This article was supported in part by BU and by the Advanced Energy Consortium:

塩化物（CL）およびビス（トリフルオロメタンスルホン酸）イミド（TFSI）陰イオンと対モノ - 及びジ - ホスホイオン液体の1.Synthesis 注三つヘキシルホスホニウムカチオンを取り囲む1デシルアルキル鎖を有するモノホスイオン液体のための手順が記載され、このイオン性液体は、モノHexC10Clと略記します。同じ手順を、高い収率でジホスイオン液体を得るために、1,10- dichlorodecaneを使用して繰り返され、このイオン性液体は、ジHexC10Clと略記します。 <ol><li>アルゴン下でグローブボックス内で、ガラスピペットを用いて、トリヘキシル（8.3グラム、29ミリモル）を秤量しながら、と重い壁の圧力容器に分注します。次に、同じ容器にガラスピペットを用いて、1-クロロデカン（5.22グラム、29.6ミリモル）を追加します。 PTFEブッシングとの混合物を含む容器キャップ。 </li><li>モノHexC10Clを得るために混合しながら24時間140℃にアルゴン下で得られた混合物を加熱します。混合物は次のようになります粘性来ます。 </li><li>粗製のモノHexC10Clを得るために、残りの揮発性出発物質を除去するために、攪拌しながら140℃で高真空下で混合物を置きます。 <ol><li> 250ミリリットルの分液漏斗に飽和塩化ナトリウム溶液（塩水）に1ジクロロメタン（DCM）：精製するために、1の約10ミリリットルを用いて、粗混合物からモノHexC10Clを抽出します。 DCM相を収集します。抽出工程を3回繰り返します。 </li><li>生成物を含有する収集DCM溶液15mlのを結合し、モノHexC10Cl物を得るために、ロータリーエバポレーターを用いて溶媒を蒸発させます。 </li></ol></li><li> DCM 10ml中モノHexC10Cl（7.75グラム、16.74ミリモル）を溶解し、LiTFSIと（6.25グラム、21.76ミリモル）を追加し、脱イオン水10ml中に予め溶解。得られた混合物をキャップし、24時間室温で攪拌します。 </li><li> DCMの約20ミリリットルを充填した250ミリリットルの分液漏斗を用いて混合物からモノHexC10TFSIを抽出します。内線を繰り返しractionプロセス3回。 DCMのソリューションを組み合わせます。 </li><li>有機相から塩化物アニオンの完全な除去を確認するために、1 NのAgNO DCM相の1ミリリットルに3溶液の1〜2滴を追加します。塩化物アニオンは溶液中に残っている場合、白色沈殿物が生成されます。白い沈殿物が生成されなくなるまで抽出工程を繰り返します。 </li><li> 、DCM溶液を無水MgSO 4 1gを追加し、混合物を攪拌し、次いで乾燥DCM溶液をデカントします。次に、回転蒸発により溶媒を蒸発させます。収率は、典型的には98％以上です。 </li><li>高収率で、2ジホスホイオン液体、ジHexC10ClおよびジHexC10TFSIを得るために、1,10- dichlorodecaneを使用して、同じ手順を繰り返します。 </li><li>重水素化クロロホルム中の1 H、13 C、および19 F NMRを用いてイオン性液体を特徴付ける（7.24のシフト）、元素分析および質量分析のためのサンプルを提出します。 </li></ol> 2. Charactイオン液体のerization <ol><li> 示差走査熱量測定（DSC） <ol><li>イオン性液体（記録実際の質量）の5〜10mgのを秤量し、続いて密閉されているアルミニウム製サンプルパンの中心にそれを追加します。イオン性液体は吸湿性であり、放置した場合の重量は変わります効率的に、このステップを完了してください。 </li><li>示差走査熱量計に試料パンとアンロード（参照）パンをロードします。使用される特定のDSCによって決定されるように適切な場所にサンプルおよび参照パンを配置するようにしてください。 </li><li>プログラム温度勾配とサイクル冷却：10℃/分の加熱速度で200°Cまで-70°Cから1）の熱を、2）5℃/分の冷却速度で-70℃に冷却し、 3）加熱 - 冷却サイクルを3回繰り返します。 </li><li>熱トレースを分析することにより、 融点（T m）、結晶化（T C）を決定しますガラス転移温度（T g）（該当する場合）。 </li></ol></li><li> 熱重量分析（TGA） <ol><li>清潔でTGAの可動アーム上の白金パンを風袋引き。皿の上にイオン性液体の5〜10mgのを追加します。唯一のピンセットを使ってパンをタッチします。 </li><li> 10℃/分の加熱速度で20から500℃まで試料を加熱します。 </li><li>元のサンプル重量の10％が失われた分解温度を特定します。長期安定性研究のために、長時間の設定温度で試料を加熱し、重量損失をモニターします。 </li></ol></li><li> 粘度測定 <ol><li>ガラスピペットを用いて、制御された歪みレオメーターのペルチェステージにイオン液体の1ミリリットルを配置します。アルミニウム板を完全にイオン性液体で覆われていることを確認します。 </li><li>直径20mmの平行アルミニウム板（または円錐）を使用し、アルミニウム板とTの上面との間のギャップを設定しますランのすべてで2.0ミリメートル - 彼が1.0であることをサンプリングします。 </li><li>空気中の水分の影響を最小限に抑えるために、窒素ガスを充填したグローブバッグ中で測定を行います。 </li><li>各試験の前に、サンプルが定常状態に到達するためには15分間の平衡ステップに従って、サンプルの任意の物理メモリを排除するために10秒間100ヘルツの剪断速度でサンプルを事前にせん断。 </li><li> 0.1〜10％のひずみ振幅の固定周波数（1ヘルツ）で振動ひずみ掃引を経由して、線形粘弾性領域（LVR）を決定します。 </li><li> LVRにある歪みを選択して、0.1から10 Hzの振動周波数掃引を行います。特定の周波数と歪みで複雑な粘度を決定します。 </li><li> 10から機器のソフトウェアによって制御振動温度掃引を実行します 95°C 5刻みでCを° ℃、各温度で1分間平衡。ひずみとFREQUENCを定義しますYは、例えば、それぞれ、1.0％および1ヘルツでした。異なる温度における複素粘度が読み出されます。 </li></ol></li><li> 導電率の測定 <ol><li>試験の前に微量の水分を除去するために、12時間高真空下、100℃で、イオン性液体を乾燥させます。 </li><li>アルゴン雰囲気下のグローブボックス、負荷試験管内の試料の約4ミリリットルでは、完全に導電性プローブの検知テープを浸漬するのに十分なサンプルを追加してください。 </li><li>温度を制御し、均質性を維持するために、測定中に攪拌を維持するために加熱ブロックを使用してください。 </li><li> 30分の平衡時間の後、各温度での導電率をお読みください。 </li></ol></li><li> サイクリックボルタンメトリー（CV） <ol><li>アルゴン雰囲気下のグローブボックス中でリチウム/リチウム/白金三電極系を組み立てます。 </li><li>イオン性液体と容器を充電し、すべての電極がインマであることを確認してくださいイオン性液体にrsed。アルゴン下で容器を密閉。 </li><li> 20分間所望の温度に容器を平衡化。対Li + / Li -0.2 Vと6.5 Vの間には1mV /秒の電位速度をスイープ。 </li></ol></li></ol>電解質の調製<ol><li>微量の水の除去を保証するために厳密に撹拌しながら80℃で一晩高真空下でのイオン性液体を乾燥させます。 </li><li>真空オーブン中で三日間70℃でのLiTFSIを乾燥させます。 </li><li>グローブボックスに無水イオン性液体とのLiTFSI塩を転送します。 </li><li>攪拌棒を含む、オーブン乾燥したフラスコにイオン性液体（ 例えば 、モノHexC10TFSI、4.50グラム、6.4ミリモル）とのLiTFSI（1.83グラム、6.4ミリモル）を追加します。電解液の1.6 Mの濃度を得ることが均質になるまで混合物を一晩撹拌しました。 </li></ol>リチウムイオンコイン型電池の4製作<ol><li>アルゴンatmosp下のグローブボックス内でここでは、コイン電池の底部キャップに1春と1ステンレス鋼のディスクを配置します。ステンレス製のディスクで12.7ミリメートル径のLiCoO 2電極（24 mg）を配置します。 </li><li> 15分間、ホットプレート上で60℃で、上記で調製したイオン性液体電解質中のセパレータ（多孔質ポリプロピレン膜）の2枚を浸します。 </li><li>材料が完全に電解質（≈0.5ml）で覆われるまでのLiCoO 2カソードの表面にイオン性液体電解質を加えます。 </li><li>コイン電池の中心に電解液に浸したセパレータを配置します。そして、セパレータ上にイオン性液体電解質（数マイクロリットル）の数より多くの滴を追加します。 </li><li>グローブボックス内の12.7ミリメートルの直径を有するリチウム金属片をカット。セパレータの上にリチウム金属を配置します。 </li><li>コイン電池をキャップとグローブボックス内で捲縮機でそれを封印。 </li><li>目を開始する前に、グローブボックスの外にコイン電池を移し、12時間細胞を休ま電子バッテリー/電気化学のテスト。 </li></ol> 100℃での電池の5パフォーマンス<ol><li>電気化学的試験局からのケーブルがスレッド化された後壁に小さな穴を持つ100℃で動作するオーブンでコイン電池を置きます。電気化学的試験ステーションにコイン電池を接続します。 </li><li>温度に平衡化し、30分間100℃で細胞を残します。 </li><li>電気化学的試験ステーションの定電流充放電サイクルを選択します。 500にサイクル数を設定します。 </li><li>各充電後0 Vで60秒の休止時間を設定して4.2 Vに500μAへの充電電流と電圧の上限値を設定します。 </li><li>各放電後に0 Vで60秒の休止時間を設定して3.0 Vに500μAに放電電流と電圧に下限を設定します。 </li><li>ソフトウェアを使用して、4.2 V〜3.0 Vの間に500μAの電流での充放電サイクルを開始します。電荷出力AGを評価しますainst時間。 </li></ol>

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Sci. 6, 6601-6606 (2015).</li><li>Xu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonaqueous+Liquid+Electrolytes+for+Lithium-Based+Rechargeable+Batteries.">Nonaqueous Liquid Electrolytes for Lithium-Based Rechargeable Batteries.</a> Chem. Rev. 104, 4303-4418 (2004).</li><li>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=Polymer+solid+electrolytes-an+overview.">Polymer solid electrolytes-an overview.</a> Solid State Ionics. 9-10, 745-754 (1983).</li><li>Meyer, W. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+electrolytes+for+lithium-ion+batteries.">Polymer electrolytes for lithium-ion batteries.</a> Adv. Mater. 10, 439-448 (1998).</li></ol>

The authors declare that they have no competing financial interests.

不燃性と高温機能リチウムイオン電池を開発するための我々のアプローチは、プロトタイプのコイン電池における新しいイオン液体電解質の合成とそれらのその後の評価を伴います。具体的には、モノ- HexC10TFSI及びジHexC10TFSI系電解質は、Li金属アノードとのLiCoO 2カソードを有するコイン型電池において試験しました。このアプローチ内の重要な手順は次のとおりである。1）設計仕様...

リチウムイオン電池は、電気エネルギーと化学エネルギーとの間でエネルギーを変換し、格納し、要求に応じて、オン・行くエネルギーを供給するための便利な手段を提供するデバイスです。今日、リチウムイオン電池は、高いエネルギー密度及び再帯電の携帯用電子機器市場を支配し、そのようなダウンホール掘削、自動車などの大規模な、特殊用途のために重要です。カソード、アノード、セパレータ、及び電解質：1-5電池は、4つの主要コンポーネントで構成されています。二つの電極の化学的性質は、電池の理論エネルギー密度を決定しながら、安全性と作業温度は、主に電解質材料によって制限されます。 6-9カーボネート系有機溶媒電解質（ 例えば 、ジメチルカーボネート（DMC）、エチレンカーボネート（EC））が広く、それらの低い粘度、高い導電性、および高いリチウム塩の溶解度をリチウムイオン電池に使用されます。また、特定のCOMBINAカーボネート系溶媒（DMC / EC）のションはまた、それによって、電解質と電極、および拡張するバッテリ寿命の間の分解反応を防止、安定した固体電解質界面（SEI）を形成します。しかし、炭酸塩溶媒は、短絡が存在する場合、潜在的に深刻な安全性の問題で、55℃以下にリチウムイオン電池の動作温度を制限し、低沸点及び引火点に苦しみます。 10,11 イオン性液体は、100℃以下の融解温度を有する塩のクラスです。 図12は、典型的な無機塩とは対照的に、イオン性液体は、広い液体範囲を有し、室温で液体であることができます。イオン液体は、イミダゾリウム、ホスホニウム、ピリジニウム、またはアンモニウムなどの1つまたは複数の有機カチオン性センターから構成され、例えば、メタンスルホン酸塩、ヘキサフルオロリン酸、またはハロゲン化物、無機又は有機アニオンと対になっています。 13,14可能なカチオンとアニオンの組み合わせの多様な調整可能な特性を持つ多数の組成物を可能にします。また、イオン性液体中に強いイオン相互作用が無視できる程度の蒸気圧、非可燃性、及び高い熱的および電気化学的安定性をもたらします。 15,16 イオン性液体と、従来の電解質を交換すると、現在のリチウムイオン電池に固有の安全性の問題に対処する一つの解決策であり、かつ高温での用途を可能にすることができます。 17-27は、高温用途のためのイオン性液体を含有するリチウムイオン電池を構築するために利用される一般的な合成材料の処理方法を説明するために、我々は、合成、熱特性、およびとペアモノ-およびジ-ホスホニウムイオン性液体の電気化学的特徴付けを記載するいずれかの塩化物（CL）またはビス（トリフルオロメタンスルホン酸）イミド（TFSI）アニオン。リチウムビス（トリフルオロメタン）スルホンイミド（LiTFSI）の異なる濃度は、その後ホスホニウムイオンliquに追加されidは、電解質を得ました。塩化アナログに比べて追加のLiTFSIとホスホTFSI電解質の性能に基づいて、コイン電池は、リチウム金属アノードとのLiCoO 2カソードと一緒にモノまたはジホスホTFSI電解質のいずれかで構成されています。最後に、電池性能は、二つの異なったコイン型電池を100℃で評価されます。これらの実験を行うことから得られた詳細な手順、実行中の課題、および洞察力は、以下に記載されています。

<table><tbody><tr><td>Silicone oil</td><td>Sigma-Aldrich</td><td>85409</td><td></td></tr><tr><td>Potassium hydroxide</td><td>Sigma-Aldrich</td><td>221473</td><td>Corrosive</td></tr><tr><td>Rotary evaporator</td><td>Buchi</td><td>R-124</td><td></td></tr><tr><td>High-vacuum pump</td><td>Welch</td><td>8907</td><td></td></tr><tr><td>Nitrogen, ultra high purity</td><td>Airgas</td><td>NI UHP300</td><td>Compressed gas</td></tr><tr><td>Tetrahydrofuran, stabilized with BHT</td><td>Pharmco-Aaper</td><td>346000</td><td>Flammable. Dried before use.</td></tr><tr><td>Dichloromethane</td><td>Pharmco-Aaper</td><td>313000</td><td>Flammable, toxic.</td></tr><tr><td>Separatory funnel (1 L)</td><td>Fisher Scientific</td><td>13-678-606</td><td></td></tr><tr><td>Sodium sulfate</td><td>Sigma-Aldrich</td><td>239313</td><td></td></tr><tr><td>Ethanol, absolute</td><td>Pharmco-Aaper</td><td>111USP200</td><td>Flammable, toxic.</td></tr><tr><td>Buchner funnel</td><td>Fisher Scientific</td><td>FB-966-F</td><td></td></tr><tr><td>Methanol</td><td>Pharmco-Aaper</td><td>339000ACS</td><td>Flammable, toxic.</td></tr><tr><td>Triethylamine (anhydrous)</td><td>Sigma-Aldrich</td><td>471283</td><td>Toxic, flammable, harmful to environment</td></tr><tr><td>Glass syringe</td><td>Hamilton Company</td><td>1700-series</td><td></td></tr><tr><td>Deuterated chloroform</td><td>Cambridge Isotopes Laboratories, Inc.</td><td>DLM-29-10</td><td>Toxic</td></tr><tr><td>Nuclear magnetic resonance instrument</td><td>Varian</td><td>V400</td><td></td></tr><tr><td>Hydrogen</td><td>Airgas</td><td>HY HP300</td><td>Highly flammable.</td></tr><tr><td>Hexanes</td><td>Pharmco-Aaper</td><td>359000ACS</td><td>Toxic, flammable.</td></tr><tr><td>Differential scanning calorimeter</td><td>TA Instruments</td><td>Q100</td><td></td></tr><tr><td>&lt;em&gt;N,N&lt;/em&gt;-dimethylformamide</td><td>Sigma-Aldrich</td><td>227056</td><td>Toxic, flammable.</td></tr><tr><td>Trihexylphosphone</td><td>TCI America</td><td></td><td>Toxic, flammable.</td></tr><tr><td>1-Chlorodecane</td><td>Sigma-Aldrich</td><td></td><td>Toxic, flammable.</td></tr><tr><td>Bis(trifluoromethane)sulfonimide lithium salt</td><td>Sigma-Aldrich</td><td></td><td>Hydrophilic</td></tr><tr><td>1,10-dichlorodecane</td><td>Sigma-Aldrich</td><td></td><td>Toxic, flammable.</td></tr><tr><td>Thermal Gravemetric Analysis (TGA)</td><td>TA Q50</td><td>TA instruments</td><td></td></tr><tr><td>Differential scanning calorimeter (DSC)</td><td>TA Q100</td><td>TA instruments</td><td></td></tr><tr><td>Controlled Strain Rheometer</td><td>AR 1000&amp;nbsp;</td><td></td><td></td></tr><tr><td>Conductivity Meter&amp;nbsp;</td><td>Consort</td><td>K912</td><td>4-electrode cell</td></tr><tr><td>Potentiostat/Galvanostat</td><td>Princeton Applied Research&amp;nbsp;</td><td>VersaStat MC4&amp;nbsp;</td><td>Electrochemical testing</td></tr><tr><td>Separators</td><td>Celgard&amp;nbsp;</td><td>C480&amp;nbsp;</td><td>polypropylene/polyethylene</td></tr><tr><td>CR2032 coin cells</td><td>MTI Corp.</td><td>EQ-CR2032-CASE</td><td></td></tr><tr><td>LiCoO&lt;sub&gt;2&lt;/sub&gt; electrode&amp;nbsp;</td><td>MTI Corp.</td><td>EQ-CR2032</td><td>Cathode material</td></tr><tr><td>lithium metal&amp;nbsp;</td><td>Alfa Aesar</td><td>10769</td><td>Anode Material</td></tr><tr><td>Stainless Steel Spacer</td><td>MTI Corp.</td><td>EQ-CR20-Spacer304-02</td><td>15.5 mm Dia x 0.2 mm</td></tr><tr><td>Wave Spring</td><td>MTI Corp.</td><td>EQ-CR20WS-Spring304</td><td></td></tr><tr><td>Electric Coin Cell Crimping Machine</td><td>MTI Corp.</td><td>MSK-160D</td><td></td></tr><tr><td>Glove box</td><td>Mbraun</td><td></td><td>Water free, oxygen free operation</td></tr></tbody></table>

synthesis of ionic liquid based electrolytes, assembly of li-ion batteries, and measurements of performance at high temperature

従来の電解質の化学的不安定性は、例えば、リチウムイオン電池として広く使用されているエネルギー貯蔵装置における安全性の問題のままです。高温で動作するデバイスで使用するためのリチウムイオン電池は、熱的に安定であり、不燃性電解質を必要とします。不燃性、不揮発性、熱的に安定した溶融塩であるイオン性液体（ILS）は、現在、今日使用可燃性および低沸点の有機溶媒電解質のための理想的な代替品です。当社は、本明細書に手順を説明します。1）塩化物またはビス（トリフルオロメタンスルホン酸）イミド（TFSI）アニオンと対になったモノ - およびジ - ホスホイオン液体を合成します。 2）示差走査熱量測定（DSC）及び熱重量分析（TGA）により、これらのイオン液体の熱的特性および安定性を測定します。 3）サイクリックボルタンメトリー（CV）によって、イオン性液体の電気化学的特性を測定します。 ; 4）、リチウムビス（トリフルオロメタン）スルホンアミドを含有する電解質を準備5）共同を測定温度の関数としての電解質のnductivity。 6）Li金属アノード及びLiCoO 2を正極と一緒に電解質2とコイン型電池を組み立てます。 7）100℃での電池性能を評価します。我々はさらに、実行中の課題だけでなく、これらの実験を行うことから得られた洞察を説明します。

イオン液体、モノHexC10ClおよびジHexC10Clは、求核反応を介して調製し、そしてそれに続くハロゲン交換反応は、（ 図1A）は、それぞれ、モノHexC10TFSI及びジHexC10TFSIイオン性液体を得ました。 14すべての4つのイオン性液体は無色でわずかに粘性液体（ 図1B）でした。モノHexC10TFSIイオン性液体の代表的な1 H NMRは、 図1C...

Watch this Scientific Journal Video about Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature at JoVE.com

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

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 ...

synthesis-ionic-liquid-based-electrolytes-assembly-li-ion-batteries

Universidad San Sebastian

Research

JoVE Journal

Engineering

12.9K ビュー.  Boston University. 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.

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

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 ...

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. ...

Ultrasound Velocity Measurement in a Liquid Metal Electrode

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently more difficult than measuring the flow of a transparent fluid, since optical methods are not applicable. Ultrasound can be used to measure the velocity of an opaque fluid, not only at isolated points, but at hundreds or thousands of points arrayed along lines, with good temporal resolution. When applied to a liquid metal electrode, ultrasound velocimetry involves additional challenges: high temperature, chemical activity, and electrical conductivity. Here we describe the experimental apparatus and methods that overcome these challenges and allow the measurement of flow in a liquid metal electrode, as it conducts current, at operating temperature. Temperature is regulated within &#177;2 &#176;C using a Proportional-Integral-Derivative (PID) controller that powers a custom-built furnace. Chemical activity is managed by choosing vessel materials carefully and enclosing the experimental setup in an argon-filled glovebox. Finally, unintended electrical paths are carefully prevented. An automated system logs control settings and experimental measurements, using hardware trigger signals to synchronize devices. This apparatus and these methods can produce measurements that are impossible with other techniques, and allow optimization and control of electrochemical technologies like liquid metal batteries.

Ultrasound velocimetry is used to study mixing by fluid flow in liquid metal electrodes. The focus of this manuscript is to illustrate the methods used for making precise, spatially-resolved ultrasound measurements while limiting oxidation and controlling and monitoring temperature, applied current, and the heater power being supplied.

液体金属電極中の超音波速度計測

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently ...

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 ...

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.

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 ...

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 ...

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 ...

Identification and Quantification of Decomposition Mechanisms in Lithium-Ion Batteries; Input to Heat Flow Simulation for Modeling Thermal Runaway

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of thermal runaway (TR), the exothermic decomposition reactions in anode and cathode were studied, using a Simultaneous Thermal Analysis (STA)/Gas Chromatography-Mass Spectrometry (GC-MS)/Fourier Transform Infrared (FTIR) spectrometer system. These techniques allowed the identification of the reaction mechanisms in each electrode, owing to the analysis of evolved gaseous species, the amount of heat released and mass loss. These results provided insight into the thermal events happening within a broader temperature range than covered in previously published models. This allowed the formulation of an improved thermal model to depict TR. The heat of reaction, activation energy, and frequency factor (thermal triplets) for each major exothermic process at material level were investigated in a Lithium Nickel-Manganese-Cobalt-Oxide (NMC (111))-Graphite battery cell. The results were analyzed, and their kinetics were derived. These data can be used to successfully simulate the experimental heat flow.

This work aims at determining the reaction kinetics of Li-ion battery cathode and anode materials undergoing thermal runaway (TR). Simultaneous Thermal Analysis (STA)/Fourier Transform Infrared (FTIR) spectrometer/Gas Chromatography Mass Spectrometry (GC-MS) were used to reveal thermal events and to detect evolved gases.

リチウムイオン電池の分解メカニズムの同定と定量化。熱暴走モデリングのための熱流シミュレーションへの入力

The risks and possible accidents related to the normal use of lithium-ion batteries remain a serious concern. In order to get a better understanding of ...

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

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

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

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

液体金属電極中の超音波速度計測

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

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

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

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

リチウムイオン電池の分解メカニズムの同定と定量化。熱暴走モデリングのための熱流シミュレーションへの入力

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

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

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

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

液体金属電極中の超音波速度計測

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

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

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

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

リチウムイオン電池の分解メカニズムの同定と定量化。熱暴走モデリングのための熱流シミュレーションへの入力

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

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