This material is based upon work supported by the Department of&#160;Energy, National Nuclear Security Administration,&#160;under Award Number DE-NA0002377. Funding from the Defense Threat Reduction Agency (DTRA), Grant Number HDTRA1-10-1-0119. Counter-WMD basic research program, Dr. Suhithi M. Peiris, program director is gratefully acknowledged. This work was also supported by the Ministry of Education and Science and Education of the Russian Federation in the framework of Increase Competitiveness Program of NUST &#8220;MISIS&#8221; grant No. K2-2014-001.

1.高能球磨<ol><li>制备35克初始1：1的摩尔比Ni + Al混合物。在这种情况下，称量11.02克的Al和23.98克镍粉末。 </li><li>使用不锈钢研磨罐为这个系统的高能球磨。确保该罐具有更高的硬度比所述粉末被添加，否则粉末会损坏罐子和污染也会产生。注意：典型罐子选择包括钢，氧化锆，或碳化钨。 </li><li>使用5:1球：粉末（电荷比）为这个系统中， 即 ，175克10毫米钢球。确保球是由相同的材料构成的罐否则无论是球或罐子将被损坏。 注意：荷比定义粉末和研磨剂之间的相互作用的强度。 </li><li>添加球和粉末的瓶子。 </li><li>密封的罐子和瓶子泵大气气体由机械泵和吹扫氩。进行四个周期填充和用Ar气吹洗的（这确保有剩余的罐子没有氧气）。最后，充满氩气罐子略高于（0.13兆帕）的大气压力。 </li><li>插入罐子到行星式球磨机。 </li><li>选择每分钟（rpm）650革命罐的旋转速度和1400的转速的内旋（太阳轮）。 注意：在某些情况下，总和轮（1400转）和碾磨罐（从700至1300转）的转动比（k）中的变化，以调节复合粒子的微观结构。 </li><li>运行该高能球磨过程持续15分钟。注：系统有一个关键的时候，其中所描述的条件，等于17分钟。有研磨，可以在系统上之前反应发生在罐中进行有限数量。如果高能球磨进行长于临界时间，反应将发生在球磨罐，破坏实验。 </li><li>以下的研磨时间结束时，冷却该罐至RT，然后将罐转移到通风橱。<ol><li>发泄的jar删除从最初增压和铣削过程中释放的气体可能多余的气体压力。 </li><li>从通风橱下罐子取下盖子。一定要小心打开罐子时，所形成的粉末是非常活泼。打开罐子戴耐热手套和护目镜。 </li><li>之前收集粉末，将其暴露在空气中至少5分钟，使“钝化”。 注意：这可以防止在处理的混合物中可能出现的自发反应。 </li></ol></li></ol>含能材料2.反应表征<ol><li>收集瓶子的粉末。不要使用金属铲了此过程。 <ol><li>如果分级的颗粒和分离是需要的，利用分子筛。以确保适当的分离完成后，用筛子摇动器在延长的时间周期（12+小时）。分类粉末成各种尺寸的箱（不足10微米，10-20微米，20-53微米，一波夫53微米）。从这时开始，用20-53微米大小的颗粒。 </li></ol></li><li>按筛分成粉末用单轴按设定到1100公斤5毫米的不锈钢冲压模具（1,360兆帕）为2.0分钟的停留时间沉淀。记录与微米颗粒的高度（h）和直径（d）。记录样品（米）带刻度的重量。从这里，确定该粒料的密度。计算出的理论最大密度百分比（TMD％）由下式： <img alt="式（1）" src="/files/ftp_upload/52624/52624eq1.jpg" width="400" /> 其中A 铝 ，A 镍 -铝和镍原子重量; ρ 铝和镍 ρ -铝和镍的密度。假定粉末的化学计量比保持添加的初始粉末的比率。 <ol><li>如果圆柱形粒料被用来确定一个燃烧前缘的传播速度和温度分布在反应前，确保其足够高，由高度和直径之比来确定应≥2（ 例如，D =5毫米; H≥10mm）的。 </li><li>如果粒料被用来定义点火参数，使用一个薄的磁盘（ 例如，直径为5毫米，厚度为1毫米）。 </li></ol></li><li>要定义燃烧特性，将样品到石墨板。 </li><li>使附连到可变变压器一盘绕钨丝。 </li><li>定位在W线圈，使得所述丝的螺旋部分靠在所述粒料的顶部。如果反应系统是氧敏感，为此在无氧的反应室，否则执行在露天进行反应。 </li><li>为了确定燃烧波速，使用来自高速摄像机记录。位置和集中高速热敏相机的测试样品，并开始录制。这将使准确的温度和燃烧速度的信息来收集。 </li><li&gt;慢慢转动可调变压器上，使所述钨丝升温。该反应将开始，然后传播。 </li><li>以获得在燃烧过程中所需要的参数，通过所记录的红外电影的帧进行分析帧。 <ol><li>画出反应正面传播与时间的位置。获得的曲线的斜率平均燃烧速度。 </li><li>积在样品的中间的温度变化的一个点。使用所获得的曲线图，以获得有关反应波的温度时间曲线的信息。 </li></ol></li><li>以限定点火特性（点火温度和点火延迟时间）把薄盘在热板上预热到所需的温度（ 例如，800 K）。需要注意的是，从本实验所得到的精确值将变化显著如果任何参数改变，无论是颗粒的大小，将加热板的温度，或TMD。这个分析对于determinat有用离子的发展趋势。 <ol><li>为了确定点火参数使用高速摄像机。位置和聚焦高速热敏照相机，其中所述的样品将被放置在热板上并开始记录的区域。 注意：这将使过程中精确温度信息。 <ol><li>如果反应是氧敏感，在无氧的反应室执行此。重要提示：运行这个实验中多次赢得了良好的统计数据集。 </li></ol></li><li>把球成为焦点的区域。做这样的方式，所述粒子可以看出在每个帧 - 看到的第一帧，该粒料接触的热板是重要的。 </li><li>以获得所需的点火参数，通过所记录的红外电影的帧进行分析帧。 </li><li>为了确定点火延迟时间，确定第一帧之间的时间，当粒料接触的热板的表面上，以使反应开始。 </LI&gt; <li>为了确定点火温度，标绘在颗粒上的最高温度点。当时间 - 温度分布，从该一预热温度分布到该热炸药制度的开关，拐点匹配点火温度。 </li></ol></li></ol> 3.组织分析利用场发射扫描电子显微镜（FESEM）配备了聚焦离子束（FIB） <ol><li>暂停将0.1g制备的颗粒在10毫升乙醇中并沉积一滴悬浮液上扫描电子显微镜（SEM）样本保持器的表面上。 </li><li>干燥在90℃下将样品保持器5分钟。 </li><li>将样品放入双束FIB / SEM系统。 </li><li>进行抽样等离子体清洗5分钟。注意：这降低了损坏的样品将来自曝光经历于电子束（E-束）的量。 </li><li>把电子束（5千伏，3.5 NA），并专注于一个单个粒子。链接吨他z高度的工作距离，然后抬起样品eucentric高度。 </li><li>利用电子束与气体注射针，沉积铂（70纳米）的初始层样品上，以保护免于降解从使用镓离子束（工字钢）的。 </li><li>倾斜样品52°，然后打开I-横梁上。使用工字钢（5千伏，0.28 NA），再次与气体注射针，沉积铂（0.5微米）的附加层到样品进行保护。 </li><li>削减对样品受托痕迹。磨粒子为矩形形状。这极大地增加了机会，将有足够的信用，因为将有多个切口和角落使用。 </li><li>用程序的辅助下，切片与工字钢的粒子。 <ol><li>选择“文件”，然后“图像保存位置”，选择其中的图像将被存储在目录中。 </li><li>根据单个粒子，选择适当的宽度，LENGTH和深度;通过颗粒的整个体积选择这些完全粉碎。此外，选择的切片的数目，以及每个图像切片的数量。这些选项可以在“切片”选项卡中找到。 </li><li>通过选择“工具”，然后“建议电流”设置束电流。注意：这将允许该程序来选择合适的电子束电流，以磨样品在一个合理的时间，又要防止样品损坏。 </li><li>点击“查看”，软件将提供可视化铣网格，显示了该粒子的部分将被粉碎;确保该铣削网格放置准确在粒子中要被研磨的部分上。 </li><li>每片后，采取了高品质的电子束图像重建以后。要选择合适的电子束的参数，选择“设置”菜单，然后选择“E束图像扫描参数”。 注意：这将得到一种格选择分辨率和停留时间。停留时间越高，更多的时间才能收集的图像。 </li></ol></li><li>利用三维重建软件包，如先前所描述的25重建集从FIB / SEM采集图像。注意：此产生的颗粒，然后可将其用于计算表面区域接触，单个颗粒的孔隙率，漫射层的厚度，以及无数的其他有用的参数的完整三维虚拟副本。 </li></ol>

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作者什么都没有透露。

该协议通过使用短期高能球磨法为制备活性高能（钛+ C的Ta + C的Ni + Al）的纳米复合材料与定制微结构的详细描述。的气腹异构混合物高能球磨涉及它们的处理在高速行星式球磨机，其中该混合物的颗粒进行机械冲击的力足以脆性组分的击穿（ 例如石墨）和变形的塑料部件（ 例如，铝，钛，钽，镍）。脆的反应物被研磨成较细的颗粒，并可能成为无定形的，而塑料的金属经受多种变?...

经典高能材料， 即，炸药，推进剂和烟火是一类材料，具有高含量的储存的化学能，可以在快速的放热反应1-5被释放的，例如，通常通过组合燃料和氧化剂组成生成炸药一个分子。这些材料的能量密度非常高。例如，在分解三硝基甲苯（TNT）释放7.22千焦耳/厘米3，并且形成为每100克（ 表1）气体的8.36摩尔的时间很短的时间。这些材料组成的微米级的有机和无机物质（燃料和氧化剂）的。 铝热剂系统，其中，反应取无机化合物之间发生， 即，还原性金属（ 例如，Al）和氧化物（的Fe 2 O 3，CuO的，铋2 O 3），属于另一类型的高能材料。能量密度（15-21千焦耳/厘米3）这样的系统中的超过的TNT，然而气体产物的量（每100g 0.15-0.6摩尔）典型地比对爆炸物（ 表1）少得多。另外，纳米thermites可能呈现极高速度的燃烧波的传播（&gt; 1,000米/秒）2 ​​-5。 它最近显示6-12，若干气腹异质反应系统（镍+铝，钛+ C的Ti + B）形成金属间或者难熔化合物的也可以被认为是高能材料。这些系统的能量密度（千焦耳/厘米3）的比的TNT（ 表1）的接近或更高。同时，在反应过程中不存在的气体的产品使得这种材料的优异候选者用于各种应用，包括合成的纳米材料，耐火材料和异种份的反应性粘接，气腹微发电机， 等等 11-17。然而，相对这些系统（900-3,000 K， 见表1）相比，thermites（〜1000 K）的atively高燃点温度阻碍了他们的应用程序。工程化纳米复合材料的制备中可以显著提高气腹异构系统12-14，17的点火与燃烧特性。 许多方法已被开发来制造工程改造高能纳米复合材料，如超声波混合18,19，自组装方法如图5所示 ，溶胶-凝胶20-22，气相沉积技术16,17,23,24，以及高能量的球磨（高能球磨）1,5。纳米粉末超声混合的缺点是厚（5-10纳米）氧化物壳上的金属纳米颗粒减小的能量密度，并降低反应混合物的燃烧性能。此外，燃料和氧化剂的分布是不均匀的，并且反应物之间的界面接触不是亲密。溶胶 - 凝胶的●自组装的策略是为编制具体的铝热剂纳米复合材料的发展。尽管是低成本的技术，这些战略都没有从绿色环保的角度来看。而且，大量的杂质被引入到制备复合材料。蒸镀或者磁控溅射用于制备反应性多层箔和芯 - 壳的高能材料。它提供了复合材料的无孔和良好定义的几何形状简化理论建模和提高精度。然而，这种技术是昂贵的并且难以扩大。此外，制备的层状纳米复合材料是不稳定的某些条件。 高能球磨（高能球磨）是一种环境友好，易于扩展的方法，使纳米结构复合材料精力充沛5,9 -14有效的制造。高能球磨便宜且可以与各种反应性材料的组合物（可以使用例如 ，在rmites，形成金属间化合物，碳化物，硼化物等 ）反应。 该协议通过使用短期高能球磨法为制备活性高能（镍+铝，钛+ C钽+ C）纳米复合材料与定制微结构的详细描述。它也描述了一种高速热成像技术来确定，为制造的​​高能材料的点火/燃烧特性。最后，它显示了使用场发射扫描电子显微镜（FESEM）配备了聚焦离子束（FIB）纳米复合材料的微观结构分析。该协议是对不同的精力充沛的纳米材料（无气和铝热剂系统），可以被用作高能量密度的来源或合成和先进的纳米材料的处理通过燃烧为基础的方法的制备方法的重要指南。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Titanium</td>
			<td>Alfa Aesar</td>
			<td>42624</td>
			<td>Particle size: -325 mesh</td>
			<td>Purity, 99.5%</td>
		</tr>
		<tr>
			<td>Graphite</td>
			<td>Alfa Aesar</td>
			<td>46304</td>
			<td>Particle size: 7-11 micron</td>
			<td>Purity, 99%</td>
		</tr>
		<tr>
			<td>Nickel</td>
			<td>Alfa Aesar</td>
			<td>10256</td>
			<td>Particle size: 3-7 micron</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Aluminum</td>
			<td>Alfa Aesar</td>
			<td>11067</td>
			<td>Particle size: -325 mesh</td>
			<td>Purity, 99.5%</td>
		</tr>
		<tr>
			<td>Tantalum</td>
			<td>Materion advanced chemicals</td>
			<td>T-2017</td>
			<td>Particle size: 325 mesh</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Carbon lampblack</td>
			<td>Fisher scientific</td>
			<td>C198-500</td>
			<td>Particle size: 0.1 micron</td>
			<td>Purity, 99.9%</td>
		</tr>
		<tr>
			<td>Tungsten wire</td>
			<td>Mcmaster Carr</td>
			<td>n/a</td>
			<td>0.032&#34; diameter</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Planetary Ball Mill</td>
			<td>Retsch GmbH, Germany</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Uniaxial press</td>
			<td>Carver Hydraulic</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Sieve shaker</td>
			<td>Gilson performer</td>
			<td>n/a</td>
			<td>5mm diameter</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Cylindrical stainless steel press die</td>
			<td>Action Machine</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Stainless steel sieves</td>
			<td>Mcmaster Carr</td>
			<td>Type 304</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>High-speed thermal camera (SC6000)</td>
			<td>FLIR</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Helios NanoLab 600, Field Emission Scanning Electron Microscope (FESEM) Equipped by Focus Ion Beam (FIB)</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Cylindrical reactor with a vacuum pomp</td>
			<td>Action Machine</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Autoslice and View (S&#38;V)</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
		<tr>
			<td>Avizo Fire</td>
			<td>FEI</td>
			<td>n/a</td>
			<td>n/a</td>
			<td>n/a</td>
		</tr>
	</tbody>
</table>

preparation and reactivity of gasless nanostructured energetic materials

高能球磨（高能球磨）是其中的粉末混合物放入球磨机从球经受高能碰撞一个球磨处理。除其他应用中，它是一种通用的技术，其允许有效制剂的气腹活性纳米结构材料具有高能量密度的单位体积（镍+以Al，Ta + C的Ti + C）。反应介质的结构转变，其中高能球磨过程中发生的，确定的生产充满活力的复合材料的反应机制。改变加工条件允许制造复合颗粒的研磨引起的微观结构中的微调。反过来，反应性， 即 ，自燃温度，点火延迟时间，以及反应动力学，高能量密度的材料取决于其微观结构。铣削诱导的微结构的分析表明，的试剂之间新鲜无氧亲密高表面积接触形成我š负责它们的反应性的提高。这表现在降低点火温度和延迟时间，化学反应的速率增加，反应的有效活化能的整体下降。该协议提供了使用短期高能球磨法定制微结构反应性的纳米复合材料的制备方法的详细描述。它也描述了一种高速热成像技术来确定高能材料的点火/燃烧特性。该协议可以适于制备各种纳米结构的复合材料有活力和表征。

为了制备纳米结构的复合材料有活力，希望的粉末组分的混合物（通常是微米尺寸）的预设的研磨条件下进行机械处理。处理时间（通常为几分钟）被精确地控制，以产生组成上均化的纳米复合材料的颗粒，但不允许在自立化学反应研磨期间启动。 图1和视频1表明，在复合颗粒增加几个数量级的反应物之间的接触表面面积相比，初始混合物中。高能?...

Watch this Scientific Journal Video about Preparation and Reactivity of Gasless Nanostructured Energetic Materials at JoVE.com

Preparation and Reactivity of Gasless Nanostructured Energetic Materials

本协议描述的自保纳米结构的高能材料（镍+铝，钽+ C，钛+ C）使用短期高能球磨（高能球磨）技术的准备。它还描述研究的机械制造纳米复合材料的反应性的高速热成像方法。这些协议可以扩展到其它的反应性纳米结构的高能材料。

准备和无气腹纳米结构的反应含能材料

High-Energy Ball Milling (HEBM) is a ball milling process where a powder mixture placed in the ball mill is subjected to high-energy collisions from the ...

preparation-reactivity-gasless-nanostructured-energetic

Research

JoVE Journal

Engineering

10.1K 次观看.  University of Notre Dame. 本协议描述的自保纳米结构的高能材料（镍+铝，钽+ C，钛+ C）使用短期高能球磨（高能球磨）技术的准备。它还描述研究的机械制造纳米复合材料的反应性的高速热成像方法。这些协议可以扩展到其它的反应性纳米结构的高能材料。 

视频: Preparation and Reactivity of Gasless Nanostructured Energetic Materials

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

钮扣电池锂离子电池的建设和测试

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

科研

工程学

Nanomoulding of Functional Materials, a Versatile Complementary Pattern Replication Method to Nanoimprinting

We describe a nanomoulding technique which allows low-cost nanoscale patterning of functional materials, materials stacks and full devices. Nanomoulding combined with layer transfer enables the replication of arbitrary surface patterns from a master structure onto the functional material. Nanomoulding can be performed on any nanoimprinting setup and can be applied to a wide range of materials and deposition processes. In particular we demonstrate the fabrication of patterned transparent zinc oxide electrodes for light trapping applications in solar cells.

We describe a nanomoulding technique which allows low-cost nanoscale patterning of functional materials, materials stacks and full devices. Nanomoulding can be performed on any nanoimprinting setup and can be applied to a wide range of materials and deposition processes.

Nanomoulding功能材料，灵活的互补模式的复制方法，以奈米

We describe a nanomoulding technique which  allows low-cost nanoscale patterning of functional materials, materials stacks  and full devices. Nanomoulding ...

Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. Thus, understanding of spatial variations in composition as well as electrical properties of OPV materials is of paramount importance for moving PV technology forward.1,2 In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution. Currently, materials properties measurements performed using commercially available AFM-based techniques (PeakForce, conductive AFM) generally provide only qualitative information. The values for resistance as well as Young's modulus measured using our method on the prototypical ITO/PEDOT:PSS/P3HT:PC61BM system correspond well with literature data. The P3HT:PC61BM blend separates onto PC61BM-rich and P3HT-rich domains. Mechanical properties of PC61BM-rich and P3HT-rich domains are different, which allows for domain attribution on the surface of the film. Importantly, combining mechanical and electrical data allows for correlation of the domain structure on the surface of the film with electrical properties variation measured through the thickness of the film.

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution.

并行定量的导电性和力学性能测试的有机光伏材料利用原子力显微镜

Organic photovoltaic  (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale  inhomogeneity of OPV materials affects performance ...

Characterization of Thermal Transport in One-dimensional Solid Materials

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials, including conductive, semi-conductive or nonconductive one-dimensional structures. This technique broadens the measurement scope of materials (conductive and nonconductive) and improves the accuracy and stability. If the sample (especially biomaterials, such as human head hair, spider silk, and silkworm silk) is not conductive, it will be coated with a gold layer to make it electronically conductive. The effect of parasitic conduction and radiative losses on the thermal diffusivity can be subtracted during data processing. Then the real thermal conductivity can be calculated with the given value of volume-based specific heat (&#961;cp), which can be obtained from calibration, noncontact photo-thermal technique or measuring the density and specific heat separately. In this work, human head hair samples are used to show how to set up the experiment, process the experimental data, and subtract the effect of parasitic conduction and radiative losses.

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials.

在一维固体材料的热传输的特性

The TET (transient electro-thermal) technique is an effective approach developed to measure the thermal diffusivity of solid materials, including ...

Preparation and Friction Force Microscopy Measurements of Immiscible, Opposing Polymer Brushes

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low friction at the interface. Nevertheless, these systems can be sensitive to wear due to interdigitation of the opposing brushes. In a recent publication, we have shown via molecular dynamics simulations and atomic force microscopy experiments, that using an immiscible polymer brush system terminating the substrate and the slider surfaces, respectively, can eliminate such interdigitation. As a consequence, wear in the contacts is reduced. Moreover, the friction force is two orders of magnitude lower compared to traditional miscible polymer brush systems. This newly proposed system therefore holds great potential for application in industry. Here, the methodology to construct an immiscible polymer brush system of two different brushes each solvated by their own preferred solvent is presented. The procedure how to graft poly(N-isopropylacrylamide) (PNIPAM) from a flat surface and poly(methyl methacrylate) (PMMA) from an atomic force microscopy (AFM) colloidal probe is described. PNIPAM is solvated in water and PMMA in acetophenone. Via friction force AFM measurements, it is shown that the friction for this system is indeed reduced by two orders of magnitude compared to the miscible system of PMMA on PMMA solvated in acetophenone.

The methodology to perform friction force microscopy experiments for contacting brushes is presented: Two polymer brushes that are grafted from (a) substrates and (b) colloidal probes are slid to show that, by using two contacting immiscible brush systems, friction in sliding contacts is reduced compared to miscible brush systems.

互溶的测量准备和摩擦力显微镜，反对聚合物刷

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low ...

Surface Enhanced Raman Spectroscopy Detection of Biomolecules Using EBL Fabricated Nanostructured Substrates

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules is reported. The entire sequence of relevant experimental steps is described, involving the fabrication of nanostructured substrates using electron beam lithography, immobilization of biomolecules on the substrates, and their characterization utilizing surface-enhanced Raman spectroscopy (SERS). Three different designs of nano-biological systems are employed, including protein A, glucose binding protein, and a dopamine binding DNA aptamer. In the latter two cases, the binding of respective ligands, D-glucose and dopamine, is also included. The three kinds of biomolecules are immobilized on nanostructured substrates by different methods, and the results of SERS imaging are reported. The capabilities of SERS to detect vibrational modes from surface-immobilized proteins, as well as to capture the protein-ligand and aptamer-ligand binding are demonstrated. The results also illustrate the influence of the surface nanostructure geometry, biomolecules immobilization strategy, Raman activity of the molecules and presence or absence of the ligand binding on the SERS spectra acquired.

We describe the fabrication and characterization of nano-biological systems interfacing nanostructured substrates with immobilized proteins and aptamers. The relevant experimental steps involving lithographic fabrication of nanostructured substrates, bio-functionalization, and surface-enhanced Raman spectroscopy (SERS) characterization, are reported. SERS detection of surface-immobilized proteins, and probing of protein-ligand and aptamer-ligand binding is demonstrated.

表面增强拉曼光谱检测生物分子利用EBL装配纳米衬底

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules ...

Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. Additionally, most reported graphene assemblies are held together through physical interactions (e.g., van der Waals forces) rather than chemical bonds, which limit their mechanical strength and conductivity. This video method details recently developed strategies to fabricate mass-producible, graphene-based bulk materials derived from either polymer foams or single layer graphene oxide. These materials consist primarily of individual graphene sheets connected through covalently bound carbon linkers. They maintain the favorable properties of graphene such as high surface area and high electrical and thermal conductivity, combined with tunable pore morphology and exceptional mechanical strength and elasticity. This flexible synthetic method can be extended to the fabrication of polymer/carbon nanotube (CNT) and polymer/graphene oxide (GO) composite materials. Furthermore, additional post-synthetic functionalization with anthraquinone is described, which enables a dramatic increase in charge storage performance in supercapacitor applications.

This video method describes the synthesis of high surface area, monolithic 3D graphene-based materials derived from polymer precursors as well as single layer graphene oxide.

合成和3D纳米石墨烯材料的功能化：石墨烯气凝胶和石墨烯宏组件

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. ...

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

纳米银沸石复合材料作为基于发光的湿度传感器

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

通过纳米氧化钇稳定的二氧化锆（YSZ）的支架的高温加工<em&gt;原位</em&gt;碳模板干凝胶

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.