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1，准备和PS-B-P4VP的表征（PDP）配合双Gyroid形态<ol><li>称出聚苯乙烯- 嵌段 -聚（4 -乙烯基吡啶）（PS-β-P4VP）和十五烷基苯酚（PDP中，M R =304.51克/摩尔）。为了获得gyroid形态，（根据线性AB二嵌段共聚物的相图P4VP（PDP）的嵌段的重量分数（F P4VP（PDP））应为约 0.6），小心地选择PDP的量应。通常，0.15-0.2克共聚物PS-b-P4VP的导致共聚物PS-b-P4VP（PDP）的膜为50〜100μm厚的（假定在步骤1.3中使用的培养皿的直径为5-6厘米）。根据下面的公式计算出的PDP的量: <img alt="式（1）" src="/files/ftp_upload/50673/50673eq1.jpg" /> <img alt="公式2" src="/files/ftp_upload/50673/50673eq2.jpg" /> <img alt="式（3）" src="/files/ftp_upload/50673/50673eq3.jpg" /><br/&gt; <img alt="公式4" src="/files/ftp_upload/50673/50673eq4.jpg" /></li><li>溶解共聚物PS-b-P4VP和PDP的氯仿，搅拌了几个小时，在室温下进行。保持低于2％（重量）的聚合物的浓度，以确保均匀的复合物的形成。 </li><li>将溶液倾入玻璃培养皿。 </li><li>将菜成饱和氯仿气氛。 </li><li>大约一个星期后，取出培养皿。超分子配合物的膜。 </li><li>干燥在真空薄膜在30℃下过夜。 </li><li>将膜在一个专门设计的容器中，从容器中除去空气，然后用氮气填充。 氮气气氛中以1巴的过压之下退火的薄膜在烘箱中4天120℃。 </li><li>切小片的电影，嵌入在环氧树脂和隔夜治愈它在40°C。 </li><li>样切片机用金刚石刀在室温下的厚度为约80nm。钍Ë显微切片部分会浮在水面上。接他们，并放置在铜网格。 </li><li>将含有该路段显微切片电网与碘罐。 45分钟后样品染色并准备好透射电子显微镜。 </li><li>插入的Cu网格与在透射型电子显微镜以120千伏和图像样本的加速电压下工作染色的切片。 </li><li>插入件的膜（步骤1.7之后获得）放入样品架用于小角X射线散射和带卡普顿胶带固定。将制备好的样品架插入机器的SAXS。打开X射线快门，并获得二维散射图案。整合所获得的2D模式，并分析在一维模式峰的位置。 </li></ol> 2，生成多孔结构与表征<ol><li>把一块膜（步骤1.7后获得）的乙醇，并保持了三天。 </li><li>干燥样品。 </li><li>预削时的样品1 H-NMR测量。溶解PDP粉，PS-B-P4VP粉，超分子复杂的PS-B-P4VP（PDP）（步骤1.7之后），并且多孔膜（步骤2.2以后）在CDCl 3中。在室温下记录1 H-NMR谱。 </li><li>分析PS-B-P4VP粉，超分子复杂的PS-B-P4VP（PDP）（步骤1.7之后），和多孔膜（步骤2.2后）用差示扫描量热法。使用的调制模式，用一个加热/冷却速率为1℃/分钟，0.5℃的振幅和60秒的振荡周期。平衡的样品在-30℃下，加热至180℃，冷却至-30℃，然后再加热到180℃。使用从第二加热循环中的数据进行分析。 </li><li>除气在多孔样品（步骤2.2之后）为8小时，在室温下和18小时，在70℃，并在77 K进行氮吸附测量</li><li>使用适当的软件（例如，WinADP）和模型来分析所得到的吸附等温线。 </li><li>干燥该多孔样品（步骤2.2之后），在50℃下进行8小时，脱气它在2小时室温下的0.5 Pa和压力。 </li><li>进行压汞法。 </li></ol> 3，插入镍在聚合物模板<ol><li>称取氯化锡（氯化亚锡2，M R =189.60克/摩尔），并调制成水溶液（0.1M氯化亚锡2 / 0.1 M盐酸;1.896克氯化亚锡 ，0.8毫升盐酸，和100毫升H 2 O）。把在振荡器上过夜溶液保证的SnCl 2的完全溶解。 </li><li>称出氯化钯（中PdCl 2，M R =177.33克/摩尔）和制备水 ​​溶液（0.0014 M中PdCl 2 / 0.25 M盐酸;0.025克中PdCl 2，将2ml的HCl和100毫升H 2 O）。 </li><li>准备镍镀液的组成部分1:称取6.78克六水合硫酸镍（硫酸镍4•6H 2 O，M R = 2620.85克/摩尔）和2克柠檬酸钠（Na 3 C 6 H 5 O 7，M R =258.06克/摩尔）和溶解它们在80毫升的水中。加入828微升85％乳酸（C 3 H 6 O 3，M R =90.08克/摩尔）。 </li><li>准备镍镀液中的第2部分:重出0.2克硼烷二甲基胺（（CH 3）2 NHBH 3，M R =58.92克/摩尔），溶于20毫升水中。硼烷二甲胺复杂的，应在通风良好的通风橱内进行处理。 </li><li>在氯化锡（步骤3.1）中1小时的水溶液浸渍多孔膜（步骤2.2之后）。 </li><li>用去离子水彻底冲洗胶片。 </li><li>中的氯化钯（步骤3.2）中1小时的水溶液浸渍膜。 </li><li>用去离子水彻底冲洗胶片。 </li><li>混合第1部分（3.3）和镍镀液的组成部分2（3.4）。用氢氧化铵调节pH至7.0。 </li><li>在镍电镀浴中1小时，将其浸入膜。 </li><li>用去离子水彻底冲洗胶片。 </li><li>干燥样品。 </li><li>制备的镀覆样品用于电子显微镜如在步骤1.8-1.9中描述。 </li><li>图像如在步骤1.11中描述的样品。 </li><li>插入包含​​镀样品中的高分辨率透射电子显微镜的截面铜网格。获取高分辨率的TEM照片。观察样本在显微镜下，选择通过EDX（X射线能量色散分析）元素分析的区域。执行所选择的区域的EDX分析，并分析所获得的图案。 </li></ol> 4，曝光的逆Gyroid泡沫镍<ol><li>把镀镍膜（步骤3.12后）在烘箱中于350℃，并保持1小时至4天。 </li><li>使用银糊样品附着到样品架。 </li><li>将样品放入扫描电子麦克风roscope。采集样品的多个图像。 </li><li>将样品放入扫描电子显微镜。观察样品，在显微镜下，选择用于通过EDX元素分析的区域。执行所选择的区域的EDX分析，并分析所获得的图案。 </li></ol>

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M., Wiesner, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+plumber's+nightmare:+a+new+morphology+in+block+copolymer-ceramic+nanocomposites+and+mesoporous+aluminosilicates.">The plumber's nightmare: a new morphology in block copolymer-ceramic nanocomposites and mesoporous aluminosilicates.</a> J. Am. Chem. Soc. 125, 13084-13093 (2003).</li><li>Tyler, C. A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthorhombic+Fddd+network+in+triblock+and+diblock+copolymer+melts.">Orthorhombic Fddd network in triblock and diblock copolymer melts.</a> Phys. Rev. Lett. 94, 208-302 (2005).</li><li>Ranjan, A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Landau+theory+of+the+orthorhombic+Fddd+phase.">Landau theory of the orthorhombic Fddd phase.</a> Phys. Rev. E. 74, 011803 (2006).</li><li>Kim, M. I., 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=Stability+of+the+Fddd+Phase+in+Diblock+Copolymer+Melts.">Stability of the Fddd Phase in Diblock Copolymer Melts.</a> Macromolecules. 41, 7667-7670 (2008).</li></ol>

作者宣称没有竞争的财务权益。

超分子复合物的前体秩序井然金属nanofoams成功应用。在该方法中，关键的步骤是获得合适的模板， 即与gyroid形态的模板。在嵌段共聚物的相图的gyroid区域是非常小的，这是相当困难的目标。这意味着，如果常规的嵌段共聚物被用作起始原料时，相当精细的合成必须被重复，直到所希望的组合物，其引起的gyroid形态，就达到了。在共聚物PS-b-P4VP（PDP）的配合物不同的组合物，并且因此...

有可用于金属nanofoams准备几种方法:去合金1-3，溶胶-凝胶方法4,5，nanosmelting 6,7和燃烧合成8。在脱合金过程中，起始材料通常是二元合金，例如，银和金的合金。越少的贵金属银，在这种情况下，可通过化学或电化学产生了无序多孔金泡沫与纳米韧带除去。在燃烧合成，金属是一个充满活力的前体，它在分解过程中释放出能量和驱动器的金属nanofoam 8形成的混合。研究的金属泡沫材料的机械性能表明，在无序结构的应力不能被有效地从韧带纳米发送到整体宏观9-11，因此良好有序金属nanofoams预期相比，具有优越的机械性能无序的。 这里所表示的想法是使用嵌段共聚物自组装成有序的纳米结构前体对金属nanofoams。取决于嵌段共聚物中，单体单元的总数，并经化学连接块之间的斥力的范围的组成，各种形态出现，例如:球形，圆柱形，薄片状，双gyroid，六角形层状穿孔，而其他12-14 。此外，聚合物嵌段可以选择性地降解，导致纳米多孔材料15。最常用的方法包括:臭氧分解16-18，UV照射19，反应离子蚀刻20-22和23-26的溶解。所产生的多孔结构可被回填与各种无机材料。金属氧化物（ 如 SiO 2的，TiO 2的）通常是通过溶胶-凝胶法引入到模板的通道27-29。萨尔瓦多ectrochemical和电解电镀，通常用于沉积金属之中或之上的模板30-33。最后，将剩余的聚合物可以从通过热解2，溶解34,35，紫外线劣化28,29 等的聚合物/无机纳米杂化物去除在我们的方法中，我们从聚苯乙烯- 嵌段 -聚（4 -乙烯基吡啶）的超分子复合物（PS-B-P4VP）嵌段共聚物和两亲十五烷基苯酚（PDP）的分子开始。这是复杂的PDP和吡啶环（ 图1a）之间的氢键的结果。起始嵌段共聚物的组合物和加入的PDP的量被选择在这样一种方式，所得到的体系自组装在双连续双gyroid形态与PS网络和一个P4VP（PDP）的基体（ 图1b）。 PDP分子变成选择性地溶解于乙醇和P4VP链崩溃到PS网络（图1c）。接着，用无电解电镀法，镍被沉积到模板（ 图1d）的孔中。 通过热分解除去残留的聚合物后，一个有序gyroid镍nanofoam得到（ 图1e）。

<table border="1">
 <tbody>
 <tr>
 <td>REAGENTS:</td>
 <td></td>
 <td></td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP, CAS: 26222-40-2</td>
 <td>Polymer Source Inc.</td>
 <td>P9009-S4VP 
 P136-S4VP 
 P5462-S4VP 
 P3912-S4VP</td>
 <td>additional information are provided in a separate table</td>
 </tr>
 <tr>
 <td>PDP</td>
 <td>Aldrich</td>
 <td>P4402-100G-A</td>
 <td>recrystallized twice from petroleum ether</td>
 </tr>
 <tr>
 <td>SnCl2</td>
 <td>Acros Organics</td>
 <td>196981000</td>
 <td></td>
 </tr>
 <tr>
 <td>PdCl2</td>
 <td>Aldrich</td>
 <td>76050</td>
 <td></td>
 </tr>
 <tr>
 <td>NiSO4 x H2O</td>
 <td>Sigma-Aldrich</td>
 <td>227676</td>
 <td></td>
 </tr>
 <tr>
 <td>lactic acid</td>
 <td>Aldrich</td>
 <td>W261106</td>
 <td></td>
 </tr>
 <tr>
 <td>citric acid trisodium salt</td>
 <td>Sigma-Aldrich</td>
 <td>C3674</td>
 <td></td>
 </tr>
 <tr>
 <td>borane dimethyl amine complex</td>
 <td>Aldrich</td>
 <td>180238</td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP catalogue number</td>
 <td>Mn (PS), g/mol</td>
 <td>Mn(P4VP), g/mol</td>
 <td>PDI</td>
 </tr>
 <tr>
 <td>P9009-S4VP</td>
 <td>24000</td>
 <td>9500</td>
 <td>1.1</td>
 </tr>
 <tr>
 <td>P136-S4VP</td>
 <td>31900</td>
 <td>13200</td>
 <td>1.08</td>
 </tr>
 <tr>
 <td>P5462-S4VP</td>
 <td>37500</td>
 <td>16000</td>
 <td>1.3</td>
 </tr>
 <tr>
 <td>P3912-S4VP</td>
 <td>41500</td>
 <td>17500</td>
 <td>1.07</td>
 </tr>
 </tbody>
</table>

gyroid nickel nanostructures from diblock copolymer supramolecules

纳米多孔金属泡沫体具有以下特性的独特组合， - 它们的催化活性，热和电传导性，而且，具有高孔隙率，高的表面与体积之和的强度 - 重量比。不幸的是，用于制备金属纳米结构的常见的方法使材料具有高度无序的结构，它可能对它们的机械性能有不利影响。嵌段共聚物具有的能力，以自组装成有序的纳米结构，并且可以作为用于良好有序金属nanofoams制备模板被应用。这里我们描述的嵌段共聚物为基础的超分子复合物的应用-聚苯乙烯- 嵌段 -聚（4 -乙烯基吡啶）（十五烷基）共聚物PS-b-P4VP（PDP） -作为前体为良序镍nanofoam。超分子复合物表现出类似传统嵌段共聚物的相行为，可以自组装成的双连续gyroid形态机智放置在P4VP（PDP）矩阵H两个PS网络。 PDP可以被溶解在乙醇中，导致可与金属回填多孔结构的形成。利用无电解镀法，镀镍可被插入到模板的通道。最后，将剩余的聚合物可通过从产生纳米多孔泡沫镍与逆gyroid形态学的聚合物/无机纳米杂化物的热解被除去。

。超分子复合物的形态共聚物PS-b-P4VP（PDP）x由TEM和SAXS 图2a检查和2b显示的代表超分子配合物的典型gyroid模式:双波和已知代表货车轮图案通过（211）突起和（111）面的gyroid单元电池分别。 PS块域显得明亮而P4VP（PDP）×块域出现暗由于碘染色。 图2c代表了不同的gyroid样品，其中的周期性下降时用2。SAXS峰的一个因素的双波模式位置:√6Q *√8Q *√14Q *√22q的...

Watch this Scientific Journal Video about Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules at JoVE.com

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

本文介绍了有序的镍nanofoams 通过电镀金属沉积制备从上自组装嵌段共聚物为基础获得的超分子纳米多孔模板。

Gyroid镍纳米结构的嵌段共聚物超分子

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

gyroid-nickel-nanostructures-from-diblock-copolymer-supramolecules

Research

JoVE Journal

Chemistry

12.4K 次观看.  University of Groningen. 本文介绍了有序的镍nanofoams 通过电镀金属沉积制备从上自组装嵌段共聚物为基础获得的超分子纳米多孔模板。 

视频: Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nucleoside Triphosphates - From Synthesis to Biochemical Characterization

The traditional strategy for the introduction of chemical functionalities is the use of solid-phase synthesis by appending suitably modified phosphoramidite precursors to the nascent chain. However, the conditions used during the synthesis and the restriction to rather short sequences hamper the applicability of this methodology. On the other hand, modified nucleoside triphosphates are activated building blocks that have been employed for the mild introduction of numerous functional groups into nucleic acids, a strategy that paves the way for the use of modified nucleic acids in a wide-ranging palette of practical applications such as functional tagging and generation of ribozymes and DNAzymes. One of the major challenges resides in the intricacy of the methodology leading to the isolation and characterization of these nucleoside analogues.
	
	In this video article, we present a detailed protocol for the synthesis of these modified analogues using phosphorous(III)-based reagents. In addition, the procedure for their biochemical characterization is divulged, with a special emphasis on primer extension reactions and TdT tailing polymerization. This detailed protocol will be of use for the crafting of modified dNTPs and their further use in chemical biology.

The protocol described herein aims to explain and abridge the numerous obstacles in the way of the intricate route leading to modified nucleoside triphosphates. Consequently, this protocol facilitates both the synthesis of these activated building-blocks and their availability for practical applications.

核苷三磷酸 - 从合成到生化特征

The  traditional strategy for the introduction of chemical functionalities is the  use of solid-phase synthesis by appending suitably modified ...

科研

化学

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

a硫磺共聚物基质内的免费配体硫化镉纳米粒子的合成

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

一个两亲性共聚物的阴离子聚合通过π-π堆积作用稳定嵌段共聚物胶束的制备

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

形状-各向异性胶体镉硫纳米结构的 Facet-to-facet 连接

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

铂镍纳米线的合成及减氧性能优化

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

化学沉淀法合成铌2O5改性高比表面积镍催化剂

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

C 型60/石墨烯混合纳米结构的制备与表征

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to diversify the fiber choices in the United States body armor market, copolymer fibers based on the combination of 5-amino-2-(p-aminophenyl) benzimidazole (PBIA) and the more conventional PPTA were introduced. Little is known regarding the long-term stability of these fibers, but as condensation polymers, they are expected to have potential sensitivity to moisture and humidity. Therefore, characterizing the strength of the materials and understanding their vulnerability to environmental conditions is important for evaluating their use lifetime in safety applications. Ballistic resistance and other critical structural properties of these fibers are predicated on their strength. To accurately determine the strength of the individual fibers, it is necessary to disentangle them from the yarn without introducing any damage. Three aramid-based copolymer fibers were selected for the study. The fibers were washed with acetone followed by methanol to remove an organic coating that held the individual fibers in each yarn bundle together. This coating makes it difficult to separate single fibers from the yarn bundle for mechanical testing without damaging the fibers and affecting their strength. After washing, fourier transform infrared (FTIR) spectroscopy was performed on both washed and unwashed samples and the results were compared. This experiment has shown that there are no significant variations in the spectra of poly(p-phenylene-benzimidazole-terephthalamide-co-p-phenylene terephthalamide) (PBIA-co-PPTA1) and PBIA-co-PPTA3 after washing, and only a small variation in intensity for PBIA. This indicates that the acetone and methanol rinses are not adversely affecting the fibers and causing chemical degradation. Additionally, single fiber tensile testing was performed on the washed fibers to characterize their initial tensile strength and strain to failure, and compare those to other reported values. Iterative procedural development was necessary to find a successful method for performing tensile testing on these fibers.

The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation.

解析高强共聚物芳纶纤维使其力学性能的测定

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to ...

Stable DNA Motifs, 1D and 2D Nanostructures Constructed from Small Circular DNA Molecules

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D DNA nanostructures. Over decades, the rapid development of DNA nanotechnology is attributed to the use of linear DNAs as the source materials. For example, the DAO (double crossover, antiparallel, odd half-turns) tile is well-known as a building block for construction of 2D DNA lattices; the core structure of DAO is made from two linear single-stranded (ss) oligonucleotides, like two ropes making a right hand granny&#160;knot. Herein, a new type of DNA tiles called cDAO (coupled DAO) are built using a small circular ss-DNA of c64nt or c84nt (circular 64 or 84 nucleotides) as the scaffold strand and several linear ss-DNAs as the staple strands. Perfect 1D and 2D nanostructures are assembled from cDAO tiles: infinite nanowires, nanospirals, nanotubes, nanoribbons; and finite nano-rectangles. Detailed protocols are described: 1) preparation by T4 ligase and purification by denaturing PAGE (polyacrylamide gel electrophoresis) of small circular oligonucleotides, 2) annealing of stable circular tiles, followed by native PAGE analysis, 3) assembling of infinite 1D nanowires, nanorings, nanospirals, infinite 2D lattices of nanotubes and nanoribbons, and finite 2D nano-rectangles, followed by AFM (Atomic Force Microscopy) imaging. The method is simple, robust, and affordable for most labs.

This article presents a detailed protocol for T4 ligation and denaturing PAGE purification of small circular DNA molecules, annealing and native PAGE analysis of circular tiles, assembling and AFM imaging of 1D and 2D DNA nanostructures, as well as agarose gel electrophoresis and centrifugation purification of finite DNA nanostructures.

由小圆形 DNA 分子构建的稳定 DNA 分子、一维和二维纳米结构

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D ...

Gene-therapy Inspired Polycation Coating for Protection of DNA Origami Nanostructures

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in physiological fluids induce denaturation and degradation of self-assembled DNA nanostructures. In non-viral gene delivery, enzymatic degradation of DNA is overcome by the encapsulation of the negatively charged DNA in a cationic shell. Herein, inspired by gene delivery advancements, a simple, one-step and robust methodology is presented for the stabilization of DNA origami nanostructures by coating them with chitosan and linear polyethyleneimine. The polycation coating efficiently protects DNA origami nanostructures in Mg-depleted and nuclease-rich media. This method also preserves the full addressability of enzyme- and aptamer-based functionalization of DNA nanostructures.

Here, a protocol for the protection of DNA origami nanostructures in Mg-depleted and nuclease-rich media using natural cationic polysaccharide chitosan and synthetic linear polyethyleneimine (LPEI) coatings is presented.

基因治疗诱导聚化涂层保护 dna 折纸纳米结构

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in ...