JP6784753B2 - 犠牲塩を含む正極を備えたリチウムイオン電池のセルを形成するための方法 - Google Patents
犠牲塩を含む正極を備えたリチウムイオン電池のセルを形成するための方法 Download PDFInfo
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- JP6784753B2 JP6784753B2 JP2018511149A JP2018511149A JP6784753B2 JP 6784753 B2 JP6784753 B2 JP 6784753B2 JP 2018511149 A JP2018511149 A JP 2018511149A JP 2018511149 A JP2018511149 A JP 2018511149A JP 6784753 B2 JP6784753 B2 JP 6784753B2
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- cell
- positive electrode
- lithium
- electrode material
- electrolyte
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- 229910001416 lithium ion Inorganic materials 0.000 title claims description 37
- 238000000034 method Methods 0.000 title claims description 34
- 150000003839 salts Chemical class 0.000 title claims description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000007774 positive electrode material Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 239000011149 active material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- -1 LiCH 3 SO 3 Inorganic materials 0.000 claims description 7
- 239000007773 negative electrode material Substances 0.000 claims description 7
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 229910003002 lithium salt Inorganic materials 0.000 claims description 6
- 159000000002 lithium salts Chemical class 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 4
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 claims description 3
- 229910002099 LiNi0.5Mn1.5O4 Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229910015015 LiAsF 6 Inorganic materials 0.000 claims description 2
- 229910013063 LiBF 4 Inorganic materials 0.000 claims description 2
- 229910013684 LiClO 4 Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 claims description 2
- ACFSQHQYDZIPRL-UHFFFAOYSA-N lithium;bis(1,1,2,2,2-pentafluoroethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)C(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)C(F)(F)F ACFSQHQYDZIPRL-UHFFFAOYSA-N 0.000 claims description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical group [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 2
- MCVFFRWZNYZUIJ-UHFFFAOYSA-M lithium;trifluoromethanesulfonate Chemical compound [Li+].[O-]S(=O)(=O)C(F)(F)F MCVFFRWZNYZUIJ-UHFFFAOYSA-M 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000010450 olivine Substances 0.000 claims description 2
- 229910052609 olivine Inorganic materials 0.000 claims description 2
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 claims 1
- 230000008859 change Effects 0.000 description 16
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000006870 function Effects 0.000 description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000002427 irreversible effect Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 239000012982 microporous membrane Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101100181929 Caenorhabditis elegans lin-3 gene Proteins 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005344 Li(Fe,Mn,Ni)PO4 Inorganic materials 0.000 description 1
- 229910013188 LiBOB Inorganic materials 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229920005740 STYROFAN® Polymers 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical class CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002388 carbon-based active material Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000012733 comparative method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- OGGXGZAMXPVRFZ-UHFFFAOYSA-N dimethylarsinic acid Chemical compound C[As](C)(O)=O OGGXGZAMXPVRFZ-UHFFFAOYSA-N 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- RBYFNZOIUUXJQD-UHFFFAOYSA-J tetralithium oxalate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O RBYFNZOIUUXJQD-UHFFFAOYSA-J 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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Description
(a)セルを30〜45℃の範囲内の温度T1まで加熱するステップと、
(b)セルを、4.8V以下、好ましくは、4.6〜4.8V、より好ましくは、4.7〜4.8Vの電位まで充電するステップ。
tP=(1−Dr/Dth)*100(I).
− オリビン構造のリン酸塩LivTaPO4であって、0≦v≦1であり、TaはFe、Ni、Co、Mnおよびこれらの混合物から選択される、リン酸塩、
− 式Li1+u(MaDb)1−uO2の物質であって、0.01≦u≦0.33であり、Mは、Ni、Mn、Coおよびこれらの混合物から選択され、Dは、Na、Zn、Cd、Mg、Ti、Ca、Zr、Sr、Ba、AlおよびKから選択される1つまたは複数のドーピング金属を表し、0≦b≦0.05およびa+b=1である、物質、ならびに
− LiMn2O4およびLiNi0.5Mn1.5O4から選択されるスピネル構造の物質、
から選択される活物質を含み、
より好ましくは、オリビン構造のリン酸塩、さらにより好ましくは、LiFePO4を含む。
(a)セルを40℃の温度T1まで加熱するステップと、
(b)セルを、4.7〜4.8V、好ましくは、4.8Vの電位まで充電するステップ。
1. シュウ酸リチウムを含む正極を含むリチウムイオン電池セルの調製
1.1 正極の調製
式LiFePO4の活物質が用いられる。正極は、85wt%の活物質、5wt%のSuper P(登録商標)炭素添加剤、5wt%の、N−メチル−2−ピロリドン(NMP)中のポリフッ化ビニリデン、および5wt%のシュウ酸リチウムLi2C2O4を混合することによって調製される。
ケイ素/黒鉛複合物(日立化成)に基づく負極が調製された。負極は、94wt%の活物質、2wt%のカルボキシメチルセルロース(CMC)、およびカルボキシル化スチレンブタジエンコポリマーである、4wt%のスチロファン(Styrofan)(登録商標)ラテックスを混合することによって調製される。
充電/放電サイクルの間における正極と負極との間のあらゆる短絡を防止するために、Celgard(登録商標)2325セパレータが用いられる。Celgard(登録商標)2325セパレータは、ポリプロピレンからなる25μmの厚さを有する単層微多孔膜である。
用いられる電解質は、体積で1/1/1の割合の炭酸エチレン、炭酸ジメチル、ならびに炭酸エチルおよびメチルの混合物中に溶解させられた1Mのリチウム塩LiPF6からなる。
10cm2の面積を有する正極、および上述されたとおりの負極を、上述されたとおり、セパレータを電極間に配置して積層することによって、リチウムイオン電池セルが組み立てられ、次に、上述されたように、セルに電解質が含浸させられる。
2.1 時間の関数としてのLiイオン電池セルの電位の変化の評価
方法
方法A、方法B、および方法Cとそれぞれ呼ばれる、3つの特定の形成方法が、以上において調製されたとおりのLiイオン電池セルに適用された。
図1において、曲線A、BおよびCはセルA、BおよびC電位の変化にそれぞれ対応する。
方法
本方法は、段落2.1において与えられたものと同一である。
図2において、曲線A1はセルAの放電容量の変化に対応し、曲線A2はセルAの内部抵抗の変化に対応する。曲線B1はセルBの放電容量の変化に対応し、曲線B2はセルBの内部抵抗の変化に対応する。曲線C1はセルCの放電容量の変化に対応し、曲線C2はセルCの内部抵抗の変化に対応する。
方法
3つの異なるカレンダー加工レベルによって得られた、47%、35%および42%の3つの異なる多孔性レベルをそれぞれ有する正極を各々が含んでいる、セルD、セルEおよびセルFと呼ばれる、3つのLiイオン電池セルに、本発明に係る形成方法Bが適用された。
図3において、曲線D1はセルDの放電容量の変化に対応し、曲線D2はセルDの抵抗の変化に対応する。曲線E1はセルEの放電容量の変化に対応し、曲線E2はセルEの抵抗の変化に対応する。曲線F1はセルFの放電容量の変化に対応し、曲線F2はセルFの抵抗の変化に対応する。
Claims (9)
- 20〜35%の範囲内の多孔性レベルを有し、少なくとも1つの犠牲塩を含む正極物質、負極物質、セパレータ、および電解質を含むリチウムイオン電池セルを形成するための方法であって、前記方法が、以下の(a)、(b)の順番で行われる逐次的ステップ:
(a)前記セルを30〜45℃の範囲内の温度T1まで加熱するステップと、
(b)前記セルを、充電する最初のサイクルの間に犠牲塩が酸化する電位以上であり、4.8V以下の電位まで充電するステップと、
を含み、犠牲塩が酸化時にLi+イオンを生成し、Li+イオンが電解質内へ貫入すること、ならびに、
前記正極物質が、
− オリビン構造のリン酸塩Li v T a PO 4 であって、0≦v≦1であり、T a は、Fe、Ni、Co、Mn、およびこれらの混合物から選択される、リン酸塩、
− 式Li 1+u (M a D b ) 1−u O 2 の物質であって、0.01≦u≦0.33であり、Mは、Ni、Mn、Co、およびこれらの混合物から選択され、Dは、Na、Zn、Cd、Mg、Ti、Ca、Zr、Sr、Ba、Al、およびKから選択される1つまたは複数のドーピング金属を表し、0≦b≦0.05およびa+b=1である、物質、ならびに
− LiMn 2 O 4 およびLiNi 0.5 Mn 1.5 O 4 から選択されるスピネル構造の物質、
から選択される活物質を含むこと
を特徴とする、方法。 - 前記犠牲塩が、Li2C2O4、LiN3、Li2C3O5、Li2C4O6、Li2C3O3、Li2C4O4、Li2C5O5、Li2C6O6、Li2N4O2、および[Li2N2C2O2]n(nは1〜100)から選択される、請求項1に記載の方法。
- 前記正極物質が、前記正極物質の総重量に対して、3〜10重量%の犠牲塩を含む、請求項1または2に記載の方法。
- 前記正極物質が1つまたは複数のバインダを含む、請求項1から3のいずれか一項に記載の方法。
- 前記負極物質が黒鉛に基づく、請求項1から4のいずれか一項に記載の方法。
- 前記電解質が1つまたは複数のリチウム塩を含む、請求項1から5のいずれか一項に記載の方法。
- 前記リチウム塩が、リチウムビス[(トリフルオロメチル)スルホニル]イミド(LiN(CF3SO2)2)、リチウムトリフルオロメタンスルホン酸塩(LiCF3SO3)、リチウムビス(オキサレート)ボラート(LiBOB)、リチウムビス(ペルフルオロエチルスルホニル)イミド(LiN(CF3CF2SO2)2)、LiClO4、LiAsF6、LiPF6、LiBF4、LiI、LiCH3SO3、LiB(C2O4)2、LiRFSOSRF、LiN(RFSO2)2、LiC(RFSO2)3から選択され、RFは、フッ素原子、および1〜8個の炭素原子を含むペルフルオロアルキル基から選択される基である、請求項6に記載の方法。
- 前記電解質が、炭酸エチレンと、炭酸エチルおよびメチル、炭酸ジメチル、炭酸ジエチル、ならびにこれらの混合物から選択される少なくとも1つの溶媒とを含む溶媒の混合物を含む、請求項1から7のいずれか一項に記載の方法。
- 前記温度T1が35〜45℃の範囲内にある、請求項1から8のいずれか一項に記載の方法。
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PCT/FR2016/052111 WO2017037363A1 (fr) | 2015-09-02 | 2016-08-24 | Procede de formation d'une cellule de batterie li-ion equipee d'une electrode positive comprenant un sel sacrificiel |
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