Funding from the Australian Research Council Industrial Transformation Research Hubs Scheme (Project Number IH130100017) is gratefully acknowledged. Authors gratefully acknowledge the RMIT Microscopy and Microanalysis Facility (RMMF) for providing access to the characterisation instruments. This research was also undertaken on the Infrared Microscopectroscopy beamline at the Australian Synchrotron, Victoria, Australia.

1. Steel Samples
<ol>
	<li>Obtain steel samples of 1 mm thickness from a commercial supplier. 
	NOTE: Samples were coated with either polyester or polyester coated with silica nanoparticles.</li>
	<li>Expose samples to sunlight at Rockhampton, Queensland, Australia: collect samples after one-year and five-year intervals over a total 5-year period. Cut sample panels into round discs of 1 cm diameter using hole puncher.</li>
	<li>Prior to surface characterization, rinse samples with double-distilled water, and then dry using nitrogen gas (99.99%). Keep all samples in air-tight containers to prevent any air contaminants adsorbing to the surface (Figure 1).</li>
</ol>
<img alt="Figure 1" src="/files/ftp_upload/54309/54309fig1.jpg" /> 
Figure 1. Preparation of metal discs with polyester-based coating. Samples were stored in containers until required. <a href="http://cloudfront.jove.com/files/ftp_upload/54309/54309fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
2. Chemical and Physicochemical Characterization of Surfaces
<ol>
	<li>Analyze surface chemistry using X-ray photoelectron spectroscopy.
	<ol>
		<li>Perform X-ray photoelectron spectrometry (XPS) using a monochromatic X-ray source (Al K&#945;, h&#957; = 1486.6 eV) operating at 150 W. 
		NOTE: Spot size of utilized X-ray beam is 400 &#181;m in diameter.</li>
		<li>Load samples on the sample plate. Place the sample plate into vacuum chamber of XPS then pump the chamber. Wait for the vacuum in the chamber to reach ~1 &#215; 10-9 mbar.</li>
		<li>In the photoelectron spectroscopy software, press the option of &#34;Flood Gun&#34; to flood the samples with low-energy electrons to counteract surface charging.</li>
		<li>Press &#34;Insert&#34;&#62;&#34;Point&#34;&#62;&#34;Point&#34; to insert an analysis point. 
		NOTE: This will be a location at which analysis is performed. Enable the auto height function to obtain the best height for acquisition.</li>
		<li>Press &#34;Insert&#34;&#62;&#34;Spectrum&#34;&#62;&#34;Multi Spectrum&#34; to add scans to this point. 
		NOTE: This will open a window with a periodic table; select an element by clicking on it to highlight it.</li>
		<li>After setting up the experiments, press the &#34;Play&#34; command to proceed the scans.</li>
		<li>Press &#34;Peak Fit&#34; command then press &#34;Add Peak&#34; and &#34;Fit All Level&#34; commands to resolve the chemically distinct species in the high-resolution spectra. 
		NOTE: This step will acquire the Shirley algorithm to remove the background and Gaussian-Lorentzian fitting to deconvolute the spectra19.</li>
		<li>Select all high-resolution and survey spectra. Press &#34;Charge Shift&#34; option to correct spectra using the hydrocarbon component of the C 1s peak (binding energy 285.0 eV) as a reference.</li>
		<li>After charge correction, press &#34;Export&#34; option to generate the data table of the relative atomic concentration of elements on the basis of the peak area.</li>
	</ol>
	</li>
	<li>Surface chemistry 
	NOTE: Analyze surface chemistry using attenuated total reflection infrared micro-spectroscopy (ATR-IR) on the infrared (IR) spectroscopy beamline at the Australian Synchrotron as following:
	<ol>
		<li>Load samples on the stage of microscope. Open a &#34;Start Video Assisted Measurement&#34; or &#34;Start Measurement without 3D&#34; option. Turn &#34;VIS&#34; mode on. Use the objective to focus on sample surface. Press &#34;Snapshot/Overview&#34; to take desired images. 
		NOTE: 0.5 mm thick CaF2plate can be used as the background.</li>
		<li>Change the ATR objective to the sample. Carefully move the stage to place a 45&#176; multi-reflection germanium crystal (refractive index of 4) 1-2 mm above surfaces. Right-click on the Live Video window. Press &#34;Start Measurement&#34;&#62;&#34;Change Measurement Parameters&#34;. Choose the option &#34;Never use existing BG for all positions&#34;. 
		NOTE: This will choose not to take background spectra for every measurement point.</li>
		<li>Draw a map on video screen to choose the area of interest. Press a red aperture square and choose &#34;Aperture&#34;&#62;&#34;Change Aperture&#34;. Change the actual &#34;Knife Edge Aperture&#34; settings to X = 20 &#181;m and Y = 20 &#181;m.</li>
		<li>Right-click on the newly sized aperture square and go to &#34;Aperture&#34;&#62; &#34;Set all Apertures to selected Apertures&#34;. Press &#34;Measurement&#34; icon to start the scans. Save the data. 
		NOTE: The refractive index of Ge crystal is 4, so an aperture of 20 &#181;m &#215; 20 &#181;m will define the spot size of 5 &#181;m &#215; 5 &#181;m. This step will allow setting up FTIR mapping with an aperture of 20 by 20 &#181;m, which corresponds to a 5 &#181;m by 5 &#181;m spot through the crystal across a maximum wavenumber range of 4,000-850 cm-1.</li>
		<li>Open master file using spectroscopy software. Choose the peak of interest on IR spectra. Right-click on the peak of interest. Choose &#34;Integration&#34;&#62;&#34;Integration&#34;. It will allow creating 2D false color maps</li>
	</ol>
	</li>
	<li>Surface wettability measurements 
	NOTE: Perform wettability measurement using a contact angle goniometer equipped with a nanodispenser19.
	<ol>
		<li>Place the sample on the stage. Adjust the position of the microsyringe assembly so that the bottom of the needle appears about a fourth of a way down in the Live video window screen.</li>
		<li>Raise the sample using z-axis until distance between the sample and surface is about 5 mm. Move the syringe down until a droplet of double distilled water touches the surface. Move the syringe up to its original position.</li>
		<li>Press the &#34;Run&#34; command to record the water droplet impacting on the surface for a 20 sec period using a monochrome CCD Camera which is integrated with hardware.</li>
		<li>Press the &#34;Stop&#34; command to acquire the series of images.</li>
		<li>Press &#34;Contact Angle&#34; command to measure contact angles from acquired images. Repeat the contact angle measurements at three random locations for each sample.</li>
	</ol>
	</li>
</ol>
3. Visualization of the Surface Topography
<ol>
	<li>Optical profiling measurement. 
	NOTE: The instrument is operated under the white light vertical scanning interferometry mode.
	<ol>
		<li>Place samples on the stage of the microscope. 
		NOTE: Ensure there is a sufficient gap (e.g., &#62;15 mm) between objective lens and the stage.</li>
		<li>Focus on surface using the 5&#215; objectives by controlling z-axis until the fringes appear on the screen. Press &#34;Auto&#34; command to optimize the intensity. Press &#34;Measurement&#34; command to initiate the scanning. Save the master files.</li>
		<li>Repeat the step 3.1.2 for 20&#215; and 50&#215; objectives.</li>
		<li>Prior to statistical roughness analyses, press &#34;Remove Tilt&#34; option to remove the surface waviness. Press &#34;Contour&#34; option to analyze the roughness parameters. Click on &#34;3Di&#34; option to generate three-dimensional images of optical profiling files using compatible software20.</li>
	</ol>
	</li>
	<li>Atomic force microscopy
	<ol>
		<li>Place samples on steel discs. Insert the steel discs into magnetic holder.</li>
		<li>Perform AFM scans in tapping mode21. Mechanically load phosphorus doped silicon probes with a spring constant of 0.9 N/m, tip curvature with radius of 8 nm and a resonance frequency of &#8764;20 kHz for surface imaging.</li>
		<li>Manually adjust the laser reflection on the cantilever. Choose &#34;Auto Tune&#34; command then press &#34;Tune&#34; command to tune the AFM cantilever to reach the optimum resonance frequency reported by the manufacturer.</li>
		<li>Focus on the surface. Move the tips close to sample surface. Click on Engage command to engage AFM tips on surfaces.</li>
		<li>Type &#34;1 Hz&#34; into scanning speed box. Choose the scanning areas. Press &#34;Run&#34; command to perform scan. Repeat the scanning at least for ten areas of each of five samples of each condition.</li>
		<li>Choose the leveling option to process the resulting topographical data. Save the master files.</li>
		<li>Open the compatible AFM software. Load the AFM master file. Press &#34;Leveling&#34; command to remove the tilting of surfaces. Press &#34;Smoothen&#34; command to remove the background.</li>
		<li>Press &#34;Statistical Parameters Analysis&#34; to generate the statistical roughness 21.</li>
	</ol>
	</li>
</ol>
4. Statistical Analysis
<ol>
	<li>Express the results in terms of mean value and its standard deviation. Perform statistical data processing using paired Student&#39;s two-tailed t-tests to evaluate the consistency of results. Set p-value at &#60;0.05 indicating level of statistical significance.</li>
</ol>

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The authors have nothing to disclose.

Polyester coatings have been widely used to protect steel substrata from the corrosion that would occur on an uncoated surface due to the accumulation of moisture and pollutants. The application of polyester coatings can protect the steel from corrosion; however the longer-term effectiveness of these coatings is compromised if they are exposed to high levels of ultraviolet light under humid conditions, as occurs in tropical climates. Silica nanoparticles can be applied to the surface of the polyester to improve the robus...

Environmental corrosion of metals in the environment is both prevalent and costly1-3. A recent study conducted by the Australasian Corrosion Association (ACA) reported that corrosion of metals resulted in a yearly cost of $982 million, which was directly associated with the degradation of assets and infrastructure through metallic corrosion within the water industry4. From an international perspective, the World Corrosion Organization estimated that metallic corrosion was responsible for a direct cost of $3.3 trillion, over 3% of the world's GDP5. The process of galvanizing as a corrosion preventative method has been widely used to increase the lifespan of steel material6. In humid and subtropical climates, however, water tends to condense into small pockets or grooves within the surface of the galvanized steel, leading to the acceleration of corrosion rates through pit corrosion7,8. Thermosetting polymer coatings based on polyesters have been developed to coat the galvanized steel substrata increasing their ability to withstand humid weathering conditions for items such as satellite dishes, garden furniture, air-conditioning units or agricultural construction equipment9-11. Unfortunately polymer coatings on steel surfaces have been found to be considerably adversely affected by the presence of high levels of ultraviolet (uv) radiation12-14. Coatings comprised of silica nanoparticles (SiO2) spread over a polymer layer have been widely used with a view to increasing their corrosion-, wear-, tear- and degradation-resistance15,16. The tendency of the protective polymeric coatings to form pores and cracks can be reduced by incorporating nanoparticles (NPs), which contribute to the passive obstruction of corrosion initiation17,18. Also, the mechanical stability of the protective polymeric layer can be improved by NPs inclusion. However, these coatings act as passive physical barriers and, in comparison to the galvanization approach, cannot inhibit corrosion propagation actively.
An in-depth understanding of the effect that high-levels of ultraviolet light exposure under humid conditions upon these metal coatings is yet to be obtained. In this paper, a wide range of surface analytical techniques, including X-ray photoelectron spectroscopy (XPS), attenuated total reflection infrared micro-spectroscopy (ATR IR), contact angle goniometry, optical profiling and atomic force microscopy (AFM) will be employed to examine the changes in the surface of steel coatings prepared from polyester- and silica nanoparticle-coated polyester (silica nanoparticles/polyester) after exposure to sunlight. Furthermore, the aim of this work is to give a concise, practical overview of the overall characterization techniques to examine weathered samples.

<table border="0" cellpadding="0" cellspacing="0" width="1044">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="41">
			<td height="41" style="height:41px;width:263px;">polyester-coated steel 
			silica nanoparticle-polyester coated steel substrata</td>
			<td style="width:231px;">BlueScope Steel</td>
			<td style="width:163px;"></td>
			<td style="width:387px;">Samples provided by company</td>
		</tr>
		<tr height="26">
			<td height="26" style="height:26px;width:263px;">Millipore PetriSlideTM&#160;</td>
			<td style="width:231px;">Fisher Scientific</td>
			<td style="width:163px;">PDMA04700</td>
			<td>Storing samples</td>
		</tr>
		<tr height="49">
			<td height="49" style="height:49px;width:263px;">Thermo ScientificTM K-alpha 
			X-ray Photoelectron Spectrometer</td>
			<td>Thermo Fisher Scientific, Inc.</td>
			<td>IQLAADGAAFFACVMAHV</td>
			<td>Acquire XPS spectra</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">Avantage Data System</td>
			<td>Thermo Fisher Scientific, Inc.</td>
			<td>IQLAADGACKFAKRMAVI</td>
			<td>Analyse XPS spectra</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">A Bruker Hyperion 2000 microscope&#160;</td>
			<td style="width:231px;">Bruker Corporation</td>
			<td style="width:163px;"></td>
			<td>Synchrotron integrated instrument</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Bruker Opus v. 7.2</td>
			<td style="width:231px;">Bruker Corporation</td>
			<td style="width:163px;"></td>
			<td>ATR-IR analysis software</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">Contact angle goniometer, FTA1000c</td>
			<td>First Ten &#197;ngstroms Inc., VA, USA</td>
			<td style="width:163px;"></td>
			<td>Measuring the wettability of surfaces</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">FTA v. 2.0</td>
			<td>First Ten &#197;ngstroms Inc., VA, USA</td>
			<td style="width:163px;"></td>
			<td>Anaylyzing water contact angle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Optical profiler, Wyko NT1100&#160;</td>
			<td>Bruker Corporation</td>
			<td style="width:163px;"></td>
			<td>Measure surface topography</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Innova atomic force microscope&#160;</td>
			<td>Bruker Corporation</td>
			<td style="width:163px;"></td>
			<td>Measure surface topography</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:263px;">Phosphorus doped silicon probes, MPP-31120-10</td>
			<td>Bruker Corporation</td>
			<td style="width:163px;"></td>
			<td>AFM probes</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Gwyddion software</td>
			<td style="width:231px;">http://gwyddion.net/</td>
			<td style="width:163px;"></td>
			<td>Software used to measure optical profiling and AFM data</td>
		</tr>
	</tbody>
</table>

the evolution of silica nanoparticle-polyester coatings on surfaces exposed to sunlight

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO&#903;, -H2C&#903;, -O&#903;, -CO&#903; radicals. During the degradation process, CO and CO2 were also produced.

The coated steel samples that had been subjected to exposure to the sunlight for either one or five years were collected, and water contact angle measurements were carried out to determine whether the exposure had resulted in a change in the surface hydrophobicity of the surface (Figure 2).
<img alt="Figure 2" src="/files/ftp_upload/54309/54309fig2.jpg" /> 
Figure 2. Wettability variation of surfaces with polyester or silica nanopa...

Watch this Scientific Journal Video about The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight at JoVE.com

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

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9.5K Views.  Swinburne University of Technology. Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

Video: The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Investigation of Early Plasma Evolution Induced by Ultrashort Laser Pulses

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a significant role in laser-material interaction, especially in the air environment1-11.
Early plasma evolution has been captured through pump-probe shadowgraphy1-3 and interferometry1,4-7. However, the studied time frames and applied laser parameter ranges are limited. For example, direct examinations of plasma front locations and electron number densities within a delay time of 100 picosecond (ps) with respect to the laser pulse peak are still very few, especially for the ultrashort pulse of a duration around 100 femtosecond (fs) and a low power density around 1014 W/cm2. Early plasma generated under these conditions has only been captured recently with high temporal and spatial resolutions12. The detailed setup strategy and procedures of this high precision measurement will be illustrated in this paper. The rationale of the measurement is optical pump-probe shadowgraphy: one ultrashort laser pulse is split to a pump pulse and a probe pulse, while the delay time between them can be adjusted by changing their beam path lengths. The pump pulse ablates the target and generates the early plasma, and the probe pulse propagates through the plasma region and detects the non-uniformity of electron number density. In addition, animations are generated using the calculated results from the simulation model of Ref. 12 to illustrate the plasma formation and evolution with a very high resolution (0.04 ~ 1 ps).
Both the experimental method and the simulation method can be applied to a broad range of time frames and laser parameters. These methods can be used to examine the early plasma generated not only from metals, but also from semiconductors and insulators.

An experimental method to examine the early plasma evolution induced by ultrashort laser pulses is described. Using this method, high quality images of early plasma are obtained with high temporal and spatial resolutions. A novel integrated atomistic model is used to simulate and explain the mechanisms of early plasma.

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a ...

Fabrication of Silica Ultra High Quality Factor Microresonators

Whispering gallery resonant cavities confine light in circular orbits at their periphery.1-2 The photon storage lifetime in the cavity, quantified by the quality factor (Q) of the cavity, can be in excess of 500ns for cavities with Q factors above 100 million. As a result of their low material losses, silica microcavities have demonstrated some of the longest photon lifetimes to date1-2. Since a portion of the circulating light extends outside the resonator, these devices can also be used to probe the surroundings. This interaction has enabled numerous experiments in biology, such as single molecule biodetection and antibody-antigen kinetics, as well as discoveries in other fields, such as development of ultra-low-threshold microlasers, characterization of thin films, and cavity quantum electrodynamics studies.3-7
The two primary silica resonant cavity geometries are the microsphere and the microtoroid. Both devices rely on a carbon dioxide laser reflow step to achieve their ultra-high-Q factors (Q&gt;100 million).1-2,8-9 However, there are several notable differences between the two structures. Silica microspheres are free-standing, supported by a single optical fiber, whereas silica microtoroids can be fabricated on a silicon wafer in large arrays using a combination of lithography and etching steps. These differences influence which device is optimal for a given experiment.
Here, we present detailed fabrication protocols for both types of resonant cavities. While the fabrication of microsphere resonant cavities is fairly straightforward, the fabrication of microtoroid resonant cavities requires additional specialized equipment and facilities (cleanroom). Therefore, this additional requirement may also influence which device is selected for a given experiment.
Introduction
An optical resonator efficiently confines light at specific wavelengths, known as the resonant wavelengths of the device. 1-2 The common figure of merit for these optical resonators is the quality factor or Q. This term describes the photon lifetime (&tau;o) within the resonator, which is directly related to the resonator's optical losses. Therefore, an optical resonator with a high Q factor has low optical losses, long photon lifetimes, and very low photon decay rates (1/&tau;o). As a result of the long photon lifetimes, it is possible to build-up extremely large circulating optical field intensities in these devices. This very unique property has allowed these devices to be used as laser sources and integrated biosensors.10
A unique sub-class of resonators is the whispering gallery mode optical microcavity. In these devices, the light is confined in circular orbits at the periphery. Therefore, the field is not completely confined within the device, but evanesces into the environment. Whispering gallery mode optical cavities have demonstrated some of the highest quality factors of any optical resonant cavity to date.9,11 Therefore, these devices are used throughout science and engineering, including in fundamental physics studies and in telecommunications as well as in biodetection experiments. 3-7,12
Optical microcavities can be fabricated from a wide range of materials and in a wide variety of geometries. A few examples include silica and silicon microtoroids, silicon, silicon nitride, and silica microdisks, micropillars, and silica and polymer microrings.13-17 The range in quality factor (Q) varies as dramatically as the geometry. Although both geometry and high Q are important considerations in any field, in many applications, there is far greater leverage in boosting device performance through Q enhancement. Among the numerous options detailed previously, the silica microsphere and the silica microtoroid resonator have achieved some of the highest Q factors to date.1,9 Additionally, as a result of the extremely low optical loss of silica from the visible through the near-IR, both microspheres and microtoroids are able to maintain their Q factors over a wide range of testing wavelengths.18 Finally, because silica is inherently biocompatible, it is routinely used in biodetection experiments.
In addition to high material absorption, there are several other potential loss mechanisms, including surface roughness, radiation loss, and contamination loss.2 Through an optimization of the device size, it is possible to eliminate radiation losses, which arise from poor optical field confinement within the device. Similarly, by storing a device in an appropriately clean environment, contamination of the surface can be minimized. Therefore, in addition to material loss, surface scattering is the primary loss mechanism of concern.2,8
In silica devices, surface scattering is minimized by using a laser reflow technique, which melts the silica through surface tension induced reflow. While spherical optical resonators have been studied for many years, it is only with recent advances in fabrication technologies that researchers been able to fabricate high quality silica optical toroidal microresonators (Q&gt;100 million) on a silicon substrate, thus paving the way for integration with microfluidics.1
The present series of protocols details how to fabricate both silica microsphere and microtoroid resonant cavities. While silica microsphere resonant cavities are well-established, microtoroid resonant cavities were only recently invented.1 As many of the fundamental methods used to fabricate the microsphere are also used in the more complex microtoroid fabrication procedure, by including both in a single protocol it will enable researchers to more easily trouble-shoot their experiments.

We describe the use of a carbon dioxide laser reflow technique to fabricate silica resonant cavities, including free-standing microspheres and on-chip microtoroids. The reflow method removes surface imperfections, allowing long photon lifetimes within both devices. The resulting devices have ultra high quality factors, enabling applications ranging from telecommunications to biodetection.

Whispering gallery resonant cavities confine light in circular orbits at their periphery.1-2 The photon storage lifetime in the cavity, quantified by the ...

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

High-speed Particle Image Velocimetry Near Surfaces

Multi-dimensional and transient flows play a key role in many areas of science, engineering, and health sciences but are often not well understood. The complex nature of these flows may be studied using particle image velocimetry (PIV), a laser-based imaging technique for optically accessible flows. Though many forms of PIV exist that extend the technique beyond the original planar two-component velocity measurement capabilities, the basic PIV system consists of a light source (laser), a camera, tracer particles, and analysis algorithms. The imaging and recording parameters, the light source, and the algorithms are adjusted to optimize the recording for the flow of interest and obtain valid velocity data. 
Common PIV investigations measure two-component velocities in a plane at a few frames per second. However, recent developments in instrumentation have facilitated high-frame rate (&gt; 1 kHz) measurements capable of resolving transient flows with high temporal resolution. Therefore, high-frame rate measurements have enabled investigations on the evolution of the structure and dynamics of highly transient flows. These investigations play a critical role in understanding the fundamental physics of complex flows.
A detailed description for performing high-resolution, high-speed planar PIV to study a transient flow near the surface of a flat plate is presented here. Details for adjusting the parameter constraints such as image and recording properties, the laser sheet properties, and processing algorithms to adapt PIV for any flow of interest are included.

A procedure for studying transient flows near boundaries using high-resolution, high-speed particle image velocimetry (PIV) is described here. PIV is a non-intrusive measurement technique applicable to any optically accessible flow by optimizing several parameter constraints such as the image and recording properties, the laser sheet properties, and analysis algorithms.

Multi-dimensional and transient flows play a key role in many areas of science, engineering, and health sciences but are often not well understood. The ...

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

High-resolution Thermal Micro-imaging Using Europium Chelate Luminescent Coatings

Micro-electronic devices often undergo significant self-heating when biased to their typical operating conditions. This paper describes a convenient optical micro-imaging technique which can be used to map and quantify such behavior. Europium thenoyltrifluoroacetonate (EuTFC) has a 612 nm luminescence line whose activation efficiency drops strongly with increasing temperature, due to T-dependent interactions between the Eu3+ ion and the organic chelating compound. This material may be readily coated on to a sample surface by thermal sublimation in vacuum. When the coating is excited with ultraviolet light (337 nm) an optical micro-image of the 612 nm luminescent response can be converted directly into a map of the sample surface temperature. This technique offers spatial resolution limited only by the microscope optics (about 1 micron) and time resolution limited by the speed of the camera employed. It offers the additional advantages of only requiring comparatively simple and non-specialized equipment, and giving a quantitative probe of sample temperature.

Europium thenoyltrifluoroacetonate (EuTFC) has an optical luminescence line at 612 nm, whose activation efficiency decreases strongly with temperature. If a sample coated with a thin film of this material is micro-imaged, the 612 nm luminescent response intensity may be converted into a direct map of sample surface temperature.

Micro-electronic devices often undergo significant self-heating when biased to their typical operating conditions. This paper describes a convenient ...

Evanescent Field Based Photoacoustics: Optical Property Evaluation at Surfaces

Here, we present a protocol to estimate material and surface optical properties using the photoacoustic effect combined with total internal reflection. Optical property evaluation of thin films and the surfaces of bulk materials is an important step in understanding new optical material systems and their applications. The method presented can estimate thickness, refractive index, and use absorptive properties of materials for detection. This metrology system uses evanescent field-based photoacoustics (EFPA), a field of research based upon the interaction of an evanescent field with the photoacoustic effect. This interaction and its resulting family of techniques allow the technique to probe optical properties within a few hundred nanometers of the sample surface. This optical near field allows for the highly accurate estimation of material properties on the same scale as the field itself such as refractive index and film thickness. With the use of EFPA and its sub techniques such as total internal reflection photoacoustic spectroscopy (TIRPAS) and optical tunneling photoacoustic spectroscopy (OTPAS), it is possible to evaluate a material at the nanoscale in a consolidated instrument without the need for many instruments and experiments that may be cost prohibitive.

Here we present a protocol to estimate material and surface optical properties using the photoacoustic effect combined with total internal reflection. This technique evanescent field-based photoacoustics can be used to create a photoacoustic metrology system to estimate materials&#39; thicknesses, bulk and thin film refractive indices, and explore their optical properties.

Here, we present a protocol to estimate material and surface optical properties using the photoacoustic effect combined with total internal reflection. ...

Pool-Boiling Heat-Transfer Enhancement on Cylindrical Surfaces with Hybrid Wettable Patterns

In this study, pool-boiling heat-transfer experiments were performed to investigate the effect of the number of interlines and the orientation of the hybrid wettable pattern. Hybrid wettable patterns were produced by coating superhydrophilic SiO2 on a masked, hydrophobic, cylindrical copper surface. Using de-ionized (DI) water as the working fluid, pool-boiling heat-transfer studies were conducted on the different surface-treated copper cylinders of a 25-mm diameter and a 40-mm length. The experimental results showed that the number of interlines and the orientation of the hybrid wettable pattern influenced the wall superheat and the HTC. By increasing the number of interlines, the HTC was enhanced when compared to the plain surface. Images obtained from the charge-coupled device (CCD) camera indicated that more bubbles formed on the interlines as compared to other parts. The hybrid wettable pattern with the lowermost section being hydrophobic gave the best heat-transfer coefficient (HTC). The experimental results indicated that the bubble dynamics of the surface is an important factor that determines the nucleate boiling.

Pool-boiling heat-transfer experiments were carried out to observe the effects of hybrid wettable patterns on the heat-transfer coefficient (HTC). The parameters of investigation are the number of interlines and the pattern orientation of the modified wettable surface.

In this study, pool-boiling heat-transfer experiments were performed to investigate the effect of the number of interlines and the orientation of the ...

Evaluation of Commercial-Off-The-Shelf Wrist Wearables to Estimate Stress on Students

Wearable commercial-off-the-shelf (COTS) devices have become popular during the last years to monitor sports activities, primarily among young people. These devices include sensors to gather data on physiological signals such as heart rate, skin temperature or galvanic skin response. By applying data analytics techniques to these kinds of signals, it is possible to obtain estimations of higher-level aspects of human behavior. In the literature, there are several works describing the use of physiological data collected using clinical devices to obtain information on sleep patterns or stress. However, it is still an open question whether data captured using COTS wrist wearables is sufficient to characterize the learners' psychological state in educational settings. This paper discusses a protocol to evaluate stress estimation from data obtained using COTS wrist wearables. The protocol is carried out in two phases. The first stage consists of a controlled laboratory experiment, where a mobile app is used to induce different stress levels in a student by means of a relaxing video, a Stroop Color and Word test, a Paced Auditory Serial Addition test, and a hyperventilation test. The second phase is carried out in the classroom, where stress is analyzed while performing several academic activities, namely attending to theoretical lectures, doing exercises and other individual activities, and taking short tests and exams. In both cases, both quantitative data obtained from COTS wrist wearables and qualitative data gathered by means of questionnaires are considered. This protocol involves a simple and consistent method with a stress induction app and questionnaires, requiring a limited participation of support staff.

A protocol to evaluate solutions based on commercial-off-the-shelf (COTS) wrist wearables to estimate stress in students is proposed. The protocol is carried out in two phases, an initial laboratory-based stress induction test, and a monitoring stage taking place in the classroom while the student is performing academic activities.

Wearable commercial-off-the-shelf (COTS) devices have become popular during the last years to monitor sports activities, primarily among young people. ...