Diese Arbeit wurde teilweise durch eine PEPS Projekt der Cellule Energie INSIS-CNRS (1D-RENOX) bis ACG und der spanischen Regierung (MAT2012-35324 und PIE-201460I004) finanziert.

1. Herstellung des Sol <ol><li> Es wird eine Lösung von vorhydrolysierter Tetraethylorthosilikat (TEOS) am Tag vor der Herstellung der Gel-Filme in einer Abzugshaube, in dem eine Laborwaage und einem Magnetrührer platziert werden. In diesem Schritt und in der Protokolllaborkittel, Schutzhandschuhe und Schutzbrille tragen. <ol><li> In einem 50 ml Becherglas mit einem Teflon beschichteten Magnetrührstab wiegt 1,68 g CTAB, fügen 48,13 ml Ethanol und 3,00 ml HCl 35%, decken das Becherglas mit einem Uhrglas und rühren, bis die CTAB vollständig gelöst ist. </li><li> In 7,37 ml TEOS zu dem Becherglas tropfenweise (mit einer Geschwindigkeit von ca. 1-2 Tropfen pro Sekunde) unter Rühren, decken Sie den Kolben, der mit einem Uhrglas und lassen Sie es rühren O / N. </li></ol></li><li> Am nächsten Tag, bereiten eine 1 M wässrige Lösung von Sr 2+. Führen Sie dieses und die folgenden Schritte kurz vor der Herstellung der Gel-Filme, weil eine gealterte Lösung ist anfällig für Re-Fällung des Sr-Salz. <ol><li> Wiegen 6.6654 g SrCl 2 · 6H 2 O in einen 25 ml-Meßkolben. </li><li> In hochreinem Wasser (zB Milli-Q) bis zu 25 ml (Meniskus Tangente an den Kolben Marke) und den Kolben mit einer Kunststoffkappe und der Kolben, um das Strontiumchlorid aufzulösen schütteln. </li></ol></li><li> 2 ml der 1 M wässrigen Lösung von Sr 2+ zu dem 50 ml Becherglas mit dem Sol, das übrig war Rühren O / N. Rühren Sie die Lösung für 25 min. </li><li> Entsorgen Sie die Rückstände, die schließlich nach den Sicherheits- und Umweltschutz-Protokolle aus dem Labor erzeugt wurden. </li></ol> 2. Gel-Film Deposition on Si (100) Substrate <ol><li> Herstellung der Substrate <ol><li> Geschnitten Si Platten von etwa 2 cm bis 5 cm aus einem 2-Zoll-p-leitenden (100) Siliziumwafer mit einer Dicke von 200 um durch Spalten des Wafers in einer Richtung parallel oder senkrecht zu der Scheibenfläche unter Verwendung einer Diamantspitze oder ein scharfkantigen Gegenstand. Führen Sie diesen Schritt in Ad-Vance, zum Beispiel am Tag vor der Aufbringung der Gel-Filme. </li><li> Kurz vor der Abscheidung der Gele, reinigen Sie die Substrate mit Ethanol und trocknen lassen oder mit einem Stickstoffstrom oder Druckluft, um das Trocknen zu beschleunigen. Dieser Schritt beim Warten auf den Abschluß des Schritts 1.3. </li></ol></li><li> Coat die Filme. Um eine homogene Makroporenstruktur zu erhalten führen Sie diesen Schritt unter den Bedingungen einer relativen Luftfeuchtigkeit zwischen 20% und 55% bei RT. <ol><li> Stellen Sie eine Tauchbeschichtungsfolge. Wählen der ersten und letzten Positionen unter Berücksichtigung der tatsächlichen Länge des Si-Platte und die Höhe der Lösung in dem Becher, so daß die Platte wenigstens 2 cm oberhalb der Lösungspegel in der Startposition und 1 cm über dem Boden des Becherglas am Ende des Tauch. Stellen Sie sowohl die Immersion und Abzugsgeschwindigkeiten bis 150 mm / min. Stellen Sie die Tauchzeit (Zeit in der Endposition) auf Null. </li><li> Nach Abschluss von Schritt 1.3 wird das Becherglas mit dem sosung in einer gut zentrierten Position unterhalb des Si Bramme aus dem Tauchbeschichtungsvorrichtung Arm hängt. </li><li> Fix eine Ende des Si Platte mit dem Tauchbeschichtungsvorrichtung Arm mit der Klammer, wodurch die Platte möglichst senkrecht in Bezug auf die Horizontale. </li><li> Führen Sie den Tauchbeschichtungssequenz und ausclipsen Si Bramme aus dem Tauchbeschichtungsvorrichtung Arm. Wiederholen Sie die Schritte 2.2.3 und 2.2.4 mit zusätzlichen Si Platten, mehr Filme zu produzieren, kümmert sich nicht um diese Präparate über 1 Stunde zu verlängern, um sicherzustellen, dass die Stabilität der Lösung nicht beeinträchtigt wird. </li></ol></li><li> Entsorgen Sie die Lösungen, die schließlich nach den Sicherheits- und Umweltschutz-Protokolle aus dem Labor erzeugt wurden. </li></ol> 3. Gelfilm Kristallisation durch Wärmebehandlung <ol><li> Thermische Behandlung der Gel-Filme auf Si (100). <ol><li> Von RT bei 3 ° C / min Erhitzen auf 1.000 ° C, Halten bei 1.000 °: Programm einen Ofen, um die folgende Wärmebehandlung in Luftatmosphäre durchführenC für 5 Stunden und Abkühlen auf RT bei 3 ° C / min. </li><li> Platzieren Sie die tauchbeschichtet Si-Substraten in einem Schiffchen aus Aluminiumoxid, führen sie in den Ofen und Ausführen der Wärmebehandlung. </li></ol></li><li> Reinigung der kristallisierten Filme. <ol><li> Tauchen Sie die kristallisierte Filme für 3 Stunden in konzentrierter HNO 3, um die Ansammlungen von Sr 2+, die während der Kristallisation zu der Filmoberfläche ausgestoßen worden sind, zu entfernen, und dann Spülen der Filme zunächst mit entionisiertem Wasser und dann mit Ethanol. </li></ol></li></ol>

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	<li>Esser, A. T., Smith, K. C., Gowrishankar, T. R., Vasilkoski, Z., Weaver, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mechanisms+for+the+intracellular+manipulation+of+organelles+by+conventional+electroportation.">Mechanisms for the intracellular manipulation of organelles by conventional electroportation.</a> Biophys. J. 98 (11), 2506-2514 (2010).</li><li>Stava, E., Yu, M., Shin, H. C., Shin, H., Kreft, D. J., Blick, R. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rapid+fabrication+and+piezoelectric+tuning+of+micro-+and+nanopores+in+single+crystal+quartz.">Rapid fabrication and piezoelectric tuning of micro- and nanopores in single crystal quartz.</a> Lab Chip. 13 (1), 156-160 (2013).</li><li>Varshneya, A. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Fundamentals of Inorganic Glasses. , (1994).</li><li>Christov, M., Kirov, G. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+ratio+of+dissolving+surface+area/growing+surface+area+in+the+hydrothermal+growth+of+quartz.">The ratio of dissolving surface area/growing surface area in the hydrothermal growth of quartz.</a> J. Cryst. Growth. 131 (3-4), 560-564 (1993).</li><li>Bertone, J. F., Cizeron, J., Wahi, R. K., Bosworth, J. K., Colvin, V. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrothermal+synthesis+of+quartz+nanocrystals.">Hydrothermal synthesis of quartz nanocrystals.</a> Nano Lett. 3, 655-659 (2003).</li><li>Jiang, Y., Brinker, C. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrothermal+synthesis+of+monodisperse+single-crystalline+alpha-quartz+nanospheres.">Hydrothermal synthesis of monodisperse single-crystalline alpha-quartz nanospheres.</a> Chem. Comm. 47 (26), 7524-7526 (2011).</li><li>Okabayashi, M., Miyazaki, K., Kono, T., Tanaka, M., Toda, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+of+Spherical+Particles+with+Quartz+Single.">Preparation of Spherical Particles with Quartz Single.</a> Chem. Lett. 34 (1), 58-59 (2005).</li><li>Carretero-Genevrier, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Soft-Chemistry-Based+Routes+to+Epitaxial+&#945;-Quartz+Thin+Films+with+Tunable+Textures.">Soft-Chemistry-Based Routes to Epitaxial &#945;-Quartz Thin Films with Tunable Textures.</a> Science. 340 (6134), 827-831 (2013).</li><li>Brinker, C. J., Clem, P. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quartz+on+Silicon.">Quartz on Silicon.</a> Science. 340 (6134), 818-819 (2013).</li><li>Brinker, C. J., Lu, Y., Sellinger, A., Fan, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evaporation-Induced+Self-Assembly:+Nanostructures+Made+Easy.">Evaporation-Induced Self-Assembly: Nanostructures Made Easy.</a> Adv. Mater. 11 (7), 579-585 (1999).</li><li>Griffith, C. S., Sizgek, G. D., Sizgek, E., Scales, N., Yee, P. J., Luca, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesoporous+Zirconium+Titanium+Oxides.+Part+1:+Porosity+Modulation+and+Adsorption+Properties+of+Xerogels.">Mesoporous Zirconium Titanium Oxides. Part 1: Porosity Modulation and Adsorption Properties of Xerogels.</a> Langmuir. 24 (21), 12312-12322 (2008).</li><li>Lu, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Continuous+formation+of+supported+cubic+and+hexagonal+mesoporous+films+by+sol-gel+dip-coating.">Continuous formation of supported cubic and hexagonal mesoporous films by sol-gel dip-coating.</a> Nature. 389 (6649), 364-368 (1997).</li><li>Drisko, G. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Water-Induced+Phase+Separation+Forming+Macrostructured+Epitaxial+Quartz+Films+on+Silicon.">Water-Induced Phase Separation Forming Macrostructured Epitaxial Quartz Films on Silicon.</a> Adv. Funct. Mater. 24 (35), 5494-5502 (2014).</li></ol>

Die Autoren haben nichts zu offenbaren.

Das vorgestellte Verfahren ist ein Bottom-up-Ansatz für makroporöse Quarzfilme auf Si zu erzeugen. Im Vergleich zu dem Standardverfahren der Herstellung von Quarz-Folien, eine Top-Down-Technik auf das Schneiden und Polieren von großen hydrothermisch gezüchtete Kristalle, die in dem Protokoll beschriebene Verfahren erlaubt den Erhalt viel dünnere Folien mit Dicken zwischen 150 und 450 nm, die mit der gesteuert werden kann auf der Basis Entnahmeleistung. Alle experimentellen Einzelheiten in Bezug auf die Kontrolle de...

Wenn ein piezoelektrisches Material, wie α-Quarz mit einer Vorspannung abgegeben wird es einer mechanischen Verformung. Wenn dieses Material porös ist, können diese Volumenänderungen zu Poren Expansion oder Kontraktion führen, die Schaffung eines ansprechenden Systems ähnlich dem, was in lebenden biologischen Organellen zu beachten. 1 verformbare poröse α-Quarz wurde unter Verwendung von Mikro, 2 produziert, aber diese Techniken noch nicht erzeugen 3D-Porenstrukturen, und der Porendurchmesser in der Größenordnung von mehreren hundert Nanometern. Kristallisation von strukturierten amorphen Kieselsäure durch inhomogene Keimbildung durch eine hohe Oberflächenenergien und architektonischen Verformung aufgrund der Vergröberung und Schmelzen verursacht behindert. Außerdem, da alle Formen von Siliciumdioxid sind auf äußerst stabile SiO 4 Tetraeder-Netzwerke errichtet, die freie Energie der Bildung von amorphem Siliziumdioxid, α-Quarz und andere SiO2-Modifikationen in einem weiten Bereich von Temperaturen, Makin nahezu gleich sindg es schwierig, α-Quarz als ein einziges Polymorphs aus der Kristallisation eines amorphen Kieselgel herzustellen. 3 ein weiterer Aspekt, schwieriger macht die kontrollierte Kristallisation von strukturierten amorphen Siliciumdioxids ist, dass Quarz stellt eine relativ langsame Keimbildungsgeschwindigkeit jedoch ein extrem schnelles Wachstum, zwischen 10-94 nm berichtet / sec. 4,5 Langsame Keimbildung in Verbindung mit schnellem Wachstum neigt Kristalle viel größer als die ursprüngliche nanoporöse Struktur, wodurch das ursprüngliche Morphologie verloren zu erzeugen. Alkalimetalle, wie Na + und Li +, verwendet worden, um α-Quarz kristallisieren, häufig in Kombination mit hydrothermaler Behandlung. 5,6 Auch ein Ti 4+ / Ca 2+ Kombination wurde verwendet, um kugelförmige Teilchen von Siliciumdioxid in kristallisieren Quarz durch einen Weg der sanften Chemie unter Verwendung von Silizium-Alkoxide. 7 ist die gesteuerte Kristallisation eines strukturierten amorpher Kieselsäure Film in Quarz blieb jedoch eine Herausforderung. SiO 2 bei Umgebungsdruck und relativ niedrigen Temperaturen zu katalysieren. 8,9 Epitaxy, ergibt sich aus der guten Übereinstimmung zwischen α-Quarz und der &lt;100&gt; Silizium-Substrat, Herstellung von orientierten piezoelektrischen Dünnfilme. Verdampfen induzierten Selbstorganisation mesoporösen Siliciumdioxid Folien herzustellen wird seit 1999 10 Diese Technik wurde untersucht und auf eine Vielzahl von Matrixmittel unter verschiedenen Bedingungen angelegt, um Poren von variablen Größen und Mesophasen herzustellen. Es wurde gefunden, daß subnanometric Veränderungen Mesoporengröße kann eine dramatische Auswirkung auf solute Diffusion durch poröse Systeme 11 aufweisen, Validierung dieser große Aufmerksamkeit auf die Struktur Pore. Darüber hinaus kann die Zugänglichkeit zu der internen Kieselsäure Porensystem durch Steuern der mizellaren Phase der Vorlage erhalten werden. 12 Hier wird der Syntheseweg tKappe ermöglicht uneingeschränkte Kontrolle über die Dicke und die Porengröße aus amorphem Siliciumdioxid-Schichten unter Verwendung einer neuen Phasentrennung zeigten. 13 Diese Filme werden mit Sr (II) salze und kristallisiert, um a-Quarz bei 1000 ° C an der Luft bei Umgebungsdruck infiltriert. Die Porengröße zurückhaltbar mit diesen Kristallisationsprozess wird bestimmt, und die Wirkung der Wandstärke und der Filmdicke untersucht. Schließlich die Piezoelektrizität und die Verformbarkeit des Porensystems untersucht.

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			<td height="21" style="height:21px;width:180px;">Dip coater</td>
			<td style="width:281px;">Nadetech&#160;</td>
			<td style="width:173px;">ND-DC 11/150&#160;</td>
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			<td height="21" style="height:21px;width:180px;">Furnace</td>
			<td style="width:281px;">Nabertherm&#160;</td>
			<td>R 50/250/12</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">Atomic Force Microscope</td>
			<td style="width:281px;">Agilent&#160;</td>
			<td>5500 LS</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">Materials and Reagents&#160;</td>
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			<td></td>
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		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">Silicon wafers</td>
			<td style="width:281px;">SHE Europe Ltd.</td>
			<td></td>
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			<td height="21" style="height:21px;width:180px;">SrCl2&#183;6H2O</td>
			<td style="width:281px;">Aldrich</td>
			<td>13909</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:180px;">CTAB</td>
			<td style="width:281px;">Aldrich</td>
			<td>H5582</td>
			<td></td>
		</tr>
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			<td height="21" style="height:21px;width:180px;">Ethanol Absolute&#160;</td>
			<td style="width:281px;">Aldrich</td>
			<td>161086</td>
			<td></td>
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		<tr height="21">
			<td height="21" style="height:21px;width:180px;">HCl 35% solution</td>
			<td style="width:281px;">PanReac</td>
			<td>721019</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">TEOS</td>
			<td style="width:281px;">Aldrich</td>
			<td>131903</td>
			<td></td>
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preparation of macroporous epitaxial quartz films on silicon by chemical solution deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

Das Fortschreiten der Materialsynthese wurde durch Überwachung verschiedener Aspekte gesteuert. Nach dem Tauchbeschichtungsverfahren kann man den Aspekt der Filme, den eventuellen Auftreten von Beugungsstrukturen in dem reflektierten Fleck eines grünen Lasers und der Rasterelektronenmikroskopie (SEM) in Rückstreuelektronen-Modus (1A-B) zu beobachten. Nach dem Kristallisationsverfahren ist es wichtig, die Rasterkraftmikroskopie (AFM) topografische Bilder (1C)</...

Watch this Scientific Journal Video about Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition at JoVE.com

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

Herstellung von makroporösen Epitaxial-Quarz-Films auf Silizium durch Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

preparation-macroporous-epitaxial-quartz-films-on-silicon-chemical

Research

JoVE Journal

Chemistry

9.2K Aufrufe.  CNRS-École Centrale de Lyon. A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air. 

Serie: Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

Herstellung von hydrophoben Metall-organische Gerüste über Plasma Enhanced Chemical Vapor Deposition von Perfluoralkanen für die Beseitigung von Ammoniak

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

Forschung

Chemie

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

Atomar definierte Vorlagen Epitaxieausrüstung komplexer Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in traditional materials, including low cost and mechanical flexibility. In a similar vein, it would be advantageous to expand the use of organics into high frequency electronics and spin-based electronics. This work presents a synthetic process for the growth of thin films of the room temperature organic ferrimagnet, vanadium tetracyanoethylene (V[TCNE]x, x~2) by low temperature chemical vapor deposition (CVD). The thin film is grown at &#60;60 &#176;C, and can accommodate a wide variety of substrates including, but not limited to, silicon, glass, Teflon and flexible substrates. The conformal deposition is conducive to pre-patterned and three-dimensional structures as well. Additionally this technique can yield films with thicknesses ranging from 30 nm to several microns. Recent progress in optimization of film growth creates a film whose qualities, such as higher Curie temperature (600 K), improved magnetic homogeneity, and narrow ferromagnetic resonance line-width (1.5 G) show promise for a variety of applications in spintronics and microwave electronics.

We present the synthesis of the organic-based ferrimagnet vanadium tetracyanoethylene (V[TCNE]x, x~2) via low temperature chemical vapor deposition (CVD). This optimized recipe yields an increase in Curie temperature from 400 K to over 600 K and a dramatic improvement in magnetic resonance properties.

Chemical Vapor Deposition eines Organic Magnet, Vanadium Tetracyanethylen

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in ...

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

Vorbereitung hoch poröser Koordinationspolymerbeschichtungen auf makroporösen Monoliths für verbesserte Anreicherung von Phosphopeptiden

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Preparation of Mica and Silicon Substrates for DNA Origami Analysis and Experimentation

The designed nature and controlled, one-pot synthesis of DNA origami provides exciting opportunities in many fields, particularly nanoelectronics. Many of these applications require interaction with and adhesion of DNA nanostructures to a substrate. Due to its atomically flat and easily cleaned nature, mica has been the substrate of choice for DNA origami experiments. However, the practical applications of mica are relatively limited compared to those of semiconductor substrates. For this reason, a straightforward, stable, and repeatable process for DNA origami adhesion on derivatized silicon oxide is presented here. To promote the adhesion of DNA nanostructures to silicon oxide surface, a self-assembled monolayer of 3-aminopropyltriethoxysilane (APTES) is deposited from an aqueous solution that is compatible with many photoresists. The substrate must be cleaned of all organic and metal contaminants using Radio Corporation of America (RCA) cleaning processes and the native oxide layer must be etched to ensure a flat, functionalizable surface. Cleanrooms are equipped with facilities for silicon cleaning, however many components of DNA origami buffers and solutions are often not allowed in them due to contamination concerns. This manuscript describes the set-up and protocol for in-lab, small-scale silicon cleaning for researchers who do not have access to a cleanroom or would like to incorporate processes that could cause contamination of a cleanroom CMOS clean bench. Additionally, variables for regulating coverage are discussed and how to recognize and avoid common sample preparation problems is described.

Reproducible cleaning processes for substrates used in DNA origami research are described, including bench-top RCA cleaning and derivatization of silicon oxide. Protocols for surface preparation, DNA origami deposition, drying parameters, and simple experimental set-ups are illustrated.

Herstellung von Mica und Siliziumsubstraten für die DNA-Origami-Analyse und Experimentieren

The designed nature and controlled, one-pot synthesis of DNA origami provides exciting opportunities in many fields, particularly nanoelectronics. Many of ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

Epitaxie Perowskit Strontiumtitanat auf Germanium über Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

Low Pressure Vapor-assisted Solution Process for Tunable Band Gap Pinhole-free Methylammonium Lead Halide Perovskite Films

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, we present a protocol for the fabrication of this material via the low-pressure vapor assisted solution process (LP-VASP) method, which yields ~19% power conversion efficiency in planar heterojunction perovskite solar cells. First, we report the synthesis of methylammonium iodide (CH3NH3I) and methylammonium bromide (CH3NH3Br) from methylamine and the corresponding halide acid (HI or HBr). Then, we describe the fabrication of pinhole-free, continuous methylammonium-lead halide perovskite (CH3NH3PbX3 with X = I, Br, Cl and their mixture) films with the LP-VASP. This process is based on two steps: i) spin-coating of a homogenous layer of lead halide precursor onto a substrate, and ii) conversion of this layer to CH3NH3PbI3-xBrx by exposing the substrate to vapors of a mixture of CH3NH3I and CH3NH3Br at reduced pressure and 120 &#176;C. Through slow diffusion of the methylammonium halide vapor into the lead halide precursor, we achieve slow and controlled growth of a continuous, pinhole-free perovskite film. The LP-VASP allows synthetic access to the full halide composition space in CH3NH3PbI3-xBrx with 0&#160;&#8804; x&#160;&#8804; 3. Depending on the composition of the vapor phase, the bandgap can be tuned between 1.6 eV&#160;&#8804; Eg&#160;&#8804; 2.3 eV. In addition, by varying the composition of the halide precursor and of the vapor phase, we can also obtain CH3NH3PbI3-xClx. Films obtained from the LP-VASP are reproducible, phase pure as confirmed by X-ray diffraction measurements, and show high photoluminescence quantum yield. The process does not require the use of a glovebox.

Here, we present a protocol for the synthesis of CH3NH3I and CH3NH3Br precursors and the subsequent formation of pinhole-free, continuous CH3NH3PbI3-xBrx thin films for the application in high efficiency solar cells and other optoelectronic devices.

Dampf-gestützte Lösung Niederdruckverfahren für durchstimmbare Band Gap Pinhole-frei Methylammonium Blei Halogenid Perowskit Filme

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, their high cost production and/or incompatibility with microfabrication technologies, due to the use of pre-deposited catalyst-seeds and/or high processing temperatures exceeding 900 &#176;C, represent a drawback for a widespread use of these methods. Here, however, we report the synthesis of ZnO rods via a non-catalyzed vapor-solid mechanism enabled by using an aerosol-assisted chemical vapor deposition (CVD) method at 400 &#176;C with zinc chloride (ZnCl2) as the precursor and ethanol as the carrier solvent. This method provides both single-step formation of ZnO rods and the possibility of their direct integration with various substrate types, including silicon, silicon-based micromachined platforms, quartz, or high heat resistant polymers. This potentially facilitates the use of this method at a large-scale, due to its compatibility with state-of-the-art microfabrication processes for device manufacture. This report also describes the properties of these structures (e.g., morphology, crystalline phase, optical band gap, chemical composition, electrical resistance) and validates its gas sensing functionality towards carbon monoxide.

Columnar zinc oxide structures in the form of rods are synthesized via aerosol-assisted chemical vapor deposition without the use of pre-deposited catalyst-seed particles. This method is scalable and compatible with various substrates based on either silicon, quartz or polymers.

Aerosol-assisted Chemical Vapor Deposition von Metall-Oxid-Strukturen: Zinkoxid-Stangen

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

Reaktiven Aufdampfen von konjugierten Polymerfilmen auf beliebigen Substraten

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Deposition of Porous Sorbents on Fabric Supports

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material that can be subsequently treated by dip coating. Dip coating with a sol preparation provides a supported porous layer on the fabric. In this case, the porous layer is a porphyrin functionalized sorbent system based on a powdered material that has been demonstrated previously for the capture and conversion of phosgene. A representative coating is applied to cotton fabric at a loading level of 10 mg/g. This coating has minimal impact on water vapor transport through the fabric (93% of the support fabric rate) while significantly reducing transport of 2-chloroethyl ethyl sulfide (CEES) through the material (7% of support fabric rate). The described approaches are suitable for use with other fabrics providing amine and hydroxyl groups for modification and can be used in combination with other sol preparations to produce varying functionality.

This report details a microwave-initiated approach for deposition of porphyrin functionalized porous organosilicate sorbents on a cotton fabric and demonstrates reduction in 2-chloroethyl ethyl sulfide (CEES) transport through the fabric resulting from this treatment.

Ablagerung von porösen Sorbentien auf Stoff

A microwave deposition technique for silanes, previously described for production of oleophobic fabrics, is adapted to provide a fabric support material ...