这项工作是由助理秘书长能源效率和可再生能源，能源的美国能源部车辆技术合同号DE-AC02-05CH11231办公室的支持。这项研究的部分进行了在斯坦福同步辐射一个LightSource，为SLAC国家加速器实验室一局和斯坦福大学经营了科学的能源办公室，美国能源部科学用户设施的办公室。该SSRL结构分子生物学项目是由生物和环境研究的美国能源部办公室的支持，并通过健康，国家研究资源中心，生物技术计划（P41RR001209）全国学院。

1。实验规划<ol><li>确定感兴趣的束线实验。请参阅束线网页作为指南。对于SSRL XAS和XRD，这些are: <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl4-1/" target="_blank">http://www-ssrl.slac.stanford.edu/beamlines/bl4-1/</a> and <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl4-3/" target="_blank">http://www-ssrl.slac.stanford.edu/beamlines/bl4-3/</a> and <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl11-3/" target="_blank">http://www-ssrl.slac.stanford.edu/beamlines/bl11-3/</a> <ol><li>联系光束线的科学家，讨论实验细节。 </li></ol></li><li>通过去相关网站查询期限和建议书的要求。 </li><li>写束时间的建议，并提交。 </li><li>之后，该提案已经被拿下，进度束时间。 </li><li>按照所提供的设施，为光束的时间准备的指示。考虑实验中，T的细节材料ransport（特别是含有碱金属装置）和设备，以及任何安全问题。安全培训通常需要为新用户。 </li></ol> 2。材料，电极和电池的制备<ol><li>合成或获得的利益活性物质。 </li><li>表征材料通过常规的X-射线粉末衍射仪，采用步骤2.2.1-2.2.9。 <ol><li>研磨粉和筛，以确保均匀的粒度分布。 </li><li>加载样品放入样品架。从支架上取下背板，并把它反对载玻片上。粉末填充模腔，然后将背板，支架翻转和删除幻灯片。这确保了粉末是即使在支架的表面和该表面是平的。 </li><li>登录到日志的衍射。 </li><li>将样品架成衍射仪和调整。 </li><li>关闭门衍射仪。 </li><li>使用连接到泛在计算机数据采集程序alytical衍射仪，增加电压，并适合于测量值的电流。选择实验狭缝和梁口罩。选择或修改程序扫描。 </li><li>启动程序和数据文件的名称。由当程序提示刷徽章锁定衍射仪门。收集数据。 </li><li>采用高分程序分析模式。特别是，寻找杂质（额外的反射）的存在和模式是否匹配的参考材料或计算模式。 </li><li>从衍射仪取出样本。调低电流和电压，并关闭车门。登出，并指出任何不寻常的条件。 </li></ol></li><li>获得的扫描电子显微照片，以评估颗粒形态，采用步骤2.3.1-2.3.10。 <ol><li>通过将碳胶带铝存根，并洒样品粉末粘到一边准备样品。通过举办一个厨房磁铁在样本测试磁性。 </li><li>通过airlo将样品放入扫描电镜室CK。 </li><li>一旦真空建立后，打开加速电压。 </li><li>在低倍率时，调整对比度和亮度。这是最方便地进行使用ACB按钮。 </li><li>通过手动扫描在x和y方向上找到感兴趣的区域。 </li><li>切换到SEM或温柔的光束模式，如果更高的放大倍率是需要的。选择期望的检测器，并设置工作距离为适合于实验值。 </li><li>使用ACB旋钮调节对比度和亮度。 </li><li>聚焦影像与舞台Ž控制。 </li><li>对齐束，矫正散光和重点使用x和y旋钮。 </li><li>拍照的需要，使用照片按钮，并保存到相应的文件夹在电脑上。 </li><li>完成后，关闭加速电压。移动样品交换位置，并通过气闸从室内除去。 </li></ol></li><li>如果需要，用ICP进行元素分析，并与诸如IR任何其他所需的技术特征的材料或拉曼光谱。 </li><li>制作电极，使用步骤2.5.1-2.5.8。 <ol><li>使5-6％的N-甲基吡咯烷酮（重量）聚偏二氟乙烯（PVDF）（NMP）中的溶液。 </li><li>磨一起活性物质，导电助剂（乙炔黑，石墨等 ）。 </li><li>添加NMP溶液从步骤2.3.1步骤2.3.2干燥粉末，混匀。比例取决于活性物质的性质而变化，但80:10:10（活性物质:PVDF:导电助剂）的最终干组合物是常见的。 </li><li>使用刮刀和（可选地）在真空表，铸电极浆料上的Al或Cu集流体上。碳涂层铝箔可用于锂离子电池的正极材料和所有的Na离子电极材料，铜箔，用于锂离子负极材料。 </li><li>让电极风干。 </li><li>进一步使用红外灯，加热板，或真空烘箱干燥的电极。 </li><li>切割或打孔电极所需的大小。权衡ELECTR赞歌。 </li><li>传输电极，以在惰性气氛手套箱中。使用连接到手套箱真空加热前室的额外的干燥步骤，建议以除去所有残余的水分。 </li></ol></li><li>组装电化学装置（一般硬币电池，但其它构造可用于电化学特性）对于初始特性， 易地样品，和/或束流线的实验中，使用以下步骤2.6.1-2.6.7。 <ol><li>聚集在惰性气氛手套箱所有需要的组件。 </li><li>切断锂或钠箔到所需的大小。 </li><li>切割微孔隔板到所需的大小。 </li><li>层组件在装置顺序是:电极，隔膜，电解液和锂或钠箔。 </li><li>根据需要添加垫片和波形垫圈。 </li><li>使用纽扣电池按密封电池。 </li><li> 原位 X射线衍射试验中，附上标签以纽扣电池的两侧，并在聚酯袋密封装置。</li></ol></li><li>进行电化学实验初步鉴定或异地工作，用步骤2.7.1-2.7.6。 <ol><li>由恒电位仪/恒电流仪或循环仪设备连接引线和测量开路电位。 </li><li>写程序，用于电化学实验所需或选择归档程序。 </li><li>运行试验并收集数据。 </li><li> 易地实验，拆卸装置在手套箱，注意不要短路了。对于钮扣电池，使用一个纽扣电池反汇编工具或钳子包裹特氟龙胶带。 </li><li>冲洗电极与二甲基碳酸酯以除去残留的电解质盐。让它们干燥。 </li><li>覆盖电极易地研究与卡普顿箔X射线衍射实验或透明胶带的XAS和手套箱店，直到进行实验。 </li></ol></li><li>粉末用于研究XAS应过筛，以确保粒径均质药敏实验。可将它们洒在几件透明胶带。一系列样品然后可以通过堆叠逐步更大量片粉末磁带一起制备。如果用户是不确定所需的最佳信号粉末的量，这是特别有用的。 <ol><li>另外，粉末X光吸收测量可能，如果用户有信心将导致最佳的信号是什么来稀释BN。 </li></ol></li></ol> 3。实验在同步加速器设施的性能<ol><li>数天前，实验开始，材料和设备的计划运输到工厂。 <ol><li>对于含有碱金属阳极设备，运输是必需的，以避免运输中的个人或公共车辆有关的危害。 </li><li>设备如便携式恒电流/恒电位仪和笔记本电脑无害的样品，如易地工作电极可brougHT到该设施由个人进行任何方便的方式的实验。 </li></ol></li><li>检查并登记在该设施。 </li><li>对于这两个在原地和异地 X射线衍射实验，取实验6为了校准的参考模式。 <ol><li>联系光束线的科学家和工作人员的指示。 </li><li>校准光束，以找到合适的束条件。 </li><li>测量实验6的参考模式。 </li></ol></li><li> 原位 X射线衍射实验，设置设备并开始实验以下步骤3.4.1-3.4.6。 <ol><li>插入袋入铝压力板和确保孔正确对准，以允许X射线束来传输。 </li><li>寻找最佳的光束位置和曝光时间。长期接触可导致过饱和。确定样品中是否会受到冲击或固定。 </li><li>取初始模式电化学开始之前。 </li><li>从镀锌附加信息anostat /电位到设备。 </li><li>开始电化学实验。 </li><li>获取数据。一旦实验正在进行，数据收集是自动的，用户只需要以监督，以确保试验正在按计划进行。 </li></ol></li><li>成立XAS实验。 <ol><li>检查并联系光束线的科学家和工作人员的指示。 </li><li>将样品和箔参考材料（根据被测量的金属， 如镍为镍K表边缘）。 </li><li>对准样品。 </li><li>使用IFEFFIT的赫菲斯托斯确定具体的金属边缘的能量。调整单色仪，然后去调了约30％，以消除高次谐波。改变增益调整I 1和I 2测量偏移。 </li><li>进行测量。两个或两个以上的扫描，应采取并合并为感兴趣的元素。 </li><li>额外的元素重复步骤3.5.3至3.5.5，如需要。 </li></ol></li></ol> 4。数据分析<ol><li>对于X射线衍射工作，校准实验6图像。 <ol><li>下载区衍射机，这是可以通过谷歌代码（ <a href="http://code.google.com/p/areadiffractionmachine/" target="_blank">http://code.google.com/p/areadiffractionmachine/</a> ）。 </li><li>打开图像的实验6衍射和使用初始校准值从文件头。 </li><li>打开参考Q（=2π/ D）实验6的值。 </li><li>校准用Q值和校准值的初始猜测的实验6衍射图像。 </li><li>通过图像拟合得到正确的校准值。 </li><li>保存校准值到校准文件。 </li></ol></li><li>从标定实验数据的图像。 <ol><li>打开从实验的衍射图像。 </li><li>从实验室6引用（保存在步骤4.1.6）打开校准文件。 </li><li>开放日铝或铜（集电器的电极）电子参考Q（=2π/ D）值，并把它们作为内部参考。 </li><li>通过图像拟合校正模式的图像。 </li><li>整合图像Q主场迎战强度数据（行扫描）。 </li><li>使用所需的拟合程序拟合模式（CelRef，Powdercell，RIQAS，GSAS， 等等 ）。 </li></ol></li><li>使用任何方便的绘图程序（Excel中，产地，Kaleidagraph科学，伊戈尔等 ）电化学处理数据。 </li><li>对于XAS数据，使用ARTEMIS / ATHENA在IFEFFIT软件包进行分析。 <ol><li>利用在基准金属的吸收光谱的导数的第一个峰校准数据。 </li><li>合并像扫描。 </li><li>扣除背景和规范的数据。 </li><li>使用AUTOBK函数来隔离EXAFS数据。 </li><li>傅里叶变换的EXAFS数据。 </li><li>使用适合于R或K空间傅立叶变换光谱最小二乘提取structura升信息。 </li></ol></li></ol>

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C., Pianetta, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Three-dimensional+Imaging+of+Chemical+Phase+Transformation+at+the+Nanoscale+with+Full-Field+Transmission+X-ray+Microscopy.">Three-dimensional Imaging of Chemical Phase Transformation at the Nanoscale with Full-Field Transmission X-ray Microscopy.</a> J. Synchrotron Rad. 18, 773-781 (2011).</li><li>Liu, X., 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=Phase+Transformation+and+Lithiation+Effect+on+Electronic+Structure+of+LixFePO4:+An+In-Depth+Study+by+Soft+X-ray+and+Simulations.">Phase Transformation and Lithiation Effect on Electronic Structure of LixFePO4: An In-Depth Study by Soft X-ray and Simulations.</a> J. Am. Chem. Soc. 134, 13708-13715 (2012).</li><li>Sokaras, D., 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=A+High+Resolution+and+Solid+Angle+X-ray+Raman+Spectroscopy+End-Station+at+the+Stanford+Synchrotron+Radiation+Lightsource.">A High Resolution and Solid Angle X-ray Raman Spectroscopy End-Station at the Stanford Synchrotron Radiation Lightsource.</a> Rev. Sci. Instrum. 83, 043112 (2012).</li><li>Chan, M. K. 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=Structure+of+Lithium+Peroxide.">Structure of Lithium Peroxide.</a> J. Phys. Chem. Lett. 2, 2483-2486 (2011).</li></ol>

作者什么都没有透露。

的XANES数据分析表明，随着国产的LiNi x坐标1-2X锰×○2（0.01≤X≤1）的化合物，含有Ni 2 +，Co 3 +和Mn 4 + 10上的LiNi最近原位 XAS研究0.4钴0.15铝0.05的Mn 0.4 O 2表明，Ni 2 +的氧化，镍3 +和最终的Ni 4 +脱锂过程中，但涉及的Co 3 +的氧化还原过程提供一些容量，即使在低的状态-的电荷，违背先前的假设7。涉及低钴组成的另一项研究，的LiNi 0.45公司0.1-YŸ铝锰0.45 O 2，还表示，公司是电的脱锂11的早期阶段。 同步加速器X射线衍射12和XAS一系列的NMC与组成的LiNi 0.4 11项研究5锰0.45钴0.1-Y的Al Y 2 O 2（0≤Y≤0.1）已经取得了见解的Al代变种的提高电化学性能。所获得的原始粉末的高分辨率同步加速器X射线衍射图谱分析表明，在y = 0.1的材料表现出轻微的单斜扭曲，在常规的粉末X射线衍射图谱没有可辨。以减轻应变的过渡金属架，其中包括具有不同的平衡MO距离含金属的边缘共用八面体，局部范围订货时，产生的失真。应变缓解失真是由EXAFS数据11仔细检查进一步证实。电化学循环导致额外的压力，虽然在EXAFS数据中观察到的变化是对含Al电极小。 在含锂电池原位 X射线衍射实验，这些NMC阴极过程中电池充电（delithiatio表明晶格变化n）的体积较小的铝取代的材料比为未取代的基线。在延长的循环更少的结构变化也观察到在含Al电极。 偏铝 ​​置换也已经提出，以稳定正交的LiMnO 2电极13上的可能手段。这种材料迅速地从原来的锯齿形层状结构转变为尖晶石在电化学循环，与电化学性能随之而来的恶化。然而，在此期间观察到的，用25％的Al取代的电极原位 XRD实验没有稳定效果，实际上，由于尖晶石形成的反射被观测到，即使在最初的充电电池14。 过渡金属排序在高电压尖晶石与标称成分的LiNi 0.5锰1.5 O 4，预计影响电压及其他程度在操作单元15的材料的电化学特性。在有序材料（空间群P4 3 32）中，Ni和Mn占据4a和12d的八面体位置，分别，而在无序变体（空间群Fd3_m）中的过渡金属是随机分布的八面体16d位置。 在现场实验中得到的两个样本不同程度的过渡金属订货在同步加速器X射线衍射图谱的比较显示非常不同的相行为脱锂过程中处理16。最初的脱锂在无序材料具有很宽的固溶区域，具有在高温状态 - 的电荷观察到两个窄两相区。固溶体区域小得多的排序的材料，并观察到在大约x = 0.3的组合物的3相共存中的 Li x镍0.5的Mn 1.5 O 4，由两个小的两阶段R侧翼egions。在该阶段的行为，这被认为是由于变化的锂空位排序方案的异同，提出了为有序和无序的LiNi 0.5锰1.5 O 4之间观察到的速率能力的差异作出解释。与预期相反，但是，在参照图16的更有序的材料在这方面比无序的样品表现较好。这归因于形貌的影响;无序样品的颗粒组成板的暴露（112）小面的，而那些在排序的材料呈八面体与（111）面方面。 除了 ​​订货和形态的影响，的LiNi 0.5 Mn的物理和电化学特性1.5 O 4的又依赖于杂质含量和Mn 3 +的量。在合成过程中使用的高温处理过程中，含Ni岩盐杂质形成并一些锰4 +被还原成Mn 3 +中的主相。它可以是难以检测，因为峰重叠的X射线衍射图谱少量岩盐杂质，或者确定它的确切组合物，其随热处理。的Ni和MnĶ边XANES数据分析揭示了显著量在1000℃17制成的样品中同时含有Ni和Mn岩盐杂质的存在。 这里所描述的技术被引向理解批量过程中电极进行充放电。该假设是结构改变使用非常小的光斑尺寸（ 例如，0.15毫米×0.15毫米在束线11-3）对于实验的典型的电极作为一个整体的观察。这通常适用于制作精良的电极和电池，采用低电流密度和上述相对较长的充放电次数。 易地结果也有一般LY获得上进行正常的操作，然后对已经历平衡在电池的电极。在某些情况下，然而，它可以是有启发性的非平衡条件下，得到的结果获得的电池的电极操作过程中的故障模式的理解在高电流密度或各种滥用条件下进行。不均匀的电荷分布，可能会发生在这种情况下，尤其是当电极或细胞是未优化的。的不均匀性，可能导致过度充电或放电的局部区域​​，引起结构退化，最终将导致器件的性能降低和安全性。同步加速器X射线microdiffraction技术最近被用于映射电荷分布在磷酸铁锂的电极在高利率18充电。虽然此进行易地中，LiFePO 4的氧化还原反应的两相性质本质上防止了电荷分布一旦真正水流的松弛NT中断。对于该实验中，部分充电电极为阶梯扫描使用单色（6.02 keV）的X射线束和衍射图案被收集的每个步骤。扫描进行两垂直和平行于由部分充电硬币电池和方形电池取电极集电体。在这两种情况下，观察到电荷的分布不均，随着硬币电池用电极更高电荷比活性物质靠近集电体的表面上，并且最靠近该选项卡的最高电荷从棱柱形电池所采取的电极的部分。 这些结果说明了良好的空间的重要性，以及在针对电池工作有充分的了解同步辐射实验，时间分辨率。作为该领域的进步，正在开发面向成像的电极材料在三维新技术。其中一个例子就是满场的X射线microsco的结合使用PY（TXM）与XANES遵循的NiO电极的化学和形态的变化，因为他们的细胞放电19时进行转换，以镍和锂2 O。这些实验的一个特别挑战，但是，可以是在处理大量数据时产生。 新的高通量非弹性X射线散射配置，最近还用于获得更精细的细节电池材料的运作情况。例子包括一个组合的软X光吸收（铁L-边）和磷酸铁锂的电极硬X射线拉曼散射研究，完成易地 20。后者结合了硬X射线技术（ 例如，探测散现象的能力，并最终根据各种条件进行原位实验）与软X射线XAS相关的灵敏度的优点，而且可用于低z元素如碳和氧21。非共振非弹性X射线散射问题克（NIXS）也已用于测量的 Li 2的锂和氧的K-边O 2（锂/空气电池用有机电解液放电产物），从而导致更好的理解它的结构22。 NIXS的灵敏度借给它特别好地为其中低结晶材料在遇到（如在电池中发生放电）的情况。

锂离子电池的消费电子产品目前全世界命令$ 11十亿市场( <a href="http://www.marketresearch.com/David-Company-v3832/Lithium-Ion-Batteries-Outlook-Alternative-6842261/" target="_blank">http://www.marketresearch.com/David-Company-v3832/Lithium-Ion-Batteries-Outlook-Alternative-6842261/</a> )并且是首选新兴车辆应用例如插电式混合电动车（PHEV汽车）和电动汽车（EV）。类似物，这些设备利用钠离子，而不是锂都还处于早期发展阶段，但被认为是大规模储能（ 即电网应用）基于成本和供应安全参数1，2吸引力。两个双插系统的工作原理相同;碱金属离子作为主体结构，并且经过插入过程在不同电位的两个电极之间穿梭。电化学电池本身是RELatively简单，包括对集流器，通过与通常由溶解在有机溶剂中（ 图1）的混合物的盐的电解溶液饱和的多孔膜隔开的复合正极和负极的。石墨和钴酸锂是最常用的负电极和正电极，分别为锂离子电池。几种可供选择的电极材料也已被开发为特定的应用程序，包括的LiMn 2 O 4尖晶石，LiFePO 4的具有橄榄石结构的变体，和NMC（的LiNi x的Mn x坐标1 - 2个 O 2的化合物）为阳性，和硬碳，李4的Ti 5 O 12，和锂与锡的底片3合金。高压材料，如的LiNi 0.5锰1.5 O 4，新的高容量材料，如分层，分层复合材料（ 如 XLI 2的MnO &lt;子&gt; 3·（1-x）的锰酸锂镍0.5 0.5 O 2），过渡金属，可以进行氧化还原状态的多个变化，和Li-Si合金阳极是目前激烈的研究课题，并在成功部署，应化合物提高锂离子电池的实际能量密度进一步。另一个类的材料，被称为转换电极，其中过渡金属的氧化物，硫化物或氟化物被可逆地还原为金属元素和锂盐，也在考虑用作电池的电极（主要作为替代阳极）4。基于钠的设备，硬碳，合金，NASICON结构，以及钛酸盐正在被研究用作阳极和各种过渡金属氧化物和聚阴离子化合物作为阴极。 由于锂离子和钠离子电池并非基于固定化学品，其性能特点很大的不同取决于对T他认为电极雇用。电极的氧化还原行为决定的电位分布，速率能力，以及设备的循环寿命。常规的粉末X-射线衍射（XRD）技术可被用于原始材料和循环电极易地测量的初始结构表征，但实际的考虑因素，例如低信号强度和所需的收集数据的相对长的时间限制的信息的量可以在放电和充电过程中获得。相比之下，同步辐射的高亮度和短的波长（ 例如 λ= 0.97在斯坦福同步辐射一个LightSource的光束线11-3），结合运用高通量图像探测器，采集许可证的高分辨率数据，对样本少至10秒。 原位工作在传输模式中执行对电池组件进行充电和放电在密封包装袋透明的X射线，而无需停止运行采集数据。其结果是，电极的结构变化，可以观察到"时间快照"作为细胞周期，并且可以比使用常规技术来获得更多的信息。 X射线吸收光谱（XAS），有时也被称为X-射线吸收精细结构（XAFS）给出了关于材料的本地电子和几何结构的信息。在XAS实验中，光子的能量被调谐到所调查的特定元素的特征吸收边缘。最常用的电池材料，这些能量相当于感兴趣的过渡金属的K边缘（1S轨道），但软X光吸收实验，调整到O，F，C，B，N和第一行的第l 2,3边缘过渡金属有时也进行了易地样品5。通过XAS实验产生的光谱可以被分成若干个区INCT地区，包含不同的信息（见Newville，M.，基础XAFS的， <a href="http://xafs.org/Tutorials?action=AttachFile&amp;do=get&amp;target=Newville_xas_fundamentals.pdf" target="_blank">http://xafs.org/Tutorials?action=AttachFile&amp;do=get&amp;target=Newville_xas_fundamentals.pdf</a> ）。主要特征，包括吸收边缘，并延伸大约30-50电子伏特超越是在X射线吸收近边结构（XANES）区，并指出了电离的阈值，以连续态。这包含了吸收剂的氧化态和配位化学的信息。光谱的更高能量部分被称为扩展X-射线吸收精细结构（EXAFS）区域，并对应于所喷射的光电子关闭相邻原子的散射。这个区域的傅里叶分析给出短程结构信息，如键长和键的数量和类型邻近离子。 Preedge采用了characterist以下一些化合物的IC吸收的能量也有时会出现。这些从偶极禁电子跃迁产生的空束缚态的八面体几何形状，或在四面体那些偶极允许的轨道杂化效应，往往可以关联到吸收离子（ 例如是否是四面体或八面体配位）的局部对称性6。 XAS是研究混合金属等系统的NMC确定初始氧化还原状态以及过渡金属离子在脱锂及锂化过程进行氧化还原一个特别有用的技术。在几个不同的金属的数据可以在一次实验中迅速地获得和解释是相当简单的。与此相反，穆斯堡尔谱是有限的，以在电池材料（主要是Fe和Sn）的使用仅几个金属。而磁测量也可以用于确定氧化态，磁性耦合效应可以并发症德解释特别是对于复合氧化物如NMC的。 精心策划和执行的就地和迁地保护同步加速器X射线衍射和X光吸收实验给予补充信息，并允许在比什么可以通过常规技术获得正常的电池操作发生在电极材料的结构变化更完整的画面形成。这反过来，给出了什么支配着设备的电化学行为更深入的了解。

<table><tbody><tr><td colspan="4">&lt;strong&gt;Equipment&lt;/strong&gt;</td></tr><tr><td>Inert atmosphere glovebox</td><td>Vacuum Atmospheres</td><td>Custom order, contact vendors</td><td>Used during cell assembly and to store alkali metals and moisture sensitive components. (&lt;a href=&quot;http://vac-atm.com&quot; target=&quot;_blank&quot;&gt;http://vac-atm.com&lt;/a&gt;)</td></tr><tr><td>Inert atmosphere glovebox</td><td>Mbraun</td><td></td><td>Various sizes (single, double) available, many options such as mini or heated antechambers oxygen/water removal systems, shelving, electrical feedthroughs, &lt;em&gt;etc&lt;/em&gt;. (&lt;a href=&quot;http://www.mbraunusa.com&quot; target=&quot;_blank&quot;&gt;http://www.mbraunusa.com&lt;/a&gt;)</td></tr><tr><td>X-ray powder diffractometer (XRD)</td><td>Panalytical</td><td>X&#039;Pert Powder</td><td>X&#039;Pert is a modular system. Many accessories available for specialized experiments. (&lt;a href=&quot;http://www.mbraunusa.com&quot; target=&quot;_blank&quot;&gt;www.panalytical.com&lt;/a&gt;)</td></tr><tr><td>X-ray powder diffractometer (XRD)</td><td>Bruker</td><td>Bruker D2 Phaser</td><td>Bruker D2 Phaser is compact and good for routine powder analyses. (&lt;a href=&quot;www.bruker.com&quot; target=&quot;_blank&quot;&gt;www.bruker.com&lt;/a&gt;)</td></tr><tr><td>Scanning Electron Microscope (SEM)</td><td></td><td>JSM7500F</td><td>High resolution field emission scanning electron microscope with numerous customizable options. JEOL (&lt;a href=&quot;http://www.jeolusa.com&quot; target=&quot;_blank&quot;&gt;http://www.jeolusa.com&lt;/a&gt;) Low cost tabletop versions also available. Contact vendor for options.</td></tr><tr><td>Pouch Sealer</td><td>VWR</td><td>11214-107</td><td>Used to seal pouches for &lt;em&gt;in situ &lt;/em&gt;work. (&lt;a href=&quot;https://us.vwr.com/&quot; target=&quot;_blank&quot;&gt;https://us.vwr.com&lt;/a&gt;)</td></tr><tr><td>Manual crimping tool</td><td>Pred Materials</td><td>HSHCC-2016, 2025, 2032, 2320</td><td>Used to seal coin cells. Match size to coin cell hardware. (&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Coin cell disassembling tool</td><td>Pred Materials</td><td>Contact vendor</td><td>Used to take apart coin cells to recover electrodes for &lt;em&gt;ex situ&lt;/em&gt; work. Needlenose pliers can also be used. Cover ends with Teflon tape to avoid shorting cells. (&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Film casting knives</td><td>BYK Gardner</td><td>4301, 4302, 4303, 4304,4305,2325, 2326,2327,2328, 2329</td><td>Used to cast electrodes films from slurries. Different sizes available, with either metric or English gradations. Bar film or Baker-type applicators and doctor blades are less versatile but lower cost options. Can be used by hand or with automatic film applicators. (&lt;a href=&quot;https://www.byk.com/&quot; target=&quot;_blank&quot;&gt;https://www.byk.com&lt;/a&gt;)</td></tr><tr><td>Doctor blades, Baker applicators</td><td>Pred Materials</td><td>Baker type applicator and doctor blade. Film casting knives also available.</td><td>Used to cast electrodes films from slurries. Different sizes available, with either metric or English gradations. Bar film or Baker-type applicators and doctor blades are less versatile but lower cost options. Can be used by hand or with automatic film applicators. (&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Automatic film applicator</td><td>BYK Gardner</td><td>2101, 2105, 2121, 2122</td><td>Optional. Used with bar applicators, doctor blades, or film casting knives for automatic electrode film production. Films can also be made by hand but are less uniform. (&lt;a href=&quot;https://www.byk.com/&quot; target=&quot;_blank&quot;&gt;https://www.byk.com&lt;/a&gt;)</td></tr><tr><td>Automatic film applicator</td><td>Pred Materials</td><td>Contact vendor</td><td>Optional. Used with bar applicators, doctor blades, or film casting knives for automatic electrode film production. Films can also be made by hand but are less uniform. (&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Potentiostat/Galvanostat</td><td>Bio-Logic Science Instruments</td><td>VSP</td><td>Portable 5 channel computer-controlled potentiostat/galvanostat used to cycle cells for &lt;em&gt;in situ&lt;/em&gt; experiments. (&lt;a href=&quot;http://www.bio-logic.info/&quot; target=&quot;_blank&quot;&gt;http://www.bio-logic.info&lt;/a&gt;)</td></tr><tr><td>Potentiostat/Galvanostat</td><td>Gamry Instruments</td><td>Reference 3000</td><td>Portable single channel computer-controlled potentiostat/galvanostat used to cycle cells for &lt;em&gt;in situ&lt;/em&gt; experiments. (&lt;a href=&quot;www.gamry.com&quot; target=&quot;_blank&quot;&gt;www.gamry.com&lt;/a&gt;)</td></tr><tr><td>The Area Diffraction Machine</td><td></td><td>Free download</td><td>Used for analysis of 2D diffraction data. Mac and Windows versions available. &lt;a href=&quot;http://code.google.com/p/areadiffractionmachine/&quot; target=&quot;_blank&quot;&gt;http://code.google.com/p/areadiffractionmachine/&lt;/a&gt;</td></tr><tr><td>IFEFFIT</td><td></td><td>Free download</td><td>Suite of interactive programs for XAS analysis, including Hephaestus, Athena, and Artemis. Available for Mac, Windows, and UNIX. &lt;a href=&quot;http://cars9.uchicago.edu/ifeffit/&quot; target=&quot;_blank&quot;&gt;http://cars9.uchicago.edu/ifeffit/&lt;/a&gt;</td></tr><tr><td>SIXPACK</td><td></td><td>Free download</td><td>XAS analysis program that builds on IFEFFIT. Windows and Mac versions. &lt;a href=&quot;http://home.comcast.net/~sam_webb/sixpack.html&quot; target=&quot;_blank&quot;&gt;http://home.comcast.net/~sam_webb/sixpack.html&lt;/a&gt;</td></tr><tr><td>CelRef</td><td></td><td>Free download</td><td>Graphical unit cell refinement. Windows only. &lt;a href=&quot;http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm&quot; target=&quot;_blank&quot;&gt;http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm and http://www.ccp14.ac.uk/ccp/web-mirrors/lmgp-laugier-bochu/&lt;/a&gt;</td></tr><tr><td colspan="4">&lt;strong&gt;Reagent/Material&lt;/strong&gt;</td></tr><tr><td>Electrode active materials</td><td>various</td><td></td><td>Synthesized in-house or obtained from various suppliers.</td></tr><tr><td>Synthetic flake graphite</td><td>Timcal</td><td>SFG-6</td><td>Conductive additive for electrodes. (&lt;a href=&quot;http://www.timcal.com&quot; target=&quot;_blank&quot;&gt;www.timcal.com&lt;/a&gt;)</td></tr><tr><td>Acetylene black</td><td>Denka</td><td>Denka Black</td><td>Conductive additive for electrodes. (&lt;a href=&quot;http://www.denka.co.jp/eng/index.html&quot; target=&quot;_blank&quot;&gt;http://www.denka.co.jp/eng/index.html&lt;/a&gt;)</td></tr><tr><td>1-methyl-2-pyrrolidinone (NMP)</td><td>Sigma-Aldrich</td><td>328634</td><td>Used to make electrode slurries. (&lt;a href=&quot;http://www.sigmaaldrich.com&quot; target=&quot;_blank&quot;&gt;www.sigmaaldrich.com&lt;/a&gt;)</td></tr><tr><td>Al current collectors</td><td>Exopack</td><td>z-flo 2650</td><td>Carbon-coated foils. Coated on one side. (&lt;a href=&quot;http://www.exopackadvancedcoatings.com&quot; target=&quot;_blank&quot;&gt;http://www.exopackadvancedcoatings.com&lt;/a&gt;)</td></tr><tr><td>Al current collectors</td><td>Alfa-Aesar</td><td>10558</td><td>0.025 mm (0.001 in) thick, 30 cm x 30 cm (12 in x 12 in), 99.45% (metals basis), uncoated (&lt;a href=&quot;http://www.alfa.com&quot; target=&quot;_blank&quot;&gt;http://www.alfa.com&lt;/a&gt;)</td></tr><tr><td>Cu current collectors</td><td>Pred Materials</td><td>Electrodeposited Cu foil</td><td>For use with anode materials for Li-ion batteries. (&lt;a href=&quot;http://www.predmaterials.com&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Lithium foil</td><td>Rockwood Lithium</td><td>Contact vendor</td><td>Anode for half cells. Available in different thicknesses and widths. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He or Ar (reacts with N&lt;sub&gt;2&lt;/sub&gt;). (&lt;a href=&quot;http://www.rockwoodlithium.com&quot; target=&quot;_blank&quot;&gt;www.rockwoodlithium.com&lt;/a&gt;)</td></tr><tr><td>Lithium foil</td><td>Sigma-Aldrich</td><td>320080</td><td>Anode for half cells. Available in different thicknesses and widths. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He or Ar (reacts with N&lt;sub&gt;2&lt;/sub&gt;). (&lt;a href=&quot;http://www.sigmaaldrich.com&quot; target=&quot;_blank&quot;&gt;www.sigmaaldrich.com&lt;/a&gt;)</td></tr><tr><td>Sodium ingot</td><td>Sigma-Aldrich</td><td>282065</td><td>Anodes for half cells. Can be extruded into foils. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He only. (&lt;a href=&quot;http://www.sigmaaldrich.com&quot; target=&quot;_blank&quot;&gt;www.sigmaaldrich.com&lt;/a&gt;)</td></tr><tr><td>Electrolyte solutions</td><td>BASF</td><td>Selectilyte P-Series contact vendor</td><td>Contact vendor for desired formulations. (&lt;a href=&quot;http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes&quot; target=&quot;_blank&quot;&gt;http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes&lt;/a&gt;)</td></tr><tr><td>Dimethyl carbonate (DMC)</td><td>Sigma-Aldrich</td><td>517127</td><td>Used to wash electrodes for &lt;em&gt;ex situ&lt;/em&gt; experiments. (&lt;a href=&quot;http://www.sigmaaldrich.com&quot; target=&quot;_blank&quot;&gt;www.sigmaaldrich.com&lt;/a&gt;)</td></tr><tr><td>Microporous separators</td><td>Celgard</td><td>2400</td><td>Polypropylene membranes (&lt;a href=&quot;http://www.celgard.com/&quot; target=&quot;_blank&quot;&gt;http://www.celgard.com&lt;/a&gt;)</td></tr><tr><td>Coin cell hardware (case, cap, gasket)</td><td>Pred Materials</td><td>CR2016, CR2025, CR2320, CR2032</td><td>Match size to available crimping tool, Al-clad components also available. (&lt;a href=&quot;http://www.predmaterials.com&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Wave washers</td><td>Pred Materials</td><td>SUS316L</td><td>(&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Spacers</td><td>Pred Materials</td><td>SUS316L</td><td>(&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Ni and Al pretaped tabs</td><td>Pred Materials</td><td>Contact vendor</td><td>Sizes subject to change. Inquire about custom orders. (&lt;a href=&quot;http://www.predmaterials.com/&quot; target=&quot;_blank&quot;&gt;www.predmaterials.com&lt;/a&gt;)</td></tr><tr><td>Polyester pouches</td><td>VWR</td><td>11214-301</td><td>Used to seal electrochemical cells for &lt;em&gt;in situ &lt;/em&gt;work. Avoid heavy duty pouches because of strong signal interference. (&lt;a href=&quot;https://us.vwr.com&quot; target=&quot;_blank&quot;&gt;https://us.vwr.com&lt;/a&gt;)</td></tr><tr><td>Kapton film</td><td>McMaster-Carr</td><td>7648A735</td><td>Used to cover electrodes for &lt;em&gt;ex situ&lt;/em&gt; experiments, 0.0025 in thick (&lt;a href=&quot;http://www.mcmaster.com/&quot; target=&quot;_blank&quot;&gt;www.mcmaster.com&lt;/a&gt;)</td></tr><tr><td>Helium, Argon and 4-10% hydrogen in helium or argon</td><td>Air Products</td><td>contact vendor for desired compositions and purity levels</td><td>Helium or argon used to fill glovebox where cell assembly is carried out and alkali metal is stored. (&lt;a href=&quot;http://www.airproducts.com/products/gases.aspx&quot; target=&quot;_blank&quot;&gt;http://www.airproducts.com/products/gases.aspx&lt;/a&gt;)</td></tr><tr><td colspan="4">Do not use nitrogen because it reacts with lithium. Use only helium if sodium is being stored.&lt;br/&gt; Purity level needed depends on whether the glovebox is equipped with a water and oxygen removal system. Hydrogen mixtures needed to regenerate water/oxygen removal system, if present&amp;nbsp;or any other suitable gas supplier</td></tr></tbody></table>

characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques

层间化合物等过渡金属氧化物或磷酸盐是在锂离子和钠离子电池中最常用的电极材料。在插入或除去碱金属离子，该化合物中的过渡金属的氧化还原状态的变化和结构转变诸如相变和/或晶格参数的增加或减少发生。这些行为反过来确定电池势如型材，速率能力和循环寿命的重要特征。极亮和可调X射线同步辐射产生的允许快速采集，提供有关这些进程的相关信息的高分辨率数据。在散装的材料，如相变转化，可以使用X-射线衍射（XRD）进行直接观察，而X-射线吸收光谱（XAS）给出了关于本地电子和几何结构（ 例如，改变的氧化还原状态和键信息升engths）， 在执行上操作的细胞原位实验，因为它们允许的材料的电化学性质和结构性质之间的直接相关性是特别有用的。这些实验是耗时的，并且可以是具有挑战性的设计，由于在半电池构造中使用的碱金属的阳极的反应性和空气的灵敏度，和/或从其他细胞成分和硬件信号干扰的可能性。由于这些原因，很适合开展易地实验（ 如从部分充电或循环细胞收获电极）在某些情况下。在这里，我们提出了详细的方案编制双方易地和就地样品中涉及同步辐射实验和演示如何将这些实验完成。

图2示出在现场试验用于一个典型的序列。合成和活性材料粉末的特性后，复合电极是由含有活性材料，粘合剂如聚偏氟乙烯（PVDF）和导电性添加剂，例如碳黑或石墨悬浮于N-甲基吡咯烷酮（NMP），投射到任何浆液制备铝或铜箔集电体。铝是用于锂离子电池的阴极和所有的钠离子电池的电极，并且铜用于锂离子电池的阳极。后电极被干燥，切割，并称重，将细胞用微多孔分离器，适当的电解质溶液，并包括任一Li或Na。箔负电极组装在惰性气氛手套箱中。这些部件然后被密封在一个保护袋，由聚酯制成，它保持了空气，并且是合理的透视透明的。铝和镍片被用来制造电触头对的正和负电极。在Al片被超声波焊接到阴极集电体，而用作阳极的软Li或Na。金属被简单地围绕镍片压制，从而使接触。以维持压力，袋细胞被压缩两块金属板带切割成他们允许的X射线的变速器2毫米的孔之间。电池组件之间接触不良可能导致高过电位和过早切断，尤其是当电压限制，不进行调整，以适应在这种配置中遇到的额外的过电位。过大的压力，另一方面，可以使实验的细胞短路和故障。当组件被首先组装成具有钻入外壳和隔板，然后将其密封在保护袋插片接连后小孔纽扣电池更好的压力控制的实现。波形垫圈及垫片用于填充任何分机在设备RA量，有保有压，保证了组件之间的良好接触。 一个小的便携式恒电位仪/恒电流仪和便携式计算机，然后用来进行电化学试验，并在束线中收集数据。一个充放电周期通常需要大约20小时才能完成。通常是预先选择的电压范围之间进行的恒电流循环（ 即采用恒流）。样品既可以保持静止，摇动（左/右或上/下）或围绕光束轴的光束线旋转。优势，最后两个是结果在电极的一个稍大的面积得到的，在含有粉末的电极择优取向的影响最小化，并计数统计得到改善。 透射X射线衍射环图案（参见图2，步骤5）可以在大约10秒而获得，用约1-2分钟的数据读出时间。 Ø集成f图像校准模式产生行扫描（强度与Q）。束线11-3在斯坦福同步辐射一个LightSource使用单一的Si（311）单色器，产生约0.97（12,735伏特）的入射光波长，虽然几EVS（〜0.01％），主要由于量级的能量波动要昼夜循环（每日温度波动），常常观察到在漫长的充电和放电测量的过程。因此，图像校准为每个扫描是必不可少的去卷积衍射图样的变化。校准是在与11-3束线（共同开发的区域的衍射机软件进行<a href="http://code.google.com/p/areadiffractionmachine/" target="_blank">http://code.google.com/p/areadiffractionmachine/</a> ）。 图3显示了在获得一个对Li / Li 原位 X射线衍射数据X [0.45镍锰钴0.45 0.05铝0.05] O 2 </子&gt;细胞的进行充电（黑色）和放电（绿色），校准环模式，以行扫描和转换后。从电池组件包括铝集电体，聚酯袋，和聚丙烯隔板而产生的峰均标有红色和蓝色点（锂金属基本上是透明的X射线，但如果钠金属阳极是用来将产生额外的峰）。归属于立索引的反射X [0.45镍锰钴0.45 0.05铝0.05] O 2的活性物质都标上的图案。因为晶胞参数改变为x的函数（Li含量），因此相和铝集电体的峰重叠在一定的图案。从电池组件的干扰提出了两个完美的背景减法和整个衍射图案的Rietveld精修显著的挑战。为了解决这个问题，背景是手动减去，并且LIMI泰德组峰未与细胞成分重叠的被选定为嵌合。晶胞参数在各种状态-的电荷使用可用的峰值位置和程序CelRef（随后计算由最小二乘法修正<a href="http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm" target="_blank">http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm</a> ）。到电池组件在从原位实验中获得的模式干扰的程度取决于材料的所研究的性质而变化，并且不总是遇到这些问题。在这种情况下，任何方便的细化或拟合程序可以被用来分析数据（GSAS，PowderCell，RIQAS，FullProf 等 ）。 由于时间限制，有时最好进行同步X射线衍射实验易地，这显然是不实际了很长一段时间的束线进行多个周期，例如。相反，电极可以是R从循环细胞，用溶剂冲洗，以去除残留的电解质盐，干emoved，并盖上卡普顿膜从空气中提供保护，以供以后检查。此外，它可以是有用的研究几电极在不同状态-的电荷从电化学电池收获，给予从更多地参与稍后进行现场试验，以期望的想法。这些实验是要简单得多，进行和少得多的时间耗费;几个样本通常可以在一小时内运行。一个额外的好处，以易地工作是缺乏大多数干扰小区的组件，虽然从集电体，粘结剂和导电性添加剂的信号通常仍观察和卡普顿本身有助于背景。注意事项易地工作是清洗和长或贮存不当可能会改变或降低的样品。在最坏情况下，获得易地数据甚至可能不提供相关信息由于这些问题。如果适当的谨慎保持，但是， 异地工作仍然有一些价值，虽然直接观察采用原位配置过程显然是最可取的办法只要时间条件允许的。 因为XAS实验是元件特异性的，由比所感兴趣的电极材料的其他细胞组分的干扰是不作为问题的，因为用X射线衍射（假定小区硬件不包含所关注的金属）。只有一个吸收边（元件）可以在同一时间但被测量。当切换到新能源只需几秒钟，调整，改变增益和偏移的电离室，改变参考箔，并与气体吹扫可能需要额外的十分钟。 原位运行期间从一个元素切换到另一个可能导致数据有所下降。有意义的EXAFS数据可以是困难的过程中就地工作取得，因为该结构这往往发生乌拉尔变化也有类似的时间常数的测量本身的。另一个考虑是，XAS束线往往大量认购，这意味着有限的时间内为每个用户。由于这些原因，所以一般更实际，进行X光吸收实验，对易地样品，而不是在原地进行的工作（虽然见参考文献7 就地工作的一个例子）。获取有关易地样本数据可以在任何地方从几分钟到一个小时取决于有多少元素正在研究中，并在其中工作的开展设施。在每个边缘的测量，类似的金属箔（ 例如，镍，锰，或钴）的频谱应记录为能量参考。这是同步进行的样品测定。此外，用户可能希望将记录在含有目的与已知的氧化态，单独的金属参考资料数据特别是如果不寻常的氧化还原态所涉及的电化学。例如，Li 3的MnO 4被用来作为一个最近的一系列的锂锰氧氮化物电极材料研究的参照来验证四面体配位的Mn 5 +的存在。8 针对在电极材料研究本体方法最XAS实验是在传输模式，这是合适的，当摩尔浓度的感兴趣的元素的是高于约5％-10％（运行<a href="http://xafstraining.ps.bnl.gov" target="_blank">http://xafstraining.ps.bnl.gov</a> ）。最好的结果是当样品中，x的厚度，被调整得使μX&lt;3以上的吸收边缘。如果吸收系数（μ）是未知的（ 例如，对于复杂的材料，其中包括许多电池的电极材料），也可以是有用的，开始用撒在一块透明胶带的粘性侧极少量的粉末。一或多个附加件的粉状透明胶带可以附加到原来增加信号到那里，获得最佳的反应（典型地，对应于一个吸收长度）的点。对于其中的吸收系数是已知的材料，样品可以与BN进行稀释，以使正确的吸收是在给定的厚度获得的。 在SSRL，镍，锰和钴的K-边缘，可以研究在束线4.1，而钛和S的边缘处的光束线4.3影响。约30％的失谐的双晶单色消除高次谐波。校准是通过使用在参考金属的吸收光谱的导数的第一个峰。重复扫描可运行并对准后合并来提高数据的质量。阿蒂米斯/雅典娜从软件包IFEFFIT用于分析9。样的扫描合并后，背景的贡献中减去与该数据被归一化。 EXAFS哒ta的使用AUTOBK功能分离，并且被付立叶变换。嵌合到在R或K空间的傅里叶变换光谱最小二乘然后用于提取结构信息。的XAS数据，在使MnĶ边取的例子，显示在图2中 ，步骤5和XANES和EXAFS区域标记的频谱上。 <img alt="图1" src="/files/ftp_upload/50594/50594fig1.jpg" /> 图1。原理锂离子电池用石墨阳极和层状金属氧化物阴极正在接受放。使用与参考3 许可 。 <img alt="图2" src="/files/ftp_upload/50594/50594fig2.jpg" /> 图2。小袋的原位试验典型序列。步骤包括:1）制备与样品的表征，2）制备复合电极，3）装配细胞，4）设置的原位实验中的束线，以及5）数据采集和分析。 <img alt="图3" src="/files/ftp_upload/50594/50594fig3.jpg" /> 图3。通过在对Li / Li集成图像扫描获得的线扫描X [0.45镍锰钴0.45 0.05铝0.05] O 2细胞进行充电（黑色）和放电（绿色）。思考归因于铝集电器和聚合物电池组件（袋和微孔隔板）标有蓝色和红色的点，分别。 表1，表材料。 表2。表设备。

Watch this Scientific Journal Video about Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques at JoVE.com

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

我们描述了使用同步辐射X射线吸收光谱（XAS）和X-射线衍射（XRD）技术，以探测在锂离子和钠离子电池的电极材料的嵌入/脱嵌过程的细节。无论是在就地和移地实验来了解有关设备的运行结构行为

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. ...

characterization-electrode-materials-for-lithium-ion-sodium-ion

Nanyang Technological University

Research

JoVE Journal

Engineering

25.3K 次观看.  Lawrence Berkeley National Laboratory. 我们描述了使用同步辐射X射线吸收光谱（XAS）和X-射线衍射（XRD）技术，以探测在锂离子和钠离子电池的电极材料的嵌入/脱嵌过程的细节。无论是在就地和移地实验来了解有关设备的运行结构行为

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

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

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

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

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

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

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 ...

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 ...

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 ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

电化学测试的协议及表征非质子锂的O<sub&gt; 2</sub&gt;电池

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

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

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

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

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 ...

Nanoscale Characterization of Liquid-Solid Interfaces by Coupling Cryo-Focused Ion Beam Milling with Scanning Electron Microscopy and Spectroscopy

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar energy and fuel generation, and electrochemical energy storage. Nanoscale characterization of such interfaces has recently been achieved using cryogenic electron microscopy, thereby providing a new path to advancing our fundamental understanding of interface processes.
This contribution provides a practical guide to mapping the structure and chemistry of solid-liquid interfaces in materials and devices using an integrated cryogenic electron microscopy approach. In this approach, we pair cryogenic sample preparation which allows stabilization of solid-liquid interfaces with cryogenic focused ion beam (cryo-FIB) milling to create cross-sections through these complex buried structures. Cryogenic scanning electron microscopy (cryo-SEM) techniques performed in a dual-beam FIB/SEM enable direct imaging as well as chemical mapping at the nanoscale. We discuss practical challenges, strategies to overcome them, as well as protocols for obtaining optimal results. While we focus in our discussion on interfaces in energy storage devices, the methods outlined are broadly applicable to a range of fields where solid-liquid interface play a key role.

Cryogenic Focused Ion Beam (FIB) and Scanning Electron Microscopy (SEM) techniques can provide key insights into the chemistry and morphology of intact solid-liquid interfaces. Methods for preparing high quality Energy Dispersive X-ray (EDX) spectroscopic maps of such interfaces are detailed, with a focus on energy storage devices.

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

Physical and chemical processes at solid-liquid interfaces play a crucial role in many natural and technological phenomena, including catalysis, solar ...

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

With the ever-increasing use of Li-ion batteries, especially due to their adoption in electric vehicles, their safety is in prime focus. Thus, the all-solid-state batteries (ASSBs) that use solid electrolytes instead of liquid electrolytes, which reduce the risk of flammability, have been the center stage of battery research for the last few years. However, in the ASSB, the ion transportation through the solid-solid electrolyte-electrode interface poses a challenge due to contact and chemical/electrochemical stability issues. Applying a suitable coating around the electrode and/or electrolyte particles offers a convenient solution, leading to better performance. For this, researchers are screening potential electronic/ionic conductive and nonconductive coatings to find the best coatings with suitable thickness for long-term chemical, electrochemical, and mechanical stability. Operando transmission electron microscopy (TEM) couples high spatial resolution with high temporal resolution to allow visualization of dynamic processes, and thus is an ideal tool to evaluate electrode/electrolyte coatings via studying (de)lithiation at a single particle level in real-time. However, the accumulated electron dose during a typical high-resolution in situ work may affect the electrochemical pathways, evaluation of which can be time-consuming. The current protocol presents an alternative procedure in which the potential coatings are applied on Si nanoparticles and are subjected to (de)lithiation during operando TEM experiments. The high volume changes of Si nanoparticles during (de)lithiation allow monitoring of the coating behavior at a relatively low magnification. Thus, the whole process is very electron-dose efficient and offers quick screening of potential coatings.

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

Utilizing the volume change of Si nanoparticles during (de)lithiation, the present protocol describes a screening method of potential coatings for all-solid-state batteries using in situ transmission electron microscopy.

正极材料的同步辐射技术锂离子和钠离子电池表征

摘要

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此视频中的章节

钮扣电池锂离子电池的建设和测试

原位中子衍射用特制的锂离子电池

电池的使用同步为基础的硬X射线微断层故障分析

利用同步辐射微断层调查的多尺度三维微电子封装

电化学测试的协议及表征非质子锂的O

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

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

锂离子电池材料用石墨烯液位的制备

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

使用原位透射电子显微镜筛选全固态电池涂层

正极材料的同步辐射技术锂离子和钠离子电池表征

摘要

探索更多视频

此视频中的章节

钮扣电池锂离子电池的建设和测试

原位中子衍射用特制的锂离子电池

电池的使用同步为基础的硬X射线微断层故障分析

利用同步辐射微断层调查的多尺度三维微电子封装

电化学测试的协议及表征非质子锂的O

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

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

锂离子电池材料用石墨烯液位的制备

通过冷冻聚焦离子束铣削与扫描电子显微镜和光谱学耦合，对液固界面进行纳米级表征

使用 原位 透射电子显微镜筛选全固态电池涂层

使用原位透射电子显微镜筛选全固态电池涂层