JP6069482B2 - 金属ドープされた酸化ニッケル活性材料を作製する方法 - Google Patents
金属ドープされた酸化ニッケル活性材料を作製する方法 Download PDFInfo
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- JP6069482B2 JP6069482B2 JP2015501900A JP2015501900A JP6069482B2 JP 6069482 B2 JP6069482 B2 JP 6069482B2 JP 2015501900 A JP2015501900 A JP 2015501900A JP 2015501900 A JP2015501900 A JP 2015501900A JP 6069482 B2 JP6069482 B2 JP 6069482B2
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- Prior art keywords
- nickel
- metal
- oxide
- cobalt
- doped
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- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims description 181
- 229910000480 nickel oxide Inorganic materials 0.000 title claims description 107
- 239000002184 metal Substances 0.000 title claims description 96
- 229910052751 metal Inorganic materials 0.000 title claims description 95
- 238000000034 method Methods 0.000 title claims description 38
- 239000011149 active material Substances 0.000 title description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 172
- 239000011777 magnesium Substances 0.000 claims description 74
- 239000000203 mixture Substances 0.000 claims description 74
- 230000002950 deficient Effects 0.000 claims description 64
- 239000003513 alkali Substances 0.000 claims description 62
- 239000000843 powder Substances 0.000 claims description 49
- 229910000483 nickel oxide hydroxide Inorganic materials 0.000 claims description 41
- 229910052782 aluminium Inorganic materials 0.000 claims description 39
- 229910052759 nickel Inorganic materials 0.000 claims description 36
- 229910052749 magnesium Inorganic materials 0.000 claims description 34
- 239000002243 precursor Substances 0.000 claims description 31
- -1 cobalt oxyhydroxide Chemical compound 0.000 claims description 30
- 239000002019 doping agent Substances 0.000 claims description 29
- 229910052760 oxygen Inorganic materials 0.000 claims description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 28
- 239000001301 oxygen Substances 0.000 claims description 28
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 26
- 229910017052 cobalt Inorganic materials 0.000 claims description 25
- 239000010941 cobalt Substances 0.000 claims description 25
- 150000001875 compounds Chemical class 0.000 claims description 25
- 239000006182 cathode active material Substances 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 19
- 239000011575 calcium Substances 0.000 claims description 18
- 239000011572 manganese Substances 0.000 claims description 18
- OSOVKCSKTAIGGF-UHFFFAOYSA-N [Ni].OOO Chemical compound [Ni].OOO OSOVKCSKTAIGGF-UHFFFAOYSA-N 0.000 claims description 17
- 229910052783 alkali metal Inorganic materials 0.000 claims description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 16
- 150000001340 alkali metals Chemical class 0.000 claims description 16
- 229910052755 nonmetal Inorganic materials 0.000 claims description 16
- 229910052791 calcium Inorganic materials 0.000 claims description 13
- 229910052748 manganese Inorganic materials 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 8
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 claims description 8
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 6
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 229910001868 water Inorganic materials 0.000 claims description 5
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims description 4
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 4
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 4
- 229910052732 germanium Inorganic materials 0.000 claims description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011656 manganese carbonate Substances 0.000 claims description 4
- 235000006748 manganese carbonate Nutrition 0.000 claims description 4
- 229940093474 manganese carbonate Drugs 0.000 claims description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 4
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 4
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229940119177 germanium dioxide Drugs 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 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 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 3
- 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 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 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
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 68
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 59
- 229910052744 lithium Inorganic materials 0.000 description 55
- 239000011701 zinc Substances 0.000 description 54
- 229910052725 zinc Inorganic materials 0.000 description 52
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 42
- BAPRMBRFVUJBEI-UHFFFAOYSA-N [O].[O].[Ni] Chemical compound [O].[O].[Ni] BAPRMBRFVUJBEI-UHFFFAOYSA-N 0.000 description 37
- 239000010410 layer Substances 0.000 description 33
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 30
- 230000003647 oxidation Effects 0.000 description 28
- 238000007254 oxidation reaction Methods 0.000 description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 26
- 150000002500 ions Chemical class 0.000 description 24
- 229910002804 graphite Inorganic materials 0.000 description 22
- 239000010439 graphite Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 20
- 238000003860 storage Methods 0.000 description 19
- 229940021013 electrolyte solution Drugs 0.000 description 18
- 230000014759 maintenance of location Effects 0.000 description 18
- 239000008151 electrolyte solution Substances 0.000 description 17
- 238000010306 acid treatment Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 229910013716 LiNi Inorganic materials 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 150000002641 lithium Chemical class 0.000 description 15
- 239000007787 solid Substances 0.000 description 15
- ZQQGQJKVMMDIKF-UHFFFAOYSA-N [Ni+4] Chemical compound [Ni+4] ZQQGQJKVMMDIKF-UHFFFAOYSA-N 0.000 description 14
- 239000013078 crystal Substances 0.000 description 14
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 13
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 13
- 229910001882 dioxygen Inorganic materials 0.000 description 13
- 229910001416 lithium ion Inorganic materials 0.000 description 13
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 13
- 230000008569 process Effects 0.000 description 13
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 12
- 239000002253 acid Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 11
- 229910021645 metal ion Inorganic materials 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 238000000634 powder X-ray diffraction Methods 0.000 description 10
- 229910001297 Zn alloy Inorganic materials 0.000 description 9
- 238000009826 distribution Methods 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 239000011148 porous material Substances 0.000 description 8
- 229910001413 alkali metal ion Inorganic materials 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 229910052723 transition metal Inorganic materials 0.000 description 7
- 150000003624 transition metals Chemical class 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229920000298 Cellophane Polymers 0.000 description 5
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical group [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- 239000002134 carbon nanofiber Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000002482 conductive additive Substances 0.000 description 5
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 description 5
- 239000003349 gelling agent Substances 0.000 description 5
- 238000007429 general method Methods 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 description 5
- 229910001453 nickel ion Inorganic materials 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 230000036961 partial effect Effects 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000007323 disproportionation reaction Methods 0.000 description 4
- 238000002309 gasification Methods 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 239000010954 inorganic particle Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000004584 polyacrylic acid Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910017018 Ni0.8Co0.15Al0.05 Inorganic materials 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 229920002134 Carboxymethyl cellulose Chemical class 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 2
- 238000005169 Debye-Scherrer Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Chemical class 0.000 description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 2
- 239000008112 carboxymethyl-cellulose Chemical class 0.000 description 2
- 229940105329 carboxymethylcellulose Drugs 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000011263 electroactive material Substances 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 238000010316 high energy milling Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000002563 ionic surfactant Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000011255 nonaqueous electrolyte Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
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Description
LixNi(IV)1−xNi(III)xO2+H2O→Ni(II)(OH)2+x Li++1/2 O2 (1)
2LiNi+3O2+4H+→Ni+4O2+Ni+2+2Li++2H2O (2)
LiNi+3O2+H2O→HxLi(1−x)Ni+3O2+xLiOH (3)
化学量論的ニッケル酸リチウム、LiNiO2を、93.91gの商用の球状β−オキシ水酸化ニッケル粉末(例えば、β−NiOOH、Kansai Catalyst Co.)及び42.97gの一水化水酸化リチウム(LiOH・H2O、Aldrich Chemical)を配合し、混合物を酸素ガス流下で、チューブ炉内において約210℃で約20時間、加熱することによって合成した。加熱した混合物を、周囲室温まで炉冷させ、すり鉢とすりこぎとで挽き、酸素ガス流下で更に48時間800℃にて再加熱した。最終反応生成物のX線粉末回析パターンは、例えば、米国特許第5,720,932号、J.Maruta et al.(Journal of Power Sources,2000,90,89〜94)、及びY.Sun et al.(Solid State Ionics,2006,177,1173〜7)に説明されるような、化学量論的LiNiO2(例えば、ICDD PDF No.09−0063)に関して報告されたものに厳密に対応した。
実施例1のニッケル酸リチウムを、本明細書にその全体が援用される米国出願番号第12/722,669号の実施例1に開示されるプロセスと同様の低温酸処理プロセスによって、脱リチウム化した。具体的には、約100gのLiNiO2を、0〜5℃の間に冷却した1.5Lの高速攪拌した水性6M H2SO4溶液に添加した。得られたスラリーを、攪拌し、約2℃で約20時間(実施例2a)か又は40時間(実施例2b)かのいずれかで維持する。次に、懸濁した固体を沈殿させ、上澄み液をデカンテーションによって除去し、上澄みのpHがほぼ中性(即ち、pH約6〜7)になるまで、固体を脱イオン水のアリコートで洗浄した。固体を、加圧濾過かまたは真空濾過かのいずれかによって収集し、約80℃で約24時間、空気乾燥した。乾燥させた脱リチウム化されたLixNiO2生成物の残留リチウム含量は、ICP分光法によって、x=0.31に相当する2.2重量% Li未満(実施例2a)、及びx=0.06に相当する0.4重量% Li超(実施例2b)と決定された。脱リチウム化された生成物のX線粉末回析パターンは、より高い2θ角度への回析ピーク位置の予想された移動を伴う、化学量論的LiNiO2のパターンに類似した。脱リチウム化されたLixNiO2粉末の平均粒径は、約1〜8μmの範囲であり、B.E.T.比表面積は、約1.36m2/gであった。LixNiO2粉末の真密度は、Heピクノメータによって4.70g/cm3と測定された。
図2の三成分組成図に示される金属ドープされたLi(Ni1−y−zCoyAlz)O2及びLi(Ni1−y−zCoyMgz)O2系を、合成し、脱リチウム化し、対応する脱リチウム化された(即ち、リチウム欠損)金属ドープされた酸化ニッケル活性材料の性能に関して、酸素ガス発生、初期開路電圧(OCV)、出来立て時(即ち、24時間)放電容量、並びに周囲室温及び高温で保管した後の容量保持率について評価した。
実施例3a〜nの金属ドープされたニッケル酸リチウムLiNi1−y−zCoyMa zO2(M=Mg、Al)のそれぞれ10.0g部分を、別々の6M H2SO4溶液の150mLアリコート中で同時に攪拌し、約0℃(例えば、2〜5℃)で20時間、それぞれの別の部を40時間保った。脱リチウム化された固体を、濾過によって収集し洗浄液が公称の中性pHを有するまで脱イオン水で洗浄し、80℃で空気乾燥させた。実施例4a〜nの脱リチウム化された粉末は、次の公称のNi:Co:M金属原子比を有する:実施例4a 0.96:0.04:0;4b 0.92:0.08:0;4c 0.88:0.12:0;4d−1(M=Mg)、4d−2(M=Al)0.98:0:0.2;4e−1(M=Mg)、4e−2(M=Al)0.96:0:0.04;4f−1(M=Mg)、4f−2(M=Al)0.92:0:0.08;4g−1(M=Mg)、4g−2(M=Al)0.96:0.02:0.02;4h−1(M=Mg)、4h−2(M=Al)0.92:0.06:0.02;4i−1(M=Mg)、4i−2(M=Al)0.92:0.04:0.04;4j−1(M=Mg)、4j−2(M=Al)0.92:0.02:0.06;4k−1(M=Mg)、4k−2(M=Al)0.88:0.10:0.02;4l−1(M=Mg)、4l−2(M=Al)0.88:0.08:0.04;4m−1(M=Mg)、4m−2(M=Al)0.88:0.06:0.06;4n−1(M=Mg)、4n−2(M=Al)0.88:0.04:0.08。乾燥させた固体のX線粉末回析パターンを、Cu Kα線を用いて測定した。実施例4a〜nの選択された脱リチウム化された粉末の試料の熱安定性を、DSCによって決定した。残留リチウムの量を、実施例4a〜n選択された脱リチウム化された粉末の試料に関してICP−EAによって決定し、表1に示す。
球状オキシ水酸化コバルトでコーティングされたβ−オキシ水酸化ニッケル粉末の試料を、例えば、米国特許出願第8,043,748号に開示されるような一般的な方法によって開示される通り、商用の球状β−水酸化ニッケル(例えば、Kansai Catalyst Co.,Ltd.,Osaka,Japan)から調製した。
公称組成LiNi0.8Co0.15Al0.05O2及びLi(Ni0.8Co0.15Al0.05)0.99B0.01O2(即ち、LiNi0.792Co0.149Al0.049B0.01O2)を有する商用のリチウムニッケルコバルトアルミニウム酸化物粉末(Toda America Inc.,Battle Creek,MI)の試料を、上述の実施例2の酸処理プロセスによって脱リチウム化して、それぞれ比較例2a及び2bの脱リチウム化された金属置換された酸化Ni(IV)を形成した。ボタンセルを、実施例2の一般的な方法によって製造した。比較例2のセルを、製造後24時間以内に試験した。OCV値は、約1.83〜1.85Vの範囲であった。セルを、0.8Vカットオフ電圧に対して公称C/30速度に対応する約10mA/gの一定電流にて低速で放電した。図10に、比較実施例2aの脱リチウム化された、コバルト及びアルミニウムドープされた酸化ニッケル、並びに比較実施例2bのコバルト、アルミニウム、及びホウ素ドープされた酸化ニッケルを含有するセルに関する放電曲線を、実施例2bの脱リチウム化されたLixNiO2を含有するセル、及び商用の電池グレードEMDに関するものと比較する。比較例2a及び2bの脱リチウム化されたコバルト/アルミニウム/ホウ素ドープされた酸化ニッケルを含有するセルに関する平均放電容量は、それぞれ325mAh/g及び335mAh/gであった。
公称化学組成LiNi0.9Co0.1O2及びLiNi0.8Co0.2O2を有する商用のリチウムニッケルコバルト酸化物粉末(例えば、NEI Corp.,Somerset,NJ)の試料を、上述の実施例2の酸処理プロセスによって脱リチウム化して、それぞれ比較例3a及び3bの脱リチウム化された金属ドープされた酸化ニッケル(IV)を形成した。ボタンセルを、実施例2の一般的な方法によって製造した。比較例3のセルを、製造後24時間以内に試験した。OCV値は、典型的に約1.81Vであった。セルを、0.8Vカットオフ電圧に対して公称C/30速度に対応する約10mA/gの一定電流にて低速で放電した。比較例3a及び3bの脱リチウム化されたコバルトドープされた酸化ニッケルを含有するセルに関する平均放電容量は、それぞれ355mAh/g及び335mAh/gであった。
Claims (11)
- カソード活性材料を作製する方法であって、
アルカリ含有化合物1モルあたり、0.98〜0.86モルのニッケル含有化合物と、0.02〜0.12モルの1つ以上の金属含有化合物と、0〜0.02モルの1つ以上の非金属含有化合物とを合わせて、混合物を形成する工程と、
前記混合物を、185℃と225℃との間の第1の温度にて酸素流又は酸素に富む大気内で、第1の期間にわたって加熱する工程と、
前記混合物を、少なくとも40℃まで酸素流又は酸素に富む大気内で、冷却する工程と、
前記混合物を、750℃と850℃との間の第2の温度にて酸素流又は酸素に富む大気流中で、第2の期間にわたって加熱し、ANi1−y−z−wCoyMa zMb wO2前駆体を形成する工程と、
前記ANi1−y−z−wCoyMa zMb wO2前駆体を、10℃未満の温度にて酸性水溶液で処理し、式AxNi1−y−z−wCoyMa zMb wO2を有するアルカリ金属欠損酸化ニッケルを形成する工程と、を含み、式中、Aが、アルカリ金属であり、Maが、Mg、Al、Ca、Mn、及びYからなる群から選択される金属を含む金属ドーパントであり、Mbが、B、Si、及びGeからなる群から選択される非金属を含む非金属ドーパントであり、0≦x≦0.08であり、wが0であるか、又は0≦w≦0.02であり、0.02≦y+z≦0.25である、方法。 - 前記ニッケル含有化合物が、一酸化ニッケル、三二酸化ニッケル、水酸化ニッケル、オキシ水酸化ニッケル、炭酸ニッケル、硝酸ニッケル、及びこれらの任意の組み合わせから選択される、請求項1に記載の方法。
- 前記ニッケル含有化合物が、β−オキシ水酸化ニッケル、金属ドープされたβ−オキシ水酸化ニッケル、オキシ水酸化コバルトでコーティングされたβ−オキシ水酸化ニッケル、γ−オキシ水酸化ニッケル、金属ドープされたγ−オキシ水酸化ニッケル、オキシ水酸化コバルトでコーティングされたγ−オキシ水酸化ニッケル、β−オキシ水酸化ニッケルとγ−オキシ水酸化ニッケルとの混合物、及びこれらの任意の組み合わせから選択される、請求項1に記載の方法。
- 前記金属含有化合物が、アルミニウム、マグネシウム、コバルト、マンガン金属粉末、酸化コバルト、酸化アルミニウム、酸化マグネシウム、酸化カルシウム、酸化イットリウム、酸化マンガン、水酸化コバルト、オキシ水酸化コバルト、炭酸コバルト、硝酸コバルト、水酸化アルミニウム、水酸化マグネシウム、炭酸マグネシウム、水酸化カルシウム、炭酸カルシウム、水酸化イットリウム、水酸化マンガン、炭酸マンガン、硝酸マンガン、及びこれらの任意の組み合わせからなる群から選択される、請求項1〜3のいずれか一項に記載の方法。
- 前記非金属含有化合物が、酸化ホウ素、ケイ素粉末、二酸化ケイ素、ゲルマニウム粉末、二酸化ゲルマニウム、及びこれらの任意の組み合わせからなる群から選択される、請求項1〜4のいずれか一項に記載の方法。
- 前記アルカリ含有化合物が、水酸化リチウム水和物、酸化リチウム、炭酸リチウム、硝酸リチウム、及びこれらの任意の組み合わせからなる群から選択される、請求項1〜5のいずれか一項に記載の方法。
- 前記第1の期間が、16〜20時間である、請求項1〜6のいずれか一項に記載の方法。
- 前記第2の期間が、24〜60時間である、請求項1〜7のいずれか一項に記載の方法。
- 0.02≦y≦0.15である、請求項1〜8のいずれか一項に記載の方法。
- 0.02≦z≦0.08である、請求項1〜9のいずれか一項に記載の方法。
- 0≦w≦0.02である、請求項1〜10のいずれか一項に記載の方法。
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