JP5859855B2 - 金属化合物の合成 - Google Patents
金属化合物の合成 Download PDFInfo
- Publication number
- JP5859855B2 JP5859855B2 JP2011531556A JP2011531556A JP5859855B2 JP 5859855 B2 JP5859855 B2 JP 5859855B2 JP 2011531556 A JP2011531556 A JP 2011531556A JP 2011531556 A JP2011531556 A JP 2011531556A JP 5859855 B2 JP5859855 B2 JP 5859855B2
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- JP
- Japan
- Prior art keywords
- lithium
- surfactant
- transition metal
- mesoporous
- liquid crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 230000015572 biosynthetic process Effects 0.000 title description 43
- 238000003786 synthesis reaction Methods 0.000 title description 41
- 150000002736 metal compounds Chemical class 0.000 title description 2
- 238000000034 method Methods 0.000 claims description 57
- 239000004094 surface-active agent Substances 0.000 claims description 56
- 239000004973 liquid crystal related substance Substances 0.000 claims description 50
- 229910012851 LiCoO 2 Inorganic materials 0.000 claims description 42
- 229910052744 lithium Inorganic materials 0.000 claims description 41
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 36
- 239000011541 reaction mixture Substances 0.000 claims description 32
- -1 transition metal salts Chemical class 0.000 claims description 27
- 229910052723 transition metal Inorganic materials 0.000 claims description 25
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical group [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 23
- 229910003002 lithium salt Inorganic materials 0.000 claims description 23
- 159000000002 lithium salts Chemical class 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 229910021437 lithium-transition metal oxide Inorganic materials 0.000 claims description 16
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical group [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 12
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 12
- 150000004706 metal oxides Chemical class 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002738 chelating agent Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 229910044991 metal oxide Inorganic materials 0.000 claims description 10
- 150000001868 cobalt Chemical class 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 7
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 150000003624 transition metals Chemical class 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 239000003125 aqueous solvent Substances 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- 239000012071 phase Substances 0.000 description 72
- 239000000499 gel Substances 0.000 description 49
- 239000000463 material Substances 0.000 description 33
- 239000000047 product Substances 0.000 description 29
- 239000000203 mixture Substances 0.000 description 28
- 239000000843 powder Substances 0.000 description 24
- 238000002441 X-ray diffraction Methods 0.000 description 20
- 239000011148 porous material Substances 0.000 description 15
- 239000003153 chemical reaction reagent Substances 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 235000021317 phosphate Nutrition 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 229910019142 PO4 Inorganic materials 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 239000010452 phosphate Substances 0.000 description 11
- 229910002651 NO3 Inorganic materials 0.000 description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 10
- 238000003917 TEM image Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 10
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 9
- 238000003980 solgel method Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000011572 manganese Substances 0.000 description 7
- 238000004627 transmission electron microscopy Methods 0.000 description 7
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 6
- 229910013825 LiNi0.33Co0.33Mn0.33O2 Inorganic materials 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 4
- 229910012815 LiCoNiO Inorganic materials 0.000 description 4
- 229910032387 LiCoO2 Inorganic materials 0.000 description 4
- 239000006182 cathode active material Substances 0.000 description 4
- 239000008240 homogeneous mixture Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 230000001687 destabilization Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- 150000002505 iron Chemical class 0.000 description 3
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 3
- 229940071257 lithium acetate Drugs 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 229910011157 LiMBO Inorganic materials 0.000 description 2
- 229910015868 MSiO Inorganic materials 0.000 description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- XGCTUKUCGUNZDN-UHFFFAOYSA-N [B].O=O Chemical compound [B].O=O XGCTUKUCGUNZDN-UHFFFAOYSA-N 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 150000001449 anionic compounds Chemical class 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 229940011182 cobalt acetate Drugs 0.000 description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 2
- 239000012612 commercial material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000003411 electrode reaction Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 229910001412 inorganic anion Inorganic materials 0.000 description 2
- 239000002563 ionic surfactant Substances 0.000 description 2
- 235000013490 limbo Nutrition 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 150000002891 organic anions Chemical class 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 229910000319 transition metal phosphate Inorganic materials 0.000 description 2
- FDCJDKXCCYFOCV-UHFFFAOYSA-N 1-hexadecoxyhexadecane Chemical compound CCCCCCCCCCCCCCCCOCCCCCCCCCCCCCCCC FDCJDKXCCYFOCV-UHFFFAOYSA-N 0.000 description 1
- YAMTWWUZRPSEMV-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-(2-hexadecoxyethoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCO YAMTWWUZRPSEMV-UHFFFAOYSA-N 0.000 description 1
- SOOWCACMXVNJKO-UHFFFAOYSA-L C(C(=O)[O-])(=O)[O-].[N+](=O)([O-])[O-].[Fe+3] Chemical compound C(C(=O)[O-])(=O)[O-].[N+](=O)([O-])[O-].[Fe+3] SOOWCACMXVNJKO-UHFFFAOYSA-L 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 239000004976 Lyotropic liquid crystal Substances 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 239000004990 Smectic liquid crystal Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 210000003323 beak Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229940115457 cetyldimethylethylammonium bromide Drugs 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- CKFRRHLHAJZIIN-UHFFFAOYSA-N cobalt lithium Chemical compound [Li].[Co] CKFRRHLHAJZIIN-UHFFFAOYSA-N 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000368 destabilizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- VUFOSBDICLTFMS-UHFFFAOYSA-M ethyl-hexadecyl-dimethylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CC VUFOSBDICLTFMS-UHFFFAOYSA-M 0.000 description 1
- 229960002413 ferric citrate Drugs 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- 229910001386 lithium phosphate Inorganic materials 0.000 description 1
- GQWMZSJVCWUFCR-UHFFFAOYSA-M lithium;1-dodecoxydodecane;acetate Chemical compound [Li+].CC([O-])=O.CCCCCCCCCCCCOCCCCCCCCCCCC GQWMZSJVCWUFCR-UHFFFAOYSA-M 0.000 description 1
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000012703 sol-gel precursor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- JAVMESYEMAASLS-UHFFFAOYSA-N tetraazanium dihydrogen phosphate phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].OP(O)([O-])=O.[O-]P([O-])([O-])=O JAVMESYEMAASLS-UHFFFAOYSA-N 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
Images
Classifications
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/128—Borates containing plural metal or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
-
- 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
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
-
- 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
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- H—ELECTRICITY
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Description
クエン酸Fe(III)+LiH2PO4(H3PO4及びLi3PO4から製造)、
Fe(NO3)3・9H2O+NH4H2PO4+LiNO3+クエン酸
である。
液晶相がゾル−ゲル合成の実質的にすべての間、すなわち本発明の方法のステップ(i)及び(ii)の間60〜80℃のゾル−ゲル温度範囲で安定のままであることが望ましい。その目的を達するために、好ましいヘキサゴナル(H1)液晶相の安定を2つのゾル−ゲル試薬系(酢酸リチウム/酢酸コバルト及び硝酸リチウム/硝酸コバルト)の存在下で典型的なゾル−ゲル反応温度で2つの適している界面活性剤を用いて研究した。
市販のLiCoO2は供給業者(Pred Materials,電池グレード)から黒色微粉として受け取り、XRD分析、TEM及びBET表面積分析により調べられた。XRD分析用サンプルは、まず乳棒及び乳鉢を用いて微粉に粉砕することにより調製した。TEMサンプルは、電子ビームが透過するのに十分な薄さの断片が得られるようにエタノール中で数時間超音波処理にかけた後粉末断片として調べた。BET測定は供給業者から受け取ったままの粉末に対して実施した。
LiCoO2の非テンプレート化ゾル−ゲル合成を対照実験として実施した。紫〜ピンク色の外皮のあるゲルが形成されるまで、硝酸リチウム(Suprapur,Merck Chemicals International)、硝酸コバルト(Suprapur,Merck Chemicals International)及びクエン酸(Puriss Grade,Fluka Chemie AG)の水溶液を開放溶液中で連続攪拌しながら70〜80℃に加熱した。次いで、ゲルを75℃で数時間保持した後、放冷した。生成物を微粉に粉砕した後、650〜700℃の温度で16時間焼成した。暗灰色〜黒色粉末が形成された。市販のコバルト酸リチウムの特性決定に関して上に概説した方法を用いてXRD、BET及びTEMにより生成物の特性を決定した。
LiCoO2のテンプレート化ゾル−ゲル合成を本発明に従って実施した。硝酸リチウム、硝酸コバルト及びクエン酸の水溶液を開放容器中で連続攪拌しながら55〜60℃に加熱した。溶液を更に10時間攪拌して均質混合物を得た後、100mlのBrij(登録商標)56(Sigma Aldrich Inc.)界面活性剤の溶融溶液を40℃で添加した。次いで、ヘキサゴナル液晶相が形成されるまで混合物を攪拌した。次いで、粘性ペーストのコンシステンシーを有する液晶相混合物を密封サンプルボトルに移し、60℃に加熱した。ここで、混合物は粘性液体であり、これを明紫色から暗紫色に変化するまで60℃で更に24〜36時間攪拌した。次いで、加熱を数時間続け、溶液をアルミナるつぼに移し、そこで放冷した。次いで、冷却した固体/ゲルを炉に移して600〜650℃で16時間一定加熱した。液晶のヘキサゴナル相を破壊し、よって孔構造形態の崩壊を導く水分損失が観察されたので、テンプレート化ゾル−ゲル合成を密封容器中で実施した。
LiNi0.33Co0.33Mn0.33O2のテンプレート化ゾル−ゲル合成を本発明に従って実施した。硝酸リチウム、硝酸コバルト、硝酸ニッケル、硝酸マンガン(1:0.33:0.33:0.33のモル比)及びクエン酸の水溶液を開放容器中で連続攪拌しながら55〜60℃に加熱した。溶液を更に10時間攪拌して均質混合物を得た後、40wt%の前駆体溶液を60wt%のCTABと混合した。混合物を攪拌し、安定なヘキサゴナルメソ相が形成された。次いで、液晶相混合物を密封サンプルボトルに移し、60℃に加熱した。ここで、混合物は粘性液体であり、これを明紫色から濃い紫色に変化するまで60℃で更に24〜36時間攪拌した。次いで、加熱を数時間続け、溶液をアルミナるつぼに移し、そこで放冷した。次いで、冷却した固体/ゲルを炉に移して900〜950℃で10時間一定加熱した。
本発明のテンプレート化ゾル−ゲル方法を用いて製造したLiCoO2材料の電気的性能を確認し、その性能をベンチマークの市販LiCoO2及び非テンプレート化方法由来の材料と比較するために実験を実施した。
リン酸鉄リチウム(LiFePO4)のテンプレート化ゾル−ゲル合成を本発明に従って実施した。0.5M リン酸二水素リチウム(Sigma Aldrich Inc.)、0.5M クエン酸第二鉄(Sigma Aldrich)及び1M クエン酸の水溶液を開放容器中で連続攪拌しながら55〜60℃に加熱した。溶液を更に10時間攪拌して均質混合物を得た後、100mlのBrij(登録商標)56(Sigma Aldrich Inc.)界面活性剤の溶融溶液を40℃で添加した。次いで、ヘキサゴナル液晶相が形成されるまで混合物を攪拌した。次いで、粘性ペーストのコンシステンシーを有する液晶相混合物を密封サンプルボトルに移し、60℃に加熱した。ここで、混合物は粘性液体であり、これを60℃で更に24〜36時間攪拌した。次いで、加熱を数時間続け、溶液をアルミナるつぼに移し、そこで放冷した。
Claims (18)
- (i)反応混合物中に液晶相を形成するのに十分な量の界面活性剤の存在下でリチウム塩を1つ以上の遷移金属塩と反応させるステップ、
(ii)反応混合物を加熱してゾル−ゲルを形成するステップ、及び
(iii)界面活性剤を除去して、メソポーラスなリチウム遷移金属酸化物生成物を残すステップを含み、
ステップ(ii)でリチウム塩及び1つ以上の遷移金属塩は高分子金属酸化物網状構造を形成し、
反応混合物中の界面活性剤濃度は40〜60wt%の範囲であり、
ステップ(i)及び(ii)で、反応混合物中の界面活性剤濃度をコントロールして液晶相の不安定化を防止する、メソポーラスなリチウム遷移金属酸化物の合成方法。 - ステップ(i)でリチウム塩をコバルト塩及び1つ以上の追加遷移金属塩と反応させて、化合物コバルト酸リチウムを形成する請求項1に記載の方法。
- 1つ以上の更なる塩はNi、Mn及びAlからなる群から選択される遷移金属を含む請求項2に記載の方法。
- ステップ(i)でリチウム塩をコバルト塩と反応させて、メソポーラスなLiCoO2を形成する請求項1に記載の方法。
- リチウム塩は硝酸リチウムであり、コバルト塩は硝酸コバルトである請求項4に記載の方法。
- 界面活性剤を焼成することにより除去し、焼成温度は400〜700℃の範囲である請求項4または5に記載の方法。
- 焼成温度は400〜600℃の範囲である請求項6に記載の方法。
- リチウム塩をコバルト塩と反応させてメソポーラスなLiCoO2生成物を製造し、ステップ(ii)で反応物を50〜60℃の範囲で加熱する請求項4〜7のいずれか1項に記載の方法。
- 液晶相はヘキサゴナル相である請求項1〜8のいずれかに記載の方法。
- 界面活性剤はポリオキシエチレンセチルエーテル、オクタエチレンエーテル及びCTABからなる群から選択される請求項1〜9のいずれかに記載の方法。
- 反応混合物中の界面活性剤濃度は45〜55wt%の範囲である請求項1〜10のいずれかに記載の方法。
- 反応を水性溶媒中で行う請求項1〜11のいずれかに記載の方法。
- ステップ(i)及び(ii)で水分損失をコントロールする請求項1〜12のいずれかに記載の方法。
- 水分損失を防止する請求項13に記載の方法。
- 反応混合物は更にキレート化剤を含む請求項1〜14のいずれかに記載の方法。
- キレート化剤はクエン酸及びプロピオン酸から選択される請求項15に記載の方法。
- リチウム塩は硝酸リチウムである請求項1〜16のいずれかに記載の方法。
- 1つ以上の遷移金属塩は硝酸塩である請求項1〜17のいずれかに記載の方法。
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GB2443218A (en) | 2006-10-24 | 2008-04-30 | Nanotecture Ltd | Improved Lithium Ion Elecrtochemical cells |
EP2118948A1 (en) * | 2007-03-05 | 2009-11-18 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | A material, in particular for use in electrochemical cells or supercapacitors and a method of making such a material |
GB2457952A (en) * | 2008-02-29 | 2009-09-02 | Nanotecture Ltd | Mesoporous particulate material |
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EP2356069B1 (en) | 2022-12-07 |
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