JP6114873B2 - 酸化ポリオキソアニオン塩の析出を介した無機基材上の酸化物シェルの形成 - Google Patents
酸化ポリオキソアニオン塩の析出を介した無機基材上の酸化物シェルの形成 Download PDFInfo
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- JP6114873B2 JP6114873B2 JP2016500026A JP2016500026A JP6114873B2 JP 6114873 B2 JP6114873 B2 JP 6114873B2 JP 2016500026 A JP2016500026 A JP 2016500026A JP 2016500026 A JP2016500026 A JP 2016500026A JP 6114873 B2 JP6114873 B2 JP 6114873B2
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- Prior art keywords
- oxide
- inorganic substrate
- shell
- ceramic
- polyoxoanion
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- 239000000758 substrate Substances 0.000 title claims description 83
- 230000015572 biosynthetic process Effects 0.000 title description 24
- 238000001556 precipitation Methods 0.000 title description 4
- 150000003839 salts Chemical class 0.000 title description 4
- 239000000919 ceramic Substances 0.000 claims description 80
- 238000000034 method Methods 0.000 claims description 60
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 59
- 239000000203 mixture Substances 0.000 claims description 46
- 229910001416 lithium ion Inorganic materials 0.000 claims description 44
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 44
- 238000000576 coating method Methods 0.000 claims description 39
- 239000011248 coating agent Substances 0.000 claims description 36
- -1 metalloid ions Chemical class 0.000 claims description 34
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 25
- 229910010293 ceramic material Inorganic materials 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 239000004065 semiconductor Substances 0.000 claims description 17
- 125000005207 tetraalkylammonium group Chemical group 0.000 claims description 17
- 239000010406 cathode material Substances 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- 238000000151 deposition Methods 0.000 claims description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000007529 inorganic bases Chemical class 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 6
- 150000003624 transition metals Chemical class 0.000 claims description 6
- 229910052787 antimony Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- 229910052745 lead Inorganic materials 0.000 claims description 5
- 229910052716 thallium Inorganic materials 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052752 metalloid Inorganic materials 0.000 claims description 4
- 150000001450 anions Chemical class 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000013460 polyoxometalate Substances 0.000 claims description 3
- 229910001428 transition metal ion Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 41
- 239000000243 solution Substances 0.000 description 41
- 239000000843 powder Substances 0.000 description 30
- 229910013562 LiCo0.2Ni0.8O2 Inorganic materials 0.000 description 25
- 238000002441 X-ray diffraction Methods 0.000 description 24
- 238000005755 formation reaction Methods 0.000 description 23
- 239000011258 core-shell material Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000008367 deionised water Substances 0.000 description 20
- 229910021641 deionized water Inorganic materials 0.000 description 20
- 238000001878 scanning electron micrograph Methods 0.000 description 17
- 239000013078 crystal Substances 0.000 description 16
- 229910010272 inorganic material Inorganic materials 0.000 description 15
- 239000011147 inorganic material Substances 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000001000 micrograph Methods 0.000 description 12
- 239000011572 manganese Substances 0.000 description 11
- QTHKJEYUQSLYTH-UHFFFAOYSA-N [Co]=O.[Ni].[Li] Chemical compound [Co]=O.[Ni].[Li] QTHKJEYUQSLYTH-UHFFFAOYSA-N 0.000 description 10
- 150000004706 metal oxides Chemical class 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 229910044991 metal oxide Inorganic materials 0.000 description 9
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 8
- 125000004429 atom Chemical group 0.000 description 8
- 125000001453 quaternary ammonium group Chemical group 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 235000012431 wafers Nutrition 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 229910013716 LiNi Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 150000004645 aluminates Chemical class 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 229910002102 lithium manganese oxide Inorganic materials 0.000 description 4
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 description 4
- 150000002738 metalloids Chemical class 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 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 3
- 239000006182 cathode active material Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 description 2
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 2
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 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 1
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 1
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- 229910013733 LiCo Inorganic materials 0.000 description 1
- 229910013859 LiCo0.8Mn0.2O2 Inorganic materials 0.000 description 1
- 229910011281 LiCoPO 4 Inorganic materials 0.000 description 1
- 229910010586 LiFeO 2 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015118 LiMO Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910002992 LiNi0.33Mn0.33Co0.33O2 Inorganic materials 0.000 description 1
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 1
- 229910015915 LiNi0.8Co0.2O2 Inorganic materials 0.000 description 1
- 229910015973 LiNi0.8Mn0.2O2 Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910016398 Mn0.75Ni0.25CO3 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- OZWWSDWGYVJIFD-UHFFFAOYSA-N [B]=O.[Co].[Ni].[Li] Chemical compound [B]=O.[Co].[Ni].[Li] OZWWSDWGYVJIFD-UHFFFAOYSA-N 0.000 description 1
- OGCCXYAKZKSSGZ-UHFFFAOYSA-N [Ni]=O.[Mn].[Li] Chemical compound [Ni]=O.[Mn].[Li] OGCCXYAKZKSSGZ-UHFFFAOYSA-N 0.000 description 1
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 1
- JKLVRIRNLLAISP-UHFFFAOYSA-N [O-2].[V+5].[Cu+2] Chemical compound [O-2].[V+5].[Cu+2] JKLVRIRNLLAISP-UHFFFAOYSA-N 0.000 description 1
- FBDMJGHBCPNRGF-UHFFFAOYSA-M [OH-].[Li+].[O-2].[Mn+2] Chemical compound [OH-].[Li+].[O-2].[Mn+2] FBDMJGHBCPNRGF-UHFFFAOYSA-M 0.000 description 1
- KSYAOSNGZXXRMX-UHFFFAOYSA-N [Sn]=O.[Co].[Ni].[Li] Chemical compound [Sn]=O.[Co].[Ni].[Li] KSYAOSNGZXXRMX-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- BVPMZCWLVVIHKO-UHFFFAOYSA-N lithium cobalt(2+) manganese(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Co+2].[Li+] BVPMZCWLVVIHKO-UHFFFAOYSA-N 0.000 description 1
- CASZBAVUIZZLOB-UHFFFAOYSA-N lithium iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Li+] CASZBAVUIZZLOB-UHFFFAOYSA-N 0.000 description 1
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 description 1
- SBWRUMICILYTAT-UHFFFAOYSA-K lithium;cobalt(2+);phosphate Chemical compound [Li+].[Co+2].[O-]P([O-])([O-])=O SBWRUMICILYTAT-UHFFFAOYSA-K 0.000 description 1
- VGYDTVNNDKLMHX-UHFFFAOYSA-N lithium;manganese;nickel;oxocobalt Chemical compound [Li].[Mn].[Ni].[Co]=O VGYDTVNNDKLMHX-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- ZWEKKXQMUMQWRN-UHFFFAOYSA-J manganese(2+);nickel(2+);dicarbonate Chemical compound [Mn+2].[Ni+2].[O-]C([O-])=O.[O-]C([O-])=O ZWEKKXQMUMQWRN-UHFFFAOYSA-J 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- FUHNYNGYWNVWOA-UHFFFAOYSA-H trivanadate Chemical compound O[V](O)O[V](O)(O)O[V](O)O FUHNYNGYWNVWOA-UHFFFAOYSA-H 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1229—Composition of the substrate
- C23C18/1245—Inorganic substrates other than metallic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
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- C—CHEMISTRY; METALLURGY
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Description
テトラアルキルアンモニウムポリオキソアニオンおよび過酸化水素を含有する水性組成物を提供する工程;
該水性組成物を無機基材に、該無機基材の表面に該ポリオキソアニオンから誘導された水酸化物を析出させるに充分な時間接触させて、初期コートされた無機基材を形成する工程;ならびに
該初期コートされた無機基材を、該水酸化物を酸化物に変換するに充分な時間加熱して該無機基材上に該ポリオキソアニオンから誘導された酸化物コーティングを形成する工程;
を包含する、方法に関する。
であって、
テトラアルキルアンモニウムアルミネートおよび過酸化水素を含有する水性組成物を提供する工程;
該水性組成物を無機基材に、該無機基材の表面に水酸化アルミニウムを析出させるに充分な時間接触させて、初期コートされた無機基材を形成する工程;ならびに
該初期コートされた無機基材を、該水酸化アルミニウムをアルミナに変換するに充分な時間加熱する工程;
を包含する、方法に関する。
リチウムニッケルマンガンコバルト酸化物、LiNi0.33Mn0.33Co0.33O2
リチウムニッケルコバルトアルミニウム酸化物、LiNi0.8Co0.15Al0.05O2
リチウムニッケルコバルトアルミニウム酸化物、LiNi0.79Co0.20Al0.01O2
リチウムニッケルコバルト酸化物、LiNi0.8Co0.2O2
リチウム鉄リン酸塩、LiFePO4
リチウムニッケル酸化物、LiNiO2
リチウム三バナジウム酸塩、LiV3O8
マンガンニッケル炭酸塩;Mn0.75Ni0.25CO3
銅バナジウム酸化物、CuV2O6
リチウムコバルトリン酸塩、LiCoPO4
リチウムマンガン二酸化物、LiMnO2
リチウムマンガン酸化物、LiMn2O4
リチウムマンガンニッケル酸化物、Li2Mn3NiO8
リチウム鉄酸化物、LiFeO2
リチウムコバルト酸化物、LiCoO2
リチウムモリブデン酸塩、LiMoO4
リチウムチタン酸塩、Li2TiO3
リチウムコバルトマンガン酸化物、LiCo0.8Mn0.2O2
リチウムニッケルマンガン酸化物、LiNi0.85Mn0.15O2
リチウムコバルトニッケルマンガン酸化物、LiCo0.45Ni0.45Mn0.10O2
リチウムニッケルマンガン酸化物、LiNi0.8Mn0.2O2
リチウムニッケルコバルトホウ素酸化物、LiNi0.79Co0.2B0.01O2
リチウムニッケルコバルト錫酸化物、LiNi0.79Co0.2Sn0.01O2
リチウムニッケルコバルトアルミニウム酸化物、LiNi0.72Co0.2B0.08O2。
マグネチックスターラーバーを備える200mlのフラスコに、37.51g(0.1モル)の硝酸アルミニウム九水和物および200gの脱イオン水を添加する。透明な溶液を形成するまで溶液を撹拌する。この溶液に、114.04g(0.3モル)の23.98重量%水酸化テトラメチルアンモニウム(TMAH)溶液をゆっくりと添加する。白色沈殿が直ちに生じる。得られた白色沈殿を濾過し、そして200mlの脱イオン水で3回すすぐ。得られた白色固体を凍結乾燥して、乾燥水酸化アルミニウムを得る。
100mlのプラスチックビーカーに、0.0594gの0.311mmol/gのTMAアルミネート、40gの脱イオン水および0.0594gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約3μmを有する0.5gのLiCo0.2Ni0.8O2を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱し、本発明の実施形態にしたがって、コア−シェル構造のセラミック粉末を得る。得られた生成物のXRDパターンを図2に示し、SEM顕微鏡写真を図7に示す。
100mlのプラスチックビーカーに、0.594gの0.311mmol/gのTMAアルミネート、40gの脱イオン水および0.594gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約3μmを有する0.5gのLiCo0.2Ni0.8O2を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱する。本発明の実施形態にしたがって、得られた生成物のXRDパターンを図3に示し、SEM顕微鏡写真を図8に示す。
100mlのプラスチックビーカーに、1.188gの0.311mmol/gのTMAアルミネート、40gの脱イオン水および1.188gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約3μmを有する0.5gのLiCo0.2Ni0.8O2を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱する。本発明の実施形態にしたがって、得られた生成物のXRDパターンを図4に示し、SEM顕微鏡写真を図9に示す。
100mlのプラスチックビーカーに、1.782gの0.311mmol/gのTMAアルミネート、40gの脱イオン水および1.50gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約3μmを有する0.5gのLiCo0.2Ni0.8O2を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱する。本発明の実施形態にしたがって、得られた生成物のXRDパターンを図5に示し、SEM顕微鏡写真を図10に示す。
この実験を用いて、反応混合物中のTMAHの存在のシェル形成に対する影響を測定する。
本実験を、コア−シェル構造の形成のための酸化剤(本実施例におけるH2O2)の重要性を示すために用いる。
LiCo0.2Ni0.8O2セラミック粒子のXRDパターンおよびSEM顕微鏡写真を図1および図6にそれぞれ示す。実施例1〜4は、コアとしてLiCo0.2Ni0.8O2セラミック粒子を用い、かつシェルとしてAl2O3を用いる、本発明によるコア−シェル構造の調製のための詳細な方法を記載する。コア−シェル構造を、テトラメチルアンモニウムアルミネートおよび過酸化水素を含有する水性溶液中でLiCo0.2Ni0.8O2セラミック粒子を懸濁することにより調製する。処方溶液は、調製された際にいくつか少量の気泡を発生させたが、セラミック粒子を溶液中に添加するにつれて多数の気泡が発生する。これは、本発明の反応順序におけるH2O2の崩壊を示す化学式において上述したように、表面を触媒したH2O2の分解に相当する。LiCo0.2Ni0.8O2セラミック粉末は、シェル調製のために処方溶液に充填する前に乳鉢と乳棒で注意深く粉砕され、その結果、セラミック粒子間の機械的接着がなくかつすべての粒子の表面がシェルによって覆われるようにすることができる。シェル形成プロセス後、遠心分離機により単離されるセラミック粉末は、粒子を再び凝集する傾向にある。しかし、凝集したセラミック粒子はすでにシェルでコートされている。
(実施例7(CS3P151)推定20nm二酸化ケイ素シェルを有するリチウムニッケルコバルト酸化物LiCo0.2Ni0.8O2のコア−シェル構造の調製)
100mlのプラスチックビーカーに、0.0496gの12.6重量%TMAシリケート、40gの脱イオン水および1.5gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約3μmを有する0.5gのLiCo0.2Ni0.8O2を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱し、本発明のコア−シェル構造セラミック粉末を製造する。SEM顕微鏡写真を図19に示す。
100mlのプラスチックビーカーに、0.0496gの12.6重量%TMAシリケート、40gの脱イオン水および1.5gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約1〜2μmを有する0.5gのLiMn2O4を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱し、本発明のコア−シェル構造セラミック粉末を得る。純粋なLiMn2O4のXRDを図20に示し、そしてLiMn2O4のSEM顕微鏡写真を図21に示す。調製したようなコア−シェルLiMn2O4のSEM顕微鏡写真を図22に示す。
100mlのプラスチックビーカーに、3.0gの0.311mmol/gTMAアルミネート、40gの脱イオン水および1.5gの30重量%過酸化水素を添加する。溶液の全重量を追加の脱イオン水を添加することにより50gにまで上げる。こうして調製した溶液に、平均結晶粒子サイズ約1〜2μmを有する0.5gのLiMn2O4を添加する。混合物を激しく一晩振盪し、次いで、セラミック粉末を遠心分離機により単離する。回収したセラミック粉末をオーブン内に配置し、そして500℃で5時間加熱し、コア−シェル構造セラミック粉末を得る。SEM顕微鏡写真を図23に示す。
Claims (15)
- 無機基材上に酸化物コーティングを析出させるための方法であって、
テトラアルキルアンモニウムポリオキソアニオンおよび過酸化水素を含有する水性組成物を提供する工程;
該水性組成物を無機基材に、該無機基材の表面に該ポリオキソアニオンから誘導された水酸化物を析出させるに充分な時間接触させて、初期コートされた無機基材を形成する工程;ならびに
該初期コートされた無機基材を、該水酸化物を酸化物に変換するに充分な時間加熱して該無機基材上に該ポリオキソアニオンから誘導された酸化物コーティングを形成する工程;
を包含し、
ここで、該テトラアルキルアンモニウムポリオキソアニオンが、C 1 〜C 8 の分岐または非分岐アルキル基から独立して選択されるアルキル基と一般式AxOy Z−を有するポリオキソアニオンとを含み、ここで、Aは、遷移金属のイオン、もしくはAl、Si、B、Ga、Ge、As、In、Sn、Sb、Tl、PbおよびBiから選択される金属または半金属のイオン、あるいはそれらの任意の2またはそれ以上の組合せを表し、Oは酸素イオンであり、そしてx、yおよびzの値は該ポリオキソアニオン中のAの原子価およびy>xに依存し;そして
該過酸化水素が、該水性組成物の全量に基づいて0.02重量%から1重量%の範囲の濃度で存在する、方法。 - 前記提供工程において、前記テトラアルキルアンモニウムポリオキソアニオンが、水酸化テトラメチルアンモニウムから調製される、請求項1に記載の方法。
- 前記遷移金属が、Ti、V、Zn、Ni、Co、Mn、FeおよびCuの1つまたはそれ以上を含む、請求項1に記載の方法。
- 前記無機基材がセラミック酸化物を含む、請求項1から3のいずれかに記載の方法。
- 前記セラミック酸化物が、Li+イオンを含み、そしてリチウムイオン電池セラミックカソード材料における使用のために適合する、請求項4に記載の方法。
- 前記無機基材が半導体材料を含む、請求項1から4のいずれかに記載の方法。
- 前記半導体材料が半導体ウェハを含み、ここで、必要に応じて該半導体ウェハは電子回路部品を含む、請求項6に記載の方法。
- 前記テトラアルキルアンモニウムポリオキソアニオンがテトラメチルアンモニウムアルミネートであり、そして前記無機基材がセラミック材料である、請求項1から7のいずれかに記載の方法。
- 前記セラミック材料がリチウムイオン電池カソード材料である、請求項8に記載の方法。
- 無機基材上にアルミナコーティングを析出させるための方法であって、
テトラアルキルアンモニウムアルミネートおよび過酸化水素を含有する水性組成物を提供する工程;
該水性組成物を無機基材に、該無機基材の表面に水酸化アルミニウムを析出させるに充分な時間接触させて、初期コートされた無機基材を形成する工程;ならびに
該初期コートされた無機基材を、該水酸化アルミニウムをアルミナに変換するに充分な時間加熱する工程;
を包含し、
該テトラアルキルアンモニウムアルミネートが、C 1 〜C 8 の分岐または非分岐アルキル基から独立して選択されるアルキル基を含む、方法。 - 前記無機基材がセラミック材料である、請求項10に記載の方法。
- 前記セラミック材料がリチウムイオン電池カソード材料である、請求項11に記載の方法。
- 前記テトラアルキルアンモニウムアルミネートがテトラメチルアンモニウムアルミネートである、請求項10から12のいずれかに記載の方法。
- 前記加熱工程が、450℃から1000℃の範囲の温度、または500℃の温度で行われる、請求項1から13のいずれかに記載の方法。
- 前記水性組成物がさらにリチウムイオンを含む、請求項1から9のいずれかに記載の方法。
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WO2014142802A1 (en) | 2014-09-18 |
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