Name: non-aqueous electrode processing and construction of lithium-ion coin cells
Uploaded: 2016-02-01T15:00:00.000+00:00
Duration: 12 min 28 s
Description: Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

这项工作是由得克萨斯州A与M大学教师科研启动资助（慕克吉）和德克萨斯州立大学启动资金（罗德）资助。

注意应在使用任何溶剂，试剂，或干在这个协议中使用的粉末行使。阅读所有MSDS表，并采取相应的安全措施。标准的安全装备，包括手套，防护眼镜和白大褂。 1.阴极的制备注意:阴极制造过程的示意概示于图1。 <img alt="图1" src="/files/ftp_upload/53490/53490fig1.jpg" /> 在ETSL创建阴极用的步骤图1.示意图概述。主要工艺包括制备和电极浆料浇铸到一个清洁的铝基材，接着在电极片和掺入硬币电池的干燥。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53490/53490fig1large.jpg" target="_blank">请按此查看大图已经</a>rsion这个数字。 <ol><li> 铝基准备 <ol><li>切4.5"12"的15微米厚的铝（Al）使用切纸机或剪刀箔片。 </li><li>喷干净的塑料板的表面上的丙酮坚持箔到板上，然后将金属箔片到电路板上。 </li><li>喷洒丙酮的大方量的箔的表面上，并开始擦洗用苏格兰垫与小半圆运动的整个表面。喷雾额外的丙酮在表面上，并擦拭残留物用纸巾。 </li><li>重复步骤1.1.2-1.1.3的相对侧，然后再次重复用于铸造侧。 </li><li>洗涤蚀刻铝片与去离子（DI）水铸件侧第一，然后翻转并重复相反的一侧。再擦洗的Al箔作为DI水显示器润湿性差的表面，并且不流断片的表面而不形成液滴。重复用异丙醇漂洗醇。 </li><li>传输2纸巾之间的清洗铝板，并允许干燥约20两个平坦平面和纸巾之间在压缩下分钟。 </li></ol></li><li> 浆料制备 <ol><li>选择基于所述电极片的所需组成的活性物质，导电助剂和粘合剂的重量。选择的1.25 g的总干粉末重量，用70％（重量）锂-锰-钴氧化物，的LiNi 1/3 1/3锰钴1/3 O 2（NMC，活性物质），20重量％碳黑（导电添加剂）和10％聚偏二氟乙烯（PVDF，粘合剂）。 </li><li>量出0.875克NMC和0.25g炭黑和地到玛瑙研钵和研杵。轻轻混合材料一起无需研磨。后的混合物开始形成，轧机由手在研钵和杵3-5分钟，直到形成均匀的粉末目视观察​​。 </li><li>传送该混合粉末到一次性混合管用一张称量纸。加16个玻璃球（直径6毫米）对粉末，沿着5.5毫升1-甲基-2-吡咯烷酮（NMP），非水溶剂中。 </li><li>将一次性管到管驱动站锁定到位。打开驱动器，并慢慢增加的最大速度。允许内容物混合15分钟。 </li><li>添加1.25克10％的PVDF的NMP溶液直接向管。将管放回驱动，并允许混合8分钟，之后在1.2.4相同的过程。如果管被允许铸件（以下）之前坐超过5分钟，混合内容物额外的15分钟。 </li></ol></li><li> 铸造和干燥 <ol><li>清洁自动薄膜涂布器，用异丙醇和纸巾的金属表面上。确保刮刀是干净的，并且被设置为所需的铸造高度（200微米）。 </li><li>敷一层异丙醇到薄膜敷贴的表面上，然后将DRI编铝基材光泽的一面朝下在表面上。压出过量的异丙醇与折叠纸巾，直到所有的皱纹和异丙基被除去。小心避免由牢固地保持基板的酮代替撕开基板。 </li><li>从管驱动器中取出搅拌筒，打开容器。倒在2-3英寸线大​​约1英寸从衬底的顶部（初始铸件侧）浆料到衬底的表面上。从用干净的金属镊子表中删除任何玻璃球。 </li><li>设置铸造速度20毫米/秒，并激活膜涂布的铸造臂。 </li><li>使用薄的纸板，以确保无皱纹的片材上形成解除从膜涂布器的表面流延电极。 </li><li>允许所述电极片在室温干燥16小时（〜24℃）后，在70℃下干燥〜3小时，或直到片干燥。确保电极是孤立的环境中福我罩或密封腔，防止非均匀的干燥。 </li></ol></li><li> 阴极冲孔 <ol><li>放置干燥的电极片上的铝金属的清洁片。取出一个半"打孔并轻轻将其放置到一个均匀的表面片材的区域（边缘，可能会出现不均匀的），慢慢加压，冲头（用手）和"滚动"的压力围绕的边缘冲头，以确保干净的切割。 </li><li> （替代）剪下利用代替人工冲压的精确圆盘铣刀的电极盘。 </li><li>从与清洗，塑料钳片材中取出电极，将其放入一个小瓶标记，与电极表面朝上。重复两次。 </li><li> （可选）将穿孔电极到实验室新闻的表面。应用约4兆帕（最优化的压力将根据按不同而有所不同）的压力。重复其余的电极。 </li><li>将小瓶中VACU嗯烘箱，并允许电极以进一步干燥，在120℃下以-0.1兆帕12小时以除去任何剩余的水分。后，取出电极和内部0.0001克衡量他们。 </li><li>打开手套箱的前室，然后将瓶子放在托盘上。关闭室门，保证密封用两个手指收紧前厅孵化。 </li><li>把真空下降到-0.1兆帕，然后填充氩气。重复这一过程1-2次，这取决于运入手套箱的样品。 </li></ol></li></ol> 2.阳极板的完整细胞<ol><li>重复部分1不同的是使用9微米厚的铜箔作为基材，代替铝箔。片材的组合物可被改变以适合特定需求。 </li></ol> 3.纽扣电池预装配 注意:在一个手套箱内的惰性（氩）环境下进行硬币电池的构造。 Ë的Xtreme一定要小心，以最小化内部环境与外部气氛的暴露。与手套箱内急剧材料的工作应尽可能最小化。作为一般规则，在手套箱内的任务应该比该任务将被外执行的速度的3倍以上。手套也应穿在手套箱手套不同的物质工作时，尽量减少曝光。 注意:需要的硬币电池的结构的部件，包括帽，外壳，波形弹簧，垫圈，垫片，锂色带，电解质和其余如塑料镊子（对于元件放置）工具包含一个充满氩气的手套箱内与O 2和H 2 O水平保持在低于每百万0.5份。插入到手套箱（包括无绒任务湿巾）的所有组件应加热O / N在真空烘箱中在120℃下以-0.1兆帕的压力，以消除任何湿气。 <ol><li> 反电极制备 <ol><li>内手套箱，从密封容器中取出锂色带（0.75毫米厚）和推出的部分到塑料块的表面上。用剃刀刀片，小心刮掉从箔表面的任何黑色的氧化。格外小心，避免切割手套。 </li><li>以9/16"打孔和切出一盘锂带的，用手指（从锂手套箱内分隔的橡胶手套）或其他钝的工具来推动锂盘出了一拳。 </li><li>取一0.5mm厚隔板和锂盘轻轻应用于手指之间的表面。确保锂光盘粘附到隔离物的中心，是平坦 - 不平坦表面可能导致不均匀的电流分布。 </li></ol></li><li> 电解液制备 <ol><li>存储所选择的电解质（在此情况下的1M的LiPF 6的EC / DEC 1:1体积）与在手套箱在任何时候都在铝容器中，作为电解质是光敏的。 </li><li>除去少量从源容器电解质到工作容器。 </li></ol></li><li> Celgard公司分离制备 <ol><li>放置的打印纸折叠片材之间的分隔膜的薄片。放置折叠的纸张和膜在铝金属片。 </li><li>广场上打孔顶部的缓冲层，并用锤子猛击了3/4"直径分离膜。 </li><li>转移冲孔分离盘成利用在1.4.6-1.4.7中概述的程序手套箱。 注:建议执行此步骤散装以避免冲出来单独分隔每个纽扣电池正在建设中。 </li></ol></li></ol> 4.纽扣电池组件 注意:所述硬币电池的结构示于图2。 <img alt="图1" src="/files/ftp_upload/53490/53490fig2.jpg" /> 图2.钮扣电池组件中的单元格中显示，为了安置。阴极安置其次是分隔符，垫圈，对电极和波形弹簧，然后密封电池。 <a href="https://www-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/53490/53490fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。 。</a> <ol><li>打开室内接待室的门。前厅到手套箱内拉的所有组件和重新密封室内接待室的门。 </li><li>将一个纽扣电池的情况下进入一个小权衡船。将阴极到硬币电池外壳的中心。适用电解质1-2〜30微升滴在电极的中心，并应用1滴上的​​情况下的边缘的相对侧。 </li><li>放置在单个¾"分离器到电极的表面上。力指出，成为用一对镊子的平坦边缘捕获任何气泡，并重新中心阴极由唇抓住的情况下，并轻轻拍打电极到位。应用附加的1-2滴电解质，以允许所述电极的更好的运动，如果它坚持其原来的位置。 </li><li>将垫片成的情况下，用平面朝下和唇面朝上。通过举起到光之前元插入确认衬垫的取向。 </li><li>适用电解质2-3〜30微升液滴到小区的中心，并把准备好的反电极上的中心与锂朝下。将波形弹簧上的中心电极之上。 </li><li>填充单元格的边缘（〜0.7mL）中的电解质，直到它形成了一个弧形，凸弯月形，涵盖大部分的波形弹簧表面。 </li><li>小心地将纽扣电池盖在电池使用的T顶部他用镊子按住垂直居中在单元格中的上限。小心中心盖，以避免电解质丧失过多。 </li><li>向下按压帽（用手），直到它设置成密封垫的唇。细胞转移到卷曲，并确保该单元被集中在压接模具的槽。压接小区的〜6.2兆帕（900磅），并释放压力。 </li><li>拆除压接器（手动）细胞，并清理任何多余的电解质。重复步骤4.2- 4.9，直到所有所需的细胞构造。清理溢出的电解液，将垃圾变成一个合适的容器。转移单元出来的手套箱，并贴上标签。 </li></ol> 5.电化学评定<ol><li>清洗过的细胞连接到电池循环仪。确保端子通过测量开路电位正确连接。如果不是正，反转的连接。 </li><li>计算基于所述干燥ELEC的重量所需的电流处接上的铝基板中，铝，重量的活性物质的百分比的已知质量，以及所使用的活性物质的额定容量具体的表面上。 <ol><li>与测量电极质量0.0090克中，0.0054克铝盘的质量，以及155毫安时/ g的额定容量，确定所需的电流（0.0090克 - 0.0054克）×0.70×155毫安时/ G = 0.3906毫安。对于放电所需完全放电中1小时（1C）电解槽的电流，施加的电流为0.3906毫安。 </li></ol></li><li>上设置循环仪的时间表进行充电/ 4倍的速率/ C为10（恒电流，恒电流）的4.2 V和2.8V。周期单元中的上，下电压电平之间的单元放电。然后，在C / 10的电池充电一次。 </li><li>经过5 个 C / 10充电，请从循环仪细胞（如有必要）和细胞上进行电化学阻抗谱19（EIS），休息1小时后。放置电池背在循环仪放电C / 10日。休息1小时后执行EIS一次。 </li><li>将细胞放回循环仪和循环的细胞5次，在C / 5，C，2C，5C和10C的速率，然后用100 1C循环。 </li><li>通过以mAh容量除以活性物质存在于所述阴极的质量决定了细胞在每个C-速率的比容量。由最后5 1C的平均周期比容量除以第5 1C的平均周期比容量计算容量保持率。 </li></ol>

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P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructure+Evolution+in+Lithium-Ion+Battery+Electrode+Processing.">Microstructure Evolution in Lithium-Ion Battery Electrode Processing.</a> J Electrochem Soc. 161, E3248-E3258 (2014).</li><li>Zheng, H. H., Tan, L., Liu, G., Song, X. Y., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Calendering+effects+on+the+physical+and+electrochemical+properties+of+Li[Ni1/3Mn1/3Co1/3]O-2+cathode.">Calendering effects on the physical and electrochemical properties of Li[Ni1/3Mn1/3Co1/3]O-2 cathode.</a> J Power Sources. 208, 52-57 (2012).</li><li>Zheng, H. H., Li, J., Song, X. Y., Liu, G., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+comprehensive+understanding+of+electrode+thickness+effects+on+the+electrochemical+performances+of+Li-ion+battery+cathodes.">A comprehensive understanding of electrode thickness effects on the electrochemical performances of Li-ion battery cathodes.</a> Electrochim Acta. 71, 258-265 (2012).</li><li>Marks, T., Trussler, S., Smith, A. J., Xiong, D. J., Dahn, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Guide+to+Li-Ion+Coin-Cell+Electrode+Making+for+Academic+Researchers.">A Guide to Li-Ion Coin-Cell Electrode Making for Academic Researchers.</a> J Electrochem Soc. 158, A51-A58 (2011).</li><li>Li, C. C., Wang, Y. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Binder+Distributions+in+Water-Based+and+Organic-Based+LiCoO2+Electrode+Sheets+and+Their+Effects+on+Cell+Performance.">Binder Distributions in Water-Based and Organic-Based LiCoO2 Electrode Sheets and Their Effects on Cell Performance.</a> J Electrochem Soc. 158, A1361-A1370 (2011).</li></ol>

The authors have nothing to disclose.

湿混级的优化是至关重要的浆料粘度和涂布能力，这会影响该电极的均匀性和粘附性。这里的高剪切混合方法被利用​​，其中，溶剂，添加剂，粘合剂，和活性物质混合在一起利用玻璃球存在于小瓶的动力学运动。该混合技术提供的更快速混合倍的益处相比，磁力搅拌器方法。除此之外，这种高剪切混合允许更粘性的溶液，以得到有效的混合，并提供必要的混合更困难的粘合剂的能量，如在水?...

锂离子电池代表有希望的来源以满足能量存储装置1-4的不断增加的要求。在LIBS能力的改善，不仅提高了有效程型电动车5,6，同时也通过降低放电深度，这反过来又增加LIBS的可行性在电网储能应用7使用改善他们的循环寿命。 最初用于助听器在1970 8，今天硬币电池通常用在新的和现有的电极材料的开发和评价。作为最小形式因子的电池中的一个，这些细胞代表一个简单而有效的方式，以在学术研究设置创建电池。典型的锂离子电池包括一阴极，阳极，集流器，以及防止在阳极和阴极的短路的多孔隔板。在一个锂离子电池的操作中，io的纳秒和电子是移动的。在放电过程中，离子从通过多孔分离器的负电极（阳极）并进入正​​电极，或阴极行进。同时，电子通过集电体行进，穿过外部电路，最后用在阴极侧的离子重组。为了减少与离子和电子转移相关联的任何的电阻，该组件需要正确地定向 - 的距离离子行程应最小。通常，这些部件被组合一个"夹层"结构。在电动汽车，移动电话，和消费电子产品的电池包括被螺旋缠绕或折叠，根据电池的形状因数大三明治。这些类型的细胞可以是非常困难的，而不会产生高的成本来制造在小范围。然而，在纽扣电池有细胞内只有一个三明治。虽然专门的设备仍然是必要的，以建立电极我<html> Ñ​​硬币电池，细胞本身可用手快速组装并密封在一个受控制的环境。 电池的性能，而不管类型的，依赖于形成的正，负电极，电解液的选择，和小区架构4,9-13的材料。一个典型的LIB电极由含Li的活性物质，导电助剂，聚合物粘合剂，以及填充有电解质的空隙空间的组合。电极的处理可以组织成五个主要步骤:干燥粉末的混合，湿式混合，衬底准备，薄膜应用，和干燥 - 即常很少关注的工序。当生产使用这些处理工序中的电极，最终目标是实现一个均匀的电极膜构成的活性物质，导电助剂，粘合剂的。此均匀分布是LIBS 14-18的最佳性能是至关重要的。 NT"&gt;该指南表示在得克萨斯州A＆M在能源和运输科学实验室（ETSL）和得克萨斯州立大学用于制造纽扣电池为新的和现有的电极材料评价的步骤。除了发现记录在许多来源的基本步骤，我们包括我们自己的专业知识在关键的步骤，并指出，经常被冷落的类似的方法文件和许多出版物的重要细节。此外，在我们的实验室中使用的主要物理和电化学方法（恒电流循环和电化学阻抗谱（EIS））在被阐明。

<table><tbody><tr><td>LiNiMNCoO&lt;sub&gt;2&lt;/sub&gt; (NMC, 1:1:1)</td><td>Targray</td><td>PLB-H1</td><td></td></tr><tr><td>CNERGY Super C-65</td><td>Timcal</td><td></td><td></td></tr><tr><td>Polyvinylidene Difluoride (PVDF)</td><td>Kynar</td><td>Flex 2801</td><td></td></tr><tr><td>1-Methyl-2-pyrrolidinone anhydrous, 99.5% NMP</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>1.0 M LiPF&lt;sub&gt;6&lt;/sub&gt; in EC/DEC (1:1 by vol)</td><td>BASF</td><td>50316366</td><td></td></tr><tr><td>Celgard 2500 Separator</td><td>MTI</td><td>EQ-bsf-0025-60C</td><td>25 &amp;#956;m thick; Polypropylene</td></tr><tr><td>Aluminum Foil</td><td>MTI</td><td>EQ-bcaf-15u-280</td><td></td></tr><tr><td>Lithium Ribbon</td><td>Sigma Aldrich</td><td>320080</td><td>0.75 mm thickness</td></tr><tr><td>2-Propanol, ACS reagent, &amp;ge;99.5%</td><td>Sigma Aldrich</td><td>190764</td><td></td></tr><tr><td>Acetone, ACS reagent, &amp;ge;99.5%</td><td>Sigma Aldrich</td><td>179124</td><td></td></tr><tr><td>Stainless Steel CR2032 Coin Cell Kit&amp;nbsp;</td><td>Pred Materials</td><td></td><td>case, cap, and PP gasket</td></tr><tr><td>Stainless Steel Spacer&amp;nbsp;</td><td>Pred Materials</td><td></td><td>15.5 mm diameter x 0.5&amp;nbsp;mm thickness</td></tr><tr><td>Stainless Steel Wave Spring&amp;nbsp;</td><td>Pred Materials</td><td></td><td>15 mm diameter x 1.4&amp;nbsp;mm height</td></tr><tr><td>Analytical Scale</td><td>Ohaus</td><td>Adventurer AX</td><td></td></tr><tr><td>Agate Mortar and Pestle</td><td>VWR</td><td>89037-492</td><td>5 inch diameter</td></tr><tr><td>Tube Drive</td><td>IKA</td><td>3645000</td><td></td></tr><tr><td>20 ml Stirring Tube</td><td>IKA</td><td>3703000</td><td></td></tr><tr><td>Glass balls</td><td>McMaster-Carr</td><td>8996K25</td><td>6 mm diameter</td></tr><tr><td>Automatic Film Applicator</td><td>Elcometer</td><td>K4340M10-</td><td></td></tr><tr><td>Doctor Blade</td><td>Elcometer</td><td>K0003580M005</td><td></td></tr><tr><td>Die Set</td><td>Mayhew</td><td>66000</td><td></td></tr><tr><td>Vacuum Oven</td><td>MTI</td><td></td><td></td></tr><tr><td>Vacuum Pump</td><td>MTI</td><td></td><td></td></tr><tr><td>Laboratory Press</td><td>MTI</td><td>YLJ-12</td><td></td></tr><tr><td>Hydraulic Crimper</td><td>MTI</td><td>MSK-110</td><td></td></tr><tr><td>Glovebox</td><td>MBraun</td><td>LABstar</td><td></td></tr><tr><td>Battery Cycler</td><td>Arbin Instruments</td><td>BT2000</td><td></td></tr><tr><td>Potentiostat/Galvanostat/EIS</td><td>Biologic</td><td>VMP3</td><td></td></tr></tbody></table>

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.

一个正常投电极片应该会出现均匀的表面外观，妥善坚持集。典型地剥落的电极片的被衬底的任一差蚀刻，或具有至少的NMP在初始混合阶段引起的。可替代地，过多的NMP可以使片材显示较高的孔隙度，这是不可取的。最后，一​​个第三图案可在电极表面上，在那里汇集似乎发生被观察到。相互作用与室（湿度，温度，和任何空气运动）的环境条件针对此行为的最可能的?...

Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

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

锂离子纽扣电池的非水电极加工和施工

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.

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

non-aqueous-electrode-processing-construction-lithium-ion-coin

Universidad San Sebastian

Research

JoVE Journal

Engineering

21.5K 次观看.  Texas A&M University. 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.

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

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

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

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

正极材料的同步辐射技术锂离子和钠离子电池表征

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

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 ...

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 ...

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 ...

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 ...

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate multiple processes responsible for long-term performance decay. Given the complexity of physical processes occurring inside the cell, it is often challenging to achieve a full understanding of the root causes of this performance degradation. This difficulty arises in part from the fact that any electrochemical measurement of a battery will return the combined contributions of all components in the cell. Incorporation of a reference electrode can solve part of the problem, as it allows the electrochemical reactions of the cathode and the anode to be individually probed. A variation in the voltage range experienced by the cathode, for example, can indicate alterations in the pool of cyclable lithium ions in the full-cell. The structural evolution of the many interphases existing in the battery can also be monitored, by measuring the contributions of each electrode to the overall cell impedance. Such wealth of information amplifies the reach of diagnostic analysis in Li-ion batteries and provides valuable input to the optimization of individual cell components. In this work, we introduce the design of a test cell able to accommodate multiple reference electrodes, and present reference electrodes that are appropriate for each specific type of measurement, detailing the assembly process in order to maximize the accuracy of the experimental results.

The incorporation of reference electrodes in a Li-ion battery provides valuable information to elucidate degradation mechanisms at high voltages. In this article, we present a cell design that accommodates multiple reference electrodes, along with the assembly steps to assure maximum accuracy of the data obtained in electrochemical measurements.

原位锂化参考电极: 四原位阻抗谱的电极设计

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

化学

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

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

锂离子电池三电极硬币电池制备及电沉积分析

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

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 ...