JP7117643B2 - 二次電池 - Google Patents
二次電池 Download PDFInfo
- Publication number
- JP7117643B2 JP7117643B2 JP2019515190A JP2019515190A JP7117643B2 JP 7117643 B2 JP7117643 B2 JP 7117643B2 JP 2019515190 A JP2019515190 A JP 2019515190A JP 2019515190 A JP2019515190 A JP 2019515190A JP 7117643 B2 JP7117643 B2 JP 7117643B2
- Authority
- JP
- Japan
- Prior art keywords
- positive electrode
- intermediate layer
- secondary battery
- mass
- cured product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000011347 resin Substances 0.000 claims description 72
- 239000000203 mixture Substances 0.000 claims description 61
- 239000004020 conductor Substances 0.000 claims description 32
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- -1 methacryloyl group Chemical group 0.000 claims description 25
- 229910010272 inorganic material Inorganic materials 0.000 claims description 24
- 239000011147 inorganic material Substances 0.000 claims description 24
- 239000007774 positive electrode material Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 15
- 239000003792 electrolyte Substances 0.000 claims description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 8
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 7
- 125000003277 amino group Chemical group 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 2
- RSNHXDVSISOZOB-UHFFFAOYSA-N lithium nickel Chemical compound [Li].[Ni] RSNHXDVSISOZOB-UHFFFAOYSA-N 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 20
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- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 229910003002 lithium salt Inorganic materials 0.000 description 4
- 159000000002 lithium salts Chemical group 0.000 description 4
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- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
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- 238000011088 calibration curve Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 3
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- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
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- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 2
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical compound CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 description 2
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
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- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
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- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 150000005678 chain carbonates Chemical class 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 150000005676 cyclic carbonates Chemical class 0.000 description 2
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-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
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 description 2
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- 230000020169 heat generation Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000003273 ketjen black Substances 0.000 description 2
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910001512 metal fluoride Inorganic materials 0.000 description 2
- 229940017219 methyl propionate Drugs 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
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- 239000002344 surface layer Substances 0.000 description 2
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- 239000002562 thickening agent Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
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- ARYIITVULFDIQB-UHFFFAOYSA-N (2-methyloxiran-2-yl)methyl prop-2-enoate Chemical compound C=CC(=O)OCC1(C)CO1 ARYIITVULFDIQB-UHFFFAOYSA-N 0.000 description 1
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
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- WBODDOZXDKQEFS-UHFFFAOYSA-N 1,2,3,4-tetramethyl-5-phenylbenzene Chemical group CC1=C(C)C(C)=CC(C=2C=CC=CC=2)=C1C WBODDOZXDKQEFS-UHFFFAOYSA-N 0.000 description 1
- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical compound CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 description 1
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
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- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 description 1
- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
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- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
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- ZVYGIPWYVVJFRW-UHFFFAOYSA-N 3-methylbutyl prop-2-enoate Chemical compound CC(C)CCOC(=O)C=C ZVYGIPWYVVJFRW-UHFFFAOYSA-N 0.000 description 1
- UNDXPKDBFOOQFC-UHFFFAOYSA-N 4-[2-nitro-4-(trifluoromethyl)phenyl]morpholine Chemical compound [O-][N+](=O)C1=CC(C(F)(F)F)=CC=C1N1CCOCC1 UNDXPKDBFOOQFC-UHFFFAOYSA-N 0.000 description 1
- SBUOHGKIOVRDKY-UHFFFAOYSA-N 4-methyl-1,3-dioxolane Chemical compound CC1COCO1 SBUOHGKIOVRDKY-UHFFFAOYSA-N 0.000 description 1
- BCTDCDYHRUIHSF-UHFFFAOYSA-N 5-ethenoxypentan-1-ol Chemical compound OCCCCCOC=C BCTDCDYHRUIHSF-UHFFFAOYSA-N 0.000 description 1
- NQSLZEHVGKWKAY-UHFFFAOYSA-N 6-methylheptyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C(C)=C NQSLZEHVGKWKAY-UHFFFAOYSA-N 0.000 description 1
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 description 1
- XFZOHDFQOOTHRH-UHFFFAOYSA-N 7-methyloctyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCCOC(=O)C(C)=C XFZOHDFQOOTHRH-UHFFFAOYSA-N 0.000 description 1
- CUXGDKOCSSIRKK-UHFFFAOYSA-N 7-methyloctyl prop-2-enoate Chemical compound CC(C)CCCCCCOC(=O)C=C CUXGDKOCSSIRKK-UHFFFAOYSA-N 0.000 description 1
- COCLLEMEIJQBAG-UHFFFAOYSA-N 8-methylnonyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCCCOC(=O)C(C)=C COCLLEMEIJQBAG-UHFFFAOYSA-N 0.000 description 1
- LVGFPWDANALGOY-UHFFFAOYSA-N 8-methylnonyl prop-2-enoate Chemical compound CC(C)CCCCCCCOC(=O)C=C LVGFPWDANALGOY-UHFFFAOYSA-N 0.000 description 1
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 1
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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Description
図2は、実施形態の一例である正極の断面図である。正極11は、正極集電体30と、正極合材層32と、正極集電体30と正極合材層32との間に設けられる中間層31と、を備える。
負極12は、例えば金属箔等の負極集電体と、負極集電体上に形成された負極合材層とを備える。負極集電体には、銅などの負極の電位範囲で安定な金属の箔、当該金属を表層に配置したフィルム等を用いることができる。負極合材層は、例えば、負極活物質、結着材、増粘剤等を含む。
セパレータ13には、例えば、イオン透過性及び絶縁性を有する多孔性シート等が用いられる。多孔性シートの具体例としては、微多孔薄膜、織布、不織布等が挙げられる。セパレータの材質としては、ポリエチレンやポリプロピレン等のオレフィン系樹脂、セルロースなどが好適である。セパレータ13は、セルロース繊維層及びオレフィン系樹脂等の熱可塑性樹脂繊維層を有する積層体であってもよい。また、ポリエチレン層及びポリプロピレン層を含む多層セパレータであってもよく、セパレータの表面にアラミド系樹脂、セラミック等の材料が塗布されたものを用いてもよい。
電解質は、溶媒と、溶媒に溶解した電解質塩とを含む。電解質は、液体電解質(非水電解液)に限定されず、ゲル状ポリマー等を用いた固体電解質であってもよい。溶媒には、例えばエステル類、エーテル類、アセトニトリル等のニトリル類、ジメチルホルムアミド等のアミド類、及びこれらの2種以上の混合溶媒等の非水溶媒や水を用いることができる。非水溶媒は、これら溶媒の水素の少なくとも一部をフッ素等のハロゲン原子で置換したハロゲン置換体を含有していてもよい。
[正極の作製]
酸化アルミニウム(Al2O3)を10質量部と、アセチレンブラック(AB)を50質量部と、グリシジル基含有アクリル重合体(グリシジルメタクリレートとt-ブチルアクリレートの共重合物)を40質量部とを混合し、さらにN-メチル-2-ピロリドン(NMP)を適量加えて中間層用スラリーを調製した。次に、当該スラリーを厚み15μmのアルミニウム箔からなる正極集電体の両面に塗布し、200℃で2時間加熱し、厚み5.0μmの中間層を形成した。
正極から中間層を10mg削り出し、示差走査熱量計(リガク社製、DSC8230Thermo Plus)を用い、窒素ガス雰囲気下において、25℃~200℃まで昇温速度10℃/分で測定し、得られた発熱カーブより、100℃~170℃の発熱量比を求めた。そして、予め作成しておいた、発熱量比に対する硬化度を示す検量線を用いて、上記発熱量比から硬化度を算出した。これを、中間層内の熱硬化性樹脂(グリシジル基含有アクリル重合体)の硬化物の硬化度とした。なお、検量線は、以下のようにして作成した。完全硬化した熱硬化性樹脂(硬化度100%)の100℃~170℃の発熱量比を0とする。そして、硬化する前の熱硬化性樹脂(硬化度0%)の100℃~170℃の発熱量比を測定する。そして、硬化度0%の発熱量比と、硬化度100%の発熱量比0とを結ぶ直線を検量線とする。
人造黒鉛を100質量部と、カルボキシメチルセルロース(CMC)を1質量部と、スチレン-ブタジエンゴム(SBR)を1質量部とを混合し、負極合材スラリーを調製した。次に、当該負極合材スラリーを銅箔からなる負極集電体の両面に塗布した。塗膜を乾燥させた後、圧延ローラを用いて圧延し、負極集電体の両面に負極合材層が形成された負極を作製した。
エチレンカーボネート(EC)と、メチルエチルカーボネート(EMC)と、ジメチルカーボネート(DMC)を、3:3:4の体積比で混合した。当該混合溶媒に、LiPF6を1.2mol/Lの濃度となるように溶解させて非水電解質を調製した。
上記の正極及び負極を、それぞれ所定の寸法にカットして電極タブを取り付け、セパレータを介して巻回することにより巻回型の電極体を作製した。次に、アルミラミネートフィルムに電極体を収容し、上記の非水電解質を注入し、密閉した。これを実施例1の非水電解質二次電池とした。
中間層用スラリーの調製において酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例2における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例2の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において酸化アルミニウムを添加しなかったこと、中間層用スラリーをアルミニウム箔からなる正極集電体の両面に塗布し、100℃で30分加熱したこと以外は、実施例1と同様に正極を作製した。実施例3における中間層内の熱硬化性樹脂の硬化物の硬化度は、50%であった。これを実施例3の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、ビスフェノールA型エポキシ樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例4における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例4の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、ヒドロキシ基含有アクリル樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例5における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例5の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、カルボキシル基含有アクリル樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例6における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例6の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、アミノ基含有アクリル樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例7における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例7の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、アクリロイル基含有アクリル樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例8における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例8の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、メタクリロイル基含有アクリル樹脂を熱硬化性樹脂として用いたこと、酸化アルミニウムを添加しなかったこと以外は、実施例1と同様に正極を作製した。実施例9における中間層内の熱硬化性樹脂の硬化物の硬化度は、100%であった。これを実施例9の正極として、実施例1と同様にして非水電解質二次電池を作製した。
中間層用スラリーの調製において、グリシジル基含有アクリル重合体をポリフッ化ビニリデン(PVDF)に代えたこと以外は、実施例1と同様に正極を作製した。これを比較例の正極として、実施例1と同様にして非水電解質二次電池を作製した。
各実施例及び比較例の非水電解質二次電池について、下記手順で釘刺し試験を行った。(1)25℃の環境下で、600mAの定電流で電池電圧が4.2Vになるまで充電を行い、その後定電圧で電流値が90mAになるまで充電を引き続き行った。(2)25℃の環境下で、(1)で充電した電池の側面中央部に2.7mmφの太さの丸釘の先端を接触させ、1mm/秒の速度で電池における電極体の積層方向に丸釘を突き刺し、内部短絡による電池電圧降下を検出した直後、丸釘の突き刺しを停止した。(3)丸釘によって電池が短絡を開始して1分後の電池表面温度を測定した。(4)電池温度の測定後、0.1mm/秒の速度で電池における電極体の積層方向に丸釘を0.5秒間動かし、電圧降下の有無を確認した。電圧降下があった場合には、釘と電極とが再接触していると判定し、これを、各実施例及び比較例について、10個の電池について電圧効果の有無を測定した。これにより、再接触確率を算出した。
各実施例及び比較例で用いた正極における中間層の剥離強度を、図4に示す装置を用いて測定した。図4に示す装置は、被試験体132を載せる基台131、被試験体132を固定するための接着部材133、被試験体132の一端を固定させ引き上げ台138に接続されたチャック134、基台131を水平にスライドさせるベアリング部位135、基台131のスライド時に均一に力を作用させるばね136、ばね136が接続された固定部137、ワイヤ139と滑車140を経て基台131と接続されている引き上げ台138、引き上げ台138とつかみ冶具142を接続するためのワイヤ141、つかみ冶具142に接続され引き上げ台138の荷重を検知するためのロードセル143、ロードセル143を支持する支持部144、支持部144を上下に移動させる駆動部146、つかみ冶具142の移動量を検知するリニアセンサ147、駆動部146とリニアセンサ147を内蔵する支柱145、基台131を支持する支持台148で構成され、支持台148と支柱145はベース150に固定されている。
11 正極
12 負極
13 セパレータ
14 電極体
15 ケース本体
16 封口体
17,18 絶縁板
19 正極リード
20 負極リード
21 張り出し部
22 フィルタ
22a フィルタ開口部
23 下弁体
24 絶縁部材
25 上弁体
26 キャップ
26a キャップ開口部
27 ガスケット
30 正極集電体
31 中間層
32 正極合材層
33 正極活物質粒子。
Claims (11)
- 正極と、負極と、電解質とを有する二次電池であって、
前記正極は、正極集電体と、正極活物質粒子を含む正極合材層と、前記正極集電体と前記正極合材層との間に設けられる中間層と、を備え、
前記中間層は、グリシジル基、ヒドロキシ基、カルボキシル基、アミノ基、アクリロイル基、メタクリロイル基のうち少なくともいずれか1つを有する硬化性樹脂の硬化物と、導電材と、絶縁性無機材料と、を含 み、
前記絶縁性無機材料と前記導電材との質量比(絶縁性無機材料:導電材)は、1:0.05~1:70の範囲である 、二次電池。 - 前記正極活物質粒子の一部は、前記中間層に入り込んでいる、請求項1に記載の二次電池。
- 前記硬化性樹脂は前記カルボキシル基を有する、請求項1又は2に記載の二次電池。
- 前記中間層の厚みは、0.1μm以上10μm以下である、請求項1~3のいずれか1項に記載の二次電池。
- 前記硬化性樹脂の硬化物の硬化度は、30%以上100%以下である、請求項1~4のいずれか1項に記載の二次電池。
- 前記導電材の含有量は、前記硬化物に対して1質量%以上100質量%以下である、請求項1~5のいずれか1項に記載の二次電池。
- 前記中間層は、絶縁性無機材料を含み、前記絶縁性無機材料の含有量は、前記硬化物に対して1質量%以上100質量%以下である、請求項1~5のいずれか1項に記載の二次電池。
- 前記中間層は、絶縁性無機材料を含み、前記導電材と前記絶縁性無機材料を合わせた含有量は、前記硬化物に対して25質量%以上100質量%以下である、請求項1~5のいずれか1項に記載の二次電池。
- 前記中間層は、フッ素系樹脂を含み、前記硬化性樹脂と前記フッ素系樹脂との質量比(硬化性樹脂:フッ素系樹脂)は、1:1~1:10の範囲である、請求項1~8のいずれか1項に記載の二次電池。
- 前記導電材はカーボン系粒子を含む、請求項1~9のいずれか1項に記載の二次電池。
- 前記正極活物質粒子は、リチウムニッケル複合酸化物粒子を含む、請求項1~10のいずれか1項に記載の二次電池。
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WO2018198689A1 (ja) | 2018-11-01 |
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