Name: preparation of graphene liquid cells for the observation of lithium-ion battery material
Uploaded: 2019-02-05T14:00:00
Description: Watch this Scientific Journal Video about Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material at JoVE.com

这项工作得到了韩国国家研究基金会的支持, 该方案提供了第2014r1a4a100312 (brl 方案)、韩国 ccs & d 中心 (kncrc) 由韩国政府 (科技部、信通技术 & 未来规划) 资助的赠款 (编号)。nrc-2014m1a8a1049303), 2016年由韩国政府 (科技部、ict & 未来规划部) 资助的 kaist (n11160058)、可穿戴平台材料技术技术中心 (wmc) (nr-2016r1a1009926), 国家研究机构提供的最终运行赠款韩国政府资助的韩国基金会赠款 (nrf-2017h11aa1046-global 博士研究金方案), 韩国国家研究基金会赠款, 由韩国政府资助 (msip;科技部, ict & 未来规划) (nrr-2018r1c1b1b6626), nano ·通过由科技部资助的韩国国家研究基金会 (nrf) 和韩国政府资助的信通技术和未来规划 (2009-0082580) 和国家信息技术和未来规划赠款 (msip;科技部, 信息和通信技术 & 未来规划) (nrr-2018r1c1b1b6002624)。

1. 电纺及后续热处理合成 so2 纳米管 17
<ol><li>准备一个电纺溶液。<ol>
<li>在室温下 (rt, 25°c), 将0.25 克氯化锡溶解在1.25 克乙醇和1.25 克二甲基甲酰胺 (dmf) 的溶剂混合物中。</li>
		<li>搅拌2小时后, 在电纺溶液中加入0.35 克聚乙烯醇吡咯烷酮 (pvp), 搅拌均匀均匀度再搅拌6小时。</li>
	</ol>
</li>
	<li>对 sn 前电技术进行电纺复合纳米纤维。<ol>
<li>在电解溶液准备充分的情况下, 用?...

<ol>
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Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+TEM+electrochemistry+of+anode+materials+in+lithium+ion+batteries.">In situ TEM electrochemistry of anode materials in lithium ion batteries.</a> Energy Environmental Science. 4 (10), 3844-3860 (2011).</li><li>Xie, Z. -. H., Jiang, Z., Zhang, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Review-Promises+and+Challenges+of+In+Situ+Transmission+Electron+Microscopy+Electrochemical+Techniques+in+the+Studies+of+Lithium+Ion+Batteries.">Review-Promises and Challenges of In Situ Transmission Electron Microscopy Electrochemical Techniques in the Studies of Lithium Ion Batteries.</a> Journal of the Electrochemical Society. 164 (9), 2100-2123 (2017).</li><li>Tripathi, A. M., Su, W. -. N., Hwang, B. 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Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Growth+dynamics+of+solid+electrolyte+interphase+layer+on+SnO2+nanotubes+realized+by+graphene+liquid+cell+electron+microscopy.">Growth dynamics of solid electrolyte interphase layer on SnO2 nanotubes realized by graphene liquid cell electron microscopy.</a> Nano Energy. 25, 154-160 (2016).</li><li>Lee, K., Shin, S., Degen, T., Lee, W., Yoon, Y. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+analysis+of+SnO2/Fe2O3/RGO+to+unravel+the+structural+collapse+mechanism+and+enhanced+electrical+conductivity+for+lithium-ion+batteries.">In situ analysis of SnO2/Fe2O3/RGO to unravel the structural collapse mechanism and enhanced electrical conductivity for lithium-ion batteries.</a> Nano Energy. 32, 397-407 (2017).</li><li>Chang, J. 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协议中有关键步骤。首先, 将石墨烯转移到 tem 网格上需要研究人员的仔细关注。重要的是要用子处理网格, 不要破坏任何网格, 比如破坏非晶态碳膜或弯曲框架。这类损害会导致石墨烯的覆盖率低, 并影响液袋的数量。此外, 将上网格放置在正确的位置也至关重要。如协议中所述, 在液体干燥之前, 必须快速放置顶部网格。在此过程中, 研究人员可能会损坏上网格或将其放置在错误的位置 (即, ...

最近, 能源消耗不断增加, 以及高性能储能设备的重要性。为了满足这样的需求, 开发具有高能量密度、耐用性和安全性的锂离子电池是必要的1,2。为了开发具有优异性能的电池, 对电池运行过程中的储能机制有一个基本的了解是必不可少的 3,4,5.
原位透射电子显微镜 (tem) 提供了丰富的见解, 因为它可以在电池运行过程中显示结构和化学信息3。在许多原位tem 技术中, glc 被用于观测6、7、8、9、10、11的纳米材料的岩性动态 ,12岁。glc 由一个由两个石墨烯膜密封的液体口袋组成, 通过防止液体在 tem 柱6、7的高真空内蒸发, 提供了一个实际的电极/电解质界面。glc 的优点是, 它们具有卓越的空间分辨率和较高的成像对比度, 因为它们采用电子透明的单原子厚石墨烯作为液体密封膜13,14,15 ,16。此外, 传统的 tem 可以用来观察电池的反应, 而不使用昂贵的原位tem 持有人。
本文介绍了如何用 glc 观察到锂化反应, 具体而言, 电子束辐照在液体电解质内产生了溶解电子, 它们通过将锂离子与溶剂分子分离来启动岩化。
glc 也是能够直接观测具有各种形态的纳米材料的最佳平台, 包括纳米粒子6、9、纳米管7、10、11, 甚至多层面材料12。结合电极材料在实际电化学电池测试后的原位tem 分析, 本文介绍的 glc 系统有可能用于研究其基本反应机理。
凭借 glc 和异地实验的这些优点, 本文介绍了愿意进行类似 glc 实验的研究人员的详细实验方法。协议涵盖 1) 合成锡 (iv) 氧化物 (sno2) 纳米管作为典型的一维纳米结构电极材料, 2) 电化学电池测试, 3) glc 的制备, 4) 实时 tem 的性能观察。

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			<td height="24" style="height:24px;width:373px;">Tin chloride dihyrate</td>
			<td style="width:184px;">Sigma Aldrich</td>
			<td style="width:200px;">CAS 10025-69-1</td>
			<td style="width:583px;">In a glass bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Ethanol</td>
			<td style="width:184px;">Merck</td>
			<td style="width:200px;">CAS 64-17-5</td>
			<td>In a glass bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Dimethylformamide</td>
			<td style="width:184px;">Sigma Aldrich</td>
			<td style="width:200px;">CAS 68-12-2</td>
			<td>In a glass bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Polyvinylpyrrolidone</td>
			<td style="width:184px;">Sigma Aldrich</td>
			<td style="width:200px;">CAS 9003-39-8</td>
			<td>In a plastic bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Cell tester</td>
			<td style="width:184px;">KOREA THERMO-TECH</td>
			<td style="width:200px;">Maccor Series 4000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Cell tester 2</td>
			<td style="width:184px;">WonaTech</td>
			<td style="width:200px;">WBCS4000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Sodium perchlorate</td>
			<td style="width:184px;">Sigma Aldrich</td>
			<td style="width:200px;">CAS 7601-89-0</td>
			<td>In a glass bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">25 gauge needle</td>
			<td style="width:184px;">Hwa-In Science Ltd.</td>
			<td style="width:200px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:373px;">1.3 M of lithium hexafluorophosphate (LiPF6) dissolved in EC/DEC with 10 wt% of FEC</td>
			<td style="width:184px;">PANAX ETEC</td>
			<td style="width:200px;"></td>
			<td>In a stainless steel bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Propylene carbonate</td>
			<td style="width:184px;">Sigma Aldrich</td>
			<td style="width:200px;">CAS 108-32-7</td>
			<td>In a glass bottle</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Super P Carbon Black</td>
			<td style="width:184px;">Alfa-Aesar</td>
			<td style="width:200px;">CAS 1333-86-4</td>
			<td>In a glass bottle</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:373px;">Cell components (bottom cell, top cell, separator, gasket, spring, spacer)</td>
			<td style="width:184px;">Wellcos Corporation</td>
			<td style="width:200px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Cell punch</td>
			<td style="width:184px;">Wellcos Corporation</td>
			<td style="width:200px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:373px;">Glove Box</td>
			<td style="width:184px;">Moisture Oxygen Technology (MOTEK)</td>
			<td style="width:200px;"></td>
			<td></td>
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			<td height="21" style="height:21px;width:373px;">Box Furnace</td>
			<td style="width:184px;">Naytech</td>
			<td style="width:200px;">Vulcan 3-550</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Electrospinning device</td>
			<td style="width:184px;">NanoNC</td>
			<td style="width:200px;"></td>
			<td></td>
		</tr>
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			<td height="21" style="height:21px;width:373px;">Hydrofluoric acid</td>
			<td style="width:184px;">Junsei</td>
			<td style="width:200px;">84045-0350</td>
			<td>85%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Cu foil</td>
			<td style="width:184px;">Alfaaesar</td>
			<td style="width:200px;">38381</td>
			<td>Copper Thinfoil, 0.0125mm thick, 99.9%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Holy carbon Au grid</td>
			<td style="width:184px;">SPI</td>
			<td>Quantifoil R2/2 Micromachined Holey Carbon Grids, 300 Mesh Gold</td>
			<td>Quantifoil R2/2 Micromachined Holey Carbon Grids, 300 Mesh Gold</td>
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			<td height="21" style="height:21px;width:373px;">Isoprophyl alchol</td>
			<td style="width:184px;">Sigmaaldrich</td>
			<td style="width:200px;">W292907</td>
			<td>99.70%</td>
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			<td height="21" style="height:21px;width:373px;">Ammonium persulfate</td>
			<td style="width:184px;">Sigmaaldrich</td>
			<td style="width:200px;">248614</td>
			<td>98%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Transmission electron microscope (TEM)</td>
			<td style="width:184px;">JEOL</td>
			<td style="width:200px;">JEOL JEM 3010</td>
			<td>300 kV</td>
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			<td height="21" style="height:21px;width:373px;">Chemical vapor depistion (CVD)</td>
			<td style="width:184px;">Scientech</td>
			<td style="width:200px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Charge coupled device (CCD)</td>
			<td style="width:184px;">Gatan</td>
			<td style="width:200px;">Orius SC200</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Plasma Cleaner</td>
			<td style="width:184px;">Femtoscience</td>
			<td style="width:200px;">VITA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:373px;">Electrospinning program</td>
			<td style="width:184px;">NanoNC</td>
			<td style="width:200px;">NanoNC eS- robot</td>
			<td></td>
		</tr>
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preparation of graphene liquid cells for the observation of lithium-ion battery material

本文介绍了石墨烯液电池 (glc) 的制备方法、电极材料和有机电解质在两片石墨烯片中的封装, 以及电纺法简单合成一维纳米结构的方法。glc 支持用于电极材料岩化动力学的原位透射电子显微镜 (tem)。利用电子束进行成像和光刻的原位glc-tem 不仅可以利用逼真的电池电解质, 还可以利用各种形态、相位和界面过渡的高分辨率成像。

根据 sem 图像 (图 3a), 通过电纺和随后的焙烧制备了 sno 2 纳米管, 在此过程中可以清楚地看到纳米管和多孔结构.这种纳米管结构来自 pvp 的分解, 而核心中的 sn 前驱体由于柯肯德尔效应17,18而向外移动。此外, 奥斯特瓦尔德成熟发生除了柯肯德尔效应, 导致 sno2纳米基因19的生长.<s...

Watch this Scientific Journal Video about Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material at JoVE.com

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

在这里, 我们提出了一个方案, 用于制造和制备石墨烯液体电池的原位透射电子显微镜观察, 以及电极材料的合成和电化学电池测试。

锂离子电池材料用石墨烯液位的制备

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...

这种石墨烯液体电池使这些动力学在液体电解质中能够进行传输电子显微镜。这种动力学可以提供丰富的锂离子电池工作机制信息，并有助于设计先进的电池设备。石墨烯液体电池的优点是，它允许TEM成像在液体电解质中，提供良好的空间分辨率和高成像对比度。除了卓越的图像质量外，它还可以提供各种形态相和相间过渡的信息。只有书面协议，很难遵循此方法，因为许多技术步骤都是手动执行的。很多技能需要准确性和准确性，其中强烈建议使用耐心。即使你正确地遵循每个协议，你仍然可以失败的实验，因为处理石墨烯和石墨烯传输网格是困难的。首先，准备电固定解决方案，如随附的文本协议中所述。将其转移到十毫升注射器中，并配备 25 针。然后洗掉目标。拿一块矩形的柔性不锈钢，用去维化水清洗，然后用乙醇清洗。重复此过程两到五次。清洁后，在60摄氏度下将钢风干燥10分钟。干燥后，用胶带将柔性不锈钢固定到鼓手身上。接下来，打开电击控制器软件，输入每分钟 10 微升的流速，要求总溶液量为 5 毫升。用 25 个测量针将注射器固定到电夹装置中，并使用胶带将注射器固定到位。现在，将注射器朝向收集器，直到电击溶液流过 25 测量针。然后将针尖连接到双端鳄鱼夹，这些夹也连接到收集器。在启动电击程序之前，打开滚子，以 100 rpm 转速旋转收集器。然后启动电击程序软件。当旋转开始时，将施加的电压调制为 16 千伏，以便泰勒圆锥体形成。电击工艺完成后，用剃须刀将柔性不锈钢上的 as-spun 纳米纤维报废，然后转移到氧化铝盒中。然后将氧化铝盒插入箱炉，并设置箱炉的热处理条件。烧结后，将炉子冷却至50摄氏度，然后将烧结纳米管转移到玻璃瓶中。首先，准备电极浆料。将铜箔放在玻璃基板上的铜箔顶部，使用铸造辊均匀地铸造到约 60 微米的厚度。然后在60摄氏度下将浆铸铝干燥10分钟。干燥后，密封在塑料袋中，直到准备好进行细胞组装。要开始细胞组装，将对流烤箱加热至150摄氏度，然后将浆铸铜箔放入烤箱。使用旋转泵将烤箱中的真空拉，以干燥浆料中的残留溶剂，同时避免铜箔氧化。在150摄氏度下将浆料铸铜箔加热两小时后，通过关闭真空管路并打开旋转泵中的通风管打开腔室，用空气重新填充对流炉。然后将浆铸铜箔从腔室中拿出，用圆形打孔机打孔。称重冲压的浆铸铜箔。使用半个电池组装电池，将浆铸铜箔放入电池底部。然后将样品转移到手套箱的前室。真空前室30分钟，然后将样品转移到内手套箱。在手套箱中，组装电池，从底部电池单元开始，然后浆料铸造铜箔、分离器、垫片、垫片、垫片、弹簧，最后是顶部电池。使用压实机将电池压缩到完整的电池中。然后将电池移入手套箱的前室。释放真空后，从手套箱中取出电池。在室温下将电池老化一到两天。然后将电池插入电池测试仪中。计算适当的电流，然后使用电池测试程序对每个电池施加适当的电流。首先，通过化学气相沉积合成石墨烯，用一把剪刀将铜箔与石墨烯切割成三百三毫米方。在两个玻璃滑梯之间放置四块铜箔，然后按压使其平整。下一个位置完全碳金网格在每块铜箔。在金栅铜箔组合上滴 20 微升异丙醇。然后去除酒精，在50摄氏度下干燥样品5分钟。接下来用异丙醇和去电化水清洁六厘米玻璃培养皿，以避免硅颗粒污染。然后加入十毫升0.1摩尔铵在菜和蚀刻铜箔。在溶液中孵育样品六小时。使用铂环将金栅片移动到装满去压水的玻璃培养皿中，并将其加热至 50 摄氏度，以便完全清除蚀刻中剩余的污染物。然后拆下网格，并在室温下干燥六小时。在10毫升电解质中分散0.06克纳米管粉末，由1.3摩尔六氟磷酸锂和乙烯碳酸乙烯和二甲苯碳酸酯组成，以3至7体积比，含氟乙烯碳酸10%的重量，准备电解质和纳米管混合物。然后将石墨烯转移的栅格和电解质混合物移动到装满砷的手套箱中。要组装单元格，请先在底部放置一个网格。然后在底部栅格上滴下20微升的电解质混合物。在电解质干燥之前，快速使用一对钳子将另一个网格放在底部网格的顶部。将手套箱内的样品干燥 30 分钟，在此期间，液体在干燥时自发地封装在两个石墨烯板之间。通过电击和随后的烧结制造的氧化锡纳米管如图所示。TEM 表明，这种多孔位点在视觉上更加清晰，纳米管中的一些白点表示。这是因为氧化锡的晶体结构是多晶锡石结构。就氧化锡纳米管的电化学特性而言，电荷和放电型材具有稳定的电压轮廓，初始耦合效率为67.8% 电压稳定，电压稳定在0.9伏特时，可归因于两相反应。氧化锡纳米管在500毫安/克时表现出稳定的循环，库洛比效率超过98%此外，纳米管即使在每克1000毫安的高电流密度下也保留相当大的容量。石墨烯液体细胞的时间序列TEM视频显示在多个液体口袋，其大小范围从300-400纳米。通过恒定的电子束照射，溶解的电子和基会触发盐和溶剂的二次反应。在这里观察到电解质的分解和SEI层的形成在初始阶段。处理石墨烯和 TEM 网格时要格外小心。如果您不能正确处理石墨烯和网格，它们很容易损坏。在电池组件中，必须紧密压缩电池，使电解质不会从电池中产生。该过程还可用于观察钠离子电池、镁离子电池和二次离子电池的动态。

Research

JoVE Journal

Engineering

Construction and Testing of Coin Cells of Lithium Ion Batteries

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

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

在固体氧化物燃料电池电极表面的探测和测绘

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

正极材料的同步辐射技术锂离子和钠离子电池表征

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

原位中子衍射用特制的锂离子电池

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

全套材料常数表征及其温度依赖性的压电材料使用共振超声波谱

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

锂离子纽扣电池的非水电极加工和施工

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

High-speed Continuous-wave Stimulated Brillouin Scattering Spectrometer for Material Analysis

用于材料分析的高速连续波受激布里渊散射光谱仪

Recent years have witnessed a significant increase in the use of spontaneous Brillouin spectrometers for non-contact analysis of soft matter, such as ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

基于 LiPON 的固态锂离子 Nanobatteries 的聚焦离子束制备方法在原位测试中的研究

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Preparation of Liquid Crystal Networks for Macroscopic Oscillatory Motion Induced by Light

光诱导的宏观振荡运动液晶网络的制备

A strategy based on doped liquid crystalline networks is described to create mechanical self-sustained oscillations of plastic films under continuous ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

锂离子电池三电极硬币电池制备及电沉积分析

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...