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.

<html> 1. Stahlproben <ol><li> Erhalten Stahlproben von 1 mm Dicke von einem kommerziellen Anbieter. HINWEIS: Die Proben wurden entweder mit Polyester oder Polyester mit Silica - Nanopartikel beschichtet. </li><li> Expose Proben Sonnenlicht in Rockhampton, Queensland, Australien: sammeln Proben nach einem Jahr und alle fünf Jahre auf insgesamt 5-Jahres-Zeitraum. Schneiden Sie Musterplatten in runde Scheiben von 1 cm Durchmesser unter Verwendung von Lochstanze. </li><li> Vor Charakterisierung von Oberflächen gründlich Proben mit Wasser doppelt destilliert und dann trocknen Stickstoffgas (99,99%). Halten Sie alle Proben in luftdichten Behältern ohne Luftverunreinigungen zu verhindern , dass die Oberfläche zu adsorbieren (Abbildung 1). </li></ol><img alt="Abbildung 1" src="/files/ftp_upload/54309/54309fig1.jpg" /> Abbildung 1. Herstellung von Metallscheiben mit Polyesterbasis Beschichtung. Die Proben wurden in Behältern aufbewahrt , bis sie benötigt.om / files / ftp_upload / 54309 / 54309fig1large.jpg &quot;target =&quot; _ blank &quot;&gt; Bitte hier klicken, um eine größere Version dieser Figur zu sehen. 2. Chemische und physikalisch-chemische Charakterisierung von Oberflächen <ol><li> Analysieren der Oberflächenchemie Röntgenphotoelektronenspektroskopie. <ol><li> Führen Röntgenphotoelektronenspektroskopie (XPS) unter Verwendung eines monochromatischen Röntgenquelle (Al K &amp; agr;, h &amp; ngr; = 1486,6 eV) bei 150 W. Betriebs HINWEIS: Spot - Größe der verwendeten Röntgenstrahls ist 400 &amp; mgr; m im Durchmesser. </li><li> Laden Sie die Proben auf der Probenplatte. Platzieren Sie die Probenplatte in die Vakuumkammer des XPS dann die Kammer zu pumpen. Warten für das Vakuum in der Kammer ~ 1 × 10 -9 mbar zu erreichen. </li><li> In der Photoelektronenspektroskopie Software, drücken Sie die Option &quot;Flood Gun&quot;, die Proben mit niederenergetischen Elektronen zu fluten Oberflächenladung entgegen zu wirken. </li><li> Drücken Sie auf &quot;Einfügen&quot;&gt; &quot;Point&quot;&gt; &quot;Punkt&quot; eine Analyse poin einfügent. Hinweis: Dies wird eine Stelle , an der Analyse durchgeführt wird. Aktivieren Sie die Funktion Auto-Höhe die beste Höhe für den Erwerb zu erhalten. </li><li> Drücken Sie auf &quot;Einfügen&quot;&gt; &quot;Spectrum&quot;&gt; &quot;Multi Spectrum&quot; Scans zu diesem Punkt hinzuzufügen. HINWEIS: Dies ist ein Fenster mit einem Periodensystem geöffnet; ein Element auswählen, indem Sie auf, um es zu markieren. </li><li> Nach den Versuchen Einrichten, drücken Sie die &quot;Play&quot; Befehl, um die Scans zu gelangen. </li><li> Drücken Sie &quot;Peak Fit&quot; Befehl und drücken Sie &quot;Peak In&quot; und &quot;Alle Stufe anpassen&quot; Befehle, um die chemisch verschiedenen Arten in der hochauflösenden Spektren zu lösen. HINWEIS: Dieser Schritt wird den Shirley Algorithmus erwerben den Hintergrund zu entfernen und Gaussian-Lorentz - Fitting die Spektren 19 bis dekonvolutieren. </li><li> Wählen Sie alle hochauflösenden und Umfrage-Spektren. Drücken Sie &quot;Charge Shift&quot; Option Spektren zur Korrektur der hydroca mitrbon Komponente des C 1s-Peak (285,0 eV Bindungsenergie) als Referenz. </li><li> Nach Ladungskorrektur, drücken Sie &quot;Export&quot; Option, die Datentabelle der relativen Atomkonzentration von Elementen auf der Basis der Peakfläche zu erzeugen. </li></ol></li><li> Oberflächenchemie HINWEIS: Analysieren Chemie Oberfläche abgeschwächte Totalreflexion Infrarot - Mikrospektroskopie (ATR-IR) auf dem Infrarot (IR) -Spektroskopie - Strahlrohr an der Australian Synchrotron mit , wie folgend: <ol><li> Laden Sie die Proben auf der Bühne des Mikroskops. Öffnen Sie ein &quot;Start Video Assisted Measurement&quot; oder &quot;Start Messung ohne 3D&quot; Option. Turn &quot;VIS&quot; -Modus auf. Verwenden Sie das Ziel auf Probenoberfläche zu fokussieren. Drücken Sie auf &quot;Snapshot / Übersicht&quot; gewünschten Bilder zu nehmen. HINWEIS: 0,5 mm dicken CaF 2 - Platte kann als Hintergrund verwendet werden. </li><li> Ändern Sie die ATR Ziel auf die Probe. Vorsichtig die Bühne bewegen, um eine 45 ° Multi-Reflexion ger zu platzierenmanium Kristall (Brechungsindex von 4) 1-2 mm über Oberflächen. Rechtsklicken Sie auf das Live-Video-Fenster. Drücken Sie &quot;Start Messung&quot;&gt; &quot;Ändern Messparameter&quot;. Wählen Sie die Option &quot;Verwenden Sie niemals BG bestehenden für alle Positionen&quot;. Hinweis: das wird nicht wählen Hintergrundspektren für jeden Messpunkt zu nehmen. </li><li> Zeichnen Sie eine Karte auf Video-Bildschirm den Bereich von Interesse zu wählen. Drücken Sie eine rote Öffnung Quadrat und wählen Sie &quot;Aperture&quot;&gt; &quot;Ändern der Blende&quot;. Ändern Sie die eigentliche &quot;Knife Edge Aperture&quot; Einstellungen X = 20 &amp; mgr; m und Y = 20 &amp; mgr; m. </li><li> Rechtsklick auf die neu bemessen Öffnung Platz und gehen Sie zu &quot;Aperture&quot;&gt; &quot;Alle Apertures Set an ausgewählte Apertures&quot;. Drücken Sie &quot;Messung&quot; Symbol, um die Scans zu starten. Speichern Sie die Daten. HINWEIS: Der Brechungsindex von Ge - Kristall ist 4, so dass eine Öffnung von 20 &amp; mgr; m × 20 &amp; mgr; m wird die Punktgröße von 5 &amp; mgr; m × 5 &amp; mgr; m definieren. This Schritt wird die Einrichtung FTIR - Mapping mit einer Öffnung von 20 erlauben durch 20 um, die von 5 &amp; mgr; m Fleck durch den Kristall in einem maximalen Wellenzahlbereich von 4,000-850 cm zu einem 5 &amp; mgr; m entspricht - 1. </li><li> Offene Master-Datei-Spektroskopie-Software. Wählen Sie die Spitze des Interesses an IR-Spektren. Rechtsklicken Sie auf den Gipfel des Interesses. Wählen Sie &quot;Integration&quot;&gt; &quot;Integration&quot;. Es erlaubt 2D-Falschfarben Erstellen von Karten </li></ol></li><li> Oberflächenbenetzbarkeit Messungen HINWEIS: Führen Sie eine Messung der Benetzbarkeit mit einem Kontaktwinkel - Goniometer mit einem Nanodispenser 19 ausgestattet ist . <ol><li> Legen Sie die Probe auf der Bühne. Stellen Sie die Position der Mikroanordnung, so dass der Boden der Nadel etwa ein Viertel des Weges erscheint unten im Live-Video-Fenster-Bildschirm. </li><li> Erhöhen Sie die Probe z-Achse bis Abstand zwischen der Probe und Oberfläche mit etwa 5 mm beträgt. Bewegen Sie die Spritze, bis ein Tröpfchen von doub nach untenle destilliertes Wasser die Oberfläche berührt. Bewegen Sie die Spritze in seine ursprüngliche Position. </li><li> Drücken Sie den Befehl &quot;Ausführen&quot; die Wassertropfen auf der Oberfläche zu erfassen für eine 20 Sekunden Zeitraum auswirken mit einem Monochrom-CCD-Kamera, die mit Hardware integriert ist. </li><li> Drücken Sie die &quot;Stop&quot; Befehl, um die Serie von Bildern zu erwerben. </li><li> Drücken Sie auf &quot;Kontaktwinkel&quot; Dieser Befehl Kontaktwinkel von akquirierten Bildern messen. Wiederholen Sie die Kontaktwinkelmessungen an drei zufälligen Stellen für jede Probe. </li></ol></li></ol> 3. Visualisierung der Oberflächentopographie <ol><li> Optische Profilmessung. HINWEIS: Das Gerät wird unter dem weißen Licht vertikalen Scan - Interferometrie - Modus betrieben. <ol><li> Platz Proben auf der Bühne des Mikroskops. HINWEIS: Achten Sie auf eine ausreichende Lücke (zB&gt; 15 mm) zwischen Objektivlinse und der Bühne. </li><li> Konzentrieren Sie sich auf Oberfläche mit der5 × Ziele von z-Achse, bis die Streifen auf dem Bildschirm erscheinen zu steuern. Drücken Sie auf &quot;Auto&quot; Befehl, um die Intensität zu optimieren. Drücken Sie &quot;Messung&quot; Befehl den Scan zu starten. Speichern Sie die Master-Dateien. </li><li> Wiederholen Sie den Schritt 3.1.2 für 20 × und 50 × Ziele. </li><li> Vor der statistischen Analysen Rauheit, drücken Sie &quot;entfernen Tilt&quot; Option, um die Oberflächenwelligkeit zu entfernen. Drücken Sie &quot;Kontur&quot; Option, um die Rauheitsparametern zu analysieren. Klicken Sie auf &quot;3Di&quot; Option dreidimensionale Bilder von optischen Profildateien zu erzeugen mit kompatiblen Software 20. </li></ol></li><li> Rasterkraftmikroskopie <ol><li> Prüfmuster auf Stahlscheiben. Legen Sie die Stahlscheiben in Magnethalterung. </li><li> Führen Sie AFM - Scans im Tapping - Modus 21. Mechanisch Last Phosphor Silizium-Sonden mit einer Federkonstante von 0,9 N / m, Spitzenkrümmung mit einem Radius von 8 nm und einer Resonanzfrequenz von ~ 20 kHz für Oberflächen-Belichtungs dotiert. </li> &lt;li&gt; Manuelle Einstellung der Laserreflektion auf dem Ausleger. Wählen Sie &quot;Auto Tune&quot; Befehl und drücken Sie &quot;Tune&quot; Befehl, um die AFM Cantilever abzustimmen, die optimale Resonanzfrequenz vom Hersteller angegeben, zu erreichen. </li><li> Konzentrieren Sie sich auf der Oberfläche. Bewegen Sie die Spitzen der Nähe der Probenoberfläche. Klicken Sie auf Befehl Engage an AFM-Spitzen auf Oberflächen angreifen. </li><li> Geben Sie &quot;1 Hz&quot; in Abtastgeschwindigkeit Box. Wählen Sie die Scanbereiche. Drücken Sie Befehl &quot;Ausführen&quot; Scan durchführen. Wiederholen Sie das Scannen mindestens für zehn Bereiche jeweils fünf Proben jeder Bedingung. </li><li> Wählen Sie die Option Nivellierung des erhaltenen topographischen Daten zu verarbeiten. Speichern Sie die Master-Dateien. </li><li> Öffnen Sie die kompatiblen AFM-Software. Laden Sie die AFM-Master-Datei. Drücken Sie &quot;Leveling&quot; Befehl, um die Neigung der Oberflächen zu entfernen. Drücken Sie &quot;Smoothen&quot; Befehl, um den Hintergrund zu entfernen. </li><li> Drücken Sie die &quot;Statistische Parameter - Analyse&quot; zu erzeugen , die statistische Rauheit 21. </li></ol></li&gt; </ol> 4. Statistische Analyse <ol><li> Die Ergebnisse sind in Bezug auf Mittelwert und der Standardabweichung. Führen Sie statistische Datenverarbeitung unter Verwendung von gepaarte Student-two-tailed t- Tests , um die Konsistenz der Ergebnisse zu bewerten. Set p - Wert bei &lt;0,05 Anzeige statistische Signifikanzniveau. </li></ol>

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The authors have nothing to disclose.

Polyester-Beschichtungen wurden weit verbreitet Stahl substrata von der Korrosion zu schützen, die aufgrund der Ansammlung von Feuchtigkeit und Schadstoffe auf einer unbeschichteten Oberfläche auftreten würde. Die Anwendung von Polyester-Beschichtungen können den Stahl vor Korrosion zu schützen; aber die längerfristige Wirksamkeit dieser Beschichtungen beeinträchtigt wird, wenn sie auf ein hohes Maß an UV-Licht unter feuchten Bedingungen ausgesetzt sind, wie in tropischen Klimazonen auftritt. Silica-Nanopartikel...

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

Die Korrosion von metallischen Oberflächen ist weit verbreitet in der Umwelt und ist von großer Bedeutung in vielen Bereichen, einschließlich der militärischen, Transport, Luftfahrt, Bau- und Lebensmittelindustrie, unter anderem. Polyester und Beschichtungen sowohl Polyester und Silica - Nanopartikel (SiO 2 NPs) , die verwendet worden sind , weit verbreitet Stahl substrata vor Korrosion zu schützen. In dieser Studie verwendeten wir Röntgenphotoelektronenspektroskopie, abgeschwächte Totalreflexion Infrarot-Mikrospektroskopie, Wasserkontaktwinkelmessungen, optische Profilierung und Rasterkraftmikroskopie einen Einblick, wie Sonneneinstrahlung zur Verfügung zu stellen Veränderungen in der Mikro- verursachen können und nanoskaligen Integrität der Beschichtungen. Keine signifikante Veränderung der Oberflächenmikrotopographie wurde unter Verwendung von optischen Profilometer erkannt, jedoch statistisch signifikante nanoskaligen Änderungen an der Oberfläche wurden mit Hilfe der Rasterkraftmikroskopie nachgewiesen. Analyse der Röntgen-Photoelektronen-Spektroskopie und abgeschwächte Totalreflexion Infrarot mikro-Spektroskopie Daten zeigten , dass der Abbau der Estergruppen durch Einwirkung von ultraviolettem Licht erfolgt war COO · zu bilden, -H 2 C ·, -O ·, -CO · Radikale. Während des Abbauprozesses, CO und CO 2 wurden ebenfalls hergestellt.

<html> Die beschichteten Stahlproben, die entweder für einen, fünf Jahren gesammelt wurden dem Sonnenlicht Belichtung unterworfen worden war, und Wasserkontaktwinkel - Messungen wurden durchgeführt , um zu bestimmen , ob die Belichtung in einer Änderung der Oberflächenhydrophobie der Oberfläche (2 geführt hatten ). <img alt="Figur 2" src="/files/ftp_upload/54309/54309fig2.jpg" /> Abbildung 2. Die Benetzbark...

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

Zwei Arten von Oberflächen, polyesterbeschichteter Stahl und Polyester beschichtet mit einer Schicht aus Siliciumdioxid-Nanoteilchen, wurden untersucht. Beide Oberflächen wurden dem Sonnenlicht ausgesetzt, die wesentliche Änderungen in der Chemie und nanoskalige Topographie der Oberfläche zu bewirken, gefunden wurde.

Die Evolution der Silica-Nanopartikel-Polyester-Beschichtungen auf Oberflächen Sonnenlicht ausgesetzt

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

the-evolution-silica-nanoparticle-polyester-coatings-on-surfaces

Research

JoVE Journal

Engineering

9.5K Aufrufe.  Swinburne University of Technology.  Zwei Arten von Oberflächen, polyesterbeschichteter Stahl und Polyester beschichtet mit einer Schicht aus Siliciumdioxid-Nanoteilchen, wurden untersucht. Beide Oberflächen wurden dem Sonnenlicht ausgesetzt, die wesentliche Änderungen in der Chemie und nanoskalige Topographie der Oberfläche zu bewirken, gefunden wurde. 

Serie: 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.

Untersuchung der frühen Evolution von Plasma ultrakurzer Laserpulse

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

Forschung

Ingenieurwesen

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.

Herstellung von Silica Ultra High Quality Factor Mikroresonatoren

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.

Sondieren und Mapping-Elektrode Oberflächen 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 ...

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.

Herstellung von transparenten leitenden Oxide durch Pulsed Laser Deposition Nano-engineered

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.

High-Speed-Particle Image Velocimetry Nahe 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 ...

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 Kontakt Dotierung von Silizium-Oberflächen und Nanodrähte Mit Phosphororganische Verbindungen

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.

Hochauflösende Thermal Micro-Bildgebung Europiumchelatlösung Lumineszente Coatings

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.

Abklingende Feld Basierend Photoakustik: Optische Objektbewertung an Oberflächen

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.

Pool-Boiling Wärmeübertragung Enhancement auf zylindrischen Oberflächen mit Hybrid Benetzbare 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 ...

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.

Bewertung der Commercial-Off-The-Shelf Handgelenk Wearables, Stress auf Studenten zu schätzen

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