JP2022036097A - リチウムイオン電池材料 - Google Patents
リチウムイオン電池材料 Download PDFInfo
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- JP2022036097A JP2022036097A JP2021198612A JP2021198612A JP2022036097A JP 2022036097 A JP2022036097 A JP 2022036097A JP 2021198612 A JP2021198612 A JP 2021198612A JP 2021198612 A JP2021198612 A JP 2021198612A JP 2022036097 A JP2022036097 A JP 2022036097A
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- Prior art keywords
- lithium
- droplets
- precursor solution
- particles
- microwave
- Prior art date
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- Granted
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- 239000000463 material Substances 0.000 title claims abstract description 66
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 47
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 182
- 239000002243 precursor Substances 0.000 claims abstract description 120
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 105
- 239000007858 starting material Substances 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 121
- 238000000034 method Methods 0.000 claims description 104
- 239000000203 mixture Substances 0.000 claims description 47
- 229910013716 LiNi Inorganic materials 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 30
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 26
- 238000010791 quenching Methods 0.000 claims description 26
- 230000000171 quenching effect Effects 0.000 claims description 26
- 239000011572 manganese Substances 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 21
- 229910052760 oxygen Inorganic materials 0.000 claims description 21
- 238000009826 distribution Methods 0.000 claims description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 229910002651 NO3 Inorganic materials 0.000 claims description 12
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 12
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 12
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 10
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 10
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 150000001868 cobalt Chemical class 0.000 claims description 5
- 229940071257 lithium acetate Drugs 0.000 claims description 5
- 229940071125 manganese acetate Drugs 0.000 claims description 5
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 4
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- 229910003002 lithium salt Inorganic materials 0.000 claims description 4
- 159000000002 lithium salts Chemical class 0.000 claims description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- 229940078494 nickel acetate Drugs 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001882 dioxygen Inorganic materials 0.000 claims description 3
- 229910019556 Coz O2 Inorganic materials 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 abstract description 5
- 210000002381 plasma Anatomy 0.000 description 81
- 230000008569 process Effects 0.000 description 27
- 238000000576 coating method Methods 0.000 description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 229910052799 carbon Inorganic materials 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 14
- 239000012071 phase Substances 0.000 description 12
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 11
- 239000010406 cathode material Substances 0.000 description 11
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 11
- 239000011257 shell material Substances 0.000 description 10
- 230000008901 benefit Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 239000012705 liquid precursor Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000007784 solid electrolyte Substances 0.000 description 4
- 238000005118 spray pyrolysis Methods 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910016118 LiMn1.5Ni0.5O4 Inorganic materials 0.000 description 3
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- -1 for example Inorganic materials 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 229910001867 inorganic solvent Inorganic materials 0.000 description 3
- 239000003049 inorganic solvent Substances 0.000 description 3
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 description 3
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 description 3
- 229940078487 nickel acetate tetrahydrate Drugs 0.000 description 3
- OINIXPNQKAZCRL-UHFFFAOYSA-L nickel(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Ni+2].CC([O-])=O.CC([O-])=O OINIXPNQKAZCRL-UHFFFAOYSA-L 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 2
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 2
- 229910012748 LiNi0.5Mn0.3Co0.2O2 Inorganic materials 0.000 description 2
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 2
- 229910014422 LiNi1/3Mn1/3Co1/3O2 Inorganic materials 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000005112 continuous flow technique Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012456 homogeneous solution Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000037361 pathway Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 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 description 1
- 229910013733 LiCo Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910011322 LiNi0.6Mn0.2Co0.2O2 Inorganic materials 0.000 description 1
- 229910015915 LiNi0.8Co0.2O2 Inorganic materials 0.000 description 1
- 229910014421 LiNi1/3Mn1/3CO1/3 Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910012305 LiPON Inorganic materials 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910015228 Ni1/3Mn1/3CO1/3 Inorganic materials 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 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 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- NDPGDHBNXZOBJS-UHFFFAOYSA-N aluminum lithium cobalt(2+) nickel(2+) oxygen(2-) Chemical compound [Li+].[O--].[O--].[O--].[O--].[Al+3].[Co++].[Ni++] NDPGDHBNXZOBJS-UHFFFAOYSA-N 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002902 bimodal effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011221 initial treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- QEXMICRJPVUPSN-UHFFFAOYSA-N lithium manganese(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Li+] QEXMICRJPVUPSN-UHFFFAOYSA-N 0.000 description 1
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000013387 non optimize process Methods 0.000 description 1
- 230000005019 pattern of movement Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/34—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of sprayed or atomised solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/10—Nitrates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1235—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O4]2-, e.g. Li2Mn2O4, Li2[MxMn2-x]O4
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0072—Mixed oxides or hydroxides containing manganese
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C53/00—Saturated compounds having only one carboxyl group bound to an acyclic carbon atom or hydrogen
- C07C53/08—Acetic acid
- C07C53/10—Salts thereof
-
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Abstract
Description
組み合わせて、リチウムを含む均質前駆体溶液を形成すること、及び液滴生成器(droplet maker)を用いて、制御されたサイズを有する均質前駆体溶液の液滴を生成することを含む。この方法はさらに、均質前駆体溶液の液滴をマイクロ波生成プラズマ中に導入すること、マイクロ波生成プラズマからミクロン又はサブミクロンスケールのリチウム含有粒子を作製すること、リチウム含有粒子を捕集すること、及びリチウム含有粒子を含むスラリーを形成して、リチウムイオン電池材料を形成することも含む。
リ秒間で完了することができるシングルフロープロセス(single flow process)を用い
て作製することができる。リチウム含有粒子を作製するためのプロセスが大きく単純化され、加速されるだけでなく、最終製品のサイズが非常により均一となり、多孔度、形態、及び化学組成の精密な調製が可能となる。本明細書で述べる技術を用いて、リチウム系電池のためのカソード、アノード、又は固体電解質材料を作製することができる。カソード、アノード、及び電解質のうちの1又は複数に用いられる例示的材料としては、限定されないが、LiNixMnyCozO2、LiNixCoyAlzO2、LiFePO4、Li8ZrO6、Li2FeMn3O8、Li4Ti5O12、SnO2、Co9S8、LiVP2O7、NaLaTi2O6、LixPOyNz、Liガーネット、及びLi10GeP2O12が挙げられる。
などの様々な混合物を含み得るプラズマプロセス雰囲気を制御することによって調節されてもよい。
チウムを含む均質前駆体溶液が形成される。ある実施形態では、均質前駆体溶液は、前駆体溶液中において出発物質が均等に分布されるように、分子レベルで混合される。例えば、均質前駆体溶液は、酢酸リチウム、酢酸ニッケル四水和物、酢酸マンガン四水和物、及び酢酸コバルト四水和物などのすべて水などの溶媒に溶解された金属塩から成る水溶液を含み得る。別の例では、均質前駆体溶液は、硝酸リチウム、硝酸ニッケル、硝酸マンガン、及び硝酸コバルトなどのすべて水などの溶媒に溶解された金属塩から成る水溶液を含み得る。上記で考察したように、異なる化学量論的割合の出発物質からは、最終リチウム含有粒子の異なる化学組成が得られる結果となり得る。
が必要となる。これらの工程としては、例えば、すべてスラリーが形成され得る前の撹拌、沈澱、ろ過、洗浄、乾燥、篩掛け、混合、焼成、分級、及び被覆が挙げられ得る。そのような技術は、出発物質の各バッチに対して完了するのに、最大で何日間も掛かり得る。対照的に、本開示で述べる連続プロセスフロー20は、ミリ秒から分の単位で完了することができる単一の連続工程で、一式の出発物質からリチウム含有粒子を形成することができる。具体的には、出発物質が溶解されて前駆体水溶液とされると、前駆体溶液の液滴が、単一工程でリチウム含有粒子が作製されるプラズマトーチ中へ導入される。プラズマトーチ内で発生する反応、システムの様々なコンポーネント、さらには前駆体溶液を作製することができる方法の例は、図1、4、及び5に関してより詳細に記載される。
の様々な混合物及び割合が前駆体溶液に用いられてよい。
放射線源409を制御してよい。例えば、マイクロ波放射線源409は、約6000Kの実質的に均一な温度プロファイルを生成するように制御されてよい。出発物質の量及び割合は、ある実施形態では、以下の表1に示される割合に従って選択されてよい。
Ni0.5O4、LiCoO2、LiNiO2など)。さらに、前駆体物質及び/若しくは添加剤に対する変動又は制御による勾配又は層状の組成変化も可能である。本開示で述べるプロセスが本質的に連続的であることにより、各層の化学組成がその厚さ方向全体にわたって変動して所望される物質のいずれの有益性をも利用することができるように、カソード材料の層ごとの積層が可能である。連続プロセスであることはまた、従来の電池生産技術で発生するバッチ間の変動も排除する。加えて、プロセスが単純であることにより、従来の生産技術では不可能であり得るか又は高コストであり得る迅速な材料開発及び新規な材料配合(例:広範なNMC配合及び/又はドーパントの添加)の有益性の研究も可能である。
溶媒の種類、溶液がアトマイザーを通される圧力、反応チャンバー内でのアトマイザーの向き、酸素濃度、及び高温ゾーン内の温度を制御することによって調整又は調製され得る。
入されてよく、そこで、LCO前駆体溶液が、第三の液滴生成器を用いて第三のプラズマ中へ注入される。LCO被覆領域から排出された後、電池カソードは、電池内にすぐに設置できる状態であり得る。各層の厚さは、ある実施形態では、前駆体供給速度の調整並びに/又は集電板が動く速度及びパターンの制御によって、独立して制御することができる。1つの例としての実施形態では、各層の所望される厚さは、約34~100μmであり、合わせた厚さは、約100~300μmである。
Claims (20)
- 出発物質を組み合わせて、リチウムを含む均質前駆体溶液を形成すること;
液滴生成器(droplet maker)を用いて、制御されたサイズを有する前記均質前駆体溶液の液滴を生成すること;
前記均質前駆体溶液の前記液滴をマイクロ波生成プラズマ中に導入すること;
前記マイクロ波生成プラズマからミクロン又はサブミクロンスケールのリチウム含有粒子を作製すること;
前記リチウム含有粒子を捕集すること;及び
前記リチウム含有粒子を含むスラリーを形成して、リチウムイオン電池材料を形成すること
を含む、リチウムイオン電池材料を製造するための方法。 - 前記リチウム含有粒子を捕集することが、前記リチウム含有粒子を急冷することを含み、前記方法はさらに:
急冷流体の選択、急冷流体の流速の制御、又は急冷流体温度の制御によって、前記リチウム含有粒子の急冷速度を制御すること
を含む、請求項1に記載の方法。 - 前記液滴生成器を用いて、前記均質前駆体溶液の前記液滴のサイズを制御することをさらに含む、請求項1に記載の方法。
- プラズマガスの流速、前記マイクロ波生成プラズマのパワー密度、又は前記液滴生成器から排出される前記液滴の速度のうちの少なくとも1つを制御することによって、前記マイクロ波生成プラズマ内での前記均質前駆体溶液の前記液滴の滞留時間を制御することをさらに含む、請求項1に記載の方法。
- 前記均質前駆体溶液が、酢酸リチウム、酢酸ニッケル、酢酸マンガン、及び酢酸コバルトの水和又は非水和形態の水溶液を含む、請求項1に記載の方法。
- 前記均質前駆体溶液が、硝酸リチウム、硝酸ニッケル、硝酸マンガン、及び硝酸コバルトの水溶液を含む、請求項1に記載の方法。
- 前記制御されたサイズの液滴を生成することが、異なる径を有する液滴の2つ以上の流れを生成することを含む、請求項1に記載の方法。
- 前記マイクロ波生成プラズマが、酸素ガス又は酸素含有ガス中で生成される、請求項1に記載の方法。
- 出発物質を組み合わせて、リチウムを含む均質前駆体溶液を形成すること;
液滴生成器を用いて、制御されたサイズを有する前記均質前駆体溶液の液滴を生成すること;
前記均質前駆体溶液の前記液滴をマイクロ波生成プラズマ中に導入すること;
前記マイクロ波生成プラズマからミクロン又はサブミクロンスケールのリチウム含有粒子を作製すること;
前記リチウム含有粒子を急冷すること;並びに
前駆体溶液の化学的性質、液滴サイズ、プラズマガス流量、前記マイクロ波生成プラズマ内での前記液滴の滞留時間、急冷速度、又は前記マイクロ波生成プラズマのパワー密度のうちの少なくとも1つを制御することによって、前記リチウム含有粒子の多孔度、形態、粒子径、粒度分布、又は化学組成のうち少なくとも1つを調製すること
を含む、リチウムイオン電池材料を調製する方法。 - 前記リチウム含有粒子の前記形態を調製することが、前記マイクロ波生成プラズマ及び前記マイクロ波生成プラズマのアフターグロー領域内での前記液滴の前記滞留時間を制御することを含む、請求項9に記載の方法。
- 前記リチウムイオン粒子の前記多孔度を制御することが、前記均質前駆体溶液中の硝酸塩物質及び酢酸塩物質の量、溶液前駆体の化学的性質、又は前記マイクロ波生成プラズマ内での前記液滴の前記滞留時間のうちの少なくとも1つを制御することを含む、請求項9に記載の方法。
- 前記リチウム含有粒子の前記化学組成を制御することが、前記前駆体溶液中の前記出発物質の割合を制御することを含む、請求項9に記載の方法。
- 前記リチウムイオン粒子の前記粒子径を制御することが、前記前駆体溶液の前記液滴の前記液滴サイズを制御すること、又は前記前駆体溶液中の出発物質の濃度を制御することのうちの少なくとも1つを含む、請求項9に記載の方法。
- 制御されたサイズを有する液滴を生成することが、異なる径を有する液滴の2つ以上の流れを生成することを含む、請求項9に記載の方法。
- 前記液滴の2つ以上の流れが、前記液滴生成器の異なるノズル又は開口部を用いて生成される、請求項14に記載の方法。
- 前記リチウムイオン粒子の前記化学組成を調製することが:
前記均質前駆体溶液を形成する前に前記リチウムイオン粒子の所望される化学組成を決定すること;及び
前記リチウムイオン粒子の前記所望される化学組成に基づいて前記出発物質の化学量論的割合を算出すること
を含む、請求項9に記載の方法。 - 式LiNixMnyCozO2で表され、式中、x≧0、y≧0、z≧0、及びx+y+z=1であるリチウム含有粒子を製造するための方法であって、前記方法は:
リチウム塩、ニッケル塩、マンガン塩、及びコバルト塩の組み合わせを溶媒中に溶解して均質前駆体溶液を形成すること;
液滴生成器を用いて、制御されたサイズを有する前記均質前駆体溶液の液滴を生成すること;
前記液滴をマイクロ波生成プラズマ中に導入すること;
前記マイクロ波生成プラズマからミクロン又はサブミクロンスケールのLiNixMnyCozO2の粒子を作製すること;並びに
LiNixMnyCozO2の前記粒子を捕集すること
を含む、方法。 - 制御されたサイズを有する液滴を生成することが、LiNixMnyCozO2の前記粒子に多峰性の粒度分布を発生させる目的で、異なる径を有する液滴の2つ以上の流れを生成することを含む、請求項17に記載の方法。
- 式LiNixCoyAlzO2で表され、式中、x=約0.8、y=約0.15、z=約0.05であるリチウム含有粒子を製造するための方法であって、前記方法は:
リチウム塩、ニッケル塩、コバルト塩、及びアルミニウム塩の組み合わせを溶媒中に溶
解して均質前駆体溶液を形成すること;
液滴生成器を用いて、均一なサイズの前記均質前駆体溶液の液滴を生成すること;
前記均一なサイズの液滴をマイクロ波生成プラズマ中に導入すること;
前記マイクロ波生成プラズマからミクロン又はサブミクロンスケールのLiNixCoyAlzO2の粒子を作製すること;並びに
LiNixCoyAlzO2の前記粒子を捕集すること
を含む、方法。 - 制御されたサイズを有する液滴を生成することが、LiNixCoyAlzO2の前記粒子に多峰性の粒度分布を発生させる目的で、異なる径を有する液滴の2つ以上の流れを生成することを含む、請求項19に記載の方法。
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CN109562342A (zh) | 2019-04-02 |
JP2023112094A (ja) | 2023-08-10 |
WO2017223482A1 (en) | 2017-12-28 |
EP3474978B1 (en) | 2021-10-13 |
HUE056425T2 (hu) | 2022-02-28 |
CN109562342B (zh) | 2022-08-12 |
EP3474978A4 (en) | 2020-03-04 |
EP3984629A1 (en) | 2022-04-20 |
US20210367264A1 (en) | 2021-11-25 |
US20170373344A1 (en) | 2017-12-28 |
JP7303281B2 (ja) | 2023-07-04 |
CN115215387A (zh) | 2022-10-21 |
ES2899399T3 (es) | 2022-03-11 |
JP2019522319A (ja) | 2019-08-08 |
PL3474978T3 (pl) | 2022-01-31 |
EP3474978A1 (en) | 2019-05-01 |
JP6991165B2 (ja) | 2022-01-12 |
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