Ce travail a été partiellement financé par un projet PEPS de Cellule Energie INSIS-CNRS (1D-RENOX) à ACG et le gouvernement espagnol (MAT2012-35324 et Pie-201460I004).

1. Préparation du Sol <ol><li> Préparer une solution d&#39;orthosilicate de tétraéthyle préhydrolysé (TEOS), le jour avant la préparation des films de gel dans une hotte de laboratoire dans lequel une balance de laboratoire et d&#39;un agitateur magnétique sont placés. Dans cette étape et dans le protocole de porter une blouse de laboratoire, des gants et des lunettes de sécurité. <ol><li> Dans un bécher de 50 ml contenant une barre d&#39;agitation magnétique revêtu de Téflon pèse 1,68 g de CTAB, ajouter 48,13 ml d&#39;éthanol et 3,00 ml de HCl 35%, couvrir le bécher avec un verre de montre et mélanger jusqu&#39;à ce que le CTAB est complètement dissous. </li><li> Ajouter 7,37 ml de TEOS goutte à goutte au bécher (à un taux d&#39;environ 1-2 gouttes par seconde) tout en remuant, couvrir le ballon avec un verre de montre et laisser remuer O / N. </li></ol></li><li> Le lendemain, préparer une solution aqueuse 1 M de Sr 2+. Effectuer cette les étapes suivantes et juste avant la préparation des films de gel, car une solution vieillie est sujette à re-précipitation du sel Sr. <ol><li> Peser 6,6654 g de SrCl2 · 6H 2 O dans une fiole jaugée de 25 ml. </li><li> Ajouter de l&#39;eau ultra-pure (par exemple, Milli-Q) à 25 ml (ménisque tangente à la marque de ballon) et boucher la fiole avec un bouchon en plastique et secouez doucement le flacon pour dissoudre le chlorure de strontium. </li></ol></li><li> Ajouter 2 ml de la solution aqueuse 1 M de Sr 2+ dans le bêcher en verre de 50 ml contenant le sol qui a été laissé sous agitation O / N. Agiter la solution pendant 25 min. </li><li> Eliminer les résidus qui ont été éventuellement générés selon les protocoles de protection sécurité et d&#39;environnement du laboratoire. </li></ol> 2. Gel Film dépôt sur Si (100) Supports <ol><li> Préparation des substrats <ol><li> Couper plaques de silicium de l&#39;ordre de 2 cm par 5 cm, sur un type p de 2 pouces (100) plaquette de silicium d&#39;une épaisseur de 200 microns par clivage de la plaquette dans une direction parallèle ou perpendiculaire à la plate de la plaquette à l&#39;aide d&#39;une pointe de diamant ou une objet tranchant. Effectuez cette étape dans l&#39;annonceVance, par exemple le jour avant le dépôt des films de gel. </li><li> Juste avant le dépôt des gels, nettoyer les substrats avec de l&#39;éthanol et les laisser sécher ou utiliser un flux d&#39;azote ou de l&#39;air comprimé pour accélérer le séchage. Effectuez cette étape en attendant l&#39;achèvement de l&#39;étape 1.3. </li></ol></li><li> Enduire les films. Afin d&#39;obtenir une structure de macropores homogène effectuer cette étape dans des conditions d&#39;humidité relative entre 20% et 55% à température ambiante. <ol><li> Établir une séquence de revêtement par immersion. Sélectionner des positions initiales et finales en tenant compte de la longueur réelle de la dalle de Si et le niveau de la solution dans le bécher de sorte que la dalle est d&#39;au moins 2 cm au-dessus du niveau de la solution à la position de départ et de 1 cm au-dessus du fond de la bêcher à la fin de l&#39;immersion. Réglez les deux vitesses d&#39;immersion et de retrait à 150 mm / min. Réglez le temps d&#39;immersion (de temps à la position finale) à zéro. </li><li> À l&#39;issue de l&#39;étape 1.3 Placer le bécher avec le soilution dans une position bien centrée sous la dalle Si accroché au bras dip-coucheuse. </li><li> Fixer une extrémité de la dalle Si au bras immersion cathodique avec le clip, assurant la dalle est aussi perpendiculairement que possible par rapport à l&#39;horizontale. </li><li> Exécuter la séquence de revêtement par immersion et déclipser la dalle Si du bras dip-coucheuse. Répétez les étapes 2.2.3 et 2.2.4 avec dalles Si supplémentaires pour produire plus de films, en prenant soin de ne pas prolonger au-delà de ces préparations 1 h, pour assurer que la stabilité de la solution ne soit pas compromise. </li></ol></li><li> Jeter les solutions qui ont été éventuellement générés selon les protocoles de protection sécurité et d&#39;environnement du laboratoire. </li></ol> 3. Gel Film cristallisation par traitement thermique <ol><li> Traitement thermique des films de gel de Si (100). <ol><li> Programme d&#39;un four pour effectuer le traitement thermique suivant dans une atmosphère d&#39;air: chauffage de la température ambiante à 1 000 ° C à 3 ° C / min, maintien à 1000 °; C pendant 5 heures et refroidissement à TA à 3 ° C / min. </li><li> Placez les substrats de Si revêtus par immersion dans une nacelle en alumine, l&#39;introduire dans le four et exécuter le traitement thermique. </li></ol></li><li> Nettoyage des films cristallisées. <ol><li> Plonger les films cristallisés pendant 3 heures dans HNO 3 concentré afin d&#39;éliminer les accumulations de Sr 2+ qui ont été expulsés à la surface du film lors de la cristallisation, puis rincez les films d&#39;abord avec de l&#39;eau déminéralisée, puis avec de l&#39;éthanol. </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>

Les auteurs ont rien à révéler.

La méthode présentée est une approche bottom-up pour produire des films de quartz macroporeuses sur Si. Par rapport à la méthode standard de production de films de quartz, une technologie de haut en bas basé sur la coupe et le polissage de gros cristaux hydrothermique cultivées, la méthode décrite dans le protocole permet d&#39;obtenir des films beaucoup plus minces avec des épaisseurs comprises entre 150 et 450 nm, qui peuvent être contrôlées avec le le taux de retrait. Tous les détails expérimentaux con...

Quand un matériau piézoélectrique comme α-quartz est soumis à une tension de polarisation il subit une déformation mécanique. Si ce matériau est poreux, ces changements de volume peuvent conduire à l&#39;expansion des pores ou de contraction, la création d&#39;un système sensible similaire à ce qui peut être observé à vivre organites biologiques. 1 déformable poreuse α-quartz a été produite en utilisant la microfabrication, 2, mais ces techniques ne peuvent pas encore produire des structures de pores 3-D, et des diamètres de pores sont de l&#39;ordre de plusieurs centaines de nanomètres. La cristallisation de la silice amorphe structuré a été entravée par la nucléation inhomogène causée par les énergies de surface élevées et la déformation architecturale due à grossissement et la fusion. De plus, comme toutes les formes de silice sont construits sur des réseaux SiO 4 tétraédriques extrêmement stables, les énergies libres de formation de la silice amorphe, du quartz α-SiO 2 et d&#39;autres formes polymorphes sont à peu près égales dans une gamme étendue des températures, Making, il est difficile de produire des α-quartz comme une seule polymorphe de la cristallisation d&#39;un gel de silice amorphe. 3 Un autre aspect qui rend plus difficile la cristallisation contrôlée de silice amorphe structurée est que le quartz présente une vitesse de nucléation relativement lente, mais un taux de croissance extrêmement rapide, rapporté entre 10-94 nm / s. 4,5 nucléation lente couplée à la croissance rapide tend à générer des cristaux beaucoup plus grande que la structure nanoporeuse original, donc la morphologie d&#39;origine est perdue. Les métaux alcalins, tels que Na + et Li +, ont été utilisés pour cristalliser α-quartz, souvent en combinaison avec un traitement hydrothermique. 5,6 En outre, un Ti4 + / Ca 2+ combinaison a été utilisée pour cristalliser des particules sphériques de silice dans quartz par un circuit de chimie douce en utilisant alcoxydes de silicium. 7 Toutefois, la cristallisation contrôlée d&#39;un film de silice amorphe structurée en quartz reste un défi. 2 cristallisé sous la pression ambiante et des températures relativement basses. 8,9 épitaxie, provient de la non-concordance favorable entre α-quartz et le substrat&gt; de silicium &lt;100, produire des films minces piézoélectriques orientés. Induite par évaporation-auto-assemblage pour produire des films de silice mésoporeuse a été utilisé depuis 1999. 10 Cette technique a été étudié et appliqué à une multitude d&#39;agents servant de modèle dans diverses conditions pour produire des pores de tailles et de mésophases variables. Il a été constaté que les changements dans la taille de subnanométriques mésopore peuvent avoir un effet dramatique sur la diffusion de soluté à travers des systèmes poreux 11, validant cette grande attention à la structure de pore. De plus, l&#39;accessibilité au réseau de pore interne de silice peut être obtenue en commandant la phase micellaire de la matrice 12. Ici, la voie de synthèse tchapeau permet un contrôle sans précédent sur ​​la taille de l&#39;épaisseur et des pores de couches de silice amorphe en utilisant une nouvelle séparation de phase est mise en évidence. 13 Ces films sont infiltrés avec des sels de Sr (II) et cristallisé à l&#39;a-quartz à 1000 ° C sous air à la pression ambiante. La taille de pores capable de retenir à l&#39;aide de ce processus de cristallisation est déterminée, et l&#39;effet de l&#39;épaisseur de paroi et l&#39;épaisseur du film est étudiée. Enfin la piézo-électricité et la déformabilité du système de pores sont étudiés.

<table border="0" cellpadding="0" cellspacing="0" width="714">
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		<tr height="21">
			<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>
			<td style="width:80px;"></td>
		</tr>
		<tr height="21">
			<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>
			<td style="width:281px;"></td>
			<td></td>
			<td></td>
		</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>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">SrCl2&#183;6H2O</td>
			<td style="width:281px;">Aldrich</td>
			<td>13909</td>
			<td></td>
		</tr>
		<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>
		<tr height="21">
			<td height="21" style="height:21px;width:180px;">Ethanol Absolute&#160;</td>
			<td style="width:281px;">Aldrich</td>
			<td>161086</td>
			<td></td>
		</tr>
		<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>
		</tr>
	</tbody>
</table>

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.

Le déroulement de la synthèse matériau a été contrôlée par la surveillance des aspects différents. Après le processus de revêtement par immersion, on peut observer l&#39;aspect des films, l&#39;apparition éventuelle de structures de diffraction dans le spot réfléchie d&#39;un laser vert et de la microscopie électronique à balayage (MEB) des images en mode rétrodiffusion des électrons (figure 1A-B). Après le processus de cristallisation, il est important...

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.

Préparation de macroporeuses Épitaxial Quartz Films de silicium par dépôt chimique Solution

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

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9.2K vues.  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. 

Vidéo: 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.

Préparation de hydrophobes cadres métal-organiques via Plasma Enhanced Chemical Vapor Deposition de perfluoroalcanes pour l&#39;enlèvement de l&#39;ammoniac

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

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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.

Modèles atomique définies pour croissance épitaxiale d&#39;oxyde complexe couches minces

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 d&#39;un aimant Organic, Vanadium tétracyanoéthylène

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.

Préparation de la grande porosité de coordination Polymer Coatings sur macroporeuses Polymer monolithes pour enrichissement accrue des Phosphopeptides

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.

Préparation de Mica et Silicon substrats pour l&#39;ADN Origami Analyse et Expérimentation

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.

Croissance épitaxiale de perovskite Strontium Titanate sur 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 ...

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.

Processus de Solution assistée par vapeur basse pression pour bande accordable Gap sténopé méthylammonium plomb halogénure Perovskite Films

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.

Aérosol-assisted Chemical Vapor Deposition de Structures d’oxyde métallique : tiges d’oxyde de Zinc

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.

Réactif de Vapor Deposition de Films polymères conjugués sur substrats arbitraires

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.

Dépôt des adsorbants ou des absorbants poreux sur des Supports de tissu

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