JP5686441B2 - ケイ素系正極活物質及びこれを含む二次電池 - Google Patents
ケイ素系正極活物質及びこれを含む二次電池 Download PDFInfo
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- JP5686441B2 JP5686441B2 JP2012172533A JP2012172533A JP5686441B2 JP 5686441 B2 JP5686441 B2 JP 5686441B2 JP 2012172533 A JP2012172533 A JP 2012172533A JP 2012172533 A JP2012172533 A JP 2012172533A JP 5686441 B2 JP5686441 B2 JP 5686441B2
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- 239000007774 positive electrode material Substances 0.000 title claims description 107
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 106
- 239000010703 silicon Substances 0.000 title claims description 106
- 229910052710 silicon Inorganic materials 0.000 title claims description 105
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 116
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 52
- 229910052799 carbon Inorganic materials 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 41
- 229910052744 lithium Inorganic materials 0.000 claims description 38
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007773 negative electrode material Substances 0.000 claims description 30
- 238000004519 manufacturing process Methods 0.000 claims description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims description 26
- 239000000377 silicon dioxide Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- 239000002798 polar solvent Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000011149 active material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 description 17
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 16
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 16
- -1 aluminum-cadmium Chemical compound 0.000 description 14
- 238000000034 method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 9
- 239000013078 crystal Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 230000001965 increasing effect Effects 0.000 description 8
- 239000004020 conductor Substances 0.000 description 7
- 229910021488 crystalline silicon dioxide Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 239000002210 silicon-based material Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 229910008065 Si-SiO Inorganic materials 0.000 description 4
- 229910006405 Si—SiO Inorganic materials 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000001939 inductive effect Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000006182 cathode active material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 229910015645 LiMn Inorganic materials 0.000 description 2
- 229910014689 LiMnO Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 239000011255 nonaqueous electrolyte Substances 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000007784 solid electrolyte Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- QDDVNKWVBSLTMB-UHFFFAOYSA-N [Cu]=O.[Li] Chemical compound [Cu]=O.[Li] QDDVNKWVBSLTMB-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- NCZAACDHEJVCBX-UHFFFAOYSA-N [Si]=O.[C] Chemical compound [Si]=O.[C] NCZAACDHEJVCBX-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000006232 furnace black Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000010220 ion permeability Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical class [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- VROAXDSNYPAOBJ-UHFFFAOYSA-N lithium;oxido(oxo)nickel Chemical compound [Li+].[O-][Ni]=O VROAXDSNYPAOBJ-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920005608 sulfonated EPDM Polymers 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000006234 thermal black Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- 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
-
- 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
- H01M4/364—Composites as mixtures
-
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Description
前記ステップで製造された混合物から前記極性溶媒を蒸発させたあと熱処理するステップとを含むケイ素系正極活物質の製造方法を提供する。
前記ステップで製造された混合物から前記極性溶媒を蒸発させたあと熱処理するステップと、
前記ステップで熱処理された混合物に炭素を被覆するステップとを含むケイ素系正極活物質の製造方法を提供する。
アルカリ系水酸化物とケイ素系物質の混合
水酸化ナトリウム50mgをエタノールに溶解して製造された水酸化ナトリウム溶液に一酸化ケイ素1gを投入して10分以上攪拌した。
80〜120℃に加熱されているアルミナボートに一酸化ケイ素と水酸化ナトリウムを混合した溶液を注入してエタノールを蒸発させた。溶媒の蒸発が完了すると、一酸化ケイ素と水酸化ナトリウムの混合物が盛られたアルミナボートを石英管ファーネス(Quartz Tube Furnace)に投入した後、アルゴンガスを流しながら800℃の温度で5分間熱処理し、石英管ファーネスを常温まで冷却させてケイ素系正極活物質を製造した。
アルミナボートに盛られているケイ素系正極活物質を回収し、蒸留水に2時間のあいだ浸漬して濾過し、ケイ素系正極活物質の表面に付着している水酸化ナトリウムを除去した(図1を参照)。
熱処理時間を10分間行ったことを除いては、前記実施例1と同一の方法でケイ素系正極活物質を製造した。
熱処理時間を30分間行ったことを除いては、前記実施例1と同一の方法でケイ素系正極活物質を製造した。
熱処理時間を60分間行ったことを除いては、前記実施例1と同一の方法でケイ素系正極活物質を製造した。
熱処理時間を120分間行ったことを除いては、前記実施例1と同一の方法でケイ素系正極活物質を製造した。
前記実施例1で製造された20gのケイ素系正極活物質を回転管状炉に投入し、アルゴンガスを0.5L/分で流したあと温度を5℃/分の速度で800℃まで昇温させた。回転管状炉を10rpm/分の速度で回転させながらアルゴンガスを1.8L/分、アセチレンガスを0.3L/分で流しながら5時間のあいだ熱処理し、導電性炭素被覆層が形成されたケイ素系正極活物質を製造した。このときの導電性炭素被覆層の炭素含量は正極活物質に対し10重量%であった。
前記実施例2で製造された20gのケイ素系正極活物質を回転管状炉に投入したことを除いては、前記実施例6と同一の方法で導電性炭素被覆層が形成されたケイ素系正極活物質を製造した。このときの導電性炭素被覆層の炭素含量は、正極活物質に対して10重量%であった。
前記実施例3で製造された20gのケイ素系正極活物質を回転管状炉に投入したことを除いては、前記実施例6と同一の方法で導電性炭素被覆層が形成されたケイ素系正極活物質を製造した。このときの導電性炭素被覆層の炭素含量は、正極活物質に対して10重量%であった。
前記実施例4で製造された20gのケイ素系正極活物質を回転管状炉に投入したことを除いては、前記実施例6と同一の方法で導電性炭素被覆層が形成されたケイ素系正極活物質を製造した。このときの導電性炭素被覆層の炭素含量は、正極活物質に対して10重量%であった。
前記実施例5で製造された20gのケイ素系正極活物質を回転管状炉に投入したことを除いては、前記実施例6と同一の方法で導電性炭素被覆層が形成されたケイ素系正極活物質を製造した。このときの導電性炭素被覆層の炭素含量は、正極活物質に対して10重量%であった。
一酸化ケイ素のみを用いて正極活物質を製造した。
一酸化ケイ素を前記実施例6と同一の方法で被覆させて正極活物質を製造した。
前記実施例1乃至10及び比較例1乃至2の正極活物質を導電材に、アセチレンブラック及びバインダーとしてポリビニリデンフルオリド(polyvinylidene fluoride、PVdF)を88:2:10の重量比で混合し、これらを溶媒であるN−メチル−2−ピロリドン(N-methyl-2-pyrrolidone、NMP)とともに混合して均一な電極スラリーを製造した。製造された電極スラリーを銅集電体の一面に65μmの厚さに被覆し、乾燥及び圧延したあと必要な大きさにパンチング(punching)して電極を製造した。
本発明の一実施例に係るケイ素系正極活物質の表面、構造及び成分を調べるため走査電子顕微鏡(SEM)、透過電子顕微鏡(TEM)、X-線回折分析(XRD)で分析し、その結果を図2乃至図5に示した。
Claims (15)
- ケイ素系リチウム二次電池用負極活物質であって、
SiOx(0<x<2)相と、前記SiOx(0<x<2)の不均等化により形成されるケイ素相及び二酸化ケイ素相とを含んでなり、
前記二酸化ケイ素相が、結晶質である粒子を含んでなることを特徴とする、ケイ素系リチウム二次電池用負極活物質。 - 前記二酸化ケイ素相が、前記SiOx(0<x<2)相に分散されていることを特徴とする、請求項1に記載のケイ素系リチウム二次電池用負極活物質。
- 前記SiOx(0<x<2)が、一酸化ケイ素であることを特徴とする、請求項1又は2に記載のケイ素系リチウム二次電池用負極活物質。
- 前記二酸化ケイ素相が、クリストバライト(cristoballite)を含むことを特徴とする、請求項1〜3の何れか一項に記載のケイ素系リチウム二次電池用負極活物質。
- 前記二酸化ケイ素相が、前記負極活物質に対して2〜50重量%で含まれてなることを特徴とする、請求項1〜4の何れか一項に記載のケイ素系リチウム二次電池用負極活物質。
- 前記ケイ素相が、前記ケイ素系リチウム二次電池用負極活物質の中心周辺部より中心部で濃度がさらに大きいことを特徴とする、請求項1〜5の何れか一項に記載のケイ素系リチウム二次電池用負極活物質。
- 前記二酸化ケイ素相が、前記ケイ素系リチウム二次電池用負極活物質の中心部より中心周辺部で濃度がさらに大きいことを特徴とする、請求項1〜6の何れか一項に記載のケイ素系リチウム二次電池用負極活物質。
- 炭素被覆材をさらに含むことを特徴とする、請求項1〜7の何れか一項に記載のケイ素系リチウム二次電池用負極活物質。
- リチウム二次電池であって、
負極活物質を含む負極と、正極活物質を含む正極と、及び分離膜とを備えてなり、
前記負極活物質が、請求項1〜8の何れか一項に記載のケイ素系リチウム二次電池用負極活物質を含んでなるものである、リチウム二次電池。 - ケイ素系リチウム二次電池用負極活物質の製造方法であって、
アルカリ系水酸化物を極性溶媒に溶解させた後、SiOx(0<x<2)と混合するステップと、
前記ステップで製造された混合物から前記極性溶媒を蒸発させた後、熱処理するステップとを含んでなり、
前記アルカリ系水酸化物が、前記混合物の総重量に対して、0.01〜30重量%であり、
前記熱処理が、750〜1000℃で5〜120分間行われてなるものである、ケイ素系リチウム二次電池用負極活物質の製造方法。 - 前記アルカリ系水酸化物が、LiOH、NaOH、KOH、Be(OH)2、Mg(OH)、Ca(OH)2及びこれらの水化物からなる群から選択される一種以上のものであることを特徴とする、請求項10に記載のケイ素系リチウム二次電池用負極活物質の製造方法。
- 前記極性溶媒が、水又はアルコールであることを特徴とする、請求項10又は11に記載のケイ素系リチウム二次電池用負極活物質の製造方法。
- 前記熱処理された混合物を濾過するステップをさらに含んでなることを特徴とする、請求項10〜12の何れか一項に記載のケイ素系リチウム二次電池用負極活物質の製造方法。
- 前記熱処理された混合物に炭素を被覆するステップをさらに含んでなることを特徴とする、請求項10〜13の何れか一項に記載のケイ素系リチウム二次電池用負極活物質の製造方法。
- 前記炭素が、前記ケイ素系リチウム二次電池用負極活物質の総重量に対して1〜30重量%で包含してなることを特徴とする、請求項14に記載のケイ素系リチウム二次電池用負極活物質の製造方法。
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JP2019220350A (ja) * | 2018-06-20 | 2019-12-26 | 株式会社ダイネンマテリアル | リチウムイオン電池用負極材料、リチウムイオン電池用負極及びリチウムイオン電池 |
JP7098144B2 (ja) | 2018-06-20 | 2022-07-11 | 株式会社ダイネンマテリアル | リチウムイオン電池用負極材料、リチウムイオン電池用負極及びリチウムイオン電池 |
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US20130280614A1 (en) | 2013-10-24 |
US9780357B2 (en) | 2017-10-03 |
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