この作品は、財政的にテキサスA＆M大学教員の研究開始許可（ムカジー）とテキサス州立大学起動資金（ローズ）でサポートされています。

このプロトコルで利用される溶媒、試薬、または乾燥粉末のいずれかを使用する場合には注意が必要です。すべてのMSDSシートを読み、適切な安全対策をとります。標準的な安全装置は、手袋、安全眼鏡、と白衣が含まれています。 1.カソードの準備注：陰極の製造工程の概略を図1に示されています。 <img alt="図1" src="/files/ftp_upload/53490/53490fig1.jpg" /> 図1.カソードを作成するETSLで利用手順の概略図。メインプロセスはコイン細胞に電極シートおよび組み込みの乾燥し、洗浄アルミニウム基板上に電極スラリーの製造及び鋳造が含まれています。 <a href="https://www.jove.com/files/ftp_upload/53490/53490fig1large.jpg" target="_blank">こちらをクリックしてください。大きなVeを見ます</a>この図のrsion。 <ol><li> アルミニウム基板の準備 <ol><li>カット「12による「4.5ペーパーカッターやハサミを使って厚さ15μmのアルミニウム（Al）箔のシート。 </li><li>ボードに箔を接着した後、基板に箔シートを配置するためにクリーンなプラスチック板の表面にアセトンをスプレーします。 </li><li>箔の表面にアセトンの寛大な量をスプレーし、小さな半円形の動きとスコッチパッドを使用して表面全体をスクラブし始めます。表面に追加のアセトンをスプレーし、ペーパータオルで残留物を拭いてください。 </li><li>反対側のための手順を1.1.2-1.1.3繰り返した後、鋳造側のためもう一度繰り返します。 </li><li>洗浄フリップフロッと反対側で繰り返し、次いで、第一の側面の鋳造に脱イオン（DI）水を用いてアルミニウムシートをエッチングします。 DI水が悪い湿潤性を表示し、液滴を形成することなく、シートの表面から流れないようにAl箔の表面を再スクラブ。イソプロピルでリンスを繰り返しアルコール。 </li><li> 2紙タオルの間に洗浄のAlシートを移し、2つの平坦面と紙タオルの間に圧縮状態で約20分間乾燥させます。 </li></ol></li><li> スラリー調製 <ol><li>電極シートの所望の組成に基づき、活物質、導電助剤及び結着剤の重量を選択してください。 （70重量％のリチウム-マンガン-コバルト酸化物、マンガンのLiNi 1/3 1/3 Co 1/3 O 2（NMC、活物質）、20重量％のカーボンブラック、導電性の1.25グラムの総乾燥粉末重量を選択します添加剤）および10％ポリビニリデンジフルオリド（PVDFバインダー）。 </li><li> NMCのうち0.875グラムとめのう乳鉢と乳棒にカーボンブラックと場所の0.25グラムを測定します。軽く研削せずに材料を一緒に混ぜます。混合物を均一な粉末が視覚的に観察されるまで、3〜5分間、乳鉢と乳棒で手でミルを形成するために開始された後。 </li><li>使い捨てミキシングチューブに混合粉末を移します秤量紙の切れ端で。 1-メチル-2-ピロリジノンを5.5 mlの（NMP）、非水性溶媒と一緒に、粉末16のガラス球（直径6mm）を加えます。 </li><li>管駆動ステーションに使い捨てチューブを置き、所定の位置にロックします。ドライブの電源を入れ、ゆっくりと最高速度まで上昇。内容は15分間混合することができます。 </li><li>チューブに直接NMP溶液中で10％のPVDFの1.25グラムを追加します。 1.2.4での同様の手順で、バックドライブにチューブを置き、8分間の混合を可能にします。チューブは、従来（下）鋳造に5分以上放置された場合、さらに15分間内容物を混合します。 </li></ol></li><li> 鋳造および乾燥 <ol><li>イソプロピルアルコール、ペーパータオルで自動フィルムアプリケーターの金属表面を清掃してください。ドクターブレードがきれいで、希望鋳造の高さ（200ミクロン）に設定されていることを確認してください。 </li><li>フィルムアプリケーターの表面にイソプロピルアルコールの層を適用し、DRIを配置EDのアルミニウム基板表面に光沢のあるダウンサイド。すべてのしわ及びイソプロピルが削除されるまで折り畳まれた紙タオルで過剰のイソプロピルアルコールを押します。しっかりと所定の位置に基板のいずれかを保持することにより、基板を引き裂くないように注意してください。 </li><li>チューブドライブから混合管を外し、コンテナを開きます。約1インチ基板の上面（初期鋳造側）2から3インチラインの基板の表面にスラリーを注ぎます。きれいな金属ピンセットでシートから任意のガラスのボールを削除します。 </li><li> 20ミリメートル/秒に鋳造速度を設定し、フィルムアプリケーターの鋳造アームを活性化させます。 </li><li>しわがシートに形成されない保証するために、段ボールの薄片を用いたフィルムアプリケーターの表面からキャスト電極を持ち上げます。 </li><li>電極シートを室温で16時間乾燥することができます（〜24℃）〜3時間またはシートが乾燥するまで70℃で乾燥しました。電極はFUで、環境的に絶縁されていることを確認してください私は、フードまたは不均一な乾燥を防ぐために密閉室。 </li></ol></li><li> カソード電極パンチング <ol><li>アルミニウム金属の洗浄シート上に乾燥した電極シートを配置します。のエッジの周りの圧力を½ &quot;穴パンチを、均一な表面とシートの領域にそっと置きます（エッジが不均一に表示される場合があります）。ゆっくりと（手で）パンチに圧力を適用し、「取り出しロール」きれいにカットを確保するためのパンチ。 </li><li> （代替）マニュアルパンチングの代わりに正確なディスクカッターを利用した電極板を切り取り。 </li><li>洗浄、プラスチックピンセットでシートから電極を外し、電極表面を上に向けて、標識されたバイアル中に配置します。二回繰り返します。 </li><li> （オプション）ラボ機の表面にパンチング電極を配置します。およそ4 MPaの（最適な圧力を利用プレスによって異なります）の圧力を適用します。残りの電極について、この手順を繰り返します。 </li><li>バキュにバイアルを置きますええとオーブン、残りの水分を除去する12時間-0.1 MPaので120℃での電極は、さらに乾燥することができます。後、電極を除去し、0.0001グラム内でそれらの重量を量ります。 </li><li>グローブボックスの副室を開き、トレイにバイアルを置きます。室にドアを閉じて、準備室のハッチを締め2本の指を使って、気密シールを確保します。 </li><li>ダウン-0.1 MPaのに真空を持参した後、アルゴンを充填。グローブボックス内に搬入サンプルに応じて、このプロセスを1-2回繰り返します。 </li></ol></li></ol>全セルのた​​めの2アノードシート<ol><li>代わりに、アルミニウム箔の基材として厚さ9μmの銅箔を用いた以外は繰り返しセクション1。シートの組成物は、特定のニーズに合うように変更することができます。 </li></ol> 3.コイン電池プレアセンブリ 注意：コイン電池の構成はグローブボックス内の不活性（アルゴン）環境内で実行されます。 Eエクストリームの注意が外部雰囲気に内部環境の露出を最小限に抑えるように注意する必要があります。可能な場合は、グローブボックス内に鋭い材料との作業は最小限にすべきです。一般的な規則として、グローブボックス内のタスクは、タスクの外部で実行されるであろう速度よりも3倍の時間を取る必要があります。手袋はまた、異なる物質で作業するときの露出を最小限にするためにグローブボックス用手袋の上から着用する必要があります。 注意：このような（部品配置のための）プラスチックピンセットなどのツールキャップ、ケース、波バネ、 ​​ガスケット、スペーサー、リチウムリボン、電解質を含む残りのコイン電池の構築に必要なコンポーネントは、アルゴンを充填したグローブボックス内に含まれています万人あたり0.5部未満に維持し、O 2とH 2 Oのレベルを持ちます。 （リントフリーのタスクワイプを含む）をグローブボックスに挿入されたすべてのコンポーネントがどれかを削除するには-0.1 MPaの圧力で120℃の真空オーブン中でO / N加熱しなければなりません水分。 <ol><li> 対向電極の作製 <ol><li>グローブボックス内では、密閉された容器から（0.75 mm厚）リチウムリボンを削除し、プラスチックブロックの表面に一部をロールアウト。カミソリの刃を使用して、慎重に箔表面からの黒色の酸化を削り取ります。手袋を切断避けるために細心の注意を払ってください。 </li><li> 9/16「穴パンチを取り、リチウムリボンのディスクをパンチアウト。パンチのうち、リチウムディスクをプッシュする（グローブボックス内のゴム手袋によりリチウムから分離された）人間の指など、鈍いツールを使用します。 </li><li>厚さ0.5mmのスペーサーを取り、ゆっくりと指の間の表面にリチウムディスクを適用します。スペーサーの中心にリチウムディスクスティックを確認し、平坦である - 不均一な表面に凹凸電流分布を引き起こす可能性があります。 </li></ol></li><li> 電解質の準備 <ol><li> （：1容量EC / 12月1日で、この場合の1 MのLiPF 6）を選択した電解質を保存電解質としてアルミニウム容器で常にグローブボックス内に感光性です。 </li><li>作業容器内に、原料容器から電解液の少量を削除します。 </li></ol></li><li> セルガードセパレータの準備 <ol><li>プリンタ用紙の折りシートとの間にセパレータ膜のシートを配置します。アルミニウム金属のシートに折り畳まれた紙と膜を配置します。 </li><li>穴パンチの上にクッション層を配置し、¾ &quot;直径のセパレータ膜をパンチするためにハンマーを使用しています。 </li><li> 1.4.6-1.4.7で説明した手順を利用し、グローブボックスに打ち​​抜いたセパレータディスクを転送します。 注意：これは、構築されている各コイン電池のための個々のセパレータをパンチアウトすることを避けるために大量にこのステップを実行することをお勧めします。 </li></ol></li></ol> 4.コイン電池組立 注意：コイン電池の構成は図2に示します 。 <img alt="図1" src="/files/ftp_upload/53490/53490fig2.jpg" /> 図セル内の配置順に表示2.コイン電池部品。カソードの配置はセルのシールが続くと、セパレータ、ガスケット、対極及びウェーブスプリングが続いている。 <a href="https://www.jove.com/files/ftp_upload/53490/53490fig2large.jpg" target="_blank">この図の拡大版を表示するには、こちらをクリックしてください。</a> <ol><li>インテリア控えの間の扉を開きます。グローブボックスに控えの間に他の部品を引き、内部控えの間のドアを再シール。 </li><li>小さな計量ボートにコイン電池ケースを置きます。コイン電池ケースの中央にカソードを配置します。電極の中心に電解液の1-2〜30μlの滴を適用し、例リムの両側に1滴を適用します。 </li><li>上の単一¾ &quot;セパレーターを配置電極の表面に。フォースアウトリップによってケースをつかんで軽く場所に電極をタップして、ピンセットの平らなエッジを使用し、再センター陰極捕捉される気泡を。それは元の位置に貼り付ける場合は、電極のより良い動きを可能にするために、電解質の追加の1〜2滴を適用します。 </li><li>平らな面を下にし、唇側を上に向けた状態で、ケースにガスケットを配置します。前セル挿入を光にかざすことにより、ガスケットの向きを確認してください。 </li><li>セルの中心に電解液の2-3〜30μlの滴を適用し、下に向けリチウムを中心に準備された対向電極を配置します。中心の対向電極の上にウェーブスプリングを配置します。 </li><li>それは波形ばね表面の大部分をカバーし、湾曲した凸状メニスカスを形成するまで電解液でいっぱい（〜0.7ミリリットル）にセルを埋めます。 </li><li>トンを利用した細胞の上にコイン電池キャップを慎重に置きます彼は、セルの上に垂直方向の中央キャップを保持するためにピンセット。電解質の過度の損失を回避するためにキャップを中央に注意してください。 </li><li>それはガスケットのリップにセットされるまで（手で）キャップを押し下げます。クリンパに細胞を移し、細胞を圧着金型の溝の中央に配置されていることを確認します。 〜6.2メガパスカル（​​900 PSI）と解放の圧力にセルを圧着します。 </li><li> （手で）クリンパからセルを削除し、余分な電解質を落とします。全ての所望の細胞が構築されるまで、ステップ4.2- 4.9を繰り返します。いずれのこぼれた電解質を清掃し、適切な容器にゴミを置きます。グローブボックスの外に細胞を移し、それらにラベルを付けます。 </li></ol> 5.電気化学的評価<ol><li>バッテリーサイクラーに洗浄セルを接続します。端子が正しく開回路電位を測定することにより、接続されていることを確認します。正でない場合は、接続を逆にします。 </li><li>乾燥ELECの重量に基づいて所望の電流を計算しますアルミニウム基板、アルミニウム、重量活物質の割合、および利用活性物質の定格比容量の既知の質量の表面にtrode。 <ol><li> 0.70×155ミリアンペア時/グラム= 0.3906ミリアンペア× - 0.0090グラムの測定電極質量、0.0054グラムのアルミディスク質量、および155ミリアンペア時/グラムの定格容量と、（0.0054グラム0.0090グラム）などの所望の電流を決定します。完全に1時間（1C）でセルを放電するのに必要な電流での放電のために、印加電流は0.3906ミリアンペアです。 </li></ol></li><li>充電/ 4倍、Cの速度/ 10（定電流、定電流）で4.2 Vと2.8 Vのサイクルセルの上下の電圧レベルとの間のセルを放電するためにサイクラーにスケジュールを設定します。そして、C / 10で一度電池を充電します。 </li><li> 5 回目の C / 10充電した後、サイクラーからセルを削除する（必要な場合）、1時間休憩した後、細胞に電気化学インピーダンス分光法19（EIS）を行います。バックセルを配置C / 10でサイクラーと放電に。 1時間休憩した後、もう一度、EISを実行します。 </li><li> 100 1Cサイクルに続いて、C / 5、C、2C、5C、および10Cのレートでは、サイクラーおよびサイクルに戻ってセル5回セルを配置します。 </li><li>カソード中に存在する活性物質の質量ミリアンペア時のキャパシティを分割して各Cレートでの細胞の特定の容量を決定します。最初の5 1Cサイクルの平均比容量によって最後の5 1Cサイクルの平均比容量を分割することにより、容量保持率を計算します。 </li></ol>

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J., Lu, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effects+of+Inhomogeneities-Nanoscale+to+Mesoscale-on+the+Durability+of+Li-Ion+Batteries.">Effects of Inhomogeneities-Nanoscale to Mesoscale-on the Durability of Li-Ion Batteries.</a> J Phys Chem C. 117, 6481-6492 (2013).</li><li>Liu, G., Zheng, H., Song, X., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Particles+and+Polymer+Binder+Interaction:+A+Controlling+Factor+in+Lithium-Ion+Electrode+Performance.">Particles and Polymer Binder Interaction: A Controlling Factor in Lithium-Ion Electrode Performance.</a> J Electrochem Soc. 159, A214-A221 (2012).</li><li>Zheng, H. H., Yang, R. Z., Liu, G., Song, X. Y., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cooperation+between+Active+Material,+Polymeric+Binder+and+Conductive+Carbon+Additive+in+Lithium+Ion+Battery+Cathode.">Cooperation between Active Material, Polymeric Binder and Conductive Carbon Additive in Lithium Ion Battery Cathode.</a> J Phys Chem C. 116, 4875-4882 (2012).</li><li>Liu, Z. X., Battaglia, V., Mukherjee, P. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mesoscale+Elucidation+of+the+Influence+of+Mixing+Sequence+in+Electrode+Processing.">Mesoscale Elucidation of the Influence of Mixing Sequence in Electrode Processing.</a> Langmuir. 30, 15102-15113 (2014).</li><li>Liu, Z. X., Mukherjee, P. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructure+Evolution+in+Lithium-Ion+Battery+Electrode+Processing.">Microstructure Evolution in Lithium-Ion Battery Electrode Processing.</a> J Electrochem Soc. 161, E3248-E3258 (2014).</li><li>Zheng, H. H., Tan, L., Liu, G., Song, X. Y., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Calendering+effects+on+the+physical+and+electrochemical+properties+of+Li[Ni1/3Mn1/3Co1/3]O-2+cathode.">Calendering effects on the physical and electrochemical properties of Li[Ni1/3Mn1/3Co1/3]O-2 cathode.</a> J Power Sources. 208, 52-57 (2012).</li><li>Zheng, H. H., Li, J., Song, X. Y., Liu, G., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+comprehensive+understanding+of+electrode+thickness+effects+on+the+electrochemical+performances+of+Li-ion+battery+cathodes.">A comprehensive understanding of electrode thickness effects on the electrochemical performances of Li-ion battery cathodes.</a> Electrochim Acta. 71, 258-265 (2012).</li><li>Marks, T., Trussler, S., Smith, A. J., Xiong, D. J., Dahn, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Guide+to+Li-Ion+Coin-Cell+Electrode+Making+for+Academic+Researchers.">A Guide to Li-Ion Coin-Cell Electrode Making for Academic Researchers.</a> J Electrochem Soc. 158, A51-A58 (2011).</li><li>Li, C. C., Wang, Y. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Binder+Distributions+in+Water-Based+and+Organic-Based+LiCoO2+Electrode+Sheets+and+Their+Effects+on+Cell+Performance.">Binder Distributions in Water-Based and Organic-Based LiCoO2 Electrode Sheets and Their Effects on Cell Performance.</a> J Electrochem Soc. 158, A1361-A1370 (2011).</li></ol>

The authors have nothing to disclose.

湿式混合段階の最適化は、スラリー粘度とコーティング能力、電極の影響均一性と密着性に極めて重要です。ここで、高せん断混合法を利用し、溶剤、添加剤、結合剤、及び活性物質がバイアル中に存在するガラス・ボールの運動の動きを利用して一緒に混合されます。この混合技術は、磁気撹拌法に比べてはるかに迅速な混合時間の利点を提供しています。これを越えて、この高剪断混合?...

リチウムイオン電池は、エネルギー貯蔵装置1-4の絶えず増大する要求を満たすための有望な供給源を表します。 LIBSの能力の向上は、電気自動車5,6の有効範囲を改善するだけでなく、次にグリッドエネルギー貯蔵アプリケーション7で使用するためのLIBSの生存率を増加させ、放電の深さを、減少させることによって、そのサイクル寿命を改善しないであろう。 もともと1970年代8に補聴器に使用し、コイン電池、今日は、一般的に、新規および既存の電極材料の開発、評価で使用されています。電池のための最小のフォームファクタの一つとして、これらの細胞は、学術研究の設定の電池を作成するための簡単​​かつ効果的な方法を表します。一般的なリチウムイオン電池は、正極、負極集電体、およびアノードとカソードの短絡を防ぐ多孔質セパレータで構成されています。リチウムイオン電池の作動中に、IONSと電子が移動体です。放電時に、イオンが多孔質セパレータを介して負極（アノード）からおよび正電極、又はカソードに移動します。一方、電子は、最終的には、カソード側のイオンと再結合、外部回路全体で、集電体を通って移動します。イオンおよび電子移動に関連した任意の抵抗を低減するために、コンポーネントが適切に配向する必要がある - 距離イオンの移動が最小化されるべきです。典型的には、これらのコンポーネントは、「サンドイッチ」の設定を組み合わせています。電気自動車で使用される電池、携帯電話、家電、電池のフォームファクタに応じて、螺旋状に巻かれたまたは折り畳まれている大規模なサンドイッチで構成されています。細胞のこれらのタイプは、高いコストをかけず、小さなスケールで製造するのが非常に困難な場合があります。しかし、コイン電池のセル内の単一のサンドイッチがあります。特殊な装置は、電極を作成することが必要であるが、私<html>コインセルを、N、細胞自体を迅速に手で組み立てられ、制御された環境内に密封することができます。 電池の性能は、タイプに関係なく、正と負極、電解質の選択、およびセルアーキテクチャ4,9-13を形成する材料に依存しています。典型的なLIB電極はLi含有活物質、導電助剤、ポリマーバインダー、および電解質で充填される空隙の組み合わせで構成されています。 - 多くの場合、ほとんど注目されているステップ、乾燥粉末混合、湿式混合、基板準備、フィルム塗布、乾燥：電極の処理は、5つの主要なステップにまとめることができます。これらの処理ステップを使用して電極を製造する場合、最終目標は、活物質、導電助剤、結着剤からなる均一な電極膜を達成することです。この均一な分布がLIBS 14-18の最適なパフォーマンスに重要です。 NT &quot;&gt;このガイドでは、新規および既存の電極材料の評価のためにコイン電池を製造するためのエネルギーと交通科学研究所（ETSL）でテキサスA＆Mで、テキサス州立大学で利用手順を表します。多くのソースで文書発見の基本的な手順を超えて、私たちはしばしば同様の方法文書や多くの出版物から除外されている重要な詳細に注目し、重要なステップで私たち自身の専門知識が含まれている。また、私たちの研究室で利用主要な物理的および電気化学的方法（定電流サイクリング、電気化学インピーダンス分光法（EIS））内解明されています。

<table border="0" cellpadding="0" cellspacing="0" width="992">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">LiNiMNCoO2 (NMC, 1:1:1)</td>
			<td style="width:159px;">Targray</td>
			<td style="width:139px;">PLB-H1</td>
			<td style="width:291px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">CNERGY Super C-65</td>
			<td style="width:159px;">Timcal</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Polyvinylidene Difluoride (PVDF)</td>
			<td style="width:159px;">Kynar</td>
			<td style="width:139px;">Flex 2801</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:405px;">1-Methyl-2-pyrrolidinone anhydrous, 99.5% NMP</td>
			<td style="width:159px;">Sigma-Aldrich</td>
			<td style="width:139px;">328634</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">1.0 M LiPF6 in EC/DEC (1:1 by vol)</td>
			<td style="width:159px;">BASF</td>
			<td style="width:139px;">50316366</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Celgard 2500 Separator</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">EQ-bsf-0025-60C</td>
			<td>25um thick; Polypropylene</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Aluminum Foil</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">EQ-bcaf-15u-280</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Lithium Ribbon</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">320080</td>
			<td>0.75 mm thickness</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">2-Propanol, ACS reagent, &#8805;99.5%</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">190764</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Acetone, ACS reagent, &#8805;99.5%</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">179124</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel CR2032 Coin Cell Kit&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>case, cap, and PP gasket</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel Spacer&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>15.5 mm diameter x 0.5 mm thickness</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel Wave Spring&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>15 mm diameter x 1.4 mm height</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Analytical Scale</td>
			<td style="width:159px;">Ohaus</td>
			<td style="width:139px;">Adventurer AX</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Agate Mortar and Pestle</td>
			<td style="width:159px;">VWR</td>
			<td style="width:139px;">89037-492</td>
			<td>5 inch diameter</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Tube Drive</td>
			<td style="width:159px;">IKA</td>
			<td style="width:139px;">3645000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">20 ml Stirring Tube</td>
			<td style="width:159px;">IKA&#160;</td>
			<td style="width:139px;">3703000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Glass balls</td>
			<td style="width:159px;">McMaster-Carr</td>
			<td style="width:139px;">8996K25</td>
			<td>6 mm diameter</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Automatic Film Applicator</td>
			<td style="width:159px;">Elcometer</td>
			<td style="width:139px;">K4340M10-</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Doctor Blade</td>
			<td style="width:159px;">Elcometer</td>
			<td style="width:139px;">K0003580M005</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Die Set</td>
			<td style="width:159px;">Mayhew</td>
			<td style="width:139px;">66000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Vacuum Oven</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Vacuum Pump</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Laboratory Press</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">YLJ-12</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Hydraulic Crimper</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">MSK-110</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Glovebox</td>
			<td style="width:159px;">MBraun</td>
			<td style="width:139px;">LABstar</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Battery Cycler</td>
			<td style="width:159px;">Arbin Instruments</td>
			<td style="width:139px;">BT2000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Potentiostat/Galvanostat/EIS</td>
			<td style="width:159px;">Biologic</td>
			<td style="width:139px;">VMP3</td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

正しくキャスト電極シートは、表面外観に均一に見えるし、適切に集電体に付着する必要があります。通常、電極シートの剥離が悪い基板のエッチング、または最初の混合段階ではほとんどのNMPを有するいずれかが原因で発生します。また、あまりにも多くのNMPは望ましくない多孔性の高い程度を、表示するシートを引き起こす可能性があります。最後に、第3のパタ...

Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

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

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

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.

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

non-aqueous-electrode-processing-construction-lithium-ion-coin

Research

JoVE Journal

Engineering

21.4K ビュー.  Texas A&M University. 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.

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

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

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 &deg;C), flammable, and volatile organic electrolytes. These organic based electrolyte systems are viable at ambient temperatures, but require a cooling system to ensure that temperatures do not exceed 80 &deg;C. These cooling systems tend to increase battery costs and can malfunction which can lead to battery malfunction and explosions, thus endangering human life. Increases in petroleum prices lead to a huge demand for safe, electric hybrid vehicles that are more economically viable to operate as oil prices continue to rise. Existing organic based electrolytes used in lithium ion batteries are not applicable to high temperature automotive applications. A safer alternative to organic electrolytes is solid polymer electrolytes. This work will highlight the synthesis for a graft copolymer electrolyte (GCE) poly(oxyethylene) methacrylate (POEM) to a block with a lower glass transition temperature (Tg) poly(oxyethylene) acrylate (POEA). The conduction mechanism has been discussed and it has been demonstrated the relationship between polymer segmental motion and ionic conductivity indeed has a Vogel-Tammann-Fulcher (VTF) dependence. Batteries containing commercially available LP30 organic (LiPF6 in ethylene carbonate (EC):dimethyl carbonate (DMC) at a 1:1 ratio) and GCE were cycled at ambient temperature. It was found that at ambient temperature, the batteries containing GCE showed a greater overpotential when compared to LP30 electrolyte. However at temperatures greater than 60 &deg;C, the GCE cell exhibited much lower overpotential due to fast polymer electrolyte conductivity and nearly the full theoretical specific capacity of 170 mAh/g was accessed.

Lithium ion batteries employ flammable and volatile organic electrolytes that are suitable for ambient temperature applications. A safer alternative to organic electrolytes are solid polymer batteries. Solid polymer batteries operate safely at high temperatures (&gt;120 &deg;C), thus making them applicable to high temperature applications such as deep oil drilling and hybrid electric vehicles. This paper will discuss (a) the polymer synthesis, (b) the polymer conduction mechanism, and (c) provide temperature cycling for both solid polymer and organic electrolytes.

リチウム電池アプリケーションのためのソリッドステートグラフトコポリマー電解質

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

固体酸化物形燃料電池の電極表面をプロービングとマッピング

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

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. ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

その場中性子粉末回折ではカスタムメイドのリチウムイオン電池を使用して、

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Wicking Tests for Unidirectional Fabrics: Measurements of Capillary Parameters to Evaluate Capillary Pressure in Liquid Composite Molding Processes

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify their influence on void formation in composite parts. Wicking in a fibrous medium described by the Washburn equation was considered equivalent to a flow under the effect of capillary pressure according to the Darcy law. Experimental tests for the characterization of wicking were conducted with both carbon and flax fiber reinforcement. Quasi-unidirectional fabrics were then tested by means of a tensiometer to determine the morphological and wetting parameters along the fiber direction. The procedure was shown to be promising when the morphology of the fabric is unchanged during capillary wicking. In the case of carbon fabrics, the capillary pressure can be calculated. Flax fibers are sensitive to moisture sorption and swell in water. This phenomenon has to be taken into account to assess the wetting parameters. In order to make fibers less sensitive to water sorption, a thermal treatment was carried out on flax reinforcements. This treatment enhances fiber morphological stability and prevents swelling in water. It was shown that treated fabrics have a linear wicking trend similar to those found in carbon fabrics, allowing for the determination of capillary pressure.

An experimental method to measure geometrical parameters and the apparent advancing contact angles describing capillary wicking in unidirectional synthetic and natural fabrics is proposed. These parameters are mandatory for the determination of the capillary pressures that must be taken into account for liquid composite molding (LCM) applications.

単方向生地のためのテストをウィッキング：キャピラリーパラメータの測定を液体複合成形プロセスに毛細管圧力を評価します

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify ...

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 ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

金属-セラミック部品の溶融フィラメント製作 (FFF)

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...

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 ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

セメント細孔溶液の化学組成の蛍光 x 線を用いた比抵抗解析式

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...