Research at Argonne National Laboratory was funded by U.S. Department of Energy, FreedomCAR and Vehicle Technologies Office. Use of the Advanced Photon Source and research carried out in the Electron Microscopy Center at Argonne National Laboratory was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

使用前に、関連するすべての化学物質等安全データシート（MSDS）を参照してください。これらの合成に使用される化学物質のいくつかは、急性毒性及び発がん性があります。ナノ材料は、そのバルク対応物に比べて付加的な危険性を有していてもよいです。工学的制御（ヒュームフード、グローブボックス）および個人用保護具（安全眼鏡、手袋、白衣、完全長ズボン、閉じたつま先の靴）の使用を含むナノ結晶反応を行う際に、すべての適切な安全対策を使用してください。次の手順の一部は、標準的な空気のないハンドリング技術を含みます。 カソード材料の1の合成注：カソード材料は、原子層堆積又は湿式化学反応のいずれかによって合成することができます。 <ol><li> 原子層堆積（ALD） <ol><li> 12時間、磁気撹拌下、100ミリリットル1 MのKMnO 4溶液に多孔性炭素の5グラムを分散させます。 </li><li>目の100 mgのスプレッドeはALD装置のステンレススチールトレイ上にカーボン粉末を酸化し、トレイ上のステンレスメッシュカバーをクランプ。 </li><li> 30分間、1トルの圧力で300sccmの超高純度窒素キャリアガスの連続的な流れの下で200℃でトレイに炭素粉末を保持します。 </li><li>次のように完全なALDサイクルと炭素粉末を扱います。 注：このプロトコルにおける電極触媒の例として、パラジウムナノ粒子を取ります。試薬は、特定の要件に応じて変更することができます。さらに精製することなく受け取ったまま、全ての試薬が使用されます。 <ol><li> 100分間200℃で、パラジウムヘキサフルオロ炭素基板（100 mg）をパラジウム（Pd（HFAC）2、99.9％）を露出させます。 </li><li> 300分間の1トルの圧力で300sccmの超高純度窒素キャリアガスの連続的な流れとトレイをパージします。 </li><li> 100分間、200℃で（H 2 Oインチ％HCHO 37重量）ホルマリンに炭素基質を公開します。 </li><li>パージトン彼は、300分間の1トルの圧力で300sccmの超高純度窒素キャリアガスの連続流とトレイ。 </li></ol></li><li>必要に応じて、ALDサイクルを繰り返します。通常3-10繰り返し。 </li></ol></li><li> 湿式化学反応 注：このプロトコルにおける電極触媒の例として、鉄ナノ粒子を取ります。試薬は、特定の要件に応じて変更することができます。さらに精製することなく受け取ったまま、全ての試薬が使用されます。 <ol><li> 12時間、磁気撹拌下、100ミリリットル1 MのKMnO 4溶液に多孔性炭素の5グラムを分散させます。 </li><li>脱イオン水で酸化炭素を洗ってください。 </li><li>ガラス繊維を取り付けたフィルターフラスコで洗浄し、炭素をフィルタリングし、その後12時間110℃のオーブンでそれを乾燥させてください。 </li><li> 100ミリリットルの脱イオン水に乾燥したカーボンを分散させ、その後、磁気攪拌下でのFeCl 3の1グラムを追加します。 </li><li> 1MのNaOH溶液を用いて、約9のpH値を調整します。 </li><li> Rをかき混ぜます5時間スラリーをesulting、その後、ガラス繊維を取り付けたフィルターフラスコとのスラリーをフィルタリングします。 </li><li>脱イオン水とエタノールで製品を洗ってください。次いで、一晩110℃のオーブンで乾燥します。 </li><li>石英管炉内のH 2 /アルゴン混合物（4％のH 2）の連続流で450℃で生成物を加熱処理します。 5時間、100ml /分の流速を使用。 </li></ol></li></ol>電極と電解質の調製<ol><li> 陰極 <ol><li> 1の重量比：4のように調製したカソード材料を混合し、バインダー、ポリ（フッ化ビニリデン）（PVDF）。 注：混合物の合計は、カソードの量に依存します。各片の陰極材料の負荷は、0.1ミリグラムの範囲です。 </li><li>混合物に1-メチル-2-ピロリジノン（NMP）を追加し、さらにテクスチャスラリーを作るためによくかき混ぜます。混合物の約3倍の重量でNMPを追加します。 </li><li>炭の上にコートスラリー100μmの周りの厚さでドクターブレードにより、n個の紙。 </li><li>一晩、100℃の真空オーブン中で積層体を乾燥させます。 </li><li> 7/16インチの直径に穴パンチャーとディスクへのラミネートをパンチし、それを量ります。 </li></ol></li><li> 非プロトン性電解質 <ol><li>一晩100℃で真空オーブン中で乾燥したトリフルオロメタンスルホン酸リチウム（LiCF 3 SO 3）。 </li><li>テトラエチレングリコールジメチルエーテル中のSO 3 LiCF 3を乾燥追加、塩が溶解するまで1モル/ Lの濃度（TEGDME H 2 O〜10 ppm）を、次いで、磁気攪拌しながら、溶液をかき混ぜます。 </li><li> Arで満たされたグローブボックス内で電解質を保ちます。 </li></ol></li><li> アノード <ol><li> 7/16インチの直径に穴パンチャーとディスクへのリチウム箔/チップをパンチ。 </li></ol></li></ol> 3.電気化学的試験<ol><li> スウェージロックセルのアセンブリ&lt;/強いです&gt; 注意：アセンブリのすべてのステップは3.1.9を除いて、アルゴンを充填したグローブボックス内で動作されます。 <ol><li> 図1aに示すように、スウェージロックセットを組み立てます。アノード端を締め、およびカソード端を緩めます。 </li><li>アノード端のステンレス鋼棒の上にリチウム金属チップ（直径7/16インチ）の作品を置きます。 </li><li>リチウム金属負極の上にガラス繊維セパレータ（直径1/2インチ）の作品を置きます。 </li><li>完全にガラス繊維セパレータを濡らすために、電解質の5-7滴を追加します。ゆっくりと気泡を除去するために、セパレータを押してください。 </li><li>アノードに面した活物質で、湿らせたセパレータの上に陰極の一部を入れてください。 </li><li>アルミメッシュ（直径7/16インチ）の一部とカソードをカバーしています。 </li><li>プレスアルミニウム管と上記の層は、その後、カソード端を締めます。 </li><li>に示すように、ガラスチャンバー内の全スウェージロックセルを密閉し、クランプでチャンバーを修正<st栄&gt;図1。 </li><li>グローブボックスの外にセル全体を取ります。超高純度の酸素タンクにガラス容器を接続し、そして30分間、1気圧での連続酸素流とそれをパージ。 </li></ol></li><li> バッテリーの性能テスト <ol><li> 25℃にサーモスタットを設定します。 </li><li>サーモスタットへの細胞と電極（ケーブルで機器に接続された電子クリップ）を入れて、それらを修正。 </li><li>電子クリップを対応するガラスチャンバー上に陰極と陽極をクリップ。 </li><li>バッテリテストシステムのオペレーティングソフトウェアを開き、ケーブルで接続されたチャネルを選択します。 </li><li>電気化学的試験の手順を設定します。 注：100ミリアンペア/グラム活物質の電流密度を設定し、2.2から4.5 Vの電圧範囲<ol><li>放電試験用の2.2 Vの放電終止電圧を設定します。 </li><li>容量制御サイクル試験のために5または10時間の放電/充電ステップ時間を設定します。 </李&gt; <li>電圧制御サイクル試験用に2.2 Vの放電終止電圧は4.5 Vの充電終止電圧を設定します。 </li></ol></li><li>ソフトウェアインターフェイス上で「実行」ボタンをクリックして手順を実行します。 </li></ol></li><li> セルの分解掃除 <ol><li>グローブボックス内のセルを分解します。 </li><li>以下の特徴付けのためのガラスバイアル内の電極を保管してください。グローブボックスの外に他の細胞部分を転送します。 </li><li>ビーカーにアセトン溶液（〜20％）または脱イオン水にスウェージロック部品、ステンレス鋼棒、アルミチューブ、アルミメッシュを入れ、15〜30分間、超音波でそれらをきれいに。 </li><li> 60〜80℃に設定したサーモスタットで部品やガラス室を乾燥させます。 </li></ol></li></ol>特性評価試験片の4準備注意：試料は空気のために（のように調製した材料のための）フードまたはArで満たされたグローブボックス（に用意されています敏感な標本）。 <ol><li> SEMおよびXPS用の試験片 <ol><li>試料ステージ上にカーボンテープを貼り付けます。カーボンテープは、試料片として試料台と大きく、又は小さくすることができます。 </li><li> 5ミリメートル約2標本の一部をカットし、カーボンテープに貼り付け。 注意：試料は、任意の非磁性サンプルすることができます。電気化学試験後の試験片については、カーボンテープにスティック前に、電解質溶媒でそれらを洗ってください。 </li><li>測定前にメイソンジャー内の空気に敏感な標本を封印。 </li><li>製造元の指示に従ってSEM 34-36またはXPS 37,38を操作してください。 </li></ol></li><li> TEM用の試験片 <ol><li>試料粉末のミル1ミリグラム。 注：電極検体の場合、製粉前にカーボン紙を活性材料を削り取ります。 </li><li>銅グリッド上に試料粉末をロードし、ルースパウダーを削除します。 </li><li>銅グラムをロードしますTEM試料ホルダに取り除きます。 注：空気に敏感な試料に対してできるだけ速く行われ、このステップを取得します。 </li><li> TEMを実行します。39-41 </li></ol></li><li> 高エネルギーX線回折用の試験片 <ol><li> 粉末試料 <ol><li>粘土または接着剤によって、ポリイミドチューブの一端をシール。 </li><li>チューブ内に粉末をロードします。 </li><li>チューブのもう一方の端をシールします。 </li></ol></li><li> ディスク試験片 注：電極上に活物質を測定するために、別のオプションは、カーボン紙を、それらを掻き落とし、ステップ4.3.1に従うことです。 <ol><li>ポリアミドテープの切れ端でサンプル作品を封印。テープの一片の中央に試料を入れ、テープの別の部分でそれらを覆うことによってシールします。 注：電気化学試験後の試料について、封止前の電解質溶媒でそれらを洗ってください。 </li></ol></li><li>高度なpHの高エネルギーX線回折42-44を操作アルゴンヌ国立研究所でソースoton。 </li></ol></li><li> XANESのための試験片 <ol><li> 粉末試料 <ol><li>測定元素の濃度は、希釈剤として窒化ホウ素（BN）、またはカーボンブラックのいずれかを使用して、高い場合、サンプルを希釈します。ここでは、3-5重量に希釈します。 ％。 </li><li> 、7ミリメートルの直径と1mm程度の厚さでディスクへの粉末を押すとKBrプレスキットを使用し、7ミリメートルは、ダイセット。 </li><li>ウィンドウフィルムを使用してディスクを封印。 </li></ol></li><li> ディスク試験片 <ol><li>ウィンドウフィルムで試料を密封します。 </li></ol></li><li>高エネルギーは、アルゴンヌ国立研究所で光量子ソースで45-47 XANES操作してください。 </li></ol></li><li> ATR-FTIRのための試験片 <ol><li>前と測定後のダイヤモンド減衰全反射（ATR）ユニットを清掃してください。 </li><li>興味のあるすべてのサンプルについてのダイヤモンドのユニットに検体を入れてください。 </li><li> ATR-FTIR分光法を実行します。48,49 </li></ol></li><li> ラマンスペクトルのための試験片 <ol><li>平板上に試料を入れて（ガラス、ステンレス鋼、 など 。）。 </li><li>カバースライドで試料をカバーしています。 </li><li>空気に敏感なサンプル用のセットを封印。 </li><li>ラマン分光法を実行します。50,51 </li></ol></li></ol>

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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=Molecular-Level+Insights+into+the+Reactivity+of+Siloxane-Based+Electrolytes+at+a+Lithium-Metal+Anode.">Molecular-Level Insights into the Reactivity of Siloxane-Based Electrolytes at a Lithium-Metal Anode.</a> ChemPhysChem. 15, 2077-2083 (2014).</li><li>Du, P., 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=Compatibility+of+lithium+salts+with+solvent+of+the+non-aqueous+electrolyte+in+Li-O2+batteries.">Compatibility of lithium salts with solvent of the non-aqueous electrolyte in Li-O2 batteries.</a> Phys. Chem. Chem. Phys. 15, 5572-5581 (2013).</li><li>Aleshin, G. Y., 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=Protected+anodes+for+lithium-air+batteries.">Protected anodes for lithium-air batteries.</a> Solid State Ion. 184, 62-64 (2011).</li><li>Assary, R. 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C., 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=Theoretical+Exploration+of+Various+Lithium+Peroxide+Crystal+Structures+in+a+Li-Air+Battery.">Theoretical Exploration of Various Lithium Peroxide Crystal Structures in a Li-Air Battery.</a> Energies. 8, 529-548 (2015).</li><li>Black, 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=Screening+for+Superoxide+Reactivity+in+Li-O2+Batteries:+Effect+on+Li2O2/LiOH+Crystallization.">Screening for Superoxide Reactivity in Li-O2 Batteries: Effect on Li2O2/LiOH Crystallization.</a> J. Am. Chem. Soc. 134, 2902-2905 (2012).</li><li>Gallant, B. M., 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=Influence+of+Li2O2+morphology+on+oxygen+reduction+and+evolution+kinetics+in+Li-O2+batteries.">Influence of Li2O2 morphology on oxygen reduction and evolution kinetics in Li-O2 batteries.</a> Energy Environ. Sci. 6, 2518-2528 (2013).</li><li>Lu, J., 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=Magnetism+in+Lithium-Oxygen+Discharge+Product.">Magnetism in Lithium-Oxygen Discharge Product.</a> ChemSusChem. 6, 1196-1202 (2013).</li><li>Xu, J. -. J., Wang, Z. -. L., Xu, D., Zhang, L. -. L., Zhang, X. -. 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X-Ray Photoelectron Spectrometer Operation Procedure Available from: <a target="_blank" href="https://nanofabrication.4dlabs.ca">https://nanofabrication.4dlabs.ca</a> (2015)</li><li>Haasch, R. T., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 93-132 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> JEM-2100F Field Emission Transmission Electron Microscope. , (2015).</li><li>Wen, J. -. G., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 189-229 (2014).</li><li>Williams, D. B., Carter, C. 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R., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 1-41 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 9-BM-B,C: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 20-BM-B: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>Bunker, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy. , (2010).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet FT-IR User's Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet iS5 User Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw inVia Raman Microscope Training Notebook. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw InVia Quick Operation Summary. , (2015).</li><li>Mitchell, R. 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The authors have nothing to disclose.

空気へのLi-O 2電池システムの感度を考慮すると、特にCO 2および湿度、プロトコルのステップの多くは、干渉を低減し、副反応を避けるために必要です。例えば、スウェージロック型の細胞はO 2 &lt;0.5ppmの及びH 2 O &lt;0.5 ppm以下でアルゴンを充填したグローブボックス内で組み立てられます。そして、すべてのカソード材料、電解質溶媒及び塩、ガラス繊維、ス...

1996年に、アブラハムと江1は、多孔質炭素陰極、有機電解液、およびLi-金属アノードから成る第一の可逆非水性のLi-O 2バッテリーを報告しました。それ以来、何らかの他の既存のエネルギー貯蔵システムのそれを超えて、非常に高い理論エネルギー密度に、アノードにおけるリチウムの酸化による電流の流れとカソードにおける酸素の還元を（誘導のLi-O 2電池全体の反応のLi + + O 2 + E - ↔のLi 2 O 2）は 、最近大きな関心を受けている1-8。 次の要件を有するカソード材料は、Li-O 2電池の高性能化のニーズに応えることができるだろう：（1）高速酸素拡散。 （2）良好な電気およびイオン伝導性を。 （3）高比表面積; （4）安定性。両方のカソードの表面積及び気孔率は、のために重要です。リチウムO 2電池の電気化学的性能9-12多孔質構造は、O 2でのLiカチオンの反応から生成された固体の放電生成物の付着を可能にします。より大きな表面積は、電気化学反応を促進電気触媒粒子を収容するためにそれ以上の活性部位を提供します。このような電極触媒は、13-17。基板の元の多孔質表面構造の保存と、基板と触媒粒子の良好な制御に強い接着を提供する特定の堆積法によってカソード材料に添加されるように調製された材料は、試験されます非プロトン性のLi-O 2電池のカソードとしてスウェージロック型細胞です。しかし、電池の性能は、カソード材料の性質に依存するだけでなく、非プロトン性電解質18〜22とリチウム金属アノードの種類のみならず。23-26より影響は、材料の量および濃度を含み、そしてP充電/放電試験に用いrocedure。適切な条件およびプロトコルを最適化し、電池材料の全体的な性能を向上させるであろう。 電気化学的試験の結果に加えて、電池性能にも自然のままの材料との反応生成物を特徴づけることによって評価することができる。27-33走査電子顕微鏡（SEM）は、カソード材料の表面の微細構造および形態を調査するために使用され放電生成物の進化。透過型電子顕微鏡（TEM）エッジ構造（XANES）の近くに、X線吸収、及びX線光電子分光法（XPS）は、特に、触媒ナノ粒子のために、素子の超微細構造、化学的状態、およびコンポーネントを決定するために用いることができます。高エネルギーX線回折（XRD）を直接結晶放電生成物を識別するために使用されます。可能な電解液の分解は減衰全反射フーリエ変換によって決定することができる変換赤外線（ATR-FTIR）及びラマンスペクトル。 この記事では、電池材料および付属品の準備、電気化学的性能試験、自然のままの材料および反応生成物の特性を含む非プロトン性のLi-O 2電池の通常の試験の体系的かつ効率的な配置を示しているプロトコルです。詳細なビデオプロトコルは、フィールドに新しい実践者は、Li-O 2電池の性能試験および特性評価に関連した多くの一般的な落とし穴を避けるのを助けることを意図しています。

<table><tbody><tr><td>1-Methyl-2-pyrrolidinone (NMP), 99.5%</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>Battery test system</td><td>MACCOR</td><td>Series 4000 Automated Test System</td><td></td></tr><tr><td>Dimethyl carbonate (DMC), &amp;ge;99%</td><td>Sigma-Aldrich</td><td>517127</td><td></td></tr><tr><td>Ethyl alcohol, &amp;ge;99.5%</td><td>Sigma-Aldrich</td><td>459844</td><td></td></tr><tr><td>Formaldehyde solution, 37 wt. % in H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>252549</td><td></td></tr><tr><td>Graphitized Carbon black, &gt;99.95%</td><td>Sigma-Aldrich</td><td>699632</td><td></td></tr><tr><td>Iron(III) chloride (FeCl&lt;sub&gt;3&lt;/sub&gt;), 97%</td><td>Sigma-Aldrich</td><td>157740</td><td></td></tr><tr><td>Kapton polyimide tubing</td><td>Cole-Parmer</td><td>EW-95820-09</td><td></td></tr><tr><td>Kapton polymide tape</td><td>Cole-Parmer</td><td>EW-08277-80</td><td></td></tr><tr><td>Kapton window film</td><td>SPEX Sample Prep</td><td>3511</td><td></td></tr><tr><td>Lithium Chip (99.9% Lithium)</td><td>MTI Corporation</td><td>EQ-Lib-LiC25</td><td></td></tr><tr><td>Lithium trifluoromethanesulfonate (LiCF&lt;sub&gt;3&lt;/sub&gt;SO&lt;sub&gt;3&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>481548</td><td></td></tr><tr><td>Palladium hexafluoroacetylacetonate (Pd(hfac)&lt;sub&gt;2&lt;/sub&gt;), 99.9%</td><td>Aldrich</td><td>401471</td><td></td></tr><tr><td>Poly(vinylidene fluoride) (PVDF)</td><td>Aldrich</td><td>182702</td><td></td></tr><tr><td>Potassium permanganate (KMnO&lt;sub&gt;4&lt;/sub&gt;), &amp;ge;99.0%&amp;nbsp;</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Sodium hydroxide (NaOH), &amp;ge;97.0%</td><td>Sigma-Aldrich</td><td>221465</td><td></td></tr><tr><td>Tetraethylene glycol dimethyl ether (TEGDME), &amp;ge;99%</td><td>Aldrich</td><td>172405</td><td></td></tr><tr><td>Toray 030 carbon paper</td><td>ElectroChem Inc.</td><td>590637</td><td></td></tr></tbody></table>

protocol of electrochemical test and characterization of aprotic li-o2 battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

図1aは、Li-O 2バッテリテストのスウェージロック型セルのセットアップを示しています。リチウムフィルム片は、アノード側に、ステンレス鋼棒上に配置されます。多孔質カソードは、アルミニウム管を通って、純粋なO 2に開放されています。ガラス繊維は、セパレータと、非プロトン性電解質の吸収材として使用されます。そして、Al?...

Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

非プロトン性のLi-Oの電気化学的試験のプロトコルとキャラクタリゼーション<sub&gt; 2</sub&gt;バッテリー

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

protocol-electrochemical-test-characterization-aprotic-li-o2

Universidad San Sebastian

Research

JoVE Journal

Engineering

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

11.4K ビュー.  Argonne National Laboratory. A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here. 

ビデオ: Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

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

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

放射光技術を用いたリチウムイオンとナトリウムイオン電池用電極材料のキャラクタリゼーション

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational analysis. Testing of lithium-ion batteries in an academic setting has taken on several forms, but at the most basic level lies the coin cell construction. In traditional LIB electrode preparation, a multi-phase slurry composed of active material, binder, and conductive additive is cast out onto a substrate. An electrode disc can then be punched from the dried sheet and used in the construction of a coin cell for electrochemical evaluation. Utilization of the potential of the active material in a battery is critically dependent on the microstructure of the electrode, as an appropriate distribution of the primary components are crucial to ensuring optimal electrical conductivity, porosity, and tortuosity, such that electrochemical and transport interaction is optimized. Processing steps ranging from the combination of dry powder, wet mixing, and drying can all critically affect multi-phase interactions that influence the microstructure formation. Electrochemical probing necessitates the construction of electrodes and coin cells with the utmost care and precision. This paper aims at providing a step-by-step guide of non-aqueous electrode processing and coin cell construction for lithium-ion batteries within an academic setting and with emphasis on deciphering the influence of drying and calendaring.

Non-aqueous electrode processing is central to the construction of coin cells and the evaluation of new electrode chemistries for lithium-ion batteries. A step-by-step guide to the basic practices needed as an electrochemical engineer working with batteries in an academic experimental setting is furnished.

リチウムイオンコイン電池の非水系電極加工および建設

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

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 ...

化学

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

イオン液体系電解質、リチウムイオン電池の組立、および高温でのパフォーマンスの測定の合成

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

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 ...

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate multiple processes responsible for long-term performance decay. Given the complexity of physical processes occurring inside the cell, it is often challenging to achieve a full understanding of the root causes of this performance degradation. This difficulty arises in part from the fact that any electrochemical measurement of a battery will return the combined contributions of all components in the cell. Incorporation of a reference electrode can solve part of the problem, as it allows the electrochemical reactions of the cathode and the anode to be individually probed. A variation in the voltage range experienced by the cathode, for example, can indicate alterations in the pool of cyclable lithium ions in the full-cell. The structural evolution of the many interphases existing in the battery can also be monitored, by measuring the contributions of each electrode to the overall cell impedance. Such wealth of information amplifies the reach of diagnostic analysis in Li-ion batteries and provides valuable input to the optimization of individual cell components. In this work, we introduce the design of a test cell able to accommodate multiple reference electrodes, and present reference electrodes that are appropriate for each specific type of measurement, detailing the assembly process in order to maximize the accuracy of the experimental results.

The incorporation of reference electrodes in a Li-ion battery provides valuable information to elucidate degradation mechanisms at high voltages. In this article, we present a cell design that accommodates multiple reference electrodes, along with the assembly steps to assure maximum accuracy of the data obtained in electrochemical measurements.

Operando のインピー ダンス分光法の 4 電極設計場前記参照電極。

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

The Effect of Charging and Discharging Lithium Iron Phosphate-graphite Cells at Different Temperatures on Degradation

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. The degradation of the cells is assessed by using 10 charging and discharging temperature permutations ranging from -20 &#176;C to 30 &#176;C. This allows an analysis of the effect of charge and discharge temperatures on aging, and their associations. A total of 100 charge/discharge cycles were carried out. Every 25 cycles a reference cycle was performed to assess the reversible and irreversible capacity degradation. A multi-factor analysis of variance was used, and the experimental results were fitted showing: i) a quadratic relationship between the rate of degradation and the temperature of charge, ii) a linear relationship with the temperature of discharge, and iii) a correlation between the temperature of charge and discharge. It was found that the temperature combination for charging at +30 &#176;C and discharging at -5 &#176;C led to the highest rate of degradation. On the other hand, the cycling in a temperature range from -20 &#176;C to 15 &#176;C (with various combinations of temperatures of charge and discharge), led to a much lower degradation. Additionally, when the temperature of charge is 15 &#176;C, it was found that the degradation rate is nondependent on the temperature of discharge.

This article describes the effect of dissimilar charging/discharging temperatures on the degradation of lithium iron phosphate-graphite pouch cells, aiming at simulating close to real case scenarios. In total, 10 temperature combinations are investigated in the range -20 to 30 &#176;C in order to analyze the impact of temperature on degradation.

急速な充放電リチウム鉄リン酸グラファイト電池劣化で異なる温度での効果

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

3 電極コイン セル準備およびリチウム イオン電池用電着分析

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...

非プロトン性のLi-Oの電気化学的試験のプロトコルとキャラクタリゼーション

要約

さらに動画を探す

この動画の章

リチウムイオン電池のコイン細胞の構築とテスト

放射光技術を用いたリチウムイオンとナトリウムイオン電池用電極材料のキャラクタリゼーション

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

リチウムイオンコイン電池の非水系電極加工および建設

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

イオン液体系電解質、リチウムイオン電池の組立、および高温でのパフォーマンスの測定の合成

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

Operando のインピーダンス分光法の 4 電極設計場前記参照電極。

急速な充放電リチウム鉄リン酸グラファイト電池劣化で異なる温度での効果

3 電極コインセル準備およびリチウムイオン電池用電着分析

非プロトン性のLi-Oの電気化学的試験のプロトコルとキャラクタリゼーション

要約

さらに動画を探す

この動画の章

リチウムイオン電池のコイン細胞の構築とテスト

放射光技術を用いたリチウムイオンとナトリウムイオン電池用電極材料のキャラクタリゼーション

シンクロトロンベースのハードX線マイクロトモグラフィーを用いて電池の故障解析

リチウムイオンコイン電池の非水系電極加工および建設

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

イオン液体系電解質、リチウムイオン電池の組立、および高温でのパフォーマンスの測定の合成

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

Operando のインピー ダンス分光法の 4 電極設計場前記参照電極。

急速な充放電リチウム鉄リン酸グラファイト電池劣化で異なる温度での効果

3 電極コイン セル準備およびリチウム イオン電池用電着分析

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

Operando のインピーダンス分光法の 4 電極設計場前記参照電極。

3 電極コインセル準備およびリチウムイオン電池用電着分析