JP2021177463A - 非水電解質蓄電素子及びその製造方法 - Google Patents
非水電解質蓄電素子及びその製造方法 Download PDFInfo
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- JP2021177463A JP2021177463A JP2020082276A JP2020082276A JP2021177463A JP 2021177463 A JP2021177463 A JP 2021177463A JP 2020082276 A JP2020082276 A JP 2020082276A JP 2020082276 A JP2020082276 A JP 2020082276A JP 2021177463 A JP2021177463 A JP 2021177463A
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- positive electrode
- aqueous electrolyte
- active material
- sulfur
- electrode active
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- 239000011255 nonaqueous electrolyte Substances 0.000 title claims abstract description 120
- 238000003860 storage Methods 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 69
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000000654 additive Substances 0.000 claims abstract description 67
- 239000011593 sulfur Substances 0.000 claims abstract description 67
- 230000000996 additive effect Effects 0.000 claims abstract description 54
- 239000007774 positive electrode material Substances 0.000 claims abstract description 51
- 150000001875 compounds Chemical class 0.000 claims abstract description 44
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 229910052796 boron Inorganic materials 0.000 claims abstract description 28
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims description 23
- 150000001923 cyclic compounds Chemical class 0.000 claims description 21
- 150000008053 sultones Chemical group 0.000 claims description 9
- 239000011149 active material Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 abstract description 21
- -1 organic disulfide compounds Chemical class 0.000 description 65
- 239000000463 material Substances 0.000 description 48
- 239000010410 layer Substances 0.000 description 41
- 239000007773 negative electrode material Substances 0.000 description 31
- 239000002585 base Substances 0.000 description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 23
- 229910052744 lithium Inorganic materials 0.000 description 21
- 239000006258 conductive agent Substances 0.000 description 14
- 229910052783 alkali metal Inorganic materials 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 13
- 239000003575 carbonaceous material Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- 150000001340 alkali metals Chemical class 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000003125 aqueous solvent Substances 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 9
- 229910003002 lithium salt Inorganic materials 0.000 description 9
- 159000000002 lithium salts Chemical class 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 238000007599 discharging Methods 0.000 description 8
- 238000003682 fluorination reaction Methods 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 239000002562 thickening agent Substances 0.000 description 8
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 7
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- 125000004432 carbon atom Chemical group C* 0.000 description 6
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- 230000000052 comparative effect Effects 0.000 description 6
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 6
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 6
- 239000007784 solid electrolyte Substances 0.000 description 6
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- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 125000001153 fluoro group Chemical group F* 0.000 description 4
- 150000002484 inorganic compounds Chemical class 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 125000004206 2,2,2-trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 description 3
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
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- 239000006230 acetylene black Substances 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 150000001733 carboxylic acid esters Chemical class 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 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 description 3
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 3
- JLEXUIVKURIPFI-UHFFFAOYSA-N tris phosphate Chemical compound OP(O)(O)=O.OCC(N)(CO)CO JLEXUIVKURIPFI-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- ZPFAVCIQZKRBGF-UHFFFAOYSA-N 1,3,2-dioxathiolane 2,2-dioxide Chemical compound O=S1(=O)OCCO1 ZPFAVCIQZKRBGF-UHFFFAOYSA-N 0.000 description 2
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 2
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 2
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
- WQADWIOXOXRPLN-UHFFFAOYSA-N 1,3-dithiane Chemical compound C1CSCSC1 WQADWIOXOXRPLN-UHFFFAOYSA-N 0.000 description 2
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- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
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- 229920002943 EPDM rubber Polymers 0.000 description 2
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- 241000156302 Porcine hemagglutinating encephalomyelitis virus Species 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
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- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 2
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- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
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- 239000006229 carbon black Substances 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 2
- TXCDCPKCNAJMEE-UHFFFAOYSA-N dibenzofuran Chemical compound C1=CC=C2C3=CC=CC=C3OC2=C1 TXCDCPKCNAJMEE-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
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- 239000002612 dispersion medium Substances 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
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- 229910052748 manganese Inorganic materials 0.000 description 2
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- NDZWKTKXYOWZML-UHFFFAOYSA-N trilithium;difluoro oxalate;borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-].FOC(=O)C(=O)OF NDZWKTKXYOWZML-UHFFFAOYSA-N 0.000 description 2
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- 238000004804 winding Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
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- VSKCGJBMHRNFCZ-UHFFFAOYSA-N (2,2-dioxo-1,3,2-dioxathiolan-4-yl)methyl methanesulfonate Chemical compound CS(=O)(=O)OCC1COS(=O)(=O)O1 VSKCGJBMHRNFCZ-UHFFFAOYSA-N 0.000 description 1
- BODYVHJTUHHINQ-UHFFFAOYSA-N (4-boronophenyl)boronic acid Chemical compound OB(O)C1=CC=C(B(O)O)C=C1 BODYVHJTUHHINQ-UHFFFAOYSA-N 0.000 description 1
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Images
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Abstract
Description
本発明の一実施形態に係る非水電解質蓄電素子は、正極、負極及び非水電解質を有する。以下、非水電解質蓄電素子の一例として、非水電解質二次電池(以下、単に「二次電池」ともいう。)について説明する。上記正極及び負極は、通常、セパレータを介して積層又は巻回により交互に重畳された電極体を形成する。この電極体は容器に収納され、この容器内に非水電解質が充填される。上記非水電解質は、正極と負極との間に介在する。また、上記容器としては、二次電池の容器として通常用いられる公知の金属容器、樹脂容器等を用いることができる。
正極は、正極基材、及びこの正極基材に直接又は中間層を介して配される正極活物質層を有する。
上記負極は、負極基材、及びこの負極基材に直接又は中間層を介して配される負極活物質層を有する。上記中間層は正極の中間層と同様の構成とすることができる。
セパレータは、公知のセパレータの中から適宜選択できる。セパレータとして、例えば、基材層のみからなるセパレータ、基材層の一方の面又は双方の面に耐熱粒子とバインダーとを含む耐熱層が形成されたセパレータ等を使用することができる。セパレータの基材層の材質としては、例えば、織布、不織布、多孔質樹脂フィルム等が挙げられる。これらの材質の中でも、強度の観点から多孔質樹脂フィルムが好ましく、非水電解質の保液性の観点から不織布が好ましい。セパレータの基材層の材料としては、シャットダウン機能の観点から例えばポリエチレン、ポリプロピレン等のポリオレフィンが好ましく、耐酸化分解性の観点から例えばポリイミドやアラミド等が好ましい。セパレータの基材層として、これらの樹脂を複合した材料を用いてもよい。
非水電解質は、フッ素化溶媒及び添加剤を含む。上記添加剤は、硫黄を含む環状化合物及びホウ素を含む化合物の少なくとも一方である。非水電解質は、通常、上記フッ素化溶媒を含む非水溶媒と、この非水溶媒に溶解されている電解質塩及び上記添加剤とを含む非水電解液である。上記添加剤が塩である場合、上記添加剤とは別にさらに電解質塩が含有されていてもよく、含有されていなくてもよい。
LiN(SO2F)2(リチウムビス(フルオロスルホニル)イミド:LiFSI)、LiN(SO2CF3)2(リチウムビス(トリフルオロメタンスルホニル)イミド:LiTFSI)、LiN(SO2C2F5)2(リチウムビス(ペンタフルオロエタンスルホニル)イミド:LiBETI)、LiN(SO2C4F9)2(リチウムビス(ノナフルオロブタンスルホニル)イミド)、CF3−SO2−N−SO2−N−SO2CF3Li2、FSO2−N−SO2−C4F9Li、CF3−SO2−N−SO2−CF2−SO2−N−SO2−CF3Li2、CF3−SO2−N−SO2−CF2−SO3Li2、CF3−SO2−N−SO2−CF2−SO2−C(−SO2CF3)2Li2等のリチウムスルホニルイミド塩;
LiN(POF2)2(リチウムビス(ジフルオロホスホニル)イミド:LiDFPI)等のリチウムホスホニルイミド塩等を挙げることができる。
本実施形態の非水電解質蓄電素子は、電気自動車(EV)、ハイブリッド自動車(HEV)、プラグインハイブリッド自動車(PHEV)等の自動車用電源、パーソナルコンピュータ、通信端末等の電子機器用電源、又は電力貯蔵用電源等に、複数の非水電解質蓄電素子1を集合して構成した蓄電ユニット(バッテリーモジュール)として搭載することができる。この場合、蓄電ユニットに含まれる少なくとも一つの非水電解質蓄電素子に対して、本発明の一実施形態に係る技術が適用されていればよい。
本発明の一実施形態に係る非水電解質蓄電素子の製造方法は、正極活物質を含む正極を準備することと、フッ素化溶媒及び添加剤を含む非水電解質を準備することとを備え、上記正極活物質が、硫黄を含み、上記添加剤が、硫黄を含む環状化合物及びホウ素を含む化合物の少なくとも一方である。
本発明は、上記実施形態に限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々変更を加えてもよい。例えば、ある実施形態の構成に他の実施形態の構成を追加することができ、また、ある実施形態の構成の一部を他の実施形態の構成又は周知技術に置き換えることができる。さらに、ある実施形態の構成の一部を削除することができる。また、ある実施形態の構成に対して周知技術を付加することができる。
添加剤A:ビス(オキサラト)ホウ酸リチウム(LiBOB)
添加剤B:ジフルオロ(オキサラト)ホウ酸リチウム(LiDFOB)
添加剤C:テトラフルオロホウ酸リチウム(LiBF4)
添加剤D:(3−メチル−2,4−ペンタンジオナト)(オキサラト)ボレート(MOAB)
添加剤E:1,3−プロペンスルトン(PRS)
添加剤F:メチレンメタンジスルホン酸エステル(MMDS)
添加剤a:ビニレンカーボネート(VC)
添加剤b:ジフルオロリン酸リチウム(LiDFP)
添加剤c:リン酸トリス(2,2,2−トリフルオロエチル)(TFEP)
(非水電解質の調製)
フルオロエチレンカーボネート(FEC)と2,2,2−トリフルオロエチルメチルカーボネート(TFEMC)との混合溶媒(体積比50:50)にリチウムビス(トリフルオロメタンスルホニル)イミド(LiTFSI)を1.0mol/dm3の濃度で溶解させた。この溶液に添加剤として1質量%の濃度で添加剤A(ビス(オキサラト)ホウ酸リチウム(LiBOB))を添加し、非水電解質を調製した。
硫黄と、多孔質カーボン(CNovel(クノーベル))(東洋炭素株式会社製)とを質量比72:28で混合した。この混合物を、密封式の電気炉に入れた。1時間のアルゴンフローを行った後、昇温速度5℃/分で150℃まで昇温し、5時間保持した後、硫黄が固化する温度である80℃まで放冷し、その後、再び5℃/分で300℃まで昇温し、2時間保持する熱処理を行い、硫黄−多孔質カーボン複合体(SPC)を作製した。なお、本実施例の多孔質カーボンには、平均細孔径5nm、細孔体積1.7mLg−1、比表面積1500m2g−1のものを用いた。
負極として、シート状の金属リチウムを用意した。セパレータとして、ポリエチレン製微多孔膜を用意した。上記正極、負極、セパレータ及び非水電解質を用いて、実施例1の非水電解質蓄電素子としての二次電池を得た。
添加剤Aに替えて表1に記載の各添加剤を添加した又は添加剤を添加しなかったこと以外は、実施例1と同様にして、実施例2から6及び比較例1から4の各二次電池を得た。なお、表1中、「−」は添加剤を添加していないことを示す。
(充放電サイクル試験)
得られた各二次電池について、25℃で1Vまで0.1Cの定電流放電を行った。放電後に25℃で3Vまで0.2Cの定電流充電を行った。これら放電及び充電の工程を1サイクルとして、このサイクルを80サイクル繰り返した。なお、放電後及び充電後には25℃にて10分間の休止を設けた。放電、充電及び休止ともに25℃の恒温槽内でおこなった。
1サイクル目の放電電気量、80サイクル目の放電電気量、及び容量維持率として1サイクル目の放電電気量に対する80サイクル目の放電電気量の比を表1に示す。
2 電極体
3 容器
4 正極端子
41 正極リード
5 負極端子
51 負極リード
20 蓄電ユニット
30 蓄電装置
Claims (4)
- 正極活物質を含む正極と、
フッ素化溶媒及び添加剤を含む非水電解質と
を備え、
上記正極活物質が、硫黄を含み、
上記添加剤が、硫黄を含む環状化合物及びホウ素を含む化合物の少なくとも一方である非水電解質蓄電素子。 - 上記添加剤が上記ホウ素を含む化合物であり、
上記ホウ素を含む化合物が塩である請求項1に記載の非水電解質蓄電素子。 - 上記添加剤が上記硫黄を含む環状化合物であり、
上記硫黄を含む環状化合物がスルトン類である請求項1に記載の非水電解質蓄電素子。 - 正極活物質を含む正極を準備することと、
フッ素化溶媒及び添加剤を含む非水電解質を準備することと
を備え、
上記正極活物質が、硫黄を含み、
上記添加剤が、硫黄を含む環状化合物及びホウ素を含む化合物の少なくとも一方である非水電解質蓄電素子の製造方法。
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WO2023090445A1 (ja) * | 2021-11-22 | 2023-05-25 | 学校法人 関西大学 | 非水電解質蓄電素子、機器及び非水電解質蓄電素子の製造方法 |
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