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<sup...

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 border="1">
	<tbody>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Equipment</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. (<a href="http://vac-atm.com" target="_blank">http://vac-atm.com</a>)</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, etc. (<a href="http://www.mbraunusa.com" target="_blank">http://www.mbraunusa.com</a>)</td>
		</tr>
		<tr>
			<td>X-ray powder diffractometer (XRD)</td>
			<td>Panalytical</td>
			<td>X&#39;Pert Powder</td>
			<td>X&#39;Pert is a modular system. Many accessories available for specialized experiments. (<a href="http://www.mbraunusa.com" target="_blank">www.panalytical.com</a>)</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. (<a href="www.bruker.com" target="_blank">www.bruker.com</a>)</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 (<a href="http://www.jeolusa.com" target="_blank">http://www.jeolusa.com</a>) 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 in situ work. (<a href="https://us.vwr.com/" target="_blank">https://us.vwr.com</a>)</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. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</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 ex situ work. Needlenose pliers can also be used. Cover ends with Teflon tape to avoid shorting cells. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</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. (<a href="https://www.byk.com/" target="_blank">https://www.byk.com</a>)</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. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</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. (<a href="https://www.byk.com/" target="_blank">https://www.byk.com</a>)</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. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</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 in situ experiments. (<a href="http://www.bio-logic.info/" target="_blank">http://www.bio-logic.info</a>)</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 in situ experiments. (<a href="www.gamry.com" target="_blank">www.gamry.com</a>)</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. <a href="http://code.google.com/p/areadiffractionmachine/" target="_blank">http://code.google.com/p/areadiffractionmachine/</a></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. <a href="http://cars9.uchicago.edu/ifeffit/" target="_blank">http://cars9.uchicago.edu/ifeffit/</a></td>
		</tr>
		<tr>
			<td>SIXPACK</td>
			<td></td>
			<td>Free download</td>
			<td>XAS analysis program that builds on IFEFFIT. Windows and Mac versions. <a href="http://home.comcast.net/~sam_webb/sixpack.html" target="_blank">http://home.comcast.net/~sam_webb/sixpack.html</a></td>
		</tr>
		<tr>
			<td>CelRef</td>
			<td></td>
			<td>Free download</td>
			<td>Graphical unit cell refinement. Windows only. <a href="http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm" target="_blank">http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm and http://www.ccp14.ac.uk/ccp/web-mirrors/lmgp-laugier-bochu/</a></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Reagent/Material</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. (<a href="http:/www.timcal.com" target="_blank">www.timcal.com</a>)</td>
		</tr>
		<tr>
			<td>Acetylene black</td>
			<td>Denka</td>
			<td>Denka Black</td>
			<td>Conductive additive for electrodes. (<a href="http://www.denka.co.jp/eng/index.html" target="_blank">http://www.denka.co.jp/eng/index.html</a>)</td>
		</tr>
		<tr>
			<td>1-methyl-2-pyrrolidinone (NMP)</td>
			<td>Sigma-Aldrich</td>
			<td>328634</td>
			<td>Used to make electrode slurries. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Al current collectors</td>
			<td>Exopack</td>
			<td>z-flo 2650</td>
			<td>Carbon-coated foils. Coated on one side. (<a href="http://www.exopackadvancedcoatings.com" target="_blank">http://www.exopackadvancedcoatings.com</a>)</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 (<a href="http://www.alfa.com" target="_blank">http://www.alfa.com</a>)</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. (<a href="http://www.predmaterials.com" target="_blank">www.predmaterials.com</a>)</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 N2). (<a href="http://www.rockwoodlithium.com" target="_blank">www.rockwoodlithium.com</a>)</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 N2). (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</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. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Electrolyte solutions</td>
			<td>BASF</td>
			<td>Selectilyte P-Series contact vendor</td>
			<td>Contact vendor for desired formulations. (<a href="http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes" target="_blank">http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes</a>)</td>
		</tr>
		<tr>
			<td>Dimethyl carbonate (DMC)</td>
			<td>Sigma-Aldrich</td>
			<td>517127</td>
			<td>Used to wash electrodes for ex situ experiments. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Microporous separators</td>
			<td>Celgard</td>
			<td>2400</td>
			<td>Polypropylene membranes (<a href="http://www.celgard.com/" target="_blank">http://www.celgard.com</a>)</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. (<a href="http://www.predmaterials.com" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Wave washers</td>
			<td>Pred Materials</td>
			<td>SUS316L</td>
			<td>(<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Spacers</td>
			<td>Pred Materials</td>
			<td>SUS316L</td>
			<td>(<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</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. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Polyester pouches</td>
			<td>VWR</td>
			<td>11214-301</td>
			<td>Used to seal electrochemical cells for in situ work. Avoid heavy duty pouches because of strong signal interference. (<a href="https://us.vwr.com" target="_blank">https://us.vwr.com</a>)</td>
		</tr>
		<tr>
			<td>Kapton film</td>
			<td>McMaster-Carr</td>
			<td>7648A735</td>
			<td>Used to cover electrodes for ex situ experiments, 0.0025 in thick (<a href="http://www.mcmaster.com/" target="_blank">www.mcmaster.com</a>)</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. (<a href="http://www.airproducts.com/products/gases.aspx" target="_blank">http://www.airproducts.com/products/gases.aspx</a>)</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Do not use nitrogen because it reacts with lithium. Use only helium if sodium is being stored. 
			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&#160;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...

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

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

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 &deg;C), flammable, and volatile organic electrolytes. These organic based electrolyte systems are viable at ambient temperatures, but require a cooling system to ensure that temperatures do not exceed 80 &deg;C. These cooling systems tend to increase battery costs and can malfunction which can lead to battery malfunction and explosions, thus endangering human life. Increases in petroleum prices lead to a huge demand for safe, electric hybrid vehicles that are more economically viable to operate as oil prices continue to rise. Existing organic based electrolytes used in lithium ion batteries are not applicable to high temperature automotive applications. A safer alternative to organic electrolytes is solid polymer electrolytes. This work will highlight the synthesis for a graft copolymer electrolyte (GCE) poly(oxyethylene) methacrylate (POEM) to a block with a lower glass transition temperature (Tg) poly(oxyethylene) acrylate (POEA). The conduction mechanism has been discussed and it has been demonstrated the relationship between polymer segmental motion and ionic conductivity indeed has a Vogel-Tammann-Fulcher (VTF) dependence. Batteries containing commercially available LP30 organic (LiPF6 in ethylene carbonate (EC):dimethyl carbonate (DMC) at a 1:1 ratio) and GCE were cycled at ambient temperature. It was found that at ambient temperature, the batteries containing GCE showed a greater overpotential when compared to LP30 electrolyte. However at temperatures greater than 60 &deg;C, the GCE cell exhibited much lower overpotential due to fast polymer electrolyte conductivity and nearly the full theoretical specific capacity of 170 mAh/g was accessed.

Lithium ion batteries employ flammable and volatile organic electrolytes that are suitable for ambient temperature applications. A safer alternative to organic electrolytes are solid polymer batteries. Solid polymer batteries operate safely at high temperatures (&gt;120 &deg;C), thus making them applicable to high temperature applications such as deep oil drilling and hybrid electric vehicles. This paper will discuss (a) the polymer synthesis, (b) the polymer conduction mechanism, and (c) provide temperature cycling for both solid polymer and organic electrolytes.

接枝共聚物固态电解质的锂离子电池的应用

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. From the measured surface, 3D topographic maps can be subsequently analyzed using a variety of software packages to extract the information that is needed.
In this article we describe how white light interferometry, and optical profilometry (OP) in general, combined with generic surface analysis software, can be used for materials science and engineering tasks. In this article, a number of applications of white light interferometry for investigation of surface modifications in mass spectrometry, and wear phenomena in tribology and lubrication are demonstrated. We characterize the products of the interaction of semiconductors and metals with energetic ions (sputtering), and laser irradiation (ablation), as well as ex situ measurements of wear of tribological test specimens.
Specifically, we will discuss:
<ol class="lroman">
	<li>Aspects of traditional ion sputtering-based mass spectrometry such as sputtering rates/yields measurements on Si and Cu and subsequent time-to-depth conversion.</li>
	<li>Results of quantitative characterization of the interaction of femtosecond laser irradiation with a semiconductor surface. These results are important for applications such as ablation mass spectrometry, where the quantities of evaporated material can be studied and controlled via pulse duration and energy per pulse. Thus, by determining the crater geometry one can define depth and lateral resolution versus experimental setup conditions.</li>
	<li>Measurements of surface roughness parameters in two dimensions, and quantitative measurements of the surface wear that occur as a result of friction and wear tests.</li>
</ol>
Some inherent drawbacks, possible artifacts, and uncertainty assessments of the white light interferometry approach will be discussed and explained.

White light microscope interferometry is an optical, noncontact and quick method for measuring the topography of surfaces. It is shown how the method can be applied toward mechanical wear analysis, where wear scars on tribological test samples are analyzed; and in materials science to determine ion beam sputtering or laser ablation volumes and depths.

白光干涉表面改性中的应用离子溅射，激光烧蚀，与摩擦学实验表征

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. ...

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 ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

环境钚的薄膜弥散形态和生物利用度测量

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

欧姆接触制造用聚焦离子束技术和电气特性的半导体层的纳米结构

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

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 ...

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 ...

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

离子液体基电解质的合成，装配锂离子电池，并在高温性能的测量

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...