C.R.C. would like to acknowledge the Ramsay Memorial Trust for funding.

1.硒化镉/ ZnS核/壳量子点的制备<ol><li> 在三辛基的制备（TOP）-Se解决方案 <ol><li>通过在氮气下或者在手套箱硒适量混入TOP的Schlenk烧瓶（每个反应8需要毫升，通常为0.4克浓度在10毫升的TOP）制备硒的TOP中的0.5M的溶液。 </li><li>搅拌该混合物以溶解硒1小时，从而在TOP-硒复合物的灰色溶液。 </li><li>确保溶液然后冷冻 - 泵 - 解冻脱气5次。将所得储备溶液可以在氮气下储存3个月。 </li></ol></li><li> 在核心的CdSe的制备 <ol><li>称出镉氧化物（51毫克，0.4毫摩尔），顶部氧化物（3.7克，9.6毫摩尔），十六烷基胺（1.93克，8毫摩尔）和1-十二烷基膦酸（0.22克，0.88毫摩尔）和结合成一个三颈250毫升圆底烧瓶中。添加搅拌棒。 </li><li>关闭两个颈部用隔膜和保证第三附连到长回流冷凝器和氮气/真空的Schlenk线。通过一个隔膜插入一个加热罩温度探头直接到混合物中。泵/用氮气再填充烧瓶五次。 </li><li>加热烧瓶至320℃，并在氮气氛下搅拌1小时熔化。 </li><li>降低壁炉的至270℃的温度，然后用大的注射器和大口径针（20毫升为3mm孔）脱气用氮气5次。 </li><li>采取了8个毫升TOP-硒溶液（步骤1.1）的，并仔细但迅速注入到三颈烧瓶中，通过隔膜。 </li><li>搅拌在270℃下进行30秒分钟之间和10，以控制产生的颗粒的大小的反应。对于红光（〜600纳米），7-9分钟为宜。 </li><li>制备沸水（大到足以浸没在反应容器的一半）下向反应混合物和地点的碗。反应时间结束后，迅速冷却在boili反应纳克水漩。 小心:冷却可导致烧瓶破裂。以极大的关怀和穿着厚厚的防渗透手套。 </li><li>一旦冷却，注入10ml氯仿入烧瓶以溶解所有产品，并划分两个50毫升离心管之间的混合物。 </li><li>顶端的每个管高达50毫升EtOH中并离心在3,600×g的10分钟以沉淀颗粒。弃去上清液，并在总共10毫升正己烷的再分散的粒料。 </li></ol></li><li> 在CdSe核的ZnS，脱壳: <ol><li>的己烷添加芯到100毫升圆底烧瓶中含有锌二乙基二（0.5克，1.4毫摩尔），油胺（3毫升，9.12毫摩尔），三辛基膦（3毫升，6.73毫摩尔）和1-十八碳烯（10毫升）中。添加搅拌棒。交换反应气氛氮气。 </li><li>热在部分真空下3.3℃/分钟的加热板，搅拌器的反应，直至70℃，并使用的Schlenk线去除己烷。 </li&gt; <li>气氛切换为氮气，继续加热以这样的速率到120℃。搅拌在120℃下进行2小时。 </li><li>让反应冷却，并分成2×50毫升离心管之间的混合物。确保将管加满至50ml用EtOH在3,600×g下使粒子沉淀，离心10分钟。 </li><li>弃去上清液，并在总共10毫升正己烷的再分散的粒料。 </li><li>离心该溶液（3 600 XG，10分钟）再次以除去任何不溶性杂质，被倾入一个样品管之前，并储存在冰箱（4℃）在氮气氛下长达三个月。 </li></ol></li></ol> 2.纳米颗粒的封装肿胀到PDMS <ol><li> 肿胀液的配制: <ol><li>通过混合36毫升正己烷用4ml的CdSe量子点分散体（如合成）制备的CdSe量子点的储备溶液和磁力搅拌该溶液中。&lt;/ LI&gt; <li>预留每个由9毫升原液作为指定肿胀溶液两小瓶。 </li><li>使用的原液的不同QD浓度的进一步肿胀方案编制的剩余部分。通过稀释原液，得到66％（体积/体积）溶液，50％溶液和33％的溶液制备降低QD浓度三个肿胀的解决方案。 <ol><li>通过混合6毫升所述的CdSe QD原液用3毫升正己烷制备66％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li><li>通过混合4.5毫升所述的CdSe QD原液用4.5毫升正己烷制备50％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li><li>通过混合将3ml的CdSe QD原液用6ml正己烷制备33％（体积/体积）溶液。搅拌溶液磁，以确保完全混合。 </li></ol></li><li>存储所有黑暗的条件下，QD的解决方案，在室温下。&lt;/ LI&gt; </ol></li><li> 聚合物的制备和QD融合-在改变肿胀液的浓度QD: <ol><li>剪下用一个新的手术刀刀片四家医疗级硅胶广场（11毫米×11毫米）。 </li><li>在每个不同％QD浓度的四个溶胀溶液的浸入医用级硅氧烷正方形:储备溶液，66％（V / V），50％（体积/体积）和33％（体积/体积）。允许聚合物样品溶胀黑暗条件下24小时，并在室温下。 </li><li> 48小时，在此期间中的残留溶剂蒸发，聚合物收缩回其初始尺寸除去黑暗条件下从相应的溶胀溶液和空气干燥溶胀的聚合物样品。 </li><li>用去离子水彻底清洗QD-掺入样品以除去任何表面结合的材料。 </li></ol></li><li> 聚合物的制备和QD融合-改变聚合物曝光时间去肿解决方案: </strong&gt;的<ol><li>制备四种多医用级硅氧烷正方形（11毫米×11毫米），如在2.2.1说明。 </li><li>沉浸在股票溶胀溶液的医用级硅酮平方用于改变时间周期:1小时，3小时，6小时和24小时。 </li><li>从溶胀溶液除去后，空气干燥黑暗条件下溶胀的聚合物样品48小时，使得样品收缩回其以前的尺寸。 </li><li>用去离子水彻底清洗QD-掺入样品以除去任何表面结合材料或残余溶剂。 </li></ol></li></ol> 3.纳米可视化骤升到封装PDMS <ol><li> 硅胶试样制备: <ol><li>切出两个硅氧烷广场用新鲜的手术刀刀片（5.5毫米×11毫米）。确保此公开硅氧烷样品的内表面。 </li></ol></li><li> 荧光成像: <ol><li>将硅样品上microsco用于成像的pe滑动，确保聚合物的新切割面，使与载玻片完全接触。按硅氧烷部分轻轻向下，以确保与载玻片平滑的接触。将样品在显微镜的阶段。 </li><li>完整寿命荧光测量使用488nm的光谱滤光的激光线在20MHz或类似的速率包含5皮秒脉冲。23使用一个声光调谐滤光器系统中，可直接联接到激光输出，以生成488纳米激光线。用一个定制的激光扫描单元（参见补充信息），它是由二向色镜（488纳米）转换成10X物镜的后孔径反射，然后到样品聚焦的​​激光束。 <ol><li>收集具有相同目标的荧光发射，这之后，通过相同的分色镜。这直接朝着光的雪崩光电二极管单光子计数模式下工作。流程lifeti<html>我23测量使用时间相关单光子计数（TCSPC）板。 </li></ol></li><li>记录在开头的仪器响应函数（IRF）和各实验会话结束23 注意:在TCSPC实验中的记录的信号应显示在检测器的光子到达和生产随后的激光脉冲之间的时间延迟。这个时间延迟然而，应与测量装置的IRF进行卷积。因此，在IRF被作为仪器至100nM金胺O，从而具有相对于仪器响应一个显著寿命较短（约100皮秒）的反应测定。 </li><li>提取由荧光强度的指数衰减的非线性拟合的寿命和使用最大似然估计（MLE）算法25-27从IRF解卷积此。最大似然估计（γj）的计算为 eq1.jpg"/&gt; 其中，n i是在信道i光子计数的数目，k是信道（或容器）的每个荧光衰变的数目，P I（j）是一组的光子会落在信道，如果我的颗粒具有的概率一生j和N是数为给定的衰减的总数量。 </li><li>记录每个样品的荧光强度和寿命数据5分钟，创造了连续扫描由264的图像的大小为512×512像素。结合这提供二维荧光强度，寿命和强度加权终身地图，计算MLE拥有150光子阈值，这个过程用MATLAB。 </li></ol></li></ol>

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The authors have nothing to disclose.

Cross-sectional fluorescence imaging allows for direct visualization of nanoparticles during swell encapsulation. The kinetics of encapsulation has been shown, with the drive toward a high nanoparticle surface concentration demonstrated. The extent of nanoparticle incorporation is shown to vary with swell encapsulation time (described in section 2.3), with the total amount of incorporated nanoparticles increasing as this time is extended, with the particle concentration localized at the surface if the polymer samples are used. The variation in the concentration of the nanoparticle solution (up to a 3&#215; dilution, described in section 2.2), indicates there is little change in the amount of encapsulated particles. The swell encapsulation behavior of the particles used (CdSe QDs, &#216; - 12.6 &#177; 2.1 nm) have also been shown to be comparable to particles of similar size (Titanium dioxide, &#216; - 13.1 &#177; 5.6 nm),22 which demonstrates the potential use of this technique as a valuable tool for further investigating swell encapsulation kinetics. The swell encapsulation rates observed in these experiments are imagined to be sensitive to nanoparticle size, and so any size variation may result in a modification of the encapsulation rate.
The accurate quantification of nanoparticles within nanocomposites is a challenge that faces many research groups.1-3 Fundamental methods exist which allow the identification of a materials overall composition, however an substantial increase in complexity arises when assessing localized nanoparticle concentration, or concentration gradients over micrometer (or even nanometer) distances. Existing standards rely upon bulk measurements, such as EDS and XPS, in addition to estimating the surface concentration through functional testing, however using these methods means the precise surface composition would remain unknown.17-21 The analysis technique detailed herein, provides direct imaging and facilitates quantitative analysis of these materials. Quantification of precise nanoparticle concentrations within the polymer is possible, when the fluorescence images are evaluated against known concentrations of the fluorescent material. It is hoped that the techniques described are able to contribute toward a developing a standard test for accurate surface concentration analysis of nanocomposites to further research in the development of more potent antimicrobial materials, as well as functional materials.
Cross-sectional fluorescence imaging has the potential to be applied to any fluorescent nanoparticulate species, it is possible that the fluorescence could originate from the nanoparticle itself or the surrounding ligands. Limitations of this technique will stem from the inability to incorporate nanoparticulate fluorescent species. Future developments of these experiments could aim to explore the nanoparticle size dependence of the swell encapsulation rate, with the composition of the swelling solvent also a potential focus. The development of a full understanding of the encapsulation process will be vital in the advance of swell encapsulation as a process for fabricating functional materials.

纳米材料的应用曾长期担任增加对新技术感兴趣的一个领域。1-3这包括越来越多地使用的日常用品，包括化妆品，服装，包装，电子纳米粒子的4-6倾向于使用纳米颗粒的主要驱动器在功能性材料从较高相对于材料它们的反应性茎，除了在颗粒尺寸的能力来调整属性由变异7另一个优点是容易地形成的复合材料的能力，引入关键属性的基质，如催化功能材料的强化和电性能的调优。8-12 其中最简单的纳米颗粒-聚合物复合材料可通过一系列的技术来实现，是基质的制造过程中直接整合所需的纳米粒子。13,14该Results在均质材料均匀间距的纳米材料贯穿始终。然而，许多应用仅仅要求活性物质存在于纳米复合材料的外部接口。其结果是，直接掺入不导致有效地使用有时昂贵纳米材料作为存在通过散装的材料的多纳米颗粒废物。15,16为了实现直接掺入，纳米颗粒还必须与主体基质形成兼容。这可能是具有挑战性的，尤其是在要求多面的反应，如在通常由可以由高活性的纳米颗粒的影响金属配合物催化剂的机制促进热固性聚合物的情况下合成。14 聚合物合成过程中直接​​纳米粒子掺入相关联的相当大的缺点，已导致的技术旨在限制纳米颗粒incorporati发展到表面层。17-21胀大封装是在文献中报道的最成功的策略之一，以实现高的表面的纳米粒子的浓度，与在聚合物本体有限浪费。17-19该技术利用聚合物的溶剂从动溶胀矩阵，允许分子种类和纳米颗粒的侵入。在除去溶胀溶剂，在基质内的物种成为固定到位，以在表面局部物种的浓度最高。迄今为止，大多数膨胀包封的报道使用均朝向抗微生物聚合物的制造中，在那里它是关键的活性剂是在该材料的表面上。虽然许多这些报告显示增强的抗菌活性，精确的表面的纳米颗粒组合物进行详细很少探测。克里克等人最近证明为纳米粒子侵入的直接可视化的方法，提供了重要的INSIGHT成涌浪封装实现动力学和表面的纳米颗粒的浓度。22 这个工作详细硒化镉量子点（QD），其溶胀封装到聚二甲基硅氧烷（PDMS），并使用荧光成像它们掺入的直接可视化的合成。变溶胀封装时间和纳米粒子的浓度在溶胀溶液的效果进行了探索。荧光可视化技术允许纳米粒子侵入的直接成像到PDMS并表明量子点的最高浓度是在该材料的表面上。

<table border="0" cellpadding="0" cellspacing="0" width="573">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polydimethylsiloxane sheets</td>
			<td style="width:71px;">NuSil</td>
			<td style="width:119px;">-</td>
			<td style="width:167px;">Medical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O7805</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">117854</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine oxide</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">346187</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Octadecene</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O806</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Zinc diethyldithiocarbamate</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">329703</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleic acid</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">364525</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Triethylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">471283</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Cadmium oxide</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">33235</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Hexadecylamine</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">B22459</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Dodecylphosphonic acid</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">H26259</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Selenium powder</td>
			<td style="width:71px;">Acros</td>
			<td style="width:119px;">19807</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Chloroform</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">366919</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">n-Hexane</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">208752</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Microscope slides</td>
			<td style="width:71px;">VWR</td>
			<td style="width:119px;">631-0137</td>
			<td>Thickness No. 1</td>
		</tr>
	</tbody>
</table>

advanced compositional analysis of nanoparticle-polymer composites using direct fluorescence imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

量子点表现出红色荧光，与λ最大值的大约600纳米。22,28的红色发射是由于激子由量子棒，其大小尺寸的强约束状态中的限制。 Li等人表明，量子棒，发射移动到与增加宽度或所述杆的长度降低能源。他们进一步发现，发射主要由横向限制，即使当杆是很长的，特别是当宽度小于有问题，因为它是在强约束状态的材料的玻尔半径起着重要的作用来确定。29透射电子显微镜（TEM）成像显示了量子点的细长形状（长宽比〜2.5）。量子点的平均长度被证明是12.6毫微米±2.1纳米（N = 200）（ 图1）。量子点溶液在冷藏条件下是稳定的，最多3米onths。在补充资料中提供了量子点的低倍率的图像（SI - 1）。 在封装过程中，硅样品目视膨胀，膨胀到在肿胀15毫米后1毫米×15毫米×2小时的最大尺寸（原件的尺寸，11毫米×11毫米×1毫米）。样本缩小到其原始大小一旦残留的溶剂蒸发（ 图2）。 UV-Vis光谱表明，纳米颗粒包封没有影响聚合物着色，由此谱仍然是所有的封装样本不变。溶胀封装后的有机硅的扫描电子显微镜（SEM）成像显示起皱的表面，引起胀缩过程。能量色散X射线谱（EDS）分析表明，硒化镉量子点的证据，并表示有增加这些元素（CD /硒）具有溶胀T的存在我。的EDS分析的大检测体积并不允许表面覆盖的可靠的定量分析。 SEM图像和能谱数据在补充信息（ - 2/3 SI）提供。 通过聚合物的纳米颗粒穿透的轮廓是通过硅氧烷样品的横截面切割所示，在用激光激发结合（在补充信息SI所示显微镜设置 - 4）。荧光量子点纳米粒子回答了在488纳米入射激光扫描，在可见光谱的红色部分发光。指出的CdSe量子点的采样数据被集中在聚硅氧烷的外表面，以从样品的中心始发基本上降低的信号。量子点的侵入硅氧烷聚合物成像的使用二维强度加权寿命（τw）映射（光子计数×寿命）。交叉sectio的曝光沿着硅氧烷样品的中间最终轮廓确保了纳米颗粒运动通过聚合物的充分的程度可以被可视化（ 图3）。再膨胀封装倍（48小时）设置有两个颗粒的最高表面浓度，和颗粒渗透最高量的样品通过向批量的聚合物的，一直到样品中央。较短的时间的封装时间（1,4和24小时）仍显示在表面上的较高的粒子数目，但是颗粒的数量减少（ 图3）。从原液（100％）连续稀释被用来研究改变纳米粒子的浓度，对纳米颗粒的后续吸收入聚合物的效果。的储备溶液稀释至达到以下相对浓度溶胀溶液至66％，50％和33％体积:体积。没有观察到荧光成像没有明显的差异时的浓度是变化的，<html>当溶胀封装48小时，表明溶胀溶液的纳米颗粒的浓度不影响纳米颗粒的摄取到聚合物中。 观察的最高纳米颗粒表面的浓度为样品溶胀封装48小时。这些样品的荧光强度是在膨润液比得上[〜0.7μM]（补充信息 - 司 - 5）。粒子的最大渗透被示出为从外缘〜163微米，与经过100微米的浓度达到半最大。最大颗粒渗透速度显示为减缓由于封装时间增加，从3.4微米/小时的平均渗透速度增加48小时的样品，以28微米/小时的样品的速率溶胀封装4小时（补充信息 - SI - 5）。 S / ftp_upload / 54178 / 54178fig1.jpg"/&gt; 图1. 量子点图像的CdSe /硫化锌量子点TEM照片显示棒状纳米粒子。比例尺显示10纳米。单个粒子的轮廓覆盖。 <a href="https://www.jove.com/files/ftp_upload/54178/54178fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/54178/54178fig2.jpg" /> 图2. 聚合物溶胀。图为硅酮样品（ 一 ）前，（b）在与溶剂诱导的肿胀（c）之后。尺寸增加（11至15mm），则在硅氧烷充分干燥逆转。比例尺显示10mm以下。 <a href="https://www.jove.com/files/ftp_upload/54178/54178fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> </p&gt; <img alt="图3" src="/files/ftp_upload/54178/54178fig3.jpg" /> 图3. 荧光寿命图像。图像显示2D强度加权终身地图（光子计数寿命）。的图像显示在聚合物部分的后中心的横截面外形:（A）0小时，（B）中为1小时，（C）的4小时后，（D）在24小时和（E）48小时溶胀封装的。 （F）的封装进展通过分析归一化的强度称量寿命为每个图像示出。刻度条表示100μm左右。误差棒是显示在所获得的结果的变化的一个标准偏差。这个数字已经从修改[22]，由皇家化学学会转载。 <a href="https://www.jove.com/files/ftp_upload/54178/54178fig3large.jpg" target="_blank">请点击此处为vi</a>EW这个数字的放大版本。

Watch this Scientific Journal Video about Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging at JoVE.com

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

纳米粒子 - 聚合物复合材料使用直接荧光成像的先进成分分析

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

advanced-compositional-analysis-nanoparticle-polymer-composites-using

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Engineering

7.6K 次观看.  Imperial College London. Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

视频: Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs along the interface between the fuel and core materials. Simultaneously, dynamic changes in thermal and chemical potentials across the micro/nanostructured materials result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. We demonstrate the entire procedure of a thermopower wave experiment, from synthesis to evaluation. Thermal chemical vapor deposition and the wet impregnation process are respectively employed for the synthesis of a multi-walled carbon nanotube array and a hybrid composite of picric acid/sodium azide/multi-walled carbon nanotubes. The prepared hybrid composites are used to fabricate a thermopower wave generator with connecting electrodes. The combustion of the hybrid composite is initiated by laser heating or Joule-heating, and the corresponding combustion propagation, direct electrical energy generation, and real-time temperature changes are measured using a high-speed microscopy system, an oscilloscope, and an optical pyrometer, respectively. Furthermore, the crucial strategies to be adopted in the synthesis of hybrid composite and initiation of their combustion that enhance the overall thermopower wave energy transfer are proposed.

A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described.

化学燃料和多壁碳纳米管的混杂复合材料的热电波的研究准备和评估

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs ...

科研

工程学

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

电池的使用同步为基础的硬X射线微断层故障分析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

对于新材料的低温磁输运测量先进的实验方法

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

Ultrasonic Welding of Thermoplastic Composite Coupons for Mechanical Characterization of Welded Joints through Single Lap Shear Testing

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ultrasonic welding process described in this paper is based on three main pillars. Firstly, flat energy directors are used for preferential heat generation at the joining interface during the welding process. A flat energy director is a neat thermoplastic resin film that is placed between the parts to be joined prior to the welding process and heats up preferentially owing to its lower compressive stiffness relative to the composite substrates. Consequently, flat energy directors provide a simple solution that does not require molding of resin protrusions on the surfaces of the composite substrates, as opposed to ultrasonic welding of unreinforced plastics. Secondly, the process data provided by the ultrasonic welder is used to rapidly define the optimum welding parameters for any thermoplastic composite material combination. Thirdly, displacement control is used in the welding process to ensure consistent quality of the welded joints. According to this method, thermoplastic-composite flat coupons are individually welded in a single lap configuration. Mechanical testing of the welded coupons allows determining the apparent lap shear strength of the joints, which is one of the properties most commonly used to quantify the strength of thermoplastic composite welded joints.

A straightforward procedure for ultrasonic welding of thermoplastic composite coupons for basic mechanical testing is described. Key characteristics of this ultrasonic welding process are the use of flat energy directors for simplified process preparation and the use of process data for the fast definition of optimum processing conditions.

通过单搭接剪切试验的热塑性复合材料优惠券焊接接头的力学特性的超声波焊接

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ...

Use of a Multi-compartment Dynamic Single Enzyme Phantom for Studies of Hyperpolarized Magnetic Resonance Agents

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due to fundamental constraints imposed by the hyperpolarized state, exotic imaging and reconstruction techniques are commonly used. A practical system for characterization of dynamic, multi-spectral imaging methods is critically needed. Such a system must reproducibly recapitulate the relevant chemical dynamics of normal and pathological tissues. The most widely utilized substrate to date is hyperpolarized [1-13C]-pyruvate for assessment of cancer metabolism. We describe an enzyme-based phantom system that mediates the conversion of pyruvate to lactate. The reaction is initiated by injection of the hyperpolarized agent into multiple chambers within the phantom, each of which contains varying concentrations of reagents that control the reaction rate. Multiple compartments are necessary to ensure that imaging sequences faithfully capture the spatial and metabolic heterogeneity of tissue. This system will aid the development and validation of advanced imaging strategies by providing chemical dynamics that are not available from conventional phantoms, as well as control and reproducibility that is not possible in vivo.

A multi-compartment dynamic phantom is used to simulate some biology of interest for metabolic studies using hyperpolarized magnet resonance agents.

一个多腔动态单一酶幻影超极化磁共振剂研究的用途

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

利用同步辐射微断层调查的多尺度三维微电子封装

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

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 ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

矿物和岩石样品的同步辐射 x 射线 Microdiffraction 和荧光成像

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

胶孔溶液的表达及其化学成分和电阻率的 X 射线荧光分析

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

Excitation-Scanning Hyperspectral Imaging Microscopy to Efficiently Discriminate Fluorescence Signals

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence signals were proven cumbersome until the advent of hyperspectral imaging, in which fluorescence sources can be separated from each other as well as from background signals and autofluorescence (given knowledge of their spectral signatures). However, traditional, emission-scanning hyperspectral imaging suffers from slow acquisition times and low signal-to-noise ratios due to the necessary filtering of both excitation and emission light. It has been previously shown that excitation-scanning hyperspectral imaging reduces the necessary acquisition time while simultaneously increasing the signal-to-noise ratio of acquired data. Using commercially available equipment, this protocol describes how to assemble, calibrate, and use an excitation-scanning hyperspectral imaging microscopy system for separation of signals from several fluorescence sources in a single sample. While highly applicable to microscopic imaging of cells and tissues, this technique may also be useful for any type of experiment utilizing fluorescence in which it is possible to vary excitation wavelengths, including but not limited to: chemical imaging, environmental applications, eye care, food science, forensic science, medical science, and mineralogy.

Spectral imaging has become a reliable solution for identification and separation of multiple fluorescence signals in a single sample and can readily distinguish signals of interest from background or autofluorescence. Excitation-scanning hyperspectral imaging improves on this technique by decreasing the necessary image acquisition time while simultaneously increasing the signal-to-noise ratio.

激发-扫描高光谱成像显微镜，以有效区分荧光信号

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence ...