我々は感謝していない助成金の下で、米国国立科学財団の材料研究の部門で陶芸のプログラムからの支援を認める。 DMR-1006515（プログラム·マネージャー、博士Lynnette D.マドセン）。

1。作用電極の作製<ol><li> 〜6重量％の混合物を準備します。 N-メチル-2 - ピロリドン（NMP）の％ポリフッ化ビニリデン（PVDF）バインダー。 </li><li> 80重量を量る。 ％の活性物質（この場合のLiCoO 2）、および10重量。その後、％Cブラック（アセチレン、99.9 +％）、1分間ボルテックスで混ぜる。 </li><li>バインダーが10重量％を構成するようなNMP-バインダー混合物を追加します。混合物の総重量の％。 </li><li>小さなガラスバイアルと約30分間最大rpmでボルテックスミキサーでミックスに上記混合物を転送します。 5 mmの直径の2つのジルコニアボールの方が、混合用のメディアとして使用することができます。必要に応じて、必要な一貫性のスラリーを得るために多くのNMPを追加します。 </li><li>ガラス板の上にコレクタ電流（典型的には、アノードの陰極と銅のアルミニウム）の金属箔を広げた。アセトンを使用して、箔とガラス板との間に気泡が存在しないことを確認してください。トラックとdefを形成するために、マスキングテープの二層を使用します。コー​​ティングされる領域をピペリジン。 </li><li>ステンレス製のへらを使用して、金属箔の上にスラリーを適用して、カミソリの刃を使用してトラックに均一にスラリーを広げた。 </li><li> 90から120で〜を空気中または真空中でコーティングを乾燥°C約2から8時間（使用する材料とバインダーに依存して調整する必要があります）。 </li><li> 2枚の鋼板（およびコーティングを保護する2つの秤量紙）と油圧プレスを用いて〜3000ポンドの負荷の下で記者の間で被覆した金属箔を配置します。 </li><li>直径8 mmのディスク（できればグローブボックス内）に乾燥させた被覆金属箔を開ける。グローブボックスに転送する前に、カソードを秤量し、それらをラップします。 </li><li>直径8 mmのディスクに同じ材料のコーティングされていない金属箔を開けると、これらのディスクの重量を量る。 </li></ol> 2。電解質の調製<ol><li>ナルゲンbottlに電解液が感光性であるため、（DECこの例では：DMC ECに1M LiPF 6）を電解質を保存するeは、アルミホイルでラップされた。 </li></ol> 3。対向電極の作製（この場合はリチウム箔） <ol><li>光沢のある銀色の表面が（アルゴングローブボックス内）が表示されるまでナイロンブラシ/ステンレススチールメスを用いたリチウム箔の表面を清掃してください。 </li><li>パンチ½インチ径（アルゴングローブボックス内）のディスクにリチウム箔。 </li></ol> 4。コイン電池アセンブリ<ol><li> 図2は、コイン·セル·アセンブリの概略を示しています。 </li><li>直径としてそれらを使用するセパレータの19ミリメートルのディスクにパンチセルガードはC480膜。 </li><li>グローブボックス（アルゴンとの交換を5回フラッシュした後）にコイン電池ケース（CR2032）、バネとスペーサー（MTI社から購入）、セパレータ、作用電極を転送します。 </li><li>グローブボックス内でコイン電池を組み立てる。 </li><li>セルカップへの電解液2滴を追加し、それに取り組んで電極を配置します。別の3を追加します。電解質と場所、それらの間の電解液2滴を持つ2つのセパレータの滴。その上にリチウム対電極を配置する前に、電解質の2つの滴を追加します。リチウムディスク上の2つのステンレス製のスペーサーとスプリングを配置します。 </li><li>セルキャップを使用して、セルを閉じて、コンパクトな圧着機を使用して3-4回を圧着（MTI社から購入）。 </li><li>セルを組み立てた後、プラスチック製のピンセットを（短絡を避けるため）を使用して、完成した細胞を処理します。 </li><li>紙ナプキンを使用して、セルの側面から漏れる過剰な電解質をクリーニングします。 </li><li>セルは、テストの準備ができているとグローブボックスから取り出すことができる。 </li></ol> 5。コイン電池のテスト<ol><li>それの準備ができ次第、一時間のためのオープン回路電圧（OCV）モードでバッテリーテスターに​​接続してコイン電池を保持します。 </li><li>作用電極に使用される活物質に基づいてセルをテストするための電圧ウィンドウを定義します。 </li><li>計算する以下に示す計算を使用してセルのoretical容量。 </li></ol>コレクタ電流= W EOの電極ディスクの重量同じ直径のコーティングされていないコレクタ電流ディスクの重量= W CC 電極材料の重量、W EMは 、次式で与えられます。 <img alt="式（1）" src="/files/ftp_upload/4104/4104eq1.jpg" />電極の活物質、W AMの重量は次式で与えられる。 <img alt="式（2）" src="/files/ftp_upload/4104/4104eq2.jpg" />電極ディスク、C EDのための理論容量は次式で与えられます。 <img alt="式（3）" src="/files/ftp_upload/4104/4104eq3.jpg" /> Cは理論的なのである活物質のpecific容量。 <ol start="4"><li>必要なCレートでの充放電サイクルにコイン電池をテストします。 </li></ol> 6。代表的な結果例として、コイン型セルは作用電極の活物質としてLiCoO 2を用いて構築した。建設後、細胞は、C / 5の速度でテストされています。得られたプロファイルを図3に示します。電圧ウィンドウは、このコイン電池のために3〜4.3 Vに設定されました。容量は、最初の充電サイクルの155ミリアンペア時/ gで、最初の放電サイクルは140ミリアンペア時/ gであった。 <img alt="図1" src="/files/ftp_upload/4104/4104fig1.jpg" /> コイン電池の構築手順の図1のフローチャート。最初に、作用電極活物質の粉体から調製される。その後、対向電極は、クリーンなリチウム箔から調製され、区切り記号が打ち抜かれています。最後に、細胞であるアルゴングローブボックスの内側に組み立てられた。 <img alt="図2" src="/files/ftp_upload/4104/4104fig2.jpg" /> 図2。彼らはコイン電池ケース内に配置された順序ですべてのコンポーネントを示すコイン電池の組立工程の模式図。 <img alt="図3" src="/files/ftp_upload/4104/4104fig3.jpg" /> （3）代表的な結果はLiCoO 2とリチウム箔対極から作られた作用電極を使用して構築コイン電池から得られた図 。プロットは、C / 5のレートで充放電されたコイン電池のための最初の充電と、最初の放電曲線を示しています。 <img alt="図4" src="/files/ftp_upload/4104/4104fig4.jpg" /> 図4。良い面と悪い面のコーティングの比較は、それらが乾燥された後。過剰NMPおよび多孔性コーティングsから一般的に結果を持っているスラリーから一般的に結果ひび割れ塗装不十分なNMPを持っていlurry。 <img alt="図5" src="/files/ftp_upload/4104/4104fig5.jpg" /> 図5非圧着細胞と一緒によく圧着コイン電池とひどく圧着コイン電池の比較。一般的に、ひどく圧着コイン電池は、水分との反応後のリチウム箔の膨潤に起因する周囲の数時間後にオープンを分割します。

<ol>
	<li>Cairns, E. J., Albertus, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Batteries+for+Electric+and+Hybrid-Electric+Vehicles.">Batteries for Electric and Hybrid-Electric Vehicles.</a> Annual Review of Chemical and Biomolecular Engineering. 1, 299-320 (2010).</li><li>Dunn, B., Kamath, H., Tarascon, J. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+Energy+Storage+for+the+Grid:+A+Battery+of+Choices.">Electrical Energy Storage for the Grid: A Battery of Choices.</a> Science. 334, 928-935 (2011).</li><li>Goodenough, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode+materials:+A+personal+perspective.">Cathode materials: A personal perspective.</a> J. Power Sources. 174, 996-1000 (2007).</li><li>Yamada, A., Chung, S. C., Hinokuma, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimized+LiFePO4+for+lithium+battery+cathodes.">Optimized LiFePO4 for lithium battery cathodes.</a> Journal of the Electrochemical Society. 148, A224-A229 (2001).</li><li>Whittingham, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+batteries+and+cathode+materials.">Lithium batteries and cathode materials.</a> Chemical Reviews. 104, 4271-4301 (2004).</li><li>Tarascon, J. M., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Issues+and+challenges+facing+rechargeable+lithium+batteries.">Issues and challenges facing rechargeable lithium batteries.</a> Nature. 414, 359-367 (2001).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+Rechargeable+Li+Batteries.">Challenges for Rechargeable Li Batteries.</a> Chemical Materials. 22, 587-603 (2010).</li><li>Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Identification+of+cathode+materials+for+lithium+batteries+guided+by+first-principles+calculations.">Identification of cathode materials for lithium batteries guided by first-principles calculations.</a> Nature. 392, 694-696 (1998).</li><li>Chung, S. Y., Bloking, J. T., Chiang, Y. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electronically+conductive+phospho-olivines+as+lithium+storage+electrodes.">Electronically conductive phospho-olivines as lithium storage electrodes.</a> Nature Materials. 1, 123-128 (2002).</li><li>Bruce, P. G., Scrosati, B., Tarascon, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanomaterials+for+rechargeable+lithium+batteries.">Nanomaterials for rechargeable lithium batteries.</a> Angewandte Chemie-International Edition. 47, 2930-2946 (2008).</li><li>Arico, A. S., Bruce, P., Scrosati, B., Tarascon, J. M., Van Schalkwijk, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+materials+for+advanced+energy+conversion+and+storage+devices.">Nanostructured materials for advanced energy conversion and storage devices.</a> Nature Materials. 4, 366-377 (2005).</li><li>Hochbaum, A. I., Yang, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+Nanowires+for+Energy+Conversion.">Semiconductor Nanowires for Energy Conversion.</a> Chemical Reviews. 110, 527-546 (2010).</li><li>Wang, Y., Cao, G. Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Developments+in+nanostructured+cathode+materials+for+high-performance+lithium-ion+batteries.">Developments in nanostructured cathode materials for high-performance lithium-ion batteries.</a> Advanced Materials. 20, 2251-2269 (2008).</li><li>Kang, B., Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Battery+materials+for+ultrafast+charging+and+discharging.">Battery materials for ultrafast charging and discharging.</a> Nature. 458, 190-193 (2009).</li><li>Liu, J., Manthiram, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improved+Electrochemical+Performance+of+the+5+V+Spinel+Cathode+LiMn1.5Ni0.42Zn0.08O4+by+Surface+Modification.">Improved Electrochemical Performance of the 5 V Spinel Cathode LiMn1.5Ni0.42Zn0.08O4 by Surface Modification.</a> Journal of the Electrochemical Society. 156, A66-A72 (2009).</li><li>Kayyar, A., Qian, H. J., Luo, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+adsorption+and+disordering+in+LiFePO4+based+battery+cathodes.">Surface adsorption and disordering in LiFePO4 based battery cathodes.</a> Applied Physics Letters. 95, (2009).</li><li>Sun, K., Dillon, S. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+mechanism+for+the+improved+rate+capability+of+cathodes+by+lithium+phosphate+surficial+films.">A mechanism for the improved rate capability of cathodes by lithium phosphate surficial films.</a> Electrochemistry Communications. 13, 200-202 (2011).</li><li>Kovalenko, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Major+Constituent+of+Brown+Algae+for+Use+in+High-Capacity+Li-Ion+Batteries.">A Major Constituent of Brown Algae for Use in High-Capacity Li-Ion Batteries.</a> Science. 333, 75-79 (2011).</li></ol>

利害の衝突が宣言されません。

我々の経験では、作用電極の調製における最も重要なステップは、一貫性の良好なスラリーを行っています。 図4に示すように、不足してNMPは多孔性コーティングをもたらすことができますが、スラリーの過剰NMPは、ひびの入った塗装になる可能性があります。ここで紹介する研究では、直径20 mmであるCR2032コイン電池ケースが使用されています。これは、電極のサイズはそれに?...

<table border="1"><tbody><tr><td> 試薬の名前 </td><td> 会社 </td><td> カタログ番号 </td></tr><tr><td>ポリ（フッ化ビニリデン） </td><td> Sigma-Aldrich社</td><td> 182702 </td></tr><tr><td> 1 - メチル-2 - ピロリジノン、99.5％ </td><td>アルファAesar社</td><td> 31903 </td></tr><tr><td> LiCoO 2は </td><td>アルファAesar社</td><td> 42090 </td></tr><tr><td>カーボンブラック、アセチレン、99.9 +％ </td><td>アルファAesar社</td><td> 39724 </td></tr><tr><td> ECのLiPF 6：DMC：DEC </td><td> MTI株式会社</td><td> EQ-BE-LiPF6と</td></tr><tr><td>セルガードのセパレータ</td><td>セルガード</td><td> C480 </td></tr><tr><td>アナログボルテックスミキサー</td><td> VWR </td><td> 58816-121 </td></tr><tr><td>真空オーブン</td><td></td><td></td></tr><tr><td>真空ポンプ</td><td></td><td></td></tr><tr><td>油圧プレス</td><td></td><td></td></tr><tr><td>コイン電池ケース</td><td> MTI株式会社</td><td> EQ-CR2032-CASE-304 </td></tr><tr><td>バネとスペーサー</td><td> MTI株式会社</td><td> EQ-CR20SprSpa-304 </td></tr><tr><td>グローブボックス</td><td> mBraun </td><td> UNILAB </td></tr><tr><td>バッテリーテスタ</td><td>アルビン·インスツルメンツ</td><td> BT2143 </td></tr></tbody></table>

construction and testing of coin cells of lithium ion batteries

充電式リチウムイオン電池は、お客様がいつもより多くの容量と長寿命を要求するエレクトロニクスの幅広い用途を有する。リチウムイオン電池は、電気自動車、ハイブリッド自動車、1または偶数の電気グリッド安定化システム2に使用されると考えられてきた。すべてのこれらのアプリケーションは10-13、コーティング又は表面改質14から17と新規バインダー18をナノ構造、9ドーピング、新材料3,8を含む電池材料3-7の研究開発、劇的な増加をシミュレートします。その結果、物理学者、化学者や材料科学者の増加数は、最近この分野に進出しています。コインセルは広く新しい電池材料をテストするために研究室で使用されます。さらに研究開発の対象となる大規模かつ高電力アプリケーションという、小さなコインセルは、多くの場合の容量と速度の機能をテストするために使用され初期段階での新素材。 2010年に、我々は表面吸着と電池材料の無秩序化（助成金なし。DMR-1006515）を調査する研究プロジェクトを後援した国立科学財団（NSF）を開始しました。このプロジェクトの初期段階で、我々は他の大学（頻繁に通話、メール交換と2つのサイトの訪問を通して）他の研究者の多くの助けなしには達成できないコイン型セルを組み立て、テストするためのテクニックを学ぶのに苦労しました。したがって、我々はそれが、テキストとビデオの両方で、この分野で他の新しい研究者を助けるコイン電池の組み立てとテストのプロトコルを文書化するために有益であると感じています。この取り組みは、私たちのNSFプロジェクトの &quot;広範な影響&quot;の活動を表し、それはまた、学生を​​教育し、鼓舞するのに役立ちます。 このビデオの記事では、我々は、LiCoO 2は作用電極、リチウムカウンター電極とCR2032コイン電池を組み立てるためにプロトコルを文書化と（主に一般的に使用される）ポリフッ化ビニリデン（PVDF）バインダー。容易にプロトコルを繰り返すための新しい学習者を確保するために、我々はできるだけ具体的かつ明示的にプロトコルを保持します。しかし、それは具体的な研究と開発作業では、多くのパラメータが変化することができますここで採用していることに注意する必要があります。まず、一つは、異なるサイズのコイン型セルを作ると、Li以外のカウンタ電極に対して作用電極をテストすることができます。第二に、Cと黒のバインダーの量は、しばしば研究の特定の目的に合わせて変化させる作用電極に加え、例えば、C黒、あるいは不活性粉体の大量の &quot;本質的な&quot;パフォーマンスをテストするための作用電極に追加されました正極材料14。第三に、優れたバインダーは、（PVDF以外）も開発し、18を使用しています 。最後に、電解質（代わりにLiPF 6の）他のタイプも使用できます。実際には、一定の高電圧電極材料は、特殊なelectrolの使用が必要になりますytes 7。

Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

Construction and Testing of Coin Cells of Lithium Ion Batteries

リチウムイオン電池のコインセルを構築し、テストするプロトコルが記述されています。 、作用電極を作るカウンター電極を準備し、グローブボックス内のセルを組み立て、セルをテストするための具体的な手順が提示されています。

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 ...

construction-and-testing-of-coin-cells-of-lithium-ion-batteries

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Engineering

31.2K ビュー.  Clemson University. リチウムイオン電池のコインセルを構築し、テストするプロトコルが記述されています。 、作用電極を作るカウンター電極を準備し、グローブボックス内のセルを組み立て、セルをテストするための具体的な手順が提示されています。

ビデオ: Construction and Testing of Coin Cells of Lithium Ion Batteries

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. ...

工学

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 ...

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 ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

薄膜における拡散を用いた環境プルトニウムのスペシエーションと生物学的利用能の測定

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

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 ...

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 ...

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 ...

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

グラフェン液セルのリチウム イオン電池材料の観察のための準備

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...

Methods Article

リチウムイオン電池のコイン細胞の構築とテスト