著者は、このプロジェクトに資金を供給するための国立科学財団賞1006568を確認したいと思います。

1。準備ナノVB 2 ナノVB 2が直接1：02モル比でボールミルを介して元素バナジウムおよびホウ素から合成される。 <ol><li> 50ミリリットルの炭化タングステンの粉砕ジャーと10 10 mmのタングステンカーバイドボールを清掃します。 100℃のオーブンで空気中で乾燥させ℃で1時間は、すべての水が蒸発したことを確認する。 </li><li>残留物が表示されている場合は、手順1.1を繰り返し、残渣残ってないことを保証するために製粉瓶の内側をきれいに拭いてください。 </li><li> 10分毎に時間をアルゴン3Xとグローブボックスの副室をパージします。アルゴン充填のグローブボックスに製粉ジャー、ボール、そしてきれいなへらを転送します。 </li><li> 1:2のモル比でバナジウムおよびホウ素粉末を秤量、バナジウム0.500グラムとフライスジャーに0.212グラムのホウ素は、ボールを追加し、製粉瓶を密封。 </li><li>グローブボックスから密封された製粉ジャーを外し、600 rpmにして4時間のために工場に遊星ボールミルに入れてください。 </li><li> completio後にnは、ミリングジャーをボールミルから取り出す前に室温に冷却させる。 </li><li> 10分毎に時間をアルゴン3Xとグローブボックスの副室をパージします。グローブボックス内にミリングジャー、丸底フラスコに、パラフィンフィルム、へら、および磁気攪拌棒を転送する。 </li><li>以下のように調製されたナノVB 2に酸化ジルコニウムコーティングを施す。 <ol><li>内側にグローブボックスは、以前の出発質量の大半が回収されるまでの粉砕ジャーの壁をこすり取るようにへらを用いて調製したナノVB 2を収集します。丸底フラスコに集めナノVB 2を秤量し、転送します。 </li><li>収集VB 2に比べて塩化ジルコニウムの3.5重量％を秤量し、次いで回収したナノVB-2を含有する丸底フラスコに粉末を加える。 </li><li>フラスコに、磁気攪拌バーを追加し、グローブボックスから除去する前に開口部を封止パラフィンフィルムを用いた。また、セプタムは、同等の結果がグローブボックスから丸底フラスコをクリアで使用されている。 </li><li>を10mlのシリンジを使用して、丸底フラスコに10mlのジエチルエーテルを転送する。迅速にパラフィルムの追加部分でパラフィンフィルムでシリンジで作成穴をカバーしています。 </li><li>メディア設定で一時間撹拌プレート上でフラスコを混ぜる。 </li><li> 1時間後、コーティングされたナノVB-2になるまでロータリーエバポレーターまたは他のポンプ構成を用いたナノVB 2の残りのジエチルエーテルを蒸発、乾燥されます。 </li><li>ナノVB 2コーティングのZrは完全に乾燥した後、収集します。 </li></ol></li></ol> 2。電解液の調製<ol><li> 4 M KOH及び電解質として使用するための4 M水酸化ナトリウム溶液の混合物を調製する。 （注：などの新しいセルを形成するために必要な繰り返し、必要なだけの数週間続くようにしてください）​​。 NaOHおよびKOHの水性水酸化電解質が実行された濃度範囲、過去に検討されている飽和に8 Mのパトン。 4 M NaOHおよびKOH 4 Mの組み合わせは、純粋な水酸化ナトリウム電解質を用いた以前の結果と比較してわずかに改善された高レート性能が得られる。 </li></ol> 3。亜鉛/空気電池の分解バッテリーメーカーとモデル番号の詳細については、試薬や材料の表を参照してください。 <ol><li> VB 2 /空気電池の後製作のための亜鉛/空気セルを開く。 <ol><li>斜めのカッティングプライヤーを使用してコイン電池ケースのリップでカットを作成します。 </li><li>外側リップの縁取り外を圧着。二回セルの周囲を完全に行った後、それが開くことは簡単なはずです。 </li><li>カミソリの刃を使用し、ゆっくりとキャップの縁を押し上げ、優しく細胞を開き強制。注：これは、セルが開いて取得するにはしばらく時間がかかる場合があります。この手順を実行する際、任意の部分をクラックまたは損傷しない患者と注意してください。セルは無傷のままにする必要があります。 </li></ol></li><li>使用するためのバッテリーを準備する<ol><li>セルは2つの部分（キャップ​​と底部）に開かれると優しくキャップからと底部の亜鉛負極材料を除去するために開始します。 </li><li>カミソリの刃でできるだけ多くの固体亜鉛として削除します。底をこすりしないでください、それはすべての部品を損傷しないことが重要です。セパレーター（下）とガスケット（両側）は簡単にカミソリの刃で適用あまりにも多くの圧力によってパンクすることができ、単一の不透明なオーバーレイを形成している。セパレーターを貫通する空気極を損傷することになります。ガスケットが乱れている場合に加えて、電気的に絶縁されるべきセルの信頼性が失われる。 </li><li>綿棒を使用すると、慎重にキャップ、ボトム、およびセパレータから残り亜鉛、残渣を拭いてください。 </li><li>イソプロピルアルコールで細胞のキャップと外側をきれい。 </li></ol></li></ol> 4。 70/30乾燥混合で5 mAhの作用電極の作製<ol><li>アクティブ、材質として合成のZrコーティングナノVB 2を使用ら、電極当たり0.0012グラムを作製する秤量（通常は5から10の細胞を一度にテストされています）と乳鉢と乳棒に移す。 </li><li>モルタルで活物質まで秤量VB 2の30％、グラファイトカーボンブラック（当たり電極）の0.0005グラムを追加し、30分間乳棒と挽く。 </li><li>材料のない大規模な、目に見えるクラスタが存在しないことを確認して、粉を収集します。 </li><li>へらを使ってきれいな電極キャップ当たり70/30-powder混合物の約0.0017グラムを秤量する。 （一度に複数のセルを準備する場合は、そうしないと電極キャップに材料を移す）。 </li><li>そこには塊がありませんし、懸濁液を均等にキャップの上部に分散されるまでへらまたは他の小さな尖った先端を持つ各キャップとスワール粉末にイソプロピルアルコールの一滴を追加します。 </li><li>電極は30分間乾燥させます。 </li></ol> 5。 VB 2 -空気電池アセンブリ-乾式法<ol><li>亜鉛/ AIから逆に細胞を組み立てる作用電極とRセル、キャップ、逆さまに。 </li><li>二列で、​​1でキャップなどに対応するボトムス - 各セル（10はテストされている5）整理。アノード材料が均等に分散し、割れていないことを保証するために、各キャップを点検します。 </li><li>各セパレータ4 M KOH / 4 M NaOHを電解液の27μlを添加。 </li><li>ゆっくりとボトムの内側に一度だけ軽くたたく綿を使用して底から余分な電解質を除去する。 </li><li>慎重に、ボトムスのそれぞれを取るそれらを裏返し、と陽極材が電解液と接触しているように、キャップの上に置きます。 </li><li>圧力をかけると速乾性エポキシ樹脂を使用して密封する。 </li></ol> 6。ナノVB 2 /空気電池のテスト<ol><li>製造プロセスが完了すると、放電ラックまたは電池ホルダーの場所細胞。 </li><li>各セルのセルが放電する前に平衡ことを確認するために10分の最初の残りステップを可能にする。 </li><li>放電バッテリーテスターを使用した3,000Ωの一定の負荷（または別の所望の負荷）の細胞。 </li><li>平衡化工程の後、開回路電位の測定を行う。 </li><li> 0.4 Vの停止電圧に達するまで、一定の負荷の下で放電してください。 </li><li>クーロン効率は、次いで4,060 kgでああ-1の理論アノード11電子放電容量と比較して測定された容量の割合を算出することができる。 </li></ol>

<ol>
	<li>Linden, D., Reddy, T. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of Batteries. , (2010).</li><li>Rogulski, Z., Czerwin'ski, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode+Modification+in+the+Leclanche'+Cell.">Cathode Modification in the Leclanche' Cell.</a> Journal of Solid State Electrochemistry. 7, 118-121 (2003).</li><li>Neburchilov, V., Wang, H., Martin, J. J., Qu, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+review+on+air+cathodes+for+zinc+-+air+fuel+cells.">A review on air cathodes for zinc - air fuel cells.</a> Journal of Power Sources. 195, 1271-1291 (2010).</li><li>Yu, X., Licht, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High+capacity+alkaline+super-iron+boride+battery.">High capacity alkaline super-iron boride battery.</a> Electrochimica Acta. 52, 8138-8143 (2007).</li><li>Licht, S., Wang, B., Ghosh, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Energetic+Iron(VI)+Chemistry:+The+Super-Iron+Battery.">Energetic Iron(VI) Chemistry: The Super-Iron Battery.</a> Science. 285, 1039-1042 (1990).</li><li>Licht, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+aluminum+batteries:+a+step+towards+derivation+of+superbatteries.">Novel aluminum batteries: a step towards derivation of superbatteries.</a> Colloids and Surfaces A: Physicochemical and Engineering Aspects. , 134-241 (1998).</li><li>Licht, S., Myung, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fluorinated+Graphites+as+Energetic+Cathodes+for+Nonaqueous+Al+Batteries.">Fluorinated Graphites as Energetic Cathodes for Nonaqueous Al Batteries.</a> Electrochem. Solid-State Lett. 5, A160-A163 (2002).</li><li>Licht, S., Ghosh, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High+power+BaFe(VI)O4/MnO2+composite+cathode+alkaline+super-iron+batteries.">High power BaFe(VI)O4/MnO2 composite cathode alkaline super-iron batteries.</a> Journal of Power Sources. 109, 465-468 (2002).</li><li>Licht, S., Myung, N., Peramunage, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultrahigh+Specific+Power+Electrochemistry,+Exemplified+by+Al/MnO4-+and+Cd/AgO+Redox+Chemistry.">Ultrahigh Specific Power Electrochemistry, Exemplified by Al/MnO4- and Cd/AgO Redox Chemistry.</a> The Journal of Physical Chemistry B. 102, 6780-6786 (1998).</li><li>Licht, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Aluminum/Sulfur+Battery+Discharge+in+the+High+Current+Domain.">Aluminum/Sulfur Battery Discharge in the High Current Domain.</a> J. Electrochem. Soc. 144, L133-L136 (1997).</li><li>Gao, X. -. P., Yang, H. -. X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multi-electron+materials+for+high+energy+density+batteries.">Multi-electron materials for high energy density batteries.</a> Energy and Environmental Science. 3, 174-189 (2010).</li><li>Yang, H. X., Wang, Y. D., Ai, X. P., Cha, C. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Metal+Borides:+Competitive+High+Capacity+Anode+Materials+for+Aqueous+Primary+Batteries.">Metal Borides: Competitive High Capacity Anode Materials for Aqueous Primary Batteries.</a> Electrochemical and Solid-State. 7, A212-A215 (2004).</li><li>Licht, S., Yu, X., Qu, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Novel+Alkaline+Redox+Couple:+Chemistry+of+the+Fe6+/B2-+Super-iron+Boride+Battery.">Novel Alkaline Redox Couple: Chemistry of the Fe6+/B2- Super-iron Boride Battery.</a> Chemical Communications. 2007, 2753-2755 (2007).</li><li>Licht, S., Wu, H., Yu, X., Wang, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Renewable+Highest+Capacity+VB2/Air+Energy+Storage.">Renewable Highest Capacity VB2/Air Energy Storage.</a> Chemical Communications. 2008, 3257-3259 (2008).</li><li>Light, S., Ghosh, S., Wang, B., Jiang, D., Asercion, J., Bergmann, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanoparticle+Facilitated+Charge+Transfer+and+Voltage+of+a+High+Capacity+VB2+Anode.">Nanoparticle Facilitated Charge Transfer and Voltage of a High Capacity VB2 Anode.</a> Electrochemical and Solid-State. 14, 83-85 (2011).</li><li>Licht, S., 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=Nano-VB2+Synthesis+from+Elemental+Vanadium+and+Boron:+Nano-VB2+Anode/Air+Batteries.">Nano-VB2 Synthesis from Elemental Vanadium and Boron: Nano-VB2 Anode/Air Batteries.</a> Electrochemical and Solid-State Letters. 15, A12-A14 (2012).</li></ol>

著者、クリスロードス、ルーベン·ロペス、Xuguang李、マヘーシュWaje、とマシューのマリングズはLynntech社の従業員である

このようにVB 2 /空気電池の建設は新たな大容量バッテリの可能性を可能にし、発生した分子の電荷移動当たり11電子を勉強し、プローブする機能を提供します。場合得られた結果は、キャップに活物質の均一な分散が存在すること、亜鉛陽極の材料の全てがバッテリから除去されたことを確認して、再現可能な結果を​​示さないため、細胞を適切にリークすることなく、任意に接着...

陽極としてバナジウムホウ 任意の負極材の最高容積充電容量の間で持っています。このプロトコルは、この魅力的な材料を研究するための方法を紹介します。金属亜鉛は5.8電気量L -1とそれぞれ820ああキロ-1、の亜鉛金属の高い二電子の体積と重量電荷蓄積容量に起因する水系主要システムにおける優勢なアノード材料となっています。として知られる*亜鉛カーボン電池、ルクランシェ電池は、最初に塩化物電解質1に二酸化マンガン（炭素集電体）カソードと亜鉛アノードを組み合わせることで、19 世紀に導入されました。一般的なアルカリ電池は、同じカップルを利用しますが、水酸化アルカリ電解液と塩化物電解質に置き換えられます。一緒に亜鉛炭素とアルカリ電池は一次電池の大部分を構成するには、1を売却した。アルカリ電池における二酸化マンガンのカソードが交換されると空気極によって、実質的に高いエネルギー貯蔵容量が達成される。この空気亜鉛電池は、空気から酸素を利用し、共通1-3補聴器電池に見出される。 より大容量のバッテリーストレージのため、Googleの検索は、分子4-11ごとに複数の電子を転送することができます材料に焦点を当てている。我々は検討されている酸化還元対の多種多様な中で、VB 2が 20.7電気量L -1の体積と重量容量を持つ、VB 2あたり11の電子を放出することが可能な臨時アルカリ陽極として際立っていると4060ああ、それぞれ-1キロ。で* 2004年、ヤンと共同研究者は、VB 2の排出を報告しただけでなく、VB 2はアルカリメディア12での腐食の影響を受けやすくなっている拡張ドメインを記録した。 2007年には、VB 2粒子でコーティングがVB 2 /空気Bのデモにつながる、この腐食13を防止することが報告2008年14 attery。 本稿では、VB 2 /空気電池に適用される以前に亜鉛/空気電池のために開発された技術を採用した新しい金属/空気システムを調査するために使用されるプロトコルを提示します。 nanoscopicVB 2アノードは増加し、バッテリ電圧とバッテリの負荷能力に-1キロ4060ああの理論的な固有の能力に近づい11電子酸化反応を示すことができる高エネルギーの高電力密度アノードとして提示される。 VB 2 /空気カップル亜鉛/空気電池1から抽出された同じ酸素空気カソードを採用し、KOH /水酸化ナトリウムのアルカリ電解液を使用しています。炭素電極触媒カソードは、放電中に消費されていません。 さらに、電池性能を向上させるために、より深い理解のために必要VB 2 /空気システムが存在する。ナノVB 2材料の特性と性能をtを用いて検討することができます亜鉛/空気電池15,16の彼はセル構成。電気化学試験は、ナノスケールのVB 2に対して実行することができます 様々な速度でのパーセント効率化によるパフォーマンスを比較することができます。

<table border="1">
	<tbody>
		<tr>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
			<td>MATERIALS</td>
		</tr>
		<tr>
			<td>Boron</td>
			<td>Alfa Aesar</td>
			<td>11337</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Diethyl Ether</td>
			<td>J.T. Baker</td>
			<td>9244-06</td>
			<td>4L</td>
		</tr>
		<tr>
			<td>Epoxy</td>
			<td>Loctite</td>
			<td>&nbsp;</td>
			<td>Heavy Duty 5 min setting time</td>
		</tr>
		<tr>
			<td>Isopropyl Alcohol</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Panasonic 675 Zinc/Air cell</td>
			<td>Panasonic</td>
			<td>PR675H</td>
			<td>Made in Japan (not German)</td>
		</tr>
		<tr>
			<td>C-NERGY Super C65</td>
			<td>Timcal</td>
			<td>&nbsp;</td>
			<td>Graphitic carbon black</td>
		</tr>
		<tr>
			<td>Vanadium</td>
			<td>Aldrich</td>
			<td>262935</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Vanadium Diboride</td>
			<td>American Elements</td>
			<td>12007-37-3</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Zirconium Chloride</td>
			<td>Spectrum</td>
			<td>Z20001</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
			<td>EQUIPTMENT</td>
		</tr>
		<tr>
			<td>50-mL round bottom flask</td>
			<td>Fisher Scientific Co LLC</td>
			<td>CG151001</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Diagonal cutting pliers</td>
			<td>Hardware store</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Hot/stir plate</td>
			<td>IKA</td>
			<td>C-MAG HS 7</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Glove box</td>
			<td>Labconco</td>
			<td>Precision Basic</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Ten 10-mm tungsten carbide balls</td>
			<td>Lab Synergy</td>
			<td>55.0100.08</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Tungsten carbide milling jar</td>
			<td>Lab Synergy</td>
			<td>50.8600.00</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Razor blade</td>
			<td>Hardware store</td>
			<td>&nbsp;</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Retsch PM 100 planetary ball mill</td>
			<td>Retsch</td>
			<td>205400003</td>
			<td>&nbsp;</td>
		</tr>
		<tr>
			<td>Stir bar</td>
			<td>VWR International</td>
			<td>58947-140</td>
			<td>&nbsp;</td>
		</tr>
	</tbody>
</table>

fabrication of vb2/air cells for electrochemical testing

新しいマルチ電子金属/空気電池システムの特性および性能を調査するための手法が提案され、提示されます。ナノVB 2を合成する方法は、放電時に安定化のためのVB 2粒子に酸化ジルコニウムコーティングを塗布するためだけでなく段階的な手順として提示される。既存の亜鉛/空気電池を分解するためのプロセスは、ナノVB 2アノードを有する従来の亜鉛/空気電池アノードに代わる新たな作用電極の付加構造において、示されている。最後に、完成したVB 2 /空気電池の放電が報告されます。我々はテストベッドとして、亜鉛/空気電池を使用して、高エネルギー、高容量ナノVB 2陽極の性能を研究する一貫性のある構成を提供することが有用であることを示している。

電気化学的試験は、VB 2 /空気電池の性能を決定するために行われる。複数のセルについて得られた結果は、電池性能の再現性の証拠を提供する。 図1は、3,000Ω（左）および1,000Ω（右）の放電時にVB 2 /空気電池とを比較する。放電電圧、ならびに4,060ああの割合が-1固有の容量をキログラムなお、巨視的VB 2陽極セルと比較してナノスケールのVB 2...

Watch this Scientific Journal Video about Fabrication of VB2/Air Cells for Electrochemical Testing at JoVE.com

Fabrication of VB2/Air Cells for Electrochemical Testing

プロトコルは、亜鉛/空気電池用に開発以前の技術を使用して、マルチ電子金属/空気電池システムを研究するために提示される。電気化学的テストは、パフォーマンスを評価するために作製した電池に対して行われる。

VBの作製<sub&gt; 2</sub電気テスト用&gt; /空気電池

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

fabrication-of-vb2air-cells-for-electrochemical-testing

Research

JoVE Journal

Engineering

Fabrication of VB2/Air Cells for Electrochemical Testing

11.8K ビュー.  The George Washington University. プロトコルは、亜鉛/空気電池用に開発以前の技術を使用して、マルチ電子金属/空気電池システムを研究するために提示される。電気化学的テストは、パフォーマンスを評価するために作製した電池に対して行われる。

ビデオ: Fabrication of VB2/Air Cells for Electrochemical Testing

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

リチウムイオン電池のコイン細胞の構築とテスト

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

工学

Fabrication and Testing of Microfluidic Optomechanical Oscillators

Cavity optomechanics experiments that parametrically couple the phonon modes and photon modes have been investigated in various optical systems including microresonators. However, because of the increased acoustic radiative losses during direct liquid immersion of optomechanical devices, almost all published optomechanical experiments have been performed in solid phase. This paper discusses a recently introduced hollow microfluidic optomechanical resonator. Detailed methodology is provided to fabricate these ultra-high-Q microfluidic resonators, perform optomechanical testing, and measure radiation pressure-driven breathing mode and SBS-driven whispering gallery mode parametric vibrations. By confining liquids inside the capillary resonator, high mechanical- and optical- quality factors are simultaneously maintained.

Parametric optomechanical excitations have recently been experimentally demonstrated in microfluidic optomechanical resonators by means of optical radiation pressure and stimulated Brillouin scattering. This paper describes the fabrication of these microfluidic resonators along with methodologies for generating and verifying optomechanical oscillations.

作製とマイクロ流体光力学発振器のテスト

Cavity optomechanics experiments that parametrically couple the phonon modes and photon modes have been investigated in various optical systems including ...

Fabrication Process of Silicone-based Dielectric Elastomer Actuators

This contribution demonstrates the fabrication process of dielectric elastomer transducers (DETs). DETs are stretchable capacitors consisting of an elastomeric dielectric membrane sandwiched between two compliant electrodes. The large actuation strains of these transducers when used as actuators (over 300% area strain) and their soft and compliant nature has been exploited for a wide range of applications, including electrically tunable optics, haptic feedback devices, wave-energy harvesting, deformable cell-culture devices, compliant grippers, and propulsion of a bio-inspired fish-like airship. In most cases, DETs are made with a commercial proprietary acrylic elastomer and with hand-applied electrodes of carbon powder or carbon grease. This combination leads to non-reproducible and slow actuators exhibiting viscoelastic creep and a short lifetime. We present here a complete process flow for the reproducible fabrication of DETs based on thin elastomeric silicone films, including casting of thin silicone membranes, membrane release and prestretching, patterning of robust compliant electrodes, assembly and testing. The membranes are cast on flexible polyethylene terephthalate (PET) substrates coated with a water-soluble sacrificial layer for ease of release. The electrodes consist of carbon black particles dispersed into a silicone matrix and patterned using a stamping technique, which leads to precisely-defined compliant electrodes that present a high adhesion to the dielectric membrane on which they are applied.

This manuscript shows the fabrication process for the manufacture of dielectric elastomer soft actuators based on silicone membranes. The three key stages of production are presented in detail: blade casting of thin silicone membranes; pad printing of compliant electrodes; and the assembly of all the components.

シリコーン系誘電エラストマーアクチュエータの製造工程

This contribution demonstrates the fabrication process of dielectric elastomer transducers (DETs). DETs are stretchable capacitors consisting of an ...

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.

プラズマトロン内のアブレーション材料試験中の放射分光境界層調査

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 ...

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.

電子衝撃イオン化のためのシャープフィールドエミッションポイントの電気化学エッチングとキャラクタリゼーション

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.

エキシプレックスからの安定した発光と白色発光電気化学セルの作製

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

Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering thermal wave fields that are disturbed by the defect. This effect is measured and used to locate the defect. We form the destructively interfering wave fields by using a modified projector. The original light engine of the projector is replaced with a fiber-coupled high-power diode laser. Its beam is shaped and aligned to the projector&#39;s spatial light modulator and optimized for optimal optical throughput and homogeneous projection by first characterizing the beam profile, and, second, correcting it mechanically and numerically. A high-performance infrared (IR) camera is set up according to the tight geometrical situation (including corrections of the geometrical image distortions) and the requirement to detect weak temperature oscillations at the sample surface. Data acquisition can be performed once a synchronization between the individual thermal wave field sources, the scanning stage, and the IR camera is established by using a dedicated experimental setup which needs to be tuned to the specific material being investigated. During data post-processing, the relevant information on the presence of a defect below the surface of the sample is extracted. It is retrieved from the oscillating part of the acquired thermal radiation coming from the so-called depletion line of the sample surface. The exact location of the defect is deduced from the analysis of the spatial-temporal shape of these oscillations in a final step. The method is reference-free and very sensitive to changes within the thermal wave field. So far, the method has been tested with steel samples but is applicable to different materials as well, in particular to temperature sensitive materials.

This method aims at locating vertical subsurface defects. Here, we couple a laser with a spatial light modulator and trigger its video input to heat a sample surface deterministically with two anti-phased modulated lines while acquiring highly resolved thermal images. The defect position is retrieved from evaluating thermal wave interference minima.

レーザー光熱サーモグラフィーを用いた構造化加熱による地中欠陥局在

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

その場でテスト用 LiPON ベース固体リチウム イオン Nanobatteries の集束イオンビーム ビーム加工

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in industry. The wettability of the produced surface was analyzed by bouncing drop experiments and the topography was analyzed by confocal microscopy. In addition, we show various methodologies to measure its durability and anti-icing properties. Superhydrophobic surfaces hold a special texture that must be preserved to keep their water-repellency. To fabricate durable surfaces, we followed two strategies to incorporate a resistant texture. The first strategy is a direct incorporation of roughness to the metal substrate by acid etching. After this surface texturization, the surface energy was decreased by silanization or fluoropolymer deposition. The second strategy is the growth of a ceria layer (after surface texturization) that should enhance the surface hardness and corrosion resistance. The surface energy was decreased with a stearic acid film.
The durability of the superhydrophobic surfaces was examined by a particle impact test, mechanical wear by lateral abrasion, and UV-ozone resistance. The anti-icing properties were explored by studying the ability to repeal subcooled water, freezing delay, and ice adhesion.

We illustrate several methodologies to produce superhydrophobic metal surfaces and to explore their durability and anti-icing properties.

防氷用超撥水の金属表面の作製

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in ...

Fabrication of an Optical Cell Dryer for the Spectroscopic Analysis Cells

Optical cells, which are experimental instruments, are small, square tubes sealed on one side. A sample is placed in this tube, and a measurement is performed with a spectroscope. The materials used for optical cells generally include quartz glass or plastic, but expensive quartz glass is reused by removing substances, other than liquids, to be analyzed that adhere to the interior of the container. In such a case, the optical cells are washed with water or ethanol and dried. Then, the next sample is added and measured. Optical cells are dried naturally or with a manual hairdryer. However, drying takes time, which makes it one of the factors that increase the experiment time. In this study, the objective is to drastically reduce the drying time with a dedicated automatic dryer that can dry multiple optical cells at once. To realize this, a circuit was designed for a microcomputer, and the hardware using it was independently designed and manufactured.

A protocol for fabricating a device for simultaneously drying multiple optical cells is presented.

光学セルの作製分光分析セル用ドライヤー

Optical cells, which are experimental instruments, are small, square tubes sealed on one side. A sample is placed in this tube, and a measurement is ...