JP2022518681A - リチウム二次電池 - Google Patents
リチウム二次電池 Download PDFInfo
- Publication number
- JP2022518681A JP2022518681A JP2021539357A JP2021539357A JP2022518681A JP 2022518681 A JP2022518681 A JP 2022518681A JP 2021539357 A JP2021539357 A JP 2021539357A JP 2021539357 A JP2021539357 A JP 2021539357A JP 2022518681 A JP2022518681 A JP 2022518681A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- sulfur
- secondary battery
- positive electrode
- lithium
- 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.)
- Granted
Links
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011593 sulfur Substances 0.000 claims abstract description 69
- 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
- 239000007774 positive electrode material Substances 0.000 claims abstract description 66
- GJEAMHAFPYZYDE-UHFFFAOYSA-N [C].[S] Chemical compound [C].[S] GJEAMHAFPYZYDE-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 43
- 239000011800 void material Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims description 97
- 239000003575 carbonaceous material Substances 0.000 claims description 70
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 claims description 62
- 239000008151 electrolyte solution Substances 0.000 claims description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- -1 denka black Substances 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 16
- 239000012528 membrane Substances 0.000 claims description 15
- 229910003002 lithium salt Inorganic materials 0.000 claims description 12
- 159000000002 lithium salts Chemical class 0.000 claims description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 11
- 229910001416 lithium ion Inorganic materials 0.000 claims description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 9
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
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- DOESGSGKEZIPFW-UHFFFAOYSA-N 1,1,1,2,3,3-hexafluoro-3-(2,2,3,3-tetrafluoropropoxy)propane Chemical group FC(F)C(F)(F)COC(F)(F)C(F)C(F)(F)F DOESGSGKEZIPFW-UHFFFAOYSA-N 0.000 claims description 5
- 239000004210 ether based solvent Substances 0.000 claims description 5
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- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 claims description 5
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- JOROOXPAFHWVRW-UHFFFAOYSA-N 1,1,1,2,3,3-hexafluoro-3-(2,2,3,3,3-pentafluoropropoxy)propane Chemical compound FC(F)(F)C(F)C(F)(F)OCC(F)(F)C(F)(F)F JOROOXPAFHWVRW-UHFFFAOYSA-N 0.000 claims description 2
- WSIIYENBWBHASS-UHFFFAOYSA-N 1-(difluoromethoxy)-1,1,2,3,3,3-hexafluoropropane Chemical compound FC(F)OC(F)(F)C(F)C(F)(F)F WSIIYENBWBHASS-UHFFFAOYSA-N 0.000 claims description 2
- ZASBKNPRLPFSCA-UHFFFAOYSA-N 2-(difluoromethoxy)-1,1,1-trifluoroethane Chemical compound FC(F)OCC(F)(F)F ZASBKNPRLPFSCA-UHFFFAOYSA-N 0.000 claims description 2
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
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- 239000000654 additive Substances 0.000 description 8
- 229920003048 styrene butadiene rubber Polymers 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 235000013365 dairy product Nutrition 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 7
- 239000007773 negative electrode material Substances 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 235000019241 carbon black Nutrition 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
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- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 5
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- 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 5
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- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 229910013553 LiNO Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 239000011149 active material Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
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- 239000011777 magnesium Substances 0.000 description 3
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- 229910052712 strontium Inorganic materials 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
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- 239000010936 titanium Substances 0.000 description 3
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
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- 101710137710 Thioesterase 1/protease 1/lysophospholipase L1 Proteins 0.000 description 2
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 description 2
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- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
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- 239000001913 cellulose Substances 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- AJAFRMGZWFDZAS-UHFFFAOYSA-M cesium;nitrite Chemical compound [Cs+].[O-]N=O AJAFRMGZWFDZAS-UHFFFAOYSA-M 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- JLQNHALFVCURHW-UHFFFAOYSA-N cyclooctasulfur Chemical compound S1SSSSSSS1 JLQNHALFVCURHW-UHFFFAOYSA-N 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- IOCGMLSHRBHNCM-UHFFFAOYSA-N difluoromethoxy(difluoro)methane Chemical compound FC(F)OC(F)F IOCGMLSHRBHNCM-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- UZZWBUYVTBPQIV-UHFFFAOYSA-N dme dimethoxyethane Chemical compound COCCOC.COCCOC UZZWBUYVTBPQIV-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 150000002461 imidazolidines Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910001959 inorganic nitrate Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229940006487 lithium cation Drugs 0.000 description 1
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 1
- IDNHOWMYUQKKTI-UHFFFAOYSA-M lithium nitrite Chemical compound [Li+].[O-]N=O IDNHOWMYUQKKTI-UHFFFAOYSA-M 0.000 description 1
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- LRMHVVPPGGOAJQ-UHFFFAOYSA-N methyl nitrate Chemical compound CO[N+]([O-])=O LRMHVVPPGGOAJQ-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- CSDTZUBPSYWZDX-UHFFFAOYSA-N n-pentyl nitrite Chemical compound CCCCCON=O CSDTZUBPSYWZDX-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- VLZLOWPYUQHHCG-UHFFFAOYSA-N nitromethylbenzene Chemical compound [O-][N+](=O)CC1=CC=CC=C1 VLZLOWPYUQHHCG-UHFFFAOYSA-N 0.000 description 1
- 239000011356 non-aqueous organic solvent Substances 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 235000010289 potassium nitrite Nutrition 0.000 description 1
- 239000004304 potassium nitrite Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- KAOQVXHBVNKNHA-UHFFFAOYSA-N propyl nitrite Chemical compound CCCON=O KAOQVXHBVNKNHA-UHFFFAOYSA-N 0.000 description 1
- 229920001384 propylene homopolymer Polymers 0.000 description 1
- XLABPPWWFVQMBZ-UHFFFAOYSA-O pyridin-1-ium;nitrate Chemical compound [O-][N+]([O-])=O.C1=CC=[NH+]C=C1 XLABPPWWFVQMBZ-UHFFFAOYSA-O 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 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
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- WZEOZJQLTRFNCU-UHFFFAOYSA-N trifluoro(trifluoromethoxy)methane Chemical compound FC(F)(F)OC(F)(F)F WZEOZJQLTRFNCU-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
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- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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Abstract
Description
正極;負極;分離膜;及び電解液を含むリチウム二次電池であって、
下記数学式1で表されるED factor値が850以上である、リチウム二次電池を提供する:
[数学式1]
[数学式2]
前記電解液は、溶媒及びリチウム塩を含み、
前記溶媒は、下記数学式4で表されるDV2 factor値が1.75以下である第1の溶媒及びフッ素化されたエーテル系溶媒である第2の溶媒を含むことを特徴とすることができる:
[数学式4]
DVは、単位体積当たりの双極子モーメント(D・mol/L)であり、
μは、溶媒の粘度((cP、25℃))であり、
γは、100(定数)である。
SC factorは、前記数学式2により定義された値と同一であり、
DV2 factorは、前記数学式4により定義された値と同一である。
[数学式2]
前記リチウム二次電池は、下記数学式1で表されるED factor値が850以上であり、
[数学式1]
[数学式2]
前記電解液は、溶媒及びリチウム塩を含み、
前記溶媒は、
下記数学式4で表されるDV2 factor値が1.75以下である第1の溶媒;及び
フッ素化されたエーテル系溶媒である第2の溶媒を含むことを特徴とするリチウム二次電池を提供する:
[数学式4]
製造例1:硫黄-炭素複合体物質の製造
比表面積が319m2/gであり、電気伝導度(粉体抵抗測定装置(ハンテック、powder resistivity measurement system)を用いて2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した値)が62S/cmであるカーボンナノチューブ(AC factor=156)と硫黄(S8)を1:3の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
比表面積が1400m2/gであり、電気伝導度(粉体抵抗測定装置(ハンテク、powder resistivity measurement system)を用いて2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した値)が26S/cmであるカーボンブラック(AC factor=192)と硫黄(S8)を1:3の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
比表面積が184m2/gであり、電気伝導度(粉体抵抗測定装置(ハンテク、powder resistivity measurement system)を用いて2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した値)が41S/cmであるカーボンナノチューブ(AC factor=100)と硫黄(S8)を1:3の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
比表面積が191m2/gであり、電気伝導度(粉体抵抗測定装置(ハンテク、powder resistivity measurement system)を用いて2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した値)が47S/cmであるカーボンナノチューブ(AC factor=113)と硫黄(S8)を1:3の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
比表面積が58m2/gであり、電気伝導度(粉体抵抗測定装置(ハンテク、powder resistivity measurement system)を用いて2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した値)が33S/cmであるカーボンナノチューブ(AC factor=72)と硫黄(S8)を1:3の重量比で均一に混合し、乳鉢混合(mortar mixing)で粉砕した後、155℃のオーブンで30分間置いて硫黄-炭素複合体を製造した。
前記製造例1~4で製造された硫黄-炭素複合体88重量%、または比較製造例1で製造された硫黄-炭素複合体88重量%、導電材としてデンカブラック5重量%、及びバインダーとしてSBRとCMC7重量%を蒸留水と混合し、活物質層形成用組成物を製造した。
水を溶媒とし、硫黄、スーパーP(Super-P、SP)、導電材及びバインダーをボールミルで混合し、正極活物質層形成用組成物を製造した。このとき、導電材としてはデンカブラックを、バインダーとしてはSBRとCMCの混合形態のバインダーを用い、混合比率は重量比で硫黄及びSP(重量比9:1):導電材:バインダーが90:10:10となるようにした。製造した正極活物質層形成用組成物をアルミニウム集電体に塗布した後、乾燥して正極を製造した(正極のエネルギー密度:6.18mAh/cm2)。製造された正極で正極活物質層の空隙率は75%、正極活物質層の単位面積当たりの硫黄の質量が3.1mg/cm2、これに基づいて計算されたSC factor値が0.41であった。
前記製造例5~8で製造されたそれぞれの正極と、負極として150μm厚さのリチウム箔を用い、分離膜として厚さ20μm、気孔度45%のポリエチレンを用いて、正極と負極を対面するように位置させた後、これらの間に分離膜を介在して電極組立体を製造した。
前記比較製造例2で製造された正極を用いたことを除いては、前記実施例1と同様の方法でリチウム-硫黄二次電池を製造した。
前記比較製造例3で製造された正極を用いたことを除いては、前記実施例1と同様の方法でリチウム-硫黄二次電池を製造した。
電解液の製造条件を変更して、第2の溶媒として1H,1H,2’H,3H-デカフルオロジプロピルエーテルの代わりに、ジメトキシエタン(Dimethoxyethane、DME)が適用された電解液を用いたことを除いては、比較例1と同様の方法でリチウム-硫黄二次電池を製造した。
電解液の製造条件を変更して、第1の溶媒としてプロピオニトリルの代わりに、単位体積当たりの双極子モーメントが96.13 D・mol/L、溶媒の粘度が1.71cP、これに基づいて計算されたDV2 factor値が1.77であるプロピレンカーボネート(Propylene carbonate)を用いたことを除いては、比較例1と同様の方法でリチウム-硫黄二次電池を製造した。
実施例1~4と比較例1~4で製造されたリチウム-硫黄二次電池を充放電測定装置を用いて1.0Vから3.6Vまでの容量を測定した。
充放電測定装置(LAND CT-2001A、ウハン(Wuhan)、中国)を用いて、初期放電-充電-放電-充電-放電の2.5サイクルの間に0.1Cの速度で充電-放電を行い、その後、充電-放電0.2C、3サイクル行った後、充電は0.3C、放電は0.5Cの速度で行って50サイクルまで充電-放電を行いながら、実施例1~4と比較例1~4によるリチウム-硫黄二次電池のED factor値を測定して下記表3に示した。
実施例5
(1)正極の製造
硫黄と点型炭素材であるケッチェンブラックを70:30の重量比で混合した後、155℃で30分間熱処理を行って硫黄-炭素複合体を製造した。
上述した方法で製造した正極と負極を対面するように位置させた後、厚さ20μm、気孔度45%のポリエチレン分離膜を前記正極と負極との間に介在した。
正極活物質層の空隙率が55%、正極活物質層の単位面積当たりの硫黄の質量が5.0Mg/cm2、これに基づいて計算されたSC factor値(0.91)を有する正極を製造したことを除いては、実施例5と同様の方法でリチウム-硫黄二次電池を製造した。
電解液に用いられた有機溶媒の種類を変更して、DOL(ジオキソラン)(第1の溶媒)とDME(ジメトキシエタン)(第2の溶媒)を5:5の重量比で混合した溶媒を用い、前記電解液に添加剤としてLiNO3を1重量%添加して用いたことを除いては、実施例5と同様の方法でリチウム-硫黄二次電池を製造した。前記第1の溶媒において単位体積当たりの双極子モーメント(DV)は33.66D・mol/Lであり、溶媒の粘度(μ)は0.7cPであった。これに基づいて計算されたDV2 factor値は2.07であった。
硫黄-炭素複合体の製造時に用いた炭素材として、点型炭素材でなくCNTを用いて硫黄-炭素複合体を製造したことを除いては、比較例5と同様の方法でリチウム-硫黄二次電池を製造した。
硫黄-炭素複合体の製造時に用いた炭素材を点型炭素でなくCNTを用いて硫黄-炭素複合体を製造したことを除いては、実施例5と同様の方法でリチウム-硫黄二次電池を製造した。
実施例5で正極製造時、圧延前及び後の正極脱離現象が発生するか否かを観察した。
実施例及び比較例でそれぞれ製造された正極及び二次電池の条件を整理して下記表4に示した。
Claims (15)
- 正極;負極;分離膜;及び電解液を含むリチウム二次電池であって、
下記数学式1で表されるED factor値が850以上である、リチウム二次電池:
[数学式1]
[数学式2]
- 前記炭素材は、比表面積が100~4500m2/gである、請求項2に記載のリチウム二次電池。
- 前記炭素材は、気孔容積が0.8~5cm3/gである、請求項2または3に記載のリチウム二次電池。
- 前記炭素材に2000kgfの圧力を加えた状態で測定したパウダーの抵抗値を伝導度に換算した電気伝導度が10~100S/cmである、請求項2から4のいずれか一項に記載のリチウム二次電池。
- 前記炭素材は、黒鉛、カーボンナノチューブ、グラフェン、非晶質炭素、カーボンブラック、及び活性炭からなる群より選択される1種以上である、請求項2から5のいずれか一項に記載のリチウム二次電池。
- 前記正極は、点型炭素材を含む、請求項1に記載のリチウム-硫黄二次電池。
- 前記点型炭素材は、カーボンブラック、ケッチェンブラック、デンカブラック、アセチレンブラック、チャンネルブラック、ファーネスブラック、ランプブラック、及びサーマルブラックからなる群より選択される1種以上を含む、請求項7に記載のリチウム二次電池。
- 前記第1の溶媒は、プロピオニトリル、ジメチルアセトアミド、ジメチルホルムアミド、γ-ブチロラクトン、トリエチルアミン及び1-ヨードプロパンからなる群より選択される1種以上を含む、請求項9に記載のリチウム二次電池。
- 前記第2の溶媒は、1H,1H,2’H,3H-デカフルオロジプロピルエーテル、ジフルオロメチル2,2,2-トリフルオロエチルエーテル、1,2,2,2-テトラフルオロエチルトリフルオロメチルエーテル、1,1,2,3,3,3-ヘキサフルオロプロピルジフルオロメチルエーテル、ペンタフルオロエチル2,2,2-トリフルオロエチルエーテル、及び1H、1H、2’H-パーフルオロジプロピルエーテルからなる群より選択される1種以上を含む、請求項9または10に記載のリチウム二次電池。
- 前記溶媒は、前記溶媒全体の重量を基準として、第1の溶媒を1~50重量%で含む、請求項9から11のいずれか一項に記載のリチウム二次電池。
- 前記溶媒は、前記溶媒全体の重量を基準として、第2の溶媒を50~99重量%で含む、請求項9から12のいずれか一項に記載のリチウム二次電池。
- 前記溶媒は、第1の溶媒と第2の溶媒を3:7~1:9の重量比で含む、請求項9から13のいずれか一項に記載のリチウム二次電池。
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