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>

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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 border="0" cellpadding="0" cellspacing="0" width="830">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">1-Methyl-2-pyrrolidinone (NMP), 99.5%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">328634</td>
			<td style="width:63px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Battery test system</td>
			<td style="width:160px;">MACCOR</td>
			<td colspan="2">Series 4000 Automated Test System</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Dimethyl carbonate (DMC), &#8805;99%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">517127</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Ethyl alcohol, &#8805;99.5%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">459844</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Formaldehyde solution, 37 wt. % in H2O</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">252549</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Graphitized Carbon black, &#62;99.95%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">699632</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Iron(III) chloride (FeCl3), 97%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">157740</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Kapton polyimide tubing</td>
			<td style="width:160px;">Cole-Parmer</td>
			<td>EW-95820-09</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Kapton polymide tape</td>
			<td style="width:160px;">Cole-Parmer</td>
			<td>EW-08277-80</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Kapton window film</td>
			<td style="width:160px;">SPEX Sample Prep</td>
			<td style="width:219px;">3511</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Lithium Chip (99.9% Lithium)</td>
			<td style="width:160px;">MTI Corporation</td>
			<td style="width:219px;">EQ-Lib-LiC25</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Lithium trifluoromethanesulfonate (LiCF3SO3)</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">481548</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Palladium hexafluoroacetylacetonate (Pd(hfac)2), 99.9%</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">401471</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Poly(vinylidene fluoride) (PVDF)</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">182702</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Potassium permanganate (KMnO4), &#8805;99.0%&#160;</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">223468</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Sodium hydroxide (NaOH), &#8805;97.0%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">221465</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Tetraethylene glycol dimethyl ether (TEGDME), &#8805;99%</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">172405</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">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

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

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

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

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

接枝共聚物固态电解质的锂离子电池的应用

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

科研

工程学

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

在固体氧化物燃料电池电极表面的探测和测绘

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Fabrication of VB2/Air Cells for Electrochemical Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for synthesizing nanoscopic VB2 is presented as well as step-by-step procedure for applying a zirconium oxide coating to the VB2 particles for stabilization upon discharge. The process for disassembling existing zinc/air cells is shown, in addition construction of the new working electrode to replace the conventional zinc/air cell anode with a the nanoscopic VB2 anode. Finally, discharge of the completed VB2/air battery is reported. We show that using the zinc/air cell as a test bed is useful to provide a consistent configuration to study the performance of the high-energy high capacity nanoscopic VB2 anode.

Fabrication of VB2/Air Cells for Electrochemical Testing

A protocol is presented to study multi-electron metal/air battery systems by using previous technology developed for the zinc/air cell. Electrochemical testing is then performed on fabricated batteries to evaluate performance.

VB制作<sub&gt; 2</sub&gt; /空气电池电化学测试

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for ...

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. ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

烧蚀材料在试验过程中等离子体发生器发射光谱边界层研究

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

Fabrication and Characterization of Superconducting Resonators

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors (MKIDs) for the detection of faint astrophysical signatures, as well as for quantum computing applications and materials characterization. In this paper, procedures are presented for the fabrication and characterization of thin-film superconducting microwave resonators. The fabrication methodology allows for the realization of superconducting transmission-line resonators with features on both sides of an atomically smooth single-crystal silicon dielectric. This work describes the procedure for the installation of resonator devices into a cryogenic microwave testbed and for cool-down below the superconducting transition temperature. The set-up of the cryogenic microwave testbed allows one to do careful measurements of the complex microwave transmission of these resonator devices, enabling the extraction of the properties of the superconducting lines and dielectric substrate (e.g., internal quality factors, loss and kinetic inductance fractions), which are important for device design and performance.

Superconducting microwave resonators are of interest for detection of light, quantum computing applications and materials characterization. This work presents a detailed procedure for fabrication and characterization of superconducting microwave resonator scattering parameters.

制备与表征超导谐振器的

Superconducting microwave resonators are of interest for a wide range of applications, including for their use as microwave kinetic inductance detectors ...

Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. The results of studies in which the etching current and the molarity of the NaOH solution used in the etching process were varied are presented. The investigation of the geometry of the tips, by imaging them with a scanning electron microscope, and by operating them in field emission mode is also described. The field emission tips produced are intended to be used as an electron beam source for ion production via electron impact ionization of background gas or vapor in Penning trap mass spectrometry applications.

A method for electrochemically etching field emission tips is presented. Etching parameters are characterized and the operation of the tips in field emission mode is investigated.

电化学腐蚀和电子碰撞电离夏普场发射点的表征

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. ...

Fabrication of White Light-emitting Electrochemical Cells with Stable Emission from Exciplexes

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active layer which consists of blue-fluorescent poly(9,9-di-n-dodecylfluorenyl-2,7-diyl) (PFD) and &#960;-conjugated triphenylamine molecules. This white light emission originates from exciplexes formed between PFD and amines in electronically excited states. A device containing PFD, 4,4&#39;,4&#39;&#39;-tris[2-naphthyl(phenyl)amino]triphenylamine (2-TNATA), Poly(ethylene oxide) and K2CF3SO3 showed white light emission with Commission internationale de l&#39;&#233;clairage (CIE) coordinates of (0.33, 0.43) and a Color Rendering Index (CRI) of Ra = 73 at an applied voltage of 3.5 V. Constant voltage measurements showed that the CIE coordinates of (0.27, 0.37), Ra of 67, and the emission color observed immediately after application of a voltage of 5 V were nearly unchanged and stable after 300 sec.

The authors present a method for fabricating stable white-light-emitting electrochemical cells utilizing emission from exciplexes formed between a blue-emitting fluorene polymer and aromatic amines.

白的制造发光电化学细胞与来自激发络合物稳定的发射

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active ...

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 ...

Optimization, Test and Diagnostics of Miniaturized Hall Thrusters

Miniaturized spacecraft and satellites require smart, highly efficient and durable low-thrust thrusters, capable of extended, reliable operation without attendance and adjustment. Thermochemical thrusters which utilize thermodynamic properties of gases as a means of acceleration have physical limitations on their exhaust gas velocity, resulting in low efficiency. Moreover, these engines demonstrate extremely low efficiency at small thrusts and may be unsuitable for continuously operating systems which provide real-time adaptive control of the spacecraft orientation, velocity and position. In contrast, electric propulsion systems which use electromagnetic fields to accelerate ionized gases (i.e., plasmas) do not have any physical limitation in terms of exhaust velocity, allowing virtually any mass efficiency and specific impulse. Low-thrust Hall thrusters have a lifetime of several thousand hours. Their discharge voltage ranges between 100 and 300 V, operating at a nominal power of &lt;1 kW. They vary from 20 to 100 mm in size. Large Hall thrusters can provide fractions of millinewton of thrust. Over the past few decades, there has been an increasing interest in small mass, low power, and high efficiency propulsion systems to drive satellites of 50-200 kg. In this work, we will demonstrate how to build, test, and optimize a small (30 mm) Hall thruster capable of propelling a small satellite weighing about 50 kg. We will show the thruster operating in a large space environment simulator, and describe how thrust is measured and electric parameters, including plasma characteristics, are collected and processed to assess key thruster parameters. We will also demonstrate how the thruster is optimized to make it one of the most efficient small thrusters ever built. We will also address challenges and opportunities presented by new thruster materials.

Here, we present a protocol to test and optimize space propulsion systems based on miniaturized Hall-type thrusters.

小型化霍尔推进器的优化、测试和诊断

Miniaturized spacecraft and satellites require smart, highly efficient and durable low-thrust thrusters, capable of extended, reliable operation without ...