我们非常感谢美国国家科学基金会材料研究部从陶瓷计划的支持下，没有授予。的DMR-1006515（项目经理，的琳内特四博士马德森）。

1。工作电极的制备<ol><li>准备一个混合物〜6重量。 ％的聚偏二氟乙烯（PVDF）粘结剂在2-N-甲基吡咯烷酮（NMP）。 </li><li>称量80 WT。 ％活性物质（2）在这种情况下，钴酸锂和10 WT。 ％C处的黑色（乙炔，99.9％），然后在1分钟的旋涡混合。 </li><li> NMP-粘结剂混合物添加粘结剂等构成10 WT。 ％的混合物的总重量。 </li><li>上述混合物转移到一个小玻璃瓶，并在最高转速约30分钟的旋涡混合器混合。两个氧化锆球直径为5毫米，可用于为更好的混合媒体。如果需要，添加更多的NMP的，以获得所需的一致性的泥浆。 </li><li>散布目前收集到玻璃板上（通常情况下，阴极和阳极铜，铝）的金属箔。使用丙酮和确保箔和玻璃板之间有没有气泡。使用两层胶带，形成轨道和def址错误发生在被涂的区域。 </li><li>适用于金属箔，用不锈钢锅铲的泥浆和泥浆均匀蔓延的轨道上来，用刀片。 </li><li>干燥的涂层在空气或真空〜90-120℃，约2-8小时（取决于使用的材料和粘结剂应调整）。 </li><li>将两钢板（和两个称重文件保护涂层）和新闻稿〜3000磅用液压机的负载下涂层的金属箔。 </li><li>冲成光盘的直径为8毫米（最好是在一个手套箱）干涂层的金属箔。权衡阴极和包装之前，他们转移到手套箱。 </li><li>冲直径8毫米的光碟相同的材料未涂布的金属箔和权衡这​​些光盘。 </li></ol> 2。电解质的制备<ol><li>作为电解液是感光，存储电解液（1M LIPF在EC：DMC的：DEC在这种情况下）在NALGENE bottl的的é铝箔包裹。 </li></ol> 3。准备一个反电极（在这种情况下，锂箔） <ol><li>清洁表面的锂金属箔，用尼龙刷/不锈钢手术刀，直到出现一个闪亮的银色表面内的氩气手套箱。 </li><li>冲成半英寸直径（内氩气手套箱）光盘，锂箔。 </li></ol> 4。钮扣电池组件<ol><li> 图2显示了一个纽扣电池组件的示意图。 </li><li>冲床Celgard C480膜直径和使用它们分离到19毫米的光碟。 </li><li>转入手套箱纽扣电池（CR2032）提供案件，弹簧和垫片（台扬科技公司购买），分离器和工作电极（冲洗后与氩气换热器的五倍）。 </li><li>在手套箱中装配的纽扣电池。 </li><li>加入两滴电解质对细胞杯，并把它的工作电极。添加其他三个滴滴它们之间的电解液的电解质和地方两个分隔。之前添加上放置电极锂电解液滴。锂光盘上放置两个不锈钢垫片和弹簧。 </li><li>关闭电池使用的电池盖和压3-4次使用的紧凑型扣压机（台扬科技公司购买）。 </li><li>组装后的细胞，处理成品用塑料镊子（避免短路）的细胞。 </li><li>清理多余的电解质从使用餐巾纸细胞的“双方泄漏。 </li><li>细胞是准备进行测试，并可以采取的手套箱。 </li></ol> 5。钮扣电池测试<ol><li>保持钮扣电池，只要它是准备一小时连接到电池的开路电压（OCV）模式测试。 </li><li>定义为在工作电极的活性物质为基础的单元测试，电压窗口。 </li><li>计算的使用如下所示的计算细胞的理论体系的理论容量。 </li></ol>目前收藏家= W 电光与电极片的重量涂层直径相同的集流盘的重量= W CC 电极材料，钨的EM，重量 <img alt="式（1）" src="/files/ftp_upload/4104/4104eq1.jpg" />重量活性物质在电极，钨上午 ，由 <img alt="公式（2）" src="/files/ftp_upload/4104/4104eq2.jpg" />理论容量电极盘，C 海关给予 <img alt="公式（3）" src="/files/ftp_upload/4104/4104eq3.jpg" /> 其中 C是理论的小号pecific能力的活性物质。 <ol start="4"><li>测试所需的C率充放电循环的纽扣电池。 </li></ol> 6。代表结果作为一个例子，构建了一个钮扣电池用钴酸锂作为工作电极的活性物质。项目建成后，细胞C / 5的速率进行了测试。所获得的配置如图3所示。被设置为3和4.3之间至五这个纽扣电池的电压窗口。容量为155毫安时/克的第一个充电周期，首次放电周期为140毫安时/克。 <img alt="图1" src="/files/ftp_upload/4104/4104fig1.jpg" /> 图1。钮扣电池的施工程序流程图。首先，准备工作电极活性物质的粉末。然后，电极准备从一个干净的锂箔和分隔砸出了。最后，一​​个细胞内氩气手套箱组装。 <img alt="图2" src="/files/ftp_upload/4104/4104fig2.jpg" /> 图2。一个纽扣电池装配在他们放在里面的纽扣电池案顺序显示所有的组件的过程示意图。 <img alt="图3" src="/files/ftp_upload/4104/4104fig3.jpg" /> 图3。代表结果获得从一个硬币使用钴酸锂和锂箔电极工作电极的构造单元。图中显示的第一次充电纽扣电池被指控和C / 5的速度排出，首次放电曲线。 <img alt="图4" src="/files/ftp_upload/4104/4104fig4.jpg" /> 图4。比较好的和坏的涂料后，他们已干涸。破涂层通常会导致有多余的NMP和多孔涂层通常​​从业绩从泥浆lurry，有足够的NMP的。 <img alt="图5" src="/files/ftp_upload/4104/4104fig5.jpg" /> 图5。良好的卷曲的纽扣电池和严重卷曲的纽扣电池，随着联合国轧花细胞的比较。通常情况下，严重卷曲的硬币细胞分裂后，锂箔肿胀反应与水分后因周围几个小时开放。

<ol>
	<li>Cairns, E. J., Albertus, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Batteries+for+Electric+and+Hybrid-Electric+Vehicles.">Batteries for Electric and Hybrid-Electric Vehicles.</a> Annual Review of Chemical and Biomolecular Engineering. 1, 299-320 (2010).</li><li>Dunn, B., Kamath, H., Tarascon, J. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+Energy+Storage+for+the+Grid:+A+Battery+of+Choices.">Electrical Energy Storage for the Grid: A Battery of Choices.</a> Science. 334, 928-935 (2011).</li><li>Goodenough, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode+materials:+A+personal+perspective.">Cathode materials: A personal perspective.</a> J. Power Sources. 174, 996-1000 (2007).</li><li>Yamada, A., Chung, S. C., Hinokuma, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimized+LiFePO4+for+lithium+battery+cathodes.">Optimized LiFePO4 for lithium battery cathodes.</a> Journal of the Electrochemical Society. 148, A224-A229 (2001).</li><li>Whittingham, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+batteries+and+cathode+materials.">Lithium batteries and cathode materials.</a> Chemical Reviews. 104, 4271-4301 (2004).</li><li>Tarascon, J. M., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Issues+and+challenges+facing+rechargeable+lithium+batteries.">Issues and challenges facing rechargeable lithium batteries.</a> Nature. 414, 359-367 (2001).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+Rechargeable+Li+Batteries.">Challenges for Rechargeable Li Batteries.</a> Chemical Materials. 22, 587-603 (2010).</li><li>Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Identification+of+cathode+materials+for+lithium+batteries+guided+by+first-principles+calculations.">Identification of cathode materials for lithium batteries guided by first-principles calculations.</a> Nature. 392, 694-696 (1998).</li><li>Chung, S. Y., Bloking, J. T., Chiang, Y. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electronically+conductive+phospho-olivines+as+lithium+storage+electrodes.">Electronically conductive phospho-olivines as lithium storage electrodes.</a> Nature Materials. 1, 123-128 (2002).</li><li>Bruce, P. G., Scrosati, B., Tarascon, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanomaterials+for+rechargeable+lithium+batteries.">Nanomaterials for rechargeable lithium batteries.</a> Angewandte Chemie-International Edition. 47, 2930-2946 (2008).</li><li>Arico, A. S., Bruce, P., Scrosati, B., Tarascon, J. M., Van Schalkwijk, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+materials+for+advanced+energy+conversion+and+storage+devices.">Nanostructured materials for advanced energy conversion and storage devices.</a> Nature Materials. 4, 366-377 (2005).</li><li>Hochbaum, A. I., Yang, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+Nanowires+for+Energy+Conversion.">Semiconductor Nanowires for Energy Conversion.</a> Chemical Reviews. 110, 527-546 (2010).</li><li>Wang, Y., Cao, G. Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Developments+in+nanostructured+cathode+materials+for+high-performance+lithium-ion+batteries.">Developments in nanostructured cathode materials for high-performance lithium-ion batteries.</a> Advanced Materials. 20, 2251-2269 (2008).</li><li>Kang, B., Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Battery+materials+for+ultrafast+charging+and+discharging.">Battery materials for ultrafast charging and discharging.</a> Nature. 458, 190-193 (2009).</li><li>Liu, J., Manthiram, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improved+Electrochemical+Performance+of+the+5+V+Spinel+Cathode+LiMn1.5Ni0.42Zn0.08O4+by+Surface+Modification.">Improved Electrochemical Performance of the 5 V Spinel Cathode LiMn1.5Ni0.42Zn0.08O4 by Surface Modification.</a> Journal of the Electrochemical Society. 156, A66-A72 (2009).</li><li>Kayyar, A., Qian, H. J., Luo, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+adsorption+and+disordering+in+LiFePO4+based+battery+cathodes.">Surface adsorption and disordering in LiFePO4 based battery cathodes.</a> Applied Physics Letters. 95, (2009).</li><li>Sun, K., Dillon, S. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+mechanism+for+the+improved+rate+capability+of+cathodes+by+lithium+phosphate+surficial+films.">A mechanism for the improved rate capability of cathodes by lithium phosphate surficial films.</a> Electrochemistry Communications. 13, 200-202 (2011).</li><li>Kovalenko, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Major+Constituent+of+Brown+Algae+for+Use+in+High-Capacity+Li-Ion+Batteries.">A Major Constituent of Brown Algae for Use in High-Capacity Li-Ion Batteries.</a> Science. 333, 75-79 (2011).</li></ol>

没有利益冲突的声明。

根据我们的经验，在最关键的一步准备工作电极与一致性良好的泥浆。 如图4所示，多余的NMP的泥浆可以导致裂纹的涂料，而NMP的不足可能会导致一种多孔涂层。在这里介绍的工作，是在直径20毫米的CR2032钮扣电池的情况下使用。应当指出，不同大小的纽扣电池的情况下可以使用，其中应更改相应的电极大小。细胞大会期间，要使用适当的间隔取决于厚度的锂箔电极和细胞的高度。这?...

<table border="1"><tbody><tr><td> 试剂名称 </td><td> 公司 </td><td> 目录编号 </td></tr><tr><td>聚（偏二氟乙烯） </td><td> Sigma-Aldrich公司</td><td> 182702 </td></tr><tr><td> 1 - 甲基-2 - 吡咯烷酮，99.5％ </td><td>阿法埃莎</td><td> 31903 </td></tr><tr><td> 钴酸锂</td><td>阿法埃莎</td><td> 42090 </td></tr><tr><td>炭黑，乙炔，99.9％; </td><td>阿法埃莎</td><td> 39724 </td></tr><tr><td> 6 LIPF在EC：DMC的：DEC </td><td>台扬科技股份有限公司</td><td>情商是LiPF6的</td></tr><tr><td> celgard分隔</td><td> celgard </td><td> C480 </td></tr><tr><td>模拟旋涡混合器</td><td>厂商VWR </td><td> 58816-121 </td></tr><tr><td>真空烘箱</td><td></td><td></td></tr><tr><td>真空抽</td><td></td><td></td></tr><tr><td>液压机</td><td></td><td></td></tr><tr><td>纽扣电池案</td><td>台扬科技股份有限公司</td><td> EQ-CR2032锂案例-304 </td></tr><tr><td>春和间隔</td><td>台扬科技股份有限公司</td><td> EQ-CR20SprSpa-304 </td></tr><tr><td>手套箱</td><td> mBraun </td><td> UNILAB </td></tr><tr><td>电池测试仪</td><td> arbin仪器</td><td> BT2143 </td></tr></tbody></table>

construction and testing of coin cells of lithium ion batteries

可充电锂离子电池，具有广泛的应用在电子，客户总是要求更多的能力和更长的使用寿命。锂离子电池也被认为是用于电动和混合动力汽车，1甚至电网稳定系统2。所有这些应用模拟在3-7电池材料，其中包括3,8新材料的研究和开发的急剧增加，掺杂，纳米构型10-13，涂层或表面改性14-17和新型粘合剂18。因此，越来越多的物理学家，化学家和材料科学家最近涉足这一领域。纽扣电池被广泛用于研究的实验室测试新的电池材料的研究和发展目标的大规模和高功率的应用，小钮扣电池通常用于测试的能力和速度能力在初始阶段的新材料。 在2010年，我们开始了国家科学基金会（NSF）资助的研究项目，以调查在电池材料表面吸附和无序（赠款。的DMR-1006515）。在这个项目的初始阶段，我们一直在努力学习钮扣电池，不能没有其他大学的其他研究人员通过频繁的电话，电子邮件交流和两个实地考察的许多帮助的情况下取得的组装和测试技术。因此，我们认为它是有益的，通过文字和视频记录，组装和测试一个钮扣电池，这将有助于在这一领域的其他新的研究协议。这方面的努力表示“更广泛的影响”我们的国家科学基金会项目活动，它也将帮助教育和启发学生。 在这部影片的文章，我们记录协议与1 钴酸锂的工作电极，李电极组装CR2032纽扣电池（大多常用）聚偏二氟乙烯（PVDF）粘结剂。为了确保新的学习者很容易重复的协议，我们作为具体和明确的，我们可以保持协议。然而，重要的是要注意，在具体的研究和开发工作，通过这里可以改变许多参数。首先，可以使不同大小的纽扣电池和一个反电极比李对测试工作电极。第二，碳黑色和粘合剂的金额加入到工作电极，以适应特定的研究目的往往不同，例如，大量的C或黑色甚至是惰性粉末添加到工作电极的“内在”性能测试正极材料14。第三，更好的粘合剂（比氟碳其他）还开发和使用18。最后，还可以用于其他类型的电解质（而不是6 LIPF），事实上，某些高电压的电极材料将需要特别electrol用途ytes 7。

Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

Construction and Testing of Coin Cells of Lithium Ion Batteries

构建和测试钮扣电池的锂离子电池的协议描述。使工作电极，电极准备，手套箱内组装电池和测试细胞的具体程序。

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 ...

construction-and-testing-of-coin-cells-of-lithium-ion-batteries

Research

JoVE Journal

Engineering

31.2K 次观看.  Clemson University. 构建和测试钮扣电池的锂离子电池的协议描述。使工作电极，电极准备，手套箱内组装电池和测试细胞的具体程序。

视频: Construction and Testing of Coin Cells of Lithium Ion Batteries

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. ...

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 ...

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 ...

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 ...

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 ...

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 ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

胶孔溶液的表达及其化学成分和电阻率的 X 射线荧光分析

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

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 ...