JP2021022580A - 安定したシリコンイオン液体界面のリチウムイオン電池 - Google Patents
安定したシリコンイオン液体界面のリチウムイオン電池 Download PDFInfo
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- JP2021022580A JP2021022580A JP2020184856A JP2020184856A JP2021022580A JP 2021022580 A JP2021022580 A JP 2021022580A JP 2020184856 A JP2020184856 A JP 2020184856A JP 2020184856 A JP2020184856 A JP 2020184856A JP 2021022580 A JP2021022580 A JP 2021022580A
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 title claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 16
- 239000010703 silicon Substances 0.000 title claims description 16
- 239000002608 ionic liquid Substances 0.000 title description 12
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- -1 1-ethyl Chemical group 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 36
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 13
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- KTQDYGVEEFGIIL-UHFFFAOYSA-N n-fluorosulfonylsulfamoyl fluoride Chemical compound FS(=O)(=O)NS(F)(=O)=O KTQDYGVEEFGIIL-UHFFFAOYSA-N 0.000 description 5
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- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
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- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
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- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910004499 Li(Ni1/3Mn1/3Co1/3)O2 Inorganic materials 0.000 description 1
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- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical group OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 1
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
Description
本出願は、2014年10月30日付出願の米国出願第62/072,957号の利益を主張するものである。この出願の全内容は、参照により本明細書に組み込まれる。
nSi−cPAN及びLi(Ni1/3Mn1/3Co1/3)O2電極は、我々の手順に従って製造された。カソードとアノードの両方での活物質の質量負荷は、以前の研究の少なくとも2倍である。イオン性液体電解質は、Boulder Ionics Corporation(米国)によって提供され、ハロゲン化物不純物についてスキャンされた。不純物(F−、CI−、Br−、SO4 −)は、Dionex ICS−1100のクロマトグラフを用いて定量化され、1ppmの低感度で較正された。イオンクロマトグラフィーは、この研究で使用した全てのイオン性液体及びリチウム塩について実施され、各溶液の全不純物含有量は、電解質の全質量中の電解質成分の質量百分率に基づいて計算された。溶液は、20ppm(w/w)未満の水分と、10ppm(w/w)未満のハロゲン化物及び金属イオン不純物とを含有した。エチレンカーボネート:炭酸ジエチル(50:50、Soulbrain)中の1M LiPF6は、従来の有機電解質として使用された。
電気化学的測定は、Arbin(商標)のBT2000の電池試験ステーションを用いて行われた。すべての半電池は、準備したnSi−cPAN電極を作用電極として、リチウム金属箔を対電極として用いて組み立てられた。セパレータは、ガラスマイクロファイバーディスク(Whatman(商標)GF/F)であり、シェルは、ステンレス鋼CR2032のコインセル(プレッドマテリアル(Pred Materials))であった。使用された電解質系は、EC/DEC(1M LiPF6)、PYR13FSI(1.2M LiFSI)、PYR13TFSI(0.6M LiTFSI)、及びEMIMFSI(1.2M LiFSI)であった。我々は、半電池をサイクルさせるための定電流(CC)の試験スキームを使用した。セルのクーロン効率の真の性能を明らかにするために、サイクリング中に保持が利用されなかった。半電池は、0.05と1V(対Li/Li+)の間で様々なサイクル電流(C/10の比率が353.6μA/cm−2に等しい)で放電されたり(リチオ化される)、充電された(脱リチオ化される)。半電池の電気化学的測定は、各電極においてSi活物質の質量(典型的には1.1−1.3mg)に基づいてすべて標準化された。我々は、フルセルをサイクルさせるために定電流定電圧(CCCV)の試験方式を使用した。フルセルは、2と4.15V(対Li/Li+)の間で、様々なサイクリング電流で充放電された(C/2の比率が、図6(A)のフルセルに対する502.9μA・cm−2及び図6(B)のフルセルに対する197.3μA・cm−2に相当する)。フルセルの電気化学的測定は、カソード電極とアノード電極の両方における電気活性材料の総質量(典型的には7−9mg)に関して全て平均化された。
2種類の計算は、上記のように行われた。また、静的クラスタ系計算やLi13S4のスラブを用いた非経験的分子動力学(AIMD)のシミュレーションの詳細な説明が、含まれている。
可動エアロックチャンバーを備えたFIB(FEI、NOVA200のデュアルビームシステム)は、TEMサンプルの調製に使用された。TEM及びEELS分析は、200keVで操作されるFEI Tecnai F20を用いて行われた。
コインセル試験用の電極調製と同様に、nSi−cPAN膜は、直径1インチのPt5MHzの共鳴水晶(スタンフォード・リサーチ・システム(Stanford Research Systems);SRS)上にコーティングされた。セルにおける電気化学的活性領域は、結晶上のPtパターンに基づいて、1.359cm2であると決定された。石英結晶上の厚膜を使用して周波数測定に伴う誤差を緩和するために、すべてのnSi−cPAN膜は、10μm未満の厚さで製造された。結晶は、SRS QCM200の結晶ホルダに入れられた。ホルダは、2.5mLの容量のスタンドアロンセルをふたで囲まれ得るように、PEEKの絶縁材で改造された。セルの天井は、Liのホイル対電極に並べられ、銅線に接続された。全ての電流及び潜在的パラメータは、コインセルの電気化学的特性と一致した。
フルセルは、送達可能な容量に基づいて選択された前処理された電極から作製された。活物質の質量から計算することで、nSi−cPANのアノードは、総アノード容量がカソード容量の約160%となるように製造されると共に、L333のカソードと合わせた。両方の電極は、前処理された:アノードは、半電池の構成で10回の充放電のサイクルで運転させることが許容され、完全リチオ化後にアノードを停止されたが、一方で、カソードは、半電池の構成で3回の充放電サイクルで運転されることが許容され、完全脱リチオ化後に停止された。次いで、半電池は、分解されると共に、電極を用いて2032のコインセル(Al被覆のカソードカップ)タイプのフルセルを作製するのに用いられた。この予備調整の方法は、システム内のリチウムの量を完全に制御することを可能にする。
図8は、FSI−及びTFSI−のアニオンの単電子還元を示す。図(A)は、Li+(TFSI−)2を示す。図(B)は、過剰な電子を(A)に添加することが、得られたFSI−のラジカル・ジアニオンを自発的に分解することを示す。図(C)は、Li+(TFSI−)2を示す。図(D)は、電子を(C)に添加することが、得られたTFSI−のジアニオンを分解することを示す。理論的研究の第1のタイプは、孤立したFSI−(図8(A))やTFSI−(図8(B))のアニオンであって、Li+に配位し、その周りのイオン性液体の影響を近似する誘電連続体に「溶媒和」したアニオン上のクラスタ系の局部的基礎計算からなる。これらは、バルク液体電解質中の1電子還元経路を模倣し、初期のSEI形成によって電子伝達速度が遅くなるときに起こるはずである。誘電的に溶媒和されたLi+(TFSI−)2のクラスタに過剰な電子を加えることは、自発的に幾何学的な最適化計算におけるFSI2−のラジカル・ジアニオンからF−の損失をもたらす(図8(C))。Li+(TFSI−)2にe−を注入し、幾何学的な最適化を実行することは、得られるTFSI2−を分解して、図9(d)に示された2つのフラグメント:SO2CF3 −及びNSO2CF3 −をもたらす。後者はラジカル・アニオンである。TFSI−に関する我々の予測は、Li+なしの孤立したTFSI−で行われた計算と一致する。予測は、ハイブリッドPBEO機能が使用される場合と同様である。これらの計算は、4配位のLi+を与えるための2つのFSI−又はTFSI−で使用される。1つの過剰な電子をLi+FSI−又はLi+TFSI−のクラスタに加えることは、配位の低いLi+の非物理的な還元をLi0にもたらす。注:上記は、反応速度論又は電子移動速度には無関係な単一過剰電子系の静的計算である。
2種類の計算が行われた。Li及び2つのFSI−又はTFSI−のアニオンを用いた静的クラスタ系計算は、ガウスの一連のプログラム、PBE及びPBE0関数の両方、最適化のための基底6−31+G(d、p)、及び誘電率εが40程度に設定されたSMDの誘電連続体を用いて実行された。クラスタが−2|e|の正味電荷と正味スピンを示すように、1つの過剰な電子はこれらの計算で加えられる。
上述の「潜在的なオーバーシュート」現象は、コインセル及びEQCMの浸水セル構成において有機的及びIL系電解質の両方を使用する以前の研究で観察されている。ポリマーマトリックス内に埋め込まれた非晶質SiOスラリーと同様に、蒸着されたSiOx膜に見られる。式Siのように、シリコン膜上の自然酸化膜が減少するので、オーバーシュートは、一般的に、Li2O及び他の分解生成物の核形成に起因する。
〔付記1〕
活物質を含むアノードであって、前記活物質はナノシリコン粒子を含み、前記ナノシリコン粒子は環化ポリアクリロニトリルでコーティングされているアノードと、
室温イオン性液体電解質及び塩を含むイオン性液体電解質と、
前記アノードの全ての露出した表面に形成された膜であって、当該膜はフッ素、酸素、硫黄、炭素、及びリチウムを含む膜と、
カソードと、
を備えた電気エネルギー貯蔵装置。
〔付記2〕
前記室温イオン性液体電解質は、ピロリジニウム、1−エチル−3−メチル−イミダゾリウム、ビス(トリフルオロメタンスルホニル)イミド、及びビス(フルオロスルホニル)イミドからなる群から選択される、付記1に記載の装置。
〔付記3〕
前記イオン性液体電解質の前記塩が、リチウムビス(フルオロスルホニル)イミド塩(LiFSI)を含む、付記1に記載の装置。
〔付記4〕
前記イオン性液体電解質は、PYR13FSIを含む、付記1から3のいずれか一項に記載の装置。
〔付記5〕
前記アノードは、バルク型複合アノードを含む、付記1から4のいずれか一項に記載の装置。
〔付記6〕
前記バルク型複合アノードは、約5マイクロメートルより大きい厚さを有する、付記5に記載の装置。
〔付記7〕
電池を充放電する工程であって、前記電池は、
活物質を含むアノードであって、前記活物質はナノシリコン粒子を含み、前記ナノシリコン粒子は環化ポリアクリロニトリルでコーティングされているアノードと、
室温イオン性液体電解質及び塩を含むイオン性液体電解質と、
カソードと、を備える、工程と、
前記アノードの全ての露出した表面にフッ素、酸素、硫黄、炭素、及びリチウムを含む固体電解質中間膜を形成する工程と、
を含む方法。
Claims (8)
- 電極システムであって、
複数のナノシリコンを含む活物質と、
前記活物質を結合させて電気及びリチウムイオンを伝導させるポリアクリロニトリルポリマーであって、当該ポリアクリロニトリルポリマーが前記複数のナノシリコン粒子のそれぞれをコンフォーマル且つ個別にカバーするポリアクリロニトリルポリマーと、を備える、
電極システムと、
第2の電極と、
前記電極システムと第2電極とを接触させるための室温イオン性液体電解質であって、当該室温イオン性液体電解質がピロリジニウム及び1−エチル1−3−メチルイミダゾリウムからなる群から選択される陽イオン種を含む室温イオン性液体電解質と、
を備える電気エネルギー貯蔵装置。 - 前記電極システムは、環化ポリアクリロニトリルシリコンのナノコンポジット(nSi−cPAN)を含む、請求項1に記載の装置。
- 前記電極システムは、nSi−cPANを含み、前記室温イオン性液体電解質は、PYR13FSIを備える、請求項1に記載の装置。
- 前記電極システムは、バルク型複合電極を含む、請求項3に記載の装置。
- 前記バルク電極は、約5マイクロメートルより大きい厚さを有する、請求項4に記載の装置。
- 前記ナノシリコン粒子は、1〜500nmの範囲の大きさを有する、請求項1に記載の装置。
- 前記電極システムは、約70wt%のナノシリコン粒子と、約30wt%のポリアクリロニトリルポリマーとを含む、請求項1に記載の装置。
- 前記電極システムは、10〜50μmの範囲の厚さを有する、請求項1に記載の装置。
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WO2022244271A1 (ja) * | 2021-05-21 | 2022-11-24 | 昭和電工マテリアルズ株式会社 | エネルギー貯蔵デバイス用電極、エネルギー貯蔵デバイス、エネルギー貯蔵デバイス用電極の製造方法及び結着材 |
WO2022244884A1 (ja) * | 2021-05-21 | 2022-11-24 | 昭和電工マテリアルズ株式会社 | エネルギー貯蔵デバイス用電極、エネルギー貯蔵デバイス、エネルギー貯蔵デバイス用電極の製造方法及び結着材 |
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KR20240005174A (ko) | 2024-01-11 |
CN115275320A (zh) | 2022-11-01 |
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JP2017539051A (ja) | 2017-12-28 |
KR102619076B1 (ko) | 2024-01-05 |
US20170338474A1 (en) | 2017-11-23 |
EP3213363B1 (en) | 2021-01-06 |
WO2016070120A1 (en) | 2016-05-06 |
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