Name: protocol of electrochemical test and characterization of aprotic li-o2 battery
Uploaded: 2016-07-12T13:00:00.000+00:00
Duration: 8 min 18 s
Description: Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

Research at Argonne National Laboratory was funded by U.S. Department of Energy, FreedomCAR and Vehicle Technologies Office. Use of the Advanced Photon Source and research carried out in the Electron Microscopy Center at Argonne National Laboratory was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

使用前请咨询所有相关的材料安全数据表（MSDS）。几个在这些合成中使用的化学品是剧毒和致癌性。相比，他们的大部分对手纳米材料可能有额外的危害。进行纳米晶体的反应包括利用工程控制（通风橱，手套箱）和个人防护装备时，请使用所有适当安全守则（安全眼镜，手套，实验室外套，全长裤，封闭趾鞋）。以下过程部分涉及标准自由的空气处理技术。 1.正极材料的合成注意:阴极材料可通过任一原子层沉积或湿化学反应来合成。 <ol><li> 原子层沉积（ALD） <ol><li>分散在100毫升的1M的KMnO 4溶液5克多孔碳的磁力搅拌下12小时。 </li><li>价差100毫克的第Ë氧化炭末到ALD仪器的不锈钢托盘，并夹紧在托盘不锈钢网罩。 </li><li>保持在200℃下在托盘碳粉下在1乇的压力30分钟，300sccm的超高纯度氮气载气的连续流动。 </li><li>具有完整的ALD循环处理碳粉末如下。 注:以钯纳米粒子如在本协议的电催化剂的一个例子。试剂可根据具体要求而改变。使用的所有试剂无需任何进一步纯化原样接收。 <ol><li>在200℃下100分钟暴露碳基板（100毫克）与钯六氟钯（Pd（HFAC）2，99.9％）。 </li><li>在1乇的压力为300分钟吹扫用300sccm的超高纯度氮气载气的连续流动的托盘。 </li><li>暴露在200℃下在碳基材福尔马林（甲醛37％（重量）的H 2 O）为100分钟。 </li><li>清除ŧ他与在1乇的压力为300分钟300标准立方厘米的超高纯度氮气载气的连续流动托盘。 </li></ol></li><li>重复ALD循环是必要的。通常3-10重复。 </li></ol></li><li> 湿化学反应 注:以铁纳米颗粒在本协议的电极催化剂的一个例子。试剂可根据具体要求而改变。使用的所有试剂无需任何进一步纯化原样接收。 <ol><li>分散在100毫升的1M的KMnO 4溶液5克多孔碳的磁力搅拌下12小时。 </li><li>洗用离子交换水氧化碳。 </li><li>过滤用安装有一个玻璃纤维过滤器烧瓶中的洗涤碳，然​​后在110℃干燥它在烘箱中12小时。 </li><li>分散在100ml的去离子水将干燥的碳，再加入磁力搅拌下1克的FeCl 3。 </li><li>调节pH值至约9，使用1M NaOH溶液。 </li><li>搅拌第resulting浆液5小时，然后过滤用安装有一个玻璃纤维过滤器烧瓶中的淤浆。 </li><li>用去离子水和乙醇洗涤产物。然后在110℃下烘干的烘箱中过夜。 </li><li>在450℃下在石英管炉的 H 2 / Ar混合（4％的H 2）的连续流加热处理的产物。用100毫升/分钟的流速为5小时。 </li></ol></li></ol> 2.电极和电解液的制备<ol><li> 阴极 <ol><li> 1重量比在4混合所制备的阴极材料和粘合剂聚（偏二氟乙烯）（PVDF）。 注:混合物的总取决于阴极的量。阴极材料的每片上的负载量为0.1-1毫克的范围内。 </li><li> 1-甲基-2-吡咯烷酮（NMP）加入到该混合物中，并搅拌均匀，使偶数纹理化浆料。在该混合物的大约三倍的重量添加NMP。 </li><li>涂层浆料到鸬鹚通过用大约100微米的厚度的刮刀Ñ纸张。 </li><li>干燥在真空烘箱叠层在100℃下过夜。 </li><li>冲层压到磁盘用打孔器到直径7/16英寸，并称重。 </li></ol></li><li> 非质子电解质 <ol><li>干三氟甲磺酸锂（LiCF 3 SO 3）中，在100℃的真空烘箱中过夜。 </li><li>加入干燥LiCF 3 SO 3在四乙二醇二甲醚（TEGDME; H 2 O〜10ppm的）用1mol / L的浓度，再搅拌用磁力搅拌该溶液直到盐溶解。 </li><li>保持电解液中充氩手套箱。 </li></ol></li><li> 阳极 <ol><li>用打孔器成直径为7/16英寸的冲锂箔/芯片到磁盘。 </li></ol></li></ol> 3.电化学测试<ol><li> 世伟洛克电池的组装&lt;/ STRONG&gt; 注:大会所有的步骤在充满氩气手套箱进行操作，除了3.1.9。 <ol><li>组装洛克集， 如图1a中 。拧紧阳极结束，松开阴极结束。 </li><li>把一块锂金属片（直径7/16英寸）的在阳极部的不锈钢棒的顶端。 </li><li>把一块玻璃纤维隔板（直径1/2英寸）的对锂金属阳极的顶部。 </li><li>添加电解质的5-7滴充分润湿玻璃纤维隔板。轻压分离去除气泡。 </li><li>把一块阴极上的润湿隔板的顶部，面向阳极的活性材料。 </li><li>覆盖用一块铝网（直径7/16英寸）的阴极。 </li><li>按与铝管上述层，然后拧紧阴极结束。 </li><li>密封在一个玻璃室中的整个洛克细胞，并用夹具固定该腔室，如图<st荣&gt;图1。 </li><li>以整个小区出来手套箱。玻璃室连接到超高纯度氧气罐，并在30分钟1个大气压的压力连续氧气流吹扫它。 </li></ol></li><li> 电池性能测试 <ol><li>设置一个恒温器至25℃。 </li><li>把细胞和电极（通过电缆连接到所述设备的电子剪辑）到温控器，并解决这些问题。 </li><li>夹在玻璃室中的阴极和阳极与相应的电子剪辑。 </li><li>打开电池测试系统的操作软件，并选择与电缆连接的通道。 </li><li>设置电化学测试的一个过程。 注意:组100毫安/ g 活性物质的电流密度，和2.2-4.5 V的电压范围<ol><li>设定的2.2 V放电测试放电截止电压。 </li><li>设置5或10小时的能力控制循环测试中的放电/充电步的时间。 </LI&gt; <li>设置的4.5 V为电压控制循环试验2.2 V和充电截止电压的放电截止电压。 </li></ol></li><li>通过点击软件界面上的"运行"按钮来运行程序。 </li></ol></li><li> 拆卸和小区的清洁 <ol><li>拆卸细胞在手套箱。 </li><li>保持在玻璃小瓶电极为以下特征。转让的其他电池相关零部件出了手套箱。 </li><li>放洛克份，不锈钢棒，铝管和铝网眼的丙酮溶液（〜20％）或去离子水在烧杯中，并用超声波清洗它们15-30分钟。 </li><li>干的部件和玻璃腔室中设定为60-80℃的恒温。 </li></ol></li></ol> 4.表征试样的制备注:样品在通风橱制备（对于所制备的材料）或手套箱填充有氩（对于空气敏感的标本）。 <ol><li> 标本进行SEM和XPS <ol><li>贴在样品台上的碳胶带。碳胶带可以是一样大的试料台，或者小如试样片。 </li><li>切下一块试样约5 平方毫米，并坚持其碳磁带上。 注:样品可以是任何非磁性样品。对于之后的电化学测试的样本，粘在碳带之前，电解液溶剂清洗。 </li><li>测量前密封的玻璃瓶空气敏感的标本。 </li><li>根据制造商的说明进行操作的扫描电镜34-36或XPS 37,38。 </li></ol></li><li> 标本TEM <ol><li>穆勒1毫克的样品粉末。 注意:对于电极标本，研磨前刮掉活性材料关复写纸。 </li><li>装载样品粉末在铜网格，并删除散粉。 </li><li>装入铜摹去掉通过TEM的样品架。 注意:获取此步骤尽可能快地完成对空气敏感的样品。 </li><li>透射电镜执行。39-41 </li></ol></li><li> 标本的高能量X射线衍射 <ol><li> 粉末样品 <ol><li>由粘土或胶密封聚酰亚胺管的一端。 </li><li>加载粉末进入管道。 </li><li>密封该管的另一端。 </li></ol></li><li> 磁盘标本 注意:为了测量电极活性材料，另一种选择是刮不送炭纸，并按照步骤4.3.1。 <ol><li>密封件样品用一块尼龙胶带。通过将在一块带的中间的样品，并与另一条胶带覆盖它们密封。 注意:对于之后的电化学测试样品，在密封前与电解质溶剂清洗。 </li></ol></li><li>操作高能量X射线衍射42-44高级博士OTON源在阿贡国家实验室。 </li></ol></li><li> 标本XANES <ol><li> 粉末样品 <ol><li>稀释样品，如果所测量的元素的浓度高，即使用氮化硼（BN）或炭黑作为稀释剂。在这里，稀释至3-5重量。 ％。 </li><li>按粉末进入盘具有7毫米直径和大约1毫米的厚度，使用的是溴化钾新闻资料到7mm模具组。 </li><li>与密封窗膜的磁盘。 </li></ol></li><li> 磁盘标本 <ol><li>与密封窗膜标本。 </li></ol></li><li>操作高能XANES在先进光子源在阿贡国家实验室45-47。 </li></ol></li><li> 标本ATR-FTIR <ol><li>前后测量后清洁钻石衰减全反射（ATR）单元。 </li><li>把标本感兴趣的所有样品的钻石机。 </li><li>执行ATR-FTIR光谱。48,49 </li></ol></li><li> 标本拉曼光谱 <ol><li>把样品在平板上（玻璃，不锈钢等 ）。 </li><li>盖上盖玻片的标本。 </li><li>密封空气敏感的样本集。 </li><li>执行拉曼光谱。50,51 </li></ol></li></ol>

<ol>
	<li>Abraham, K. M., Jiang, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+polymer+electrolyte-based+rechargeable+lithium/oxygen+battery.">A polymer electrolyte-based rechargeable lithium/oxygen battery.</a> J. Electrochem. Soc. 143, 1-5 (1996).</li><li>Bruce, P. G., Freunberger, S. A., Hardwick, L. J., 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=Li-O2+and+Li-S+batteries+with+high+energy+storage.">Li-O2 and Li-S batteries with high energy storage.</a> Nat. Mater. 11, 19-29 (2012).</li><li>Lu, J., 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=Aprotic+and+Aqueous+Li-O2+Batteries.">Aprotic and Aqueous Li-O2 Batteries.</a> Chem. Rev. 114, 5611-5640 (2014).</li><li>Black, R., Adams, B., Nazar, L. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Non-Aqueous+and+Hybrid+Li-O2+Batteries.">Non-Aqueous and Hybrid Li-O2 Batteries.</a> Adv. Energy Mater. 2, 801-815 (2012).</li><li>Bruce, P. G., Hardwick, L. J., Abraham, K. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium-air+and+lithium-sulfur+batteries.">Lithium-air and lithium-sulfur batteries.</a> MRS Bull. 36, 506-512 (2011).</li><li>Christensen, J., 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+Critical+Review+of+Li/Air+Batteries.">A Critical Review of Li/Air Batteries.</a> J. Electrochem. Soc. 159, 1-30 (2012).</li><li>Girishkumar, G., McCloskey, B., Luntz, A. C., Swanson, S., Wilcke, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium-Air+Battery:+Promise+and+Challenges.">Lithium-Air Battery: Promise and Challenges.</a> J. Phys. Chem. Lett. 1, 2193-2203 (2010).</li><li>Lu, J., Amine, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+Research+Progress+on+Non-aqueous+Lithium-Air+Batteries+from+Argonne+National+Laboratory.">Recent Research Progress on Non-aqueous Lithium-Air Batteries from Argonne National Laboratory.</a> Energies. 6, 6016-6044 (2013).</li><li>Ding, N., 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=Influence+of+carbon+pore+size+on+the+discharge+capacity+of+Li-O2+batteries.">Influence of carbon pore size on the discharge capacity of Li-O2 batteries.</a> J. Mater. Chem. A. 2, 12433 (2014).</li><li>Nimon, V. Y., Visco, S. J., De Jonghe, L. C., Volfkovich, Y. M., Bograchev, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+and+Experimental+Study+of+Porous+Carbon+Cathodes+in+Li-O2+Cells+with+Non-Aqueous+Electrolyte.">Modeling and Experimental Study of Porous Carbon Cathodes in Li-O2 Cells with Non-Aqueous Electrolyte.</a> ECS Electrochem. Lett. 2, 33-35 (2013).</li><li>Ottakam Thotiyl, M. M., Freunberger, S. A., Peng, Z., Bruce, P. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Carbon+Electrode+in+Nonaqueous+Li-O2+Cells.">The Carbon Electrode in Nonaqueous Li-O2 Cells.</a> J. Am. Chem. Soc. 135, 494-500 (2012).</li><li>Park, J. -. B., Lee, J., Yoon, C. S., Sun, Y. -. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ordered+Mesoporous+Carbon+Electrodes+for+Li-O2+Batteries.">Ordered Mesoporous Carbon Electrodes for Li-O2 Batteries.</a> Acs Appl. Mater. Interfaces. 5, 13426-13431 (2013).</li><li>Lei, 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=Synthesis+of+porous+carbon+supported+palladium+nanoparticle+catalysts+by+atomic+layer+deposition:+application+for+rechargeable+lithium-O2+battery.">Synthesis of porous carbon supported palladium nanoparticle catalysts by atomic layer deposition: application for rechargeable lithium-O2 battery.</a> Nano Lett. 13, 4182-4189 (2013).</li><li>Lu, J., 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=Effect+of+the+size-selective+silver+clusters+on+lithium+peroxide+morphology+in+lithium-oxygen+batteries.">Effect of the size-selective silver clusters on lithium peroxide morphology in lithium-oxygen batteries.</a> Nat. Commun. 5, 4895 (2014).</li><li>Lu, J., 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+nanostructured+cathode+architecture+for+low+charge+overpotential+in+lithium-oxygen+batteries.">A nanostructured cathode architecture for low charge overpotential in lithium-oxygen batteries.</a> Nat. Commun. 4, 2383 (2013).</li><li>Lu, J., 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=Synthesis+and+characterization+of+uniformly+dispersed+Fe3O4/Fe+nanocomposite+on+porous+carbon:+application+for+rechargeable+Li-O2+batteries.">Synthesis and characterization of uniformly dispersed Fe3O4/Fe nanocomposite on porous carbon: application for rechargeable Li-O2 batteries.</a> RSC Adv. 3, 8276-8285 (2013).</li><li>Luo, 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=Pd+nanoparticles+on+ZnO-passivated+porous+carbon+by+atomic+layer+deposition:+an+effective+electrochemical+catalyst+for+Li-O2+battery.">Pd nanoparticles on ZnO-passivated porous carbon by atomic layer deposition: an effective electrochemical catalyst for Li-O2 battery.</a> Nanotechnology. 26, 164003 (2015).</li><li>Freunberger, S. A., 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=The+Lithium-Oxygen+Battery+with+Ether-Based+Electrolytes.">The Lithium-Oxygen Battery with Ether-Based Electrolytes.</a> Angew. Chem. Int. Ed. 50, 8609-8613 (2011).</li><li>Laoire, C. O., Mukerjee, S., Abraham, K. M., Plichta, E. J., Hendrickson, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+Nonaqueous+Solvents+on+the+Electrochemistry+of+Oxygen+in+the+Rechargeable+Lithium-Air+Battery.">Influence of Nonaqueous Solvents on the Electrochemistry of Oxygen in the Rechargeable Lithium-Air Battery.</a> J. Phys. Chem. C. 114, 9178-9186 (2010).</li><li>McCloskey, B. D., Bethune, D. S., Shelby, R. M., Girishkumar, G., Luntz, A. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvents'+Critical+Rope+in+Nonaqueous+Lithium-Oxygen+Battery+Electrochemistry.">Solvents' Critical Rope in Nonaqueous Lithium-Oxygen Battery Electrochemistry.</a> J. Phys. Chem. Lett. 2, 1161-1166 (2011).</li><li>Assary, R. S., 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=Molecular-Level+Insights+into+the+Reactivity+of+Siloxane-Based+Electrolytes+at+a+Lithium-Metal+Anode.">Molecular-Level Insights into the Reactivity of Siloxane-Based Electrolytes at a Lithium-Metal Anode.</a> ChemPhysChem. 15, 2077-2083 (2014).</li><li>Du, P., 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=Compatibility+of+lithium+salts+with+solvent+of+the+non-aqueous+electrolyte+in+Li-O2+batteries.">Compatibility of lithium salts with solvent of the non-aqueous electrolyte in Li-O2 batteries.</a> Phys. Chem. Chem. Phys. 15, 5572-5581 (2013).</li><li>Aleshin, G. 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=Protected+anodes+for+lithium-air+batteries.">Protected anodes for lithium-air batteries.</a> Solid State Ion. 184, 62-64 (2011).</li><li>Assary, R. S., 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=The+Effect+of+Oxygen+Crossover+on+the+Anode+of+a+Li-O2+Battery+using+an+Ether-Based+Solvent:+Insights+from+Experimental+and+Computational+Studies.">The Effect of Oxygen Crossover on the Anode of a Li-O2 Battery using an Ether-Based Solvent: Insights from Experimental and Computational Studies.</a> ChemSusChem. 6, 51-55 (2013).</li><li>Aurbach, D., Zinigrad, E., Cohen, Y., Teller, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+short+review+of+failure+mechanisms+of+lithium+metal+and+lithiated+graphite+anodes+in+liquid+electrolyte+solutions.">A short review of failure mechanisms of lithium metal and lithiated graphite anodes in liquid electrolyte solutions.</a> Solid State Ion. 148, 405-416 (2002).</li><li>Dey, A. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+Anode+Film+And+Organic+And+Inorganic+Electrolyte+Batteries.">Lithium Anode Film And Organic And Inorganic Electrolyte Batteries.</a> Thin Solid Films. 43, 131-171 (1977).</li><li>Lau, K. C., Lu, J., Luo, X., Curtiss, L. A., Amine, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Implications+of+the+Unpaired+Spins+in+Li-O2+Battery+Chemistry+and+Electrochemistry:+A+Minireview.">Implications of the Unpaired Spins in Li-O2 Battery Chemistry and Electrochemistry: A Minireview.</a> ChemPlusChem. 80, 336-343 (2015).</li><li>Lau, K. C., 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=Theoretical+Exploration+of+Various+Lithium+Peroxide+Crystal+Structures+in+a+Li-Air+Battery.">Theoretical Exploration of Various Lithium Peroxide Crystal Structures in a Li-Air Battery.</a> Energies. 8, 529-548 (2015).</li><li>Black, R., 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=Screening+for+Superoxide+Reactivity+in+Li-O2+Batteries:+Effect+on+Li2O2/LiOH+Crystallization.">Screening for Superoxide Reactivity in Li-O2 Batteries: Effect on Li2O2/LiOH Crystallization.</a> J. Am. Chem. Soc. 134, 2902-2905 (2012).</li><li>Gallant, B. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+Li2O2+morphology+on+oxygen+reduction+and+evolution+kinetics+in+Li-O2+batteries.">Influence of Li2O2 morphology on oxygen reduction and evolution kinetics in Li-O2 batteries.</a> Energy Environ. Sci. 6, 2518-2528 (2013).</li><li>Lu, J., 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=Magnetism+in+Lithium-Oxygen+Discharge+Product.">Magnetism in Lithium-Oxygen Discharge Product.</a> ChemSusChem. 6, 1196-1202 (2013).</li><li>Xu, J. -. J., Wang, Z. -. L., Xu, D., Zhang, L. -. L., Zhang, X. -. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tailoring+deposition+and+morphology+of+discharge+products+towards+high-rate+and+long-life+lithium-oxygen+batteries.">Tailoring deposition and morphology of discharge products towards high-rate and long-life lithium-oxygen batteries.</a> Nat. Commun. 4, 2438 (2013).</li><li>Zhong, L., 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=In+Situ+Transmission+Electron+Microscopy+Observations+of+Electrochemical+Oxidation+of+Li2O2.">In Situ Transmission Electron Microscopy Observations of Electrochemical Oxidation of Li2O2.</a> Nano Lett. 13, 2209-2214 (2013).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Hitachi S-4700 SEM Training &amp; Reference Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> SEM Hitachi S4700 User Manual. , (2015).</li><li>Goldstein, J., 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> Scanning Electron Microscopy and X-ray Microanalysis. , (2003).</li><li>. X-Ray Photoelectron Spectrometer Operation Procedure Available from: <a target="_blank" href="https://nanofabrication.4dlabs.ca">https://nanofabrication.4dlabs.ca</a> (2015)</li><li>Haasch, R. T., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 93-132 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> JEM-2100F Field Emission Transmission Electron Microscope. , (2015).</li><li>Wen, J. -. G., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 189-229 (2014).</li><li>Williams, D. B., Carter, C. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Transmission Electron Microscopy. , (2009).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 11-ID-C: High-energy Diffraction Beamline. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 11-ID-D: Sector 11 - Time Resolved X-ray Spectroscopy and Scattering. , (2015).</li><li>Sardela, M. R., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 1-41 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 9-BM-B,C: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 20-BM-B: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>Bunker, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy. , (2010).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet FT-IR User's Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet iS5 User Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw inVia Raman Microscope Training Notebook. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw InVia Quick Operation Summary. , (2015).</li><li>Mitchell, R. R., Gallant, B. M., Thompson, C. V., Shao-Horn, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=All-carbon-nanofiber+electrodes+for+high-energy+rechargeable+Li-O2+batteries.">All-carbon-nanofiber electrodes for high-energy rechargeable Li-O2 batteries.</a> Energy Environ. Sci. 4, 2952-2958 (2011).</li></ol>

The authors have nothing to disclose.

考虑锂的 O 2的电池系统的空气的敏感性，特别是CO 2和水分，大量的在协议的步骤，以减少干扰物和避免副反应是必要的。例如，洛克式电池在充满氩气与O 2的&lt;0.5ppm的和H 2 O &lt;0.5ppm的手套箱组装;和所有的阴极材料，电解质溶剂和盐，玻璃纤维，洛克的部件，在玻璃室组装前干燥以减少水分污染。阳极端是一个不锈钢棒，以避免锂金属和O 2之间?...

1996年，亚伯拉罕和江1报告的第一个可逆的非水性锂O 2的电池由多孔碳阴极，有机电解质和锂金属阳极。自那时以来，由于其极高的理论能量密度超过任何其他现有的能量存储系统中，锂O 2电池，其诱导在阳极上的电流流动通过锂的氧化和氧的在阴极的还原（整体反应力+ + O 2 + E - ↔李2 O 2），最近收到显著的兴趣1-8。 下列要求的负极材料，将能够满足的李-O高性能需求2电池:（1）快速氧气扩散; （2）良好的电气和离子导电性; （3）高比表面积和（4）的稳定性。两个阴极的表面积和孔隙率的临界。李-O 2电池电化学性能9-12的多孔结构允许从锂阳离子与O 2反应产生的固体排放产品的沉积;和更大的表面积提供更多的活性位点，以适应电粒子加速电化学反应。例如电催化剂是由特定的沉积方法，其提供到基底和催化剂颗粒的良好控制附着力强，与基板的原始多孔表面结构的保存加到阴极材料13-17所制备的材料进行测试在世伟洛克型细胞作为非质子锂O 2电池的阴极。然而，电池的性能不仅取决于阴极材料的性质，而且还对非质子电解质18-22和锂金属阳极的类型。23-26更多影响包括的量和材料的浓度和p在充电/放电测试中使用rocedure。适当的条件和协议将优化和改进电池材料的整体性能。 除了 ​​电化学测试的结果，电池的性能还可以通过表征原始材料和反应产物进行评价。27-33扫描电子显微镜（SEM）被用来研究在阴极材料和形态的表面微观结构放电产物的演变。透射电子显微镜（TEM），X射线近边结构（XANES）吸收，和X射线光电子能谱（XPS）可以被用来确定超微结构，化学状态，和元件的组成部分，特别是对于那些催化剂纳米颗粒。高能量X射线衍射（XRD）用于直接识别该结晶放电产物。可能的电解质的分解可以通过衰减全反射傅立叶变换确定红外（ATR-FTIR）和拉曼光谱。 本文是演示的非质子锂O 2电池的常规试验，包括准备电池材料及配件，电化学性能测试和表征质朴的材料和反应产物的系统和有效的安排的协议。详细的视频协议是为了帮助在该领域从业者的新避免与李-O 2电池的性能测试和表征相关的许多常见的陷阱。

<table><tbody><tr><td>1-Methyl-2-pyrrolidinone (NMP), 99.5%</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>Battery test system</td><td>MACCOR</td><td>Series 4000 Automated Test System</td><td></td></tr><tr><td>Dimethyl carbonate (DMC), &amp;ge;99%</td><td>Sigma-Aldrich</td><td>517127</td><td></td></tr><tr><td>Ethyl alcohol, &amp;ge;99.5%</td><td>Sigma-Aldrich</td><td>459844</td><td></td></tr><tr><td>Formaldehyde solution, 37 wt. % in H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>252549</td><td></td></tr><tr><td>Graphitized Carbon black, &gt;99.95%</td><td>Sigma-Aldrich</td><td>699632</td><td></td></tr><tr><td>Iron(III) chloride (FeCl&lt;sub&gt;3&lt;/sub&gt;), 97%</td><td>Sigma-Aldrich</td><td>157740</td><td></td></tr><tr><td>Kapton polyimide tubing</td><td>Cole-Parmer</td><td>EW-95820-09</td><td></td></tr><tr><td>Kapton polymide tape</td><td>Cole-Parmer</td><td>EW-08277-80</td><td></td></tr><tr><td>Kapton window film</td><td>SPEX Sample Prep</td><td>3511</td><td></td></tr><tr><td>Lithium Chip (99.9% Lithium)</td><td>MTI Corporation</td><td>EQ-Lib-LiC25</td><td></td></tr><tr><td>Lithium trifluoromethanesulfonate (LiCF&lt;sub&gt;3&lt;/sub&gt;SO&lt;sub&gt;3&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>481548</td><td></td></tr><tr><td>Palladium hexafluoroacetylacetonate (Pd(hfac)&lt;sub&gt;2&lt;/sub&gt;), 99.9%</td><td>Aldrich</td><td>401471</td><td></td></tr><tr><td>Poly(vinylidene fluoride) (PVDF)</td><td>Aldrich</td><td>182702</td><td></td></tr><tr><td>Potassium permanganate (KMnO&lt;sub&gt;4&lt;/sub&gt;), &amp;ge;99.0%&amp;nbsp;</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Sodium hydroxide (NaOH), &amp;ge;97.0%</td><td>Sigma-Aldrich</td><td>221465</td><td></td></tr><tr><td>Tetraethylene glycol dimethyl ether (TEGDME), &amp;ge;99%</td><td>Aldrich</td><td>172405</td><td></td></tr><tr><td>Toray 030 carbon paper</td><td>ElectroChem Inc.</td><td>590637</td><td></td></tr></tbody></table>

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.

图1a所示为锂O 2的电池测试的世伟洛克型格的设置。一块锂膜的阳极端被放置在一个不锈钢棒。多孔阴极通过铝管是开放的纯O 2。玻璃纤维被用作隔板和非质子电解质的吸收;和Al-网格被用作集电体。整个洛克型电池被密封在填充有超高纯度氧的玻璃室中。在深入研究中，多个表征方法被施加到检查的电池系统，包括所制备的电极材料和反应产...

Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

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 ...

protocol-electrochemical-test-characterization-aprotic-li-o2

Universidad San Sebastian

Research

JoVE Journal

Engineering

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

11.4K 次观看.  Argonne National Laboratory. 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. 

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

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

钮扣电池锂离子电池的建设和测试

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

科研

工程学

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

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

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

正极材料的同步辐射技术锂离子和钠离子电池表征

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

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

电池的使用同步为基础的硬X射线微断层故障分析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

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

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

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

锂离子纽扣电池的非水电极加工和施工

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

A Protocol for Electrochemical Evaluations and State of Charge Diagnostics of a Symmetric Organic Redox Flow Battery

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid and deployment of renewable energy technologies. Among the many flow battery chemistries, non-aqueous flow batteries have the potential to achieve high energy density because of the broad voltage windows of non-aqueous electrolytes. However, significant technical hurdles exist currently limiting non-aqueous flow batteries to demonstrate their full potential, such as low redox concentrations, low operating currents, under-explored battery status monitoring, etc. In an attempt to address these limitations, we recently reported a non-aqueous flow battery based on a highly soluble, redox-active organic nitronyl nitroxide radical compound, 2-phenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (PTIO). This redox material exhibits an ambipolar electrochemical property, and therefore can serve as both anolyte and catholyte redox materials to form a symmetric flow battery chemistry. Moreover, we demonstrated that Fourier transform infrared (FTIR) spectroscopy could measure the PTIO concentrations during the PTIO flow battery cycling and offer reasonably accurate detection of the battery state of charge (SOC), as cross-validated by electron spin resonance (ESR) measurements. Herein we present a video protocol for the electrochemical evaluation and SOC diagnosis of the PTIO symmetric flow battery. With a detailed description, we experimentally demonstrated the route to achieve such purposes. This protocol aims to spark more interests and insights on the safety and reliability in the field of non-aqueous redox flow batteries.

We present the protocols for electrochemically evaluating a symmetric non-aqueous organic redox flow battery and for diagnosing its state of charge using FTIR.

- 电化学评估和对称有机氧化还原液流电池的充电诊断状态协议

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid ...

化学

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 ...

The Effect of Charging and Discharging Lithium Iron Phosphate-graphite Cells at Different Temperatures on Degradation

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. The degradation of the cells is assessed by using 10 charging and discharging temperature permutations ranging from -20 &#176;C to 30 &#176;C. This allows an analysis of the effect of charge and discharge temperatures on aging, and their associations. A total of 100 charge/discharge cycles were carried out. Every 25 cycles a reference cycle was performed to assess the reversible and irreversible capacity degradation. A multi-factor analysis of variance was used, and the experimental results were fitted showing: i) a quadratic relationship between the rate of degradation and the temperature of charge, ii) a linear relationship with the temperature of discharge, and iii) a correlation between the temperature of charge and discharge. It was found that the temperature combination for charging at +30 &#176;C and discharging at -5 &#176;C led to the highest rate of degradation. On the other hand, the cycling in a temperature range from -20 &#176;C to 15 &#176;C (with various combinations of temperatures of charge and discharge), led to a much lower degradation. Additionally, when the temperature of charge is 15 &#176;C, it was found that the degradation rate is nondependent on the temperature of discharge.

This article describes the effect of dissimilar charging/discharging temperatures on the degradation of lithium iron phosphate-graphite pouch cells, aiming at simulating close to real case scenarios. In total, 10 temperature combinations are investigated in the range -20 to 30 &#176;C in order to analyze the impact of temperature on degradation.

不同温度下的磷酸铁锂-石墨电池充放电对降解的影响

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. ...

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 ...

电化学测试的协议及表征非质子锂的O

摘要

探索更多视频

此视频中的章节