这项研究由美国海军研究办公室资助。

1. 制造Zn-海绵电极的乳液方法
<ol><li>在 100 mL 玻璃烧杯中加入 2.054 毫升的去离子水。</li>
	<li>在烧饼中加入 4.565 mL 的脱脂。</li>
	<li>搅拌0.1000±0.0003克硫酸钠（SDS），直到溶解。</li>
	<li>用手搅拌0.0050±0.0003克 水溶性 中粘性甲基纤维素（CMC）钠盐5分钟或直到CMC完全溶解。 注意:使用塑料或塑料涂层的搅拌工具。用金属表面的工具搅拌会对由此产生的 Zn 海绵产生不利影响。</li>
	<li>搅拌0.844±0.002克 水溶性 预膨胀的卡盒甲基纤维素树脂。 注:这种类型的水溶性树脂是昂贵的（420公斤=1）6。</li>
	<li>使用装有塑料桨的架空桨搅拌器，在 1，000 rpm 下搅拌该混合物 5 分钟。</li>
	<li>将 50 克 Zn 粉末（平均颗粒大小为 50 μm，含 307 ppm 的双糖和 307 ppm 的钛用于抑制腐蚀）倒入烧杯中，而头顶搅拌器继续以 1，000 rpm 的速度旋转。</li>
	<li>继续搅拌 Zn 糊以相同的速度再搅拌 5 分钟， 1，000 rpm 。</li>
	<li>停止搅拌器，取出烧嘴，在室温下将烧嘴及其内装物在真空中放置5分钟，使混合物过气。</li>
	<li>将 Zn 粘贴成聚丙烯模具（直径为 10 毫米，高度为 ±5 mm），并在露天过夜干燥。模具的形状决定了干燥糊的形式和由此产生的Zn海绵。 注:模具大小和形状可能有所不同。过去的实验5 成功使用直径接近10毫米的圆柱形模具。填充 Zn 粘贴，高度可达 5 mm 或更少。高度越短，所需的干燥时间越短。有关商用模具 的材料表 。。</li>
	<li>小心地从模具中取出干燥的 Zn 糊状物，并将其放入网状外壳中，该套管靠在5、6的氧化铝支架上。 注:例如，通过将穿孔黄铜板弯曲成直径略大于 Zn-海绵电极所需直径的圆柱体来制造网状外壳。弯曲成所需的形状后，用氮化物润滑剂喷洒穿孔金属板。</li>
	<li>将装配件放入管炉（直径为 67 毫米），并带有进出管子的气体端口。 注:使用一个端口（入口端口）将气体输送到炉子中。使用另一个（出口端口）将管炉中的气体排出到烟气罩中。</li>
	<li>将 N2 气体管道送入炉内 30 分钟，速度为 5.7 厘米[最小±1]， 以清除炉内空气。 注:第 1.13 步可以通过将 N2 气体罐与数字控制流量计连接到连接到其中一个入口端口的管子来实现。气体流量计可以手动控制或由计算机控制。</li>
	<li>在 30 分钟的清除后，将 N2 气体限制在 2.8 cm+ 最小+1 的恒定速率。</li>
	<li>将炉子在 68 分钟内将温度线性地从 20 升到 369 °C，在 369 °C 保持 5 小时，在 105 分钟内线性地从 369 °C 上升至 584 °C，然后关闭。</li>
	<li>启动炉子程序，而 N2 气体继续流动。</li>
	<li>手动停止N2气体流动后，5小时的温度保持和管道呼吸空气在2.8厘米+最小+1。 注:第 1.17 步可以通过将呼吸空气罐（不是合成空气）与数字控制流量计连接到连接到其他入口端口的管子来实现。</li>
	<li>加热程序停止后，让炉子冷却到室温，而无需主动冷却，但保持呼吸空气流动。</li>
	<li>取出冷却的 Zn 海绵，看到它们和/或将它们砂到所需的尺寸。 注:各种锯具可用于手持旋转锯或垂直带锯。磨蚀性或金刚石叶片是适当的。</li>
</ol>2. 一种基于船的制造Zn海绵电极的方法
<ol><li>在 100 毫升玻璃烧杯中加入 10.5 毫升的去离子水。</li>
	<li>搅拌0.120±0.001克 水溶性 高粘度纤维素胶，也称为卡盒甲基纤维素（CMC）钠盐。 注意:使用塑料或塑料涂层的搅拌工具。用金属表面的工具搅拌会对由此产生的 Zn 海绵产生不利影响。</li>
	<li>漩涡，用手搅拌5分钟或直到CMC溶解。</li>
	<li>搅拌2.400±0.001克玉米淀粉，同时再漩涡2分钟。</li>
	<li>搅拌 120.00 ± 0.01 克 Zn 粉末（平均颗粒大小为 50 μm，含有 307 ppm 的双糖和 307 ppm 的钛，用于抑制腐蚀），同时再涡流 2 分钟。</li>
	<li>将生成的 Zn 粘贴按入所需的模具腔中。 注:模具大小和形状可能有所不同。过去的实验6 成功使用直径接近10毫米的圆柱形模具。填充 Zn 粘贴，高度可达 50 mm 或更少。水性 Zn 糊比乳液 Zn 糊更干燥，因此水性版本可用于制作需要较少干燥时间的较大海绵。高度越短，所需的干燥时间越短。模具需要能够分成两半，因为与乳液 Zn 糊不同，在干燥后，作为液态 Zn 粘贴的最小收缩。无盐黄油可用于润滑模具，然后按压在无色 Zn 糊中，以帮助脱销。 图 1A 显示按照基于水的协议，用 Zn 糊包装的定制模具。 图1B 显示了手工制作的网状套管、带状氧化铝支架，以及由此产生的Zn海绵，使用基于 asous 的方法制造。</li>
	<li>让充满 Zn 糊的模具在 70 °C 的露天在熔炉中干燥过夜。</li>
	<li>遵循乳液方法中描述的相同处理和热处理步骤（1.11/1.19）。</li>
</ol>

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J.F.P.、D.R.R.和J.W.L.拥有与锌电极有关的专利:美国专利第9802254、10008711、10720635和10763500、欧盟专利无2926395、中国专利104813521。

与这些协议相关的修改和故障排除包括将新混合的 Zn 糊填充到模具腔中。应小心避免气囊。填充后或灌装时点击模具可减少不需要的空隙。由于水性 Zn 糊是干燥的，因此可以直接施加压力到 Zn 糊中，以在填充模具腔的同时推出气囊。
方法的一个局限性是Zn-海绵毛孔结构紊乱，但Zn和波源粒子大小可用于改变孔隙形态。使用添加剂制造可以制造出更有序、可能更坚固、更轻的...

报告的制造方法的目的是制造锌（Zn）海绵电极，抑制树突的形成和形状的变化。从历史上看，这些问题限制了Zn电池的循环寿命。锌海绵电极解决了这些问题，使Zn电池的循环寿命更长，1，2，3，4，5，6。海绵结构抑制树突的形成和形状的变化，因为（1） 融合的Zn框架电导海绵的整个体积:（2） 孔隙在Zn-海绵表面附近持有锌酸盐:和（3）海绵有一个高表面积，降低局部电流密度低于价值确定发芽树突在碱性电解质7。但是，如果海绵表面积过高，则会发生大量腐蚀。如果海绵毛孔太大，海绵的体积容量将很低。此外，如果海绵孔隙过小，Zn电极在放电过程中电解质将不足以进入Zn，导致功率和容量低5，6。
报告制造方法背后的理由是制造具有适当海绵孔隙和孔径的Zn海绵。实验中，我们发现Zn海绵的孔隙在50%到70%之间，孔径接近10μm的周期在全电池中，并显示低腐蚀率5。我们注意到，现有的商业金属泡沫制造方法未能在这些长度尺度8上达到类似的形态，因此需要报告的制造方法。
这里报告的方法比替代品的优势是，海绵特征的精细控制，并能够制造大型，密集的Zn海绵与技术相关的是容量值5，6，9，10。创建 Zn 泡沫的替代方法可能无法创建具有海绵孔隙接近 50% 的可比 10 μm 毛孔。然而，这种替代品可能需要更少的能量来制造，因为它们避免了高温处理步骤。替代过程包括以下策略:冷烧结Zn粒子11，将Zn沉积在三维宿主结构12，13，14，15，16，17，切割Zn箔成二维泡沫18，并通过脊柱分解19或渗透溶解20产生Zn泡沫。
所报告的方法在更广泛的出版的文献中是主要由钻头等人的作品建立的。他们采用了制造多孔陶瓷的方法，为电池制造了最早报道的三维（尽管很脆弱）Zn泡沫之一。然而，这些作者未能证明可充电性，可能是因为Zn粒子之间的连接性差。在可充电的 Zn-海绵电极之前，Zn 箔电极的最佳替代品是 Zn 粉末电极，其中 Zn 粉末与凝胶电解质混合。锌粉电极在原石碱性电池（Zn-MnO2）中用于商业用途，但充电性差，因为Zn粒子由Zn氧化物（ZnO）钝化，这可以增加局部电流密度，刺激树突生长3，22。我们注意到，还有其他树突抑制策略，不涉及泡沫或海绵结构23，24。
据报道，Zn-海绵的制造方法需要一个管炉，空气和氮气的来源（N2）和烟罩。所有步骤都可以在没有环境控制的情况下在实验室办公桌前执行，但在热处理过程中管炉的排气应管道输送到烟气罩。由此产生的电极适合那些有兴趣创建可充电的Zn电极能够高正位容量（>10毫安厘米地球+2）6。
第一个报告的制造方法是一种基于乳液的路线，以创建Zn-海绵电极。第二，是一条基于阿苏的路线。乳液路线的一个优点是它能够创建 Zn 糊状体，当干燥时，很容易从模具腔中脱下。缺点是它依赖昂贵的材料。对于海绵路线，海绵预制件可能具有挑战性，但这个过程使用廉价和丰富的材料。
这两种方法都涉及将 Zn 颗粒与粥原和粘度增强剂混合。产生的混合物在N2 下加热，然后呼吸空气（不是合成空气）。在N2下加热时，Zn颗粒退火和粥原分解:在呼吸空气下，退火的Zn颗粒熔断，粥原燃烧。这些工艺产生金属泡沫或海绵。Zn 海绵的机械和电化学特性可以通过不同的 Zn-porogen 质量比、N2 下的加热时间和空气以及 Zn 和聚源颗粒的大小和形状来调整。

<table>
	<tbody>
		<tr>
			<td>Corn starch</td>
			<td>Argo</td>
			<td>Not applicable</td>
			<td>This acts as a porogen and viscosity-enhancing agent.</td>
		</tr>
		<tr>
			<td>Decane</td>
			<td>MilliporeSigma</td>
			<td>D901</td>
			<td></td>
		</tr>
		<tr>
			<td>Medium viscosity water-soluble carboxymethyl cellulose (CMC) sodium salt</td>
			<td>MilliporeSigma</td>
			<td>C4888-500G</td>
			<td>This CMC acts primarily as a viscosity-enhancing agent.</td>
		</tr>
		<tr>
			<td>Overhead stirrer</td>
			<td>Caframo Lab Solutions</td>
			<td>BDC3030</td>
			<td></td>
		</tr>
		<tr>
			<td>Small cylindrical models for Zn sponges</td>
			<td>VWR</td>
			<td>66014-358</td>
			<td>The caps of the vials can be used as molds.</td>
		</tr>
		<tr>
			<td>Sodium dodecyl sulfate</td>
			<td>MilliporeSigma</td>
			<td>436143</td>
			<td></td>
		</tr>
		<tr>
			<td>Water-insoluble IonSep CMC 52 preswollen carboxymethyl cellulose resin</td>
			<td>BIOpHORETICS</td>
			<td>B45019.01</td>
			<td>This CMC acts as a porogen and viscosity-enhancing agent.</td>
		</tr>
		<tr>
			<td>Zn powder</td>
			<td>EverZinc</td>
			<td>Custom order</td>
			<td></td>
		</tr>
	</tbody>
</table>

zinc-sponge battery electrodes that suppress dendrites

我们报告了两种方法来制造锌海绵电极，以抑制树突的形成和可充电锌电池的形状变化。这两种方法的特点是创建由锌颗粒、有机粥原和粘度增强剂制成的糊糊，这些粘稠性增强剂在惰性气体下加热，然后在空气中加热。在惰性气体加热过程中，锌颗粒一起退火，波源分解:在空气中，锌熔断和残余有机物燃烧，产生开放细胞金属泡沫或海绵。我们通过不同的锌与孢子质量比、惰性气体和空气下的加热时间以及锌和粥原颗粒的大小和形状来调整锌海绵的机械和电化学特性。报告方法的一个优点是它们能够微调锌海绵结构。锌和粥原颗粒的选定大小和形状影响孔隙结构的形态。一个限制是，由此产生的海绵有紊乱的孔隙结构，导致低体积锌（<30%）的机械强度低。这些锌海绵电极的应用包括用于电网存储、个人电子产品、电动汽车和电力航空的电池。用户可以期望锌海绵电极以技术相关速率循环高达 40% 的放电深度，并且无需形成分离器穿孔树突。

由此产生的，完全热处理，乳液为基础的Zn海绵有2.8克+厘米+3的密度，而水性海绵接近3.3克+厘米+3。在空气加热过程中，Zn 表面形成一层 ZnO，厚度应为 0.5°1.0 μm（使用扫描电子显微镜观察）5。产生的海绵中的固体应该是72%Zn（乳液版本）或78%Zn（水文版本），其余的为ZnO（X射线衍射测量）6。两种海绵的孔隙应接近50%，孔径分布以10μm为中心，?...

Watch this Scientific Journal Video about Zinc-Sponge Battery Electrodes that Suppress Dendrites at JoVE.com

Zinc-Sponge Battery Electrodes that Suppress Dendrites

报告协议的目标是制造可充电的锌海绵电极，以抑制锌电池（如镍锌或锌空气）的树突和形状变化。

抑制登德里特的锌海绵电池电极

We report two methods to create zinc-sponge electrodes that suppress dendrite formation and shape change for rechargeable zinc batteries. Both methods are ...

zinc-sponge-battery-electrodes-that-suppress-dendrites

Research

JoVE Journal

Chemistry

4.3K 次观看.  U.S. Naval Research Laboratory, Washington, DC, 20375, United States. 报告协议的目标是制造可充电的锌海绵电极，以抑制锌电池（如镍锌或锌空气）的树突和形状变化。

视频: Zinc-Sponge Battery Electrodes that Suppress Dendrites

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is one surface modification technique that electrodeposits a polymeric film at the surface of an electrode by utilizing an applied potential to initiate the polymerization of substrates in the Helmholtz layer. This useful technique was first established by a Murray-Meyer collaboration at the University of North Carolina at Chapel Hill in the early 1980s and utilized to study numerous physical phenomena of films containing inorganic complexes as the monomeric substrate. Here, we highlight a procedure for coating electrodes with an inorganic complex by performing reductive electropolymerization of the vinyl-containing poly-pyridyl complex onto glassy carbon and fluorine doped tin oxide coated electrodes. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization but are far less sensitive to oxygen and water.

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

在玻碳和氟掺杂的氧化锡电极的含乙烯基聚吡啶基复合还原电聚合

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

科研

化学

A Colorimetric Assay that Specifically Measures Granzyme B Proteolytic Activity: Hydrolysis of Boc-Ala-Ala-Asp-S-Bzl

The serine protease Granzyme B (GzmB) mediates target cell apoptosis when released by cytotoxic T lymphocytes (CTL) or natural killer (NK) cells. GzmB is the most studied granzyme in humans and mice and therefore, researchers need specific and reliable tools to study its function and role in pathophysiology. This especially necessitates assays that do not recognize proteases such as caspases or other granzymes that are structurally or functionally related. Here, we apply GzmB&#8217;s preference for cleavage after aspartic acid residues in a colorimetric assay using the peptide thioester Boc-Ala-Ala-Asp-S-Bzl. GzmB is the only mammalian serine protease capable of cleaving this substrate. The substrate is cleaved with similar efficiency by human, mouse and rat GzmB, a property not shared by other commercially available peptide substrates, even some that are advertised as being suitable for this purpose. This protocol is demonstrated using unfractionated lysates from activated NK cells or CTL and is also suitable for recombinant proteases generated in a variety of prokaryotic and eukaryotic systems, provided the correct controls are used. This assay is a highly specific method to ascertain the potential pro-apoptotic activity of cytotoxic molecules in mammalian lymphocytes, and of their recombinant counterparts expressed by a variety of methodologies.

We describe a simple, quantitative colorimetric assay that specifically measures the proteolytic activity of human, mouse or rat Granzyme B (GzmB). This protocol can be easily adapted for determining protease activity of other granule serine proteases by the hydrolysis of other synthetic peptide substrates with an appropriate recognition sequence.

比色测定的具体措施颗粒酶B蛋白水解活动:水解的Boc-丙氨酸 - 丙氨酸-ASP-S-BZL的

The serine protease Granzyme B (GzmB) mediates target cell apoptosis when released by cytotoxic T lymphocytes (CTL) or natural killer (NK) cells. GzmB is ...

Metal-silicate Partitioning at High Pressure and Temperature: Experimental Methods and a Protocol to Suppress Highly Siderophile Element Inclusions

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from their extraction to the core during terrestrial accretion. Experiments to investigate the partitioning of these elements between metal and silicate melts suggest that the PUM composition is best matched if metal-silicate equilibrium occurred at high pressures and temperatures, in a deep magma ocean environment. The behavior of the most highly siderophile elements (HSEs) during this process however, has remained enigmatic. Silicate run-products from HSE solubility experiments are commonly contaminated by dispersed metal inclusions that hinder the measurement of element concentrations in the melt. The resulting uncertainty over the true solubility and metal-silicate partitioning of these elements has made it difficult to predict their expected depletion in PUM. Recently, several studies have employed changes to the experimental design used for high pressure and temperature solubility experiments in order to suppress the formation of metal inclusions. The addition of Au (Re, Os, Ir, Ru experiments) or elemental Si (Pt experiments) to the sample acts to alter either the geometry or rate of sample reduction respectively, in order to avoid transient metal oversaturation of the silicate melt. This contribution outlines procedures for using the piston-cylinder and multi-anvil apparatus to conduct solubility and metal-silicate partitioning experiments respectively. A protocol is also described for the synthesis of uncontaminated run-products from HSE solubility experiments in which the oxygen fugacity is similar to that during terrestrial core-formation. Time-resolved LA-ICP-MS spectra are presented as evidence for the absence of metal-inclusions in run-products from earlier studies, and also confirm that the technique may be extended to investigate Ru. Examples are also given of how these data may be applied.

We present a procedure to determine the metal-silicate partitioning of siderophile elements, emphasizing techniques that suppress the formation of metal inclusions in experiments for the noble metals. The results of these experiments are used to demonstrate the effect of core-formation on the highly siderophile element composition of the mantle.

金属硅酸盐分区在高压和高温:实验方法和协议，以抑制高亲铁元素元素夹杂物

Estimates of the primitive upper mantle (PUM) composition reveal a depletion in many of the siderophile (iron-loving) elements, thought to result from ...

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 ...

Simple Methods for the Preparation of Non-noble Metal Bulk-electrodes for Electrocatalytic Applications

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and composition of the material was characterized via powder X-ray diffraction (PXRD), M&#246;ssbauer spectroscopy (MB), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX). Two preparation methods of pentlandite bulk electrodes are presented. In the first approach a piece of synthetic pentlandite rock is directly contacted via a wire ferrule. The second approach utilizes pentlandite pellets, pressed from finely ground powder, which is immobilized in a Teflon casing. Both electrodes, whilst being prepared by an additive-free method, reveal high durability during electrocatalytic conversions in comparison to common drop-coating methods. We herein showcase the striking performance of such electrodes to accomplish the hydrogen evolution reaction (HER) and present a standardized method to evaluate the electrocatalytic performance by electrochemical and gas chromatographic methods. Furthermore, we report stability tests via potentiostatic methods at an overpotential of 0.6 V to explore the material limitations of the electrodes during electrolysis under industrial relevant conditions.

A facile preparation method of electrodes using the bulk material Fe4.5Ni4.5S8 is presented. This method provides an alternative technique to conventional electrode fabrication and describes prerequisites for unconventional electrode materials including a straightforward electrocatalytic testing method.

用于制备用于电催化应用的非贵金属体电极的简单方法

The rock material pentlandite with the composition Fe4.5Ni4.5S8 was synthesized via high temperature synthesis from the elements. The structure and ...

Accelerating Rate Calorimetry and Complementary Techniques to Characterize Battery Safety Hazards

The hazards associated with lithium-based battery chemistries are well-documented due to their catastrophic nature. Risk is typically qualitatively assessed through an engineering risk matrix. Within the matrix, potentially hazardous events are categorized and ranked in terms of severity and probability to provide situational awareness to decision makers and stakeholders. The stochastic nature of battery failures, particularly the lithium-ion chemistry, makes the probability axis of a matrix difficult to properly assess. Fortunately, characterization tools exist, such as accelerated rate calorimetry (ARC), that characterize degrees of battery failure severity. ARC has been used extensively to characterize reactive chemicals but can provide a new application to induce battery failures under safe, controlled experimental conditions and quantify critical safety parameters. Due to the robust nature of the extended volume calorimeter, cells may be safely taken to failure due to a variety of abuses: thermal (simple heating of cell), electrochemical (overcharge), electrical (external short circuit), or physical (crush or nail penetration). This article describes the procedures to prepare and instrument a commercial lithium-ion battery cell for failure in an ARC to collect valuable safety data: onset of thermal runaway, endotherm associated with polymer separator melting, pressure release during thermal runaway, gaseous collection for analytical characterization, maximum temperature of complete reaction, and visual observation of decomposition processes using a high temperature borescope (venting and cell can breach). A thermal &#8220;heat-wait-seek&#8221; method is used to induce cell failure, in which the battery is heated incrementally to a set point, then the instrument identifies heat generation from the battery. As heat generates a temperature rise in the battery, the calorimeter temperature follows this temperature rise, maintaining an adiabatic condition. Therefore, the cell does not exchange heat with the external environment, so all heat generation from the battery under failure is captured.

A method to characterize the potential failure hazards of lithium batteries is achieved with accelerating rate calorimetry. Heat and pressure release, visual observation of the failure event, and the capture of evolved gases are collected in this experiment to identify the worst credible threats of batteries taken to failure.

The hazards associated with lithium-based battery chemistries are well-documented due to their catastrophic nature. Risk is typically qualitatively ...

Fabrication of Thin Film Silver/Silver Chloride Electrodes with Finely Controlled Single Layer Silver Chloride

This paper aims to present a protocol to form smooth and well-controlled films of silver/silver chloride (Ag/AgCl) with designated coverage on top of thin film silver electrodes. Thin film silver electrodes sized 80 &#181;m x 80 &#181;m and 160 &#181;m x 160 &#181;m were sputtered on quartz wafers with a chromium/gold (Cr/Au) layer for adhesion. After passivation, polishing and cathodic cleaning processes, the electrodes underwent galvanostatic oxidation with consideration of Faraday&#39;s Law of Electrolysis to form smooth layers of AgCl with a designated degree of coverage on top of the silver electrode. This protocol is validated by inspection of scanning electron microscope (SEM) images of the surface of the fabricated Ag/AgCl thin film electrodes, which highlights the functionality and performance of the protocol. Sub-optimally fabricated electrodes are fabricated as well for comparison. This protocol can be widely used to fabricate Ag/AgCl electrodes with specific impedance requirements (e.g., probing electrodes for impedance sensing applications like impedance flow cytometry and interdigitated electrode arrays).

This paper aims to present a method to form smooth and well-controlled films of silver chloride (AgCl) with designated coverage on top of thin film silver electrodes.

薄膜银/银氯化银电极的制造，具有精细控制的单层氯化银

This paper aims to present a protocol to form smooth and well-controlled films of silver/silver chloride (Ag/AgCl) with designated coverage on top of thin ...

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

With the ever-increasing use of Li-ion batteries, especially due to their adoption in electric vehicles, their safety is in prime focus. Thus, the all-solid-state batteries (ASSBs) that use solid electrolytes instead of liquid electrolytes, which reduce the risk of flammability, have been the center stage of battery research for the last few years. However, in the ASSB, the ion transportation through the solid-solid electrolyte-electrode interface poses a challenge due to contact and chemical/electrochemical stability issues. Applying a suitable coating around the electrode and/or electrolyte particles offers a convenient solution, leading to better performance. For this, researchers are screening potential electronic/ionic conductive and nonconductive coatings to find the best coatings with suitable thickness for long-term chemical, electrochemical, and mechanical stability. Operando transmission electron microscopy (TEM) couples high spatial resolution with high temporal resolution to allow visualization of dynamic processes, and thus is an ideal tool to evaluate electrode/electrolyte coatings via studying (de)lithiation at a single particle level in real-time. However, the accumulated electron dose during a typical high-resolution in situ work may affect the electrochemical pathways, evaluation of which can be time-consuming. The current protocol presents an alternative procedure in which the potential coatings are applied on Si nanoparticles and are subjected to (de)lithiation during operando TEM experiments. The high volume changes of Si nanoparticles during (de)lithiation allow monitoring of the coating behavior at a relatively low magnification. Thus, the whole process is very electron-dose efficient and offers quick screening of potential coatings.

Screening of Coatings for an All-Solid-State Battery Using In Situ Transmission Electron Microscopy

Utilizing the volume change of Si nanoparticles during (de)lithiation, the present protocol describes a screening method of potential coatings for all-solid-state batteries using in situ transmission electron microscopy.