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ホーム / ブログ / ESM:実用的な高エネルギーリチウム電池用の過フッ素化電解質の内蔵ウルトラコンフォーマルインターフェース ESM:実用的な高エネルギーリチウム電池用の過フッ素化電解質の内蔵ウルトラコンフォーマルインターフェース
研究の背景
リチウムイオン電池では、350 Wh Kg-1の目標を達成するために、カソード材料はニッケルに富む層状酸化物(LiNixMnyCozO2、x + y + z = 1、NMCxyzと呼ばれる)を使用します。 エネルギー密度の増加に伴い、LIBの熱暴走に関連する危険性が人々の注目を集めています。 材料の観点から、ニッケルに富む正極には重大な安全上の問題があります。 さらに、有機液体や負極などの他のバッテリーコンポーネントの酸化/クロストークも熱暴走を引き起こす可能性があり、これは安全上の問題の主な原因と考えられています。 安定した電極-電解質界面のその場で制御可能な形成は、次世代の高エネルギー密度リチウムベースの電池の主要な戦略です。 具体的には、より高い熱安定性の無機成分を備えた固体で高密度の陰極-電解質中間相(CEI)は、酸素の放出を抑制することによって安全性の問題を解決することができます。 これまでのところ、CEIカソード改質材料とバッテリーレベルの安全性に関する研究は不足しています。
アチーブメント表示
最近、清華大学のFeng Xuning、Wang Li、およびOuyang Minggaoは、エネルギー貯蔵材料に関する「内蔵の超共形中間相が高安全で実用的なリチウム電池を可能にする」というタイトルの研究論文を発表しました。 著者は、実用的なNMC811 / Grソフトパックフルバッテリーの安全性能と対応するCEI正極の熱安定性を評価しました。 材料とソフトパック電池の間の熱暴走抑制メカニズムが包括的に研究されています。 不燃性の過フッ素化電解液を使用して、NMC811 / Grポーチタイプのフルバッテリーを準備しました。 NMC811の熱安定性は、無機LiFが豊富なその場で形成されたCEI保護層によって改善されました。 LiFのCEIは、相変化によって引き起こされる酸素放出を効果的に軽減し、喜んでいるNMC811とフッ素化電解質の間の発熱反応を抑制することができます。
グラフィックガイド
図1過フッ素化電解液と従来の電解液を使用した実用的なNMC811 / Grポーチ型フルバッテリーの熱暴走特性の比較。 従来の(a)EC / EMCおよび(b)過フッ素化FEC / FEMC / HFE電解質ポーチタイプのフルバッテリーの100サイクル後。 (c)従来のEC / EMC電解および(d)XNUMXサイクル後にエージングされた過フッ素化FEC / FEMC / HFE電解質ポーチタイプのフルバッテリー。
811サイクル後の従来の電解液を使用したNMC1 / Grバッテリー(図2a)の場合、T202.5は2°Cです。 T2は、開回路電圧が低下したときに発生します。 しかし、過フッ素化電解質を使用したバッテリーのT220.2は1°Cに達し(図2b)、これは、過フッ素化電解質がより高い熱安定性により、バッテリーの固有の熱安全性をある程度改善できることを示しています。 バッテリーが古くなると、従来の電解質バッテリーのT195.2値は1°Cに低下します(図2c)。 ただし、エージングプロセスは、過フッ素化電解質を使用するバッテリーのT1には影響しません(図113d)。 さらに、TR中に従来の電解質を使用したバッテリーの最大dT / dt値は1°Cs-32と高く、過フッ素化電解質を使用したバッテリーはわずか1°Cs-2です。 経年劣化したバッテリーのT811の違いは、喜びのNMCXNUMXの固有の熱安定性に起因する可能性があります。これは、従来の電解質では低下しますが、過フッ素化電解質では効果的に維持できます。
図2脱リチウム化NMC811正極とNMC811 / Grバッテリー混合物の熱安定性。 (A、b)C-NMC811およびF-NMC811シンクロトロン高エネルギーXRDの等高線図と対応する(003)回折ピークの変化。 (c)C-NMC811およびF-NMC811の正極の加熱および酸素放出挙動。 (d)喜ばしい正極、リチウム化された負極、および電解質のサンプル混合物のDSC曲線。
図2aおよびbは、従来の電解質の存在下で、室温から81°Cまでの期間における、さまざまなCEI層を備えた喜ばしいNMC600のHEXRD曲線を示しています。 結果は、電解質の存在下で、強力なCEI層がリチウム堆積カソードの熱安定性を助長することを明確に示しています。 図2cに示すように、単一のF-NMC811は233.8°Cでより遅い発熱ピークを示しましたが、C-NMC811の発熱ピークは227.3°Cで現れました。 さらに、C-NMC811の相転移によって引き起こされる酸素放出の強度と速度はF-NMC811のものよりも厳しく、堅牢なCEIがF-NMC811の固有の熱安定性を改善することをさらに確認します。 図2dは、喜んでいるNMC811と他の対応するバッテリーコンポーネントの混合物に対してDSCテストを実行します。 従来の電解液の場合、1サイクルと100サイクルのサンプルの発熱ピークは、従来の界面の経年劣化により熱安定性が低下することを示しています。 対照的に、過フッ素化電解質の場合、1サイクル後と100サイクル後の図は、TRトリガー温度(T2)に沿って、広く穏やかな発熱ピークを示しています。 結果(図1)は一貫しており、強力なCEIが、老朽化して喜んでいるNMC811およびその他のバッテリーコンポーネントの熱安定性を効果的に改善できることを示しています。
図3過フッ素化電解液中の喜ばれたNMC811正極の特性評価。 (ab)老化したF-NMC811正極の断面SEM画像と対応するEDSマッピング。 (ch)要素の分布。 (ij)仮想xy上の老化したF-NMC811正極の断面SEM画像。 (km)3DFIB-SEM構造の再構築とF要素の空間分布。
フッ素化CEIの制御可能な形成を確認するために、実際のソフトパックバッテリーで回収された老化したNMC811正極の断面形態と元素分布を、FIB-SEMで特性評価しました(図3ah)。 過フッ素化電解液では、F-NMC811の表面に均一なフッ素化CEI層が形成されます。 逆に、従来の電解液中のC-NMC811はFを欠き、不均一なCEI層を形成します。 F-NMC811の断面のF元素含有量(図3h)はC-NMC811の含有量よりも高く、無機フッ素化中間相のその場形成が喜びのNMC811の安定性を維持するための鍵であることをさらに証明しています。 図3mに示すように、FIB-SEMおよびEDSマッピングの助けを借りて、F-NMC3の表面の811Dモデルで多くのF要素を観察しました。
図4a)元の喜びのNMC811正極の表面での元素の深さの分布。 (ac)FIB-TOF-SIMSは、NMC811の正極にF、O、およびLi元素の分布をスパッタリングしています。 (df)NMC811のF、O、およびLi要素の表面形態と深さ分布。
FIB-TOF-SEMは、NMC811の正極表面の元素の深さ分布をさらに明らかにしました(図4)。 元のサンプルおよびC-NMC811サンプルと比較して、F-NMC811の上面層でFシグナルの有意な増加が見られました(図4a)。 さらに、表面の弱いOおよび高いLi信号は、FおよびLiに富むCEI層の形成を示しています(図4b、c)。 これらの結果はすべて、F-NMC811がLiFに富むCEI層を持っていることを確認しました。 C-NMC811のCEIと比較して、F-NMC811のCEI層にはより多くのFおよびLi元素が含まれています。 また、図1および図2に示すように、 4d-f、イオンエッチングの深さの観点から、元のNMC811の構造は、喜んでいるNMC811の構造よりも堅牢です。 時効したF-NMC811のエッチング深さはC-NMC811よりも浅く、F-NMC811の構造安定性に優れています。
図5NMC811の正極表面のCEI化学組成。 (a)NMC811正極CEIのXPSスペクトル。 (bc)元のNMC1正極CEIのXPSC1sおよびF811sスペクトル。 (d)低温透過型電子顕微鏡:F-NMC811の元素分布。 (e)F-NMC81上に形成されたCEIの凍結TEM画像。 (fg)C-NMC811のSTEM-HAADFおよびSTEM-ABF画像。 (hi)F-NMC811のSTEM-HAADFおよびSTEM-ABF画像。
彼らはXPSを使用して、NMC811のCEIの化学組成を特徴付けました(図5)。 オリジナルのC-NMC811とは異なり、F-NMC811のCEIには、大きいFとLiが含まれていますが、小さいCが含まれています(図5a)。 C種の減少は、LiFが豊富なCEIが電解質との持続的な副反応を減少させることによってF-NMC811を保護できることを示しています(図5b)。 さらに、少量のCOおよびC = Oは、F-NMC811の加溶媒分解が制限されていることを示します。 XPSのF1sスペクトル(図5c)で、F-NMC811は強力なLiF信号を示し、CEIにフッ素化溶媒に由来するLiFが大量に含まれていることを確認しました。 F-NMC811粒子の局所領域のF、O、Ni、Co、およびMn元素のマッピングは、詳細が全体として均一に分布していることを示しています(図5d)。 図5eの低温TEM画像は、CEIがNMC811正極を均一に覆う保護層として機能できることを示しています。 界面の構造変化をさらに確認するために、高角度円形暗視野走査透過電子顕微鏡(HAADF-STEMおよび円形明視野走査透過電子顕微鏡(ABF-STEM)実験)を実施しました。炭酸電解質(C -NMC811)、循環する正極の表面は急激な相変化を起こし、正極の表面には無秩序な岩塩相が蓄積します(図5f)。過フッ素化電解質の場合、F-NMC811の表面正極は層状構造を維持し(図5h)、有害であることを示しています。相は効果的に抑制されます。さらに、F-NMC811の表面に均一なCEI層が観察されました(図5i-g)。これらの結果は、過フッ素化電解質中のNMC811の正極表面のCEI層。
図6a)NMC811正極の表面の相間相のTOF-SIMSスペクトル。 (ac)NMC811の正極上の特定の180番目のイオンフラグメントの詳細な分析。 (df)元のC-NMC811およびF-NMC811でのXNUMX秒のスパッタリング後のXNUMX番目のイオンフラグメントのTOF-SIMS化学スペクトル。
C2Fフラグメントは一般にCEIの有機物質と見なされ、LiF2-およびPO2-フラグメントは通常無機種と見なされます。 実験では、LiF2-およびPO2-の大幅に増強された信号が得られ(図6a、b)、F-NMC811のCEI層に多数の無機種が含まれていることを示しています。 逆に、F-NMC2のC811F信号はC-NMC811の信号よりも弱いため(図6c)、F-NMC811のCEI層には脆弱な有機種が含まれていません。 さらなる研究により、F-NMC6のCEIには無機種が多く、C-NMC811には無機種が少ないことがわかりました(図811d-f)。 これらの結果はすべて、過フッ素化電解質に無機物に富む固体CEI層が形成されていることを示しています。 従来の電解質を使用したNMC811 / Grソフトパックバッテリーと比較して、過フッ素化電解質を使用したソフトパックバッテリーの安全性の向上は、次の理由によるものです。まず、無機LiFが豊富なCEI層のその場形成が有益です。 喜ばれるNMC811正極の固有の熱安定性は、相転移によって引き起こされる格子酸素の放出を減らします。 第二に、固体無機CEI保護層は、反応性の高い脱リチウム化NMC811が電解質に接触するのをさらに防ぎ、発熱副反応を低減します。 第三に、過フッ素化電解質は高温で高い熱安定性を持っています。
結論と展望
この研究は、過フッ素化電解質を使用した実用的なGr / NMC811ポーチタイプのフルバッテリーの開発を報告しました。これにより、安全性能が大幅に向上しました。 固有の熱安定性。 TR抑制メカニズムと材料とバッテリーレベルの相関関係の詳細な研究。 エージングプロセスは、ストーム全体での過フッ素化電解質バッテリーのTRトリガー温度(T2)に影響を与えません。これは、従来の電解質を使用するエージングバッテリーに比べて明らかな利点があります。 さらに、発熱ピークはTRの結果と一致しており、強いCEIがリチウムを含まない正極やその他のバッテリーコンポーネントの熱安定性を助長していることを示しています。 これらの結果は、安定したCEI層のその場制御設計が、より安全な高エネルギーリチウム電池の実用化にとって重要な指針となる重要性を持っていることを示しています。
文学情報
内蔵の超コンフォーマル中間相により、安全性の高い実用的なリチウム電池、エネルギー貯蔵材料、2021年が可能になります。