JP4625536B2 - 電極活物質であるアニオン不足型非化学量論リン酸鉄リチウム、その製造方法、及びそれを利用した電気化学素子 - Google Patents
電極活物質であるアニオン不足型非化学量論リン酸鉄リチウム、その製造方法、及びそれを利用した電気化学素子 Download PDFInfo
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- JP4625536B2 JP4625536B2 JP2009287137A JP2009287137A JP4625536B2 JP 4625536 B2 JP4625536 B2 JP 4625536B2 JP 2009287137 A JP2009287137 A JP 2009287137A JP 2009287137 A JP2009287137 A JP 2009287137A JP 4625536 B2 JP4625536 B2 JP 4625536B2
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- Prior art keywords
- iron phosphate
- lithium iron
- anion
- lithium
- stoichiometric
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims description 184
- 150000001450 anions Chemical class 0.000 title claims description 128
- 230000002950 deficient Effects 0.000 title claims description 93
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 239000007772 electrode material Substances 0.000 title claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 144
- 229910052744 lithium Inorganic materials 0.000 claims description 67
- 238000000034 method Methods 0.000 claims description 59
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000002243 precursor Substances 0.000 claims description 45
- 239000000126 substance Substances 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 22
- -1 phosphate compound Chemical class 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 229910019142 PO4 Inorganic materials 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000012692 Fe precursor Substances 0.000 claims description 11
- 230000003113 alkalizing effect Effects 0.000 claims description 11
- 239000010452 phosphate Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 description 73
- 229910052742 iron Inorganic materials 0.000 description 56
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 52
- 230000000052 comparative effect Effects 0.000 description 44
- 230000003647 oxidation Effects 0.000 description 44
- 238000007254 oxidation reaction Methods 0.000 description 44
- 150000001768 cations Chemical class 0.000 description 39
- 229910001416 lithium ion Inorganic materials 0.000 description 35
- 239000000203 mixture Substances 0.000 description 34
- 239000007864 aqueous solution Substances 0.000 description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 28
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 26
- 239000013078 crystal Substances 0.000 description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical class N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 24
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 23
- 230000008569 process Effects 0.000 description 21
- 229910052698 phosphorus Inorganic materials 0.000 description 19
- 239000007774 positive electrode material Substances 0.000 description 19
- 238000009792 diffusion process Methods 0.000 description 18
- 239000012535 impurity Substances 0.000 description 18
- 239000002245 particle Substances 0.000 description 18
- 238000010304 firing Methods 0.000 description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 14
- 238000005481 NMR spectroscopy Methods 0.000 description 12
- 230000007547 defect Effects 0.000 description 12
- 229910000358 iron sulfate Inorganic materials 0.000 description 12
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 12
- 239000002002 slurry Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910021529 ammonia Inorganic materials 0.000 description 11
- 238000007599 discharging Methods 0.000 description 11
- 239000008187 granular material Substances 0.000 description 11
- 230000005291 magnetic effect Effects 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 235000021317 phosphate Nutrition 0.000 description 10
- 229910052723 transition metal Inorganic materials 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 239000010450 olivine Substances 0.000 description 8
- 229910052609 olivine Inorganic materials 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- 238000003991 Rietveld refinement Methods 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009616 inductively coupled plasma Methods 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000004611 spectroscopical analysis Methods 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 239000007833 carbon precursor Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 238000002050 diffraction method Methods 0.000 description 4
- 239000011267 electrode slurry Substances 0.000 description 4
- 150000002642 lithium compounds Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 238000004685 neutron diffraction pattern Methods 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011149 active material Substances 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
- 239000002019 doping agent Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000011882 ultra-fine particle Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 230000005343 Curie-Weiss law Effects 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 238000001669 Mossbauer spectrum Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011361 granulated particle Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 150000008040 ionic compounds Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 238000004448 titration 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
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- 241000238366 Cephalopoda Species 0.000 description 1
- 208000032953 Device battery issue Diseases 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910010586 LiFeO 2 Inorganic materials 0.000 description 1
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 238000004813 Moessbauer spectroscopy Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000006713 insertion reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Inorganic materials [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 1
- 229910001386 lithium phosphate Inorganic materials 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 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
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
-
- 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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/447—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on phosphates, e.g. hydroxyapatite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Description
Li1−xFe(PO4)1−y
(0<x≦0.15であり、0<y≦0.05である)
(a)Fe前駆体、リン酸化合物、アルカリ化剤及びリチウム前駆体を混合し、リン酸鉄リチウム前駆体を生成する段階;
(b)前記段階(a)のリン酸鉄リチウム前駆体を、温度200〜700℃、圧力180〜550barの反応条件下で水と混合し、アニオン不足型非化学量論リン酸鉄リチウムを生成し、その後に乾燥させる段階;
(c)前記段階(b)の生成物を焼成する、又は顆粒化した後に焼成する段階。
Li1−xFe(PO4)1−y
(a)共沈工程:3LiNO3+3Fe(NO3)2・nH2O+3(NH4)2HPO4→Fe3(PO4)2・nH2O+Li3PO4+6NH3+9HNO3;
(b)焼成工程:Fe3(PO4)2・nH2O+Li3PO4→3LiFePO4+nH2O
FeSO4・7H2O+H3PO4+LiOH→LiFePO4+H2SO4+8H2O
Claims (9)
- 電極活物質である、下記の化学式で表されるアニオン不足型非化学量論リン酸鉄リチウム。
(化1)
Li1−xFe(PO4)1−y
(式中、0.06≦x≦0.15であり、0.02≦y≦0.05である。) - 前記yの範囲が0.03≦y≦0.05であることを特徴とする、請求項1に記載のアニオン不足型非化学量論リン酸鉄リチウム。
- 請求項1または請求項2に記載のアニオン不足型非化学量論リン酸鉄リチウムを含む二次電池の正極。
- 二次電池であって、
(a)請求項1または請求項2に記載のアニオン不足型非化学量論リン酸鉄リチウムを含む正極と、
(b)負極と、
(c)分離膜と、
(d)電解質とを含む二次電池。 - (a)Fe前駆体、リン酸化合物、アルカリ化剤及びリチウム前駆体を混合させてリン酸鉄リチウム前駆体を生成する段階と、
(b)前記段階(a)で生成されたリン酸鉄リチウム前駆体を、温度200〜700℃、圧力18〜55MPa(180〜550bar)の反応条件下で水と混合させてアニオン不足型非化学量論リン酸鉄リチウムを生成し、その後、乾燥させる段階と、
(c)前記段階(b)で生成されたアニオン不足型非化学量論リン酸鉄リチウムを、焼成するか又は顆粒化した後に焼成する段階とを含む、
電極活物質である、下記の化学式で表されるアニオン不足型非化学量論リン酸鉄リチウムの製造方法。
(化1)
Li1−xFe(PO4)1−y
(式中、0<x≦0.15であり、0<y≦0.05である)。 - 前記アニオン不足型非化学量論リン酸鉄リチウムにおける前記yの範囲が0.01≦y≦0.05であることを特徴とする請求項5に記載の方法。
- 前記アニオン不足型非化学量論リン酸鉄リチウムにおける前記yの範囲が0.02≦y≦0.05であることを特徴とする請求項5に記載の方法。
- 前記アニオン不足型非化学量論リン酸鉄リチウムにおける前記yの範囲が0.03≦y≦0.05であることを特徴とする請求項5に記載の方法。
- 前記段階(b)の前記反応条件のpHの範囲が4<pH≦9であることを特徴とする請求項5に記載の方法。
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KR1020090005540A KR100939647B1 (ko) | 2009-01-22 | 2009-01-22 | 전극 활물질인 음이온 부족형 비화학양론 리튬 전이금속 다중산 화합물, 그 제조 방법 및 그를 이용한 전기화학 소자 |
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JP2011547778A Active JP5318969B2 (ja) | 2009-01-22 | 2010-01-21 | 電極活物質であるアニオン不足型リン酸遷移金属リチウム化合物、その製造方法、及びそれを利用した電気化学素子 |
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CN115072694A (zh) * | 2022-06-28 | 2022-09-20 | 衢州华友钴新材料有限公司 | 磷酸铁锂正极材料及其制备方法以及锂离子电池 |
CN116779778B (zh) * | 2023-08-11 | 2024-02-09 | 深圳海辰储能控制技术有限公司 | 正极极片及其制备方法、储能装置和用电装置 |
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WO2000060679A1 (en) | 1999-04-06 | 2000-10-12 | Sony Corporation | Method for manufacturing active material of positive plate and method for manufacturing nonaqueous electrolyte secondary cell |
WO2000060680A1 (fr) | 1999-04-06 | 2000-10-12 | Sony Corporation | Materiau actif pour plaque positive, cellule secondaire a electrolyte non aqueuse, et leurs procedes de fabrication respectifs |
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CN100448071C (zh) * | 2003-03-18 | 2008-12-31 | 黄穗阳 | 锂电池正极材料及其制备方法 |
JP2005158673A (ja) * | 2003-10-31 | 2005-06-16 | Toyota Motor Corp | 電極活物質およびその製造方法ならびに非水電解質二次電池 |
TWI279020B (en) * | 2004-11-03 | 2007-04-11 | Tatung Co Ltd | Preparation of olivine LiFePO4 cathode materials for lithium batteries via a solution method |
CN100377392C (zh) * | 2004-12-21 | 2008-03-26 | 中国科学院物理研究所 | 用于二次锂电池的含氧空位的磷酸铁锂正极材料及其用途 |
DE102005012640B4 (de) * | 2005-03-18 | 2015-02-05 | Süd-Chemie Ip Gmbh & Co. Kg | Kreisprozess zur nasschemischen Herstellung von Lithiummetallphosphaten |
US7939201B2 (en) * | 2005-08-08 | 2011-05-10 | A123 Systems, Inc. | Nanoscale ion storage materials including co-existing phases or solid solutions |
US7524529B2 (en) | 2005-09-09 | 2009-04-28 | Aquire Energy Co., Ltd. | Method for making a lithium mixed metal compound having an olivine structure |
US7494744B2 (en) * | 2006-03-08 | 2009-02-24 | Changs-Ascending Enterprise Co. | Cathode material for Li-ion battery applications |
CN101212048A (zh) * | 2006-12-30 | 2008-07-02 | 比亚迪股份有限公司 | 一种锂离子二次电池的正极材料及含有该正极材料的电池 |
KR20090005540A (ko) | 2007-07-09 | 2009-01-14 | 엘지디스플레이 주식회사 | 액정표시장치 |
US8052897B2 (en) * | 2008-02-29 | 2011-11-08 | Byd Company Limited | Composite compound with mixed crystalline structure |
JP5474991B2 (ja) * | 2008-10-22 | 2014-04-16 | エルジー・ケム・リミテッド | 電極の効率及びエネルギー密度を改良するカソード活性材料 |
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TW201036235A (en) | 2010-10-01 |
JP2010170997A (ja) | 2010-08-05 |
US20120021288A1 (en) | 2012-01-26 |
WO2010085104A9 (ko) | 2010-10-14 |
WO2010085104A2 (ko) | 2010-07-29 |
WO2010085104A3 (ko) | 2010-12-02 |
CA2750328A1 (en) | 2010-07-29 |
CA2750328C (en) | 2014-03-18 |
EP2211404A1 (en) | 2010-07-28 |
HK1144616A1 (en) | 2011-02-25 |
US7858233B2 (en) | 2010-12-28 |
CN101789507A (zh) | 2010-07-28 |
TWI383533B (zh) | 2013-01-21 |
JP5318969B2 (ja) | 2013-10-16 |
US20100183924A1 (en) | 2010-07-22 |
JP2012516016A (ja) | 2012-07-12 |
CN102292855A (zh) | 2011-12-21 |
TW201032377A (en) | 2010-09-01 |
CN101789507B (zh) | 2013-08-14 |
KR100939647B1 (ko) | 2010-02-03 |
EP2390948A2 (en) | 2011-11-30 |
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