JP2022539947A - 再充電可能なバッテリーセル用のso2ベースの電解質および再充電可能なバッテリーセル - Google Patents
再充電可能なバッテリーセル用のso2ベースの電解質および再充電可能なバッテリーセル Download PDFInfo
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- JP2022539947A JP2022539947A JP2021568388A JP2021568388A JP2022539947A JP 2022539947 A JP2022539947 A JP 2022539947A JP 2021568388 A JP2021568388 A JP 2021568388A JP 2021568388 A JP2021568388 A JP 2021568388A JP 2022539947 A JP2022539947 A JP 2022539947A
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- SGYOHBMMKNRZRP-UHFFFAOYSA-M [Li+].[O-]S(Cl)(=O)=O Chemical compound [Li+].[O-]S(Cl)(=O)=O SGYOHBMMKNRZRP-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- HNCXPJFPCAYUGJ-UHFFFAOYSA-N dilithium bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].[Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F HNCXPJFPCAYUGJ-UHFFFAOYSA-N 0.000 description 1
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 description 1
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- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 1
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- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 description 1
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- 239000002931 mesocarbon microbead Substances 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
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- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 239000007774 positive electrode material Substances 0.000 description 1
- XIUFWXXRTPHHDQ-UHFFFAOYSA-N prop-1-ene;1,1,2,2-tetrafluoroethene Chemical group CC=C.FC(F)=C(F)F XIUFWXXRTPHHDQ-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 125000004309 pyranyl group Chemical group O1C(C=CC=C1)* 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
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- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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- 229910052717 sulfur Inorganic materials 0.000 description 1
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- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
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- VRSRNLHMYUACMN-UHFFFAOYSA-H trilithium;hexafluoroaluminum(3-) Chemical compound [Li+].[Li+].[Li+].[F-].[F-].[F-].[F-].[F-].[F-].[Al+3] VRSRNLHMYUACMN-UHFFFAOYSA-H 0.000 description 1
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Images
Classifications
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Abstract
Description
-広い電気化学的ウィンドウ(electrochemical window)を有するため、正電極での酸化的な電解質の分解が起こらない。
-負電極に安定した最上層(top layer)を形成し、それによって最上層の容量が低くなり、さらなる動作中に負電極でさらなる還元性電解質の分解が起こらない。
-広い電気化学的ウィンドウのため、高電圧のカソードを有する再充電可能なバッテリーセルの動作が可能になる。
-導電性塩類の溶解度が高く、イオン伝導性と電子絶縁性に優れているため、イオン輸送を促進し、自己放電を最小限に抑える。
-セパレータ、電極材料、セルパック材料など、再充電可能なバッテリーセルの他の構成要素に対しても不活性である。
-様々な誤使用(電気的、機械的、熱的誤使用など)に対して耐性がある。
-再充電可能なバッテリーセルのセル構成要素に含まれる残留水分量に対する安定性が向上している。
-電気的性能が向上し、特にエネルギー密度レベルが高い。
-過充電や過剰放電能が改善される。
-自己放電が少ない。
-耐用年数の向上、特に使用可能な充放電サイクル数の増加を示す。
-総重量の減少。
-より厳しい車内環境下でも操作上の安全性が向上する。
-製造コストの削減。
-好ましくはC2-C4アルキルの、特に好ましくはアルキル基2-プロピル、メチルおよびエチルの、C1-C6アルキル;
-好ましくはC2-C4アルケニルの、特に好ましくはアルケニル基エテニルおよびプロペニルの、C2-C6アルケニル;
-好ましくはC2-C4アルキニルの、C2-C6アルキニル;
-C3-C6シクロアルキル;
-フェニル;および
-C5-C7ヘテロアリール
からなる群から選択されることが提供される。
(i)5~99.4重量%の二酸化硫黄、
(ii)0.6~95重量%の第1導電性塩、
(iii)0~25重量%の第2導電性塩、および
(iv)0~10重量%の添加剤
以下では、活性金属に関する本発明による再充電可能なバッテリーセルの有利なさらなる実施形態を説明する。
-アルカリ金属、特にリチウムまたはナトリウム;
-アルカリ土類金属、特にカルシウム;
-元素周期表の第12族の金属、特に亜鉛;または
-アルミニウム
である。
以下では、本発明による再充電可能なバッテリーセルの、負電極に関する有利なさらなる実施形態を説明する。
以下では、本発明による再充電可能なバッテリーセルの有利なさらなる実施形態について、正電極に関して説明する。
-M’は、Ti、V、Cr、Mn、Fe、Co、Ni、CuおよびZnの元素からなる群から選択される少なくとも1種の金属である;
-M”は、元素周期表の第2族、第3族、第4族、第5族、第6族、第7族、第8族、第9族、第10族、第11族、第12族、第13族、第14族、第15族および第16族の元素からなる群から選択される少なくとも1種の元素である;
-xおよびyは、0より大きい;
-zは、0以上である;そして
-aは、0より大きい。
本発明による再充電可能なバッテリーセルの有利なさらなる実施形態は、その設計に関して以下に説明される。
後述する実施例で使用する参照電解質は、欧州特許第2954588号明細書に記載されている手順で調製した。まず、塩化リチウム(LiCl)を120℃で3日間、真空下で乾燥させた。また、アルミニウム粒子(Al)を450℃で2日間、真空下で乾燥させた。LiCl、塩化アルミニウム(AlCl3)、およびAlを、AlCl3:LiCl:Alのモル比が1:1.06:0.35となるように、ガス抜き用の開口部を有するガラス瓶に入れて混合した。次いで、この混合物を段階的に熱処理して溶融塩を生成した。冷却後、形成された塩の溶融物をろ過し、次に室温まで冷却した。最後に、LiAlCl4に対するSO2の所望のモル比が形成されるまで、SO2を加えた。このようにして形成された参照電解質は、LiAlCl4 *xSO2という組成を有し、ここでxは加えられたSO2の量に依存する。
以下に説明する実験のために、本発明による電解質の3つの実施形態例1,2および3を調製した(以下、電解質1,2および3と称する)。この目的のために、まず、以下の文献に記載されている製造プロセスの式(I)による第1の3種類の異なる導電性塩を調製した。
“I.Krossing,Chem.Eur.J.2001,7,490;
S.M.Ivanova et al, Chem.Eur.J.2001,7,503;
Tsujioka et al, J.Electrochem.Soc.,2004,151,A1418”
1)ライザーパイプ付きの圧力ピストンにおけるそれぞれの化合物1,2および3を供給、
2)圧力ピストンの排気、
3)液体SO2の流入、および
4)目標量のSO2が添加されるまで、ステップ2+3を繰り返す。
後述する実験で用いたフルセルは、セパレータで隔てられた2つの負電極と1つの正電極を有する再充電可能なバッテリーセルである。正電極は、活物質としてのLiFePO4、導電性媒介剤、バインダーを含んでいた。負電極は、活物質としてグラファイトおよびバインダーを含んでいた。各フルセルには、実験に必要な電解質、すなわち参照電解質、または電解質1,2もしくは3の何れかが充填された。
本発明による電解質がフルセルのサイクル挙動に悪影響を及ぼさないかどうかをテストするために、まず、参照電解質中に化合物1または化合物3のいずれかを少量ずつ含む混合電解質を調製した。
実施例1で調製した参照電解質と、実施例2で調製した電解質1,2または3を用いて、実施例3によるフルセルで実験を行った。参照電解質および電解質1,2および3は、それぞれ導電塩の濃度が0.6mol/lであった。4つのフルセルに電解質を充填した。3.6Vの電位になるまで50mAで充電し、電流が40mAに低下するまで3.6Vの電位を維持した。
電解質1,2および3の高電圧能力を実証するために、実施例3によるフルセルでの実験を行った。フルセルには、電解質1リットルに基づき第1導電性塩として化合物1を1mol/lの濃度で含有している、実施例2に記載した電解質1を充填させた。
充電の上限電位を3.6ボルトから5.0ボルトまで0.2ボルト刻みで増加させた点が異なるが、充電/放電実験3を繰り返した。これは、8サイクル実行されたことを意味する。表2に、それぞれのケースで達成されたサイクル効率を示す。
本発明による電解質3を、サイクル実験において、参照電解質と比較した。この目的のために、実施例3に記載した3つのフルセルを使用した。それぞれ1つのフルセルに参照電解質を充填し、2つのフルセルに電解質3を充填した。フルセルは、3.6ボルトの電位まで充電され、2.5ボルトまで放電された。参照電解質を充填したフルセルは100mAの電流で動作させ、より低い導電率に適合させた電解質3を充填した2つのフルセルは、それぞれ10mAと5mAで1回充電または放電させた。図9は、得られた充電/放電曲線を示す。すべてのフルセルで、安定した充電と安定した放電が行われていることがわかる。低電流では、電解質3の到達可能容量が増加する。
この実験では、先行技術の参照電解質に代わるものとして、本発明による電解質の使用を検討した。
化合物1の濃度を変えて電解質1を調製することにより導電率を測定した。化合物1の濃度ごとに、導電率測定法を用いて電解質1の導電率を測定した。温度調整後、2電極センサーを溶液に接触させ、0~50mS/cmの範囲で測定を行った。表4に、様々な濃度、対応するSO2含有量、および測定された導電率の値を示す。
この実験では、負電極上に最上層を形成するための第1サイクルで消費される容量を調査した。この最上層は、フルセルが初めて充電されるときに負電極上に形成される。リチウムイオンはこのコーティング形成のために不可逆的に消費されるため、フルセルがその後のサイクルに利用できるサイクル容量は少なくなる。
カバー層の容量=(Qcha(125mAh)-Qdis(×mAh))/QNEL
本発明による電解質の低温挙動を参照電解質と比較して決定するために、実験1に記載されているように、2つのフルセルに、一方は参照電解質、他方は電解質1を充填した。
Claims (24)
- 前記置換基R1,R2,R3およびR4が、独立して、
-好ましくはC2-C4アルキルの、特に好ましくはアルキル基2-プロピル、メチルおよびエチルの、C1-C6アルキル;
-好ましくはC2-C4アルケニルの、特に好ましくはアルケニル基エテニルおよびプロペニルの、C2-C6アルケニル;
-好ましくはC2-C4アルキニルの、C2-C6アルキニル;
-C3-C6シクロアルキル;
-フェニル;および
-C5-C7ヘテロアリール
からなる群から選択される、請求項1に記載の電解質。 - 前記置換基R1,R2,R3およびR4のうちの少なくとも1つが、少なくとも1つのフッ素原子および/または少なくとも1つの化学基によって置換されており、前記化学基が、C1~C4アルキル、C2~C4アルケニル、C2~C4アルキニル、フェニルおよびベンジルからなる群から選択される、請求項1または2に記載の電解質。
- 前記置換基R1,R2,R3およびR4のうち少なくとも1つが、CF3基またはOSO2CF3基である、請求項1~3の何れか1項に記載の電解質。
- 式(I)による第1導電性塩とは異なる少なくとも1つの第2導電性塩を含む、請求項1~5の何れか1項に記載の電解質。
- 前記第2導電性塩が、アルミン酸塩、ハロゲン化物、シュウ酸塩、ホウ酸塩、リン酸塩、ヒ酸塩および没食子酸塩からなる群から選択される、アルカリ金属化合物、特にリチウム化合物である、請求項6に記載の電解質。
- 前記第2導電性塩が、テトラハロゲンアルミン酸リチウム、特にテトラクロロアルミン酸リチウムである、請求項6または7に記載の電解質。
- 少なくとも1つの添加剤を含む、請求項1~8の何れか1項に記載の電解質。
- 前記添加剤が、ビニレンカーボネートおよびその誘導体、ビニルエチレンカーボネートおよびその誘導体、メチルエチレンカーボネートおよびその誘導体、(ビスオキサラト)ホウ酸リチウム、ジフルオロ(オキサラト)ホウ酸リチウム、テトラフルオロ(オキサラト)リン酸リチウム、シュウ酸リチウム、2-ビニルピリジン、4-ビニルピリジン、環状のエキソメチレンカーボネート類、スルトン類、環状および非環状のスルホン酸塩類、非環状の亜硫酸塩類、環状および非環状のスルフィン酸塩類、有機エステル類、無機酸類、1バールで少なくとも36℃の沸点を有する非環状および環状のアルカン類、芳香族化合物類、ハロゲン化された環状および非環状スルホニルイミド類、ハロゲン化された環状および非環状リン酸エステル類、ハロゲン化された環状および非環状ホスフィン類、ハロゲン化された環状および非環状ホスファイト類、ハロゲン化された環状および非環状のホスファゼン類、ハロゲン化された環状および非環状のシリルアミン類、ハロゲン化された環状および非環状のハロゲン化エステル類、ハロゲン化された環状および非環状のアミド類、ハロゲン化された環状および非環状の無水物類、ならびにハロゲン化された有機複素環類からなる群から選択される、請求項9に記載の電解質。
- 前記電解質組成物の総重量に基づいて、
(i)5~99.4重量%の二酸化硫黄、
(ii)0.6~95重量%の第1導電性塩、
(iii)0~25重量%の第2導電性塩、および
(iv)0~10重量%の添加剤
の組成を有する、請求項1~10の何れか1項に記載の電解質。 - 前記第1導電性塩のモル濃度が、前記電解質の全体積を基準にして、0.05mol/l~10mol/l、好ましくは0.1mol/l~6mol/l、特に好ましくは0.2mol/l~3.5mol/lの範囲内である、請求項1~11の何れか1項に記載の電解質。
- 導電性塩1molあたり、少なくとも0.1molのSO2、好ましくは少なくとも1molのSO2、より好ましくは少なくとも5molのSO2、より好ましくは少なくとも10molのSO2、特に好ましくは少なくとも20molのSO2を含む、請求項1~12の何れか1項に記載の電解質。
- 請求項1~13の少なくとも1項に記載の電解質と、活性金属と、少なくとも1つの正電極(4)と、少なくとも1つの負電極(5)と、ハウジング(1)とを備える、再充電可能なバッテリーセル(2)。
- 前記活性金属が、
-アルカリ金属、特にリチウムまたはナトリウム;
-アルカリ土類金属、特にカルシウム;
-元素周期表の第12族の金属、特に亜鉛;または
-アルミニウム
である、請求項14に記載の再充電可能なバッテリーセル(2)。 - 前記負電極(5)が、好ましくは活物質としてのカーボン、特にグラファイト変形物を含む挿入電極である、請求項14または15に記載の再充電可能なバッテリーセル(2)。
- 前記正電極(4)が、活物質として少なくとも1つのインターカレーション化合物を含み、前記インターカレーション化合物が、好ましくは、組成LixM’yM”zOaを有し、式中、
-M’は、Ti、V、Cr、Mn、Fe、Co、Ni、CuおよびZnの元素からなる群から選択される少なくとも1種の金属であり、
-M”は、元素周期表の第2族、第3族、第4族、第5族、第6族、第7族、第8族、第9族、第10族、第11族、第12族、第13族、第14族、第15族および第16族の元素からなる群から選択される少なくとも1種の元素であり、
-xおよびyは、0より大きく、
-zは、0以上であり、そして
-aは、0より大きい、
請求項14~16の何れか1項に記載の再充電可能なバッテリーセル(2)。 - 前記インターカレーション化合物が、LixM’yM”zOaの組成を有し、式中、M’は鉄であり、M”はリンであり、好ましくはx、yおよびzは1に等しく、aは4に等しい、請求項17に記載の再充電可能なバッテリーセル(2)。
- 前記インターカレーション化合物が、LixM’yM”zOaの組成を有し、式中、M’はマンガンであり、M”はコバルトであり、好ましくはx、yおよびzは1に等しく、aは4に等しい、請求項17または18に記載の再充電可能なバッテリーセル(2)。
- 前記インターカレーション化合物が、LixM’yM”zOaの組成を有し、式中、M’はニッケルおよびマンガンを含み、M”はコバルトである、請求項17または18に記載の再充電可能なバッテリーセル(2)。
- 前記正電極(4)が、金属酸化物、金属ハロゲン化物および金属リン酸塩からなる群から選択される少なくとも1つの金属化合物を含み、前記金属化合物の金属が、好ましくは、元素の周期表の原子番号が22から28の遷移金属、特にコバルト、ニッケル、マンガンまたは鉄である、請求項14~20の何れか1項に記載の再充電可能なバッテリーセル(2)。
- 正電極(4)および/または負電極(5)が、好ましくは、
-金属板または金属箔の形態において、平面的な形状、または
-特に発泡金属(18)の形態における、多孔質金属構造の形態における三次元的な形状である
導電性素子(34、35)を備える、請求項14~21の何れか1項に記載の再充電可能なバッテリーセル(2)。 - 正電極(4)および/または負電極(5)が、少なくとも1つのバインダー、好ましくはフッ素系バインダー、特にポリフッ化ビニリデン、ならびに/またはテトラフルオロエチレン、ヘキサフルオロプロピレンおよびフッ化ビニリデンのターポリマー、または
共役カルボン酸のモノマー構造単位、または前記共役カルボン酸のアルカリ金属、アルカリ土類金属、アンモニウム塩、またはこれらの組み合わせから構成されるポリマーからなるバインダー、または
モノマースチレンおよびブタジエン構造単位をベースとするポリマーからなるバインダー、またはカルボキシメチルセルロースの群からのバインダー、を含み、
ここで、前記バインダーが、前記正電極の総重量に基づいて、好ましくは最大で20重量%、より好ましくは最大で15重量%、より好ましくは最大で10重量%、より好ましくは最大で7重量%、より好ましくは最大で5重量%、特に好ましくは最大で2重量%の濃度で存在する、請求項14~22の何れか1項に記載の再充電可能なバッテリーセル(2)。 - ハウジング(1)内に交互に配置された複数の負電極(5)および複数の正電極(4)を備え、前記正電極(4)および前記負電極(5)が、好ましくは、セパレータ(11)によって互いに電気的に分離されている、請求項14~23の何れか1項に記載の再充電可能なバッテリーセル(2)。
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