Name: in situ neutron powder diffraction using custom-made lithium-ion batteries
Uploaded: 2014-11-10T15:00:00.000+00:00
Duration: 11 min 25 s
Description: Watch this Scientific Journal Video about In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries at JoVE.com

We thank AINSE Ltd for providing support through the research fellowship and postgraduate award scheme.

1.需要电池组件在施工前注:钒可以被常规用于NPD的实验，它是被密封的一端，而在另一公开的全钒管。因此几乎从钒NPD的数据没有信号。 <ol><li>切下一块锂金属箔的向尺寸相匹配的钒罐的容积。例如，切一块约120×35毫米，9毫米口径的钒即可。此外，使用更薄的锂箔，以尽量减少中子吸收，并指出，厚度小于125微米可能难以处理而不会撕裂。 </li><li>预选择分离器的类型可以使用。切割的片材分离，使得所述尺寸比电极稍大， 例如 140×40毫米。 注意:当多孔聚乙烯基二氟乙烯（PVDF）膜容易吸收了电解液，它是昂贵的，并且可以很容易损坏和撕裂，如果不是在小心处理建设。可替换地，可商购的聚乙烯基片是更健壮，但是它们不吸收电解质那样容易和一般的信号 - 噪声降低由于较大的氢含量。 </li><li>使正电极由以下列出由标记的准则等 31即，结合的PVDF，碳黑，以及所述活性材料以选定的比例。典型地，使用聚偏氟乙烯的10:10:80的比例:碳:活性材料，但在调查调整这取决于材料。研磨混合物并加入正-甲基吡咯烷酮（NMP）中的溶液，直至浆液的形式，然后搅拌过夜。 </li><li>涂布在利用刮刀技术的铝箔（厚度为20μm）的混合物。 <ol><li>通过将几滴乙醇上的表面和将所述集电体的表面上附着的尺寸200×70毫米的光滑表面（ 例如玻璃）的集电板。另外，美国E，这可以拉动一个轻微的真空从光滑表面的电流收集器的工具。平滑的电流收集器，以确保没有皱纹或折痕之前施加的浆料。 </li><li>将浆液的齿或宽半圆状熔池上的集电体的一端。使用切口棒，辊子或专门设计的涂布器（具有预先定义的高度以上的集电体的凹口棒， 例如 100或200微米，通常使用）通过在集电体的滑动所选择的设备分散浆料中的集电和浆料，导致浆料的铺展在集电体表面。 </li><li>轻轻地除去从光滑表面的集电体，然后将集电体和分散浆料放入真空烘箱中干燥。 注:该扩频技术中更详细地Marks 等人描述31 </li></ol></li><li>切正极准备红色在步骤1.3，使得尺寸相匹配的锂箔。确保有未涂覆的金属集电体的一端约为0.5厘米的长度的"标签"。以提高电池的性能，按干燥正极片成用平板压制集电体。 注: 图1示出了在隔膜与正极组成部分的相对大小。在电极的最小活性材料量是300毫克，然而，较大的量（相对于其他电池组件），更好的NPD的信号。较大的信号可以允许更详细的信息可以从NPD的数据和更好的时间分辨率萃取。 </li><li>在氘代碳酸亚乙酯和氘代碳酸二甲酯的1:1（体积）％的混合物预先制备的1M六氟磷酸锂。确保所有的LiPF 6溶解和电解质彻底在使用前混合。 </li><li>切一块吨的集电他相同的尺寸，在步骤1.5的正极和称重的集电体和正极。减去这些质量，得到电极混合物的质量。乘以0.8的电极混合物的质量，得到活性物质的质量。 </li></ol> 2.小​​区建设<ol><li>之前组装在氩气填充的手套箱内的细胞，放下任一个塑料托盘或gloxebox的基础上，一些其他非金属覆盖物。 </li><li>栈的各个组件中的顺序如下:隔板的长条形，与浆料正极朝上和铝棒（或铜线），另一端卷绕在"标签"，分离器的所述第二条带，最后是锂金属与铜线缠绕在锂金属（同一端的铝棒）的端部。 </li><li>开始从一端与铝杆和铜线轧制所述层，从而确保两电极不接触到接触。 </li><li>如果聚乙烯系片被选定为隔板，偶尔几滴电解质添加到锂金属和正极沿层叠体的整个长度之间的分隔符。可替换地，在轧制过程中逐渐添加的液滴。如果PVDF膜作为隔膜此步骤不是必要的。 </li><li>小心以确保该电极被卷紧，该层保持对准。 注意:如果该层变得不对准的轧制过程中可能需要重新启动，但是，一定要小心，作为电解质溶液是极不稳定的，更可能需要添加。 </li><li>确保较长的一块隔板的完全堆叠周围包裹或滚使得电极不暴露（ 即在电极不碰钒壳体）。 </li><li>插入卷绕叠装入钒可以使得铜线和铝线杆伸出2-3厘米以外钒罐的顶部。添加剩余的电解液滴下到钒的​​顶部可以使用1.5毫升总共。 </li><li>加橡胶塞与凹槽切割在两侧的铝棒和铜线插入钒罐的顶部。通过熔化牙科蜡在罐的顶部和周围的铜线的塑料护套的端部密封罐。检查， 如图2中的最终细胞出现。 </li><li>让细胞"年龄"或"湿"水平为12-24小时。在使用之前，通过连接铝杆和铜线的多米端子和测量构成电池的电势测试开路电位。另外，还要确保没有泄漏目测。 </li></ol>

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Power Sources. 236, 163-168 (2013).</li><li>Doeff, M. M., 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=Characterization+of+electrode+materials+for+lithium+ion+and+sodium+ion+batteries+using+synchrotron+radiation+techniques.">Characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques.</a> J. Visualized Exp. , 50591-50594 (2013).</li></ol>

The authors have nothing to disclose.

当设计和现场试验执行，或者用"翻车"中子衍射细胞或另一种设计方案中，有一个数字，必须小心地控制，以确保成功的实验方面。这些包括仔细选择的类型和细胞组分的量，以确保所制得的电极和最终构建的细胞都是高质量的，选择合适的衍射条件，规划的电化学循环的步骤可以预先进行，终于了解什么产生的数据也并不能告诉一个约的材料正在调查中。 细胞成分的...

可充电锂离子电池为现代电子设备提供便携的能量，并在高能应用中非常重要，如电动汽车，并为大规模可再生能源发电的储能装置。3-7仍然存在一些挑战，实现普遍使用的可充电电池中的车辆与大型存储，包括能量密度和安全性。 原位方法中的用途的探测原子和分子级的电池功能操作期间正变得越来越普遍，获得了在这些实验中的信息可以直接的方法来改进现有的电池材料， 例如 ，通过确定可能的故障机制，8-10和通过揭示晶体结构可以考虑为下一代的材料。11 原位 NPD的主要目标是探测电池内部组件的晶体结构演变作为充电/放电的功能。为了测量晶体结构演变的组件必须是结晶，其重点是晶体有序电极等的研究。它是在该电荷载流子（锂）插入/抽出而这种变化之后的NPD的电极。 原位 NPD提供了可能性"跟踪"不仅反应机理和晶格参数的电极的演进，也插入/抽出从电极锂。基本上在锂离子电池的电荷载流子可以遵循。这使电池功能的锂为中心的视图，并且在只有少数的研究最近已经证明11-13 NPD是一种理想的技术，研究含有锂的材料和锂离子电池。这是因为，NPD的依赖于中子束和样品之间的相互作用。不像X射线粉末衍射（XRD），其中，所述相互作用的X射线辐射主要是与样品中的电子，从而线性地原子序数而变化，在NPD的相互作用是由导致更复杂的和明显的随机变异原子序数中子核的相互作用介导的。因此， 在原位 NPD是用于锂离子电池材料研究特别有希望的，由于多种因素，如NPD的朝锂原子在较重的元素的存在下的敏感性，中子与所述电池的非破坏性的相互作用，以及高穿透深度的中子使商用设备中使用的尺寸的整个电池中的电池组件的块状晶体结构的检查。因此， 原位 NPD是用于锂离子电池的研究，这些优势的结果是特别有用的。尽管如此， 在现场 NPD实验的电池研究界的摄取是有限的，仅占25出版物罪CE 1998年14所述的吸收有限是采用原位 NPD为电池研究的第一份报告，由于一些主要实验的障碍，如需要占很大的非相干中子散射横氢在电解质溶液和隔膜部在电池中，这是不利的NPD的信号。这通常是通过用与氘（2H）电解质溶液并用备用的无氢或较差的材料代替隔板克服15的另一个障碍是，需要有足够的样品中的中子束，一个要求，即往往需要使用的较厚的电极而这又限制了最大充电/可施加到电池放电速率。一个更实际关注的是相对小一些世界范围内的中子衍射仪相对于X射线衍射仪，其能力- 例如时间和角分辨率。随着新的中子diffractomeTER值都来网上和上述障碍克服， 就地 NPD实验种植数量。 有两个选项进行原位 NPD的实验中，使用商业或定制细胞。商业的细胞已被证明以显示结构的信息，包括锂的含量和分布在电极上的演变。8-11,16-20但是，使用商用单元限制了可以研究那些已经市售的电极的数量，并且其中厂家或选择研究设施从事生产商用型细胞尚未未商业化的材料。商用型电池的生产依赖于足量的电极材料用于制作电池的情况，典型的公斤的量级和显著高于电池的研究中使用，它可以是一个障碍，细胞产量更高。商业细胞TYpically设有两个电极中的充电/放电是进化和两个电极的演化会在所得的衍射图案被捕获。这是因为，中子束高度穿透性和能穿透单个锂离子电池（ 例如 ，18650细胞的整个体积）。两个电极的演变可以使数据的分析变得复杂，但是，如果两个电极的足够的布拉格反射被观测到，这些可使用全粉图案的方法来模拟。但是，定做半电池可以构造在其中一个电极是锂，且应在充电/放电结构上不发生变化，因此，作为一个（或另一个）内部标准。只留下一个应该表现出结构性变化，简化了数据分析电极。也必须小心，以确保所有感兴趣的电极反射不与其他组件的反射发生在细胞结构变化的重叠。广告定做的细胞的优势在于，组件可以被交换，以改变在衍射图案反射位置。此外，定制的细 ​​胞使得研究者的选项，在原则上，改善信号对噪声的比率，并调查所取得在较小规模的研究批次，由此允许更大的各种材料的原位 NPD的研究材料。 到目前为止，已经在原位的NPD的研究已经6的电化学电池设计为报告，其中包括三个圆柱形设计，14,15,21,22 2的硬币型电池的设计23-26和袋的单元设计。12,27第一圆柱形电池设计中使用限于非常低的充电/由于大量的电极材料使用的放电速率。14,21的翻转的设计，下面15详细描述的，修改后的版本的原始筒状细胞的22克服了许多的与T有关的问题他第一圆柱形设计，并且可以用于可靠地相关联的电极材料的结构与其电化学。硬币电池设计用于原位 NPD还允许相似量的电极材料被探测相对于该翻转单元，同时具有在施工，适用的充电率和成本方面的细微差别。15具体地，币形电池类型最近有报道使用的Ti-Zn系合金作为外壳材料（零矩阵），它产生没有信号在NPD的图案已经被建造。26这类似于以下描述的翻车设计的使用钒罐。能够影响适用的充电/放电率（和偏振）的关键因素是电极的厚度，其中典型地较厚的电极需要低电流的应用。小区设计，现在变得更流行的是小袋的细胞与并联连接的多个个体的细胞，或片材的片材看得太被卷在一个类似的方式的锂离子电池中的移动电子设备中找到的建筑。12,27这种细胞是矩形（袋），其可以在更高的充电/放电率比翻车或硬币型函数细胞。在这项工作中，我们把重点放在&#39;翻车&#39;单元设计，显示单元建设，使用，以及使用电池了一定的成效。 该电极准备翻车设计的电池实际上是类似的电极制备用于传统纽扣电池使用到。该电极可浇铸到集电体通过刮刀，具有最大的不同之处在于，电极需要跨越尺寸大于35×120-150毫米。这可能难以均匀地涂布与每一个电极的材料。在集电体上的集电体，隔板和锂金属箔与电极的层布置，轧制，并插入到钒罐。电解液使用d为的LiPF 6，在锂离子电池用氘代碳酸乙烯酯和氘代碳酸二甲酯是最常用的一种盐。此细胞已被成功地用于在四个报告的研究和在下文中更详细地描述。15,28-30

<table><tbody><tr><td colspan="4">&lt;strong&gt;Slurry Preparation&lt;/strong&gt;</td></tr><tr><td>PVDF</td><td>MTI Corporation</td><td>EQ-Lib-PVDF</td><td>http://www.mtixtl.com/PVDFbinderforLi-ionbatteryelectrodes80g/bag-EQ-Lib-PVDF.aspx</td></tr><tr><td>Active Electrode Material</td><td>Researcher makes*</td><td></td><td>This is dependent on the electrode under investigation, typically made in-house by the researcher and varies every time</td></tr><tr><td>Carbon black</td><td>MTI Corporation</td><td>EQ-Lib-SuperC65</td><td>http://www.mtixtl.com/TimicalSUPERC65forLithium-IonBatteries80g/bag-EQ-Lib-SuperC65.aspx</td></tr><tr><td>NMP</td><td>MTI Corporation</td><td>EQ-Lib-NMP</td><td>http://www.mtixtl.com/N-Methyl-2-pyrrolidoneNMPsolventforPVDF&lt;br/&gt; 250g/bottleLib-NMP.aspx</td></tr><tr><td>Magnetic stirrer</td><td>IKA</td><td>C-MAG HS 7 IKAMAG</td><td>http://www.ika.in/owa/ika/catalog.product_detail?iProduct=3581200</td></tr><tr><td colspan="4">&lt;strong&gt;Electrode Fabrication&lt;/strong&gt;</td></tr><tr><td>Doctor blade (notch bar)</td><td>DPM Solutions Inc.</td><td>100, 200, 300 &amp;amp; 400 micron&amp;nbsp; 4-Sided Notch Bar</td><td></td></tr><tr><td>Al or Cu current collectors</td><td>MTI Corporation</td><td>EQ-bcaf-15u-280</td><td>http://www.mtixtl.com/AluminumFoilforBatteryCathodeSub&lt;br/&gt; strate-EQ-bcaf-15u-280.aspx</td></tr><tr><td>Vacuum Oven</td><td>Binder</td><td>&lt;em&gt;e.g.&lt;/em&gt; VD 53</td><td>http://www.binder-world.com/en/vacuum-drying-oven/vd-series/vd-53/</td></tr><tr><td>Flat-plate press</td><td>MTI Corporation</td><td>EQ-HP-88V-LD</td><td>http://www.mtixtl.com/25THydraulicFlat&lt;br/&gt; HotPress-EQ-HP-88V.aspx</td></tr><tr><td colspan="4">&lt;strong&gt;Roll-over cell construction&lt;/strong&gt;</td></tr><tr><td>V can</td><td></td><td></td><td></td></tr><tr><td>electrode on Al/Cu</td><td>MTI Corporation</td><td>EQ-bcaf-15u-280</td><td>http://www.mtixtl.com/AluminumFoilforBatteryCathodeSub&lt;br/&gt; strate-EQ-bcaf-15u-280.aspx</td></tr><tr><td>polyethylene-based or PVDF membrane</td><td>MTI Corporation</td><td>EQ-bsf-0025-400C</td><td>http://www.mtixtl.com/separatorfilm-EQ-bsf-0025-400C.aspx</td></tr><tr><td>LiPF&lt;sub&gt;6&lt;/sub&gt;</td><td>Sigma-Aldrich</td><td>450227</td><td>http://www.sigmaaldrich.com/catalog/product/aldrich/450227?lang=en&amp;amp;region=AU</td></tr><tr><td>deuterated dimethyl carbonate</td><td>Cambridge Isotopes</td><td>DLM-3903-PK&amp;nbsp;</td><td>http://shop.isotope.com/productdetails.aspx?id=10032379&amp;amp;itemno=DLM-3903-PK</td></tr><tr><td>deuterated ethylene carboante</td><td>CDN Isotopes</td><td>D-5489</td><td>https://www.cdnisotopes.com/as/products/specifications/D-5489.php?ei=YWVraWmjoJ1i0lZ7nkr0RpwHr&lt;br/&gt; Hxc9ornu14O4WUtZKbZWZrcq6j55&lt;br/&gt; G0lOab3Wi0dMZ7xc+0Yse1leWVtZ&lt;br/&gt; LnrGKvta7v591o4JrnkbRowHt/r</td></tr><tr><td>Li metal foil</td><td>MTI Corporation</td><td>Lib-LiF-30M</td><td>http://www.mtixtl.com/Li-Foil-30,000 ml-35 mmW-0.17 mm&lt;br/&gt; Th.aspx</td></tr><tr><td>Rubber stopper cut to size</td><td>generic eraser</td><td></td><td>cut a generic eraser to size</td></tr><tr><td>dental wax</td><td>Ainsworth Dental</td><td>AIW042</td><td>http://www.ainsworthdental.com.au/catalogue/Ainsworth-Modelling-Wax-500g.html</td></tr><tr><td>Copper wire (insulated)</td><td>generic</td><td></td><td>sheathed Cu wire that can be cut to size</td></tr><tr><td>Aluminum rod (&amp;lt;2 mm diameter)</td><td>generic</td><td></td><td>cut to size as required</td></tr><tr><td>Glovebox</td><td>Mbraun</td><td>UNILab</td><td>http://www.mbraun.com/products/glovebox-workstations/unilab-glovebox/</td></tr><tr><td>Scissors&amp;nbsp;</td><td>generic</td><td></td><td></td></tr><tr><td>Soldering iron</td><td>generic</td><td></td><td></td></tr><tr><td colspan="4">&lt;strong&gt;&lt;em&gt;In situ&lt;/em&gt; NPD&lt;/strong&gt;</td></tr><tr><td>Appropriate neutron diffractometer</td><td>ANSTO</td><td>Wombat</td><td>http://www.ansto.gov.au/ResearchHub/Bragg/Facilities/Instruments/Wombat/</td></tr><tr><td>Potentiostat/galvanostat</td><td>Autolab</td><td>PGSTAT302N</td><td>http://www.ecochemie.nl/Products/Echem/NSeriesFolder/PGSTAT302N</td></tr><tr><td>Connections to battery from potentiostat/galvanostat</td><td>generic</td><td></td><td></td></tr><tr><td>Training of NPD instrument and use</td><td></td><td></td><td></td></tr><tr><td colspan="4">&lt;strong&gt;Data analysis&lt;/strong&gt;</td></tr><tr><td>Data visualisation and peak fitting, .&lt;em&gt;e.g.&lt;/em&gt; LAMP suite</td><td>ILL</td><td>LAMP</td><td>http://www.ill.eu/instruments-support/computing-for-science/cs-software/all-software/lamp/</td></tr><tr><td>Rietveld analysis software, &lt;em&gt;e.g.&lt;/em&gt; GSAS</td><td>APS</td><td>GSAS</td><td>https://subversion.xray.aps.anl.gov/trac/EXPGUI</td></tr></tbody></table>

in situ neutron powder diffraction using custom-made lithium-ion batteries

锂离子电池被广泛应用于便携式电子装置和被认为是有前途的候选者能量较高的应用，如电动汽车。1,2-然而，许多挑战，如能量密度和电池寿命，需要在此之前尤其要克服电池技术可广泛实施中这样的应用程序。3本研究是具有挑战性的，并且我们概述的方法，以解决利用原位 NPD的探测电极进行电化学循环（充电/放电）在电池中的晶体结构，这些挑战。 NPD的数据帮助确定负责一系列的电极性能的潜在的结构性机制，这些信息可以直接更好的电极和电池的发展。 我们简要回顾一下六类电池设计定做的NPD的实验和细节构造"翻转"电池，我们有方法成功地用在高强度NPD仪，WOMBAT，在澳大利亚核科学和技术组织（ANSTO）。用于细胞结构的设计考虑和材料结合实际的原位 NPD的实验和初始方向的各方面讨论给出关于如何分析这样复杂的现场数据。

我们已经证明了通用性使用文献15,28-30此翻车细胞，在这里我们提出一个例子与李锶0.18 0.66 0.5钛铌0.5 O 3电极。32 之前尝试顺序Rietveld精修（全谱拟合为充电状态的函数），多相模型到第一数据集的一个单一的细化进行，在该数据收集之前，当前的应用程序的原始细胞。几种模式进行了测试，以确定哪个结构参数可以精确地细化。理想?...

Watch this Scientific Journal Video about In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries at JoVE.com

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

我们描述了电极材料采用原位中子衍射（NPD）考试的电化学电池的设计和施工。我们简单地交替在原地 NPD单元设计意见，并讨论了相应的使用这种细胞原位产生的NPD数据的分析方法。

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 ...

in-situ-neutron-powder-diffraction-using-custom-made-lithium-ion

Research

JoVE Journal

Engineering

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

15.7K 次观看.  University of Sydney. 我们描述了电极材料采用原位中子衍射（NPD）考试的电化学电池的设计和施工。我们简单地交替在原地 NPD单元设计意见，并讨论了相应的使用这种细胞原位产生的NPD数据的分析方法。 

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

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

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

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

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. ...

Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions.

A shear cell is developed for small-angle neutron scattering measurements in the velocity-velocity gradient plane of shear and is used to characterize complex fluids. Spatially resolved measurements in the velocity gradient direction are possible for studying shear-banding materials. Applications include investigations of colloidal dispersions, polymer solutions, and self-assembled structures.

测量材料在微流使用1-2面流小角中子散射

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is ...

Using Neutron Spin Echo Resolved Grazing Incidence Scattering to Investigate Organic Solar Cell Materials

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped crystallites. Neutrons are passed through two well defined regions of magnetic field; one before and one after the sample. The two magnetic field regions have opposite polarity and are tuned such that neutrons travelling through both regions, without being perturbed, will undergo the same number of precessions in opposing directions. In this case the neutron precession in the second arm is said to &#34;echo&#34; the first, and the original polarization of the beam is preserved. If the neutron interacts with a sample and scatters elastically the path through the second arm is not the same as the first and the original polarization is not recovered. Depolarization of the neutron beam is a highly sensitive probe at very small angles (&#60;50&#160;&#956;rad) but still allows a high intensity, divergent beam to be used. The decrease in polarization of the beam reflected from the sample as compared to that from the reference sample can be directly related to structure within the sample.
In comparison to scattering observed in neutron reflection measurements the SERGIS signals are often weak and are unlikely to be observed if the in-plane structures within the sample under investigation are dilute, disordered, small in size and polydisperse or the neutron scattering contrast is low. Therefore, good results will most likely be obtained using the SERGIS technique if the sample being measured consist of thin films on a flat substrate and contain scattering features that contains a high density of moderately sized features (30 nm to 5 &#181;m) which scatter neutrons strongly or the features are arranged on a lattice. An advantage of the SERGIS technique is that it can probe structures in the plane of the sample.

Progress has been made in utilizing spin echo resolved grazing incidence scattering (SERGIS) as a neutron scattering technique to probe the length-scales in irregular samples. Crystallites of [6,6]-phenyl-C61-butyric acid methyl ester have been probed using the SERGIS technique and the results confirmed by optical and atomic force microscopy.

使用中子自旋回声解决放牧发生率散射调查有机太阳能电池材料

The spin echo resolved grazing incidence scattering (SERGIS) technique has been used to probe the length-scales associated with irregularly shaped ...

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 ...

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

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational analysis. Testing of lithium-ion batteries in an academic setting has taken on several forms, but at the most basic level lies the coin cell construction. In traditional LIB electrode preparation, a multi-phase slurry composed of active material, binder, and conductive additive is cast out onto a substrate. An electrode disc can then be punched from the dried sheet and used in the construction of a coin cell for electrochemical evaluation. Utilization of the potential of the active material in a battery is critically dependent on the microstructure of the electrode, as an appropriate distribution of the primary components are crucial to ensuring optimal electrical conductivity, porosity, and tortuosity, such that electrochemical and transport interaction is optimized. Processing steps ranging from the combination of dry powder, wet mixing, and drying can all critically affect multi-phase interactions that influence the microstructure formation. Electrochemical probing necessitates the construction of electrodes and coin cells with the utmost care and precision. This paper aims at providing a step-by-step guide of non-aqueous electrode processing and coin cell construction for lithium-ion batteries within an academic setting and with emphasis on deciphering the influence of drying and calendaring.

Non-aqueous electrode processing is central to the construction of coin cells and the evaluation of new electrode chemistries for lithium-ion batteries. A step-by-step guide to the basic practices needed as an electrochemical engineer working with batteries in an academic experimental setting is furnished.

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 ...

Measuring Spray Droplet Size from Agricultural Nozzles Using Laser Diffraction

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to make an application so that the material reaches the target site (i.e., plant). Information critical in this process is the droplet size that a particular spray nozzle, spray pressure, and spray solution combination generates, as droplet size greatly influences product efficacy and how the spray moves through the environment. Researchers and product manufacturers commonly use laser diffraction equipment to measure the spray droplet size in laboratory wind tunnels. The work presented here describes methods used in making spray droplet size measurements with laser diffraction equipment for both ground and aerial application scenarios that can be used to ensure inter- and intra-laboratory precision while minimizing sampling bias associated with laser diffraction systems. Maintaining critical measurement distances and concurrent airflow throughout the testing process is key to this precision. Real time data quality analysis is also critical to preventing excess variation in the data or extraneous inclusion of erroneous data. Some limitations of this method include atypical spray nozzles, spray solutions or application conditions that result in spray streams that do not fully atomize within the measurement distances discussed. Successful adaption of this method can provide a highly efficient method for evaluation of the performance of agrochemical spray application nozzles under a variety of operational settings. Also discussed are potential experimental design considerations that can be included to enhance functionality of the data collected.

We present protocols to be used in the measurement of spray droplet size from agricultural nozzles used in both aerial and ground based agrochemical applications. These methods presented were developed to provide consistent and repeatable droplet size data both inter- and intra-laboratory, when using laser diffraction systems.

从农业喷嘴采用激光衍射测量喷雾的雾滴尺寸

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to ...

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

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

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

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

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 ...

Elemental-sensitive Detection of the Chemistry in Batteries through Soft X-ray Absorption Spectroscopy and Resonant Inelastic X-ray Scattering

Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid based on volatile solar and wind sources. The pressing demand of developing high-performance electrochemical energy storage solutions, i.e., batteries, relies on both fundamental understanding and practical developments from both the academy and industry. The formidable challenge of developing successful battery technology stems from the different requirements for different energy-storage applications. Energy density, power, stability, safety, and cost parameters all have to be balanced in batteries to meet the requirements of different applications. Therefore, multiple battery technologies based on different materials and mechanisms need to be developed and optimized. Incisive tools that could directly probe the chemical reactions in various battery materials are becoming critical to advance the field beyond its conventional trial-and-error approach. Here, we present detailed protocols for soft X-ray absorption spectroscopy (sXAS), soft X-ray emission spectroscopy (sXES), and resonant inelastic X-ray scattering (RIXS) experiments, which are inherently elemental-sensitive probes of the transition-metal 3d and anion 2p states in battery compounds. We provide the details on the experimental techniques and demonstrations revealing the key chemical states in battery materials through these soft X-ray spectroscopy techniques.

Here, we present a protocol for typical experiments of soft X-ray absorption spectroscopy (sXAS) and resonant inelastic X-ray scattering (RIXS) with applications in battery material studies.

软 x 射线吸收光谱和共振非弹性 x 射线散射法检测电池化学成分的元素敏感度

Energy storage has become more and more a limiting factor of today's sustainable energy applications, including electric vehicles and green electric grid ...

化学

Identification and Quantification of Decomposition Mechanisms in Lithium-Ion Batteries; Input to Heat Flow Simulation for Modeling Thermal Runaway

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of thermal runaway (TR), the exothermic decomposition reactions in anode and cathode were studied, using a Simultaneous Thermal Analysis (STA)/Gas Chromatography-Mass Spectrometry (GC-MS)/Fourier Transform Infrared (FTIR) spectrometer system. These techniques allowed the identification of the reaction mechanisms in each electrode, owing to the analysis of evolved gaseous species, the amount of heat released and mass loss. These results provided insight into the thermal events happening within a broader temperature range than covered in previously published models. This allowed the formulation of an improved thermal model to depict TR. The heat of reaction, activation energy, and frequency factor (thermal triplets) for each major exothermic process at material level were investigated in a Lithium Nickel-Manganese-Cobalt-Oxide (NMC (111))-Graphite battery cell. The results were analyzed, and their kinetics were derived. These data can be used to successfully simulate the experimental heat flow.

This work aims at determining the reaction kinetics of Li-ion battery cathode and anode materials undergoing thermal runaway (TR). Simultaneous Thermal Analysis (STA)/Fourier Transform Infrared (FTIR) spectrometer/Gas Chromatography Mass Spectrometry (GC-MS) were used to reveal thermal events and to detect evolved gases.

锂离子电池分解机理的鉴定和量化;用于模拟热失控的热流仿真输入

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of ...