这项工作是部分被CELLULE科特布斯INSIS-CNRS（1D-RENOX），以ACG和西班牙政府（MAT2012-35324和PIE-201460I004）的PEPS项目资助。

1.准备溶胶<ol><li>制备预水解原硅酸四乙酯（TEOS）在通风橱中的凝胶膜，其中实验室天平和磁力搅拌器被放置的制备前一天的溶液。在这一步，整个协议穿白大褂，手套和护目镜。 <ol><li>在50ml烧杯中含有特氟隆涂层的磁力搅拌棒称量1.68克的CTAB，加入48.13毫升乙醇和3.00毫升的HCl的35％，覆盖烧杯用表面玻璃和搅拌，直至CTAB完全溶解。 </li><li>添加7.37 ml的TEOS与烧杯滴加（以约1-2的速率每秒滴剂），同时搅拌，覆盖用表玻璃烧瓶，让它搅拌O / N。 </li></ol></li><li>第二天，制备锶2+的1M水溶液。只是凝胶薄膜的制备之前执行此和下面的步骤，因为老化的解决方案很容易重新沉淀的锶盐。 <ol><li>称取6.6654克SRCL 2·6H 2 O在25mL容量瓶中。 </li><li>添加超纯水（例如，纯水）高达25毫升（弯月面相切的烧瓶标记）和用塑料盖封闭烧瓶中，并轻轻摇动烧瓶以溶解氯化锶。 </li></ol></li><li>加入2毫升锶2+的1M的水溶液与含被保持搅拌O / N溶胶中的50ml的玻璃烧杯中。搅拌25分钟溶液。 </li><li>处置已根据实验室的安全和环保协议被最终产生的残留物。 </li></ol> 2.凝胶薄膜沉积在Si（100）衬底<ol><li>所述预处理<ol><li>切成约2厘米的S​​i板坯由5厘米出一个2英寸P型（100）硅晶片的厚度为200微米的通过使用金刚石尖端或一个切割晶片的方向平行或垂直于晶片平锋利的对象。执行此步骤的广告万斯，例如凝胶膜的沉积的前一天。 </li><li>只是凝胶的沉积之前，清洗衬底用乙醇，让它们干燥，或使用氮气流或压缩空气，以加速干燥。同时等待完成步骤1.3的执行该步骤。 </li></ol></li><li>涂层薄膜。为了得到均匀的大孔结构执行的20％，并在室温相对湿度55％的条件下，这一步骤。 <ol><li>建立浸涂序列。选择考虑到硅板的实际长度，并在烧杯中的溶液的水平的初始和最终位置，使得铸坯为至少2厘米上方的起始位置的溶液级和1厘米的底部上方烧杯在浸没的末端。设置浸泡和卷取速度150毫米/分钟两者。设置浸渍时间（时间在最终位置）到零。 </li><li>一旦步骤完成1.3到位所谓的烧杯lution在硅板悬挂在浸渍涂布机臂下方一个良好的中心位置。 </li><li>固定在Si板坯到浸渍涂布机臂与夹子的一端，确保板坯尽可能垂直于相对于水平。 </li><li>执行浸涂序列和unclip从浸渍涂布机臂上的硅板。重复步骤2.2.3和2.2.4用另外的硅钢坯，以产生更多层膜，注意不要这些制剂延伸超过1小时，以确保该溶液的稳定性不受损害。 </li></ol></li><li>处置已根据实验室的安全和环保协议被最终产生的解决方案。 </li></ol> 3.凝胶薄膜晶化热处理<ol><li>凝胶薄膜在Si热处理（100）。 <ol><li>从室温加热至1000℃以3℃/分钟，保持在1000℃：方案的炉来执行在空气氛围下的热处理下加热5小时，冷却至RT，在3℃/分钟。 </li><li>放置浸涂Si衬底在氧化铝舟皿，在炉中引入它并执行热处理。 </li></ol></li><li>清洁结晶膜。 <ol><li>浸泡3小时在浓HNO 3的结晶化膜，以除去锶2+的积累已被逐出到膜表面的结晶过程，然后先用离子交换水，然后冲洗所述膜用乙醇。 </li></ol></li></ol>

<ol>
	<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>

作者什么都没有透露。

所提出的方法是一种自下而上的方式产生对大孔硅的石英片。相比生产的石英片的标准方法，一个顶向下的技术的基础上切割和大型水热生长的晶体抛光，在协议中所描述的方法允许获得薄得多薄膜150和450纳米之间的厚度，可与控制回避率。关于石英片厚度，压电响应的控制所有的实验细节文献报道的8.13。通过标准方法获得的石英膜的厚度不能小于10微米，对于大多数应用，这些都需要?...

当像α石英的压电材料被提交给一个电压偏置它经受机械变形。如果该材料是多孔的，这些量的变化可导致毛孔扩张或收缩，产生类似于可在活生物细胞器可以观察到一个响应系统1可变形多孔α-石英已制作使用微细加工，2，但这些技术还不能产生的3-D孔结构，和孔径为几百纳米的数量级上。结构的无定形二氧化硅的结晶受到阻碍而引起高表面能和建筑变形由于粗化和熔化不均匀成核。此外，由于各种形式的二氧化硅，都构建在极其稳定的SiO 4四面体网络中，形成无定形二氧化硅，α石英和其它的 SiO 2多晶型物的自由能在一个宽的温度范围，马金几乎相等克它难以生产α-石英作为来自无定形二氧化硅凝胶的结晶的单一多晶型3的另一个方面，使更硬结构的无定形二氧化硅的控制的结晶是石英呈现出相对较慢的成核速率，但以极快的速度增长， 10-94纳米的报道/秒4,5慢速核加上快速增长往往会产生晶体比原来的纳米多孔结构，因此原来的形态丢失大得多。碱金属， 如 Na +和Li +，已用于结晶α-石英，经常与水热处理组合。5,6-此外，的Ti 4+ / 钙组合物采用结晶二氧化硅的球形颗粒引入石英通过使用硅醇盐的软化学路线7然而，结构化的无定形二氧化硅膜进入石英的控制的结晶仍然是一个挑战。 的 SiO 2的生长。8,9-外延，起因于α石英和&lt;100&gt;的硅衬底之间的有利匹配，生产取向的压电薄膜。蒸发引起的自组装，以产生介孔二氧化硅膜已被用于自1999年10这种技术进行了研究并应用于多种模板剂的各种条件下，以产生可变的尺寸和中间相的孔隙。已经发现，在孔尺寸subnanometric变化对溶质扩散产生巨大影响，通过多孔系统11，验证这个广泛关注孔隙结构。而且，更容易了解内部二氧化硅孔系统可通过控制模板的胶束相而获得。12 这里，合成路径吨帽允许前所未有的控制使用一种新的相分离证实无定形二氧化硅层的厚度和孔径13这些薄膜在环境压力下的空气渗透有锶（II）盐并结晶成α-石英在1000℃。使用这种结晶过程的细孔径可保持被确定，并且壁厚和膜厚度的效果进行了研究。最后，压电和孔系统的变形进行了研究。

<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.

该材料合成的进程通过监测不同的方面进行控制。在浸涂工艺后可以观察的膜的方面中，衍射结构的绿色激光和扫描电子显微镜（SEM）在背散射电子模式 （图1A-B）中的图像的反射光点的最终外观。结晶过程后它记录的原子力显微镜（AFM）的地形图（ 图1C），并通过该膜的X射线衍射得到的极点图，表明α-石英膜之间的外延关系（α-Q是...

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.

化学溶液沉积在硅外延大孔石英薄膜的制备

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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Chemistry

9.2K 次观看.  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. 

视频: 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.

增强型氟烷烃的化学气相沉积等离子通过疏水金属 - 有机骨架的制备氨的去除

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

科研

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.

原子定义模板复合氧化物薄膜的外延生长

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.

化学气相沉积的有机磁体，钒四氰

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.

对磷酸增强富集制备高度多孔配位聚合物涂层的孔聚合物石柱的

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.

对于DNA折纸分析和实验准备云母和硅衬底

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.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

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.

可调谐带隙无针孔 Methylammonium 铅卤化物钙钛矿薄膜的低压蒸气辅助解决工艺

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.

金属氧化物结构的气溶胶辅助化学气相沉积: 氧化锌棒

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.

任意基底上共轭聚合物薄膜的反应气相沉积

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.

织物支架上多孔吸附剂的沉积

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