering of light from spherical particles. A few years later, Gustav Mie developed a more complete theory of light scattering for spherical nanoparticles; Mie's theory is still widely used accross many disciplines \cite{mei1908} \cite{wriedt2008}.
-Motivation:
-\begin{itemize}
- \item The properties of solids can be understood in terms of an infinite periodic lattice
- \item In reality, every solid must have a finite spatial extent. The surface is extremely important because it is the interface for all physical/chemical interactions with the solid and its environment.
- \item Thin films can have extremely complicated and interesting properties.
- \item The characterisation of thin films is important research in electronics as the surface to volume ratio increases.
- \item Most recent research has been into constructing ``meta-materials'' which can be exploited for nanoscale applications. Eg: plasmonic based circuitry.
- \item Somehow link to metallic-black films (?)
-\end{itemize}
+Many of the properties investigated by Faraday are now understood in terms of the behaviour of the electron gas in a metal, and in particular the ability for thin metal films to support plasmonic resonance effects. A plasmon is a quasiparticle which describes the collective oscillation of conduction electrons in a metal. The behvaiour of plasmons is well understood in terms of classical models for a free electron gas; in the Lorentz model electrons are treated as damped harmonic oscillators. When light is incident on a metal, the electrons may collectively resonate in response to the sinusoidal forcing field.
+Recently there has been much interest in the exploitation of plasmonic effects in nanoscale devices for a bewildering array of applications from improvement of photovoltaic solar cell efficiency \cite{atwater2010,linic2011} to biosensing \cite{maksymov2011}, and even the potential for plasmonic based computing devices \cite{maksymov2010}. %The extremely rapid developement of the field of plasmonics during the last decade has been stimulated by advances in nano-fabrication technology \cite{}.
-\emph{More about metallic-black films}
+A fascinating phenomena first observed in the 1930s \cite{pfund1930} is the tendency for metal films deposited in high pressure\footnote{Of the order of $10^{-2}$mbar} atmospheres to appear completely black at visible wavelengths. Such films have found use in a range of optical applications as near perfect black bodies with very low thermal mass \cite{pfund1930,harris1948,harris1952,harris1953}.
-So called metallic-black films are the result of deposition of metal elements at a relatively high pressure (of the order of $10^{-2}$ mbar). The films are named due to their high absorbance at visible wavelengths; they appear black to the naked eye. There is a remarkable contrast between such films and films deposited under low pressure (less than $10^{-6}$mbar), which are typically highly reflective and brightly coloured.
+Recently, so called ``black metal'' films have been found to enhance the efficiency of thin film solar cells; this is consistent with the presence of plasmonic effects in the films \cite{panjwani2011}.
-% First mentions and early research; Pfund
-This phenomenom has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of metallic-blacks \cite{pfund1930}, and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared \cite{pfund1933}. More extensive research on the structural and optical properties of these films by Louis Harris and others during the 1940s and 1950s \cite{harris1948}, \cite{harris1952}, \cite{harris1953}.
+\begin{comment}
+Just several months ago, an ``artificially blackened'' plasmonic meta-material termed has been produced with similar applications in mind to those of the ``traditional'' black metal films. This technology has largely been motivated by the difficulty of theoretically modelling the traditional Black metal samples. \cite{sondergaard2012}.
+\end{comment}
-% Research by Harris concluding ``condensor'' like structure
-Harris et al. have produced experimental results of the transmission of metallic-black films from visible wavelengths to the far-infrared \cite{}. By modelling the film as a layer of metallic strands, acting as ``condensors'', Harris et al. arrived at an expression for the electron relaxation time of [element]-black \cite{}, leading to a a transmission spectrum in good agreement with experimental results.
+The aim of this project has been the preparation and characterisation of thin metal film samples, with a focus on black metal films. We have also investigated the possibility for plasmonic behaviour in Black metal films. We have prepared samples for subsequent study with both electronic and optical spectroscopic techniques.
-% Mckenzie
-Mckenzie has established that the presence of oxygen effects the optical and electrical properties of metallic-blacks \cite{mckenzie2006}.
+The remainder of this report will be organised as follows: in chapter \ref{chapter_overview} we will present an overview of past research into the characterisation of black metal films, followed by a brief explanation of plasmonic behaviour based on the Lorentz model. Chapter \ref{chapter_techniques} will give an overview of the two main experimental techniques employed during this study (Total Current Spectroscopy and Ellipsometry). In chapter \ref{chapter_results} we will present results and discussion of experiments, which will be followed with the conclusions of this study.
-% More recent research
-More recently, it was shown that Au-black coatings increased the efficiency of thin film solar cells \cite{}. In this study, a simulation approximating an Au-black film as a layer of semi-spherical structures showed plasmonic behaviour which lead to an increase in electric field behind the film.
-
-
-% Artificially ``blackened'' thin films
-Metallic-black films have proven useful in applications requiring efficient absorption of light, including the. Recently there has been interest in artificial ``blackening'' of metal surfaces in ways which simplify the characterisation of the surfaces for practical applications.
-
-Sondergaard et al. have produced metallic-black surfaces capable of suporting surface plasmon modes \cite{sondergaard2012}. These films exhibit similar optical properties to the previously considered ``evaporated'' metallic-black surfaces.
-
-% What I will be doing with metallic-black films
-This project will employ several techniques, including:Total Current Specroscopy; Ellipsometry and Optical Spectroscopy to investigate the difference between metallic films deposited at low pressure, and high pressure (metallic-blacks).
-
-This report will be organised as follows...
-You just read the introduction, which comes first. After that we talk about theory and then experimental stuff.
+\subsubsection*{A Note on Terminology}
+There is some possibility for confusion when referring to metal films evaporated at high pressure, which appear black at visible wavelengths, and metal films evaporated at low pressure, which are typically highly reflective. In the remainder of this report, we will refer to the former as ``black metal'' films and the latter simply as ``metal'' films (regardless of whether the film is thick enough for the colour to be visible to the naked eye).
-\chapter{Introduction}
+\chapter{Introduction} \label{chapter_introduction}
-% TODO: Broad general sweeping statements about thin films
+Interest in the optical properties of nanostructured thin films can be traced back to the 19th century. In the 1857 Bakerian Lecture, Michael Faraday discussed a range of unusual optical effects exhibited by thin films of Au and other metals subjected to different treatements \cite{faraday1857}. The role of metallic nanoparticles of gold in producing the colours of stained glass was first investigated by Garnet in 1904 \cite{garnet1904} using Rayleigh's theory for scattering of light from spherical particles. A few years later, Gustav Mie developed a more complete theory of light scattering for spherical nanoparticles; Mie's theory is still widely used accross many disciplines \cite{mei1908} \cite{wriedt2008}.
-Motivation:
-\begin{itemize}
- \item The properties of solids can be understood in terms of an infinite periodic lattice
- \item In reality, every solid must have a finite spatial extent. The surface is extremely important because it is the interface for all physical/chemical interactions with the solid and its environment.
- \item Thin films can have extremely complicated and interesting properties.
- \item The characterisation of thin films is important research in electronics as the surface to volume ratio increases.
- \item Most recent research has been into constructing ``meta-materials'' which can be exploited for nanoscale applications. Eg: plasmonic based circuitry.
- \item Somehow link to metallic-black films (?)
-\end{itemize}
+Many of the properties investigated by Faraday are now understood in terms of the behaviour of the electron gas in a metal, and in particular the ability for thin metal films to support plasmonic resonance effects. A plasmon is a quasiparticle which describes the collective oscillation of conduction electrons in a metal. The behvaiour of plasmons is well understood in terms of classical models for a free electron gas; in the Lorentz model electrons are treated as damped harmonic oscillators. When light is incident on a metal, the electrons may collectively resonate in response to the sinusoidal forcing field.
+Recently there has been much interest in the exploitation of plasmonic effects in nanoscale devices for a bewildering array of applications from improvement of photovoltaic solar cell efficiency \cite{atwater2010,linic2011} to biosensing \cite{maksymov2011}, and even the potential for plasmonic based computing devices \cite{maksymov2010}. %The extremely rapid developement of the field of plasmonics during the last decade has been stimulated by advances in nano-fabrication technology \cite{}.
-\emph{More about metallic-black films}
+A fascinating phenomena first observed in the 1930s \cite{pfund1930} is the tendency for metal films deposited in high pressure\footnote{Of the order of $10^{-2}$mbar} atmospheres to appear completely black at visible wavelengths. Such films have found use in a range of optical applications as near perfect black bodies with very low thermal mass \cite{pfund1930,harris1948,harris1952,harris1953}.
-So called metallic-black films are the result of deposition of metal elements at a relatively high pressure (of the order of $10^{-2}$ mbar). The films are named due to their high absorbance at visible wavelengths; they appear black to the naked eye. There is a remarkable contrast between such films and films deposited under low pressure (less than $10^{-6}$mbar), which are typically highly reflective and brightly coloured.
+Recently, so called ``black metal'' films have been found to enhance the efficiency of thin film solar cells; this is consistent with the presence of plasmonic effects in the films \cite{panjwani2011}.
-% First mentions and early research; Pfund
-This phenomenom has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of metallic-blacks \cite{pfund1930}, and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared \cite{pfund1933}. More extensive research on the structural and optical properties of these films by Louis Harris and others during the 1940s and 1950s \cite{harris1948}, \cite{harris1952}, \cite{harris1953}.
+\begin{comment}
+Just several months ago, an ``artificially blackened'' plasmonic meta-material termed has been produced with similar applications in mind to those of the ``traditional'' black metal films. This technology has largely been motivated by the difficulty of theoretically modelling the traditional Black metal samples. \cite{sondergaard2012}.
-% Research by Harris concluding ``condensor'' like structure
-Harris et al. have produced experimental results of the transmission of metallic-black films from visible wavelengths to the far-infrared \cite{}. By modelling the film as a layer of metallic strands, acting as ``condensors'', Harris et al. arrived at an expression for the electron relaxation time of [element]-black \cite{}, leading to a a transmission spectrum in good agreement with experimental results.
+The aim of this project has been the preparation and characterisation of thin metal film samples, with a focus on black metal films. We have also investigated the possibility for plasmonic behaviour in Black metal films. We have prepared samples for subsequent study with both electronic and optical spectroscopic techniques.
-% Mckenzie
-Mckenzie has established that the presence of oxygen effects the optical and electrical properties of metallic-blacks \cite{mckenzie2006}.
+The remainder of this report will be organised as follows: in chapter \ref{chapter_overview} we will present an overview of past research into the characterisation of black metal films, followed by a brief explanation of plasmonic behaviour based on the Lorentz model. Chapter \ref{chapter_techniques} will give an overview of the two main experimental techniques employed during this study (Total Current Spectroscopy and Ellipsometry). In chapter \ref{chapter_results} we will present results and discussion of experiments, which will be followed with the conclusions of this study.
-% More recent research
-More recently, it was shown that Au-black coatings increased the efficiency of thin film solar cells \cite{}. In this study, a simulation approximating an Au-black film as a layer of semi-spherical structures showed plasmonic behaviour which lead to an increase in electric field behind the film.
-
-
-% Artificially ``blackened'' thin films
-Metallic-black films have proven useful in applications requiring efficient absorption of light, including the. Recently there has been interest in artificial ``blackening'' of metal surfaces in ways which simplify the characterisation of the surfaces for practical applications.
-
-Sondergaard et al. have produced metallic-black surfaces capable of suporting surface plasmon modes \cite{sondergaard2012}. These films exhibit similar optical properties to the previously considered ``evaporated'' metallic-black surfaces.
-
-% What I will be doing with metallic-black films
-This project will employ several techniques, including:Total Current Specroscopy; Ellipsometry and Optical Spectroscopy to investigate the difference between metallic films deposited at low pressure, and high pressure (metallic-blacks).
+\subsubsection*{A Note on Terminology}
+There is some possibility for confusion when referring to metal films evaporated at high pressure, which appear black at visible wavelengths, and metal films evaporated at low pressure, which are typically highly reflective. In the remainder of this report, we will refer to the former as ``black metal'' films and the latter simply as ``metal'' films (regardless of whether the film is thick enough for the colour to be visible to the naked eye).
--- /dev/null
+\relax
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+\citation{pfund1933}
+\citation{harris1948}
+\citation{harris1952}
+\citation{panjwani2011}
+\citation{mckenzie2006}
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+\citation{oates2011}
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+\citation{ferrel1958}
+\citation{oates2011}
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+\citation{oates2011}
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+\citation{bohm1953}
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+\citation{oates2011}
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+\citation{oates2011}
+\@writefile{lof}{\contentsline {figure}{\numberline {2.1}{\ignorespaces Illustration of the charge distribution and electric fields of a surface plasmon polariton taken from Oates et al. \cite {oates2011}\relax }}{7}{figure.caption.6}}
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--- /dev/null
+\chapter{Overview} \label{chapter_overview}
+
+\section{Black Metal Films}
+
+So called black metal films\footnote{Naming conventions vary in the literature} are the result of deposition of metal elements at a relatively high pressure\footnote{of the order of $10^{-2}$ mbar} or ``bad vacuum''. The films are named due to their high absorbance at visible wavelengths; a sufficiently thick film will appear black to the naked eye. There is a remarkable contrast between such films and metal films deposited under low pressure\footnote{less than $10^{-5}$mbar}, which are typically highly reflective and brightly coloured at comparable thicknesses. It has been established that Black metal films may be prepared in any gas, but when oxygen is present the resulting films contain tungsten oxides due to the use of tungsten heating filaments for the deposition of films\cite{harris1952} \cite{mckenzie2006}.
+
+% First mentions and early research; Pfund
+The formation of black-metal films at high pressure has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s, motivated by the potential application of black-metal films to radiometetric devices \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of black-metals and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared. Subsequent researchers have also focused on measuring the properties of black-metal films as a function of preparation conditions, with the aim of producing selective filters for infra-red detectors. \cite{harris1948} \cite{harris1952}. More recently, it was shown that black-Au coatings can be used to increase the efficiency of thin film solar cells \cite{panjwani2011}.
+
+There have been several attempts to relate the structure of black-metal films to measured optical and electrical properties. Metallic nanostructured films deposited at low pressures generally consist of a series of metallic islets; for such films, Mie theories of scattering are often used. However, it is clear that black-metal films usually consist of a highly irregular strandlike structure; Mie theories fail to accurately predict the optical properties of such films \cite{mckenzie2006}.
+
+Harris et al. have produced experimental results of the transmission of black-metal films from visible wavelengths to the far-infrared. By modelling black-metal films as consisting of layers of ``yarn like'' metal strands, Harris et al. have arrived at an expression for the electron relaxation time of Au-black, leading to a calculated transmission spectrum in good agreement with experimental results \cite{harris1953}.
+
+
+% Artificially ``blackened'' thin films
+The optical properties of black-metal films have been found to vary due to changes in structure when the film is exposed to atmosphere, or is heated \cite{advena1993}. This ``degradation'' of the black-metal films is inconvenient for maintaining consistent calibration of devices. Recently there has been interest in artificial ``blackening'' of metal surfaces for optical applications. These ``meta-materials'' offer a promising alternative to the traditional black-metal films, due to the ability to more precisely control properties of the film. In particular, artifially blackened metal films have been produced which suppress reflection of light via surface plasmon resonances \cite{sondergaard2012}.
+
+In light of the wealth of previous research, the aims of this project were first to reproduce black-metal films using equipment available in the CAMSP research group, and then employ several techniques for the study of these samples in comparison with other metal films. Most of the existing research has been conducted using optical transmission or reflection spectroscopy techniques. A total current secondary electron spectroscopy experiment was therefore integrated into the sample preparation vacuum chamber, to allow for almost immediate study of prepared samples using this technique. A Variable Angle Spectroscopic Ellipsometer (VASE) has been used in an attempt to relate the optical and structural properties of the samples. We have also used optical transmission spectroscopy at visible wavelengths to characterise the transmission of black-metal films.
+
+
+\section{Plasmonics}
+
+Since optical properties of nanostructured films are often determined by plasmon-photon interaction, a brief description will be given of plasmonic behaviour in such films. Generally the optical properties of a metal are modelled using a combination of classical and quantum theories. For noble metals (eg: Au and Ag), conduction band electrons are well described by free electron gas models \cite{oates2011}.
+
+\subsection{Bulk Plasmons}
+
+In the Lorentz model, electrons responding to incident light are modelled as non-interacting, damped and forced harmonic oscillators. For each electron:
+\begin{align}
+ m \frac{d^2 \vect{x}}{dt^2} &= -m_e \Gamma \der{\vect{x}}{t} - m_e \omega_0^2 \vect{x} - e \vect{E_0} e^{-i\omega t} \label{lorentz}
+\end{align}
+where $m$ is the electron mass, $\vect{x}$ is the displacement of the electron from equilibrium, $\Gamma$ is the damping constant, $-m \omega_0^2 \vect{x}$ is the restoring force, and $-e \vect{E_0} e^{-i\omega t}$ is the forcing term due to an incident plane wave of frequency $\omega$.
+
+The polarisation density $\vect{P}$\footnote{Not to be confused with the polarisation state of light} of the electron gas describes the material's response to the incident light. It can be writen as \cite{oates2011}:
+\begin{align*}
+ \vect{P} &= \phasor{\epsilon} \vect{E} = -e N \vect{x}(t)
+\end{align*}
+Where $\phasor{\epsilon}$ is the psuedo-dielectric constant and $N$ is the number of electrons per unit volume.
+
+Solving \label{lorentz} for $\vect{x}(t)$ gives the Lorentz Oscillator expression:
+\begin{align*}
+ \phasor{\epsilon}(\omega) &= 1 + \frac{e^2 N}{\epsilon_0 m} \frac{1}{\omega_0^2 - \omega^2 - i \Gamma \omega}
+\end{align*}
+
+In the noble metals (Au, Ag, etc), conduction electrons are extremely loosely bound. The Drude model, which neglects the restoring force, is a good model for electron behaviour in these metals. In this case, $\omega_0 = 0$, and:
+\begin{align*}
+ \phasor{\epsilon}(\omega) &= 1 - \frac{\omega_p^2}{\omega^2 + \Gamma^2} + i \frac{\omega_p^2 \Gamma}{\omega(\omega^2 + \Gamma^2)}
+\end{align*}
+where the Drude Plasma frequency $\omega_p$ is:
+\begin{align*}
+ \omega_p &= \sqrt{\frac{e^2 N}{\epsilon_0 m}}
+\end{align*}
+
+If $\Gamma$ is small, (as for the noble metals), then as $\omega$ approaches $\omega_{p}$, the real part of $\phasor{\epsilon}$ approaches zero, and longitudinal oscillating waves may propagate through the material \cite{oates2011}. These oscillations are called ``Bulk'' or ``Volume'' plasmons. They were first excited in Electron Energy Loss Spectroscopy (EELS) experiments by Ferrel in 1958 \cite{ferrel1958}.
+
+In real metals, interband transitions contribute to $\phasor{\epsilon}$. The ``screened'' plasmon frequency is given by:
+\begin{align}
+ \omega_{sp}^2 &= \frac{\omega_p^2}{\epsilon_\infty} - \Gamma^2 \label{screened_plasmon}
+\end{align}
+where $\epsilon_\infty$ is a constant representing the real part of $\phasor{\epsilon}$ with the contribution of interband transitions.
+The accuracy of this formula decreases as $\hbar \omega$ approaches the energy for interband transitions. \cite{oates2011}.
+
+From \eqref{screened_plasmon}, it can be seen that interband transitions effectively reduce the frequency at which bulk plasmons are excited. For example, in Ag $\epsilon_\infty \approx 4$ and $\hbar \omega_{sp} = 2.8$ eV. Observed values for the bulk plasmon frequency in Ag are typically $\hbar \omega = 3.8\text{ eV}$ \cite{kittel}. Ag's relatively low plasmon threshold energy makes it a material of choice for plasmonic meta-material applications \cite{oates2011}.
+
+
+
+\subsection{Surface Plasmons}
+
+One of the most important developments leading to the modern field of plasmonics has been the prediction of so called Surface Plasmons (SP) in 1957 by Ritchie \cite{ritchie1957}. In his paper, Ritchie predicted surface plasmons as the mechanism for energy loss of electrons passing through a thin film, building on previous work by Pines and Bohm \cite{bohm1951} \cite{bohm1952} \cite{bohm1953}. Ritchie's prediction was experimentally verified here at UWA by Cedric Powel and John Swan just three years later \cite{powel1959}.
+
+A coupled Surface Plasmon and Photon are referred to as a Surface Plasmon Polariton (SPP). The behaviour of SPPs can be derived by solving Maxwell's equations for $p$ (parallel to the plane of incidence) and $s$ (parallel to the surface) polarised light at the interface between a metal and a dielectric \cite{pitark2007}.
+
+The Surface plasmon frequency is given by:
+\begin{align*}
+ \omega_{s} &= \frac{\omega_p}{\sqrt{1 + \epsilon_a}}
+\end{align*}
+where $\epsilon_a$ is the dielectric constant for the dielectric. For air, $\epsilon_a = 1$ and $\omega_{s} = \frac{\omega_p}{\sqrt{2}}$
+
+Theoretically, SPPs can only couple to $p$ polarised light. This makes Ellipsometry, which measures the change in polarisation of reflected light, a useful technique for detecting excitation of SPPs \cite{oates2011}.
+
+In order to excite an SPP in a flat surface, some form of ``third body'' is required to match the wavevector of the photon with the plasmon. The Kretchsman configuration is one possible method, in which light is totally internally reflected at the interface between a glass prism and one side of the metal film. The evanescent fields created at the interface between a thin film and the glass may lead to the excitation of a SPP on the other side of the thin film.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.6\textwidth]{figures/plasmon/spp.png}
+ \caption{Illustration of the charge distribution and electric fields of a surface plasmon polariton taken from Oates et al. \cite{oates2011}}
+\end{figure}
+
+\subsection{Surface Plasmon Resonances}
+
+Due to different boundary conditions, a nanostructured surface exhibits very different plasmonic effects to a smooth surface.
+Although the term ``plasmon'' was not coined until the 1950s, Mie's solution for scattering of light from spherical nanoparticles does incorporate the Drude model, and predicts resonance of the free electron gas inside the metal spheres. These are now refered to as Mie plasmons, or surface plasmon resonances (SPR) \cite{pitark2007,oates2011}. The frequency of these resonances is:
+\begin{align}
+ \omega_{pp}^2 &= \frac{\omega_p^2}{\epsilon_\infty + 2 \epsilon_a} - \Gamma^2
+\end{align}
+For a pure Drude metal, this reduces to $\omega_{pp} = \frac{\omega_p}{\sqrt{3}}$. Light of frequency $\omega_{pp}$ is preferentially scattered.
--- /dev/null
+\chapter{Overview} \label{chapter_overview}
+
+\section{Black Metal Films}
+
+So called black metal films\footnote{Naming conventions vary in the literature} are the result of deposition of metal elements at a relatively high pressure\footnote{of the order of $10^{-2}$ mbar} or ``bad vacuum''. The films are named due to their high absorbance at visible wavelengths; a sufficiently thick film will appear black to the naked eye. There is a remarkable contrast between such films and metal films deposited under low pressure\footnote{less than $10^{-5}$mbar}, which are typically highly reflective and brightly coloured at comparable thicknesses. It has been established that Black metal films may be prepared in any gas, but when oxygen is present the resulting films contain tungsten oxides due to the use of tungsten heating filaments for the deposition of films\cite{harris1952} \cite{mckenzie2006}.
+
+% First mentions and early research; Pfund
+The formation of black-metal films at high pressure has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s, motivated by the potential application of black-metal films to radiometetric devices \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of black-metals and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared. Subsequent researchers have also focused on determining measuring the properties of black-metal films as a function of preparation conditions, with the aim of producing selective filters for infra-red detectors. \cite{harris1948} \cite{harris1952}. More recently, it was shown that black-Au coatings can be used to increase the efficiency of thin film solar cells \cite{panjwani2011}.
+
+There have been several attempts to relate the structure of black-metal films to measured optical and electrical properties. Metallic nanostructured films deposited at low pressures generally consist of a series of metallic islets; for such films, Mie theories of scattering are often used. However it is clear that black-metal films usually consist of a highly irregular strandlike structure; Mie theories fail to accurately predict the optical properties of all such films \cite{mckenzie2006}.
+
+Harris et al. have produced experimental results of the transmission of black-metal films from visible wavelengths to the far-infrared. By modelling black-metal films as consisting of layers of ``yarn like'' metal strands, Harris et al. have arrived at an expression for the electron relaxation time of Au-black, leading to a calculated transmission spectrum in good agreement with experimental results \cite{harris1953}.
+
+
+% Artificially ``blackened'' thin films
+The optical properties of black-metal films have been found to vary due to changes in structure when the film is exposed to atmosphere, or heated \cite{advena1993}. This ``degradation'' of the black-metal films is inconvenient for maintaining consistent calibration of devices. Recently there has been interest in artificial ``blackening'' of metal surfaces for optical applications. These ``meta-materials'' offer a promising alternative to the traditional black-metal films, due to the ability to more precisely control properties of the film. In particular, artifially blackened metal films have been produced which suppress reflection of light via surface plasmon resonances \cite{sondergaard2012}.
+
+In light of the wealth of previous research, the aims of this project were first to reproduce black-metal films using equipment available at CAMSP, and then employ several techniques for the study of these samples in comparison with other metal films. Most of the existing research has been conducted using optical transmission or reflection spectroscopy techniques. A total current secondary electron spectroscopy experiment was therefore integrated into the sample preparation vacuum chamber, to allow for almost immediate study of prepared samples using this technique. A Variable Angle Spectroscopic Ellipsometer (VASE) has been used in an attempt to relate the optical and structural properties of the samples. We have also used optical transmission spectroscopy at visible wavelengths to characterise the transmission of black-metal films.
+
+
+\section{Plasmonics}
+
+Since optical properties of nanostructured films are often determined plasmon-photon interaction, we will briefly give a description of plasmonic behaviour in such films. Generally the optical properties of a metal are modelled using a combination of classical and quantum theories. For noble metals (eg: Au and Ag), conduction band electrons are well described by free electron gas models \cite{oates2011}.
+
+\subsection{Bulk Plasmons}
+
+In the Lorentz model, electrons responding to incident light are modelled as uninteracting, damped and forced harmonic oscillators. For each electron:
+\begin{align}
+ m \frac{d^2 \vect{x}}{dt^2} &= -m_e \Gamma \der{\vect{x}}{t} - m_e \omega_0^2 \vect{x} - e \vect{E_0} e^{-i\omega t} \label{lorentz}
+\end{align}
+Where $m$ is the electron mass, $\vect{x}$ is the displacement of the electron from equilibrium, $\Gamma$ is the damping constant, $-m \omega_0^2 \vect{x}$ is the restoring force, and $-e \vect{E_0} e^{-i\omega t}$ is the forcing term due to an incident plane wave of frequency $\omega$.
+
+The polarisation $\vect{P}$ of the electron gas describes the material's response to the incident light. It can be writen as:
+\begin{align*}
+ \vect{P} &= \phasor{\epsilon} \vect{E} = -e N \vect{x}(t)
+\end{align*}
+Where $\phasor{\epsilon}$ is the psuedo-dielectric constant and $N$ is the number of electrons per unit volume.
+
+Solving \label{lorentz} for $\vect{x}(t)$ gives the Lorentz Oscillator expression:
+\begin{align*}
+ \phasor{\epsilon}(\omega) &= 1 + \frac{e^2 N}{\epsilon_0 m} \frac{1}{\omega_0^2 - \omega^2 - i \Gamma \omega}
+\end{align*}
+
+In the noble metals (Au, Ag, etc), conduction electrons are extremely loosely bound. The Drude-Sommerfield model, which neglects the restoring force, may be used to describe electron behaviour. In this case, $\omega_0 = 0$, and:
+\begin{align*}
+ \epsilon(\omega) &= 1 - \frac{\omega_p^2}{\omega^2 + \Gamma^2} + i \frac{\omega_p^2 \Gamma}{\omega(\omega^2 + \Gamma^2)}
+\end{align*}
+Where the Drude Plasma frequency $\omega_p$ is:
+\begin{align*}
+ \omega_p &= \sqrt{\frac{e^2 N}{\epsilon_0 m}}
+\end{align*}
+
+As $\omega$ approaches $\omega_{p}$, the real part of $\phasor{\epsilon}$ approaches zero. If $\Gamma$ is small (as for the noble metals), then $\phasor{\epsilon} \equiv \epsilon \to 0$ and longitudinal oscillating waves may propagate through the material. These oscillations are called ``Bulk'' or ``Volume'' plasmons. They were first excited in Electron Energy Loss Spectroscopy (EELS) experiments by Ferrel in 1958 \cite{ferrel1958}.
+
+In real metals, interband transitions contribute to $\phasor{\epsilon}$. The ``screened'' plasmon frequency is given by:
+\begin{align}
+ \omega_{sp}^2 &= \frac{\omega_p^2}{\epsilon_\infty} - \Gamma^2 \label{screened_plasmon}
+\end{align}
+Where $\epsilon_\infty$ is a constant representing real part of $\phasor{\epsilon}$ with the contribution of interband transitions.
+The accuracy of this formula decreases as $\hbar \omega$ approaches the energy for interband transitions. \cite{oates2011}.
+
+From \eqref{screened_plasmon}, it can be seen that interband transitions effectively reduce the frequency at which bulk plasmons are excited. For example, in Ag $\epsilon_\infty \approx 4$ and $\hbar \omega_{sp} = 2.8$. Observed values for the bulk plasmon frequency in Ag are typically $\hbar \omega = 3.8\text{eV}$ \cite{kittel}. Ag's relatively low plasmon threshold energy makes it a material of choice for plasmonic meta-material applications \cite{oates2011}.
+
+\subsection{Plasmon Polaritons}
+
+Plasmons may either
+
+\subsection{Surface Plasmons}
+
+One of the most important developments leading to the modern field of plasmonics has been the prediction of so called Surface Plasmons (SP) in 1957 by Ritchie \cite{ritchie1957}. In his paper, Ritchie predicted surface plasmons as the mechanism for energy loss of electrons passing through a thin film, building on previous work by Pines and Bohm \cite{bohm1951} \cite{bohm1952} \cite{bohm1953}. Ritchie's prediction was experimentally verified here at UWA by Cedric Powel and John Swan just three years later \cite{powel1959}.
+
+A coupled Surface Plasmon and Photon are referred to as a Surface Plasmon Polariton (SPP). The behaviour of SPPs can be derived by solving Maxwell's equations for $p$ and $s$ polarised light\footnote{With the electric field being parallel to and perpendicular to the plane of the surface respectively} at the interface between a metal and a dielectric \cite{pitark2007}. If the dielectric constant of the dielectric is $\epsilon_a$
+
+The Surface plasmon frequency is given by:
+\begin{align*}
+ \omega_{sp} &= \frac{\omega_p}{\sqrt{1 + \epsilon_a}}
+\end{align*}
+where $\epsilon_a$ is the dielectric constant for the dielectric. For air, $\epsilon_a = 1$ and $\omega_{sp} = \frac{\omega_p}{\sqrt{2}}$
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/plasmon/spp.png}
+ \caption{Schematic of the charge distribution and electric fields of a surface plasmon polariton taken from Oates et al. \cite{oates2011}}
+\end{figure}
+
+For an idealised flat surface, only the $p$ polarised
+
+May be excited by $p$ polarised light
+Generally need to couple the wavevector of the photon to the plasmon; in thin films this may occur due to surface roughness. In bulk materials the Kretschman configuration is used. Possibility to detect directly with the ellipsometer by measuring a dip in $s$ polarised reflection.
+
+Surface plasmons cannot be excited directly by light, due to the requirement for ``coupling'' of a photon wavevector with the. In the Kretchsman configuration, a
+
+\subsection{Plasmons in Nanostructured Materials}
+
+Nanostructured surfaces can exhibit extremely different optical properties to a flat surface. This is due to the differences in boundary conditions for light incident on a roughened interface.
+
+Although the term ``plasmon'' was not coined until the 1950s, Mie's solution for scattering of light from spherical nanoparticles does incorporate the Drude model, and predicts resonance of the free electron gas inside the metal spheres. These resonances are now referred to variously as localized SPR, localized SPP, Mie plasmon polaritons, particle plasmon polaritons, or particle plasmon resonances \cite{pitark2007,oates2011}. The frequency of
+
+
+
+
--- /dev/null
+\chapter{Overview} \label{chapter_overview}
+
+\section{Black Metal Films}
+
+So called black metal films\footnote{Naming conventions vary in the literature} are the result of deposition of metal elements at a relatively high pressure\footnote{of the order of $10^{-2}$ mbar} or ``bad vacuum''. The films are named due to their high absorbance at visible wavelengths; a sufficiently thick film will appear black to the naked eye. There is a remarkable contrast between such films and metal films deposited under low pressure\footnote{less than $10^{-5}$mbar}, which are typically highly reflective and brightly coloured at comparable thicknesses. It has been established that Black metal films may be prepared in any gas, but when oxygen is present the resulting films contain tungsten oxides due to the use of tungsten heating filaments for the deposition of films\cite{harris1952} \cite{mckenzie2006}.
+
+% First mentions and early research; Pfund
+The formation of black-metal films at high pressure has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s, motivated by the potential application of black-metal films to radiometetric devices \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of black-metals and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared. Subsequent researchers have also focused on measuring the properties of black-metal films as a function of preparation conditions, with the aim of producing selective filters for infra-red detectors. \cite{harris1948} \cite{harris1952}. More recently, it was shown that black-Au coatings can be used to increase the efficiency of thin film solar cells \cite{panjwani2011}.
+
+There have been several attempts to relate the structure of black-metal films to measured optical and electrical properties. Metallic nanostructured films deposited at low pressures generally consist of a series of metallic islets; for such films, Mie theories of scattering are often used. However, it is clear that black-metal films usually consist of a highly irregular strandlike structure; Mie theories fail to accurately predict the optical properties of such films \cite{mckenzie2006}.
+
+Harris et al. have produced experimental results of the transmission of black-metal films from visible wavelengths to the far-infrared. By modelling black-metal films as consisting of layers of ``yarn like'' metal strands, Harris et al. have arrived at an expression for the electron relaxation time of Au-black, leading to a calculated transmission spectrum in good agreement with experimental results \cite{harris1953}.
+
+
+% Artificially ``blackened'' thin films
+The optical properties of black-metal films have been found to vary due to changes in structure when the film is exposed to atmosphere, or is heated \cite{advena1993}. This ``degradation'' of the black-metal films is inconvenient for maintaining consistent calibration of devices. Recently there has been interest in artificial ``blackening'' of metal surfaces for optical applications. These ``meta-materials'' offer a promising alternative to the traditional black-metal films, due to the ability to more precisely control properties of the film. In particular, artifially blackened metal films have been produced which suppress reflection of light via surface plasmon resonances \cite{sondergaard2012}.
+
+In light of the wealth of previous research, the aims of this project were first to reproduce black-metal films using equipment available in the CAMSP research group, and then employ several techniques for the study of these samples in comparison with other metal films. Most of the existing research has been conducted using optical transmission or reflection spectroscopy techniques. A total current secondary electron spectroscopy experiment was therefore integrated into the sample preparation vacuum chamber, to allow for almost immediate study of prepared samples using this technique. A Variable Angle Spectroscopic Ellipsometer (VASE) has been used in an attempt to relate the optical and structural properties of the samples. We have also used optical transmission spectroscopy at visible wavelengths to characterise the transmission of black-metal films.
+
+
+\section{Plasmonics}
+
+Since optical properties of nanostructured films are often determined by plasmon-photon interaction, a brief description will be given of plasmonic behaviour in such films. Generally the optical properties of a metal are modelled using a combination of classical and quantum theories. For noble metals (eg: Au and Ag), conduction band electrons are well described by free electron gas models \cite{oates2011}.
+
+\subsection{Bulk Plasmons}
+
+In the Lorentz model, electrons responding to incident light are modelled as non-interacting, damped and forced harmonic oscillators. For each electron:
+\begin{align}
+ m \frac{d^2 \vect{x}}{dt^2} &= -m_e \Gamma \der{\vect{x}}{t} - m_e \omega_0^2 \vect{x} - e \vect{E_0} e^{-i\omega t} \label{lorentz}
+\end{align}
+where $m$ is the electron mass, $\vect{x}$ is the displacement of the electron from equilibrium, $\Gamma$ is the damping constant, $-m \omega_0^2 \vect{x}$ is the restoring force, and $-e \vect{E_0} e^{-i\omega t}$ is the forcing term due to an incident plane wave of frequency $\omega$.
+
+The polarisation density $\vect{P}$\footnote{Not to be confused with the polarisation state of light} of the electron gas describes the material's response to the incident light. It can be writen as:
+\begin{align*}
+ \vect{P} &= \phasor{\epsilon} \vect{E} = -e N \vect{x}(t)
+\end{align*}
+Where $\phasor{\epsilon}$ is the psuedo-dielectric constant and $N$ is the number of electrons per unit volume.
+
+Solving \label{lorentz} for $\vect{x}(t)$ gives the Lorentz Oscillator expression:
+\begin{align*}
+ \phasor{\epsilon}(\omega) &= 1 + \frac{e^2 N}{\epsilon_0 m} \frac{1}{\omega_0^2 - \omega^2 - i \Gamma \omega}
+\end{align*}
+
+In the noble metals (Au, Ag, etc), conduction electrons are extremely loosely bound. The Drude model, which neglects the restoring force, is a good model for electron behaviour in these metals. In this case, $\omega_0 = 0$, and:
+\begin{align*}
+ \phasor{\epsilon}(\omega) &= 1 - \frac{\omega_p^2}{\omega^2 + \Gamma^2} + i \frac{\omega_p^2 \Gamma}{\omega(\omega^2 + \Gamma^2)}
+\end{align*}
+where the Drude Plasma frequency $\omega_p$ is:
+\begin{align*}
+ \omega_p &= \sqrt{\frac{e^2 N}{\epsilon_0 m}}
+\end{align*}
+
+If $\Gamma$ is small, (as for the noble metals), then as $\omega$ approaches $\omega_{p}$, the real part of $\phasor{\epsilon}$ approaches zero, and longitudinal oscillating waves may propagate through the material \cite{oates2011}. These oscillations are called ``Bulk'' or ``Volume'' plasmons. They were first excited in Electron Energy Loss Spectroscopy (EELS) experiments by Ferrel in 1958 \cite{ferrel1958}.
+
+In real metals, interband transitions contribute to $\phasor{\epsilon}$. The ``screened'' plasmon frequency is given by:
+\begin{align}
+ \omega_{sp}^2 &= \frac{\omega_p^2}{\epsilon_\infty} - \Gamma^2 \label{screened_plasmon}
+\end{align}
+where $\epsilon_\infty$ is a constant representing the real part of $\phasor{\epsilon}$ with the contribution of interband transitions.
+The accuracy of this formula decreases as $\hbar \omega$ approaches the energy for interband transitions. \cite{oates2011}.
+
+From \eqref{screened_plasmon}, it can be seen that interband transitions effectively reduce the frequency at which bulk plasmons are excited. For example, in Ag $\epsilon_\infty \approx 4$ and $\hbar \omega_{sp} = 2.8$ eV. Observed values for the bulk plasmon frequency in Ag are typically $\hbar \omega = 3.8\text{ eV}$ \cite{kittel}. Ag's relatively low plasmon threshold energy makes it a material of choice for plasmonic meta-material applications \cite{oates2011}.
+
+
+
+\subsection{Surface Plasmons}
+
+One of the most important developments leading to the modern field of plasmonics has been the prediction of so called Surface Plasmons (SP) in 1957 by Ritchie \cite{ritchie1957}. In his paper, Ritchie predicted surface plasmons as the mechanism for energy loss of electrons passing through a thin film, building on previous work by Pines and Bohm \cite{bohm1951} \cite{bohm1952} \cite{bohm1953}. Ritchie's prediction was experimentally verified here at UWA by Cedric Powel and John Swan just three years later \cite{powel1959}.
+
+A coupled Surface Plasmon and Photon are referred to as a Surface Plasmon Polariton (SPP). The behaviour of SPPs can be derived by solving Maxwell's equations for $p$ (parallel to the plane of incidence) and $s$ (parallel to the surface) polarised light at the interface between a metal and a dielectric \cite{pitark2007}.
+
+The Surface plasmon frequency is given by:
+\begin{align*}
+ \omega_{s} &= \frac{\omega_p}{\sqrt{1 + \epsilon_a}}
+\end{align*}
+where $\epsilon_a$ is the dielectric constant for the dielectric. For air, $\epsilon_a = 1$ and $\omega_{s} = \frac{\omega_p}{\sqrt{2}}$
+
+Theoretically, SPPs can only couple to $p$ polarised light. This makes Ellipsometry, which measures the change in polarisation of reflected light, a useful technique for detecting excitation of SPPs \cite{oates2011}.
+
+In order to excite an SPP in a flat surface, some form of ``third body'' is required to match the wavevector of the photon with the plasmon. The Kretchsman configuration is one possible method, in which light is totally internally reflected at the interface between a glass prism and one side of the metal film. The evanescent fields created at the interface between a thin film and the glass may lead to the excitation of a SPP on the other side of the thin film.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.6\textwidth]{figures/plasmon/spp.png}
+ \caption{Illustration of the charge distribution and electric fields of a surface plasmon polariton taken from Oates et al. \cite{oates2011}}
+\end{figure}
+
+\subsection{Surface Plasmon Resonances}
+
+Due to different boundary conditions, a nanostructured surface exhibits very different plasmonic effects to a smooth surface.
+Although the term ``plasmon'' was not coined until the 1950s, Mie's solution for scattering of light from spherical nanoparticles does incorporate the Drude model, and predicts resonance of the free electron gas inside the metal spheres. These are now refered to as Mie plasmons, or surface plasmon resonances (SPR) \cite{pitark2007,oates2011}. The frequency of these resonances is:
+\begin{align}
+ \omega_{pp}^2 &= \frac{\omega_p^2}{\epsilon_\infty + 2 \epsilon_a} - \Gamma^2
+\end{align}
+For a pure Drude metal, this reduces to $\omega_{pp} = \frac{\omega_p}{\sqrt{3}}$. Light of frequency $\omega_{pp}$ is preferentially scattered.
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-\chapter{Results and Discussion}
+\chapter{Experimental Results and Discussion} \label{chapter_results}
+
\section{Scanning Electron Microscopy}
-A number of samples of metallic-black and metallic-bright films were sent to the Centre for Microscopy Characterisation and Analysis (CMCA) at UWA for study. In this section we will present and discuss some of the images produced by CMCA. These images provide an invaluable aid to understanding the structural differences between metallic-black and metallic-bright films.
+A number of samples of black and non-black metal films were prepared and sent to the Centre for Microscopy Characterisation and Analysis (CMCA) at UWA for study. In this section we will present and discuss two of the images produced by CMCA. These images proved to be an invaluable aid in understanding the structural differences between metallic-black and metallic-bright films.
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.7\textwidth]{figures/sem/Au_semi-shiny_1_SEM.png}
+ \caption{SEM Image of a Au film. Pressure of preparation $10^{-6}$ mbar. Dimensions approx. 2500 x 1900 nm}
+ \label{sem_au}
+\end{figure}
-Figure \ref{SEM_images} shows a comparison of an Au-Black and Au-Bright film imaged using a scanning electron microscope (SEM). The intensity of each pixel is proportional to the total current of secondary electrons scattered from the surface at that point from the metal in the film (the current due to the Si substrate has been subtracted from the image), which is in turn proportional to the density of metal at the considered point.
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.7\textwidth]{figures/sem/Au_BLACK_200nm.png}
+ \caption{SEM Image of a Black Au film. Pressure of preparation $0.18$ mbar. Dimensions approx. 2500 x 1900 nm}
+ \label{sem_blackau}
+\end{figure}
-\begin{center}
+\begin{comment}
+\begin{figure}[H]
+ \centering
+ \begin{tabular}{ll}
+ \includegraphics[width=0.45\textwidth]{figures/sem/Au_semi-shiny_1_SEM.png} \\
+ \includegraphics[width=0.45\textwidth]{figures/sem/Au_BLACK_200nm.png}
-\begin{tabular}{cc}
- \includegraphics[scale=0.20]{figures/sem/Au_BLACK_200nm.png} & %\captionof{figure}{Au-Black SEM Image} \label{Au_BLACK_200nm.png} &
- \includegraphics[scale=0.20]{figures/sem/Au_semi-shiny_1_SEM.png} %\captionof{figure}{Au SEM Image} \label{Au_semi-shiny_1_SEM.png}
-
+ \end{tabular}
+ \caption{SEM Images of Au and Black Au films. Pressures of preparation were $10^{-6}$mbar and $0.18$mbar respectively. Dimensions are approx. 2500 x 1900 nm}
\label{SEM_images}
-\end{tabular}
-
- \captionof{figure}{{\bf 2500 x 1900nm SEM images of Au-Black (left) and Au-Bright (right) deposited on Si} \\ Preparation pressures were $2\times10^{-2}$mbar and $1\times10^{-6}$mbar respectively. \\ The films are sufficiently thick to be able to observe the colour with the naked eye.}
-
-\end{center}
-
-The structural differences between the two films are striking. The surface of the Au-bright film appears to consist of a layer of well defined metallic nanoparticles with sizes ranging from $20$ to $100$nm. In contrast, the Au-black film shows a highly irregular pattern, of interconnected strands of material. This pattern has lead some researchers to refer to metallic-black films as ``smokes'' \cite{}.
+\end{figure}
+\end{comment}
+Figures \ref{sem_au} and \ref{sem_blackau} shows a comparison of a Black Au and a Au film imaged using a scanning electron microscope (SEM). The structural difference between the two films is striking. The surface of the Au film appears to consist of a layer of well defined metallic nanoparticles with sizes ranging from $20$ to $100$nm. In contrast, the Black Au film shows a highly irregular, patchlike pattern. Previous studies have produced similar SEM images \cite{harris1952,panjwani2011,mckenzie2006}.
-\subsection*{Fourier Analysis of SEM Images}
+Intensity distributions of the SEM images (Figure \ref{SEM_levels}) show a smooth gaussian like peak for the Au film. In contrast, the intensity distribution of the Black Au film reveals an extremely high maxima at zero intensity, indicating that most of the surface has a very low secondary electron emission coefficient. The tail of this distribution is very flat, and extends to high intensity values, consistent with the observed patch like regions of high intensity values.
-Fourier Analysis of the above SEM images can be used to provide more quantitative information about the structural differences between the two films.
-The two dimensional Discrete Fourier Transform is given by:
-\begin{align}
- F(k_x, k_y) &= \displaystyle\sum_{x=0}^{N-1}\displaystyle\sum_{y=0}^{N-1} f(x, y) e^{\frac{-2 \pi i}{N}\left(k_x x + k_y y\right)} \label{dft}
-\end{align}
-Where $f(x, y)$ is a discrete data value (in this case the pixel intensity of the image) co-ordinates $(x, y)$, $N \times N$ are the dimensions of the image, and $F(k_x, k_y)$ gives the Fourier Coefficient. If the image represents a region with dimensions of $L \times L$, then the largest frequency components that can be contained in $F$ are $\frac{N}{L}$ \cite{}.
-
-Figures \ref{} and \ref{} show the amplitude plots of the DFT for each of the SEM images in figure \ref{SEM_images}. Since the phase plots give little additional information, they will not be presented or discussed here.
-
-There are two notable differences between the SEM images. Firstly, the central peak in low frequency components appears isotropic for the Au-Black sample, but is elliptically shaped for the Au-Bright image, indicating a. Secondly the
+\begin{figure}[H]
+ \centering
+ \begin{tabular}{ll}
+ \includegraphics[width=0.8\textwidth]{figures/sem/au_levels.eps} \\
+ \includegraphics[width=0.8\textwidth]{figures/sem/blackau_levels.eps}
+ \end{tabular}
+
+ \caption{Intensity distributions for the SEM images in Figures \ref{sem_au} and \ref{sem_blackau}. The total number of pixels for each intensity level (0-255) is shown. Similar analysis have been performed by Panjwani \cite{panjwani2011}.}
-Equation \eqref{dft} actually gives the Fourier coefficients of the infinite periodic extension of $f(x, y)$. If $f(x, y)$ is not periodic, then applying \eqref{dft} introduces extra high frequency components due to sharp discontinuities at the boundaries. (I think this is why FFTs show the perpendicular lines running through the centre... you can apply windows to reduce this effect, but since this is qualitative I haven't bothered).
-
-\pagebreak
-\begin{center}
- \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_abs.png}
- \captionof{figure}{Amplitude density plot of DFT for Au-Black SEM image}
- %\captionof[figure]{Amplitude density plot of DFT for Au-Black}
-\end{center}
-\begin{center}
- \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_abs.png}
- \captionof{figure}{Amplitude density plot of DFT for Au-Bright SEM image}
-\end{center}
-
-
-%\begin{center}
-% \includegraphics[scale=0.35]{fourier/Au_BLACK_82pix_200nm_fft_phase.png}
-% \captionof{figure}{Phase density plot of DFT for Au-Black}
-%\end{center}
-%\begin{center}
-% \includegraphics[scale=0.35]{fourier/Au_BRIGHT_42pix_100nm_fft_phase.png}
-% \captionof{figure}{Phase density plot of DFT for Au-Bright}
-%\end{center}
-%\pagebreak
-
-\subsection{Higher Magnification Images of Au-Black}
+ \label{SEM_levels}
+\end{figure}
+\begin{comment}
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth]{figures/sem/Au_BLACK_increasing_magnifications.jpg}
- \caption{Increasing magnification images of Au-Black}
+ \includegraphics[width=0.8\textwidth]{figures/sem/au_black_magnified.png}
+ \caption{Increasing magnification images of Black Au taken at CMCA}
\label{Au_BLACK_increasing_magnifications.jpg}
\end{figure}
-\section{Atomic Force Microscopy of Au}
-One of the Au-Bright samples sent to CMCA was imaged using Atomic Force Microscopy.
+Several higher magnification SEM images of the Black Au film were also prepared by CMCA. These reveal structure on a range of scales from several nanometers, to several hundred nanometers. The structures seen in Figure \ref{} are only several nanometers in size. Since classical descriptions of plasmonic behaviour tend to break down below 20nm length scales, a theoretical description of plasmonic behaviour in these structures may need to consider quantum effects \cite{}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth]{figures/afm/Au_BRIGHT_amplitude.png}
- \caption{AFM amplitude image of Au-Bright}
- \label{afm/Au_BRIGHT_AFM.tif}
-\end{figure}
+\begin{comment}
+
+As it is well known that plasmonic resonances can be created in highly periodic nanostructures, there has been some interest in using Fourier Techniques for description of more complicated structures in terms of periodic plasmonic components\cite{} \cite{sersic2011}. However, Discrete Fourier Transforms (DFT) of the SEM images in Figure \ref{SEM_images} revealed little information not already clear from the original image; cross sections of the DFT showed a similar spectra to $\frac{1}{f}$ (pink) noise. We have presented these results in an Appendix. Taking the DFT has limitations with regards to resolution and introduced noise; a more effective approach may be to use Fourier Microscopy techniques for producing the Fourier Transform directly within the SEM \cite{sersic2011}.
-\pagebreak
+\end{comment}
\section{Total Current Spectropy}
+\subsection{Tuning the Electron Gun}
+In \ref{tcs}, it was assumed that all primary electrons were incident normal to the surface, with an energy distribution $f(E - E_1)$ determined by the cathode. In reality, the primary beam has both angular and energy distributions. One can think of the cathode as producing initial angular and energy distributions, which are altered by the focusing properties of the electron gun to produce the distributions at the sample.
-\subsection{Effect of Focusing of the Electron Gun on the TCS}
+\begin{comment}
-{\bf Note: Maybe this should be put into the appendix ``Electron Optics''}
+The angular and energy distributions may be crudely combined into an effective energy distribution by considering each electron arriving at angle $\theta$ to the surface as having effective energy $E' = E \cos^2 \theta$, where the $\cos^2 \theta$ arises from considering only the component of momentum normal to the surface.
-The goal of electron optics applied to TCS is to minimise the effective energy distribution $f(E - E_1)$ of primary electrons at the surface. $f(E - E_1)$ is limited by the emission properties of the cathode, but significantly affected by the focus of the electron gun.
+\end{comment}
+%\footnote{An expression for the effective energy distribution is: $f'(E' - E_1') = \int \int f(E - E_1) n(\theta - \theta_1) \delta(E' - E \cos^2 \theta) d\theta dE$}
-The angular distribution of electrons incident on the sample can be related to $f(E - E_1)$ by treating each electron arriving at angle $\theta$ to the surface as having an effective energy $E_{eff} = E \cos^2 (\theta)$. The width of this angular distribution determines the width of $f(E - E_1)$, whilst the centre determines the value of $U$ for which the measured TCS elastic peak occurs.
+\begin{comment}
+An expression for the effective energy distribution in terms of $f(E - E_1)$ and the angular distribution $n(\theta - \theta_1)$ is:
+
+\begin{align*}
+ f'(E' - E_1') &= \int_{-\infty}^{\infty} \int_{-\frac{\pi}{2}}{\frac{\pi}{2}} f(E - E_1) n(\theta - \theta_1) \delta(E' - E \cos^2 \theta) d\theta dE
+\end{align*}
+\end{comment}
-It is also important to ensure that the primary electron beam only strikes the sample of interest (and not the sample holder).
-\emph{TODO: Choose which plots to include; Can get a range of similar effects from adjustment of each electrode potential; I have reproduced all the plots here for now}.
+As discussed in \ref{tcs}, the effective energy distribution of primary electrons appears at the contact potential as the first peak in $S(U)$. Any peaks due to inelastic processes are convolved with the effective energy distribution. If the angular distribution is not centred about $\theta_1 = 0$ (due to misalignment of the sample holder) the observed contact potential is increased. Therefore it is desirable to adjust the electron gun so as to produce the narrowest possible distribution, at the lowest possible contact potential. In Figure \ref{focus_central_tcs.eps} we show the adjustment of the central electrodes to minimise the width of the elastic scattering peak.
-Figure \ref{focus_accel_tcs.eps} - Adjusting the accelerating potential
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_accel_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_accel_tcs.eps}
+ \includegraphics[width=0.5\textwidth, angle=270]{figures/tcs/plots/focus_central_tcs.eps}
+ \caption{Adjusting the central electrodes to optimise the effective energy distribution}
+ \label{focus_central_tcs.eps}
\end{figure}
+\subsection{Electron gun simulation}
+
+Figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} show the results of an electron gun simulation written for this project. The results of this simulation were not used to focus the actual electron gun; however Figure \ref{egun_simulation1.pdf} was useful, as it shows the possibility for electrons to strike the insulating posts holding the gun together. An insulating material in the path of the electron beam would become charged over time, and affect the focusing properties of the gun. When these posts were covered with tantalum strips connected to the final electrode, the stability of the measured current at fixed $U$ was improved.
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_central_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_central_tcs.eps}
+ \includegraphics[scale=0.4, angle=270]{figures/egun/egun_simulation1.pdf}
+ \caption{Simulated electron trajectories}
+ \label{egun_simulation1.pdf}
\end{figure}
+
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_deflection_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_deflection_tcs.eps}
+ \includegraphics[scale=0.4, angle=270]{figures/egun/egun_simulation2.pdf}
+ \captionof{figure}{2D Simulation of the electrostatic potential produced by the electron gun}\label{egun_simulation2.pdf}
\end{figure}
+
+\subsection{Deposition of Ag films onto a Si substrate}
+
+We have measured the total current spectra for Ag films deposited onto an Si substrate. An optically thick layer of Ag, followed by a thin layer of Black Ag \footnote{pressures approx $10^{-7}$ and $0.18\text{mbar}$ respectively} were deposited, with measurements performed before and after each deposition.
+
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_wenhault_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_wenhault_tcs.eps}
+ \includegraphics[width=0.80\textwidth, angle=0]{figures/tcs/plots/ag_si.eps}
+ \caption{Comparison of Si and Ag on Si TCS}
+ \label{agsiI_tcs}
\end{figure}
+In Figure \ref{agsiI_tcs}, the total current spectrum of the sample changes dramatically with the Ag deposition. The contact potential of the surface decreases by about $1.7$V. Typical literature values for Si and Ag work functions would predict a shift of at most $4.9 - 4.2 = 0.7$V. In interpreting this shift it is important to note that our surfaces are not atomically clean.
+Ellipsometric measurements had found that the Si substrates used in this study had $\text{SiO}_2$ surface layers with thicknesses of several nanometers. Comparing literature values for Ag and $\text{SiO}_2$ work functions shows that the expected difference in contact potentials for an Ag and $\text{SiO}_2$ is between $0.8$V and $1.8$V\footnote{The exact values of the work functions depend upon the orientation of the crystal lattice at the surface layer and shape of the Fermi-surface of the material}.
+In addition to the change in contact potential of the surface, an inflection point is visible in the Ag spectrum at the location of the contact potential for $\text{SiO}_2$. Even though the Ag sample was optically thick, it seems that the surface potential of the underlying $\text{SiO}_2$ layer may still be contributing to $S(U)$.
-\subsection{Effect of Evaporation of Ag onto an Si substrate}
-\emph{Note to Sergey: I know you said not to do any more experiments, but I did these on Tuesday night because I wanted to compare curves taken under as similar conditions as possible (most previous results were obtained over several days at the least). I used Ag because I was running low on Au.}
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.80\textwidth]{figures/tcs/plots/blackag_ag.eps}
+ \caption{Comparison of Ag/Si and Black Ag on Ag/Si spectra}
+ \label{blackagsiI_tcs}
+\end{figure}
-Figures \ref{agsiI_tcs.eps} and \ref{agsiII_tcs.eps} show the processed TCS curves for layers of Ag, followed by Ag-Black, evaporated on Si substrates. For comparison, the sample holder (stainless steel) TCS is also shown.
+Figure \ref{blackagsiI_tcs} shows the change in TCS after a layer of Black Ag is deposited on the existing Ag layer. The contact potential of the surface changes only slightly. This is unsurprising, as the new surface layer consists mostly of the same material. However, the surface peak has narrowed, despite no change in the focusing of the electron gun. This change in surface peak may be attributed to a change in the surface potential of the sample after the Black Ag layer was deposited. In particular the surface peak has narrowed, which is indicative of either a sharper potential barrier at the surface, or a more uniform potential accross the irradiated surface area.
+Our experimental setup has been limited to applied potentials of $0$ to $16$V. The contact potentials of the surfaces have limited the range of primary electron energies to just over $10$ eV. Referring to Figure \ref{komolov1979} (which is idealised), it is recommended that this range be extended if the experiment were to be used for study of inelastic scattering processes.
-The electron gun was focused on the sample shown in \ref{agsiI_tcs.eps}. The sample shown in \ref{agsiII_tcs.eps} was placed in a second sample holder on the opposite side of a rotation manipulator; the gun was not refocused on this sample.
+\begin{comment}
+Each stage in this experiment was repeated for another Si sample in the second sample holder. Although the exact shape of the total current spectra differed\footnote{The contact potentials were roughly 5V higher. This is most likely because the optimum focusing potentials for the first sample holder were suboptimal for the second, due to differences in height and distance from the electron gun}, we observed similar changes in the contact potential difference with the deposition of Ag and Black-Ag films.
+\end{comment}
+%\begin{figure}[H]
+% \centering
+% \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagII_agsiII_siII_holderII_tcs.eps}
+% \caption{The above TCS comparison repeated for a second sample \\(NB: Ag evaporation time is half that of the first sample; layer is still visible by eye)}
+% \label{agsiII_tcs.eps}
+%\end{figure}
-\emph{TODO: Explain curves!}
-\begin{enumerate}
- \item Contact potential decreases in going from Si to Ag on Si
- \item BlackAg appears to have a higher elastic peak
- \item The gun electrodes are the same, but the two sets of curves are clearly different; due to dodgy sample holder; best not mention
- (Only present one of these graphs?)
- \item Can see that beam is not hitting the sample holder (best seen in the second plot), because the elastic peak of the sample holder is clearly not visible in the TCS of the Si substrate.
- \item Positive TCS - Indicates more inelastic interaction mechanisms are possible (threshold energy reached)
- \item Negative TCS - Indicates fewer inelastic interaction mechanisms. ???
- \item Why does TCS change very smoothly? Is the convolution of primary and secondary maxima sufficient to explain this?
- \begin{itemize}
- \item I can fit for the location and size of gaussian peaks if required.
- \end{itemize}
- \item TCS of BlackAg appears very similar, but shifted, for the two trials
-\end{enumerate}
+%\begin{comment}
-\emph{Note: I also have plots of I(E) curves}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagI_agsiI_siI_holderI_tcs.eps}
- \caption{Successive TCS curves for a BlackAg evaporated on Ag on a Si substrate.}
- \label{agsiI_tcs.eps}
-\end{figure}
+\section{Optical Transmission Spectroscopy}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagII_agsiII_siII_holderII_tcs.eps}
- \caption{The above TCS comparison repeated for a second sample \\(NB: Ag evaporation time is half that of the first sample; layer is still visible by eye)}
- \label{agsiII_tcs.eps}
-\end{figure}
-
-\subsection{Effect of Evaporation of Au on Si}
-
-Figure \ref{increased_au_thickness_tcs.eps} shows the comparison between TCS obtained from a thin layer of Au on Si and a thicker layer of Au.
+In the transmission spectroscopy experiments, white light has been shone through a thin metallic film mounted on a glass slide. A commercial visible range optical spectrometer\footnote{OceanOptics QE65000} was used to measure the spectrum of the transmitted light in comparison. The transmission of a sample can be determined after first measuring the spectrum of the white light source. For thin films on a glass substrate, the transmission spectrum may be estimated after first determining the transmission spectrum of the glass.
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/increased_au_thickness_tcs.eps}
- \label{increased_au_thickness_tcs.eps}
+ \includegraphics[width=0.6\textwidth]{figures/transmission_spectroscopy/transmission_spectroscopy.pdf}
+ \caption{Setup for a transmission spectroscopy experiment}
\end{figure}
-Figure \ref{blackau_on_au_on_si_tcs.eps} shows the effect of evaporating Black-Au on a thick layer of Au on Si.
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackau_on_au_on_si_tcs.eps}
- \label{blackau_on_au_on_si_tcs.eps}
-\end{figure}
-Disagrees with the BlackAg on Ag on Si... I am really confused.
+A 653nm filter was used to test the response of the spectrometer. The measured wavelength for peak transmission was $650.8$nm. The stated uncertainty in the filter's peak transmission wavelength was $\pm 2\%$ (approx. 13nm).
-\pagebreak
-\section{Variable Angle Spectroscopy Ellipsometry}
-\subsection{Ag-Bright on Si substrate}
+\subsection{Reference Spectrum}
+The Ellipsometer's Xe Arc Lamp was used as a light source. Its spectrum $I_0(\lambda)$ is shown in Figure \ref{reference.eps}. This measurement established that the Xe Arc lamp was indistinguishable from background light levels below $\lambda \approx 320$nm. %The Xe arc lamp has several strong emission lines in the near infra-red (above 800nm). %The subsequent results have all been normalised to this reference spectrum.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/psi_final_model.png}
- \label{psi_final_model.png}
+ \includegraphics[width=0.7\textwidth]{figures/transmission_spectroscopy/reference.eps}
+ \caption{Xe Lamp reference spectrum}
+ \label{reference.eps}
\end{figure}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/delta_final_model.png}
- \label{delta_final_model.png}
-\end{figure}
+\begin{comment}
+\subsection{Testing the Spectrometer}
+
+A 653nm filter was used to test the response of the spectrometer. Figure \ref{653nm_filter.eps} shows a spectrum for the Xe lamp shone through this filter; according to the spectrometer, the location of the peak is at 650.8nm. The stated uncertainty in the filter's peak transmission wavelength is $\pm 2$.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/ag_fit_vs_bulk_opticalconstants.png}
- \label{ag_fit_vs_bulk_opticalconstants.png}
+ \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/653nm_filter.eps}
+ \caption{Tested Spectrometer with 653nm Filter}
+ \label{653nm_filter.eps}
\end{figure}
+\end{comment}
-The plots show the measured and fitted ellipsometric parameters for a thin film of Ag on a Si substrate. The model was constructed to include an $\text{SiO}^2$ oxide layer on the Si, and a surface roughness Effective Medium Approximation (EMA) (Bruggeman). A fit was first performed for the thickness of the Ag film assuming bulk optical constants; this fit was then improved by allowing the software to adjust the Ag film's optical constants. Final model:
-\begin{center}
- \begin{tabular}{lll}
- {\bf Layer} & {\bf Thickness} \\
- Ag (fit for $n$ and $k$) & $16.092 \pm 2.7$ nm \\
- Intermix (Ag/$\text{SiO}^2$) & $0.267 \pm 0.03$ nm \\
- $\text{SiO}^2$ & $4.02 \pm 0.57$ nm \\
- Si & (substrate)
- \end{tabular}
- \captionof{table}{Model for thin Ag on Si}
-\end{center}
+\begin{comment}
+\subsection{Transmission Spectra of Glass}
-\subsection{Black Ag on Si}
+Past studies of the transmissive properties of Black Metal films have generally used nitrocellulose backings for the film \cite{pfund1933} \cite{harris1948}. For our purpose more qualitative measurements were sufficient, and so microscope slide glass available at CAMSP have been used instead. Figure \ref{glass.eps} shows the calculated transmission spectrum for a piece of microscope slide glass. The formula used in calculating the spectrum is:
+
+\begin{align}
+ t(\lambda) &= \frac{I_{\text{measured}}(\lambda)}{I_0(\lambda)} \label{transmission_formula}
+\end{align}
+Where $I_\text{measured}$ is the measured intensity and $I_0$ is the intensity of the reference spectrum.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/psi.png}
- \label{psi_final_model.png}
+ \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/glass.eps}
+ \caption{Glass reference transmission spectrum}
+ \label{glass.eps}
\end{figure}
+\end{comment}
+
+\subsection{Transmission Spectra of Au and Black Au on Glass}
+
+Transmission spectra for similar thickness Au and Black Au films were measured, accounting for the transmission of the glass and the reference spectrum.
+\begin{comment}
+Equation \ref{shitty_assumption} does not take into account possible backside reflections at the interfaces between the air and glass, and the glass and the film. Such reflections would lead to interference effects, dependent upon the optical properties of both the films and glass, as well as the film thickness. Because the transmission of the glass was measured to be relatively high, \eqref{shitty_assumption} may be used to obtain a reasonable first approximation of the metal films' transmission spectra. Ellipsometric measurement would better characterise the sample.
+\end{comment}
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/delta.png}
- \label{delta_final_model.png}
+ \includegraphics[width=0.8\textwidth]{figures/transmission_spectroscopy/blackau.eps}
+ \caption{Transmission Spectra of Au and Black Au films}
\end{figure}
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/blackag_opticalconstants_comparison.png}
- \label{ag_fit_vs_bulk_opticalconstants.png}
+ \begin{tabular}{ll}
+ \includegraphics[width=0.5\textwidth]{figures/transmission_spectroscopy/au_zoom.eps} &
+ \includegraphics[width=0.5\textwidth]{figures/transmission_spectroscopy/blackau_zoom.eps}
+ \end{tabular}
+ \caption{Transmission Spectra for $\lambda \leq 620$nm}
+ \label{zoom_transmission}
\end{figure}
-\begin{center}
- \begin{tabular}{lll}
- {\bf Layer} & {\bf Thickness} \\
- Surface roughness EMA (75.8\% void) & 2.708 nm \\
- Black Ag (fit for $n$ and $k$) & 3.726 nm \\
- $\text{SiO}^2$ & 8.00 nm \\
- Si & (substrate)
- \end{tabular}
- \captionof{table}{Model for thin Ag on Si}
-\end{center}
+The results show that Black Au is far less transmissive than Au in the visible part of the spectrum. Both spectra reveal a similar double peak shape. As found by Pfund and other researchers, the transmission of the Black Au film increases into the infra-red part of the spectrum\cite{pfund1933,harris1942,harris1953}. There are particularly interesting differences near $350$nm. The Black Au film shows a dip in transmission which is notably absent in the Au film.
-\pagebreak
-\section{Optical Reflection Spectroscopy using the VASE}
-\subsection{Au on Si}
+\begin{comment}
+It is difficult to arrive at a possible explanation for this dip based upon the transmission data alone. Plasmonic behaviour is often sensitive to the polarisation of incident light. Ellipsometry, which measures polarisation, was found to be more useful for characterising samples\footnote{The Ellipsometer was unavailable at the time of the Optical Transmission Spectroscopy measurements}.
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/au_on_si.png}
- \caption{figure}{Reflection measurements for Au layers on Si}
-\end{figure}
+\subsection{Effect of Atmosphere on Transmission Spectra of Black Au}
+Harris et al \cite{harris1952} and other studies \cite{mckenzie2006} have examined the differences between Black Au deposited in an atmosphere with or without oxygen present. The Black Au prepared in air may contain traces of tungsten oxides formed at the tungsten filament, whilst Black Au prepared in inert gases was shown to consist entirely of Au. This was the motivation for making a comparison between samples prepared in air and He atmospheres.
-\subsection{Au on Au-Black on Au on Si}
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/au_on_blackau_si.png}
- \caption{figure}{Reflection measurements for an Au layer on Au-Black on Au layers on Si}
+ \includegraphics[width=0.6\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/he_blackau_vs_air_blackau.eps}
+ \caption{Transmission Spectra for Black Au films prepared in different atmospheres}
+ \label{he_blackau_vs_air_blackau.eps}
\end{figure}
-\subsection{Comparison with model of 50nm Au on Si}
-
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/generated_au_on_si_reflection.png}
- \caption{Generated 50nm on Si}
-\end{figure}
+\end{comment}
\pagebreak
-\section{Optical Transmission Spectroscopy using OceanOptics Spectrometer}
+\section{Variable Angle Spectroscopy Ellipsometry}
-\subsection{Dark Spectrum}
-{\bf NOTE: Probably won't include in the final thesis}
-Figure \ref{dark_comparison.eps} shows the spectrum of the background (taken at different times on the same day), without the light source.
-The room lights were off, the experiment was covered with a cardboard box and layers of black plastic sheeting; but the spectra still changed for different times of the day.
+\subsection{Model for Ag and Black Ag on a Si substrate}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/dark_comparison.eps}
- \caption{Dark spectra}
- \label{dark_comparison.eps}
-\end{figure}
+Testing showed that it is difficult to use Ellipsometry to characterise black metal films of considerable thickness (estimated $>30nm$), due to the extremely low reflectivity of such films. However, using the WVASE32 software, it was possible to fit for the optical constants of an extremely thin layer of Black Ag prepared on Si using ellipsometric measurements. Figures \ref{n_compare.pdf} and \ref{k_compare.pdf} show the fitted optical constants for the Ag layer in a multilayered model for both a Black Ag thin film, and Ag thin film. Bulk Ag optical constants from Palik's Handbook \cite{palik} were specified for the initial values.
-In all subsequent experiments, the dark intensity has been subtracted from measured intensity counts:
+The models include an $\text{SiO}_2$ surface layer, with the thickness fit. The EMA layer models the effect of surface roughness in the film. This layer uses the Bruggeman model to describe the surface as a set of spherical inclusions of the Black Ag material in a void. The Bruggeman EMA formula is \cite{bruggeman1935, oates2011}:
\begin{align*}
- I(\lambda) = I_{\text{measured}}(\lambda) - I_{\text{dark}}(\lambda)
+ F \frac{\epsilon_b - \epsilon_{eff}}{\epsilon_b + 2 \epsilon_{eff}} + (1 - F) \frac{\epsilon_c - \epsilon_{eff}}{\epsilon_c + 2\epsilon_{eff}} &= 0
\end{align*}
+where $\epsilon_b$ and $\epsilon_c$ are the dielectric functions of the two materials (in our case, material $b$ is air; $\epsilon_b = 1$), and $F$ is the volume fraction of material $b$. This model is incorporated into the WVASE32 software.
-\pagebreak
-\subsection{Reference Spectrum}
-
-{\bf Note: Also don't include in final thesis? Or at least, remove the time dependence; just show one curve.}
-
-The Ellipsometer's Xe Arc Lamp was used as a light source. It's spectrum $I_0(\lambda)$ is shown in Figure \ref{reference.eps}
-
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/reference.eps}
- \caption{Xe Lamp reference spectra}
- \label{reference.eps}
-\end{figure}
-Because the dark spectra changed over time scales comparable to the length of measurement, some features in the processed spectra are due to the reference spectra of the Xe lamp.
+Although from SEM images it is clear that the structure of Black films is far more complicated than this approximation, fitting for the fraction of Black Ag in the surface layer shows a majority of the surface is empty. This is consistent with the porous nature of Black metal films seen in SEM images. The thickness of this layer was also a free parameter in the model.
-\pagebreak
-\subsection{Testing the Spectrometer}
+Both the refractive index and extinction coefficient of the Black Ag film show a strong peak around $370$ nm. From the refractive index, the Black Ag film has a much stronger dispersion relation than the Ag film. The extinction coefficient peak indicates a preferential scattering or absorbsion of light at $370$ nm. This may be indicative of surface plasmon resonance effects \cite{oates2011, sonnichsen2001, zheng2008}, particularly since it occurs near to the bulk plasmon frequency for Ag. It is interesting to note that the peak in extinction for the thin Ag film occurs within $30$ nm of the dip in transmission measured for an Au film (Figure \ref{zoom_transmission}).
-{\bf Note: Also don't include?}
-The spectrometer was tested using a 653nm filter. \ref{653nm_filter.eps}
\begin{figure}[H]
\centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/653nm_filter.eps}
- \caption{Tested Spectrometer with 653nm Filter}
- \label{653nm_filter.eps}
+ \includegraphics[width=0.80\textwidth]{figures/ellipsometer/ag_vs_blackag/n_compare.pdf}
+ \caption{Fitted refractive index for the Ag layer in multilayered models for Ag and Black Ag (step size 50 nm)}
+ \label{n_compare.pdf}
\end{figure}
-The transmission was calculated as:
-\begin{align}
- t(\lambda) &= \frac{I(\lambda)}{I_0{\lambda}} \label{transmission1}
-\end{align}
-Where $I_0(\lambda)$ was the intensity (arbitrary units) of the Xe Arc Lamp at wavelength $\lambda$, and $I(\lambda)$ was the measured intensity.
-
-\subsection{Transmission Spectra of Glass}
-
-{\bf Note: Should probably include this, as the substrate is important to the final transmission}
-
-All films were prepared on microscope glass; the transmission of the glass must be known to determine the transmission of the films.
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/glass_transmission.eps}
- \caption{Glass reference transmission spectrum}
- \label{glass_transmission.eps}
+ \includegraphics[width=0.80\textwidth]{figures/ellipsometer/ag_vs_blackag/k_compare.pdf}
+ \caption{Fitted extinction coefficient for the Ag layer in multilayered models for Ag and Black Ag (step size 50 nm)}
+ \label{k_compare.pdf}
\end{figure}
-{\bf NOTE:} The reason that the glass has transmission $> 1$ is (probably) because the background level has increased between the reference measurement and the measurement of glass. I should probably normalise the glass transmission spectrum to its maximum value.
-
-Transmission was calculated using \eqref{transmission1}.
-
-\subsection{Transmission Spectra of Au and Au-Black on Glass}
-Figure \ref{blackau_vs_au.eps} shows all measured transmission spectra for Au vs Au-Black (pressure 1e-6 is for the Au-bright films, all others are Au-Black) {\bf NOTE: Need to relabel plot}
+\subsection{Surface and Bulk Plasmons in the Ag and Black Ag films}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/blackau_vs_au.eps}
- \caption{Transmission Spectra for various Au films}
- \label{blackau_vs_au.eps}
-\end{figure}
-
-Transmission is calculated as:
+The bulk loss function as introduced in Section \ref{tcs_e} is:
\begin{align*}
- t &= \frac{I(\lambda)}{I_0(\lambda)} \times \frac{I_\text{glass}(\lambda)}{I_0(\lambda)}
+ L_b = -\text{Im}\frac{1}{\phasor{\epsilon}}
\end{align*}
-Where $t_{\text{glass}} = \frac{I_\text{glass}}{I_0}$ is the transmission spectrum of the microscope slide glass.
-{\bf Note: I should select just 2 or 3 of these spectra to use in the final report}
+The occurance of maxima in $L_b$ can be used as a condition for determining bulk plasmon excitation frequencies \cite{komolov}.
-The general trends:
-\begin{enumerate}
- \item Thin films (low current or short evaporation time) show similar shape regardless of pressure (1e-6 or 1e-2 mbar)
- \item Thicker layers all show peak near 500nm, followed by minima at 600-700nm
- \item All curves show fine structure at same wavelengths above 800nm. This may be due to the Xe lamp spectrum; if the background level has increased, then Xe lamp spectral features will show up in the final spectrum.
- \item Thick layers of Au-Black show much lower transmission to 700nm, but a much faster increase at longer $\lambda$
- \item At least one of the Au-Black samples shows a similar spectrum to a (thick) Au-Bright sample.
-\end{enumerate}
+For surface plasmon excitations, the surface loss function is \cite{ibach2010}:
+\begin{align*}
+ L_s &= -\omega \text{Im}\left(\frac{1}{1 + \phasor{\epsilon}}\right)
+\end{align*}
-\subsubsection{Effect of Atmosphere on Transmission Spectra of Au-Black}
+When applied to the thin Ag film (Figure \ref{ag_loss}) the bulk loss function shows a strong peak at $320$nm, and is otherwise rather flat. This peak corresponds to the bulk plasmon frequency for Ag ($\hbar \omega_p \approx 3.8\text{eV}$. It should be noted that the stated uncertainty of Ellipsometric measurements is above 20\% for wavelengths below $320$nm. In addition we initially specified the film to have bulk optical constants, for which this result is to be expected.
-A paper \cite{} has found differences between Au-Black prepared in Air or an inert gas. The Au-Black prepared in Air contains traces of Tungsten Oxides; the Au-Black prepared in an inert gas does not. This was the motivation for making a comparison between samples prepared in Air and He.
+When the bulk and surface loss functions are applied to the Black Ag film (Figure \ref{blackag_loss}), there is in fact a shallow minima at $370$nm. In contrast to the Ag film, the loss functions appear to increase monatomically for longer wavelengths.
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/he_blackau_vs_air_blackau.eps}
- \caption{Transmission Spectra for Black Au films prepared in different atmospheres}
- \label{he_blackau_vs_air_blackau.eps}
-\end{figure}
-\subsection{Transmission Spectra of Ag}
+Based upon these results, we cannot conclude that this particular Black Ag film will support surface or bulk plasmon oscillations. However, we cannot rule out that localised plasmonic resonance effects contribute to a scattering of light causing the peak in $k$ around $3800$. Due to the complicated structure of the surface it would be difficult to theoretically describe the nature of such effects. A starting point for future theoretical work may be Harris' models of black metal films as a series of interwoven conducting strands \cite{harris1952}.
-A pre-existing Ag sample (unknown preparation conditions), on glass.
\begin{figure}[H]
\centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/silver_transmission.eps}
- \caption{Transmission Spectra for a Silver film on glass}
- \label{silver_transmission.eps}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ag_loss.eps}
+ \caption{Pseudo-loss functions for the Ag thin film}
+ \label{ag_loss}
\end{figure}
-\subsection{Transmission Spectra of Ag and Ag-Black on Glass}
-
-The Ag sample compared with Ag-Black.
-Notice fine structure not in original Ag sample. Probably due to dark spectrum changing.
-
-A pre-existing Ag sample (unknown preparation conditions), on glass.
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/blackag_vs_ag.eps}
- \caption{Transmission Spectra for a Silver film on glass}
- \label{blackag_vs_ag.eps}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/blackag_loss.eps}
+ \caption{Pseudo-loss functions for the Black Ag thin film}
+ \label{blackag_loss}
\end{figure}
-{\bf Note:} The Ag-Black is much thinner than the Ag-Bright sample; by eye it appears to be a thin grey layer. Also, the Ag-Bright sample was not uniformly thick; part of the film had been scratched or wiped off.
+\pagebreak
+
-\chapter{Results and Discussion}
+\chapter{Experimental Results and Discussion} \label{chapter_results}
+
\section{Scanning Electron Microscopy}
-A number of samples of metallic-black and metallic-bright films were sent to the Centre for Microscopy Characterisation and Analysis (CMCA) at UWA for study. In this section we will present and discuss some of the images produced by CMCA. These images provide an invaluable aid to understanding the structural differences between metallic-black and metallic-bright films.
+A number of samples of black and non-black metal films were prepared and sent to the Centre for Microscopy Characterisation and Analysis (CMCA) at UWA for study. In this section we will present and discuss two of the images produced by CMCA. These images proved to be an invaluable aid in understanding the structural differences between metallic-black and metallic-bright films.
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.7\textwidth]{figures/sem/Au_semi-shiny_1_SEM.png}
+ \caption{SEM Image of a Au film. Pressure of preparation $10^{-6}$ mbar. Dimensions approx. 2500 x 1900 nm}
+ \label{sem_au}
+\end{figure}
-Figure \ref{SEM_images} shows a comparison of an Au-Black and Au-Bright film imaged using a scanning electron microscope (SEM). The intensity of each pixel is proportional to the total current of secondary electrons scattered from the surface at that point from the metal in the film (the current due to the Si substrate has been subtracted from the image), which is in turn proportional to the density of metal at the considered point.
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.7\textwidth]{figures/sem/Au_BLACK_200nm.png}
+ \caption{SEM Image of a Black Au film. Pressure of preparation $0.18$ mbar. Dimensions approx. 2500 x 1900 nm}
+ \label{sem_blackau}
+\end{figure}
-\begin{center}
+\begin{comment}
+\begin{figure}[H]
+ \centering
+ \begin{tabular}{ll}
+ \includegraphics[width=0.45\textwidth]{figures/sem/Au_semi-shiny_1_SEM.png} \\
+ \includegraphics[width=0.45\textwidth]{figures/sem/Au_BLACK_200nm.png}
-\begin{tabular}{cc}
- \includegraphics[scale=0.20]{figures/sem/Au_BLACK_200nm.png} & %\captionof{figure}{Au-Black SEM Image} \label{Au_BLACK_200nm.png} &
- \includegraphics[scale=0.20]{figures/sem/Au_semi-shiny_1_SEM.png} %\captionof{figure}{Au SEM Image} \label{Au_semi-shiny_1_SEM.png}
-
+ \end{tabular}
+ \caption{SEM Images of Au and Black Au films. Pressures of preparation were $10^{-6}$mbar and $0.18$mbar respectively. Dimensions are approx. 2500 x 1900 nm}
\label{SEM_images}
-\end{tabular}
-
- \captionof{figure}{{\bf 2500 x 1900nm SEM images of Au-Black (left) and Au-Bright (right) deposited on Si} \\ Preparation pressures were $2\times10^{-2}$mbar and $1\times10^{-6}$mbar respectively. \\ The films are sufficiently thick to be able to observe the colour with the naked eye.}
-
-\end{center}
-
-The structural differences between the two films are striking. The surface of the Au-bright film appears to consist of a layer of well defined metallic nanoparticles with sizes ranging from $20$ to $100$nm. In contrast, the Au-black film shows a highly irregular pattern, of interconnected strands of material. This pattern has lead some researchers to refer to metallic-black films as ``smokes'' \cite{}.
-
-
-\subsection*{Fourier Analysis of SEM Images}
+\end{figure}
+\end{comment}
-Fourier Analysis of the above SEM images can be used to provide more quantitative information about the structural differences between the two films.
+Figures \ref{sem_au} and \ref{sem_blackau} shows a comparison of a Black Au and a Au film imaged using a scanning electron microscope (SEM). The structural difference between the two films is striking. The surface of the Au film appears to consist of a layer of well defined metallic nanoparticles with sizes ranging from $20$ to $100$nm. In contrast, the Black Au film shows a highly irregular, patchlike pattern. Previous studies have produced similar SEM images \cite{harris1952,panjwani2011,mckenzie2006}.
-The two dimensional Discrete Fourier Transform is given by:
-\begin{align}
- F(k_x, k_y) &= \displaystyle\sum_{x=0}^{N-1}\displaystyle\sum_{y=0}^{N-1} f(x, y) e^{\frac{-2 \pi i}{N}\left(k_x x + k_y y\right)} \label{dft}
-\end{align}
+Intensity distributions of the SEM images (Figure \ref{SEM_levels}) show a smooth gaussian like peak for the Au film. In contrast, the intensity distribution of the Black Au film reveals an extremely high maxima at zero intensity, indicating that most of the surface has a very low secondary electron emission coefficient. The tail of this distribution is very flat, and extends to high intensity values, consistent with the observed patch like regions of high intensity values.
-Where $f(x, y)$ is a discrete data value (in this case the pixel intensity of the image) co-ordinates $(x, y)$, $N \times N$ are the dimensions of the image, and $F(k_x, k_y)$ gives the Fourier Coefficient. If the image represents a region with dimensions of $L \times L$, then the largest frequency components that can be contained in $F$ are $\frac{N}{L}$ \cite{}.
-Figures \ref{} and \ref{} show the amplitude plots of the DFT for each of the SEM images in figure \ref{SEM_images}. Since the phase plots give little additional information, they will not be presented or discussed here.
-There are two notable differences between the SEM images. Firstly, the central peak in low frequency components appears isotropic for the Au-Black sample, but is elliptically shaped for the Au-Bright image, indicating a. Secondly the
+\begin{figure}[H]
+ \centering
+ \begin{tabular}{ll}
+ \includegraphics[width=0.8\textwidth]{figures/sem/au_levels.eps} \\
+ \includegraphics[width=0.8\textwidth]{figures/sem/blackau_levels.eps}
+ \end{tabular}
+
+ \caption{Intensity distributions for the SEM images in Figures \ref{sem_au} and \ref{sem_blackau}. The total number of pixels for each intensity level (0-255) is shown. Similar analysis have been performed by Panjwani \cite{panjwani2011}.}
-Equation \eqref{dft} actually gives the Fourier coefficients of the infinite periodic extension of $f(x, y)$. If $f(x, y)$ is not periodic, then applying \eqref{dft} introduces extra high frequency components due to sharp discontinuities at the boundaries. (I think this is why FFTs show the perpendicular lines running through the centre... you can apply windows to reduce this effect, but since this is qualitative I haven't bothered).
-
-\pagebreak
-\begin{center}
- \includegraphics[scale=0.35]{figures/sem/Au_BLACK_82pix_200nm_fft_abs.png}
- \captionof{figure}{Amplitude density plot of DFT for Au-Black SEM image}
- %\captionof[figure]{Amplitude density plot of DFT for Au-Black}
-\end{center}
-\begin{center}
- \includegraphics[scale=0.35]{figures/sem/Au_BRIGHT_42pix_100nm_fft_abs.png}
- \captionof{figure}{Amplitude density plot of DFT for Au-Bright SEM image}
-\end{center}
-
-
-%\begin{center}
-% \includegraphics[scale=0.35]{fourier/Au_BLACK_82pix_200nm_fft_phase.png}
-% \captionof{figure}{Phase density plot of DFT for Au-Black}
-%\end{center}
-%\begin{center}
-% \includegraphics[scale=0.35]{fourier/Au_BRIGHT_42pix_100nm_fft_phase.png}
-% \captionof{figure}{Phase density plot of DFT for Au-Bright}
-%\end{center}
-%\pagebreak
-
-\subsection{Higher Magnification Images of Au-Black}
+ \label{SEM_levels}
+\end{figure}
+\begin{comment}
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth]{figures/sem/Au_BLACK_increasing_magnifications.jpg}
- \caption{Increasing magnification images of Au-Black}
+ \includegraphics[width=0.8\textwidth]{figures/sem/au_black_magnified.png}
+ \caption{Increasing magnification images of Black Au taken at CMCA}
\label{Au_BLACK_increasing_magnifications.jpg}
\end{figure}
-\section{Atomic Force Microscopy of Au}
-One of the Au-Bright samples sent to CMCA was imaged using Atomic Force Microscopy.
+Several higher magnification SEM images of the Black Au film were also prepared by CMCA. These reveal structure on a range of scales from several nanometers, to several hundred nanometers. The structures seen in Figure \ref{} are only several nanometers in size. Since classical descriptions of plasmonic behaviour tend to break down below 20nm length scales, a theoretical description of plasmonic behaviour in these structures may need to consider quantum effects \cite{}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth]{figures/afm/Au_BRIGHT_amplitude.png}
- \caption{AFM amplitude image of Au-Bright}
- \label{afm/Au_BRIGHT_AFM.tif}
-\end{figure}
+\begin{comment}
+
+As it is well known that plasmonic resonances can be created in highly periodic nanostructures, there has been some interest in using Fourier Techniques for description of more complicated structures in terms of periodic plasmonic components\cite{} \cite{sersic2011}. However, Discrete Fourier Transforms (DFT) of the SEM images in Figure \ref{SEM_images} revealed little information not already clear from the original image; cross sections of the DFT showed a similar spectra to $\frac{1}{f}$ (pink) noise. We have presented these results in an Appendix. Taking the DFT has limitations with regards to resolution and introduced noise; a more effective approach may be to use Fourier Microscopy techniques for producing the Fourier Transform directly within the SEM \cite{sersic2011}.
-\pagebreak
+\end{comment}
\section{Total Current Spectropy}
+\subsection{Tuning the Electron Gun}
+In \ref{tcs}, it was assumed that all primary electrons were incident normal to the surface, with an energy distribution $f(E - E_1)$ determined by the cathode. In reality, the primary beam has both angular and energy distributions. One can think of the cathode as producing initial angular and energy distributions, which are altered by the focusing properties of the electron gun to produce the distributions at the sample.
-\subsection{Effect of Focusing of the Electron Gun on the TCS}
+\begin{comment}
-{\bf Note: Maybe this should be put into the appendix ``Electron Optics''}
+The angular and energy distributions may be crudely combined into an effective energy distribution by considering each electron arriving at angle $\theta$ to the surface as having effective energy $E' = E \cos^2 \theta$, where the $\cos^2 \theta$ arises from considering only the component of momentum normal to the surface.
-The goal of electron optics applied to TCS is to minimise the effective energy distribution $f(E - E_1)$ of primary electrons at the surface. $f(E - E_1)$ is limited by the emission properties of the cathode, but significantly affected by the focus of the electron gun.
+\end{comment}
+%\footnote{An expression for the effective energy distribution is: $f'(E' - E_1') = \int \int f(E - E_1) n(\theta - \theta_1) \delta(E' - E \cos^2 \theta) d\theta dE$}
-The angular distribution of electrons incident on the sample can be related to $f(E - E_1)$ by treating each electron arriving at angle $\theta$ to the surface as having an effective energy $E_{eff} = E \cos^2 (\theta)$. The width of this angular distribution determines the width of $f(E - E_1)$, whilst the centre determines the value of $U$ for which the measured TCS elastic peak occurs.
+\begin{comment}
+An expression for the effective energy distribution in terms of $f(E - E_1)$ and the angular distribution $n(\theta - \theta_1)$ is:
-It is also important to ensure that the primary electron beam only strikes the sample of interest (and not the sample holder).
+\begin{align*}
+ f'(E' - E_1') &= \int_{-\infty}^{\infty} \int_{-\frac{\pi}{2}}{\frac{\pi}{2}} f(E - E_1) n(\theta - \theta_1) \delta(E' - E \cos^2 \theta) d\theta dE
+\end{align*}
+\end{comment}
-\emph{TODO: Choose which plots to include; Can get a range of similar effects from adjustment of each electrode potential; I have reproduced all the plots here for now}.
-
-Figure \ref{focus_accel_tcs.eps} - Adjusting the accelerating potential
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_accel_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_accel_tcs.eps}
-\end{figure}
+As discussed in \ref{tcs}, the effective energy distribution of primary electrons appears at the contact potential as the first peak in $S(U)$. Any peaks due to inelastic processes are convolved with the effective energy distribution. If the angular distribution is not centred about $\theta_1 = 0$ (due to misalignment of the sample holder) the observed contact potential is increased. Therefore it is desirable to adjust the electron gun so as to produce the narrowest possible distribution, at the lowest possible contact potential. In Figure \ref{focus_central_tcs.eps} we show the adjustment of the central electrodes to minimise the width of the elastic scattering peak.
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_central_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
+ \includegraphics[width=0.5\textwidth, angle=270]{figures/tcs/plots/focus_central_tcs.eps}
+ \caption{Adjusting the central electrodes to optimise the effective energy distribution}
\label{focus_central_tcs.eps}
\end{figure}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_deflection_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_deflection_tcs.eps}
-\end{figure}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/focus_wenhault_tcs.eps}
- \caption{Comparison of TCS curves due to different sets of electron gun potentials; same sample (Au on Si).}
- \label{focus_wenhault_tcs.eps}
-\end{figure}
-
-
-
-
-\subsection{Effect of Evaporation of Ag onto an Si substrate}
-
-\emph{Note to Sergey: I know you said not to do any more experiments, but I did these on Tuesday night because I wanted to compare curves taken under as similar conditions as possible (most previous results were obtained over several days at the least). I used Ag because I was running low on Au.}
-
-Figures \ref{agsiI_tcs.eps} and \ref{agsiII_tcs.eps} show the processed TCS curves for layers of Ag, followed by Ag-Black, evaporated on Si substrates. For comparison, the sample holder (stainless steel) TCS is also shown.
-
-
-The electron gun was focused on the sample shown in \ref{agsiI_tcs.eps}. The sample shown in \ref{agsiII_tcs.eps} was placed in a second sample holder on the opposite side of a rotation manipulator; the gun was not refocused on this sample.
+\subsection{Electron gun simulation}
-\emph{TODO: Explain curves!}
-\begin{enumerate}
- \item Contact potential decreases in going from Si to Ag on Si
- \item BlackAg appears to have a higher elastic peak
- \item The gun electrodes are the same, but the two sets of curves are clearly different; due to dodgy sample holder; best not mention
- (Only present one of these graphs?)
- \item Can see that beam is not hitting the sample holder (best seen in the second plot), because the elastic peak of the sample holder is clearly not visible in the TCS of the Si substrate.
- \item Positive TCS - Indicates more inelastic interaction mechanisms are possible (threshold energy reached)
- \item Negative TCS - Indicates fewer inelastic interaction mechanisms. ???
- \item Why does TCS change very smoothly? Is the convolution of primary and secondary maxima sufficient to explain this?
- \begin{itemize}
- \item I can fit for the location and size of gaussian peaks if required.
- \end{itemize}
- \item TCS of BlackAg appears very similar, but shifted, for the two trials
-\end{enumerate}
-
-\emph{Note: I also have plots of I(E) curves}
+Figures \ref{egun_simulation1.pdf} and \ref{egun_simulation2.pdf} show the results of an electron gun simulation written for this project. The results of this simulation were not used to focus the actual electron gun; however Figure \ref{egun_simulation1.pdf} was useful, as it shows the possibility for electrons to strike the insulating posts holding the gun together. An insulating material in the path of the electron beam would become charged over time, and affect the focusing properties of the gun. When these posts were covered with tantalum strips connected to the final electrode, the stability of the measured current at fixed $U$ was improved.
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagI_agsiI_siI_holderI_tcs.eps}
- \caption{Successive TCS curves for a BlackAg evaporated on Ag on a Si substrate.}
- \label{agsiI_tcs.eps}
+ \includegraphics[scale=0.4, angle=270]{figures/egun/egun_simulation1.pdf}
+ \caption{Simulated electron trajectories}
+ \label{egun_simulation1.pdf}
\end{figure}
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagII_agsiII_siII_holderII_tcs.eps}
- \caption{The above TCS comparison repeated for a second sample \\(NB: Ag evaporation time is half that of the first sample; layer is still visible by eye)}
- \label{agsiII_tcs.eps}
+ \includegraphics[scale=0.4, angle=270]{figures/egun/egun_simulation2.pdf}
+ \captionof{figure}{2D Simulation of the electrostatic potential produced by the electron gun}\label{egun_simulation2.pdf}
\end{figure}
-\subsection{Effect of Evaporation of Au on Si}
+\subsection{Deposition of Ag films onto a Si substrate}
-Figure \ref{increased_au_thickness_tcs.eps} shows the comparison between TCS obtained from a thin layer of Au on Si and a thicker layer of Au.
+We have measured the total current spectra for Ag films deposited onto an Si substrate. An optically thick layer of Ag, followed by a thin layer of Black Ag \footnote{pressures approx $10^{-7}$ and $0.18\text{mbar}$ respectively} were deposited, with measurements performed before and after each deposition.
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/increased_au_thickness_tcs.eps}
- \label{increased_au_thickness_tcs.eps}
+ \includegraphics[width=0.80\textwidth, angle=0]{figures/tcs/plots/ag_si.eps}
+ \caption{Comparison of Si and Ag on Si TCS}
+ \label{agsiI_tcs}
\end{figure}
-Figure \ref{blackau_on_au_on_si_tcs.eps} shows the effect of evaporating Black-Au on a thick layer of Au on Si.
+In Figure \ref{agsiI_tcs}, the total current spectrum of the sample changes dramatically with the Ag deposition. The contact potential of the surface decreases by about $1.7$V. Typical literature values for Si and Ag work functions would predict a shift of at most $4.9 - 4.2 = 0.7$V. In interpreting this shift it is important to note that our surfaces are not atomically clean.
+
+Ellipsometric measurements had found that the Si substrates used in this study had $\text{SiO}_2$ surface layers with thicknesses of several nanometers. Comparing literature values for Ag and $\text{SiO}_2$ work functions shows that the expected difference in contact potentials for an Ag and $\text{SiO}_2$ is between $0.8$V and $1.8$V\footnote{The exact values of the work functions depend upon the orientation of the crystal lattice at the surface layer and shape of the Fermi-surface of the material}.
+
+In addition to the change in contact potential of the surface, an inflection point is visible in the Ag spectrum at the location of the contact potential for $\text{SiO}_2$. Even though the Ag sample was optically thick, it seems that the surface potential of the underlying $\text{SiO}_2$ layer may still be contributing to $S(U)$.
+
+
\begin{figure}[H]
\centering
- \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackau_on_au_on_si_tcs.eps}
- \label{blackau_on_au_on_si_tcs.eps}
+ \includegraphics[width=0.80\textwidth]{figures/tcs/plots/blackag_ag.eps}
+ \caption{Comparison of Ag/Si and Black Ag on Ag/Si spectra}
+ \label{blackagsiI_tcs}
\end{figure}
-Disagrees with the BlackAg on Ag on Si... I am really confused.
-\pagebreak
+Figure \ref{blackagsiI_tcs} shows the change in TCS after a layer of Black Ag is deposited on the existing Ag layer. The contact potential of the surface changes only slightly. This is unsurprising, as the new surface layer consists mostly of the same material. However, the surface peak has narrowed, despite no change in the focusing of the electron gun. This change in surface peak may be attributed to a change in the surface potential of the sample after the Black Ag layer was deposited. In particular the surface peak has narrowed, which is indicative of either a sharper potential barrier at the surface, or a more uniform potential accross the irradiated surface area.
-\section{Variable Angle Spectroscopy Ellipsometry}
+Our experimental setup has been limited to applied potentials of $0$ to $16$V. The contact potentials of the surfaces have limited the range of primary electron energies to just over $10$ eV. Referring to Figure \ref{komolov1979} (which is idealised), it is recommended that this range be extended if the experiment were to be used for study of inelastic scattering processes.
-\subsection{Ag-Bright on Si substrate}
+\begin{comment}
+Each stage in this experiment was repeated for another Si sample in the second sample holder. Although the exact shape of the total current spectra differed\footnote{The contact potentials were roughly 5V higher. This is most likely because the optimum focusing potentials for the first sample holder were suboptimal for the second, due to differences in height and distance from the electron gun}, we observed similar changes in the contact potential difference with the deposition of Ag and Black-Ag films.
+\end{comment}
+%\begin{figure}[H]
+% \centering
+% \includegraphics[width=0.6\textwidth, angle=270]{figures/tcs/plots/blackagII_agsiII_siII_holderII_tcs.eps}
+% \caption{The above TCS comparison repeated for a second sample \\(NB: Ag evaporation time is half that of the first sample; layer is still visible by eye)}
+% \label{agsiII_tcs.eps}
+%\end{figure}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/psi_final_model.png}
- \label{psi_final_model.png}
-\end{figure}
+%\begin{comment}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/delta_final_model.png}
- \label{delta_final_model.png}
-\end{figure}
+
+\section{Optical Transmission Spectroscopy}
+
+In the transmission spectroscopy experiments, white light has been shone through a thin metallic film mounted on a glass slide. A commercial visible range optical spectrometer\footnote{OceanOptics QE65000} was used to measure the spectrum of the transmitted light in comparison. The transmission of a sample can be determined after first measuring the spectrum of the white light source. For thin films on a glass substrate, the transmission spectrum may be estimated after first determining the transmission spectrum of the glass.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/ag_on_si/ag_fit_vs_bulk_opticalconstants.png}
- \label{ag_fit_vs_bulk_opticalconstants.png}
+ \includegraphics[width=0.6\textwidth]{figures/transmission_spectroscopy/transmission_spectroscopy.pdf}
+ \caption{Setup for a transmission spectroscopy experiment}
\end{figure}
-The plots show the measured and fitted ellipsometric parameters for a thin film of Ag on a Si substrate. The model was constructed to include an $\text{SiO}^2$ oxide layer on the Si, and a surface roughness Effective Medium Approximation (EMA) (Bruggeman). A fit was first performed for the thickness of the Ag film assuming bulk optical constants; this fit was then improved by allowing the software to adjust the Ag film's optical constants. Final model:
+A 653nm filter was used to test the response of the spectrometer. The measured wavelength for peak transmission was $650.8$nm. The stated uncertainty in the filter's peak transmission wavelength was $\pm 2\%$ (approx. 13nm).
-\begin{center}
- \begin{tabular}{lll}
- {\bf Layer} & {\bf Thickness} \\
- Ag (fit for $n$ and $k$) & $16.092 \pm 2.7$ nm \\
- Intermix (Ag/$\text{SiO}^2$) & $0.267 \pm 0.03$ nm \\
- $\text{SiO}^2$ & $4.02 \pm 0.57$ nm \\
- Si & (substrate)
- \end{tabular}
- \captionof{table}{Model for thin Ag on Si}
-\end{center}
-\subsection{Black Ag on Si}
+\subsection{Reference Spectrum}
+The Ellipsometer's Xe Arc Lamp was used as a light source. Its spectrum $I_0(\lambda)$ is shown in Figure \ref{reference.eps}. This measurement established that the Xe Arc lamp was indistinguishable from background light levels below $\lambda \approx 320$nm. %The Xe arc lamp has several strong emission lines in the near infra-red (above 800nm). %The subsequent results have all been normalised to this reference spectrum.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/psi.png}
- \label{psi_final_model.png}
+ \includegraphics[width=0.7\textwidth]{figures/transmission_spectroscopy/reference.eps}
+ \caption{Xe Lamp reference spectrum}
+ \label{reference.eps}
\end{figure}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/delta.png}
- \label{delta_final_model.png}
-\end{figure}
+\begin{comment}
+\subsection{Testing the Spectrometer}
+
+A 653nm filter was used to test the response of the spectrometer. Figure \ref{653nm_filter.eps} shows a spectrum for the Xe lamp shone through this filter; according to the spectrometer, the location of the peak is at 650.8nm. The stated uncertainty in the filter's peak transmission wavelength is $\pm 2$.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth, angle=0]{figures/ellipsometer/blackag_on_si/blackag_opticalconstants_comparison.png}
- \label{ag_fit_vs_bulk_opticalconstants.png}
+ \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/653nm_filter.eps}
+ \caption{Tested Spectrometer with 653nm Filter}
+ \label{653nm_filter.eps}
\end{figure}
+\end{comment}
-\begin{center}
- \begin{tabular}{lll}
- {\bf Layer} & {\bf Thickness} \\
- Surface roughness EMA (75.8\% void) & 2.708 nm \\
- Black Ag (fit for $n$ and $k$) & 3.726 nm \\
- $\text{SiO}^2$ & 8.00 nm \\
- Si & (substrate)
- \end{tabular}
- \captionof{table}{Model for thin Ag on Si}
-\end{center}
-\pagebreak
+\begin{comment}
+\subsection{Transmission Spectra of Glass}
+
+Past studies of the transmissive properties of Black Metal films have generally used nitrocellulose backings for the film \cite{pfund1933} \cite{harris1948}. For our purpose more qualitative measurements were sufficient, and so microscope slide glass available at CAMSP have been used instead. Figure \ref{glass.eps} shows the calculated transmission spectrum for a piece of microscope slide glass. The formula used in calculating the spectrum is:
+
+\begin{align}
+ t(\lambda) &= \frac{I_{\text{measured}}(\lambda)}{I_0(\lambda)} \label{transmission_formula}
+\end{align}
+Where $I_\text{measured}$ is the measured intensity and $I_0$ is the intensity of the reference spectrum.
-\section{Optical Reflection Spectroscopy using the VASE}
-\subsection{Au on Si}
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/au_on_si.png}
- \caption{figure}{Reflection measurements for Au layers on Si}
+ \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/glass.eps}
+ \caption{Glass reference transmission spectrum}
+ \label{glass.eps}
\end{figure}
+\end{comment}
+
+\subsection{Transmission Spectra of Au and Black Au on Glass}
+Transmission spectra for similar thickness Au and Black Au films were measured, accounting for the transmission of the glass and the reference spectrum.
+\begin{comment}
+Equation \ref{shitty_assumption} does not take into account possible backside reflections at the interfaces between the air and glass, and the glass and the film. Such reflections would lead to interference effects, dependent upon the optical properties of both the films and glass, as well as the film thickness. Because the transmission of the glass was measured to be relatively high, \eqref{shitty_assumption} may be used to obtain a reasonable first approximation of the metal films' transmission spectra. Ellipsometric measurement would better characterise the sample.
+\end{comment}
-\subsection{Au on Au-Black on Au on Si}
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/au_on_blackau_si.png}
- \caption{figure}{Reflection measurements for an Au layer on Au-Black on Au layers on Si}
+ \includegraphics[width=0.8\textwidth]{figures/transmission_spectroscopy/blackau.eps}
+ \caption{Transmission Spectra of Au and Black Au films}
\end{figure}
-
-\subsection{Comparison with model of 50nm Au on Si}
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/au_and_blackau/generated_au_on_si_reflection.png}
- \caption{Generated 50nm on Si}
+ \begin{tabular}{ll}
+ \includegraphics[width=0.5\textwidth]{figures/transmission_spectroscopy/au_zoom.eps} &
+ \includegraphics[width=0.5\textwidth]{figures/transmission_spectroscopy/blackau_zoom.eps}
+ \end{tabular}
+ \caption{Transmission Spectra for $\lambda \leq 620$nm}
+ \label{zoom_transmission}
\end{figure}
-Peaks
+The results show that Black Au is far less transmissive than Au in the visible part of the spectrum. Both spectra reveal a similar double peak shape. As found by Pfund and other researchers, the transmission of the Black Au film increases into the infra-red part of the spectrum. There are particularly interesting differences near $350$nm. The Black Au film shows a dip in transmission which is notably absent in the Au film.
-\pagebreak
-\section{Optical Transmission Spectroscopy using OceanOptics Spectrometer}
-\subsection{Dark Spectrum}
+\begin{comment}
+It is difficult to arrive at a possible explanation for this dip based upon the transmission data alone. Plasmonic behaviour is often sensitive to the polarisation of incident light. Ellipsometry, which measures polarisation, was found to be more useful for characterising samples\footnote{The Ellipsometer was unavailable at the time of the Optical Transmission Spectroscopy measurements}.
-{\bf NOTE: Probably won't include in the final thesis}
+\subsection{Effect of Atmosphere on Transmission Spectra of Black Au}
-Figure \ref{dark_comparison.eps} shows the spectrum of the background (taken at different times on the same day), without the light source.
-The room lights were off, the experiment was covered with a cardboard box and layers of black plastic sheeting; but the spectra still changed for different times of the day.
+Harris et al \cite{harris1952} and other studies \cite{mckenzie2006} have examined the differences between Black Au deposited in an atmosphere with or without oxygen present. The Black Au prepared in air may contain traces of tungsten oxides formed at the tungsten filament, whilst Black Au prepared in inert gases was shown to consist entirely of Au. This was the motivation for making a comparison between samples prepared in air and He atmospheres.
\begin{figure}[H]
\centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/dark_comparison.eps}
- \caption{Dark spectra}
- \label{dark_comparison.eps}
+ \includegraphics[width=0.6\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/he_blackau_vs_air_blackau.eps}
+ \caption{Transmission Spectra for Black Au films prepared in different atmospheres}
+ \label{he_blackau_vs_air_blackau.eps}
\end{figure}
-In all subsequent experiments, the dark intensity has been subtracted from measured intensity counts:
-\begin{align*}
- I(\lambda) = I_{\text{measured}}(\lambda) - I_{\text{dark}}(\lambda)
-\end{align*}
+\end{comment}
\pagebreak
-\subsection{Reference Spectrum}
-
-{\bf Note: Also don't include in final thesis? Or at least, remove the time dependence; just show one curve.}
-The Ellipsometer's Xe Arc Lamp was used as a light source. It's spectrum $I_0(\lambda)$ is shown in Figure \ref{reference.eps}
+\section{Variable Angle Spectroscopy Ellipsometry}
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/reference.eps}
- \caption{Xe Lamp reference spectra}
- \label{reference.eps}
-\end{figure}
-Because the dark spectra changed over time scales comparable to the length of measurement, some features in the processed spectra are due to the reference spectra of the Xe lamp.
-\pagebreak
-\subsection{Testing the Spectrometer}
+\subsection{Model for Ag and Black Ag on a Si substrate}
-{\bf Note: Also don't include?}
+Testing showed that it is difficult to use Ellipsometry to characterise black metal films of considerable thickness (estimated $>30nm$), due to the extremely low reflectivity of such films. However, using the WVASE32 software, it was possible to fit for the optical constants of an extremely thin layer of Black Ag prepared on Si using ellipsometric measurements. Figures \ref{n_compare.pdf} and \ref{k_compare.pdf} show the fitted optical constants for the Ag layer in a multilayered model for both a Black Ag thin film, and Ag thin film. Bulk Ag optical constants from Palik's Handbook \cite{palik} were specified for the initial values.
-The spectrometer was tested using a 653nm filter. \ref{653nm_filter.eps}
+The models include an $\text{SiO}_2$ surface layer, with the thickness fit. The EMA layer models the effect of surface roughness in the film. This layer uses the Bruggeman model to describe the surface as a set of spherical inclusions of the Black Ag material in a void. The Bruggeman EMA formula is \cite{bruggeman1935, oates2011}:
+\begin{align*}
+ F \frac{\epsilon_b - \epsilon_{eff}}{\epsilon_b + 2 \epsilon_{eff}} + (1 - F) \frac{\epsilon_c - \epsilon_{eff}}{\epsilon_c + 2\epsilon_{eff}} &= 0
+\end{align*}
+where $\epsilon_b$ and $\epsilon_c$ are the dielectric functions of the two materials (in our case, material $b$ is air; $\epsilon_b = 1$), and $F$ is the volume fraction of material $b$. This model is incorporated into the WVASE32 software.
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/653nm_filter.eps}
- \caption{Tested Spectrometer with 653nm Filter}
- \label{653nm_filter.eps}
-\end{figure}
-The transmission was calculated as:
-\begin{align}
- t(\lambda) &= \frac{I(\lambda)}{I_0{\lambda}} \label{transmission1}
-\end{align}
-Where $I_0(\lambda)$ was the intensity (arbitrary units) of the Xe Arc Lamp at wavelength $\lambda$, and $I(\lambda)$ was the measured intensity.
+Although from SEM images it is clear that the structure of Black films is far more complicated than this approximation, fitting for the fraction of Black Ag in the surface layer shows a majority of the surface is empty. This is consistent with the porous nature of Black metal films seen in SEM images. The thickness of this layer was also a free parameter in the model.
-\subsection{Transmission Spectra of Glass}
+Both the refractive index and extinction coefficient of the Black Ag film show a strong peak around $370$ nm. From the refractive index, the Black Ag film has a much stronger dispersion relation than the Ag film. The extinction coefficient peak indicates a preferential scattering or absorbsion of light at $370$ nm. This may be indicative of surface plasmon resonance effects \cite{oates2011, sonnichsen2001, zheng2008}, particularly since it occurs near to the bulk plasmon frequency for Ag. It is interesting to note that the peak in extinction for the thin Ag film occurs within $30$ nm of the dip in transmission measured for an Au film (Figure \ref{zoom_transmission}).
-{\bf Note: Should probably include this, as the substrate is important to the final transmission}
-All films were prepared on microscope glass; the transmission of the glass must be known to determine the transmission of the films.
\begin{figure}[H]
\centering
- \includegraphics[width=0.5\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/glass_transmission.eps}
- \caption{Glass reference transmission spectrum}
- \label{glass_transmission.eps}
+ \includegraphics[width=0.80\textwidth]{figures/ellipsometer/ag_vs_blackag/n_compare.pdf}
+ \caption{Fitted refractive index for the Ag layer in multilayered models for Ag and Black Ag (step size 50 nm)}
+ \label{n_compare.pdf}
\end{figure}
-{\bf NOTE:} The reason that the glass has transmission $> 1$ is (probably) because the background level has increased between the reference measurement and the measurement of glass. I should probably normalise the glass transmission spectrum to its maximum value.
-
-Transmission was calculated using \eqref{transmission1}.
-
-\subsection{Transmission Spectra of Au and Au-Black on Glass}
-
-Figure \ref{blackau_vs_au.eps} shows all measured transmission spectra for Au vs Au-Black (pressure 1e-6 is for the Au-bright films, all others are Au-Black) {\bf NOTE: Need to relabel plot}
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/blackau_vs_au.eps}
- \caption{Transmission Spectra for various Au films}
- \label{blackau_vs_au.eps}
+ \includegraphics[width=0.80\textwidth]{figures/ellipsometer/ag_vs_blackag/k_compare.pdf}
+ \caption{Fitted extinction coefficient for the Ag layer in multilayered models for Ag and Black Ag (step size 50 nm)}
+ \label{k_compare.pdf}
\end{figure}
-Transmission is calculated as:
+
+\subsection{Surface and Bulk Plasmons in the Ag and Black Ag films}
+
+The bulk loss function as introduced in Section \ref{tcs_e} is:
\begin{align*}
- t &= \frac{I(\lambda)}{I_0(\lambda)} \times \frac{I_\text{glass}(\lambda)}{I_0(\lambda)}
+ L_b = -\text{Im}\frac{1}{\phasor{\epsilon}}
\end{align*}
-Where $t_{\text{glass}} = \frac{I_\text{glass}}{I_0}$ is the transmission spectrum of the microscope slide glass.
-{\bf Note: I should select just 2 or 3 of these spectra to use in the final report}
+The occurance of maxima in $L_b$ can be used as a condition for determining bulk plasmon excitation frequencies \cite{komolov}.
-The general trends:
-\begin{enumerate}
- \item Thin films (low current or short evaporation time) show similar shape regardless of pressure (1e-6 or 1e-2 mbar)
- \item Thicker layers all show peak near 500nm, followed by minima at 600-700nm
- \item All curves show fine structure at same wavelengths above 800nm. This may be due to the Xe lamp spectrum; if the background level has increased, then Xe lamp spectral features will show up in the final spectrum.
- \item Thick layers of Au-Black show much lower transmission to 700nm, but a much faster increase at longer $\lambda$
- \item At least one of the Au-Black samples shows a similar spectrum to a (thick) Au-Bright sample.
-\end{enumerate}
+For surface plasmon excitations, the surface loss function is \cite{ibach2010}:
+\begin{align*}
+ L_s &= -\omega \text{Im}\left(\frac{1}{1 + \phasor{\epsilon}}\right)
+\end{align*}
-\subsubsection{Effect of Atmosphere on Transmission Spectra of Au-Black}
+When applied to the thin Ag film (Figure \ref{ag_loss}) the bulk loss function shows a strong peak at $320$nm, and is otherwise rather flat. This peak corresponds to the bulk plasmon frequency for Ag ($\hbar \omega_p \approx 3.8\text{eV}$. It should be noted that the stated uncertainty of Ellipsometric measurements is above 20\% for wavelengths below $320$nm. In addition we initially specified the film to have bulk optical constants, for which this result is to be expected.
-A paper \cite{} has found differences between Au-Black prepared in Air or an inert gas. The Au-Black prepared in Air contains traces of Tungsten Oxides; the Au-Black prepared in an inert gas does not. This was the motivation for making a comparison between samples prepared in Air and He.
+When the bulk and surface loss functions are applied to the Black Ag film (Figure \ref{blackag_loss}), there is in fact a shallow minima at $370$nm. In contrast to the Ag film, the loss functions appear to increase monatomically for longer wavelengths.
-\begin{figure}[H]
- \centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/he_blackau_vs_air_blackau.eps}
- \caption{Transmission Spectra for Black Au films prepared in different atmospheres}
- \label{he_blackau_vs_air_blackau.eps}
-\end{figure}
-\subsection{Transmission Spectra of Ag}
+Based upon these results, we cannot conclude that this particular Black Ag film will support surface or bulk plasmon oscillations. However, we cannot rule out that localised plasmonic resonance effects contribute to a scattering of light causing the peak in $k$ around $3800$. Due to the complicated structure of the surface it would be difficult to theoretically describe the nature of such effects. A starting point for future theoretical work may be Harris' models of black metal films as a series of interwoven conducting strands \cite{harris1952}.
-A pre-existing Ag sample (unknown preparation conditions), on glass.
\begin{figure}[H]
\centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/silver_transmission.eps}
- \caption{Transmission Spectra for a Silver film on glass}
- \label{silver_transmission.eps}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ag_loss.eps}
+ \caption{Pseudo-loss functions for the Ag thin film}
+ \label{ag_loss}
\end{figure}
-\subsection{Transmission Spectra of Ag and Ag-Black on Glass}
-
-The Ag sample compared with Ag-Black.
-Notice fine structure not in original Ag sample. Probably due to dark spectrum changing.
-
-A pre-existing Ag sample (unknown preparation conditions), on glass.
-
\begin{figure}[H]
\centering
- \includegraphics[width=0.7\textwidth, angle=270]{/home/sam/Documents/University/honours/thesis/figures/transmission_spectroscopy/blackag_vs_ag.eps}
- \caption{Transmission Spectra for a Silver film on glass}
- \label{blackag_vs_ag.eps}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/blackag_loss.eps}
+ \caption{Pseudo-loss functions for the Black Ag thin film}
+ \label{blackag_loss}
\end{figure}
-{\bf Note:} The Ag-Black is much thinner than the Ag-Bright sample; by eye it appears to be a thin grey layer. Also, the Ag-Bright sample was not uniformly thick; part of the film had been scratched or wiped off.
+\pagebreak
+
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-\chapter{Experimental Techniques}
+\chapter{Techniques} \label{chapter_techniques}
+\section{Total Current Spectroscopy} \label{tcs}
-\section{Total Current Spectroscopy}
-
-In Total Current Spectroscopy experiments, a current of primary electrons $I_1$ is directed at a target surface. Upon interacting with the surface, the primary electron beam is split into two components; the transmitted current $I$, and the secondary electron current $I_2$. The current of secondary electrons includes all electrons emergent from the surface, regardless of origin. Generally $I_2$ includes components formed from elastically and inelastically scattered primary electrons, as well as electrons originating from bound states which have gained sufficient energy to leave the surface.
-
-For any given mechanism behind the origin of an electron in $I_2$, there is an associated ``threshold'' primary electron energy which must be exceeded before the process can occur. As a result, measurement of changes in $I_2$ as a function of primary electron energy $E_1$ provides a very sensitive means to characterise properties of the sample under bombardment. The energy $E_1$ of primary electrons is controlled by adjustment of the potential $U$.
-
+The optical properties of metals depend upon both conduction and valance band electrons. At the surface of a material, the electron spectrum (energy levels, band structure and densities of states) may differ greatly from the bulk. This is largely due to the sharp change in potential at the interface; rearrangement of lattice sites, ``dangling'' molecular bonds, and adsorbed defects are also contributing factors
+Total Current Spectroscopy is an electronic spectroscopy technique which is extremely sensitive to the electronic properties of the surface region. The experimental setup for Total Current Spectroscopy can be easily integrated into existing apparatus for sample preparation, which allows for measurements to be made in situ.
\begin{center}
\includegraphics[scale=0.60]{figures/tcs/tcs_simple}
- \captionof{figure}{ A simplified schematic of Total Current Spectroscopy Experiments }
+ \captionof{figure}{ A simplified schematic of a Total Current Spectroscopy Experiment}
\label{tcs_simple.pdf}
\end{center}
-Figure \ref{tcs_simple.pdf} shows a simplified schematic for a Total Current Spectroscopy experiment
-\footnote{For a more detailed description of the experimental setup, refer to Appendix \ref{}}.
-When a current is passed through the cathode, electrons are thermionically emitted with a distribution in initial velocities. A series of electrodes (an electron gun) creates a potential which focuses the emitted electrons into a beam and accelerates them towards the target. The transmitted current $I$ can be detected external to the vacuum chamber using a conventional DC ammeter\footnote{It is also possible to use lock-in amplifier techniques for noise reduction \cite{komolov}. In this study, the DC ammeter has been used due to the relative simplicity of the measurement and control circuit.}.\
+In Total Current Spectroscopy experiments (Figure \ref{tcs_simple.pdf}), a current of primary electrons $I_1$ is directed at a target surface. Upon interacting with the surface, the primary electron beam is split into two components; the transmitted current $I$, and the secondary electron current $I_2$. $I_2$ includes components formed from elastically and inelastically scattered primary electrons, as well as any ``true secondary'' electrons emitted by the surface.
+
+For each mechanism behind the origin of an electron in $I_2$, there is an associated ``threshold'' primary electron energy which must be exceeded before the process can occur. As a result, measurement of changes in $I_2$ as a function of primary electron energy $E_1$ provides a sensitive means to characterise properties of the sample under bombardment. The energy $E_1$ of primary electrons is controlled by adjustment of the potential $U$ applied between the sample and cathode.
+
+
+Primary electrons are thermionically emitted at a cathode with a distribution in energies. A series of electrodes (an electron gun) focuses the emitted electrons into a beam and produces the current $I_1$ at the target. A feedthrough connected to the sample holder allows the transmitted current $I$ to be measured external to the vacuum chamber using an electrometer. Measurement of $I$ instead of $I_2$ is generally preferred, since changes in $I$ can be directly related to changes in $I_2$.
+
The total current spectrum (TCS) is defined as:
\begin{align*}
S(E_1) &= \der{I}{E_1} = -\der{I_2}{E_1}
\end{align*}
-This result assumes that the primary electron current $I_1$ is constant. Such an assumption is valid if the cathode has reached thermal equilibrium, and the potential due to the sample can be considered to have negligable effect on the focusing properties of the electron gun.
-
-The experimental goal of Total Current Spectroscopy is the measurement of $S(E_1) \propto \der{I_2}{E_1}$. More information on the experimental setup and techniques are presented in Appendix \ref{}. The remainder of this section will give an overview of concepts needed for relating $S(E_1)$ to properties of a sample.
-
+This result assumes that the primary electron current $I_1$ is constant. This assumption is generally valid over long time scales once the cathode has reached thermal equilibrium. \footnote{In the final experimental setup, the primary electron current was found to vary by about $2\%$ over the course of several days; far longer than the time taken for total current spectrum measurements (30s to 10min)}
-\subsubsection{Relationship between $S(E_1)$ and electron-surface interactions} \label{tcs_theory1}
-Here we will summarise the approach of Komolov \cite{komolov} in constructing a theory relating $S(E_1)$ to scattering events within the target surface.
+\subsection{General form of $S(E_1)$} \label{tcs_theory1}
-% Contact potential
-A single electron arriving at the sample has energy $E = eU + c$, where $e$ is the electron charge, $U$ is the potential applied between the cathode and sample, and $c$ is a constant which includes the electron's energy relative to the sample when emitted. The minimum value for $c$ is the contact potential of the cathode relative to the sample.
+In the following, a generalised formula for $S(E_1)$ will be presented as derived by Komolov \cite{komolov}.
-At the cathode, electrons are emitted with a distribution in energies about some mean value. A realistic model should take into account this distribution.
-
-If the primary electrons are incident perpendicular to the surface, then we can write $I$ as an integral over the whole distribution of energies:
+The current of primary electrons incident perpendicular to the surface can be written as:
\begin{align*}
- I(E_1) = e A \int_0^{\infty} f(E - E_1) dE
+ I_1(E_1) = e A \int_0^{\infty} f(E - E_1) dE
\end{align*}
-where $f(E - E_1)$ is the distribution for an electron of energy $E$ arriving at the surface. Generally $f(0)$ (ie: $E = E_1$) is the maximum of $f$.
-
-\emph{TODO: Discuss angular distribution of incident electrons, due to focusing of electron gun?}
+where $f(E - E_1)$ gives the distribution for electrons of energy $E$ arriving at the surface. $f(0)$ (ie: $E = E_1$) is the maximum of $f$.
-To formulate a general expression for the secondary current, we introduce a cross section $\sigma(E)$, which gives the probability for a primary electron of energy $E$ to give rise to a secondary electron (of any energy $E_2 <= E$).
-
-Then the total current of secondary electrons is:
+The total secondary current may be written as:
\begin{align*}
I_2(E_1) &= e A \int_{0}^{\infty} f(E - E_1) \sigma(E) dE
\end{align*}
-Using $I = I_1 - I_2$, and $S(E_1) = \der{I}{E_1}$, it is straight forward to arrive at a general expression for the total current spectrum \cite{komolov}:
-\begin{align*}
- S(E_1) &= e A \left\{ [ 1 - \sigma(0) ] f(-E_1) + \int_{0}^{\infty} f(E - E_1) \der{\sigma(E_1)}{E_1} dE \right\}
-\end{align*}
+Where the cross section $\sigma(E)$ is the probability for a primary electron of energy $E$ to give rise to a secondary electron (of any energy $E_2 \leq E$).
+
+Using $I = I_1 - I_2$, it is straight forward to arrive at a general expression for $S(E_1)$:
+\begin{align}
+ S(E_1) &= e A \left\{ [ 1 - \sigma(0) ] f(-E_1) + \int_{0}^{\infty} f(E - E_1) \der{\sigma(E_1)}{E_1} dE \right\} \label{tcs_full}
+\end{align}
-All $E_1$ dependence in the first term is due soley to the distribution of primary electrons. It is clear that this term is maximised when $E_1 = 0$ with respect to the sample; ie: the contact potential between the cathode and sample is zero.
+All $E_1$ dependence in the first term is due soley to the primary electron energy distribution. This term is responsible for the first peak in an $S(E_1)$ curve.
-The second term contains dependence upon $\der{\sigma(E_1)}{E_1}$. As $E_1$ is increased past the threshold for a particular interaction, $\sigma(E_1)$ will undergo a sharp change. This corresponds to a narrow maxima or minima in the derivative $\der{\sigma(E_1)}{E_1}$. A corresponding maxima or minima will appear in $S(E_1)$, centred about the threshold for the interaction. The convolution with the primary electron distribution $f(E - E_1)$ has the effect of broadening and lowering these peaks; in other words, the resolution of Total Current Spectroscopy is limited by the distribution of primary electrons.
+The second term contains dependence upon $\der{\sigma(E_1)}{E_1}$. As $E_1$ is increased past the threshold for a particular interaction, $\sigma(E_1)$ will undergo a sharp change. This corresponds to a narrow maxima or minima in the derivative $\der{\sigma(E_1)}{E_1}$. A corresponding maxima or minima will appear in $S(E_1)$, centred about the threshold for the interaction. The convolution with the primary electron distribution $f(E - E_1)$ has the effect of broadening and lowering these peaks; in other words, the resolution of total current spectroscopy is limited by the distribution of primary electron energies.
The (unphysical) case of a mono-energetic beam is equivelant to setting $f(E - E_1) = \delta(E - E_1)$. In this case, the integrals in the expressions for $I$ and $I_2$ collapse, and the resulting total current spectrum is:
+\begin{align}
+ S(E_1) &= \der{I}{E_1} = e A \frac{d}{dE_1} \left( 1 - \sigma(E_1) \right) = e A \der{\sigma(E_1)}{E_1} \label{tcs_simple}
+\end{align}
+
+A form of \eqref{tcs_simple} is usually assumed when constructing a more detailed theory of secondary electron current formation, as the location of peaks due to $\der{\sigma(E_1)}{E_1}$ is the same in both \eqref{tcs_simple} and \eqref{tcs_full}. Figure \ref{komolov1979} illustrates an idealised total current spectrum.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/tcs/komolov1979_tcs.png}
+ \caption{An idealised total current spectrum (Komolov et al 1979 \cite{komolov1979})}
+ \label{komolov1979}
+\end{figure}
+
+\subsection{Contact Potential and the Surface Peak}
+
+The case $E_1 = 0$ does not in general correspond to $U = 0$. Figure \ref{contact.pdf} describes a simplified step potential model for the surfaces of the cathode and sample. In a classical approximation, primary electrons will be elastically scattered from the sample unless they have energy greater than its vacuum level.
+
+At the cathode, electrons are thermionically excited from the conduction band to the vacuum level. The vacuum levels of the cathode and surface are not generally equal. The contact potential is the difference in work functions of the materials. As $U$ approaches the contact potential, primary electrons are able to penetrate into the sample, and a sharp peak termed the surface peak is seen in $S(U)$. The maxima of this peak occurs at an applied potential $U$ such that $E_1 = 0$; its shape is indicative of $f(E - E_1)$.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.80\textwidth]{figures/tcs/contact.pdf}
+ \caption{Illustration of the step potential model for the surfaces}
+ \label{contact.pdf}
+\end{figure}
+
+
+
+
+\subsection{Electron-Electron Interactions}
+\label{tcs_e}
+
+
+In the Sommerfield free electron gas approximation, electrons are assumed to be contained within a rectangular potential well, with energies given by $E_k = \frac{\hbar^2 k^2}{2m}$, where $\vect{k}$ is the electron wave vector. Electrons fill states up to the Fermi level, with density of states $N(E_k)$ proportional to $\sqrt{E_k}$.
+
+An incoming primary electron interacting with the free electron gas may either excite a single electron to above the Fermi level, or a collective vibration (plasmon). A plasmon may be excited if $E_1 \geq \hbar \omega_p$.
+
+The response of a free electron gas to an external electric field is characterised by $\phasor{\epsilon}$. The imaginary part of $\phasor{\epsilon}$ describes the attenuation of the electric field; it describes the process of energy transfer from the primary electron to the electron gas. Since the intensity of the electric field entering the solid decreases by a factor of $|\phasor{\epsilon}^2|$, the efficiency of energy transfer is given by:
+
\begin{align*}
- S(E_1) &= \der{I}{E_1} = e A \frac{d}{dE_1} \left( 1 - \sigma(E_1) \right) = e A \der{\sigma(E_1)}{E_1}
+ \frac{\epsilon_2}{|\phasor{\epsilon}|^2} = -\text{Im}\left(\frac{1}{\phasor{\epsilon}}\right)
\end{align*}
-{\bf NOTE: Komolov goes on to find expressions for $\sigma(E_1)$ in terms of specific inelastic processes...}
+This function is often referred to as the ``Bulk loss''. A maxima in the bulk loss is indicative of a high probability for primary electrons to inelastically scatter from the free electron gas.
+
+
+
+
+\subsection{Implementation of Total Current Spectroscopy Experiment}
+
+As part of this project, we designed and built most of the electronics for an automated Total Current Spectroscopy setup. Figure \ref{tcs_block} shows a block diagram illustrating the key components of the setup. Figure \ref{electron_gun_circuit} shows the circuit diagram for control of the electron gun. Due to the limited range of available power supplies, our experiment has focused on the surface peak of the samples.
+
+In order to automate TCS experiments, both Digital to Analogue and Analogue to Digital Convertors were required (DAC and ADC). To provide these, a custom DAC/ADC Box was designed and constructed. The box can be controlled by any conventional computer with available RS-232 serial communication (COM) ports. The full design of both hardware and software is available on request.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/presentation/tcs_block.png}
+ \caption{Block diagram for TCS setup}
+ \label{tcs_block}
+\end{figure}
+
+\begin{landscape}
+\begin{figure}[H]
+ \includegraphics[width=1.25\textwidth]{figures/egun/electron_gun.pdf}
+ \caption{TCS circuit diagram}
+ \label{electron_gun_circuit}
+\end{figure}
+\end{landscape}
\pagebreak
-\section{Ellipsometry}
+\section{Ellipsometry} \label{Ellipsometry}
-\subsection{Overview}
+Ellipsometry is a versatile optical technique which can be used to gain a great deal of information about optical and structural properties of thin films. In particular, Ellipsometry may be used to determine the pseudo-dielectric constant $\phasor{\epsilon}$ of a sample. This makes ellipsometry a useful complementary technique to secondary electron spectroscopy experiments, where $\phasor{\epsilon}$ is important for descriptions of electron-electron interactions.
-Ellipsometry is an optical technique which measures the change in polarisation of light reflected from a surface. This change in polarisation can be related to the optical properties of the surface, including optical constants or the thickness of thin film surface layers.
+An ellipsometer is designed to establish a beam of light with known polarisation, and measure the change in polarisation due to reflection of the light from a surface. This change in polarisation can be related to the optical properties of the surface, or the thicknesses of a multi-layered sample.
-In the Jone's formalism, polarisation states may be represented by orthogonal electric field components $E_p$ and $E_s$, which are polarised parallel and perpendicular to the plane of incidence respectively. The reflection of a light ray from the surface is described by the matrix equation:
+In the Jone's formalism, polarisation states may be represented by orthogonal electric field components $E_p$ and $E_s$, which are polarised parallel and perpendicular to the plane of incidence respectively. The reflection of a polarised light ray from the surface is described by the matrix equation:
\begin{align*}
\left[\begin{array}{c} E_{rp} \\ E_{rs} \end{array}\right] &= \left[ \begin{array}{cc} r_{pp} & r_{ps} \\ r_{sp} & r_{ss} \end{array} \right] \left[\begin{array}{c} E_{ip} \\ E_{is} \end{array}\right]
\end{align*}
\begin{figure}[H]
\centering
\includegraphics[width=0.80\textwidth]{figures/ellipsometer/ellipsometer_measurement.png}
- \caption{Diagram of an Ellipsometric Measurement \cite{woolam1999}}
+ \caption{Illustration of an ellipsometric measurement \cite{oates2011}}
\label{ellipsometer_measurement}
\end{figure}
The value of $\tan(\psi)$ gives the ratio of amplitudes between the $p$ and $s$ components of the reflected electric field, whilst $\Delta$ gives the phase difference.
-In the case where the sample is anisotropic, $\psi$ and $\Delta$ alone are not sufficient to characterise the sample; three seperate ratios of fresnel reflection coefficients are required \cite{woolam2000}:
-
-
-Light may consist of two or more components of well defined polarisation states; as a result, the total beam cannot be described with a single well defined Jones vector. Ellipsometers are designed to establish a well defined polarisation state of light incident on the sample; however non-uniform films or backside reflection from a substrate may cause the reflected beam to be partially polarised. As a result, the Jone's formalism is not sufficient for characterisation of these samples, and the more general Stokes formalise (with 4 component vectors) must be employed \cite{woolam2000} \cite{oates2011}.
+For an anisotropic sample, $\psi$ and $\Delta$ alone are not sufficient to characterise the sample; three seperate ratios of fresnel reflection coefficients are required. Non-uniform films or backside reflection from a substrate may cause the reflected beam to be partially polarised. As a result, the Jone's formalism is not sufficient for characterisation of these samples, and the more general Stokes formalism (which uses 4 component vectors to describe polarisation states) must be employed \cite{woolam2000} \cite{oates2011}.
\begin{table}[H]
\centering
\includegraphics[scale=0.75]{figures/ellipsometer/linear_polarisation} \\
\end{tabular}
- \captionof{figure}{From left to right, circular, elliptical and linearly polaristed light, viewed down the axis of beam propagation}
+ \captionof{figure}{From left to right, circular, elliptical and linearly polarised light, viewed along the wavevector of the light}
\end{table}
+
+\subsection{Relation of measurements to properties of the sample}
+
+\subsubsection{Bulk Optical Constants}
+
+The simplest sample is a flat substrate of infinite thickness. In this case, the optical constants of the substrate can be determined directly from $\rho$:
+\begin{align*}
+ \phasor{\epsilon} &= \epsilon_1 + i \epsilon_2 = \sin^2 (\phi) \left( 1 + \tan^2(\phi) \frac{1 - \rho}{1 +\rho}^2\right)
+\end{align*}
+Where $\phasor{\epsilon}$ is the psueodo-dielectric function. The complex refractive index of the material can be easily related to $\phasor{\epsilon}$:
+\begin{align*}
+ \phasor{\epsilon} &= \phasor{n}^2 = (n + i \kappa)^2
+\end{align*}
+Where $n$ is the refractive index, and $\kappa$ is the extinction coefficient.
+
+
+
+\subsubsection{Multi-layered Samples}
+
+At each layer in a multi-layered film, light is be both reflected and transmitted. The measured signal is the result of interference between reflections from each layer. The phase difference for each component of the beam is determined by both the optical constants and the thicknesses of the layers through which the component has passed.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.5\textwidth]{figures/ellipsometer/multilayered.pdf}
+ \caption{Interaction of light with a multi-layered sample}
+\end{figure}
+
+
+\subsubsection*{A Note on Si Substrates}
+
+A real substrate stored in laboratory air will generally have thin surface layers of oxides. For example, most of the thin film samples produced for this study were prepared on Si substrates. The inclusion of a layer of $\text{SiO}_2$ between the Si substrate and the thin film was found to have a significant effect on the accuracy with which the properties of the sample could be fit.
+
+
+\pagebreak
+
\subsection{Variable Angle Spectroscopic Ellipsometry}
-Although Ellipsometers have been in use for thin film analysis since the ??? \cite{}, traditional instruments were usually limited to single angle and single wavelength measurements, due to the painstaking manual process of repeated measurements. With advances both in software and hardware during the last half of the 20th century, Ellipsometric measurements have become largely automated, allowing for a wide range of optical information to be obtained from a sample. Spectroscopic Ellipsometry obtains measurements for a range of wavelengths, whilst Variable Angle Spectroscopic Ellipsometry repeats these measurements over a range of angles of incidence.
+Although Ellipsometers have been in use for thin film analysis since the late 19th century, traditional instruments were usually limited to single angle and single wavelength measurements, due to the painstaking manual process involved in repeated measurements \cite{tompkins1992}. With advances both in software and hardware during the last half of the 20th century, Ellipsometric measurements have become largely automated, allowing for a huge number of measurements to be easily obtained from a sample \cite{woolam1999, woolam2000}.
-The ease with which large amounts of data can be taken from an ellipsometer means that the method is well suited to numerical analysis and fitting procedures. At CAMSP a Variable Angle Spectroscopic Ellipsometer (VASE)\footnote{J. A. Woolam and Co} and the associated software\footnote{WVASE32} have been employed in the analysis of thin film samples.
+Spectroscopic Ellipsometry obtains measurements for a range of wavelengths of the incident light. A Variable Angle Spectropic Ellipsometer (VASE) repeats measurements over a range of different angles of incidence. Because of the wealth of data aquired, these techniques are well suited to numerical analysis and fitting procedures to determine both the optical constants and thickness of unknown samples.
+
+At CAMSP a Variable Angle Spectroscopic Ellipsometer (VASE)\footnote{J. A. Woolam and Co} and the associated software (WVASE32) have been employed in the analysis of thin film samples. Figure \ref{ellipsometer.png} shows a block diagram of the VASE.
+
+The WVASE32 software allows for the construction of a model of a given sample, using tabulated literature values for optical constants, and allowing the user to specify film thicknesses. This model can then be adjusted using mean square error minimisation fitting algorithms to determine the thicknesses and/or optical constants for the model which best match the measured data. The modelling procedure is illustrated in Figure \ref{procedure.png}.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/ellipsometer.png}
- \caption{Block diagram of the VASE \\(taken from \emph{Overview of Variable Angle Spectroscopic
-Ellipsometry (VASE), Part I:
-Basic Theory and Typical Applications}
-\cite{woolam1999})}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ellipsometer.png}
+ \caption{Block diagram of the VASE \cite{woolam1999}}
\label{ellipsometer.png}
\end{figure}
-\subsection{Relation of $\psi$ and $\Delta$ to properties of the sample}
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ellipsometry_block.png}
+ \caption{Illustration of the VASE analysis and modelling procedure \cite{woolam1999}}
+ \label{procedure.png}
+\end{figure}
-\subsubsection{Bulk Substrates}
-The simplest sample is a bulk substrate. In this case,
+\section{Vacuum Techniques and Sample Preparation}
-\subsubsection{Single Layered Thin Films}
+All samples required for this study were prepared using available equipment at CAMSP. A small (approx. 25L) vacuum chamber, which has been used previously for thin film preparation at CAMSP \cite{kostylev2011} was repurposed to allow for both deposition of metallic thin films, and subsequent study using total current spectroscopy. A diagram of this setup is shown in Figure \ref{chamber}.
+A rotatable stainless steel sample holder was positioned in the centre of the vacuum chamber. A flange containing evaporators was placed on one side of the chamber, whilst the electron gun required for total current spectroscopy was placed directly opposite. Shielding was used to ensure the electron gun was not coated during deposition. Two sample holders were attached to either side of the shielding to allow for preparation and study of two samples without the need for venting the vacuum chamber.
+The evaporators consisted of a tungsten wire filament (diameter 0.5mm) attached using spot welds between two feedthroughs. A piece of the desired metal was folded over the apex of the tungsten wire. The metal was then heated by passing a current through the filament; at sufficiently high currents, the metal piece began to evaporate, with a proportion of the flux of evaporated particles striking the target sample. To remove any contaminating layers from the metal, and ensure uniform evaporation, this procedure was first performed at low pressure (below $10^{-6}$ mbar) with no sample in the chamber, with the current increased until the metal piece began to melt and form a ball on the wire.
-\subsubsection{Multi-layered Thin Films}
+This study focused primarily on depositing Au and Ag films on Si substrates (approx 10x10x3mm wafers), at both high and low pressures. To remove any organic layers, the substrates and sample holders were cleaned in an acetone bath immediately prior to insertion in the vacuum chamber. The thickness of the deposited layer was controlled by varying both deposition time and the heating current.
-Magical analysis
-\section{Optical Transmission and Reflection Spectroscopy}
+ \begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/pressure/chamber.pdf}
+ \caption{Layout of apparatus within the vacuum chamber}
+ \label{chamber}
+ \end{figure}
-Can be done with the VASE or with OceanOptics spectrometer.
-\section{Scanning Electron Microscopy}
-Done by CMCA, not me.
-\chapter{Experimental Techniques}
+\chapter{Techniques} \label{chapter_techniques}
+\section{Total Current Spectroscopy} \label{tcs}
-\section{Total Current Spectroscopy}
-
-In Total Current Spectroscopy experiments, a current of primary electrons $I_1$ is directed at a target surface. Upon interacting with the surface, the primary electron beam is split into two components; the transmitted current $I$, and the secondary electron current $I_2$. The current of secondary electrons includes all electrons emergent from the surface, regardless of origin. Generally $I_2$ includes components formed from elastically and inelastically scattered primary electrons, as well as electrons originating from bound states which have gained sufficient energy to leave the surface.
-
-For any given mechanism behind the origin of an electron in $I_2$, there is an associated ``threshold'' primary electron energy which must be exceeded before the process can occur. As a result, measurement of changes in $I_2$ as a function of primary electron energy $E_1$ provides a very sensitive means to characterise properties of the sample under bombardment. The energy $E_1$ of primary electrons is controlled by adjustment of the potential $U$.
-
+The optical properties of metals depend upon both conduction and valance band electrons. At the surface of a material, the electron spectrum (energy levels, band structure and densities of states) may differ greatly from the bulk. This is largely due to the sharp change in potential at the interface; rearrangement of lattice sites, ``dangling'' molecular bonds, and adsorbed defects are also contributing factors
+Total Current Spectroscopy is an electronic spectroscopy technique which is extremely sensitive to the electronic properties of the surface region. The experimental setup for Total Current Spectroscopy can be easily integrated into existing apparatus for sample preparation, which allows for measurements to be made in situ.
\begin{center}
\includegraphics[scale=0.60]{figures/tcs/tcs_simple}
- \captionof{figure}{ A simplified schematic of Total Current Spectroscopy Experiments }
+ \captionof{figure}{ A simplified schematic of a Total Current Spectroscopy Experiment}
\label{tcs_simple.pdf}
\end{center}
-Figure \ref{tcs_simple.pdf} shows a simplified schematic for a Total Current Spectroscopy experiment
-\footnote{For a more detailed description of the experimental setup, refer to Appendix \ref{}}.
-When a current is passed through the cathode, electrons are thermionically emitted with a distribution in initial velocities. A series of electrodes (an electron gun) creates a potential which focuses the emitted electrons into a beam and accelerates them towards the target. The transmitted current $I$ can be detected external to the vacuum chamber using a conventional DC ammeter\footnote{It is also possible to use lock-in amplifier techniques for noise reduction \cite{komolov}. In this study, the DC ammeter has been used due to the relative simplicity of the measurement and control circuit.}.\
+In Total Current Spectroscopy experiments (Figure \ref{tcs_simple.pdf}), a current of primary electrons $I_1$ is directed at a target surface. Upon interacting with the surface, the primary electron beam is split into two components; the transmitted current $I$, and the secondary electron current $I_2$. $I_2$ includes components formed from elastically and inelastically scattered primary electrons, as well as any ``true secondary'' electrons emitted by the surface.
+
+For each mechanism behind the origin of an electron in $I_2$, there is an associated ``threshold'' primary electron energy which must be exceeded before the process can occur. As a result, measurement of changes in $I_2$ as a function of primary electron energy $E_1$ provides a sensitive means to characterise properties of the sample under bombardment. The energy $E_1$ of primary electrons is controlled by adjustment of the potential $U$ applied between the sample and cathode.
+
+
+Primary electrons are thermionically emitted at a cathode with a distribution in energies. A series of electrodes (an electron gun) focuses the emitted electrons into a beam and produces the current $I_1$ at the target. A feedthrough connected to the sample holder allows the transmitted current $I$ to be measured external to the vacuum chamber using an electrometer. Measurement of $I$ instead of $I_2$ is generally preferred, since changes in $I$ can be directly related to changes in $I_2$.
+
The total current spectrum (TCS) is defined as:
\begin{align*}
S(E_1) &= \der{I}{E_1} = -\der{I_2}{E_1}
\end{align*}
-This result assumes that the primary electron current $I_1$ is constant. Such an assumption is valid if the cathode has reached thermal equilibrium, and the potential due to the sample can be considered to have negligable effect on the focusing properties of the electron gun.
-
-The experimental goal of Total Current Spectroscopy is the measurement of $S(E_1) \propto \der{I_2}{E_1}$. More information on the experimental setup and techniques are presented in Appendix \ref{}. The remainder of this section will give an overview of concepts needed for relating $S(E_1)$ to properties of a sample.
-
+This result assumes that the primary electron current $I_1$ is constant. This assumption is generally valid over long time scales once the cathode has reached thermal equilibrium. \footnote{In the final experimental setup, the primary electron current was found to vary by about $2\%$ over the course of several days; far longer than the time taken for total current spectrum measurements (30s to 10min)}
-\subsubsection{Relationship between $S(E_1)$ and electron-surface interactions} \label{tcs_theory1}
-Here we will summarise the approach of Komolov \cite{komolov} in constructing a theory relating $S(E_1)$ to scattering events within the target surface.
+\subsection{General form of $S(E_1)$} \label{tcs_theory1}
-% Contact potential
-A single electron arriving at the sample has energy $E = eU + c$, where $e$ is the electron charge, $U$ is the potential applied between the cathode and sample, and $c$ is a constant which includes the electron's energy relative to the sample when emitted. The minimum value for $c$ is the contact potential of the cathode relative to the sample.
+In the following, a generalised formula for $S(E_1)$ will be presented as derived by Komolov \cite{komolov}.
-At the cathode, electrons are emitted with a distribution in energies about some mean value. A realistic model should take into account this distribution.
-
-If the primary electrons are incident perpendicular to the surface, then we can write $I$ as an integral over the whole distribution of energies:
+The current of primary electrons incident perpendicular to the surface can be written as:
\begin{align*}
- I(E_1) = e A \int_0^{\infty} f(E - E_1) dE
+ I_1(E_1) = e A \int_0^{\infty} f(E - E_1) dE
\end{align*}
-where $f(E - E_1)$ is the distribution for an electron of energy $E$ arriving at the surface. Generally $f(0)$ (ie: $E = E_1$) is the maximum of $f$.
-
-\emph{TODO: Discuss angular distribution of incident electrons, due to focusing of electron gun?}
+where $f(E - E_1)$ gives the distribution for electrons of energy $E$ arriving at the surface. $f(0)$ (ie: $E = E_1$) is the maximum of $f$.
-To formulate a general expression for the secondary current, we introduce a cross section $\sigma(E)$, which gives the probability for a primary electron of energy $E$ to give rise to a secondary electron (of any energy $E_2 <= E$).
-
-Then the total current of secondary electrons is:
+The total secondary current may be written as:
\begin{align*}
I_2(E_1) &= e A \int_{0}^{\infty} f(E - E_1) \sigma(E) dE
\end{align*}
-Using $I = I_1 - I_2$, and $S(E_1) = \der{I}{E_1}$, it is straight forward to arrive at a general expression for the total current spectrum \cite{komolov}:
-\begin{align*}
- S(E_1) &= e A \left\{ [ 1 - \sigma(0) ] f(-E_1) + \int_{0}^{\infty} f(E - E_1) \der{\sigma(E_1)}{E_1} dE \right\}
-\end{align*}
+Where the cross section $\sigma(E)$ is the probability for a primary electron of energy $E$ to give rise to a secondary electron (of any energy $E_2 \leq E$).
+
+Using $I = I_1 - I_2$, it is straight forward to arrive at a general expression for $S(E_1)$:
+\begin{align}
+ S(E_1) &= e A \left\{ [ 1 - \sigma(0) ] f(-E_1) + \int_{0}^{\infty} f(E - E_1) \der{\sigma(E_1)}{E_1} dE \right\} \label{tcs_full}
+\end{align}
-All $E_1$ dependence in the first term is due soley to the distribution of primary electrons. It is clear that this term is maximised when $E_1 = 0$ with respect to the sample; ie: the contact potential between the cathode and sample is zero.
+All $E_1$ dependence in the first term is due soley to the primary electron energy distribution. This term is responsible for the first peak in an $S(E_1)$ curve.
-The second term contains dependence upon $\der{\sigma(E_1)}{E_1}$. As $E_1$ is increased past the threshold for a particular interaction, $\sigma(E_1)$ will undergo a sharp change. This corresponds to a narrow maxima or minima in the derivative $\der{\sigma(E_1)}{E_1}$. A corresponding maxima or minima will appear in $S(E_1)$, centred about the threshold for the interaction. The convolution with the primary electron distribution $f(E - E_1)$ has the effect of broadening and lowering these peaks; in other words, the resolution of Total Current Spectroscopy is limited by the distribution of primary electrons.
+The second term contains dependence upon $\der{\sigma(E_1)}{E_1}$. As $E_1$ is increased past the threshold for a particular interaction, $\sigma(E_1)$ will undergo a sharp change. This corresponds to a narrow maxima or minima in the derivative $\der{\sigma(E_1)}{E_1}$. A corresponding maxima or minima will appear in $S(E_1)$, centred about the threshold for the interaction. The convolution with the primary electron distribution $f(E - E_1)$ has the effect of broadening and lowering these peaks; in other words, the resolution of total current spectroscopy is limited by the distribution of primary electron energies.
The (unphysical) case of a mono-energetic beam is equivelant to setting $f(E - E_1) = \delta(E - E_1)$. In this case, the integrals in the expressions for $I$ and $I_2$ collapse, and the resulting total current spectrum is:
+\begin{align}
+ S(E_1) &= \der{I}{E_1} = e A \frac{d}{dE_1} \left( 1 - \sigma(E_1) \right) = e A \der{\sigma(E_1)}{E_1} \label{tcs_simple}
+\end{align}
+
+A form of \eqref{tcs_simple} is usually assumed when constructing a more detailed theory of secondary electron current formation, as the location of peaks due to $\der{\sigma(E_1)}{E_1}$ is the same in both \eqref{tcs_simple} and \eqref{tcs_full}. Figure \ref{komolov1979} illustrates an idealised total current spectrum.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/tcs/komolov1979_tcs.png}
+ \caption{An idealised total current spectrum (Komolov et al 1979 \cite{komolov1979})}
+ \label{komolov1979}
+\end{figure}
+
+\subsection{Contact Potential and the Surface Peak}
+
+The case $E_1 = 0$ does not in general correspond to $U = 0$. Figure \ref{contact.pdf} describes a simplified step potential model for the surfaces of the cathode and sample. In a classical approximation, primary electrons will be elastically scattered from the sample unless they have energy greater than its vacuum level.
+
+At the cathode, electrons are thermionically excited from the conduction band to the vacuum level. The vacuum levels of the cathode and surface are not generally equal. The contact potential is the difference in work functions of the materials. As $U$ approaches the contact potential, primary electrons are able to penetrate into the sample, and a sharp peak termed the surface peak is seen in $S(U)$. The maxima of this peak occurs at an applied potential $U$ such that $E_1 = 0$; its shape is indicative of $f(E - E_1)$.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.80\textwidth]{figures/tcs/contact.pdf}
+ \caption{Illustration of the step potential model for the surfaces}
+ \label{contact.pdf}
+\end{figure}
+
+
+
+
+\subsection{Electron-Electron Interactions}
+\label{tcs_e}
+
+
+In the Sommerfield free electron gas approximation, electrons are assumed to be contained within a rectangular potential well, with energies given by $E_k = \frac{\hbar^2 k^2}{2m}$, where $\vect{k}$ is the electron wave vector. Electrons fill states up to the Fermi level, with density of states $N(E_k)$ proportional to $\sqrt{E_k}$.
+
+An incoming primary electron interacting with the free electron gas may either excite a single electron to above the Fermi level, or a collective vibration (plasmon). A plasmon may be excited if $E_1 \geq \hbar \omega_p$.
+
+The response of a free electron gas to an external electric field is characterised by $\phasor{\epsilon}$. The imaginary part of $\phasor{\epsilon}$ describes the attenuation of the electric field; it describes the process of energy transfer from the primary electron to the electron gas. Since the intensity of the electric field entering the solid decreases by a factor of $|\phasor{\epsilon}^2|$, the efficiency of energy transfer is given by:
+
\begin{align*}
- S(E_1) &= \der{I}{E_1} = e A \frac{d}{dE_1} \left( 1 - \sigma(E_1) \right) = e A \der{\sigma(E_1)}{E_1}
+ \frac{\epsilon_2}{|\phasor{\epsilon}|^2} = -\text{Im}\left(\frac{1}{\phasor{\epsilon}}\right)
\end{align*}
-{\bf NOTE: Komolov goes on to find expressions for $\sigma(E_1)$ in terms of specific inelastic processes...}
+This function is often referred to as the ``Bulk loss''. A maxima in the bulk loss is indicative of a high probability for primary electrons to inelastically scatter from the free electron gas.
+
+
+
+
+\subsection{Implementation of Total Current Spectroscopy Experiment}
+
+As part of this project, we designed and built most of the electronics for an automated Total Current Spectroscopy setup. Figure \ref{tcs_block} shows a block diagram illustrating the key components of the setup. Figure \ref{electron_gun_circuit} shows the circuit diagram for control of the electron gun. Due to the limited range of available power supplies, our experiment has focused on the surface peak of the samples.
+
+In order to automate TCS experiments, both Digital to Analogue and Analogue to Digital Convertors were required (DAC and ADC). To provide these, a custom DAC/ADC Box was designed and constructed. The box can be controlled by any conventional computer with available RS-232 serial communication (COM) ports. The full design of both hardware and software is available on request.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/presentation/tcs_block.png}
+ \caption{Block diagram for TCS setup}
+ \label{tcs_block}
+\end{figure}
+
+\begin{landscape}
+\begin{figure}[H]
+ \includegraphics[width=1.25\textwidth]{figures/egun/electron_gun.pdf}
+ \caption{TCS circuit diagram}
+ \label{electron_gun_circuit}
+\end{figure}
+\end{landscape}
\pagebreak
-\section{Ellipsometry}
+\section{Ellipsometry} \label{Ellipsometry}
-\subsection{Overview}
+Ellipsometry is a versatile optical technique which can be used to gain a great deal of information about optical and structural properties of thin films. In particular, Ellipsometry may be used to determine the pseudo-dielectric constant $\phasor{\epsilon}$ of a sample. This makes ellipsometry a useful complementary technique to secondary electron spectroscopy experiments, where $\phasor{\epsilon}$ is important for descriptions of electron-electron interactions.
-Ellipsometry is an optical technique which measures the change in polarisation of light reflected from a surface. This change in polarisation can be related to the optical properties of the surface, including optical constants or the thickness of thin film surface layers.
+An ellipsometer is designed to establish a beam of light with known polarisation, and measure the change in polarisation due to reflection of the light from a surface. This change in polarisation can be related to the optical properties of the surface, or the thicknesses of a multi-layered sample.
-In the Jone's formalism, polarisation states may be represented by orthogonal electric field components $E_p$ and $E_s$, which are polarised parallel and perpendicular to the plane of incidence respectively. The reflection of a light ray from the surface is described by the matrix equation:
+In the Jone's formalism, polarisation states may be represented by orthogonal electric field components $E_p$ and $E_s$, which are polarised parallel and perpendicular to the plane of incidence respectively. The reflection of a polarised light ray from the surface is described by the matrix equation:
\begin{align*}
\left[\begin{array}{c} E_{rp} \\ E_{rs} \end{array}\right] &= \left[ \begin{array}{cc} r_{pp} & r_{ps} \\ r_{sp} & r_{ss} \end{array} \right] \left[\begin{array}{c} E_{ip} \\ E_{is} \end{array}\right]
\end{align*}
\begin{figure}[H]
\centering
\includegraphics[width=0.80\textwidth]{figures/ellipsometer/ellipsometer_measurement.png}
- \caption{Diagram of an Ellipsometric Measurement \cite{woolam1999}}
+ \caption{Illustration of an ellipsometric measurement \cite{oates2011}}
\label{ellipsometer_measurement}
\end{figure}
The value of $\tan(\psi)$ gives the ratio of amplitudes between the $p$ and $s$ components of the reflected electric field, whilst $\Delta$ gives the phase difference.
-In the case where the sample is anisotropic, $\psi$ and $\Delta$ alone are not sufficient to characterise the sample; three seperate ratios of fresnel reflection coefficients are required \cite{woolam2000}:
-
-
-Light may consist of two or more components of well defined polarisation states; as a result, the total beam cannot be described with a single well defined Jones vector. Ellipsometers are designed to establish a well defined polarisation state of light incident on the sample; however non-uniform films or backside reflection from a substrate may cause the reflected beam to be partially polarised. As a result, the Jone's formalism is not sufficient for characterisation of these samples, and the more general Stokes formalise (with 4 component vectors) must be employed \cite{woolam2000} \cite{oates2011}.
+For an anisotropic sample, $\psi$ and $\Delta$ alone are not sufficient to characterise the sample; three seperate ratios of fresnel reflection coefficients are required. Non-uniform films or backside reflection from a substrate may cause the reflected beam to be partially polarised. As a result, the Jone's formalism is not sufficient for characterisation of these samples, and the more general Stokes formalism (which uses 4 component vectors to describe polarisation states) must be employed \cite{woolam2000} \cite{oates2011}.
\begin{table}[H]
\centering
\includegraphics[scale=0.75]{figures/ellipsometer/linear_polarisation} \\
\end{tabular}
- \captionof{figure}{From left to right, circular, elliptical and linearly polaristed light, viewed down the axis of beam propagation}
+ \captionof{figure}{From left to right, circular, elliptical and linearly polarised light, viewed along the wavevector of the light}
\end{table}
+
+\subsection{Relation of measurements to properties of the sample}
+
+\subsubsection{Bulk Optical Constants}
+
+The simplest sample is a flat substrate of infinite thickness. In this case, the optical constants of the substrate can be determined directly from $\rho$:
+\begin{align*}
+ \phasor{\epsilon} &= \epsilon_1 + i \epsilon_2 = \sin^2 (\phi) \left( 1 + \tan^2(\phi) \frac{1 - \rho}{1 +\rho}^2\right)
+\end{align*}
+Where $\phasor{\epsilon}$ is the psueodo-dielectric function. The complex refractive index of the material can be easily related to $\phasor{\epsilon}$:
+\begin{align*}
+ \phasor{\epsilon} &= \phasor{n}^2 = (n + i \kappa)^2
+\end{align*}
+Where $n$ is the refractive index, and $\kappa$ is the extinction coefficient.
+
+
+
+\subsubsection{Multi-layered Samples}
+
+At each layer in a multi-layered film, light is be both reflected and transmitted. The measured signal is the result of interference between reflections from each layer. The phase difference for each component of the beam is determined by both the optical constants and the thicknesses of the layers through which the component has passed.
+
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.5\textwidth]{figures/ellipsometer/multilayered.pdf}
+ \caption{Interaction of light with a multi-layered sample}
+\end{figure}
+
+
+\subsubsection*{A Note on Si Substrates}
+
+A real substrate stored in laboratory air will generally have thin surface layers of oxides. For example, most of the thin film samples produced for this study were prepared on Si substrates. The inclusion of a layer of $\text{SiO}_2$ between the Si substrate and the thin film was found to have a significant effect on the accuracy with which the properties of the sample could be fit.
+
+
+\pagebreak
+
\subsection{Variable Angle Spectroscopic Ellipsometry}
-Although Ellipsometers have been in use for thin film analysis since the ??? \cite{}, traditional instruments were usually limited to single angle and single wavelength measurements, due to the painstaking manual process of repeated measurements. With advances both in software and hardware during the last half of the 20th century, Ellipsometric measurements have become largely automated, allowing for a wide range of optical information to be obtained from a sample. Spectroscopic Ellipsometry obtains measurements for a range of wavelengths, whilst Variable Angle Spectroscopic Ellipsometry repeats these measurements over a range of angles of incidence.
+Although Ellipsometers have been in use for thin film analysis since the late 19th century, traditional instruments were usually limited to single angle and single wavelength measurements, due to the painstaking manual process involved in repeated measurements \cite{tompkins1992}. With advances both in software and hardware during the last half of the 20th century, Ellipsometric measurements have become largely automated, allowing for a huge number of measurements to be easily obtained from a sample \cite{woolam1999, woolam2000}.
-The ease with which large amounts of data can be taken from an ellipsometer means that the method is well suited to numerical analysis and fitting procedures. At CAMSP a Variable Angle Spectroscopic Ellipsometer (VASE)\footnote{J. A. Woolam and Co} and the associated software\footnote{WVASE32} have been employed in the analysis of thin film samples.
+Spectroscopic Ellipsometry obtains measurements for a range of wavelengths of the incident light. A Variable Angle Spectropic Ellipsometer (VASE) repeats measurements over a range of different angles of incidence. Because of the wealth of data aquired, these techniques are well suited to numerical analysis and fitting procedures to determine both the optical constants and thickness of unknown samples.
+
+At CAMSP a Variable Angle Spectroscopic Ellipsometer (VASE)\footnote{J. A. Woolam and Co} and the associated software (WVASE32) have been employed in the analysis of thin film samples. Figure \ref{ellipsometer.png} shows a block diagram of the VASE.
+
+The WVASE32 software allows for the construction of a model of a given sample, using tabulated literature values for optical constants, and allowing the user to specify film thicknesses. This model can then be adjusted using mean square error minimisation fitting algorithms to determine the thicknesses and/or optical constants for the model which best match the measured data. The modelling procedure is illustrated in Figure \ref{procedure.png}.
\begin{figure}[H]
\centering
- \includegraphics[width=0.8\textwidth]{figures/ellipsometer/ellipsometer.png}
- \caption{Block diagram of the VASE \\(taken from \emph{Overview of Variable Angle Spectroscopic
-Ellipsometry (VASE), Part I:
-Basic Theory and Typical Applications}
-\cite{woolam1999})}
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ellipsometer.png}
+ \caption{Block diagram of the VASE \cite{woolam1999}}
\label{ellipsometer.png}
\end{figure}
-\subsection{Relation of $\psi$ and $\Delta$ to properties of the sample}
+\begin{figure}[H]
+ \centering
+ \includegraphics[width=0.9\textwidth]{figures/ellipsometer/ellipsometry_block.png}
+ \caption{Illustration of the VASE analysis and modelling procedure \cite{woolam1999}}
+ \label{procedure.png}
+\end{figure}
-\subsubsection{Bulk Substrates}
-The simplest sample is a bulk substrate. In this case,
+\section{Vacuum Techniques and Sample Preparation}
-\subsubsection{Single Layered Thin Films}
+All samples required for this study were prepared using available equipment at CAMSP. A small (approx. 25L) vacuum chamber, which has been used previously for thin film preparation at CAMSP \cite{kostylev2011} was repurposed to allow for both deposition of metallic thin films, and subsequent study using total current spectroscopy. A diagram of this setup is shown in Figure \ref{chamber}.
+A rotatable stainless steel sample holder was positioned in the centre of the vacuum chamber. A flange containing evaporators was placed on one side of the chamber, whilst the electron gun required for total current spectroscopy was placed directly opposite. Shielding was used to ensure the electron gun was not coated during deposition. Two sample holders were attached to either side of the shielding to allow for preparation and study of two samples without the need for venting the vacuum chamber.
+The evaporators consisted of a tungsten wire filament (diameter 0.5mm) attached using spot welds between two feedthroughs. A piece of the desired metal was folded over the apex of the tungsten wire. The metal was then heated by passing a current through the filament; at sufficiently high currents, the metal piece began to evaporate, with a proportion of the flux of evaporated particles striking the target sample. To remove any contaminating layers from the metal, and ensure uniform evaporation, this procedure was first performed at low pressure (below $10^{-6}$ mbar) with no sample in the chamber, with the current increased until the metal piece began to melt and form a ball on the wire.
-\subsubsection{Multi-layered Thin Films}
+This study focused primarily on depositing Au and Ag films on Si substrates (approx 10x10x3mm wafers), at both high and low pressures. To remove any organic layers, the substrates and sample holders were cleaned in an acetone bath immediately prior to insertion in the vacuum chamber. The thickness of the deposited layer was controlled by varying both deposition time and the heating current.
-Magical analysis
-\section{Optical Transmission and Reflection Spectroscopy}
+ \begin{figure}[H]
+ \centering
+ \includegraphics[width=0.8\textwidth]{figures/pressure/chamber.pdf}
+ \caption{Layout of components within the vacuum chamber}
+ \label{chamber}
+ \end{figure}
-Can be done with the VASE or with OceanOptics spectrometer.
-\section{Scanning Electron Microscopy}
\relax
-\@writefile{toc}{\contentsline {chapter}{\numberline {2}Overview of Theory}{3}{chapter.2}}
+\@writefile{toc}{\contentsline {chapter}{\numberline {2}Overview}{2}{chapter.2}}
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-\chapter{Overview of Theory}
+\chapter{Overview}
-I will use this section to introduce general concepts of solid state physics. The Experimental Methods section will concentrate on the theory of each method, and how this relates to the overall theory.
-\begin{itemize}
- \item {\bf What a nanostructured film is, how it differs from the bulk material}
- \begin{itemize}
- \item The surface of a solid is the interface for physical/chemical interactions with it's surrounding environment
- \item The physical and chemical properties of a material are largely determined by the electron spectra at the surface
- \begin{itemize}
- \item Electron spectra is determined by the lattice potential
- \item Characterised by
- \begin{enumerate}
- \item Band structure of energy states - due to periodic lattice potential
- \item Density of States
- \end{enumerate}
- \item Surface differs from bulk due to
- \begin{enumerate}
- \item Termination of periodic lattice
- \item Adsorbed particles on surface (thin films)
- \item Relocation of lattice sites near the surface
- \end{enumerate}
- \item Band structure for Metal's vs Semi-conductors
- \begin{enumerate}
- \item Metals:
- \item Semiconductors:
- \end{enumerate}
- \end{itemize}
-
-
- \end{itemize}
- \item {\bf Surface Plasmons}
- \begin{itemize}
- \item A collective oscillation of the electron gas in a metal
- \item Surface plasmons are confined to the surface region; 2 dimensional, differs from bulk plasmons
- \begin{itemize}
- \item In nanostructured materials, plasmons can be localised
- \end{itemize}
- \item Bohms and Ritchie
- \item Past studies at CAMSP and UWA
- \item May be caused due to excitations from
- \begin{enumerate}
- \item Electrons - refer to next section
- \item Photons
- \begin{itemize}
- \item Only light polarised in the plane of the surface can excite plasmons
- \item Need to provide an extra wavevector to ``match'' the momenta of the photon and plasmon
- \item Possibility for rough structure of metallic films to provide this wavevector
- \begin{itemize}
- \item Refer to papers on ``artificially'' blackened films
- \item Similar topic to Nikita's thesis; look at some of his references
- \end{itemize}
- \end{itemize}
- \end{enumerate}
- \end{itemize}
- \item {\bf Interactions between Electrons and Metallic Thin Films}
- \begin{enumerate}
- \item Electron-Surface Interaction
- \begin{itemize}
- \item How an incoming electron interacts with the surface as a whole
- \item Elastic reflection from potential barrier
- \item Phonon vibrations of lattice (quasi-elastic - low energy losses)
- \end{itemize}
- \item Electron-Electron Interaction
- \begin{itemize}
- \item Inelastic scattering processes determined by interaction of primary electron with the electron gas
- \item Low energy interactions (focus of low energy TCS)
- \begin{itemize}
- \item Outer electron transitions between valence and conduction band (result of interaction between primary electron and an individual bound electron)
- \item Plasmon excitation (result of interaction between incoming electron and the electron gas as a whole)
- \end{itemize}
- \item Higher energy interactions (focus of other forms of 2nd Electron Spectroscopy)
- \begin{itemize}
- \item Auger processes due to excitation of inner band electrons
- \item ``True'' secondary electrons; bound electrons given sufficient energy to leave the surface
- \end{itemize}
- \end{itemize}
- \item General structure of secondary electron energy distribution (not investigated by TCS)
- \item Mention that secondary electrons have an angular distribution (not investigated by TCS)
-
- \end{enumerate}
-\end{itemize}
\chapter{Overview of Theory}
+I will use this section to introduce general concepts of solid state physics. The Experimental Methods section will concentrate on the theory of each method, and how this relates to the overall theory.
+\begin{itemize}
+ \item {\bf What a nanostructured film is, how it differs from the bulk material}
+ \begin{itemize}
+ \item The surface of a solid is the interface for physical/chemical interactions with it's surrounding environment
+ \item The physical and chemical properties of a material are largely determined by the electron spectra at the surface
+ \begin{itemize}
+ \item Electron spectra is determined by the lattice potential
+ \item Characterised by
+ \begin{enumerate}
+ \item Band structure of energy states - due to periodic lattice potential
+ \item Density of States
+ \end{enumerate}
+ \item Surface differs from bulk due to
+ \begin{enumerate}
+ \item Termination of periodic lattice
+ \item Adsorbed particles on surface (thin films)
+ \item Relocation of lattice sites near the surface
+ \end{enumerate}
+ \item Band structure for Metal's vs Semi-conductors
+ \begin{enumerate}
+ \item Metals:
+ \item Semiconductors:
+ \end{enumerate}
+ \end{itemize}
+
+
+ \end{itemize}
+ \item {\bf Surface Plasmons}
+ \begin{itemize}
+ \item A collective oscillation of the electron gas in a metal
+ \item Surface plasmons are confined to the surface region; 2 dimensional, differs from bulk plasmons
+ \begin{itemize}
+ \item In nanostructured materials, plasmons can be localised
+ \end{itemize}
+ \item Bohms and Ritchie
+ \item Past studies at CAMSP and UWA
+ \item May be caused due to excitations from
+ \begin{enumerate}
+ \item Electrons - refer to next section
+ \item Photons
+ \begin{itemize}
+ \item Only light polarised in the plane of the surface can excite plasmons
+ \item Need to provide an extra wavevector to ``match'' the momenta of the photon and plasmon
+ \item Possibility for rough structure of metallic films to provide this wavevector
+ \begin{itemize}
+ \item Refer to papers on ``artificially'' blackened films
+ \item Similar topic to Nikita's thesis; look at some of his references
+ \end{itemize}
+ \end{itemize}
+ \end{enumerate}
+ \end{itemize}
+ \item {\bf Interactions between Electrons and Metallic Thin Films}
+ \begin{enumerate}
+ \item Electron-Surface Interaction
+ \begin{itemize}
+ \item How an incoming electron interacts with the surface as a whole
+ \item Elastic reflection from potential barrier
+ \item Phonon vibrations of lattice (quasi-elastic - low energy losses)
+ \end{itemize}
+ \item Electron-Electron Interaction
+ \begin{itemize}
+ \item Inelastic scattering processes determined by interaction of primary electron with the electron gas
+ \item Low energy interactions (focus of low energy TCS)
+ \begin{itemize}
+ \item Outer electron transitions between valence and conduction band (result of interaction between primary electron and an individual bound electron)
+ \item Plasmon excitation (result of interaction between incoming electron and the electron gas as a whole)
+ \end{itemize}
+ \item Higher energy interactions (focus of other forms of 2nd Electron Spectroscopy)
+ \begin{itemize}
+ \item Auger processes due to excitation of inner band electrons
+ \item ``True'' secondary electrons; bound electrons given sufficient energy to leave the surface
+ \end{itemize}
+ \end{itemize}
+ \item General structure of secondary electron energy distribution (not investigated by TCS)
+ \item Mention that secondary electrons have an angular distribution (not investigated by TCS)
+
+ \end{enumerate}
+\end{itemize}
--- /dev/null
+\chapter{Overview} \label{chapter_overview}
+
+\section{Black-Metal Films}
+
+So called black-metal films are the result of deposition of metal elements at a relatively high pressure\footnote{of the order of $10^{-2}$ mbar} or ``bad vacuum''. The films are named due to their high absorbance at visible wavelengths; a sufficiently thick film will appear black to the naked eye. There is a remarkable contrast between such films and metal films deposited under low pressure\footnote{less than $10^{-5}$mbar}, which are typically highly reflective and brightly coloured at comparable thicknesses. It has been established that black-metal films may be prepared in any gas, but when Oxygen is present the resulting films contain tungsten oxides \cite{harris1952} \cite{mckenzie2006}.
+
+% First mentions and early research; Pfund
+The formation of black-metal films at high pressure has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of black-metals \cite{pfund1930}, and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared \cite{pfund1933}. Pfund's research has focused on the possible applications of black-metal films as absorbing coatings for radiometric devices.
+
+Subsequent researchers have also focused on determining absorbsion properties of black-metal films as a function of preparation conditions \cite{harris1948} \cite{harris1952}, with the aim of producing selective filters for infra-red detectors.
+
+There have been several attempts to relate the structure of black-metal films to measured optical properties (usually the total reflectivity of the film). Harris et al. have produced experimental results of the transmission of black-metal films from visible wavelengths to the far-infrared. By modelling the films as a layer of metallic strands, acting as ``condensors'', Harris et al. arrived at an expression for the electron relaxation time of [element]-black \cite{}, leading to a a transmission spectrum in good agreement with experimental results.
+
+Mckenzie has established that the presence of oxygen effects the optical and electrical properties of black-metals \cite{mckenzie2006}. Although Mckenzie has been able to use Mie theory for
+
+
+% More recent research
+More recently, it was shown that black-Au coatings increased the efficiency of thin film solar cells \cite{}. In this study, a simulation approximating an black-Au film as a layer of semi-spherical structures showed plasmonic behaviour which lead to an increase in electric field behind the film.
+
+
+% Artificially ``blackened'' thin films
+The optical properties of black-metal films have been found to vary when the film is exposed to atmosphere, or heated \cite{donna1993}. This ``degradation'' of the black-metal films is inconvenient for maintaining consistent calibration of devices. Recently there has been interest in artificial ``blackening'' of metal surfaces for optical applications. These ``meta-materials'' offer a promising alternative to the traditional black-metal films, due to the ability to more precisely control properties of the film \cite{sondergaard2012}.
+
+
+In light of the wealth of previous research, the aims of this project were first to reproduce black-metal films using equipment available at CAMSP, and then employ several techniques for the study of these samples in comparison with other metal films. Most of the existing research has been conducted using optical transmission or reflection spectroscopy techniques. A total current secondary electron spectroscopy experiment was therefore integrated into the sample preparation vacuum chamber, to allow for almost immediate study of prepared samples using this technique. A Variable Angle Spectroscopic Ellipsometer (VASE) has been used in an attempt to relate the optical and structural properties of the samples. We have also used optical transmission spectroscopy in the visible region to characterise the transmission of black-metal films.
+
+\section{Plasmonic Effects}
+
+
--- /dev/null
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+ /FamilyName (Nimbus Sans L) readonly def
+ /Weight (Regular) readonly def
+ /ItalicAngle 0 def
+ /isFixedPitch false def
+ /UnderlinePosition -151 def
+ /UnderlineThickness 50 def
+end readonly def
+/Encoding 256 array
+0 1 255 {1 index exch /.notdef put} for
+dup 1 /hyphen put
+dup 3 /period put
+dup 2 /zero put
+dup 5 /one put
+dup 6 /two put
+dup 7 /four put
+dup 4 /five put
+dup 8 /six put
+dup 9 /eight put
+readonly def
+currentdict end
+currentfile eexec
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def Derivative(data, a=1, b=2, sigma=None,step=1):
+ #print "Derivative called"
result = [[]]
n = 0
dI = [0,0]
if calibrate:
data = CalibrateData(data)
- units = ["V", "uA / V"]
+ units = ["Volts", "uA / V"]
else:
units = ["DAC counts", "ADC counts / DAC counts"]
if not normalise:
- gnuplot("set ylabel \"dI(E)/dE ("+str(units[1])+")\"")
+ gnuplot("set ylabel \"S(U) ("+str(units[1])+")\"")
else:
data = MaxNormalise(data)
- gnuplot("set ylabel \"dI(E)/dE (normalised)\"")
+ gnuplot("set ylabel \"S(U) (arb. units)\"")
if (output != None and type(output) == type("")):
gnuplot("set term png size 640,480")
gnuplot("set output \""+str(output)+"\"")
if master_title == "":
- master_title = "Total Current Spectrum S(E)"
+ master_title = "Total Current Spectrum S(U)"
if type(filename) == type("") and plot == gnuplot.plot:
if filename != "tcs data":
p = ReadParameters(filename)
gnuplot("set title \""+str(master_title)+"\"")
gnuplot("set xlabel \"U ("+str(units[0])+")\"")
-
+ gnuplot("set xrange [0:16]")
+ gnuplot("set mxtics 10")
+ gnuplot("set mytics 10")
if raw:
d = Derivative(data, 1, 2, step=step)
units = ["DAC counts", "ADC counts"]
if not normalise:
- gnuplot("set ylabel \"I(E) ("+str(units[1])+")\"")
+ gnuplot("set ylabel \"I(U) ("+str(units[1])+")\"")
else:
data = MaxNormalise(data)
- gnuplot("set ylabel \"I(E) (normalised)\"")
+ gnuplot("set ylabel \"I(U) (arb. units)\"")
if (output != None and type(output) == type("")):
gnuplot("set term png size 640,480")
gnuplot("set xlabel \"U ("+str(units[0])+")\"")
- ymax = 0.005 + 1.2 * max(d, key=lambda e : e[2])[2]
- ymin = -0.005 + 1.2 * min(d, key=lambda e : e[2])[2]
+ ymax = 0.005 + 1.2 * max(data, key=lambda e : e[2])[2]
+ ymin = -0.005 + 1.2 * min(data, key=lambda e : e[2])[2]
gnuplot("set yrange ["+str(ymin)+":"+str(ymax)+"]")
#d = Derivative(data, 1, 2, step=step)
i = 1
plotFunc = ShowTCS
- normalise = False
+ normalise = True
title = ""
master_title = ""
smooth=0
print "Done. Press enter to exit, or type name of file to save as."
out = sys.stdin.readline().strip("\t\r\n #")
if out != "":
- gnuplot("set term postscript colour")
+ gnuplot("set term postscript colour enhanced \"Arial Bold,18\"")
gnuplot("set output \""+out+"\"")
gnuplot.replot()
--- /dev/null
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+ sodipodi:role="line"
+ id="tspan5462"
+ x="1449.6821"
+ y="731.14404">Spectrum of Xe Arc Lamp (Ellipsometer Light Source)</tspan></text>
+<text
+ xml:space="preserve"
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+<text
+ xml:space="preserve"
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+</g></g></svg>
\ No newline at end of file
--- /dev/null
+"Describes the use of spectroscopic ellipsometry to define plasmonic characteristics of a system."
+@article{oates2011,
+ author = "T.W.H Oats, H. Wormeester, H. Arwin",
+ title = "Characterization of plasmonic effects in thin films and metamaterials using spectroscopic ellipsometry",
+ year = 2011,
+ journal = "Progress in Surface Science (Elsevier Ltd)",
+}
+
+"The Bakerian Lecture"
+@article{faraday1857,
+ author = "M. Faraday",
+ title = "Experimental Relations of Gold (and Other Metals) to Light",
+ year = 1857,
+ journal = "M Philosophical Transactions of the Royal Society of London (1776-1886)"
+}
+
+"Source for the quote ``... the shape of a dragon from its footprints''"
+@book{bohren1983,
+ author = "C.F. Bohren, D.R. Huffman",
+ title = "Absorption and Scattering of Light by Small Particles",
+ publisher = "John Wiley and Sons, Weinheim",
+ year = 1983
+}
+
+"J.A Woolam's overview of VASE, 1999"
+"J.A Woollam Co., Inc., 645 'M' St. #102, Lincoln, NE 68508"
+"John A. Woolam, Blaine Johs, Craig M. Herzinger, James Hilfiker, Ron Synowicki and Corey L Bungay"
+@article{woolam1999,
+ author = "John A. Woolam and Co.",
+ title = "Overview of Variable Angle Spectroscopic Ellipsometry (VASE), Part I: Basic Theory and Typical Applications",
+ journal = "Optical Metrology",
+ year = 2000
+}
+
+"Harris 1948"
+"Appears to be Harris' first paper on the subject"
+@article{harris1948,
+ author = "Louis Harris, Rosemary T. McGinnies, Benjamin M. Siegel",
+ title = "The Preparation and Optical Properties of Gold Blacks",
+ journal = "Journal of the Optical Society of America",
+ year = 1948
+}
+
+"Harris 1952"
+@article{harris1952,
+ author = "Louis Harris and John K. Beasley",
+ title = "The Infrared Properties of Gold Smoke Deposits",
+ journal = "Journal of the Optical Society of America",
+ year = 1952
+}
+
+"Harris 1953"
+"Electrical conductivity of Gold-black films from reflection and transmission measurements"
+@article{harris1953,
+ author = "Louis Harris and Arthur L. Loeb",
+ title = "Conductance and Relaxation Time of Electrons in Gold Blacks from Transmission and Reflection Measurements in the Far Infrared",
+ journal = "Journal of the Optical Society of America",
+ volume = 43,
+ number = 11,
+ year = 1953
+}
+
+"Nikita's Thesis" - "CAMSP, UWA"
+@article{kostylev2011,
+ author = "Nikita Kostylev",
+ title = "Plasmonic Excitations in Nanostructures (Thesis)",
+ journal = "School of Physics, Western Australia",
+ year = 2011
+}
+
+"Pfund's first paper"
+"America Institute of Physics"
+@article{pfund1930,
+ author = "A. H Pfund",
+ title = "Bismuth Black and its Applications",
+ journal = "Review of Scientific Instruments",
+ year = 1930
+}
+
+"Pfund's second paper"
+@article{pfund1933,
+ author = "A. H Pfund",
+ title = "The Optical Properties of Metallic and Crystalline Powders",
+ journal = "Journal of the Optical Society of America",
+ year = 1933
+}
+
+"Ivan Maksymov - Simulation of Logic Gate"
+@article{maksymov2010,
+ author = "Ivan S. Maksymov",
+ title = "Optical switching and logic gates with hybrid plasmonic–photonic crystal,
+nanobeam cavities",
+ journal = "Physics Letters A",
+ year = 2010
+}
+
+"Ivan Maksymov - Nano scale Yagi-Uda antennas"
+@article{maksymov2011,
+ author = "Ivan S. Maksymov, Arthur R. Davoyan and Yuri S. Kivshar",
+ title = "Enhanced emission and light control with tapered plasmonic nanoantennas",
+ journal = "Applied Physics Letters",
+ year = 2011
+}
+
+"Heenan Thesis - MOKE"
+@article{heenan1998,
+ author = "E. Heenan",
+ title = "Spectroscopic ellipsometric characterisation of optical properties of thin films (Thesis)",
+ journal = "School of Physics, UWA",
+ year = 1998
+}
+
+"Panjwani Thesis - Solar cells"
+@article{panjwani2011,
+ author = "Deep R. Panjwani",
+ title = "Metal Blacks as scattering centers to increase the efficiency of thin film solar cells (Thesis)",
+ journal = "Department of Physics, University of Central Florida",
+ year = 2011
+}
+
+"Gordon Moore's paper"
+@article{moore1965,
+ author = "Gordon Moore",
+ title = "Cramming more components onto integrated circuits",
+ journal = "Research and Development Laboratories, Fairchild Semiconductor
+division of Fairchild Camera and Instrument Corp.",
+ year = 1965
+}
+
+@book{tompkins1992,
+ author = "Harland G. Tompkins",
+ title = "A User's Guide to Ellipsometry",
+ publisher = "Dover Publications",
+ year = 1992
+}
+
+@article{moller1999,
+author={Møller, P.J., Komolov, S.A., Lazneva, E.F.},
+title={A total current spectroscopy study of metal oxide surfaces: I. Unoccupied electronic states of ZnO and MgO},
+journal={Journal of Physics Condensed Matter},
+year={1999},
+volume={11},
+number={48},
+pages={9581-9588}
+}
+
+@article{komolov1979,
+author={S.A. Komolov, L.T. Chadderton},
+title={Total current spectroscopy},
+journal={Surface Science},
+year={1979},
+volume={90},
+number={2},
+pages={359-380}
+}
+
+@article{moller1985,
+author={P.J. Møller, M.H. Mohamed},
+title={Total current spectroscopy},
+journal={Vacuum},
+year={1985},
+volume={35},
+number={1},
+pages={29-37}
+}
+
+publisher = {American Physical Society},
+doi = {10.1103/PhysRev.82.625},
+issue = {5}
+@article{bohm1951,
+ author = {David Bohm and David Pines},
+ month = {Jun},
+ url = {http://link.aps.org/doi/10.1103/PhysRev.82.625},
+ year = {1951},
+ pages = {625--634},
+ title = {A Collective Description of Electron Interactions. I. Magnetic Interactions},
+ volume = {82},
+ journal = {Phys. Rev.},
+}
+
+doi = {10.1103/PhysRev.85.338},
+issue = {2}
+publisher = {American Physical Society},
+@article{bohm1952,
+ author = {David Pines and David Bohm},
+ month = {Jan},
+ url = {http://link.aps.org/doi/10.1103/PhysRev.85.338},
+ year = {1952},
+ pages = {338--353},
+ title = {A Collective Description of Electron Interactions: II. Collective $\mathrm{vs}$ Individual Particle Aspects of the Interactions},
+ volume = {85},
+ journal = {Phys. Rev.},
+
+}
+
+
+
--- /dev/null
+\relax
+\@setckpt{proposal/proposal.tex}{
+\setcounter{page}{40}
+\setcounter{equation}{0}
+\setcounter{enumi}{5}
+\setcounter{enumii}{0}
+\setcounter{enumiii}{0}
+\setcounter{enumiv}{34}
+\setcounter{footnote}{0}
+\setcounter{mpfootnote}{0}
+\setcounter{part}{0}
+\setcounter{chapter}{0}
+\setcounter{section}{0}
+\setcounter{subsection}{2}
+\setcounter{subsubsection}{0}
+\setcounter{paragraph}{0}
+\setcounter{subparagraph}{0}
+\setcounter{figure}{0}
+\setcounter{table}{0}
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+\setcounter{Hfootnote}{10}
+\setcounter{float@type}{4}
+\setcounter{theorem}{0}
+\setcounter{example}{0}
+\setcounter{section@level}{2}
+}
author = "T.W.H Oats, H. Wormeester, H. Arwin",
title = "Characterization of plasmonic effects in thin films and metamaterials using spectroscopic ellipsometry",
year = 2011,
- journal = "Progress in Surface Science (Elsevier Ltd)",
+ journal = "Progress in Surface Science (Elsevier Ltd)"
}
-asdfasdf
-"The Bakerian Lecture"sdf
+
+"The Bakerian Lecture"
@article{faraday1857,
author = "M. Faraday",
title = "Experimental Relations of Gold (and Other Metals) to Light",
}
+@article{bohm1953,
+ author = "David Pines and David Bohm",
+ title = "A collective description of electron interactions: III. coulomb interactions in a degenerate electron gas",
+ journal = "Physical Review",
+ volume = "92",
+ year = 1953
+}
@book{komolov,
author = "S.A. Komolov",
year = "1992",
publisher = "Gordon and Breach Science Publishers S.A",
}
+"Fourier microscopy of single plasmonic scatterers"
+@article{sersic2011,
+ author = "Ivana Sersic, Christelle Tuambilangana and A Femius Koenderink",
+ year = "2011",
+ journal = "New Journal of Physics",
+ volume = "13"
+}
+
+@article{garnet1904,
+ author = "Maxwell Garnet",
+ year = "1904",
+ journal = "Philosophical Transactions of the Royal Society A",
+ volume = "203",
+ pages = "385-420",
+}
+
+
+@article{ritchie1957,
+ author = "R. H. Ritchie",
+ year = "1957",
+ title = "Plasma Losses by Fast Electrons in Thin Films",
+ journal = "Physical Review",
+ volume = "106"
+}
+
+@article{mei1908,
+ author = "Gustav Mie",
+ year = "1908",
+ title = "Beirtrage zur optik truber medien, speziell kolloidaler metallosungen",
+ journal = "Ann. Phys. (Leipzig)",
+ volume = "25"
+}
+
+"How do you cite a conference?"
+@article{wriedt2008,
+ author = "Thomas Wriedt",
+ year = "2008",
+ title = "Mie Theory 1908-2008 - Introduction to the conference",
+ journal = "(Conference) Mie Theory 1908-2008 - Present developments and Interdisciplinary aspects of light scattering"
+}
+
+@article{atwater2010,
+ author = "Harry A. Atwater and Albert Polman",
+ year = "2010",
+ title = "Plasmonics for improved photovoltaic devices",
+ journal = "Nature materials"
+}
+
+@article{powel1959,
+ author = "C.J. Powell and J.B. Swan",
+ year = "1959",
+ title = "Origin of the Characteristic Electron Energy Losses in Aluminium",
+ journal = "Physical Review",
+ volume = "115",
+ number = "4"
+}
+
+
+@article{linic2011,
+ author = "Suljo Linic, Phillip Christopher and David B. Ingram",
+ year = "2011",
+ title = "Plasmonic-metal nanostructures for efficient conversion of solar to chemical energy",
+ journal = "Nature Materials"
+}
+
+@book{tompkins1992,
+ author = "Harland G. Tompkins",
+ title = "A User's Guide to Ellipsometry",
+ publisher = "Dover Publications",
+ year = 1992
+}
+
+@book{kittel,
+ author = "C. Kittel",
+ title = "Introduction to Solid State Physics",
+ publisher = "John Wiley and Sons, New York",
+ year = "1996",
+ edition = "7"
+}
+
+@article{ferrel1958,
+ author = "R.A. Ferrell",
+ title = "Predicted radiation of plasma oscillations in metal films",
+ journal = "Physical Review",
+ number = "111",
+ year = "1958",
+ pages="1214-1222"
+}
+
+@book{palik,
+ author = "D.W. Lynch, W.R. Hunter, E.D. Palik",
+ title = "Handbook of Optical Constants of Solids",
+ publisher = "Academic Press, New York",
+ year = "1985"
+}
+
+@book{ibach2010,
+ author = "H. Ibach, H. Lüth",
+ title = "Solid-State Physics: An Introduction to Principles of Materials Science",
+ year = "2010",
+ publisher = "Springer-Verlag, New York"
+}
+
+@article{pitark2007,
+ author = "J. M. Pitarke, V. M. Silkin, E. V. Chulkov and P. M. Echenique",
+ title = "Theory of surface plasmons and surface plasmon polaritons",
+ year = "2007",
+ journal = "Reports on Progress in Physics",
+ number = "70"
+}
+
+@article{sonnichsen2001,
+ author = "Carsten Sonnichsen",
+ title = "Plasmons in metal nanostructures (dissertation)",
+ year = "2001",
+ journal = "Ludwig-Maximilians-University of Munich"
+}
+
+@article{zheng2008,
+ author = "Yue Bing Zheng and Tony Jun Huang",
+ title = "Surface Plasmons of Metal Nanostructure Arrays: From Nanoengineering to Active Plasmonics",
+ year = "2008",
+ journal = "The Association for Laboratory Automation"
+}
+
+@article{bruggeman1935,
+ author = "D.A.G Bruggeman",
+ title = "Calculation of various physics constants in heterogenous substances I Dielectricity constants and
+conductivity of mixed bodies from isotropic substances",
+ journal = "Ann. Phys.-Berlin",
+ year = "1935",
+ number = "24",
+ pages= "636–664"
+}
author = "T.W.H Oats, H. Wormeester, H. Arwin",
title = "Characterization of plasmonic effects in thin films and metamaterials using spectroscopic ellipsometry",
year = 2011,
- journal = "Progress in Surface Science (Elsevier Ltd)",
+ journal = "Progress in Surface Science (Elsevier Ltd)"
}
-asdfasdf
-"The Bakerian Lecture"sdf
+
+"The Bakerian Lecture"
@article{faraday1857,
author = "M. Faraday",
title = "Experimental Relations of Gold (and Other Metals) to Light",
"J.A Woolam's overview of VASE, part II 2000"
"J.A Woollam Co., Inc., 645 'M' St. #102, Lincoln, NE 68508"
"John A. Woolam, Blaine Johs, Craig M. Herzinger, James Hilfiker, Ron Synowicki and Corey L Bungay"
-@article{woolam1999,
+@article{woolam2000,
author = "John A. Woolam and Co.",
title = "Overview of Variable Angle Spectroscopic Ellipsometry (VASE), Part II: Basic Theory and Typical Applications",
journal = "Optical Metrology",
}
+@article{bohm1953,
+ author = "David Pines and David Bohm",
+ title = "A collective description of electron interactions: III. coulomb interactions in a degenerate electron gas",
+ journal = "Physical Review",
+ volume = "92",
+ year = 1953
+}
@book{komolov,
author = "S.A. Komolov",
year = "1992",
publisher = "Gordon and Breach Science Publishers S.A",
}
+"Fourier microscopy of single plasmonic scatterers"
+@article{sersic2011,
+ author = "Ivana Sersic, Christelle Tuambilangana and A Femius Koenderink",
+ year = "2011",
+ journal = "New Journal of Physics",
+ volume = "13"
+}
+
+@article{garnet1904,
+ author = "Maxwell Garnet",
+ year = "1904",
+ journal = "Philosophical Transactions of the Royal Society A",
+ volume = "203",
+ pages = "385-420",
+}
+
+
+@article{ritchie1957,
+ author = "R. H. Ritchie",
+ year = "1957",
+ title = "Plasma Losses by Fast Electrons in Thin Films",
+ journal = "Physical Review",
+ volume = "106"
+}
+@article{mei1908,
+ author = "Gustav Mie",
+ year = "1908",
+ title = "Beirtrage zur optik truber medien, speziell kolloidaler metallosungen",
+ journal = "Ann. Phys. (Leipzig)",
+ volume = "25"
+}
+
+"How do you cite a conference?"
+@article{wriedt2008,
+ author = "Thomas Wriedt",
+ year = "2008",
+ title = "Mie Theory 1908-2008 - Introduction to the conference",
+ journal = "(Conference) Mie Theory 1908-2008 - Present developments and Interdisciplinary aspects of light scattering"
+}
+
+@article{atwater2010,
+ author = "Harry A. Atwater and Albert Polman",
+ year = "2010",
+ title = "Plasmonics for improved photovoltaic devices",
+ journal = "Nature materials"
+}
+
+@article{powel1959,
+ author = "C.J. Powell and J.B. Swan",
+ year = "1959",
+ title = "Origin of the Characteristic Electron Energy Losses in Aluminium",
+ journal = "Physical Review",
+ volume = "115",
+ number = "4"
+}
+
+
+@article{linic2011,
+ author = "Suljo Linic, Phillip Christopher and David B. Ingram",
+ year = "2011",
+ title = "Plasmonic-metal nanostructures for efficient conversion of solar to chemical energy",
+ journal = "Nature Materials"
+}
+
+@book{tompkins1992,
+ author = "Harland G. Tompkins",
+ title = "A User's Guide to Ellipsometry",
+ publisher = "Dover Publications",
+ year = 1992
+}
+
+@book{kittel,
+ author = "C. Kittel",
+ title = "Introduction to Solid State Physics",
+ publisher = "John Wiley and Sons, New York",
+ year = "1996",
+ edition = "7"
+}
+
+@article{ferrel1958,
+ author = "R.A. Ferrell",
+ title = "Predicted radiation of plasma oscillations in metal films",
+ journal = "Physical Review",
+ number = "111",
+ year = "1958",
+ pages="1214-1222"
+}
+
+@book{palik,
+ author = "D.W. Lynch, W.R. Hunter, E.D. Palik",
+ title = "Handbook of Optical Constants of Solids",
+ publisher = "Academic Press, New York",
+ year = "1985"
+}
+
+
+@book{ibach2010,
+ author = "H. Ibach, H. Lüth",
+ title = "Solid-State Physics: An Introduction to Principles of Materials Science",
+ year = "2010",
+ publisher = "Springer-Verlag, New York"
+}
+
+@article{pitark2007,
+ author = "J. M. Pitarke, V. M. Silkin, E. V. Chulkov and P. M. Echenique",
+ title = "Theory of surface plasmons and surface plasmon polaritons",
+ year = "2007",
+ journal = "Reports on Progress in Physics",
+ number = "70"
+}
+
+@article{sonnichsen2001,
+ author = "Carsten Sonnichsen",
+ title = "Plasmons in metal nanostructures (dissertation)",
+ year = "2001",
+ journal = "Ludwig-Maximilians-University of Munich"
+}
+
+@article{zheng2008,
+ author = "Yue Bing Zheng and Tony Jun Huang",
+ title = "Surface Plasmons of Metal Nanostructure Arrays: From Nanoengineering to Active Plasmonics",
+ year = "2008",
+ journal = "The Association for Laboratory Automation"
+}
+
+@article{bruggeman1935,
+ author = "D.A.G Bruggeman",
+ title = "Calculation of various physics constants in heterogenous substances I Dielectricity constants and
+conductivity of mixed bodies from isotropic substances",
+ journal = "Ann. Phys.-Berlin",
+ year = "1935",
+ number = "24",
+ pages= "636–664"
+}
\fi
\@input{titlepage/Titlepage.aux}
+\@input{acknowledgments/Acknowledgments.aux}
+\@input{abstract/Abstract.aux}
\@input{chapters/Introduction.aux}
-\@input{chapters/Theory.aux}
+\@input{chapters/Overview.aux}
\@input{chapters/Techniques.aux}
\@input{chapters/Results.aux}
\@input{chapters/Conclusion.aux}
\bibdata{references/refs}
\bibcite{pfund1930}{1}
-\bibcite{pfund1933}{2}
-\bibcite{harris1948}{3}
-\bibcite{harris1952}{4}
-\bibcite{harris1953}{5}
-\bibcite{mckenzie2006}{6}
-\bibcite{sondergaard2012}{7}
-\bibcite{komolov}{8}
-\bibcite{woolam1999}{9}
-\bibcite{woolam2000}{10}
-\bibcite{oates2011}{11}
+\bibcite{harris1952}{2}
+\bibcite{panjwani2011}{3}
+\bibcite{faraday1857}{4}
+\bibcite{garnet1904}{5}
+\bibcite{mei1908}{6}
+\bibcite{wriedt2008}{7}
+\bibcite{atwater2010}{8}
+\bibcite{linic2011}{9}
+\bibcite{maksymov2011}{10}
+\bibcite{maksymov2010}{11}
+\bibcite{harris1948}{12}
+\bibcite{harris1953}{13}
+\bibcite{mckenzie2006}{14}
+\bibcite{pfund1933}{15}
+\bibcite{advena1993}{16}
+\bibcite{sondergaard2012}{17}
+\bibcite{oates2011}{18}
+\bibcite{ferrel1958}{19}
+\bibcite{kittel}{20}
+\bibcite{ritchie1957}{21}
+\bibcite{bohm1951}{22}
+\bibcite{bohm1952}{23}
+\bibcite{bohm1953}{24}
+\bibcite{powel1959}{25}
+\bibcite{pitark2007}{26}
+\bibcite{komolov}{27}
+\bibcite{komolov1979}{28}
+\bibcite{woolam2000}{29}
+\bibcite{tompkins1992}{30}
+\bibcite{woolam1999}{31}
+\bibcite{kostylev2011}{32}
+\bibcite{palik}{33}
+\bibcite{bruggeman1935}{34}
+\bibcite{sonnichsen2001}{35}
+\bibcite{zheng2008}{36}
+\bibcite{ibach2010}{37}
\bibstyle{ieeetr}
-\@writefile{toc}{\contentsline {part}{References}{36}{chapter*.38}}
-\@writefile{toc}{\contentsline {chapter}{\numberline {A}READ AT YOUR OWN RISK}{37}{appendix.A}}
-\@writefile{lof}{\addvspace {10\p@ }}
-\@writefile{lot}{\addvspace {10\p@ }}
-\@input{appendices/tcs_noise.aux}
-\@input{appendices/electron_optics.aux}
-\@input{appendices/electron_gun_circuit.aux}
-\@input{appendices/data_aquisition.aux}
+\@writefile{toc}{\contentsline {part}{References}{38}{chapter*.36}}
+\@input{appendices/achievements.aux}
\BOOKMARK [0][-]{chapter.1}{Introduction}{}
-\BOOKMARK [0][-]{chapter.2}{Overview of Theory}{}
-\BOOKMARK [0][-]{chapter.3}{Experimental Techniques}{}
+\BOOKMARK [0][-]{chapter.2}{Overview}{}
+\BOOKMARK [1][-]{section.2.1}{Black Metal Films}{chapter.2}
+\BOOKMARK [1][-]{section.2.2}{Plasmonics}{chapter.2}
+\BOOKMARK [2][-]{subsection.2.2.1}{Bulk Plasmons}{section.2.2}
+\BOOKMARK [2][-]{subsection.2.2.2}{Surface Plasmons}{section.2.2}
+\BOOKMARK [2][-]{subsection.2.2.3}{Surface Plasmon Resonances}{section.2.2}
+\BOOKMARK [0][-]{chapter.3}{Techniques}{}
\BOOKMARK [1][-]{section.3.1}{Total Current Spectroscopy}{chapter.3}
+\BOOKMARK [2][-]{subsection.3.1.1}{General form of S\(E1\)}{section.3.1}
+\BOOKMARK [2][-]{subsection.3.1.2}{Contact Potential and the Surface Peak}{section.3.1}
+\BOOKMARK [2][-]{subsection.3.1.3}{Electron-Electron Interactions}{section.3.1}
+\BOOKMARK [2][-]{subsection.3.1.4}{Implementation of Total Current Spectroscopy Experiment}{section.3.1}
\BOOKMARK [1][-]{section.3.2}{Ellipsometry}{chapter.3}
-\BOOKMARK [2][-]{subsection.3.2.1}{Overview}{section.3.2}
+\BOOKMARK [2][-]{subsection.3.2.1}{Relation of measurements to properties of the sample}{section.3.2}
\BOOKMARK [2][-]{subsection.3.2.2}{Variable Angle Spectroscopic Ellipsometry}{section.3.2}
-\BOOKMARK [2][-]{subsection.3.2.3}{Relation of \040and \040to properties of the sample}{section.3.2}
-\BOOKMARK [1][-]{section.3.3}{Optical Transmission and Reflection Spectroscopy}{chapter.3}
-\BOOKMARK [1][-]{section.3.4}{Scanning Electron Microscopy}{chapter.3}
-\BOOKMARK [0][-]{chapter.4}{Results and Discussion}{}
+\BOOKMARK [1][-]{section.3.3}{Vacuum Techniques and Sample Preparation}{chapter.3}
+\BOOKMARK [0][-]{chapter.4}{Experimental Results and Discussion}{}
\BOOKMARK [1][-]{section.4.1}{Scanning Electron Microscopy}{chapter.4}
-\BOOKMARK [2][-]{subsection.4.1.1}{Higher Magnification Images of Au-Black}{section.4.1}
-\BOOKMARK [1][-]{section.4.2}{Atomic Force Microscopy of Au}{chapter.4}
-\BOOKMARK [1][-]{section.4.3}{Total Current Spectropy}{chapter.4}
-\BOOKMARK [2][-]{subsection.4.3.1}{Effect of Focusing of the Electron Gun on the TCS}{section.4.3}
-\BOOKMARK [2][-]{subsection.4.3.2}{Effect of Evaporation of Ag onto an Si substrate}{section.4.3}
-\BOOKMARK [2][-]{subsection.4.3.3}{Effect of Evaporation of Au on Si}{section.4.3}
+\BOOKMARK [1][-]{section.4.2}{Total Current Spectropy}{chapter.4}
+\BOOKMARK [2][-]{subsection.4.2.1}{Tuning the Electron Gun}{section.4.2}
+\BOOKMARK [2][-]{subsection.4.2.2}{Electron gun simulation}{section.4.2}
+\BOOKMARK [2][-]{subsection.4.2.3}{Deposition of Ag films onto a Si substrate}{section.4.2}
+\BOOKMARK [1][-]{section.4.3}{Optical Transmission Spectroscopy}{chapter.4}
+\BOOKMARK [2][-]{subsection.4.3.1}{Reference Spectrum}{section.4.3}
+\BOOKMARK [2][-]{subsection.4.3.2}{Transmission Spectra of Au and Black Au on Glass}{section.4.3}
\BOOKMARK [1][-]{section.4.4}{Variable Angle Spectroscopy Ellipsometry}{chapter.4}
-\BOOKMARK [2][-]{subsection.4.4.1}{Ag-Bright on Si substrate}{section.4.4}
-\BOOKMARK [2][-]{subsection.4.4.2}{Black Ag on Si}{section.4.4}
-\BOOKMARK [1][-]{section.4.5}{Optical Reflection Spectroscopy using the VASE}{chapter.4}
-\BOOKMARK [2][-]{subsection.4.5.1}{Au on Si}{section.4.5}
-\BOOKMARK [2][-]{subsection.4.5.2}{Au on Au-Black on Au on Si}{section.4.5}
-\BOOKMARK [2][-]{subsection.4.5.3}{Comparison with model of 50nm Au on Si}{section.4.5}
-\BOOKMARK [1][-]{section.4.6}{Optical Transmission Spectroscopy using OceanOptics Spectrometer}{chapter.4}
-\BOOKMARK [2][-]{subsection.4.6.1}{Dark Spectrum}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.2}{Reference Spectrum}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.3}{Testing the Spectrometer}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.4}{Transmission Spectra of Glass}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.5}{Transmission Spectra of Au and Au-Black on Glass}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.6}{Transmission Spectra of Ag}{section.4.6}
-\BOOKMARK [2][-]{subsection.4.6.7}{Transmission Spectra of Ag and Ag-Black on Glass}{section.4.6}
-\BOOKMARK [0][-]{chapter.5}{Conclusion}{}
-\BOOKMARK [-1][-]{chapter*.38}{References}{}
-\BOOKMARK [0][-]{appendix.A}{READ AT YOUR OWN RISK}{chapter*.38}
-\BOOKMARK [1][-]{section.A.1}{Effect of Noise on the TCS Curve}{appendix.A}
-\BOOKMARK [1][-]{section.A.2}{Electron Optics}{appendix.A}
-\BOOKMARK [2][-]{subsection.A.2.1}{A two dimensional electron gun simulation}{section.A.2}
-\BOOKMARK [1][-]{section.A.3}{Electron Gun Control Circuit}{appendix.A}
-\BOOKMARK [2][-]{subsection.A.3.1}{Control Circuit}{section.A.3}
-\BOOKMARK [2][-]{subsection.A.3.2}{The Ammeters}{section.A.3}
-\BOOKMARK [1][-]{section.A.4}{Data Aquisition Hardware}{appendix.A}
-\BOOKMARK [2][-]{subsection.A.4.1}{Overview}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.2}{Microprocessor}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.3}{ADC Inputs}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.4}{Temperature Measurement}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.5}{Power Supplies}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.6}{DAC Output}{section.A.4}
-\BOOKMARK [2][-]{subsection.A.4.7}{RS-232 Communications}{section.A.4}
+\BOOKMARK [2][-]{subsection.4.4.1}{Model for Ag and Black Ag on a Si substrate}{section.4.4}
+\BOOKMARK [2][-]{subsection.4.4.2}{Surface and Bulk Plasmons in the Ag and Black Ag films}{section.4.4}
+\BOOKMARK [0][-]{chapter.5}{Conclusions}{}
+\BOOKMARK [-1][-]{chapter*.36}{References}{}
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+
%\usepackage{natbib}
\usepackage{makeidx}
\newpage
-%include{acknowledgments/Acknowledgments} % This is who you thank
+\include{acknowledgments/Acknowledgments} % This is who you thank
\newpage
-%\include{abstract/Abstract} % This is your thesis abstract
+\include{abstract/Abstract} % This is your thesis abstract
\pagenumbering{roman}
\newpage
\include{chapters/Introduction}
-\include{chapters/Theory} % This is chapter 1
+\include{chapters/Overview} % This is chapter 1
\include{chapters/Techniques} % This is chapter 2
% Appendices
\appendix
-\renewcommand\chaptername{Appendix}
-\chapter{READ AT YOUR OWN RISK}
+\include{appendices/achievements}
+%\include{proposal/proposal.tex}
+%\renewcommand\chaptername{Appendix}
+%\chapter{Appendix}
+%\include{appendices/electron_optics}
+%\include{appendices/electron_gun_circuit}
+%\include{appendices/tcs_noise}
+%\include{appendices/data_aquisition}
-\include{appendices/tcs_noise}
-\include{appendices/electron_optics}
-\include{appendices/electron_gun_circuit}
-\include{appendices/data_aquisition}
%---------------------------------------------------------
The evaporators consist of a tungsten wire filament attached between two feedthroughs. A piece of a desired metal is folded over the apex of the tungsten wire. The metal can be heated by passing a current through the filament; near the metal's melting point it begins to evaporate. To clean the metal surface and ensure uniform evaporation, this procedure is first performed at low pressure (below $10^{-6}$ mbar) with no sample in the chamber, with the current increased until the metal piece begins to melt and forms a ball on the wire. Figure \ref{} shows an image of an evaporator that has been prepared for use.
-This study focused primarily on depositing Au films on an Si substrate, at both high and low pressures. The substrates and sample holders were cleaned in an acetone bath immediately prior to insertion in the vacuum chamber.
+This study focused primarily on depositing Au and Ag films on an Si substrate, at both high and low pressures. The substrates and sample holders were cleaned in an acetone bath immediately prior to insertion in the vacuum chamber.
\pagebreak
--- /dev/null
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+
+%\title{\bf Characterisation of nanostructured thin films}
+%\author{Sam Moore\\ School of Physics, University of Western Australia}
+%\date{April 2012}
+%\maketitle
+
+\begin{center}
+ B.Sc. (Hons) Physics Project \par
+ {\bf \Large Thesis} \par
+ Samuel Moore \\
+ School of Physics, University of Western Australia \\
+ April 2012
+\end{center}
+\section*{Characterisation of Nanostructured Thin Films}
+{\bf \emph{Keywords:}} surface plasmons, nanostructures, spectroscopy, metallic-blacks \\
+{\bf \emph{Supervisers:}} W/Prof. James Williams (UWA), Prof. Sergey Samarin (UWA) \\
+
+\pagebreak
+\tableofcontents
+
+\pagebreak
+
+\section*{Acknowledgements}
+
+I am extremely grateful for the support offered to me by many individuals during this project. There aren't many synonyms for ``Thanks'', so I'm afraid this section may be a little repetitive.
+
+Thanks to my supervisors Prof Sergey Samarin and W/Prof Jim Williams for envisioning the project, and their invaluable support throughout the year. I would also like to thank staff members at CAMSP for assisting with the supervision of this project. In particular I am extremely grateful for the help and advice given by Dr Paul Gualiardo during the construction and testing of the Total Current Spectroscopy experiment.
+
+Thanks to Alexie ??? from CMCA for producing the SEM images which proved a invaluable aid for discussing the structure of the metallic-black films. Thanks to Nikita Kostylev for helping me learn the art of operating the ellipsometer. Thanks to both Prof Mikhail Kostylev and Jeremy Hughes for lending me some samples for ellipsometric analysis. I would also like to endorse the team at J.A Woolam, who provided replacement pins for the ellipsometer alignment detector at no charge after one of the original pins became mysteriously damaged.
+
+Congratulations to Jeremy Hughes who successfully predicted that the emission current of the electron gun was varying periodically less than a quarter of the way through the first period. Condolences to Alexander Mazur, whose theory that the vacuum chamber contained a pulsar proved unfounded.
+
+Thanks to all my family and friends for their support and for continuing to put up with my slow descent into madness during the last 12 months.
+
+Finally, perhaps as a result of the aforementioned madness, I would also like to thank the various pieces of equipment and inanimate objects which have been crucial to the success of this project. This includes the ellipsometer, the ADC/DAC box, my laptop computer ``Cerberus'', and the two ammeters upon which I relied upon so heavily. Rest in peace Keithly 610B. Your death was not in vain.
+
+\pagebreak
+
+\section{Introduction}
+
+The report will be organised as follows; first we will discuss literature relating to surface science and nanostructured thin films in particular. We will then give an overview of the primary experimental techniques employed during this project, before presenting experimental results. Finally, we will discuss stuff.
+
+\emph{NOTE: Introduction needs work}
+
+\pagebreak
+
+\section{Overview}
+
+In this section we provide an overview of theoretical and experimental literature related to the properties of nanostructured thin films. We also include a summary of the past research which focuses on metallic-black films.
+
+
+
+
+
+
+
+\subsection{Electron Surface Interaction}
+
+
+% Research of Komolov
+
+\subsection{Electron Surface Interaction}
+
+
+\subsection{Plasmons}
+
+\emph{NOTE: To be completely honest, I don't think I can say much about plasmons. The TCS experiment does not detect plasmonic behaviour. The Ellipsometer can be used to determine frequencies at which plasmons might occur. However, I have not seen any dips in $\epsilon$ which would indicate plasmon thresholds.}
+
+% What are they?
+A plasmon is a quasi-particle arising due to charge density oscillations in a solid.
+
+
+
+% Early research
+
+\subsection{Metallic-Black Films}
+
+% What are they?
+So called metallic-black films are the result of deposition of metal elements at a relatively high pressure (of the order of $10^{-2}$ mbar). The films are named due to their high absorbance at visible wavelengths; they appear black to the naked eye. There is a remarkable contrast between such films and films deposited under low pressure (less than $10^{-6}$mbar), which are typically highly reflective and brightly coloured.
+
+% First mentions and early research; Pfund
+This phenomenom has been known since the early 20th century, with the first papers on the subject published by Pfund in the 1930s \cite{pfund1930}, \cite{pfund1933}. Pfund established the conditions for formation of metallic-blacks \cite{pfund1930}, and showed that the transmission spectrum of metallic black films is almost zero in visible wavelengths, but increases to a plateau in the far infrared \cite{pfund1933}. More extensive research on the structural and optical properties of these films by Louis Harris and others during the 1940s and 1950s \cite{harris1948}, \cite{harris1952}, \cite{harris1953}. It has been established that metallic blacks may be prepared in either air or inert gases
+
+
+% Pretty pictures for purpose of this discussion
+% Not really "results", since I didn't make the images
+Secondary Electron Microscope (SEM) images of Au deposited on Si at high and low pressures (in air) were produced at the Centre for Microscopy Characterisation and Analysis (CMCA), UWA. The film imaged on the left (high pressure) appears black at visible wavelengths, whilst the film on the right (low pressure) appears golden yellow.
+
+\begin{center}
+
+
+\begin{tabular}{cc}
+ \includegraphics[scale=0.2]{figures/Au_BLACK_200nm.png} & %\captionof{figure}{Au-Black SEM Image} \label{Au_BLACK_200nm.png} &
+ \includegraphics[scale=0.2]{figures/Au_semi-shiny_1_SEM.png} %\captionof{figure}{Au SEM Image} \label{Au_semi-shiny_1_SEM.png}
+
+ \label{SEM_images}
+\end{tabular}
+
+ \captionof{figure}{{\bf SEM images of Au deposited on Si at $2\times10^{-2}$mbar (left) and $1\times10^{-6}$mbar.} Note that the scales are very similar for both images.}
+
+\end{center}
+
+% Explanation of structure?
+The structural difference between the two films is striking, and yet the exact mechanism behind the formation of the metallic-black film is not well understood. The most widely accepted explanation is that the evaporated metal particles reaching the target surface have insufficient energy to form a regular crystal lattice due to cooling through collisions with the atmosphere \cite{}. As of yet, there is no detailed theoretical description of this behaviour.
+
+% Research by Harris concluding ``condensor'' like structure
+Harris et al. have produced experimental results of the transmission of metallic-black films from visible wavelengths to the far-infrared \cite{}. By modelling the film as a layer of metallic strands, acting as ``condensors'', Harris et al. arrived at an expression for the electron relaxation time of [element]-black \cite{}, leading to a a transmission spectrum in good agreement with experimental results.
+
+% Mckenzie
+Mckenzie has established that the presence of oxygen effects the optical and electrical properties of metallic-blacks \cite{mckenzie2006}.
+
+% Model of structure
+Nanostructured metal films prepared at low pressure are often approximated by an isotropic layer of spherical blobs upon the substrate, or even as a uniform layer with an ``effective'' thickness \cite{}. As the right image in Figure \ref{SEM_images} shows, this is a good representation of the structure of such a film. In contrast, the metallic-black film is highly non-uniform; as a result, detailed characterisation of the properties of such a film is difficult.
+
+
+
+
+% More recent research
+More recently, it was shown that Au-black coatings increased the efficiency of thin film solar cells \cite{}. In this study, a simulation approximating an Au-black film as a layer of semi-spherical structures showed plasmonic behaviour which lead to an increase in electric field behind the film.
+
+
+% Artificially ``blackened'' thin films
+Metallic-black films have proven useful in applications requiring efficient absorption of light, including the. Recently there has been interest in artificial ``blackening'' of metal surfaces in ways which simplify the characterisation of the surfaces for practical applications.
+
+Sondergaard et al. have produced metallic-black surfaces capable of suporting surface plasmon modes \cite{sondergaard2012}. These films exhibit similar optical properties to the previously considered ``evaporated'' metallic-black surfaces.
+
+% What I will be doing with metallic-black films
+This project will employ Total Current Specroscopy, Ellipsometry and Optical Spectroscopy methods to investigate the difference between metallic films deposited at low pressure, and high pressure (metallic-blacks). The production and study of artificially blackened films is beyond the scope of this research.
+
+
+\begin{center}
+ \includegraphics[scale=0.2]{figures/300V-01.jpg}
+ \captionof{figure}{{\bf Au-black film viewed at magnifications of x20000, x50000, x100000 and x200000} (top left, top right, bottom left, bottom right). The film appears non-isotropic, and possibly fractal like upon magnification. This structure has lead some reasearchers to refer to the deposited films as ``smokes'' \cite{}.}
+ \label{300V-01.jpg}
+\end{center}
+
+\pagebreak
+
+\section{Experimental Techniques}
+
+\subsection{Secondary Electron Spectroscopy}
+
+In this section, we will give a general overview of the basic concepts of Secondary Electron Spectroscopy. The next section will focus on low energy Total Current Spectroscopy, the particular technique which has been employed for this study.
+
+
+Secondary Electron Spectroscopy encompasses a large group of techniques used for studying the electron spectra of surfaces and solids, and processes of secondary electron emission. In these methods a beam of primary electrons is directed at a surface. The interactions between primary electrons and the surface give rise to an energy distribution of secondary electrons ejected from the surface.
+
+
+\begin{center}
+ \includegraphics[scale=0.40]{figures/se_dist.pdf}
+ \captionof{figure}{{\bf Model of Secondary Electron Distribution}}
+ \label{se_dist.pdf}
+\end{center}
+
+\emph{NOTE: I need to draw some fine structure on this curve somehow. Or find an actual spectrum to reproduce.}
+
+Figure \ref{se_dist.pdf} shows a simplified model of an energy distribution of secondary electrons.
+
+The spectrum shown in Figure \ref{se_dist.pdf} may be divided into several regions based upon the originating processes of the secondary electrons in each region. However, it is important to note that these processes are determined by the primary electron energy $E_p$; each process has a threshold energy, below which it cannot occur. For example, Auger electrons are only produced if the primary electrons have sufficient energy to excite an inner level electron to above the Fermi level.
+
+The narrow peak centred at $E = E_p$ is largely due to elastically scattered primary electrons\footnote{A typical width is $0.5-1.0$eV; as a result, small energy losses due to phonon excitations ($10-50$meV) can not resolved from truly elastic reflections \cite{komolov}}; the width of this peak is determined by the distribution of primary electron energies, as well as the resolution of the detector.
+
+Fine structure due to low energy losses can be observed just below the primary peak. These energy losses are due to transitions between the valence and conduction bands, and plasma vibration excitation. This part of the spectrum is the focus of Energy Electron Loss Spectroscopy (EELS).
+
+The central region of the distribution is mostly due to inelastically scattered (or ``rediffused'') primary electrons. If the energy of primary electrons is sufficient, this region may also contain fine structure due to Auger excitations.
+
+The broad, asymetrical curve at low energy is due to inelastically scattered primary electrons which have undergone multiple scattering events. So called ``true'' secondary electrons, the direct result of secondary electron emission, also appear in this region for sufficiently large primary electron energies.
+
+For a more detailed discussion, refer to \cite{komolov}.
+
+
+Techniques of Secondary Electron Spectroscopy can be divided into two classes. Energy-resolved methods are based upon observation of the secondary electron distribution at a fixed primary electron energy. The angular distribution of emitted electrons is often also recorded. These methods aim to examine the properties of secondary electrons emitted in a particular energy interval.
+
+
+In contrast to Energy-resolved methods, Total Current (or Yield) methods measure the total current of secondary electrons whilst varying the primary electron energy. As the primary electron energy reaches the threshold for a particular mechanism of secondary electron scattering, the analysis of the total secondary electron current as a function of energy can give information about the threshold energies for processes of interest.
+
+Total Current methods are generally simpler to realise experimentally compared with Energy-resolved methods, as they do not require energy analysers, and current measurement may be performed external to the vacuum chamber, using a conventional low current ammeter. It is also simple to combine a Total Current methods with existing Energy-resolved methods.
+
+
+\subsection{Low Energy Total Current Spectroscopy}
+
+As the name suggests, low energy Total Current Specroscopy is based upon measurement of the total secondary electron current at low primary electron energies, typically in the range of $0-15$eV. At low primary energies, the secondary electron current is predominantly composed of inelastically reflected primary electrons which have lost energy in causing interband transitions.
+
+Figure \ref{tcs_simple.pdf} shows a simplified schematic for the Total Current Spectroscopy experiments conducted during this study. Electrons are produced via thermionic emission by heating a cathode. A series of electrodes are used to accelerate and focus a current $I_1$ onto the target. The energy of primary electrons is controlled by adjusting the power supply $U$, which determines the potential between the cathode and target. The transmitted current $I$ to flow through an ammeter external to the chamber. For a more detailed description of the experimental setup, Refer to Appendix B for a discussion of hardware to automate the measurement of $I$ and control of $U$. Refer to Appendix D for a discussion of the electron gun and its control circuit.
+
+\begin{center}
+ \includegraphics[scale=0.50]{figures/tcs_simple}
+ \captionof{figure}{Simplified Diagram of TCS Experiments}
+ \label{tcs_simple.pdf}
+\end{center}
+
+The goal of Total Current Spectroscopy is to measure variations in the secondary electron current, $I_2$. It can easily be demonstrated that this can be accomplished by measurement of $I$.
+
+In the following discussion, we will summarise the approach adopted by Komolov to relate measurement of $I(E_1)$ to characteristics of the sample under study \cite{komolov}.
+
+From the above, it is obvious that $I = I_1 - I_2$. Assuming that $I$ is a constant, independent of primary electron energy $E_1$, we define the Total Current Spectrum (TCS) as:
+\begin{align*}
+ S(E_1) &= \der{I}{E_1} = - \der{I_2}{E_1}
+\end{align*}
+This result also assumes that $I$ does not vary during the time taken to perform a measurement of $S(E_1)$ for a range of $E_1$ values. This is generally valid in the period after the cathode reaches thermal equilibrium.
+
+The energy of a single primary electron arriving at the sample is given by $E = e U + c$, where $e$ is the electron charge, $U$ is the potential difference between cathode and sample, and $c$ a constant including the contact potential between the cathode and sample.
+In reality, the cathode emits electrons with a distribution of energies, which is further altered by the focusing properties of the electrodes; as a result, the energy of the incident primary electrons is described by a distribution $f(E - E_1)$ about the mean value $E_1$, with the maximum of the distribution at $E = E_1$.
+
+The primary electron current $I_1$ for a mean energy $E_1 = e U$ can be written as:
+\begin{align*}
+ I_1(E_1) &= e A \int_{0}^{\infty} f(E - E_1) dE
+\end{align*}
+Where $A$ is the surface area irradiated by the beam.
+
+Introducing the secondary emission coefficient $\sigma(E)$, which gives the probability for a primary electron of energy $E$ to give rise to a secondary electron, we can write the secondary electron current as:
+\begin{align*}
+ I_2(E_1) &= e A \int_{-E_1}^{\infty} \sigma(E_1)f( E - E_1) dE
+\end{align*}
+
+The total current $I$ may then be written as:
+\begin{align*}
+ I(E_1) &= e A \left[ \int_{0}^{\infty} f(E - E_1) dE - \int_{-E_1}^{\infty} \sigma(E_1)f( E - E_1) dE \right]
+\end{align*}
+
+Differentiating, using the fundamental theorem of calculus, we can determine the total current spectrum:
+\begin{align*}
+ S(E_1) = \der{I}{E_1} &= e A \left\{ [ 1 - \sigma(0)] f(-E_1) - \int_{0}^{\infty} f(E - E_1) \der{\sigma(E_1)}{E_1} dE \right\}
+\end{align*}
+
+The first term in the above expression is determined solely by the distribution of primary electrons $f$. This term will be maximised when $E_1 = 0$; meaning that $U$ is equal to the contact potential $c$ between the cathode and sample.
+
+The second term contains all dependence of $S(E_1)$ on characteristics of the sample. At the threshold for a particular process, the secondary emission efficiency $\sigma(E_1)$ is expected to undergo a sharp change. This results in a well defined maxima or minima in the derivative $\der{\sigma(E_1)}{E_1}$, which can be seen as a corresponding maxima or minima in the total current spectrum $S(E_1)$. From the convolving function $f(E - E_1)$, it can be seen that the distribution of primary electron energy determines the degree to which $\der{\sigma(E_1)}{E_1}$ may be resolved from measurement of $S(E_1)$.
+
+The total current spectrum $S(E_1) = \der{I}{E_1}$ can be obtained from measurement of $I(E_1)$ using a finite difference approximation. Often, the conventional ammeter and DC power supply in Figure \ref{tcs_simple.pdf} are replaced with a lock-in amplifier and AC power supply, as in Komolov's description \cite{komolov}. Lock-in amplifier techniques have the advantage of measuring $S(E)$ directly. The lock-in amplifier also eliminates unwanted sources of noise. For this study, the lock-in amplifier approach was inpractical due to the limitations on available equipment. For future studies, it is suggested that the lock-in amplifier approach be adopted.
+
+
+\subsubsection{The Secondary Emission Coefficient}
+
+$\sigma(E)$ can be written as the sum of two components, representing the probability for secondary electrons arrising due to elastic reflections or any mechanism involving primary electron energy loss.
+
+
+
+
+
+
+
+
+
+
+\subsection{Ellipsometry}
+
+Ellipsometry is an optical technique most commonly used to determine the thickness of multilayered thin films. Ellipsometry can also be used to determine the optical constants and properties of unknown materials.
+
+Essentially, ellipsometry measures the change in polarisation of light reflected from a surface. This change in polarisation can be related to properties of the surface if knowledge of the surface is correctly applied. For a bulk sample, the change in polarisation can be directly related to the optical constants of the material.
+
+
+\subsection{Vacuum Techniques and Sample Preparation}
+
+Both the TCS experiments and the deposition of films must be performed in a vacuum. For convenience and simplicity, a single vacuum chamber at CAMSP has been repurposed to perform both of these tasks. The chamber can be pumped by a molecular turbo pump, backed by a rotaray pump, to a base pressure of $2\times10^{-8}$ mbar, or by the rotary pump alone to a base pressure of $1\times10^{-3}$ mbar. The pressure is monitored using either a pirani or ion gauge (for pressures greater than and less than $10^{-3}$ mbar respectively).
+
+%TODO: Insert graphs of pressure in chamber
+
+Figure \ref{} shows a diagram of the vacuum chamber used both for the creation of nanostructured thin films and their study using TCS. A rotatable sample holder is positioned in the centre of the chamber. One flange of the chamber houses the electron gun used for TCS measurements, whilst the opposite flange contains feedthroughs on which tungsten filament evaporators are mounted. This setup allows for almost immediate study of evaporated films by simple rotation of the sample holder to face the gun.
+
+
+The evaporators consist of a tungsten wire filament attached between two feedthroughs. A piece of a desired metal is folded over the apex of the tungsten wire. The metal can be heated by passing a current through the filament; near the metal's melting point it begins to evaporate. To clean the metal surface and ensure uniform evaporation, this procedure is first performed at low pressure (below $10^{-6}$ mbar) with no sample in the chamber, with the current increased until the metal piece begins to melt and forms a ball on the wire. Figure \ref{} shows an image of an evaporator that has been prepared for use.
+
+This study focused primarily on depositing Au films on an Si substrate, at both high and low pressures. The substrates and sample holders were cleaned in an acetone bath immediately prior to insertion in the vacuum chamber.
+
+\pagebreak
+
+\section{Experimental Results and Discussion}
+\subsection{TCS Measurements}
+
+This study has focused on the evolution of the TCS of Au deposited on Si with increasing thickness of Au film. A general dependence of TCS curves on time has also been observed; it is likely that this time dependence is due to oxidation of the surface of the sample.
+
+
+
+\subsubsection{TCS of Si Substrate}
+
+Figure \ref{} shows the TCS
+
+Figure \ref{} shows the TCS of Si in the (111) and (100) orientations as presented by Komolov \cite{komolov}
+
+
+\subsection{Ellipsometric Measurements}
+
+\subsection{Transmission Spectra of Metal Films}
+
+Using the VASE and a commercial spectrometer (OceanOptics) in independent experiments, we obtained transmission spectra for metallic-black and some other metallic films.
+
+\pagebreak
+
+\section{Conclusions}
+
+\pagebreak
+
+\bibliographystyle{unsrt}
+\bibliography{thesis}
+
+
+\pagebreak
+
+\section*{List of Student Achievements}
+
+\pagebreak
+
+\section*{Appendix A - Electron Optics for Total Current Spectroscopy}
+
+
+Figure \ref{electron_gun.pdf} shows the complete electron gun control circuit. The circuit was designed and constructed as part of this project. The design is based upon examples found in \cite{komolov} and \cite{Moore}.
+
+The electron gun has been recycled from a Cathode Ray Oscilloscope. The gun contains a total of 9 electrodes; several electrodes are held at the same potential, as shown in the figure. As shown in figure \ref{electron_gun.pdf}, the electrode potentials are referenced to the cathode, not signal ground; this ensures that the focusing properties of the gun are not affected with changing potential between the cathode and ground.
+
+Here we give a general discussion of aspects of the electron gun:
+\begin{enumerate}
+ \item Cathode
+
+A high yield $\text{Ba}\text{O}^2$ filament was used as the cathode. This type of filament consists of a straight piece of tungsten wire bent at the centre into a sharp kink. A $\text{Ba}\text{O}^2$ disc is attached to the apex of the kink. A heating current (between 1.1 and 1.2A) is applied across the filament. Electrons near the surface of the disc recieve thermal energy as the filament is heated; once an electron has recieved enough energy, it is able to leave the surface of the disc through thermionic emission.
+
+By applying Kirchoff's Laws to the circuit shown in Figure \ref{electron_gun.pdf}, it can be seen that the ammeter labelled ``Emission Current'' measures the total current in all loops passing through an electrode or the sample, and the cathode. This measured current does not include electrons which pass directly through the the vacuum chamber to ground; however, due to the large distance between the gun and the chamber walls, this current can be neglected.
+
+
+ Figure \ref{} shows the measured cathode emission current as a function of time, starting several seconds prior to heating the cathode. From this graph, it can be estimated that at least $10$ minutes should be allowed for the filament to come to thermal equilibrium before commencing measurements.
+
+
+ \item Primary Energy - The potential difference between the sample and the cathode $U$. Primary electrons arriving at the sample have energy $E = eU + \text{constant}$.
+
+ For obvious reasons, it is impractical to directly attach a wire to the emitting surface of the cathode. Instead, two equal resistors are placed in series with the cathode, with the primary energy set point connected to the middle of the resistors. By applying Kirchoff's Voltage Law, making the (reasonable) assumption that both halves of the filament have equal resistance, the potential of the filament tip will be equal to that of the primary energy set point.
+
+
+ \item Wenhault
+
+ The Wenhault is a small cylindrical electrode which surrounds and houses the filament.
+
+ \item Einzel Lens
+
+ \item Deflection Plates
+
+ \item Final Electrode
+\end{enumerate}
+
+As discussed in Section \ref{}, the resolution of total current spectroscopy (and energy resolved secondary electron spectroscopy) is intrinsically linked to the distribution in energies of electrons arriving at the sample. Although the dist
+
+A two dimensional electron gun simulator has also been written in order to help produce figures for qualitative purposes; results of some simulations are shown in Figure \ref{}.
+
+
+
+
+\subsection*{Primary Energy Control and Current Measurement}
+
+In order to collect data on the large number of planned samples for the study, some form of automation was required. The automated system needed to be able to set the primary energy by adjusting the potential of the cathode relative to the sample, and simultaneously record the total current through the sample.
+
+The available power supplies at CAMSP featured analogue inputs for external control. This meant that a Digital to Analogue Convertor (DAC) card was needed to interface between the control computer and the power supply. In addition, the available instruments for current measurement produced analogue outputs. As a result, Analogue to Digital Convertors (ADCs) were required to automate the recording of total current.
+
+Although an external DAC/ADC box was already available for these purposes, initial tests showed that the ADCs on the box did not function. The decision was made to design and construct a custom DAC/ADC box, rather than wait up to two months for a commercial box to arrive. The design of the custom DAC/ADC box is discussed in detail in Appendix B, and the software written for the on-board microprocessor and the controlling computer are included in Appendix D.
+
+Figure \ref{block_diagram.pdf} shows a block diagram including all aspects of the Total Current Spectroscopy experiments. The emission current measurement point was included to allow for monitoring the behaviour of the filament, and confirm the assumptions of constant emission current. After the malfunctioning of one of the two available ammeters, it was only possible to measure sample current. However, earlier tests suggested that for short time periods (several minutes at most) the emission current's dependence upon time was negligable.
+
+\begin{center}
+ \includegraphics[scale=0.80]{figures/block_diagram}
+ \captionof{figure}{Block Diagram for TCS Experiments}
+ \label{block_diagram.pdf}
+\end{center}
+
+
+\begin{landscape}
+
+
+ \includegraphics[scale=0.85]{figures/electron_gun.pdf}
+ \captionof{figure}{Electron Gun and Control Circuit}
+ \label{electron_gun.pdf}
+
+
+\end{landscape}
+
+\section*{Appendix B - DAC/ADC Box - Hardware}
+
+\subsection*{Overview}
+
+In order to automate TCS experiments, both Digital to Analogue and Analogue to Digital Convertors were required (DAC and ADC). To provide these, a custom DAC/ADC Box was designed and constructed. The box can be controlled by any conventional computer with available RS-232 serial communication (COM) ports. Most modern computers no longer feature COM ports; a commercially available convertor can be used to interface between the box's RS-232 output and a standard Universal Serial Bus (USB) port.
+
+
+The key components of the DAC/ADC box hardware include:
+
+\begin{itemize}
+ \item Microprocessor (AVR Butterfly ATMega169)
+ \item Four Analogue to Digital Converter (ADC) inputs
+ \item Single Digital to Analogue Converter (DAC) output (Microchip MCP4922)
+ \item Analogue electronics for amplification at ADC inputs and DAC outputs
+ \item Seperate power supply circuitry for Digital and Analogue electronics
+ \item RS-232 communications for control by a conventional PC or laptop
+\end{itemize}
+
+\subsection*{Microprocessor}
+The DAC/ADC box has been based upon Atmel's AVR Butterfly; an inexpensive and simple demonstration board for the ATMega169 16 Bit microprocessor. The features of the AVR Butterfly include easily accessible ports for Analogue to Digital Convertor (ADC) inputs and digital input/output, an onboard Universal Asynchronous Reciever/Transmitter (USART) for RS-232 serial communications, and a 6 character Liquid Crystal Display (LCD). The AVR Butterfly can be programmed using a conventional computer over the USART using a RS-232 COM port. For modern computers (which do not usually posess COM ports), a RS-232 to USB converter may be used.
+
+Figure \ref{avr_butterfly.pdf} is a labelled photograph of the AVR Butterfly showing the use of the available ports for this project.
+
+
+%Figure of Butterfly
+\begin{center}
+ \includegraphics[scale=0.70]{figures/avr_butterfly.pdf}
+ \captionof{figure}{AVR Butterfly} \label{avr_butterfly.pdf}
+\end{center}
+
+Unless otherwise stated, all voltage differences are specified relative to the power supply ground of the AVR Butterfly.
+
+\subsection*{ADC Inputs}
+
+The AVR Butterfly offers easy access to four of the ATMega169's ADCs through PORTF. Each ADC is capable of measuring voltages of $0 < V_{\text{adc}} < V_{cc}$ with 10 Bit resolution. For measuring voltages outside this range, some circuitry is required between the input voltage and the ADC input. In addition, it is desirable to provide the ADC with some form of input protection against accidental overloading. Figure \ref{adc_normal.pdf} shows the input circuit which was used for three of the four available ADCs.
+
+\begin{center}
+ \includegraphics[scale=0.50]{figures/adc_normal.pdf}
+ \captionof{figure}{ADC4,6,7 Input} \label{adc_normal.pdf}
+\end{center}
+
+
+For making voltage measurements above $V_{cc}$, a voltage divider allows reduction of the voltage at the ADC. By constructing the voltage divider using a variable resistor, the range of measurable inputs could be manually adjusted.
+
+The diodes shown in Figure \ref{adc_normal.pdf} ensure that the ADC is protected from accidental exposure to voltages outside the acceptable range. In normal operation both diodes are off. If $V_{\text{adc}}$ were to become greater than the reference point $V_{cc}$, current would flow between the ADC input and the reference point, acting to reduce $V_{\text{adc}}$ until it reached $V_{cc}$. Similarly, if $V_{\text{adc}}$ fell below ground, current would flow from ground to the ADC input, acting to increase $V_{\text{adc}}$ until it reached ground.
+
+The voltage at the ADC input can be related to the input of the voltage divider using Kirchoff's Voltage Law and Ohm's Law:
+\begin{align*}
+ V_{\text{adc}} &= \frac{R_1}{R_1 + R_2} V_{\text{in}}
+\end{align*}
+Where $V_{\text{in}}$ is the voltage at the input of the circuit, $R_1$ is a fixed resistor, and $R_2$ is variable resistor.
+
+$V_{\text{in}}$ can be therefore be determined from the registered ADC counts by:
+\begin{align*}
+ V_{\text{in}} &= \left(\frac{\text{ADC counts}}{2^{10}}\right) \times \frac{R_1 + R_2}{R_1} V_{cc}
+\end{align*}
+
+\subsubsection*{Differential ADC Input}
+
+During the testing of the TCS experimental apparatus, it became desirable to measure the emission current of the electron gun. The electrometer used for this current measurement was capable of producing an analogue output in the range of $0-1V$. However, the negative terminal of this output was not at ground potential, but rather at the same terminal as the negative input terminal. Directly connecting the electrometer output to one of the ADC inputs discussed above would create a short circuit between the initial energy power supply, and ground (refer to Figures \ref{} and \ref{}). Therefore, it was decided to add a differential stage before the input of one of the ADCs.
+
+Figure \ref{adc5.pdf} shows the modification made to the input for ADC5 on the AVR Butterfly. The original voltage divider and input protection discussed above are still present. The modifications include the addition of an instrumentation amplifier, and low pass filters.
+
+\begin{center}
+ \includegraphics[scale=0.70]{figures/adc5}
+ \captionof{figure}{Differential Input stage for ADC5}
+ \label{adc5.pdf}
+\end{center}
+
+asdfa
+The instrumentation amplifier consists of two stages of operational amplifiers (op-amps); input buffers, and a difference amplifier.
+The difference amplifier can be shown using the ideal op-amp model to produce an output voltage proportional to the difference between its inputs:
+
+\begin{align*}
+ V_{out} &= \frac{R_2}{R_1} \left(V_{2} - V_{1}\right)
+\end{align*}
+
+The two op-amps at the inputs to the differential amplifier are unity gain buffers. Although the outputs of the op amps are equal to their inputs, current is prevented from flowing from the circuit under measurement, and is instead drawn from the op amp power supply.
+
+In principle, two ADC channels could be used to record the positive and negative outputs of the electrometer seperately, with differencing done in software. However this would require modification to the output cable of the electrometer, which may prove inconvenient for future uses.It was decided that the modification of the cable and added complexity of the software required would be more time consuming than differencing the two inputs using the hardware methods described above.
+
+The low pass filters were added to the inputs of ADC5 after it was found that an unacceptable level of AC noise was being output by the electrometer. The level of noise was too high to be filtered in software, for reasons that will be discussed in Appendix D.
+
+\subsection*{Temperature Measurement}
+
+The AVR Butterfly features an onboard thermistor connected to ADC0. Reading ADC0 and applying the formula given in the AVR Butterfly User's Guide \cite{} results in a temperature measurement. This was useful in establishing a link between the changing chamber pressure and the temperature of the laboratory (see Appendix C).
+
+\subsection*{Power Supplies}
+Due to the presence of both analogue and digital electronics in the DAC/ADC box, three seperate supply voltages were required:
+\begin{enumerate}
+ \item Digital logic in the range $3 \to 4.5$V
+ \item Positive op-amp supply in the range $10 \to 15$V
+ \item Negative op-amp supply in the range $-10 \to -15$V
+\end{enumerate}
+
+Circuitry was designed which allowed two seperate single pole power supplies to be used for Digital logic and the op-amps. A dual 0-30V DC power supply has been used for both digital and analogue circuitry.
+
+\subsubsection*{Logic Power Supply}
+The AVR Butterfly runs off $3V < V_{cc} < 4.5V$ DC. Since $V_{cc}$ was also used as the reference voltage for the ADCs and DAC output, it was desirable that $V_{cc}$ be kept constant, despite the absolute level of the power supply. A $3.3V$ voltage regulator has been used for this purpose. The capacitor further smooths the output by shorting high frequency fluctuations to ground.
+
+When the DAC/ADC box was first constructed $V_{cc}$ was supplied by three $1.5V$ batteries. However, due to higher than expected power usage, and the unreliability of the voltage regulator as the input voltage fell below $4V$, inputs for an external power supply were later added.
+
+\begin{center}
+ \includegraphics[scale=0.70]{figures/logic_ps}
+ \captionof{figure}{Logic Power Supply}
+ \label{logic_ps.pdf}
+\end{center}
+
+\subsubsection*{Op-amp Power Supply}
+The DAC/ADC box circuitry involves several operational amplifiers (LF356), which require dual $\pm 10-15V$ supplies. As there were no dual $\pm$ power supplies available, a single $30V$ power supply was used, with the circuit shown in figure \ref{} used to produce $\pm 15V$ relative to ground.
+
+The buffer amplifier ensures that negligable current can flow from the power supply into the logic and ADC circuits, whilst the capacitor removes high frequency fluctuations of the power supply relative to ground.
+
+\subsection*{DAC Output}
+A commercial DAC board was used to produce the DAC output. The Microchip MCP4922 ET-Mini DAC is controlled by the AVR Butterfly using Motorola's Serial Peripheral Interface (SPI) Bus. The software used to implement SPI between the MCP4922 and the AVR Butterfly is discussed in Appendix D.
+
+The ET-Mini DAC can only be powered off $3V$ to $5V$. Using $V_{cc} = 3.3V$ means that the DAC output cannot exceed $V_{cc} = 3.3V$. For TCS, energies of up to $15eV$ are required, so amplification of the DAC output was clearly necessary. A simple non-inverting amplifier with a manually adjustable gain was used to amplify the DAC output by a factor of three. This output was then used to control a laboratory power supply to produce the full range of initial energies.
+
+\subsection*{RS-232 Communications}
+
+The AVR Butterfly features an onboard USART, which can be used both for programming and communication with the ATMega169 processor. The RS-232 communications requires only three wires; Recieve (RX), Transmit (TX) and a common ground.
+
+The requirement that the AVR Butterfly share a common ground with the controlling computer lead to increased noise through ground loops. This is discussed in more detail in Appendix D.
+
+Although the RS-232 is relatively simple to implement, which makes it ideal for non-proprietry microprocessor applications, most modern computers no longer feature RS-232 COM ports. Although a computer with COM ports was available at CAMSP, due to the extreme unreliability of this computer, it was quickly replaced with a laptop that did not possess COM ports, and a commercial RS-232 to USB converter was used to interface with the laptop.
+
+\pagebreak
+
+\section*{Appendix C - Pressure Monitoring}
+
+The pressure in the chamber was monitored by a ion gauge at low pressure (below $10^{-3}$ mbar), and a pirani gauge at high pressure. The gauge included a flurescent Liquid Crystal Display (LCD). In order to automate monitoring of pressure, a USB webcam was placed in front of the gauge LCD. Software was written using the Python Imaging Library (PIL) to convert the image produced by the webcam into a pressure reading. In this way, the pressure could be recorded as a function of time, independent from other measurements performed using the ADC/DAC control box.
+
+Figures \ref{pressure_a.jpg} to \ref{pressure_c.jpg} show the process by which an image taken with the webcam was converted into a pressure reading. The software first identifies bounding rectangles for each individual digit. These are then further subdivided into 7 segments. If enough pixels in a given segment match the colour LCD segments, then the segment can be identified as activated. The software then creates a string corresponding to the activated segments, and looks up the digit in a dictionary.
+
+\begin{center}
+ \includegraphics[scale=0.50]{figures/pressure_a.jpg}
+ \captionof{figure}{An unprocessed image}
+ \label{pressure_a.jpg}
+\end{center}
+
+\begin{center}
+ \includegraphics[scale=0.50]{figures/pressure_c.jpg}
+ \captionof{figure}{Individual digits identified}
+ \label{pressure_b.jpg}
+\end{center}
+
+\begin{center}
+ \includegraphics[scale=0.50]{figures/pressure_d.jpg}
+ \captionof{figure}{Activated segments (green) for a single digit}
+ \label{pressure_c.jpg}
+\end{center}
+
+\section*{Appendix D - Sources of Error}
+
+GROUND LOOOOOOPS!
+
+\section*{Appendix E - Software}
+
+No really, you don't want to know
+
+
+
+\end{document}
+
\linespread{1.3}
\usepackage{setspace}
\onehalfspacing
+ \parskip 10pt % sets spacing between paragraphs
+ %\renewcommand{\baselinestretch}{1.5} % Uncomment for 1.5 spacing between lines
+ %\parindent 0pt % sets leading space for paragraphs
+
%\usepackage{natbib}
\usepackage{makeidx}
\newpage
-%include{acknowledgments/Acknowledgments} % This is who you thank
+\include{acknowledgments/Acknowledgments} % This is who you thank
\newpage
-%\include{abstract/Abstract} % This is your thesis abstract
+\include{abstract/Abstract} % This is your thesis abstract
\pagenumbering{roman}
\newpage
\include{chapters/Introduction}
-\include{chapters/Theory} % This is chapter 1
+\include{chapters/Overview} % This is chapter 1
\include{chapters/Techniques} % This is chapter 2
% Appendices
\appendix
-\renewcommand\chaptername{Appendix}
-\chapter{READ AT YOUR OWN RISK}
-
+\include{appendices/achievements.tex}
+%\include{proposal/proposal.tex}
+%\renewcommand\chaptername{Appendix}
+%\chapter{Appendix}
+%\include{appendices/electron_optics}
+%\include{appendices/electron_gun_circuit}
+%\include{appendices/tcs_noise}
+%\include{appendices/data_aquisition}
-\include{appendices/tcs_noise}
-\include{appendices/electron_optics}
-\include{appendices/electron_gun_circuit}
-\include{appendices/data_aquisition}
%---------------------------------------------------------
\begin{titlepage}
-\title{Honours Thesis Title}
+\title{Preparation and Characterisation of Nanostructured Metal Films}
\author{Samuel Moore \\
{{\it Supervisors:} W/Prof Jim Williams, Prof Sergey Samarin}\\
{Honours Thesis submitted as part of the B.Sc. (Honours) degree} \\ {in the School of Physics, University of Western Australia}\\ \\}
-\date{Date of submission: --/--/2012}
+\date{Date of submission: 02/11/2012}
\maketitle
\end{titlepage}
\begin{titlepage}
-\title{Honours Thesis Title}
+\title{Preparation and Characterisation of Nanostructured Metal Films}
\author{Samuel Moore \\
{{\it Supervisors:} W/Prof Jim Williams, Prof Sergey Samarin}\\
{Honours Thesis submitted as part of the B.Sc. (Honours) degree} \\ {in the School of Physics, University of Western Australia}\\ \\}
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