この研究は、米国海軍研究局によって資金提供されました。

1. Znスポンジ電極を作成するエマルジョンベースの方法
<ol><li>100 mL ガラスビーカーに2.054 mLの脱イオン水を加えます。</li>
	<li>ビーカーに4.565 mLのデカンを加えます。</li>
	<li>0.1000 ± 0.0003 g のドデシル硫酸ナトリウム (SDS) を溶解するまで撹拌します。</li>
	<li>0.0050 ± 0.0003 gの 水溶性 培地粘度カルボキシメチルセルロース (CMC) ナトリウム塩を手で 5 分間か CMC が完全に溶解するまでかき混ぜます。 注:プラスチックまたはプラスチックコーティングされた攪拌ツールを使用してください。金属表面でツールを使用して攪拌すると、得られるZnスポンジに悪影響を与える可能性があります。</li>
	<li>0.844 ± 0.002 gの 水不溶性 プレスプラウレンカルボキシメチルセルロース樹脂を撹拌します。 注:このタイプの水不溶性樹脂は高価です (USD $420 kg–1)6.</li>
	<li>プラスチックパドルを装備したオーバーヘッドパドルスターラーを使用して、この混合物を1,000 rpmで5分間かき混ぜます。</li>
	<li>Zn粉末50g(平均粒径50μm、ビスマス307ppm、腐食抑制用インジウム307ppm)をビーカーに注ぎ込み、オーバーヘッドスターラーは1,000rpmで回転し続けます。</li>
	<li>同じ速度でZnペーストを1,000rpmで5分間攪拌し続けます。</li>
	<li>攪拌機を停止し、ビーカーを取り除き、ビーカーとその内容物を室温のデシケータで5分間真空下に置いて混合物をアウトガスします。</li>
	<li>Znペーストをポリプロピレンモールド(直径約10mm、高さ約5mm)に入れ、一晩野外乾燥させます。金型の形状は、乾燥したペーストと得られるZnスポンジの形態を決定します。 注: 金型のサイズと形状は異なる場合があります。過去の実験5 は直径が10mm近い円筒形の金型をうまく使用しました。Znペーストを5mm以下の高さまで充填します。高さが短いほど、必要な乾燥時間が短くなります。市販 の金型については、材料表 を参照してください。</li>
	<li>乾燥したZnペーストプリフォームを金型から慎重に取り出し、ノッチアルミナホルダー5、6に置くメッシュケーシングに入れます。 注:例えば、Znスポンジ電極の所望の直径よりもわずかに大きい直径を持つシリンダーに穿孔真鍮シートを曲げることによって、メッシュケーシングを製造します。所望の形状に曲げた後、ホウ素窒化物潤滑油で穿フォー金属シートをスプレーします。</li>
	<li>チューブの中にガスを流し、ガスを流すポートとチューブ炉(直径67mm)にアセンブリを置きます。 注:炉にガスをパイプするには、1つのポート(入口ポート)を使用してください。もう一方(出口口)を使用して、チューブ炉からガスをガスフードに排出します。</li>
	<li>5.7 cm∙分–1の速度で炉に30分間N2ガスをパイプし、空気炉をパージします。 注:ステップ1.13は、N2 ガスのタンクとデジタル制御流量計を、いずれかの入り口ポートに接続されたチューブに接続することで達成できます。ガス流量計は、手動またはコンピュータで制御できます。</li>
	<li>30分パージ後にN2 ガスを2.8cmの∙分–1 の一定の速度にスロットルします。</li>
	<li>炉は68分間で20から369°Cに直線的に温度を上げ、369°Cで5時間保持し、105分の間に369から584 °Cに直線的に上昇し、次にオフにします。</li>
	<li>N2ガスが流れ続けている間、炉プログラムを開始します。</li>
	<li>5時間の温度保持後にN2-ガスの流れを手動で停止し、2.8cm∙分–1で空気を吸い込むパイプ。 注:ステップ1.17は、追加の入り口ポートに接続されたチューブにデジタル制御流量計と呼吸空気(合成空気ではない)のタンクを接続することによって達成することができます。</li>
	<li>加熱プログラムが停止したら、炉をアクティブな冷却せずに室温まで冷却しますが、呼吸空気を流し続けます。</li>
	<li>冷却されたZnスポンジを取り外し、それらを見たり、必要な寸法にそれらを砂で。 メモ:手持ちのロータリーソーや垂直バンドソーなど、さまざまなソーイングツールを使用できます。研磨ブレードまたはダイヤモンドブレードが適切です。</li>
</ol>2. Zn-スポンジ電極を作成する水性ベースの方法
<ol><li>100 mL ガラスビーカーに10.5 mLの脱イオン水を加えます。</li>
	<li>0.120±0.001 gの 水溶性 高粘度セルロースガム(カルボキシメチルセルロース(CMC)ナトリウム塩とも呼ばれる) を攪拌します。 注:プラスチックまたはプラスチックコーティングされた攪拌ツールを使用してください。金属表面でツールを使用して攪拌すると、得られるZnスポンジに悪影響を与える可能性があります。</li>
	<li>ボルテックスを5分間、またはCMCが溶解するまで、この混合物を手でかき混ぜます。</li>
	<li>2.400±0.001gのトウモロコシデンプンをかき混ぜながら、さらに2分間渦巻きます。</li>
	<li>120.00 ± 0.01 gのZn粉末(ビスマスの307 ppm、腐食抑制用インジウム307ppmを含む)を120.00±に攪拌し、さらに2分間ボルテックスします。</li>
	<li>生成された Zn ペーストを目的のモールド キャビティに押し込みます。 注: 金型のサイズと形状は異なる場合があります。過去の実験6 は直径が10mm近い円筒形の金型をうまく使用しました。Znペーストを50mm以下の高さまで充填します。水性ZnペーストはエマルジョンZnペーストよりも乾燥しているので、水性のバージョンは、より少ない乾燥時間を必要とするより大きなスポンジを作るために使用することができます。高さが短いほど、必要な乾燥時間が短くなります。金型は、エマルジョンZnペーストとは異なり、乾燥後に水性Znペーストが最小限に縮むので半分に分割できる必要があります。無塩バターは、デモルディングを助けるために水性Znペーストを押す前に金型を潤滑するために使用することができます。 図1A は、水性ベースのプロトコルに従ってZnペーストを詰めたカスタム加工金型を示しています。 図1B は、手作りメッシュケーシング、ノッチアルミナホルダー、および水系法を用いて作られた得られたZnスポンジを示す。</li>
	<li>Znペースト充填金型を炉内のオープンエアで70°Cで一晩乾燥させます。</li>
	<li>エマルジョンベースの方法で説明されている同じ取り扱いと熱処理手順(1.11~1.19)に従ってください。</li>
</ol>

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J.F.P.、D.R.R.、J.W.L.は、亜鉛電極に関する特許を保有しています:米国特許第9802254、10008711、10720635、10763500、EU特許2926395、中国特許第104813521。

これらのプロトコルに関連する変更およびトラブルシューティングには、新しく混合されたZnペーストを金型キャビティに充填する必要があります。エアポケットを避けるために注意する必要があります。充填後または充填中に金型をタップすることで、不要なボイドを減らすことができます。水性Znペーストは乾燥しているため、Znペーストに直接圧力をかけ、金型キャビティを満タンにし?...

報告された製造方法の目的は、デンドライトの形成および形状変化を抑制する亜鉛(Zn)スポンジ電極を作成することである。歴史的に、これらの問題はZn電池のサイクル寿命を制限してきました。亜鉛スポンジ電極は、これらの問題を解決し、長いサイクルの生命を持つZn電池を可能にしました1,2,3,4,5,6.スポンジ構造は、(1)融合されたZnフレームワークがスポンジの全容を電気的に配線するため、樹状突起の形成と形状変化を抑制する。(2)孔はZnスポンジ表面の近くに亜鉛を保持します。(3)スポンジは、アルカリ性電解質7中の樹状突起に同定された値以下の局所電流密度を減少させる高い表面積を有する。しかし、スポンジ表面積が高すぎると、実質的な腐食が5に生じる。スポンジの細孔が大きすぎる場合、スポンジは、低体積容量5を有する。また、スポンジの細孔が小さすぎると、放電中にZnにアクセスするのには、Zn電極が不十分な電解質が得られ、低電力および容量5,6が生じる。
報告された製造方法の背後にある根拠は、適切なスポンジの多孔質および細孔径を有するZnスポンジを作成することである。実験的に、50~70%の多孔質を有するZnスポンジと、10μm近くの孔径がフルセル電池で十分にサイクルし、低い腐食率を示す5を見つけた。我々は、市販の金属フォームを製造する既存の方法は、これらの長さスケール8で同様の形態を達成することができないので、報告された製造方法が必要であることに注意してください。
代替案上でここで報告される方法の利点は、スポンジの特徴の細かい制御と技術的に関連する非現実的容量値5、6、9、10を持つ大きく、密なZnスポンジを製造する能力によって特徴付けられる。Znフォームを作成する別の方法では、50%近くスポンジの多孔質を持つ同等の10 μmの細孔を作成することができない場合があります。しかし、このような代替手段は、高温処理ステップを避けるため、製造に必要なエネルギーが少なくなる可能性があります。代替プロセスは、以下の戦略を含む:冷間焼成Zn粒子11、3次元ホスト構造12、13、14、15、16、17上にZnを堆積させ、Zn箔を2次元フォーム18に切断し、スピノーダル分解19またはパーコレーション溶解20を介してZn発泡体を作成する。
出版された文献のより広い体における報告された方法の文脈は、主にDrilletらの研究によって確立される。彼らは多孔質セラミックスを製造する方法を適応し、電池用の脆弱なZnフォームにもかかわらず、最も初期に報告された3次元の1つを作成しました。しかし、これらの著者は、Zn粒子間の接続性が悪いため、再充電性を実証できなかった。再充電可能なZnスポンジ電極に先立ち、Zn箔電極に代わる最良の代替手段はZn粉末電極であり、そこでZn粉末がゲル電解質と混合された。亜鉛粉末電極は、一次アルカリ電池(Zn–MnO2)で市販されているが、Zn粒子がZn酸化物(ZnO)によって過動化するため、再充電性が悪く、樹状突起の成長に拍車をかける局所電流密度を増加させることができる3,22。我々は、発泡体やスポンジアーキテクチャ23、24を含まない他の樹状突起抑制戦略があることに注意してください。
報告されたZnスポンジの製造方法には、チューブ炉、空気と窒素ガスの供給源(N2)、およびヒュームフードが必要です。すべてのステップは環境制御なしで実験室の机で行うことができるが熱処理の間に管の炉からの排気は煙のフードに渡されるべきである。得られた電極は、高い高いareal容量(>10 mAh cmgeo–2)の可能性のある充電式Zn電極を作成することに興味がある人に適しています。
最初に報告された製造方法は、Zn-スポンジ電極を作成するためのエマルジョンベースのルートです。2 つ目は水性ベースのルートです。エマルジョン経路の利点は、Znペーストを作成する能力であり、乾燥すると、金型キャビティからデボルドしやすい。欠点は、高価な材料への依存です。水の経路のために、スポンジのプリフォームは、デボルドに挑戦することができますが、このプロセスは、安価で豊富な材料を使用しています。
いずれの方法も、Zn粒子と、多孔質および粘度増強剤を混合することを含む。得られた混合物をN2下で加熱し、次いで空気を呼吸する(合成空気ではない)。N2下での加熱時に、Zn粒子のアニールとポロゲンが分解します。呼吸する空気の下で、アニールされたZn粒子が融合し、ポロゲンが燃え尽きる。これらのプロセスは、金属の泡やスポンジを生成します。Znスポンジの機械的および電気化学的特性は、Zn-対ポロゲン質量比、空気下の加熱時間、Znおよび多孔質粒子のサイズと形状を変化させることによって調整することができます。

<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

デンドライト形成を抑制する亜鉛スポンジ電極の作成方法と、再充電可能な亜鉛電池の形状変化を報告する。いずれの方法も、亜鉛粒子、有機ポロゲン、粘度増強剤で作られたペーストを作り、不活性ガスと空気で加熱することを特徴としています。不活性ガス下での加熱時には、亜鉛粒子が一緒にアニーリングし、ポロゲンが分解します。空気の下では、亜鉛のヒューズと残留有機が燃え尽き、開いた細胞の金属フォームまたはスポンジを生み出します。亜鉛とポロゲン質量比、不活性ガスと空気の加熱時間、亜鉛粒子とポロゲン粒子の大きさと形状を変化させることにより、亜鉛スポンジの機械的および電気化学的特性を調整します。報告された方法の利点は、亜鉛スポンジアーキテクチャを細かく調整する能力です。選択した亜鉛粒子とポロゲン粒子のサイズと形状は、細孔構造の形態に影響を与えます。制限は、得られたスポンジが亜鉛の低体積分率(<30%)で低い機械的強度をもたらす無秩序な細孔構造を有していることである。これらの亜鉛スポンジ電極の用途には、グリッドストレージ用の電池、パーソナルエレクトロニクス、電気自動車、電気航空などがあります。ユーザーは、ジンクスポンジ電極がセパレータピアスデンドライトの形成なしに、技術的に関連する速度と非現実的な容量で最大40%の排出深度をサイクルすることが期待できます。

結果として、完全に熱処理されたエマルジョンベースのZnスポンジは2.8 g∙cm-3の密度を有し、水性ベースのスポンジは3.3 g∙cm-3に近づく。空気下での加熱の間に、Znの層は、0.5〜1.0 μmの厚さを有するZn表面に形成される(走査型電子顕微鏡を用いて観察される)5。得られたスポンジ中の固体は、72%Zn(エマルジョンバージョン)または78%Zn(水性バージョン)であり、...

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

Zinc-Sponge Battery Electrodes that Suppress Dendrites

報告されたプロトコルの目的は、ニッケル亜鉛や亜鉛空気などの亜鉛電池の樹状突起や形状変化を抑制する再充電可能な亜鉛スポンジ電極を作成することです。

デンドライトを抑制する亜鉛スポンジ電池電極

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

4.2K ビュー.  U.S. Naval Research Laboratory, Washington, DC, 20375, United States. 報告されたプロトコルの目的は、ニッケル亜鉛や亜鉛空気などの亜鉛電池の樹状突起や形状変化を抑制する再充電可能な亜鉛スポンジ電極を作成することです。

ビデオ: 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.

グラッシーカーボンとフ​​ッ素ドープ酸化スズ電極上にビニル含有ポリピリジル錯体の還元電解重合

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

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.

のBoc-ALA-ALA-Aspを-S-Bzlのの加水分解：具体的にグランザイムBタンパク質分解活性を測定する比色アッセイ

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.

高温高圧下における金属珪酸塩パーティション化：実験方法と非常に親鉄元素介在物を抑制するためのプロトコル

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.

電気化学的評価と対称型有機レドックスフロー電池の充電診断の状態のためのプロトコル

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.

電気化学的応用のための非貴金属バルク電極の調製のための簡単な方法

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.

細かく制御された単層塩化銀を用いた薄膜銀/塩化銀電極の製造

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.