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57 %\title{\bf Characterisation of nanostructured thin films}
58 %\author{Sam Moore\\ School of Physics, University of Western Australia}
63 B.Sc. (Hons) Physics Project \par
64 {\bf \Large Thesis} \par
66 School of Physics, University of Western Australia \\
69 \section*{Characterisation of Nanostructured Thin Films}
70 {\bf \emph{Keywords:}} surface plasmons, nanostructures, spectroscopy, metallic-blacks \\
71 {\bf \emph{Supervisers:}} W/Prof. James Williams (UWA), Prof. Sergey Samarin (UWA) \\
76 \section*{Acknowledgements}
82 \item Workshop (for producing electron gun mount?)
83 \item Peter Hammond (?)
86 \section{Introduction}
88 \item Waffle about motivation for the project
90 \item Metal-Black films may have application for ... something.
92 \item Radiometer vanes, IR detectors
93 \item Number of applications where high absorbance into IR is required
94 \item These have all been studied before though.
96 \item The electron spectra of metal-blacks have not yet been examined.
97 \item Remarkable difference between Metal-Black films (bad vacuum) and normal metal films (UHV)
99 \item No (detailed/satisfactory) explanation (that I can find...) for difference
101 \item Talk about plasmonic based computing? Moore's law? Applications to thin film solar cells?
104 \item Specific aims of project
106 \item Surface density of states / band structure of Black-Au films using TCS (The main aim)
107 \item Identification of plasmonic effects in Black-Au films (?) (If they even exist!)
109 \item Identify plasmonic effects in Au and Ag films with Ellipsometry (this is fairly simple to do)
111 \item Combination of Ellipsometry and TCS to characterise thin films (not just Black-Au)
113 \item Ie: How can one technique be used to support the other?
116 \item Structure of thesis
119 \section{Overview of Theory}
120 Summarise the literature, refer to past research etc
122 \subsection{Electron structure of surface}
124 \item Overview of electron spectrum properties
126 \item Density of states $n(E)$
127 \item Energy band structure $E(\vect{k})$
129 \item Properties of surface region
131 \item Difference between potential of surface and bulk
133 \item Change between the two limits in the ``near-surface'' region
135 \item Theoretical models for the potential, 1D vs 3D
137 \item Simplest case is a step potential.
138 \item Various improvements on this model, discussed in Komolov's book.
140 \item Possibly adapt CQM project to model these potentials, if I get time
143 \item Limitations of theoretical models
145 \item Real surface is not a step potential
146 \item Adsorption of foreign particles onto the surface also plays a large role in determining the electron spectrum.
149 \item Main reference: Komolov "Total Current Spectroscopy"
150 \item "Solid State Physics" textbooks and "Electron Spectroscopy" textbooks
153 \subsection{Plasmonics}
154 I really think I should actually find plasmonic effects before writing too much about them...
156 \item Charge density oscillations
157 \item Surface and bulk plasmons
159 \item Review article from T.W.H Oates et al about using Ellipsometry to characterise plasmonic effects
162 \subsection{Metallic-Black Thin Films}
164 \item How they are made (bad vacuum, in air or a noble gas)
166 \item If made in air, there are usually tungsten oxides present (from filament). Refer to paper by Pfund.
168 \item Structural difference between Black-Au and ``Shiny'' (need a better term) Au
170 \item Can include electron microscopy images?
171 \item An actual photograph of a Black-Au film? Not necessary?
173 \item Pfund (earliest publisher, preparation and general properties)
174 \item Louis Harris (most research in 50s and 60s)
176 \item L. Harris mostly did transmission spectroscopy in the far infra red (well beyond the ellipsometer and Ocean Optics spectrometer ranges)
177 \item The really crappy measurements I did with the Ocean Optics spectrometer seem to agree with these measurements
179 \item L. Harris' $\lambda$ has a range of 1nm to $100\mu$m; my measurements are only to $1\mu$m
180 \item Agreement in first $1\mu$m anyway
181 \item I should probably re-do those measurements with a less crappy setup, if I actually want to use them
183 \item Harris related the optical properties to the structure of the film (condensor strands) via the electronic properties
185 \item Plasmonic effects - Deep R. Panjwani (honours thesis)
187 \item Not sure if I can use an honours thesis as a reference.
188 \item Concluded that surface plasmon resonance in Black-Au film on solar cells lead to increase in solar cell efficiency
189 \item Used simulation that modelled Black-Au film as spherical balls to show E field increased by plasmon resonance
191 \item Was this model appropriate? Black-Au is more ``smoke'' or ``strand'' like according to other references. Images also do not show ``blob'' like structure.
193 \item Need to read this reference more thoroughly
197 \section{Experimental Techniques}
199 \subsection{Preparation of samples}
201 \item Black-Au - 1e-2 mbar vacuum
202 \item ``Shiny'' - 1e-6 / 1e-7
203 \item Current of ~3.5A through W wire filament spot welded onto Ta strips in turn spot welded to Mo posts
204 \item Voltage through filament is ~1 V; quote the power?
205 \item Filament isotropically coats sample with desired material.
206 \item Possibly get a curve of Au thickness estimated with Ellipsometry vs exposure time?
208 \item Probably too much work and too unreliable
209 \item Maybe do it, but only use 2/3 data points
214 \subsection{Total Current Spectroscopy}
216 \item Overview of technique
218 \item Low energy beam of electrons incident on sample
219 \item Measure slope of resulting I-V curve
220 \item Relate to density of states and electron band structure (Komolov chapter 3.2)
222 \item Description of apparatus
224 \item Electron gun and filament
225 \item Electron gun control box
226 \item ADC/DAC control box and data processing
228 \item Photographs vs Diagrams
230 \item Prefer diagrams to photographs
231 \item Especially for the ADC/DAC control box circuit. Because it looks like a horrible mess.
235 \subsection{Ellipsometry and Transmission Spectroscopy}
237 \item Overview of techniques
238 \item Description of apparatus (use VASE manual)
239 \item Ocean Optics spectrometer? Usable?
240 \item Application of Ellipsometry to finding plasmonic effects
242 \item Surface plasmons = E oscillation parallel to surface $\implies$ only $p$ component of light excites plasmons
246 \section{Experimental Results and Discussion}
247 \subsection{TCS Measurements}
250 \item TCS for Si + Au
251 \item TCS for Si + Black-Au
252 \item Affect of preparation pressure on TCS for Si + Black-Au
253 \item Repeat for Si + Ag and Si + Black-Ag (?)
256 \subsection{Ellipsometric Measurements}
258 \item Ellipsometry to estimate thickness of SiO2 layer on Si
259 \item Estimate thickness of Au/Ag on Si+SiO2
260 \item Ellipsometric measurements of Si+Black-Au/Ag
262 \item Modelling procedures to characterise Black-Au/Ag
264 \item Ellipsometric measurements of Glass+Black-Au/Ag (?)
265 \item Transmission spectra of Glass+Black-Au/Ag from earlier in year (?)
268 \section{Achievements}
270 \item Deposition of thin films of Au and Black-Au in vacuum chamber
271 \item Ellipsometric and spectroscopic measurements on these films
272 \item Repurpose vacuum chamber for sample preparation and TCS experiments
273 \item Designed and built electronics for TCS experiments
275 \item Electron gun control box
278 \item Wrote software for data aquisition and data processing
281 \section{General notes}
284 \item Optimise setup of gun
286 \item Emission current. How much does it vary, why does it vary.
287 \item Why does Is/Ie curve shift with successive sweeps? Does sweep modify sample's surface?
288 \item Is sample holder acceptable? Are ceramic washers accumulating charge?
289 \item How do I tell when the setup is optimised...
290 ``The setup was optimised by looking for an S curve''. Very scientific.
291 \item The gun was focused on the phosphor screen... and then I turned it around, changing the distance from the gun to the sample. Brilliant.
293 \item Obtain TCS spectra for Si that compares well with literature
295 \item How to relate TCS spectrum to $n(E)$ and $E(\vect{k})$
297 \item Prepare Au films, obtain TCS spectra that compares with literature
298 \item Obtain TCS spectra of Black-Au films
299 \item Use results to compare properties of films with results from other methods in the literature
302 \item Oscilloscope measurements of inputs to ADC channels under controlled conditions
304 \item Expected values are +/-3mV due to ADC channel, +/-300mV due to 610B, +/-1mV due to 602
305 \item 610B and 602 will probably be worse because they are ancient
306 \item There is about 200mV of noise between the GND of the ADC box and the electron control box.
307 \item How to reduce ground loops? Not much I can do. Rack is now also grounded to water pipe, but this doesn't seem to make a difference.
309 \item Stupid 50Hz AC noise... how to reduce with filters and/or averaging
311 \item Create circuit diagrams for Electron gun circuit
312 \item Create circuit diagrams for ADC/DAC box
314 \item Simulate behaviour of circuit
315 \item Use of instrumentation amplifier on ADC5 to make off-ground measurements
316 \item Use of low pass filter on ADC5
318 \item Include references to all datasheets, etc
321 \item Base pressure with rotary pump? Was 1e-3 after 30 minutes at start of year, but probably introduced leaks since then
322 \item Lowest pressure achieved with turbo pump is 1.1e-7 mbar as of 25/07.
323 \item Viton gaskets on some seals. Copper on other.
326 \item View window (large, view of sample \& sputtering filaments)
327 \item Rotation manipulator \& sample mount
329 \item Filament flanges 1 (used earlier in year, not anymore) and 2
330 \item Inlet with leak valve (for introducing gases into chamber)
331 \item Vent valve on turbo pump
332 \item Electron gun flange
333 \item View window (small, view of back of electron gun)
339 \bibliographystyle{unsrt}
340 \bibliography{thesis}