We thank E. Arzt for his support through INM. The research was in part supported by the Leibniz Competition 2014.

<ol>
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The authors have nothing to disclose.

所描述的协议能够在液体中金纳米粒子的茎，包括动态过程的观察。保持器的组装是容易了解的技术。但是，与液体流的TEM保持器工作时，若干方面必须加以考虑。例如，在O形环的硅微芯片或大颗粒的破碎边缘可能导致液体细胞的泄漏。另一方面，大颗粒（&gt; 200纳米; 例如，灰尘或Si碎屑）上的SiN膜可能会导致液体电池的厚度增加，从而导致低的成像造影或低空间分辨率和甚至可能导致的SiN窗破裂。重要的是，盐或其他化学品的残余物可能会影响以不希望的方式的实验的结果。因此，至关重要的是，样品制备和保持器组件的不同步骤仔细和在一个干净，无尘环境中进行。 液体CE的厚度LL确定可实现的分辨率，以及所获得的图像17的对比。该厚度可通过位于两个硅微芯片中的一个间隔物来调整。根据样品的尺寸，液体的细胞的不同的厚度就能够实现。对于金纳米粒子的研究，有可能使用小间隔物（200-500纳米），而整个真核细胞中需要较大的可达5微米的隔离物。液晶单元的厚度是通过从液体小区和周边真空之间的压力差造成的的SiN膜的窗户的膨出进一步影响。这种影响变得具有较大的SiN膜的窗口更加明显。因此，为了最大限度地减少液晶单元的厚度，建议使用小的SiN膜的窗户。在情况下，它是很难找到两个小窗口之间的重叠，它们可以在使用不同的碱微芯片的交叉配置进行组装。其他配置LARG伊利防止胀和由被柱子支撑19单片微型芯片18或膜窗，但那些表现出劣势就装样的。之一的当前技术中最具挑战性的方面是缺乏在液体厚度精确控制的。通常情况下，该液体是比什么是从所用的间隔物的尺寸预期，如在这里所示厚得多。几个研究小组使用封闭液室4，20，21，22;这些系统具有关于空间分辨率的一些优点，作为液体厚度可通过诱导在液体中气泡减少。可替代地，在SiN窗口可以被迫以折叠，导致较薄的液体层。第三，其他窗户更薄的外壳存在（ 例如，石墨烯）23，也导致薄得多液体比什么是可能的，在此协议中描述的系统。然而，这是不可能的那些系统中流动的液体。 作为任何高分辨率显微技术，一些实验方面必须加以考虑。最重要的方面是与液体或样品的电子束的相互作用。除了辐射损伤，这限制了对许多固体样品24中的可实现的空间分辨率，所述液体样品也通过电子束产生的辐解产物15，25的影响。由于这些产品可能会影响实验，细心数据解释和实验设计是必不可少的26。显微镜设置应根据特定研究的目标来选择。 ADF STEM是在较大的液体单元的厚度高原子序数（Z）的成像纳米颗粒更强大，WHI透射电镜乐给出了低Z材料更好的对比度和通常更快，但需要更薄的液体层3。代替使用ADF检测器的，则明场（BF）检测器有时被用于图像的液晶单元中，由于高炉干为在厚层27成像低Z材料是有利的。随着液体电池的厚度，则需要更多的电流。然而，这也增加了辐解产物的浓度和增加辐射伤害。还应当指出的是，对比反转在ADF检测器被观察到很厚的液体（&gt; 10微米为水）。 液体条件通过从显微镜移除保持器和交换两样品和液体我们的实验之间改变。除了改变盐的浓度，这是很容易可以通过在不同的液体流动（ 例如，一个可以改变液体的其它性质为了设置一个特定的pH 16使用缓冲溶液或可能引入的有机溶液或其它添加剂）。另外，也可以改变液体，而保持器在显微镜通过微流体系统流动的液体仍然插入。然而，在这种情况下，它是未知的，此时指向试样的变化的液体中。也值得注意的是，微芯片支承电极是可用的，所以纳米级电化学实验可进行28。 研究的对象不限于金纳米粒子在水，但可使用上述的协议，包括二氧化硅，氧化钛和聚合物进行研究的各种试样。如果对象的运动太快，收购内的图像中捕捉到，可通过一个数量级，通过使用50％甘油和50％水的混合物中来降低粘度。 从上述的点，具有许多优点，可能性，也存在缺点将变得显而易见。当与液相STEM工作，要考虑的最重要的缺点是:1）任何实验是由与整个试样（被观察物，液体，和在SiN膜）的电子束的动态相互作用的影响; 2）样品处理是繁琐的，并且它往往是难以实现的薄液体层，因为样品或微芯片包含一些微米尺寸的颗粒; 3）液体厚度通常从由间隔设置的预定厚度基本上不同;和4）的空间分辨率和对比度强烈取决于液体厚度和下观察和液体中的对象的变化密度之间的差异。 目前，为对象的液体的显微镜用纳米空间分辨率存在充足的方法。非晶冰电子显微镜是一种强大的技术29，但所涉及的实验步骤细腻，不是所有的实验允许样品在冰的制备，和时间分辨实验是不可能的。 X射线显微镜30，31原则上可以使用的，但它有一个有限的空间分辨率，而不是在实验室广泛使用。在液体原子力显微镜已经建立，但是一个表面技术仅32，33，34，35。光学显微镜未显示出足够的空间分辨率。目前，在液体电子显微镜，似乎在液体纳米级物体和过程的直接镜检最强大的技术。 液相TEM和STEM尚未常规分析技术，但仍处于发展阶段。的参数考虑到的数量是相当大的，而且它是ofteÑ难以再现的实验结果。此外，量化数据难以获得，因为所研究的影响与存在的作为电子束的结果进程交织在一起。这里描述的协议的目的是规范实验方案，从而占实验的所有相关方面的基础。我们希望，该协议将导致这一新兴领域的试点工作更好的重复性。

常规扫描透射电子显微镜（STEM）是由适合于分析的标本，特别适合于在高真空放置的干燥和固体样品的范围的限制。然而，许多科学和技术问题涉及纳米级材料和在液体环境中的流程。完全嵌入在液体样品现在可以用STEM使用涉及在透射电子显微镜（TEM）和STEM 1的试样夹持器组装的微流体室中的概念进行了研究。这种新开发的技术已经变得越来越流行，因为它提供了新的认识的各种研究课题重要过程，包括生长，溶解，和纳米颗粒2，3，4，5的聚集方法，6。不仅金属，也biominerals 7和生物系统可以研究8，9，10，11。样品装载和图像获取用于液相干比为干燥样品的干不同并涉及需要专门的培训的协议。 微流体系统包括两个硅微芯片支承氮化硅（SiN）膜的窗户的透明，在200千电子伏的能量12的电子束的（ 见图1A）。尺寸和这些芯片的处理细节可以在别处找到12，13。样品通常含有纳米级物体。在本文中，我们观察到黄金纳米粒子（纳米金）。该金纳米粒子在顶部窗口（相对于向下行进的电子束）固定或浮动在理趣ID。在STEM纳米级的空间分辨率是通过扫描电子束在金纳米颗粒和收集用环形暗场（ADF）的检测器9发送的散射电子获得。两个微芯片被放置在一个小槽在液体流动的TEM保持器1（支架为STEM操作和TEM但作为TEM的保持器被称作）的前端。一项所述的微芯片的包含一个间隔件，以便在微芯片之间形成的液体隔室。在两个微芯片的两侧的O形环提供液体隔室13（ 见图1B）的真空密封。 本文的目的是展示样和数据采集的基本步骤，让有兴趣的用户可能会发现很容易进入这个新兴的新技术。从特定的公司提供的系统被使用，但该协议也适用于其他公司的系统。该技术是比传统的TEM和STEM和一定数量的实际方面较复杂，必须与流体储存器系统13工作时被考虑。最重要的是要确保液体隔室是否正确组装，从而提供了薄液层和真空密封。因此，为了干净地工作，以防止液体流动的TEM支架的制备和组装过程中的粉尘的形成是非常重要的。具体地，O形圈和两个硅微芯片需要从所有污染。灰尘对微芯片的一个甚至小颗粒可能会严重增加组装的电池，其可以防止一个有用的空间分辨率的实现的厚度。真空密封是很重要的，这样没有污染或损坏将在实验后的电子显微镜离开了。本协议描述的加载过程和一些必要的测试。电子显微镜的操作很简单，BUt将其要求相比，固体样品的显微一些额外的步骤。随着液体的厚度，更多的电子被吸收并通过液体散射;液体厚度的测量是必要的。最后，协议说明如何图像并如何动态过程进行研究。 <img alt="图1" src="/files/ftp_upload/54943/54943fig1.jpg" /> 图1:冷却液流量为细胞扫描透射电子显微镜（STEM）。 （A）中组装的液晶单元的示意图。用氮化硅（SiN）膜Windows中两个硅微芯片位于两个O形环之间。由于液体被封闭在SiN膜之间，从而从电子显微镜的真空分开。聚焦电子束扫描过的样本。对比度是由散射电子获得的。金粒子（AuNPs）被固定在所述的SiN膜的液体内，但也可以移动的液体。 2微芯片与O形环的叠层的（B）的示意性侧视图的横截面。 <a href="http://ecsource.jove.com/files/ftp_upload/54943/54943fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

<table border="0" cellpadding="0" cellspacing="0" width="800">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:408px;">Binocular light microscope</td>
			<td style="width:141px;">Leica</td>
			<td style="width:163px;">M60 CMO</td>
			<td style="width:88px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Scanning transmission electron mircoscope with spherical aberration corrector</td>
			<td>JEOL</td>
			<td>ARM200F</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Liquid flow TEM specimen holder</td>
			<td>DENS Solutions</td>
			<td>Ocean</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Microfluidic syringe pump</td>
			<td>Harvard Scientific</td>
			<td>PicoPlus</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Plasma cleaner</td>
			<td>Gatan</td>
			<td>Solarus950</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Chemicals</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Acetone, Rotisolv&#160; Plus for HPLC</td>
			<td>Sigma-Aldrich</td>
			<td>7328.2</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Water, chromasolv Plus for HPLC</td>
			<td>Sigma-Aldrich</td>
			<td>34877-2.5L</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ethanol, Rotisolv HPLC grade</td>
			<td>Carl Roth</td>
			<td>P076.2</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Gold colloid citrate stabilized, diameter 30 nm</td>
			<td>British-Biocell</td>
			<td>EM.GC20</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Materials</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Base silicon microchips with silicon nitride membranes of 50 nm thickness and dimensions of 20 &#181;m x 0.40 mm</td>
			<td>DENS Solutions</td>
			<td>for Ocean system</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Spacer silicon microchips with silicon nitride membranes of 50 nm thickness, dimensions of 20 &#181;m x 0.40 mm, and spacer thickness of 200 nm</td>
			<td>DENS Solutions</td>
			<td>for Ocean system</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Microfluidic peek tubing</td>
			<td>Upchurch Scientific</td>
			<td>1570</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Plastic Replaceable tips Tweezers</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:408px;">(Anti-Magnetic Anti-Acid Stainless Steel body with ESD PVDF (SV) tips)</td>
			<td>ideal-tek</td>
			<td>2ASVR.SA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Teflon coated bent steel tweezers (EMS SA with &#34;PTFE&#34; Coating)</td>
			<td>Electron Microscopy Sciences</td>
			<td>78322-7Te</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Teflon coated broad beak steel tweezers (EMS 2A &#34;PTFE&#34; Coating)</td>
			<td>Electron Microscopy Sciences</td>
			<td>78322-2ATe</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Hamilton syringe, 1 mL, gastight (Model 1001 TLLX SYR)</td>
			<td>Hamilton</td>
			<td>81323</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Clean room tissue Sontara Micropure AP (224x224mm)</td>
			<td>DuPont</td>
			<td>Sontara MicroPure</td>
			<td></td>
		</tr>
	</tbody>
</table>

studying dynamic processes of nano-sized objects in liquid using scanning transmission electron microscopy

完全嵌入在液体样品可在使用中用于透射电子显微镜（TEM）和干样品架组装的微流体腔室的扫描透射电子显微镜（STEM）纳米级的空间分辨率进行研究。微流体系统包括两个硅微芯片支撑薄氮化硅（SiN）膜的窗口。本文介绍样品加载和数据采集的基本步骤。最重要的是要确保液体隔室是否正确组装，从而提供了薄液层和真空密封。该协议还包括若干以确保正确装配样品加载期间执行必要的试验。一旦样品在电子显微镜装载，液体厚度需要被测定。不正确装配可能会导致过厚的液体，而太细的液体可以指示不存在液体，当形成的气泡等。最后，协议解释如何图像并如何动态过程进行研究。含有金纳米粒子样品都在纯水和在盐水中进行成像。

液体流动的TEM支架被用来研究金纳米粒子在液体中的行为。金纳米粒子被稳定地固定在SiN膜在纯水中，并使用液相STEM（ 图6）与纳米级的分辨率进行成像。在强烈散射黄金获得良好的对比度。用于干试样测得的荧光屏上的电流密度为20 PA /平方厘米，而其量达8 PA /平方厘米与插入的液体流动的TEM持有者。使用公式1， 叔 水 = 2.4±0.5微米，比基于为200nm的隔离物厚度是预期的大得多。然而，厚度不为金纳米粒子的纳米空间分辨率成像太大。液体厚度由于鼓出的微芯片的氮化硅膜，非平坦的，和碎片驻留在微芯片比由间隔设置的200纳米厚。 16中它们的形状，虽然反应性辐解产物（例如- 水溶液 ，H•，H +，OH•）从电子束的与交互始发水可能氧化单金原子，导致纳米金15的形状的变化。然而，当液体流动系统被用来在第二个实验中引入的氯离子，所述金纳米粒子的稳定性发生变化。氯离子能够稳定在tetrachloroaureat的形式氧化金原子，AUCL 4 - 。 图7示出，在一个STEM成像时间推移系列缓慢溶解的金纳米粒子，类似的结果报告早期的16。对于所使用的电子剂量率，花〜300秒以溶解30纳米大小的金纳米粒子。 金纳米粒子的水:运动<html> R IN第三个实验中（ 图8）进行了研究。之前的实验中，将液体流动的TEM保持器以除去盐的任何痕迹进行清洗。从第一个实验的不同，使用一个替代的样品制备的方法来实现的纳米金来在SiN膜14的较弱的附着。在该实验中，金纳米粒子溶液置于在硅微芯片，并在液体流动的TEM保持器组装而不让溶液变干。以这种方式，所述金纳米颗粒容易从在SiN膜在成像在所使用的剂量率分离。一些金纳米粒子的移动离开的视图成批量溶液的字段路程，而其余的金纳米粒子在靠近在SiN窗口保持在视野内。观察这些金纳米粒子的运动，最终他们团聚。一段时间后，这些聚集体也从在SiN膜分离并移出的视场并进入溶液中。 ntent"FO:保together.within页="1"&gt; <img alt="图6" src="/files/ftp_upload/54943/54943fig6.jpg" /> 图6:顶部有一个纯净水层的金纳米粒子30纳米直径在扫描透射电子显微镜（STEM）显微图。示出的图像是原始图像的选定区域。图像大小为1,024×1,024像素，像素停留时间为19微秒，像素尺寸为0.73纳米，并且放大倍率为400,000X。电子剂量为7.1因而×10 4 E - /纳米2。在荧光屏上测得的电流密度为8 PA /厘米2，使该液体的厚度经计算为等于2.4微米。 <a href="http://ecsource.jove.com/files/ftp_upload/54943/54943fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图7" src="/files/ftp_upload/54943/54943fig7.jpg" /> 图7:时间推移系列在盐水金纳米粒子STEM显微照片。 （AD）的图片从在30秒的间隔时间推移系列STEM图像的提取。该金纳米粒子在液体逐渐溶解作为氯离子的存在下的结果。的像素停留时间为2微秒，时间经过一系列的帧时间为1.75秒，像素尺寸为0.44纳米，并且放大倍率为500,000。每幅图像的电子剂量为1.2×10 4 E - /纳米2。液体厚度为2.4微米。 <a href="http://ecsource.jove.com/files/ftp_upload/54943/54943fig7large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图8" src="/files/ftp_upload/54943/54943fig8.jpg" /> 图8:STEM金纳米粒子在纯净水移动显微照片。 （A）的SiN膜与金纳米粒子，其中一些是用箭头选中。 （ 二 ）运动轨迹所选择的金纳米粒子（见A）。一些金纳米粒子从视野中成像时搬走。剩下的金纳米粒子沿着氮化硅薄膜横向移动，并开始凝聚。在到达临界簇大小，它们从膜调度和从view.The像素停留时间字段搬开为1微秒，则帧时间为0.52秒，像素尺寸为1.8纳米，并且放大倍率为120,000X。每幅图像的电子剂量为3.5×10 2ë - /纳米2和液体厚度为2.4μm。 <a href="http://ecsource.jove.com/files/ftp_upload/54943/54943fig8large.jpg" target="_blank">请点击此处查看该图的放大版本。</a>

Watch this Scientific Journal Video about Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy at JoVE.com

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

这个协议描述一种用于扫描金纳米粒子的透射电子显微镜中的水，如用于纳米动态过程的观察液流试样保持器的操作。

使用扫描透射电子显微镜研究纳米大小的物体的动态过程中的液体

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a ...

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Research

JoVE Journal

Engineering

12.6K 次观看.  INM-Leibniz Institute for New Materials. 这个协议描述一种用于扫描金纳米粒子的透射电子显微镜中的水，如用于纳米动态过程的观察液流试样保持器的操作。 

视频: Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

在液体中使用液体池透射电子显微镜揭示材料的动态过程

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

科研

工程学

Scanning-probe Single-electron Capacitance Spectroscopy

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the electronic quantum structure of small systems - including individual atomic dopants in semiconductors. Here we present a capacitance-based method, known as Subsurface Charge Accumulation (SCA) imaging, which is capable of resolving single-electron charging while achieving sufficient spatial resolution to image individual atomic dopants. The use of a capacitance technique enables observation of subsurface features, such as dopants buried many nanometers beneath the surface of a semiconductor material1,2,3. In principle, this technique can be applied to any system to resolve electron motion below an insulating surface.
As in other electric-field-sensitive scanned-probe techniques4, the lateral spatial resolution of the measurement depends in part on the radius of curvature of the probe tip. Using tips with a small radius of curvature can enable spatial resolution of a few tens of nanometers. This fine spatial resolution allows investigations of small numbers (down to one) of subsurface dopants1,2. The charge resolution depends greatly on the sensitivity of the charge detection circuitry; using high electron mobility transistors (HEMT) in such circuits at cryogenic temperatures enables a sensitivity of approximately 0.01 electrons/Hz&frac12; at 0.3 K 5.

Scanning-probe single-electron capacitance spectroscopy facilitates the study of single-electron motion in localized subsurface regions. A sensitive charge-detection circuit is incorporated into a cryogenic scanning probe microscope to investigate small systems of dopant atoms beneath the surface of semiconductor samples.

扫描探针单电子电容谱

The integration of low-temperature scanning-probe techniques and single-electron capacitance spectroscopy represents a powerful tool to study the ...

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve geologic seals and allow CO2 to escape. However, the dissolution processes at reservoir conditions are poorly understood. Thus, time-resolved experiments are needed to observe and predict the nature and rate of dissolution at the pore scale. Synchrotron fast tomography is a method of taking high-resolution time-resolved images of complex pore structures much more quickly than traditional &#181;-CT. The Diamond Lightsource Pink Beam was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 hours. The images were segmented and the porosity and permeability were measured using image analysis and network extraction. Porosity increased uniformly along the length of the sample; however, the rate of increase of both porosity and permeability slowed at later times.

Synchrotron fast tomography was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 h.

用同步快速反应层析成像动态孔隙规模油藏条件下成像碳酸盐

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography (CT) and Light Microscopy (LM) Correlated with Scanning Electron Microscopy (SEM)

In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of micro-characterization, plays an important role. Commonly, different techniques like X-ray computed tomography (CT), light microscopy (LM) and scanning electron microscopy (SEM) are used separately. Similarly, the results have to be treated for each technique independently. Here a comprehensive study is shown which demonstrates the potentials leveraged by linking CT, LM and SEM. In depth characterization is performed on a white emitting LED, which can be operated throughout all characterization steps. Major advantages are: planned preparation of defined cross sections, correlation of optical properties to structural and compositional information, as well as reliable identification of different functional regions. This results from the breadth of information available from identical regions of interest (ROIs): polarization contrast, bright and dark-field LM images, as well as optical images of the LED cross section in operation. This is supplemented by SEM imaging techniques and micro-analysis using energy dispersive X-ray spectroscopy.

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography CT and Light Microscopy LM Correlated with Scanning Electron Microscopy SEM

A workflow for comprehensive micro-characterization of active optical devices is outlined. It contains structural as well as functional investigations by means of CT, LM and SEM. The method is demonstrated for a white LED which can be still be operated during characterization.

在通过X射线计算机断层扫描（CT）和与扫描电子显微镜相关光学显微镜（LM）的一个组合的LED深度分析（SEM）的

In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of ...

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

通过扫描电子显微镜在半导体材料的扩展缺陷的全面表征

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

Precision Milling of Carbon Nanotube Forests Using Low Pressure Scanning Electron Microscopy

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning electron microscope (ESEM) operating with a low pressure water vapor ambient. In this technique, a portion of the electron beam interacts with the water vapor in the vicinity of the CNT sample, dissociating the water molecules into hydroxyl radicals and other species by radiolysis. The remainder of the electron beam interacts with the CNT forest sample, making it susceptible to oxidation from the chemical products of radiolysis. This technique may be used to trim a selected region of an individual CNT, or it may be used to remove hundreds of cubic microns of material by adjusting ESEM parameters. The machining resolution is similar to the imaging resolution of the ESEM itself. The technique produces only small quantities of carbon residue along the boundaries of the cutting zone, with minimal effect on the native structural morphology of the CNT forest.

Low pressure scanning electron microscopy in a water vapor ambient is used to machine nanoscale to microscale features in carbon nanotube forests.

碳纳米管森林精密铣床使用低压扫描电子显微镜

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning ...

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.

超细晶和纳米晶材料的表征采用透射菊池衍射

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and ...

A Method for Obtaining Serial Ultrathin Sections of Microorganisms in Transmission Electron Microscopy

Observing cells and cell components in three dimensions at high magnification in transmission electron microscopy requires preparing serial ultrathin sections of the specimen. Although preparing serial ultrathin sections is considered to be very difficult, it is rather easy if the proper method is used. In this paper, we show a step-by-step procedure for safely obtaining serial ultrathin sections of microorganisms. The key points of this method are: 1) to use the large part of the specimen and adjust the specimen surface and knife edge so that they are parallel to each other; 2) to cut serial sections in groups and avoid difficulty in separating sections using a pair of hair strands when retrieving a group of serial sections onto the slit grids; 3) to use a 'Section-holding loop' and avoid mixing up the order of the section groups; 4) to use a 'Water-surface-raising loop' and make sure the sections are positioned on the apex of the water and that they touch the grid first, in order to place them in the desired position on the grids; 5) to use the support film on an aluminum rack and make it easier to recover the sections on the grids and to avoid wrinkling of the support film; and 6) to use a staining tube and avoid accidentally breaking the support films with tweezers. This new method enables obtaining serial ultrathin sections without difficulty. The method makes it possible to analyze cell structures of microorganisms at high resolution in 3D, which cannot be achieved by using the automatic tape-collecting ultramicrotome method and serial block-face or focused ion beam scanning electron microscopy.

This study presents reliable and easy procedures for obtaining serial ultrathin sections of a microorganism without expensive equipment in transmission electron microscopy.

一种在透射电镜中获取微生物连续超薄切片的方法

Observing cells and cell components in three dimensions at high magnification in transmission electron microscopy requires preparing serial ultrathin ...

Single-Digit Nanometer Electron-Beam Lithography with an Aberration-Corrected Scanning Transmission Electron Microscope

We demonstrate extension of electron-beam lithography using conventional resists and pattern transfer processes to single-digit nanometer dimensions by employing an aberration-corrected scanning transmission electron microscope as the exposure tool. Here, we present results of single-digit nanometer patterning of two widely used electron-beam resists: poly (methyl methacrylate) and hydrogen silsesquioxane. The method achieves sub-5 nanometer features in poly (methyl methacrylate) and sub-10 nanometer resolution in hydrogen silsesquioxane. High-fidelity transfer of these patterns into target materials of choice can be performed using metal lift-off, plasma etch, and resist infiltration with organometallics.

We use an aberration-corrected scanning transmission electron microscope to define single-digit nanometer patterns in two widely-used electron-beam resists: poly (methyl methacrylate) and hydrogen silsesquioxane. Resist patterns can be replicated in target materials of choice with single-digit nanometer fidelity using liftoff, plasma etching, and resist infiltration by organometallics.

用畸变校正扫描透射电镜进行单数字纳米电子束光刻

We demonstrate extension of electron-beam lithography using conventional resists and pattern transfer processes to single-digit nanometer dimensions by ...

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Resistive switching crossbar architecture is highly desired in the field of digital memories due to low cost and high-density benefits. Different materials show variability in resistive switching properties due to the intrinsic nature of the material used, leading to discrepancies in the field because of underlying operation mechanisms. This highlights a need for a reliable technique to understand mechanisms using nanostructural observations. This protocol explains a detailed process and methodology of in&#160;situ nanostructural analysis as a result of electrical biasing using transmission electron microscopy (TEM). It provides visual and reliable evidence of underlying nanostructural changes in real time memory operations. Also included is the methodology of fabrication and electrical characterizations for asymmetric crossbar structures incorporating amorphous vanadium oxide. The protocol explained here for vanadium oxide films can be easily extended to any other materials in a metal-dielectric-metal sandwiched structure. Resistive switching crossbars are predicted to serve the programmable logic and neuromorphic circuits for next-generation memory devices, given the understanding of the operation mechanisms. This protocol reveals the switching mechanism in a reliable, timely, and cost-effective way in any type of resistive switching materials, and thereby predicts the device&#39;s applicability.

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Presented here is a protocol for analyzing nanostructural changes during in&#160;situ biasing with transmission electron microscopy (TEM) for a stacked metal-insulator-metal structure. It has significant applications in resistive switching crossbars for the next generation of programmable logic circuits and neuromimicking hardware, to reveal their underlying operation mechanisms and practical applicability.