Name: zinc-sponge battery electrodes that suppress dendrites
Uploaded: 2020-09-29T14:00:00
Description: Watch this Scientific Journal Video about Zinc-Sponge Battery Electrodes that Suppress Dendrites at JoVE.com

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....

<ol>
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F., 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> Metal Foams: A Design Guide. , (2000).</li><li>Parker, J. F., Ko, J. S., Rolison, D. R., Long, J. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Translating+Materials-Level+Performance+into+Device-Relevant+Metrics+for+Zinc-Based+Batteries.">Translating Materials-Level Performance into Device-Relevant Metrics for Zinc-Based Batteries.</a> Joule. 2 (12), 2519-2527 (2018).</li><li>Hopkins, B. J., Chervin, C. N., Parker, J. F., Long, J. W., Rolison, D. 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M., Mumm, D. R., Mohraz, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improving+Cyclability+of+ZnO+Electrodes+through+Microstructural+Design.">Improving Cyclability of ZnO Electrodes through Microstructural Design.</a> ACS Applied Energy Materials. 2 (11), 8107-8117 (2019).</li><li>Wang, C., Zhu, G., Liu, P., Chen, Q. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Monolithic+Nanoporous+Zn+Anode+for+Rechargeable+Alkaline+Batteries.">Monolithic Nanoporous Zn Anode for Rechargeable Alkaline Batteries.</a> ACS Nano. 14 (2), 2404-2411 (2020).</li><li>Drillet, J. F., 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=Development+of+a+Novel+Zinc/Air+Fuel+Cell+with+a+Zn+Foam+Anode,+a+PVA/KOH+Membrane+and+a+MnO2/SiOC-based+Air+Cathode.">Development of a Novel Zinc/Air Fuel Cell with a Zn Foam Anode, a PVA/KOH Membrane and a MnO2/SiOC-based Air Cathode.</a> ECS Transactions. 28, 13-24 (2010).</li><li>Bozzini, B., 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=Morphological+evolution+of+Zn-sponge+electrodes+monitored+by+in+situ+X-ray+computed+microtomography.">Morphological evolution of Zn-sponge electrodes monitored by in situ X-ray computed microtomography.</a> ACS Applied Energy Materials. , (2020).</li><li>Yang, Q., 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=Do+Zinc+Dendrites+Exist+in+Neutral+Zinc+Batteries:+A+Developed+Electrohealing+Strategy+to+In+Situ+Rescue+In-Service+Batteries.">Do Zinc Dendrites Exist in Neutral Zinc Batteries: A Developed Electrohealing Strategy to In Situ Rescue In-Service Batteries.</a> Advanced Materials. 31, 1903778 (2019).</li><li>Yang, Q., 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=Hydrogen-Substituted+Graphdiyne+Ion+Tunnels+Directing+Concentration+Redistribution+for+Commercial-Grate+Dendrite-Free+Zinc+Anodes.">Hydrogen-Substituted Graphdiyne Ion Tunnels Directing Concentration Redistribution for Commercial-Grate Dendrite-Free Zinc Anodes.</a> Advanced Materials. 32, 2001755 (2020).</li><li>Narayanan, S. 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=Materials+challenges+and+technical+approaches+for+realizing+inexpensive+and+robust+iron-air+batteries+for+large-scale+energy+storage.">Materials challenges and technical approaches for realizing inexpensive and robust iron-air batteries for large-scale energy storage.</a> Solid State Ionics. 216, 105-109 (2012).</li><li>Xiong, H., 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=Effects+of+Heat+Treatment+on+the+Discharge+Behavior+of+Mg-6wt.%Al-1wt.%Sn+Alloy+as+Anode+for+Magnesium-Air+Batteries.">Effects of Heat Treatment on the Discharge Behavior of Mg-6wt.%Al-1wt.%Sn Alloy as Anode for Magnesium-Air Batteries.</a> Journal of Materials Engineering and Performance. 26, 2901-2911 (2017).</li><li>Hopkins, B. J., Shao-Horn, Y., Hart, D. 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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 ...

This protocol provides an easy, low-cost method of creating a zinc electrode that suppresses dendrites when cycled in an alkaline battery. The main advantage of this technique is that one can easily tune the structure of the zinc electrode by changing zinc particle size, type of origin and its size, or heat treatment protocol. The metal sponge created using this protocol falls into the relative density and cell size that can be difficult to achieve using standard metal foam manufacturing methods.Begin by adding 2.054 milliliters of deionized water and 4.565 milliliters of decane to a 100 milliliter glass beaker. Then dissolve 0.1 gram of SDS by stirring the solution. Next, add five milligrams of water soluble medium viscosity CMC sodium salt to the beaker and stir for five minutes or until dissolved.Use plastic or plastic-coated stirring tools because a metallic surface can adversely affect resulting zinc sponges. Add and stir 0.844 grams of water insoluble pre-swollen carboxymethyl cellulose resin to the beaker. Keep the beaker on an overhead paddle stirrer equipped with a plastic paddle and stir the entire mixture at 1, 000 RPM for five minutes.Add 50 grams of zinc powder and continue stirring for five more minutes. After five minutes, stop the stirrer and remove the beaker. Place the beaker in a desiccator for five minutes at room temperature to outcast the mixture and its contents under vacuum.Portion the zinc paste into polypropylene molds of approximately 10 millimeter diameter and five millimeter height to air-dry the paste overnight. After drying, carefully remove the zinc paste from the molds and place them into a mesh casing that rests on a notched alumina holder. Place the assembly into a tube furnace with ports to flow gas in and out of the tube.Pipe nitrogen gas into the furnace for 30 minutes at a rate of 5.7 centimeters per minute to purge the furnace of air. After 30 minutes of purging, throttle the nitrogen gas to a constant rate of 2.8 centimeters per minute. Program the temperature of the furnace to increase linearly from 20 to 369 degrees Celsius over the course of 68 minutes, hold at 369 degrees Celsius for five hours, rise linearly from 369 to 584 degrees Celsius over the course of 105 minutes, and then turn off.Start the furnace program as the nitrogen continues to flow. Stop the nitrogen gas flow manually after the five hours of temperature hold and pipe in breathing air at 2.8 centimeters per minute. Let the furnace cool to room temperature once the heating program stops while keeping the breathing air flowing.Finally, remove the cooled zinc sponges and either saw or sand them to the desired dimensions. Add 10.5 milliliters of deionized water to a 100 milliliter glass beaker. Then add 0.12 grams of water soluble high-viscosity cellulose gum and stir using a plastic-coated stirring tool.Vortex and stir this mixture by hand for five minutes or until the cellulose gum is dissolved. Add 2.4 grams of cornstarch while vortexing the beaker for two minutes and then add 120 grams of prepared zinc powder while vortexing for an additional two minutes. Once done, press the resulting zinc paste into the desired mold cavities and leave them to dry overnight at 70 degrees Celsius in open air in a furnace.After drying, carefully remove the zinc paste from the molds and place them into a mesh casing that rests on a notched alumina holder. Place the assembly into a tube furnace with ports to flow gas in and out of the tube. Pipe nitrogen gas into the furnace for 30 minutes at a rate of 5.7 centimeters per minute to purge the furnace of air.After 30 minutes of purging, throttle the nitrogen gas to a constant rate of 2.8 centimeters per minute. Program the temperature of the furnace to increase linearly from 20 to 369 degrees Celsius over the course of 68 minutes, hold at 369 degrees Celsius for five hours, rise linearly from 369 to 584 degrees Celsius over the course of 105 minutes, and then turn off. Start the furnace program as the nitrogen continues to flow.After five hours of temperature hold, stop the nitrogen gas flow manually and pipe in breathing air at 2.8 centimeters per minute. Allow the furnace to cool to room temperature once the heating program stops while keeping the breathing air flowing. Finally, remove the cooled zinc sponges and saw or sand them to the desired dimensions.This protocol was used to produce emulsion-based zinc sponges with densities of 2.8 grams per cubic centimeter and aqueous-based sponges with densities of 3.3 grams per cubic centimeter. The zinc sponges should be rigid and brittle. Their cross-sections should look similar to the ones shown here.All properties of the resulting zinc sponges should fall within the ranges provided in the text manuscript. The zinc sponge electrode shows a cycling stability at a gravimetric capacity of 328 milliampere hours per gram of zinc, which maps to a 43%depth of discharge. After extensive electrochemical cycling of the constructed zinc electrodes to estimate their efficiency, no dendrites were observed in scanning electron micrographs of the zinc sponge electrodes.The surface of the zinc sponge undergoes restructuring during cycling. The deeper the level of discharge and the greater the cycle life, the greater the amount of restructuring. When attempting this protocol, remember to stir the mixture with a plastic-coated tool.Similar fabrication processes could be used to create other types of metal foams based on different metals for numerous applications.

Research

JoVE Journal

Chemistry

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

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

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

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

- 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

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 ...

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

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 ...