Name: in situ lithiated reference electrode: four electrode design for in-operando impedance spectroscopy
Uploaded: 2018-09-12T14:00:00
Description: Watch this Scientific Journal Video about In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy at JoVE.com

作者承认美国能源部, 能源效率和可再生能源办公室的财政支持。

1. 剥铜/锡线
<ol><li>热商业获得剥离溶液。<ol>
<li>将商用工业级溶出液倒入不锈钢烧杯 (直径7.6 厘米, 高度8.5 厘米), 从底部到深度约5毫米。把烧杯放到热盘子上。开始加热速度约5°c/分钟。</li>
		<li>将便携式热电偶浸入溶液中, 密切监测溶液的温度坡道, 调整热板的加热速率以保持所需的加热速率。</li>
	</ol>
</li>
	<li>在准备参考线的夹具上设置铜/锡线。<ol>
<li>风一个粗铜线的形式的夹具 (4 厘米宽,...

<ol>
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V., 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=Quantifying+capacity+loss+due+to+solid-electrolyte-interphase+layer+formation+on+silicon+negative+electrodes+in+lithium-ion+batteries.">Quantifying capacity loss due to solid-electrolyte-interphase layer formation on silicon negative electrodes in lithium-ion batteries.</a> Journal of Power Sources. 215, 145-151 (2012).</li><li>Ender, M., Weber, A., Ellen, I. -. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Analysis+of+Three-Electrode+Setups+for+AC-Impedance+Measurements+on+Lithium-Ion+Cells+by+FEM+simulations.">Analysis of Three-Electrode Setups for AC-Impedance Measurements on Lithium-Ion Cells by FEM simulations.</a> Journal of The Electrochemical Society. 159 (2), A128-A136 (2011).</li><li>Zhou, J., Notten, P. H. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+Reliable+Lithium+Microreference+Electrodes+for+Long-Term+In+Situ+Studies+of+Lithium-Based+Battery+Systems.">Development of Reliable Lithium Microreference Electrodes for Long-Term In Situ Studies of Lithium-Based Battery Systems.</a> Journal of The Electrochemical Society. 151 (12), A2173-A2179 (2004).</li><li>Klink, S., H&#246;che, D., La Mantia, F., Schuhmann, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=FEM+modelling+of+a+coaxial+three-electrode+test+cell+for+electrochemical+impedance+spectroscopy+in+lithium+ion+batteries.">FEM modelling of a coaxial three-electrode test cell for electrochemical impedance spectroscopy in lithium ion batteries.</a> Journal of Power Sources. 240 (Supplement C), 273-280 (2013).</li><li>B&#252;nzli, C., Kaiser, H., Nov&#225;k, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Important+Aspects+for+Reliable+Electrochemical+Impedance+Spectroscopy+Measurements+of+Li-Ion+Battery+Electrodes.">Important Aspects for Reliable Electrochemical Impedance Spectroscopy Measurements of Li-Ion Battery Electrodes.</a> Journal of The Electrochemical Society. 162 (1), A218-A222 (2015).</li><li>Delacourt, C., Ridgway, P. 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D., Deshazer, H. D., Cui, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reliable+reference+electrodes+for+lithium-ion+batteries.">Reliable reference electrodes for lithium-ion batteries.</a> Electrochemistry Communications. 31 (Supplement C), 141-144 (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 Ionics. 148 (3), 405-416 (2002).</li><li>Klett, 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=Electrode+Behavior+RE-Visited:+Monitoring+Potential+Windows,+Capacity+Loss,+and+Impedance+Changes+in+Li1.03(Ni0.5Co0.2Mn0.3)0.97O2/Silicon-Graphite+Full+Cells.">Electrode Behavior RE-Visited: Monitoring Potential Windows, Capacity Loss, and Impedance Changes in Li1.03(Ni0.5Co0.2Mn0.3)0.97O2/Silicon-Graphite Full Cells.</a> Journal of The Electrochemical Society. 163 (6), A875-A887 (2016).</li><li>Zhang, W. -. 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+review+of+the+electrochemical+performance+of+alloy+anodes+for+lithium-ion+batteries.">A review of the electrochemical performance of alloy anodes for lithium-ion batteries.</a> Journal of Power Sources. 196 (1), 13-24 (2011).</li><li>Klett, M., Gilbert, J. A., Pupek, K. Z., Trask, S. E., Abraham, D. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Layered+Oxide,+Graphite+and+Silicon-Graphite+Electrodes+for+Lithium-Ion+Cells:+Effect+of+Electrolyte+Composition+and+Cycling+Windows.">Layered Oxide, Graphite and Silicon-Graphite Electrodes for Lithium-Ion Cells: Effect of Electrolyte Composition and Cycling Windows.</a> Journal of The Electrochemical Society. 164 (1), A6095-A6102 (2017).</li><li>Ma, 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=A+Guide+to+Ethylene+Carbonate-Free+Electrolyte+Making+for+Li-Ion+Cells.">A Guide to Ethylene Carbonate-Free Electrolyte Making for Li-Ion Cells.</a> Journal of The Electrochemical Society. 164 (1), A5008-A5018 (2017).</li><li>Michan, A. 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=Fluoroethylene+Carbonate+and+Vinylene+Carbonate+Reduction:+Understanding+Lithium-Ion+Battery+Electrolyte+Additives+and+Solid+Electrolyte+Interphase+Formation.">Fluoroethylene Carbonate and Vinylene Carbonate Reduction: Understanding Lithium-Ion Battery Electrolyte Additives and Solid Electrolyte Interphase Formation.</a> Chemistry of Materials. 28 (22), 8149-8159 (2016).</li><li>Rahmoun, A., Loske, M., Rosin, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+the+Impedance+of+Lithium-ion+Batteries+Using+Methods+of+Digital+Signal+Processing.">Determination of the Impedance of Lithium-ion Batteries Using Methods of Digital Signal Processing.</a> Energy Procedia. 46, 204-213 (2014).</li><li>Jiang, 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=Electrochemical+Impedance+Spectra+for+Lithium-ion+Battery+Ageing+Considering+the+Rate+of+Discharge+Ability.">Electrochemical Impedance Spectra for Lithium-ion Battery Ageing Considering the Rate of Discharge Ability.</a> Energy Procedia. 105, 844-849 (2017).</li><li>Andre, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+high-power+lithium-ion+batteries+by+electrochemical+impedance+spectroscopy.+I.+Experimental+investigation.">Characterization of high-power lithium-ion batteries by electrochemical impedance spectroscopy. I. Experimental investigation.</a> Journal of Power Sources. 196 (12), 5334-5341 (2011).</li><li>Li, S. E., Wang, B., Peng, H., Hu, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+electrochemistry-based+impedance+model+for+lithium-ion+batteries.">An electrochemistry-based impedance model for lithium-ion batteries.</a> Journal of Power Sources. 258, 9-18 (2014).</li></ol>

图 2a是全电池的电压剖面图 2b和2c显示对应于正负电极与锂/锂+情侣的电压剖面, 而整个细胞在3和 4.4 v 之间循环。可以看出, 当全细胞扫描在3和 4.4 v 之间时, 正极电极会经历3.65 伏和 4.45 v 之间的电压, 而负极与 0.65 v 和 0.05 v 之间的负电极和李/李分别。在充电过程中, lithiation 和负电极 (与锂/锂+) 的正向...

锂离子电池对高能密度的需求正在推动研究, 以了解限制锂离子电池性能1的基本因素。含有新一代层状过渡金属氧化物阴极、石墨阳极和有机碳酸盐电解质的细胞的高压运行与几种寄生反应2、3有关。其中一些反应消耗了锂离子库存, 并且经常导致细胞4、5、6、7的显著阻抗上升。锂离子的损耗也导致电极表面电位的净转移。在3电极电池设计8、9、10、11中, 对一个完整细胞与参考电极 (RE) 中单个电极的电压变化进行监测。,12,13,14. 有关电压剖面的信息和单个电极上的阻抗变化促进了对 LIB 基本退化机制的更深的理解。传统的3电极电池含有锂金属作为参考电极, 这有助于对每个电极的电化学过程有一个明确的理解。与有机电解质接触的锂金属经过自发的表面改性, 该表面层对 li 的贡献不能量化15。一些3电极的配置, 如 (a) T 模型, (b) 一个微重新定位同工作和反电极的同轴, (c) 有一个硬币电池在反电极背面,等已经提出了前面。这些细胞配置中的大部分都是从细胞夹层中重新定位的, 由于电解质的电导率低, 导致阻抗数据的显著漂移。事实证明, 在整个测量过程中, 一个具有稳定电位的 RE 必须驻扎在三明治的中心, 以确保可靠的阻抗数据。
为了解决这些差异, 我们设计了一个包含第四重16的单元格设置。一个超薄的锡镀铜丝夹在电池电极之间, 可以在原位电化学锂化, 形成锂x锡合金。当 Sn 经历 lithiation 时, 参考导线的电压下降, 而一个完全锂化的导线有可能接近 0 V vs。李/李17。锂化组合物具有与锂金属相媲美的潜力, 亚稳态合金在测量的时间段内有利于稳定电位。暴露于电解质中的锂金属易被电解质分解产物形成表面层。通过在电极和锂金属参考之间收集光谱来探测单个电极的阻抗的 EIS 测量由于这些层对阻抗的贡献而不可靠。虽然电解质还原在锂锡表面也不可避免, 但原位锂化参考线具有以下优点: (a) 没有恒定的电解质分解产物, 因为电压总是高于分解电位电解质, 除非锂化, 意味着没有损失的李库存在系统到界面层;(b) 在 Sn 线 lithiation 期间形成的层数在很小的范围内, 对 EIS 数据提供了微不足道的贡献;(c) 由于 Sn 线失去 Li 和导线的电位增加, 形成的产品降解, 导致在每 lithiation 的 lithiation 的新鲜锡线, 从而形成非常薄的界面层, 而不是增加厚度的这些层。以这些合金为参考记录的光谱提供了更准确可靠的电极阻抗数据。我们进行了标准的2032型硬币电池和4电极再电池测试, 以验证我们的设计。这些测试的结果和我们对数据的解释将被用来作为一个代表性的结果来解释我们的协议的有效性。3 - 4 . 4 V 自行车跟随了标准协议 , 包括形成周期、老化周期和周期流阻抗测量在自行车赛期间。硬币细胞测量提供了有关参数的宝贵信息, 如循环寿命, 容量保留, 交流阻抗变化等. 重细胞使监测电压变化和阻抗上升的个别电极。我们对容量衰减和阻抗上升的机械理解可以为电解质系统的发展提供指导, 并了解高压电池运行过程中每个电极的容量损失贡献。
我们的细胞包含Li 1.03 (镍0.5Co0.2锰0.3)0.97O2 (这里被表示作为 NMC532) 基正极, 石墨基负极 (这里被表示为 Gr) 和 1.2 M 解答 LiPF6在 Fluoroethylene 碳酸盐 (FEC): 乙基甲基碳酸酯 (EMC) (5:95 瓦特/瓦) 作为电解质。本研究中使用的电极是阿贡国家实验室的细胞分析、建模和原型 (阵营) 设施中制作的标准电极。正极电极由 NMC532、导电碳添加剂 (C-45) 和聚偏氟乙烯 (PVdF) 粘合剂组成, 重量比为 90:5: 5 在20µm 厚铝电流收集器上。负电极由石墨组成, 与 C-45 混合, 而 PVdF 粘结剂的重量比为 92:2: 6 在10µm 厚铜电流收集器上。从电极层压板上打了5.08 厘米直径的圆盘, 在7.62 厘米内径的夹具上用7.62 厘米的模具打孔。这些电极干燥在120°c 和分离器在75°c 在一个真空烤箱至少 12 h 在细胞汇编之前。夹具设计的示意图表示在图 1中。大的固定装置和电极确保了每单位面积的电流分布的最小不均匀性, 从而提供了阻抗谱中最小的失真。3-4. 4 V 循环遵循一个标准协议, 其中包括两个形成周期的 C/20 率, 100 老化周期以 C/3 率和两个诊断周期在 C/20。所有电池测试均在摄氏30摄氏度进行。用电池循环仪测量电化学循环数据, 利用恒电位仪系统进行电化学阻抗谱 (EIS)。

<table border="0" cellpadding="0" cellspacing="0" width="645">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Insulstrip 220</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td style="width:119px;">081607-1</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Sodium Hydroxide (23 wt%)</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td>1310-73-2</td>
			<td>Contents of Insulstrip 220</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Furfuryl Alcohol (10 wt%)</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td style="width:119px;">98-00-0</td>
			<td>Contents of Insulstrip 220</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">NCM523</td>
			<td>TODA America</td>
			<td style="width:119px;">NM4100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">C-45&#160;</td>
			<td>Timcal Inc.</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">polyvinylidene fluoride (PVdF)</td>
			<td>Sigma Aldrich</td>
			<td style="width:119px;">427152</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sn over Cu wire</td>
			<td style="width:143px;">Kanthal</td>
			<td style="width:119px;">MELT # 24633</td>
			<td>Custom ordered</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Battery cycler</td>
			<td style="width:143px;">Maccor USA</td>
			<td style="width:119px;">Series 2300&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Potentiostat</td>
			<td style="width:143px;">Solartron Analytical</td>
			<td style="width:119px;">1470 E</td>
			<td></td>
		</tr>
	</tbody>
</table>

in situ lithiated reference electrode: four electrode design for in-operando impedance spectroscopy

延长锂离子电池的工作电压会导致这些器件产生更高的能量输出。但是, 高电压可能会触发或加速多个过程, 导致长期性能衰减。考虑到在细胞内发生的物理过程的复杂性, 要充分理解这种性能退化的根本原因, 通常是有挑战性的。这一困难的部分原因是, 电池的任何电化学测量都将返回单元格中所有元件的组合贡献。加入参考电极可以解决问题的一部分, 因为它允许阴极和阳极的电化学反应被单独探测。例如, 阴极所经历的电压范围的变化可以指示全细胞内 cyclable 锂离子池的改变。通过测量每个电极对整体细胞阻抗的贡献, 也可以监测电池中存在的许多 interphases 的结构演化。这种丰富的信息放大了锂离子电池的诊断分析的范围, 为单个细胞组件的优化提供了宝贵的投入。在这项工作中, 我们介绍了能够容纳多个参考电极的测试单元的设计, 并提出了适用于每种特定测量类型的参考电极, 详细说明了装配过程, 以便最大限度地提高实验结果。

图 2是 LiPF6 (FEC) 中的单个电极的电压的典型描述: EMC (5:95 瓦特/瓦) 作为第一和第二个周期中的电解质。图 3显示了在三形成周期和周期寿命老化协议结束后细胞的 EIS 谱。在精确跟踪单个电极的阻抗变化时, 重新 lithiate 以获得 EIS 数据的能力。
<img alt="Figure 1" class="xfigimg" src="/...

Watch this Scientific Journal Video about In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy at JoVE.com

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

锂离子电池中的参考电极的加入, 为阐明高电压下的降解机理提供了有价值的信息。在本文中, 我们提出了一个单元设计, 可容纳多个参考电极, 连同组装步骤, 以确保最大的准确性, 获得的电化学测量数据。

原位锂化参考电极: 四原位阻抗谱的电极设计

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Research

JoVE Journal

Chemistry

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

在质谱选择离子软着陆准备好定义的表面原位二次离子质谱和红外光谱

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科研

化学

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

掺硼金刚石电极质量和应用，以评估<em&gt;原位</em&gt;本地pH值通过水电改造

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X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

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The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

电化学阻抗谱作为电化学速率常数估计的一种工具

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

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用于原位晶体 x 射线衍射和原位的微流控芯片系列晶体学的动态光散射

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Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

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原位金纳米粒子合成快速 Nanoprobe 信号增强

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

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一种用于分析单纳米粒子的闭式无线纳米粒子电极

Measuring the intrinsic features of single nanoparticles by nanoelectrochemistry holds deep fundamental importance and has potential impacts in ...

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

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In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids ...

Characterizing Lewis Pairs Using Titration Coupled with In Situ Infrared Spectroscopy

使用滴定与原位红外光谱相结合，对刘易斯对进行特征化

Lewis acid-activation of carbonyl-containing substrates is a fundamental basis for facilitating transformations in organic chemistry. Historically, ...

Covalent Attachment of Single Molecules for AFM-based Force Spectroscopy

基于AFM的力光谱单分子共价附价

Atomic force microscopy (AFM)-based single molecule force spectroscopy is an ideal tool for investigating the interactions between a single polymer and ...