JP6108190B2 - 炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法 - Google Patents
炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法 Download PDFInfo
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- JP6108190B2 JP6108190B2 JP2015551626A JP2015551626A JP6108190B2 JP 6108190 B2 JP6108190 B2 JP 6108190B2 JP 2015551626 A JP2015551626 A JP 2015551626A JP 2015551626 A JP2015551626 A JP 2015551626A JP 6108190 B2 JP6108190 B2 JP 6108190B2
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- Prior art keywords
- lithium
- iron phosphate
- carbon
- lithium iron
- producing
- Prior art date
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 63
- 239000011858 nanopowder Substances 0.000 title claims description 63
- 229910052799 carbon Inorganic materials 0.000 title claims description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 239000002245 particle Substances 0.000 claims description 65
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 37
- 229910052744 lithium Inorganic materials 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 29
- 239000007774 positive electrode material Substances 0.000 claims description 22
- 239000007810 chemical reaction solvent Substances 0.000 claims description 21
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 239000012692 Fe precursor Substances 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 11
- 239000012688 phosphorus precursor Substances 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 150000002894 organic compounds Chemical class 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 7
- 229960002413 ferric citrate Drugs 0.000 claims description 7
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical group [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 7
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 5
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 5
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 5
- 229910003002 lithium salt Inorganic materials 0.000 claims description 5
- 159000000002 lithium salts Chemical class 0.000 claims description 5
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 5
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical group CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 3
- 239000011255 nonaqueous electrolyte Substances 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- GZCGUPFRVQAUEE-UHFFFAOYSA-N 2,3,4,5,6-pentahydroxyhexanal Chemical compound OCC(O)C(O)C(O)C(O)C=O GZCGUPFRVQAUEE-UHFFFAOYSA-N 0.000 claims description 2
- AEMOLEFTQBMNLQ-UHFFFAOYSA-N 3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound OC1OC(C(O)=O)C(O)C(O)C1O AEMOLEFTQBMNLQ-UHFFFAOYSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 claims description 2
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 claims description 2
- 239000005955 Ferric phosphate Substances 0.000 claims description 2
- 229930091371 Fructose Natural products 0.000 claims description 2
- 239000005715 Fructose Substances 0.000 claims description 2
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 2
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 2
- 229940032958 ferric phosphate Drugs 0.000 claims description 2
- 229930182830 galactose Natural products 0.000 claims description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 2
- NPLZZSLZTJVZSX-UHFFFAOYSA-L iron(2+);oxalate;dihydrate Chemical compound O.O.[Fe+2].[O-]C(=O)C([O-])=O NPLZZSLZTJVZSX-UHFFFAOYSA-L 0.000 claims description 2
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 2
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 2
- IAQLJCYTGRMXMA-UHFFFAOYSA-M lithium;acetate;dihydrate Chemical compound [Li+].O.O.CC([O-])=O IAQLJCYTGRMXMA-UHFFFAOYSA-M 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- DDXPLCBTGWFAIG-UHFFFAOYSA-N triazanium;phosphate;trihydrate Chemical compound [NH4+].[NH4+].[NH4+].O.O.O.[O-]P([O-])([O-])=O DDXPLCBTGWFAIG-UHFFFAOYSA-N 0.000 claims description 2
- LRPQHRZRXAFVLP-UHFFFAOYSA-K trilithium phosphate dodecahydrate Chemical compound [Li+].[Li+].[Li+].O.O.O.O.O.O.O.O.O.O.O.O.[O-]P([O-])([O-])=O LRPQHRZRXAFVLP-UHFFFAOYSA-K 0.000 claims description 2
- UPLCYFWQZHLPFH-UHFFFAOYSA-N butane-1,1-diol;butane-2,3-diol Chemical compound CCCC(O)O.CC(O)C(C)O UPLCYFWQZHLPFH-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- -1 lithium iron phosphate compound Chemical class 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000011247 coating layer Substances 0.000 description 15
- 238000009826 distribution Methods 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 239000011164 primary particle Substances 0.000 description 4
- 239000007784 solid electrolyte Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000008151 electrolyte solution Substances 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- WNXJIVFYUVYPPR-UHFFFAOYSA-N 1,3-dioxolane Chemical compound C1COCO1 WNXJIVFYUVYPPR-UHFFFAOYSA-N 0.000 description 2
- AZUYLZMQTIKGSC-UHFFFAOYSA-N 1-[6-[4-(5-chloro-6-methyl-1H-indazol-4-yl)-5-methyl-3-(1-methylindazol-5-yl)pyrazol-1-yl]-2-azaspiro[3.3]heptan-2-yl]prop-2-en-1-one Chemical compound ClC=1C(=C2C=NNC2=CC=1C)C=1C(=NN(C=1C)C1CC2(CN(C2)C(C=C)=O)C1)C=1C=C2C=NN(C2=CC=1)C AZUYLZMQTIKGSC-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 239000003365 glass fiber Substances 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
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000011356 non-aqueous organic solvent Substances 0.000 description 2
- 239000010450 olivine Substances 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- PYOKUURKVVELLB-UHFFFAOYSA-N trimethyl orthoformate Chemical compound COC(OC)OC PYOKUURKVVELLB-UHFFFAOYSA-N 0.000 description 2
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical compound FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 description 1
- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- PPDFQRAASCRJAH-UHFFFAOYSA-N 2-methylthiolane 1,1-dioxide Chemical compound CC1CCCS1(=O)=O PPDFQRAASCRJAH-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229910000925 Cd alloy Inorganic materials 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
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- 229910010238 LiAlCl 4 Inorganic materials 0.000 description 1
- 229910015015 LiAsF 6 Inorganic materials 0.000 description 1
- 229910015044 LiB Inorganic materials 0.000 description 1
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 229910012513 LiSbF 6 Inorganic materials 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- ZHGDJTMNXSOQDT-UHFFFAOYSA-N NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O Chemical compound NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O.NP(N)(N)=O ZHGDJTMNXSOQDT-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
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Description
先ず、リチウム前駆体、鉄前駆体及びリン前駆体を準備し、これを反応溶媒に入れて均一な混合溶液を製造する。
次に、前記混合溶液を反応器内に投入して反応させる。前記段階では、非晶質のリチウムリン酸鉄ナノシード(seeds)粒子が製造される。
前記(b)段階を経て製造されたリチウムリン酸鉄ナノシード粒子を、非活性雰囲気下で熱処理すると、粒子の表面に炭素が一部または全体にコーティングされたリチウムリン酸鉄ナノ粉末を製造することができる。
さらに、本発明では前記オリビン結晶構造のリチウムリン酸鉄ナノ粉末を含む正極活物質を提供することができる。前記正極活物質としては、前記リチウムリン酸鉄粉末の外にも選択的に導電材、バインダ及び充填剤などをさらに含んで構成され得る。
リチウムヒドロキシドハイドレート(LiOH・H2O)2.5179g、クエン酸第二鉄水和物(FeC6H5O7・nH2O)14.6964g及びリン酸(H3PO4)5.88gを1,4-ブタンジオール300mlに入れて充分に撹拌させて混合溶液を製造した。
リチウムヒドロキシドハイドレート(LiOH・H2O)2.5179g、クエン酸第二鉄水和物(FeC6H5O7・nH2O)14.6964g及びリン酸(H3PO4)5.88gを1,4-ブタンジオール300mlに入れて充分に撹拌させて混合溶液を製造した。
リチウムヒドロキシドハイドレート(LiOH・H2O)0.42g、クエン酸第二鉄水和物(FeC6H5O7・nH2O)2.45g及びリン酸0.98gをエチレングリコール50mlに入れて充分に撹拌させて混合溶液を製造した。
Claims (18)
- (a)反応溶媒にリチウム前駆体、鉄前駆体及びリン前駆体を入れて混合溶液を製造する段階、
(b)前記混合溶液を反応器内に投入して反応させ、非晶質のリチウムリン酸鉄ナノシード(seeds)を製造する段階、及び
(c)前記製造されたリチウムリン酸鉄ナノシードを熱処理して粒子の表面に炭素が一部または全体にコーティングされたリチウムリン酸鉄ナノ粉末を製造する段階、を含み、
前記反応溶媒は、1,2-ブタンジオール(1,2-butandiol)、1,3-ブタンジオール(1,3-butandiol)、1,4-ブタンジオール(1,4-butandiol)、2,3-ブタンジオール(2,3-butandiol)及びこれらの異性質体からなる群より選択される1つ以上であり、
前記リチウムリン酸鉄ナノシードを製造する段階(b)は、120〜235℃の温度範囲内で0.1〜24時間の間進められる炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。 - 前記リチウムリン酸鉄ナノシードを製造する段階(b)で製造されたナノシード粒子は、冷却段階、洗浄段階及び乾燥段階のうち選択される一つ以上の段階を経る請求項1に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記混合溶液を製造する段階(a)、前記リチウムリン酸鉄ナノシードを製造する段階(b)または前記リチウムリン酸鉄ナノ粉末を製造する段階(c)で炭素コーティングのための有機化合物を添加する段階をさらに含む請求項1または2に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウムリン酸鉄ナノシードを製造する段階(b)は、前記反応溶媒の沸点以下の温度で進められる請求項1から3のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウムリン酸鉄ナノシードを製造する段階(b)は、150〜235℃の温度範囲内で0.1〜5時間の間進められる請求項1から4のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウムリン酸鉄ナノシードを製造する段階(b)は、10bar(1bar=105Pa)以下の圧力条件下で進められる請求項1から5のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウムリン酸鉄ナノ粉末を製造する段階(c)は、400〜900℃の温度範囲内で0.5〜5時間の間進められる請求項1から6のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記洗浄段階は、アセトンとメタノールを順次用いて洗浄する請求項2に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記乾燥段階は、20〜160℃の温度範囲内で2〜40時間の間進められる請求項2に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウム前駆体は、リチウムアセテートジハイドレート(CH3COOLi・2H2O)、リチウムヒドロキシドモノハイドレート(LiOH・H2O)、リチウムヒドロキシド(LiOH)、リチウムカーボネート(Li2CO3)、リチウムホスフェート(Li3PO4)、リチウムホスフェートドデカハイドレート(Li3PO4・2H2O)及びリチウムオキサレート(Li2C2O4)からなる群より選択される1または2以上の混合物である請求項1から9のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記鉄前駆体は、クエン酸第二鉄(FeC6H5O7)、クエン酸第二鉄水和物(FeC6H5O7・nH2O)、硫酸第一鉄七水和物(FeSO4・H2O)、シュウ酸鉄二水和物(FeC2O4・H2O)、鉄アセチルアセトネート(Fe(C5H7O2)3)、リン酸第二鉄二水和物(FePO4・H2O)及び水酸化第二鉄(FeO(OH))からなる群より選択される1または2以上の混合物である請求項1から10のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リン前駆体は、トリ-アンモニウムホスフェートトリハイドレート((NH4)3PO4・H2O)、アンモニウムホスフェート((NH4)2HPO4)、アンモニウムジハイドロジェンホスフェート(NH4H2PO4)、及びリン酸(H3PO4)からなる群より選択される1または2以上の混合物である請求項1から11のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記有機化合物は、グルコース、スクロース、ガラクトース、フルクトース、ラクトース、澱粉、マンノース、リボース、アルドヘキソース及びケトヘキソースからなる群より選択される1または2以上の混合物である請求項3に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 前記有機化合物は、(b)段階で製造されるリチウムリン酸鉄ナノシードの全体重量を基準に0.1〜5wt%で添加される請求項3に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法。
- 請求項1から14のいずれか一項に記載の炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法により炭素コーティングリチウムリン酸鉄ナノ粉末を製造する段階を含む正極活物質の製造方法。
- 前記正極活物質は、導電材、バインダ及び充填剤のうち選択される一つ以上をさらに有する請求項15に記載の正極活物質の製造方法。
- 正極集電体、及び、前記正極集電体上に塗布された正極活物質を有するリチウム二次電池用正極の製造方法であって、
請求項15または16に記載の正極活物質の製造方法により正極活物質を製造する段階を含むリチウム二次電池用正極の製造方法。 - リチウム二次電池用正極と負極、分離膜及びリチウム塩含有の非水電解液を有するリチウム二次電池の製造方法であって、
請求項17に記載のリチウム二次電池用正極の製造方法によりリチウム二次電池用正極を製造する段階を含むリチウム二次電池の製造方法。
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