この作品は、部分的に小細胞エナジーACGにINSIS-CNRS（1D-RENOX）とスペイン政府（MAT2012-35324とPIE-201460I004）のPEPSプロジェクトによって資金を供給されました。

ゾルの​​調製<ol><li>ラボバランスおよび磁気攪拌子を配置したヒュームフード中のゲルフィルムを調製する前に予め加水分解テトラエチルオルトシリケート（TEOS）日の溶液を調製します。このステップでは、プロトコルを通じてラボのコート、手袋、安全メガネを着用してください。 <ol><li>テフロンコーティングされた磁気撹拌棒がCTABの1.68グラムの重量を量る含む50ミリリットルのビーカーでは、時計皿で覆い、ビーカーを48.13エタノール10mlおよびHCl、35％の3.00ミリリットルを加え、CTABが完全に溶解するまで撹拌します。 </li><li>攪拌しながら、（約1〜2の割合で毎秒低下）をビーカーに滴下して、TEOSの7.37ミリリットルを加え、時計皿でフラスコをカバーし、それは、O / Nを攪拌してみましょう。 </li></ol></li><li>次の日、のSr 2+の1 M水溶液を調製。経年ソリューションは、Srの塩の再沈殿する傾向があるのでちょうどゲルフィルムの調製前に、この、次の手順を実行します。 <ol><li> 6.6計量25ミリリットルのメスフラスコへのSrCl 2の654グラム・6H 2 O。 </li><li> 25ミリリットル（フラスコマークにメニスカス接線）までの超純水（例えば、ミリQ）を追加し、プラスチック製のキャップでフラスコを閉じ、ゆっくりと塩化ストロンチウムを溶解するフラスコを振ります。 </li></ol></li><li> / NとOを攪拌したゾルを含む50 mlのガラスビーカーへのSr 2+の1 M水溶液2mlを加えます。 25分間溶液を撹拌しました。 </li><li>最終的には実験室の安全性と環境保護プロトコルに従って生成された残基を廃棄してください。 </li></ol> 2.ゲル膜堆積Si上の（100）基板<ol><li>基板の作製<ol><li>ダイヤモンドチップまたはAを使用して、ウェハのフラットに平行または垂直方向にウェハを切断することにより、200ミクロンの厚さを有する（100）シリコンウェハ2インチのp型の5 CMで約2cmのシリコンスラブをカット鋭利な物体。広告でこの手順を実行します例えばバンス、ゲル膜の堆積前の日。 </li><li>ただ、ゲルの堆積前に、エタノールで基板をきれいにし、それらを乾燥させたり乾燥を促進するため、窒素の流れや圧縮空気を使用しています。ステップ1.3の完了を待っている間に、この手順を実行します。 </li></ol></li><li>コー​​トフィルム。均質なマクロ孔構造を得るためには20％、RTで55％の相対湿度の条件下でのこのステップを実行します。 <ol><li>ディップコーティングシーケンスを確立します。スラブが開始位置で少なくとも2センチメートルソリューションレベルより上で、1センチ底の上になるように考慮したSiスラブの実際の長さを取って最初と最後の位置、ビーカー内の溶液のレベルを選択します浸漬の終わりにビーカー。 150ミリメートル/分浸漬し、離脱速度の両方を設定します。ゼロに浸漬時間（最終位置での時間）を設定します。 </li><li>そうでステップ1.3場所ビーカーが完了するとディップコーターアームからぶら下がったSiスラブの下によく中心の位置にリューション。 </li><li>スラブが水平に対してできるだけ垂直で確保し、クリップでディップコーターアームにシリコンスラブの一方の端を固定してください。 </li><li>ディップコーティングシーケンスを実行し、ディップコーターアームからのSiスラブをクリップを取り除きます。追加のSiスラブと手順を繰り返し2.2.3と2.2.4は、溶液の安定性が損なわれないことを確実にするために、1時間を超えてこれらの準備を拡張しないように注意しながら、より多くのフィルムを製造します。 </li></ol></li><li>最終的には実験室の安全性と環境保護プロトコルに従って生成されたソリューションを廃棄してください。 </li></ol>熱処理によって3.ジェルフィルムの結晶化<ol><li> Si上のゲル膜の熱処理（100）。 <ol><li>プログラム空気雰囲気中で、以下の熱処理を実行するための炉：3℃/分で室温から1000℃まで加熱し、1000℃で保持します; C 5時間3℃/分で室温まで冷却しました。 </li><li> 、アルミナボートに浸漬被覆Si基板を置き、炉内でそれを導入し、熱処理を行います。 </li></ol></li><li>結晶化したフィルムのクリーニング。 <ol><li>結晶化の際にフィルム表面にexpulsedされたのSr 2+の蓄積を削除してから、脱イオン水で最初の映画を洗い流した後、エタノールとするために、濃HNO 3で3時間結晶化されたフィルムを浸し。 </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>

著者らは、開示することは何もありません。

提示された方法は、Si上のマクロポーラス石英フィルムを製造するためのボトムアップ・アプローチです。石英膜の製造の標準的な方法、切断および大水熱成長した結晶の研磨に基づいて、トップダウン技術と比較して、プロトコールに記載された方法を用いて制御することができる150と450nmの間の厚さを有する非常に薄いフィルムを得ることができ離脱率。石英膜の厚さ、及び圧電応答の制...

α-水晶のような圧電材料は電圧バイアスに提出された場合には、機​​械的な変形を受けます。この材料は多孔質である場合、これらの体積変化は、生体細胞小器官を生きている中で観察することができるものと同様の応答システムを作成し、気孔膨張または収縮につながることができます。1変形可能な多孔質のα石英は微細加工、2を使用して製造されているが、このような技術はまだできません3次元細孔構造を生成し、かつ細孔直径が数百ナノメートルのオーダーです。構造化アモルファスシリカの結晶化は、高い表面エネルギーと粗大化と溶融に起因する建築変形による不均一核生成によって妨げられてきました。シリカのすべての形態が非常に安定したSiO 4四面体のネットワーク上に構築されているので、アモルファスシリカ、α石英や他のSiO 2の多形の形成の自由エネルギーは、広い温度範囲でほぼ等しく、メイキン困難非晶質シリカゲルの結晶からの単一の多形体としてα石英を生成するためにG 3構造の非晶質シリカの制御された結晶は、石英は比較的遅い核形成速度が、非常に速い成長速度を示すことである難しくなる他の態様、 10から94ナノメートル/秒の間で報告された。急速な成長と相まって4,5遅い核形成は、このように、元の形態が失われ、元のナノポーラス構造よりもはるかに大きい結晶を生成する傾向があります。例えばNa +及びLi +などのアルカリ金属は、しばしば水熱処理と組み合わせて、α石英を結晶化するために使用されている。5,6も、チタン4+ / の Ca 2+の組み合わせはにシリカの球状粒子を結晶化するために使用されましたシリコンアルコキシドを用いたソフト化学経路による石英。7しかし、石英に構造化されたアモルファスシリカ膜の制御された結晶化が課題に残りました。 2の核生成と成長を触媒することが見出されている。8,9エピタキシー」jove_content &quot;&gt;は、α石英、および&lt;100&gt;シリコン基板との良好な不整合から生じます配向圧電薄膜を製造します。蒸発によって誘導される自己組織化メソポーラスシリカフィルムを生成するためには、1999年10は 、この技術が研究されており、可変サイズと中間相の気孔を生成するために、様々な条件下でのテンプレート剤の多くに適用使用されています。これは、メソ細孔サイズのsubnanometric変化が細孔構造にこの大規模な注意を検証する、多孔システム11を介して溶質拡散に対する劇的な効果を有し得ることが見出されました。また、内部のシリカ孔系へのアクセスは、テンプレートのミセル相を制御することによって得ることができる。12 ここで、合成ルートT帽子は、新規相分離が実証されている使用して非晶質シリカ層の厚さと細孔サイズを超える空前の制御を可能にする。13これらのフィルムは、周囲圧力で空気中1000℃でのSr（II）塩、結晶化するために、α-石英を浸透させています。この結晶化プロセスを使用して保持できる細孔サイズが決定され、壁の厚さと膜厚の効果が検討されています。最後に、圧電性および細孔系の変形が検討されています。

<table border="0" cellpadding="0" cellspacing="0" width="714">
	<tbody>
		<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.

材料合成の進行は、異なる側面を監視することによって制御しました。ディップコーティングプロセスの後にいずれかのフィルムの側面、緑色レーザおよび走査電子顕微鏡（SEM）後方散乱電子モード（ 図1A-B）の画像の反射点における回折構造の最終的な外観を観察することができます。結晶化工程の後に、原子間力顕微鏡（AFM）トポグラフィ画像（ <stro...

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.

化学溶液法によるシリコン上のマクロポーラスエピタキシャル石英薄膜の作製

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

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JoVE Journal

Chemistry

9.2K ビュー.  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. 

ビデオ: 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.

プラズマを介した疎水性有機金属フレームワークの製造は、アンモニアの除去のためにペルフルオロアルカンの化学的気相成長法を強化

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

化学

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.

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

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.

有機マグネットの化学気相堆積、バナジウムテトラ

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.

リン酸化ペプチドの強化充実のためのマクロポーラスポリマーモノリスの高度に多孔性配位高分子コーティングの製造

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.

DNA折り紙解析と実験のためのマイカとシリコン基板の作製

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.

原子層堆積法を介してゲルマニウム上のペロブスカイト型チタン酸ストロンチウムのエピタキシャル成長

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.

可変バンド ギャップ ピンホール フリー メチル鉛ハライド ペロブスカイト薄膜の低圧蒸気支援ソリューション プロセス

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.

エアロゾルによる金属酸化物の構造の化学蒸着: 酸化亜鉛棒

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.

任意の基板上への共役ポリマー薄膜の反応性蒸着

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.

ファブリックのサポートに多孔質吸着剤の成

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