CN115676799B - Preparation method of modified lithium iron phosphate - Google Patents
Preparation method of modified lithium iron phosphate Download PDFInfo
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- CN115676799B CN115676799B CN202211692008.XA CN202211692008A CN115676799B CN 115676799 B CN115676799 B CN 115676799B CN 202211692008 A CN202211692008 A CN 202211692008A CN 115676799 B CN115676799 B CN 115676799B
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- iron phosphate
- lithium iron
- lithium
- phosphate
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical class [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 15
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 6
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000004254 Ammonium phosphate Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 4
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 4
- 239000000872 buffer Substances 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000000975 co-precipitation Methods 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- 229940076136 ferrous iodide Drugs 0.000 claims description 2
- 229940062993 ferrous oxalate Drugs 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- BQZGVMWPHXIKEQ-UHFFFAOYSA-L iron(ii) iodide Chemical compound [Fe+2].[I-].[I-] BQZGVMWPHXIKEQ-UHFFFAOYSA-L 0.000 claims description 2
- 239000008101 lactose Substances 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
- 229940071264 lithium citrate Drugs 0.000 claims description 2
- WJSIUCDMWSDDCE-UHFFFAOYSA-K lithium citrate (anhydrous) Chemical compound [Li+].[Li+].[Li+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WJSIUCDMWSDDCE-UHFFFAOYSA-K 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
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 claims description 2
- 235000006748 manganese carbonate Nutrition 0.000 claims description 2
- 239000011656 manganese carbonate Substances 0.000 claims description 2
- 229940093474 manganese carbonate Drugs 0.000 claims description 2
- 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 2
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 claims description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 2
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 claims description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- 229910000159 nickel phosphate Inorganic materials 0.000 claims description 2
- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 claims description 2
- 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 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000008363 phosphate buffer Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- MVGWWCXDTHXKTR-UHFFFAOYSA-J tetralithium;phosphonato phosphate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]P([O-])(=O)OP([O-])([O-])=O MVGWWCXDTHXKTR-UHFFFAOYSA-J 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000007774 positive electrode material Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910017052 cobalt Inorganic materials 0.000 description 6
- 239000010941 cobalt Substances 0.000 description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000005056 compaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 239000010406 cathode material Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- CPSYWNLKRDURMG-UHFFFAOYSA-L hydron;manganese(2+);phosphate Chemical compound [Mn+2].OP([O-])([O-])=O CPSYWNLKRDURMG-UHFFFAOYSA-L 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000007709 nanocrystallization Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- TYIQHQFQWOZFMP-UHFFFAOYSA-E lithium cobalt(2+) iron(2+) manganese(2+) nickel(2+) triphosphate Chemical compound P(=O)([O-])([O-])[O-].[Fe+2].[Ni+2].[Co+2].[Mn+2].[Li+].P(=O)([O-])([O-])[O-].P(=O)([O-])([O-])[O-] TYIQHQFQWOZFMP-UHFFFAOYSA-E 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a preparation method of modified lithium iron phosphate. The preparation method of the modified lithium iron phosphate comprises the following steps of mixing a Fe source, an M source and a P source according to Li y M (1‑x) Fe x PO 4 X is more than or equal to 0 and less than 1, and is added into a dispersing agent to obtain a precursor; performing sanding treatment and grinding treatment on the precursor; drying and calcining the precursor under the protection of atmosphere; the Li source is Li y M (1‑x) Fe x PO 4 Y is more than or equal to 1 and less than or equal to 1.18, and the Li source, the C source and the doping metal are put into a dispersing agent for sanding treatment; and drying the obtained slurry, and then sintering under the atmosphere protection. The preparation method of the modified lithium iron phosphate provided by the invention improves the energy density, voltage and low-temperature performance of the lithium iron phosphate.
Description
Technical Field
The invention relates to the field of battery materials, in particular to a preparation method of modified lithium iron phosphate.
Background
The theoretical gram capacity of the lithium iron phosphate is 170mAh, the theoretical discharge platform of the lithium iron phosphate is 3.4V, the actual level is 3.2V-3.3V, and the compaction density of the lithium iron phosphate is 2.4g/cm 3 . The lithium iron phosphate has the advantages of low price, environmental friendliness, higher safety performance, and better structural stability and cycle performance; the disadvantages are poor low temperature performance and low energy density. In order to improve the energy density, voltage and low-temperature performance of the lithium iron phosphate, the basic direction is to improve the existing preparation method of the lithium iron phosphate product, and the energy density is increased through inhibiting the growth of crystals, reducing the diffusion distance of lithium ions and nanocrystallization; the coating increases the conductivity; the cycle performance is improved by doping; the performance advantages of ternary and lithium iron phosphate are integrated, and the defects of poor high-temperature performance, large cobalt proportion, low energy density, low compaction density and low temperature performance of the ternary material are overcome.
Disclosure of Invention
The invention provides a preparation method of modified lithium iron phosphate, aiming at improving the energy density, voltage and low-temperature performance of lithium iron phosphate.
A preparation method of modified lithium iron phosphate comprises the following steps:
step 1: will be provided withFe source, M source and P source according to Li y M (1-x) Fe x PO 4 X is more than or equal to 0 and less than 1, and is added into the dispersant to obtain a precursor;
step 2: sanding and grinding the precursor until the particle size of particles in the precursor reaches 50-1000 nm and the particle morphology reaches a preset morphology;
and 3, step 3: drying and calcining the precursor under the protection of atmosphere at the calcining temperature of 300-500 ℃ to obtain a primary precursor;
and 4, step 4: mixing Li source according to the proportion in the step 1, putting Li source, C source and doping metal into a dispersing agent, sanding until the particle size reaches 100-1000 nm, adding the primary precursor and mixing;
and 5: and (4) drying the slurry treated in the step (4), and sintering under the protection of atmosphere at the sintering temperature of 650-950 ℃.
In a preferred embodiment of the preparation method of the modified lithium iron phosphate provided by the present invention, in the step 1, li y M (1-x) Fe x PO 4 Y is more than or equal to 1 and less than or equal to 1.18; in the step 4, the Li source is Li y M (1-x) Fe x PO 4 And y is more than or equal to 1 and less than or equal to 1.18. In the step 4, the mass ratio of the C source is Li y M (1-x) Fe x PO 4 0.1-10% of the whole, and the mass ratio of the doped metal is Li y M (1-x) Fe x PO 4 0.2-2% of the whole.
In a preferred embodiment of the preparation method of the modified lithium iron phosphate provided by the invention, the M source comprises a Ni source, a Co source and a Mn source, wherein the ratio of Ni: co: the molar ratio of Mn is 1:1:1,0.5:0:1.5,4:4:2,3:3:6,5:2:3,6:2:2,7:1.5:1.5,8:1:1,9:0: 1; wherein the Ni source comprises one or more of nickel sulfate, nickel nitrate, nickel phosphate, nickel acetate and nickel oxide, and the Co source comprises one or more of cobalt sulfate, cobalt nitrate, cobalt acetate, cobaltosic oxide and cobaltosic oxide; the Mn source comprises one or more of manganese dioxide EMD, manganous oxide, manganous manganic oxide, manganese carbonate, manganese nitrate, manganous acetate and manganous acetate.
The Li source comprises one or more of lithium hydroxide, lithium peroxide, lithium oxide, lithium carbonate, lithium citrate, lithium phosphate, lithium dihydrogen phosphate and lithium dihydrogen phosphate; the Fe source comprises one or more of ferrous oxide, ferroferric oxide, ferric nitrate, ferrous oxalate, ferrous sulfate, ferrous sulfide and ferrous iodide; the P source comprises one or more of phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, lithium phosphate and lithium pyrophosphate; the C source comprises glucose, sucrose, lactose, phenolic resin, graphene, carbon nano tubes and graphite; the doping element is a compound containing one or more of Zn, zr, cr, mo, pd, si, al, V, ti and F; the dispersant comprises one or more of methanol, ethanol, propanol, diethyl ether, propylene oxide, ethylene glycol monomethyl ether, polyethylene, polypropylene and universal dispersant.
In a preferred embodiment of the preparation method of the modified lithium iron phosphate provided by the present invention, in the step 1, an Fe source, an M source and a P source are added into a dispersant according to a ratio of 20% to 70% of solid content; in the step 4, the Li source, the C source and the doping metal are put into a sufficient amount of dispersant, and after the primary precursor is added, the Li source, the C source, the doping metal and the primary precursor have solid contents of 20-70%.
In the step 2 and the step 4, the sand grinding treatment is performed under the conditions that the ball-to-material ratio is 1 to 1, the stirring speed is 100rpm to 1000rpm, and ultrasonic waves are added.
Calcining for 1-10 h in the step 3, sintering for 6-15 h in the step 5, and crushing and sieving the sintered materials.
In a preferred embodiment of the preparation method of the modified lithium iron phosphate provided by the invention, in the step 2, a pH regulator and/or a buffer solution is added for grinding treatment, and coprecipitation is performed for 5 to 80 hours until the morphology of particles reaches a preset morphology.
The pH regulator comprises one or more of hydrochloric acid, sulfuric acid, acetic acid, sodium hydroxide, sodium bicarbonate and ammonia water; the buffer solution comprises one or more of phosphate buffer, borate buffer and boric acid buffer.
The ternary material has good low-temperature performance and rate charging performance, higher charging speed, good low-temperature performance, high energy density, high discharge voltage and good output power; the lithium iron phosphate has the advantages of low cost, high safety performance, high thermal stability, no spontaneous combustion during needling and overcharging, long service life, safety and no explosion risk. Compared with the prior art, the preparation method of the modified lithium iron phosphate provided by the invention has the advantages that the ternary precursor and the lithium iron phosphate precursor are subjected to molecular-level fusion from the precursor, and the obtained product has the excellent performances of both the ternary material and the lithium iron phosphate material.
The preparation method of the modified lithium iron phosphate provided by the invention reduces the diffusion distance of lithium ions by inhibiting crystal growth, and increases energy density by nanocrystallization. The conductivity is increased by cladding. The cycle performance is improved by doping. Through the addition of nickel, cobalt and manganese, the performance advantages of ternary and lithium iron phosphate are integrated, and the defects of poor high-temperature performance, large cobalt proportion, low energy density, low compaction density and low-temperature performance of the ternary material are overcome.
The nickel cobalt manganese iron lithium phosphate LMFP prepared by the preparation method of the modified lithium iron phosphate provided by the invention has the advantages that the coated crystals are inhibited from growing, the particles are nano, and the diffusion distance of lithium ions is reduced. The 0.1C discharge specific capacity reaches over 160mAh/g, the capacity is not attenuated after 500 times of circulation, and the energy density is high. The low-temperature discharge capacity of the battery can reach 94.7%, the low-temperature DCR (direct current impedance) is less than 15 omega cm, the low-temperature discharge capacity can reach more than 72% of the normal temperature, and the voltage is greatly improved. The voltage plateau reached 3.8V. The compacted density is ultrahigh, and is improved by about 16.6%. And the coating does not fall off powder in the battery making process, is uniformly distributed, has excellent processing performance, and has the excellent performances of ternary materials and lithium iron phosphate.
Drawings
FIG. 1 is an SEM (scanning electron microscope) picture of a material prepared by the preparation method of the modified lithium iron phosphate at magnifications of 1k, 10k, 20k, 30k, 50k and 70 k;
FIG. 2 is an XRD (X-ray diffraction) diagram of a material prepared by the preparation method of the modified lithium iron phosphate provided by the invention;
FIG. 3 is a charge-discharge curve diagram of the material prepared by the preparation method of the modified lithium iron phosphate provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
A preparation method of modified lithium iron phosphate comprises the following steps:
step 1: mixing an M source, ferrous oxide and ammonium phosphate according to the ratio of M: fe: p =0.4:0.6:1, the components are mixed. Wherein the M source comprises nickel sulfate, cobalt sulfate and manganese dioxide EMD, and the weight ratio of Ni: co: mn =0.5:0.2: the mixture was mixed at a molar ratio of 0.3.
And adding an M source, ferrous oxide and ammonium phosphate into propanol according to the proportion of 50% of solid content to form a mixed precursor of nickel, cobalt and manganese phosphate.
And 2, step: putting the mixed precursor of nickel, cobalt and manganese phosphate into a high-speed sand mill, and sanding for 2 hours under the conditions that the ball material ratio is 7.
Then slowly introducing into a stirring mill, and carrying out coprecipitation for 50h under the conditions that the stirring speed is 100rpm and sodium hydroxide and ammonia water are added. The particle morphology can be ensured to reach the morphology required by design by detecting through a high-power microscope and a scanning electron microscope.
And 3, step 3: drying under the protection of nitrogen atmosphere, and then continuously calcining for 5h at 300 ℃ under the protection of nitrogen atmosphere to obtain the primary precursor of nickel, cobalt and manganese phosphate. I.e. forming M 0.4 Fe 0.6 PO4 primary precursor, i.e. (Ni) 0.5 Co 0.2 Mn 0.3 ) 0.4 Fe 0.6 PO4 precursor.
And 4, step 4: lithium hydroxide was added as Li: (M + Fe) =1.04:1, graphite accounting for 2.5 percent of the whole, and Zn, zr and Cr compounds accounting for 0.6 percent of the whole.
Adding lithium hydroxide, graphite and Zn, zr and Cr compounds into enough propanol, and putting into a high-speed sand mill. The mixture is ground for 2 hours under the conditions that the ball-material ratio is 7:1, the stirring speed is 900rpm and ultrasonic waves are added, so that the particle size reaches 500nm and the fusion of molecular level is achieved.
Then introduced into a stirring mill and M is added 0.4 Fe 0.6 PO4 primary precursor. The amount of the dispersant is controlled in advance, and M is added 0.4 Fe 0.6 The PO4 primary precursor has a solid content of 50%. The mixture was uniformly mixed for 1 hour at a stirring speed of 300 rpm.
And 5: and (4) introducing the mixture into a spray tower to remove the dispersant, so as to obtain uniform dry powder. And then sintering the mixture for 9 hours at 850 ℃ under the protection of nitrogen atmosphere, and crushing and sieving the sintered material to obtain a final finished product, namely the lithium iron phosphate LMFP positive electrode material.
The obtained lithium iron phosphate LMFP anode material has good low-temperature effect, the room-temperature discharge capacity of the battery can reach 94.7 percent, the low-temperature DCR (direct current impedance) is less than 15 omega cm, the low-temperature discharge capacity can reach more than 72 percent, and the voltage of the battery is greatly improved; the compaction density is ultrahigh, and is improved by about 16.6 percent. The discharge specific capacity of the half battery at 0.1C can be more than 160 mA.h/g, and the discharge specific capacity of the full battery at 1C is more than 144mAh/g. Electrical property data see table 1:
TABLE 1
Fig. 1 shows SEM electron microscope pictures of the lithium iron phosphate LMFP cathode material prepared by the method of the present invention at magnifications of 1k, 10k, 20k, 30k, 50k, and 70 k.
Fig. 1 includes six drawings a to f, where fig. 1a is an SEM electron microscope picture of the lithium iron phosphate LMFP positive electrode material at a magnification of 1 k; FIG. 1b is an SEM electron microscope picture of the lithium iron phosphate LMFP cathode material under a magnification of 10 k; and so on.
The nano uniformity of the material under a low power electron microscope is quite good, the growth of single crystal particles is inhibited, and the D50 is at a nano level; the crystal structure of the material is compact under a high-power electron microscope, the coating layer is 10-30 nm, and the particles of the material are uniformly dispersed.
Fig. 2 shows XRD patterns of two batches of lithium iron phosphate LMFP positive electrode materials prepared by the method of the present invention.
Fig. 2 includes two drawings, a and b, wherein fig. 2a is an XRD pattern of the lithium iron phosphate LMFP positive electrode material of batch 1; fig. 2b is an XRD pattern of batch 2 lithium iron phosphate LMFP cathode material.
The diffraction spectrogram is used for qualitatively analyzing whether the unit cell expands or contracts on the basis of the number, angle position, relative intensity and diffraction peak shape of the diffraction peak by comparing an actually measured sample with a standard spectrogram 2 theta value, the size and shape of the unit cell can be determined by the peak position of XRD, and when the generated lithium iron phosphate LMFP is compared with the standard peak, the peak shape is almost consistent, 4 obvious peaks indicate that the degree of crystallization is quite good, and no impurity peak exists at the high peak, which indicates that the material is purer in preparation, the situation of crystal collapse does not occur, the synthesis effect is better, and the process route is reasonable.
Referring to fig. 3, it is a charging and discharging curve diagram of a battery prepared from two batches of lithium iron phosphate LMFP positive electrode materials by using the preparation method of modified lithium iron phosphate provided by the present invention.
Fig. 3 includes two drawings, a and b, in which fig. 3a is a charge-discharge curve diagram of a battery manufactured from the lithium iron phosphate LMFP positive electrode material of batch 1; fig. 3b is a charge-discharge curve diagram of batch 2 of lithium iron phosphate LMFP cathode material prepared into batteries for testing.
According to the lithium iron phosphate LMFP positive electrode material: acetylene black: pvdf =8:1:1, coating, drying, rolling, cutting into pieces, assembling, sealing, and placing blue electricityThe system enters testing. The voltage platform is 3.8 v-4.1 v, the electrical performance is tested, the gram capacity of 0.1C reaches 161mAh/g, the gram capacity does not attenuate after 500 times of circulation, the energy density is high, and the compaction density reaches 2.85g/cm 3 。
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A preparation method of modified lithium iron phosphate is characterized by comprising the following steps:
step 1: mixing Fe source, M source and P source according to Li y M (1-x) Fe x PO 4 X is more than or equal to 0 and less than 1, and is added into a dispersing agent to obtain a precursor;
the M source comprises a Ni source, a Co source and a Mn source, and the ratio of Ni: co: the molar ratio of Mn is 1:1:1,0.5:0:1.5,4:4:2,3:3:6,5:2:3,6:2:2,7:1.5:1.5,8:1:1,9:0: 1; wherein the Ni source comprises one or more of nickel sulfate, nickel nitrate, nickel phosphate, nickel acetate and nickel oxide, and the Co source comprises one or more of cobalt sulfate, cobalt nitrate, cobalt acetate, cobaltosic oxide and cobaltosic oxide; the Mn source comprises one or more of manganese dioxide EMD, manganous oxide, manganous manganic oxide, manganese carbonate, manganese nitrate, manganous acetate and manganous acetate;
and 2, step: sanding and grinding the precursor until the particle size of particles in the precursor reaches 50-1000 nm and the particle morphology reaches a preset morphology;
and step 3: drying and calcining the precursor under the protection of atmosphere at the calcining temperature of 300-500 ℃ to obtain a primary precursor;
and 4, step 4: mixing Li source according to the proportion in the step 1, putting the Li source, C source and doped metal into a dispersing agent, sanding until the particle size reaches 100-1000 nm, adding the primary precursor and mixing;
and 5: and (5) drying the slurry treated in the step (4), and sintering under the protection of atmosphere at the sintering temperature of 650-950 ℃.
2. The method for preparing modified lithium iron phosphate according to claim 1, wherein: in said step 1, li y M (1-x) Fe x PO 4 Y is more than or equal to 1 and less than or equal to 1.18; in the step 4, the Li source is Li y M (1-x) Fe x PO 4 And y is more than or equal to 1 and less than or equal to 1.18.
3. The method for preparing modified lithium iron phosphate according to claim 2, wherein: in the step 4, the mass ratio of the C source is Li y M (1-x) Fe x PO 4 0.1-10% of the whole, and the mass ratio of the doped metal is Li y M (1-x) Fe x PO 4 0.2 to 2 percent of the whole.
4. The method for preparing modified lithium iron phosphate according to claim 1, wherein: the Li source comprises one or more of lithium hydroxide, lithium peroxide, lithium oxide, lithium carbonate, lithium citrate, lithium phosphate, lithium dihydrogen phosphate and lithium dihydrogen phosphate; the Fe source comprises one or more of ferrous oxide, ferroferric oxide, ferric nitrate, ferrous oxalate, ferrous sulfate, ferrous sulfide and ferrous iodide; the P source comprises one or more of phosphoric acid, ammonium dihydrogen phosphate, lithium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, lithium phosphate and lithium pyrophosphate; the C source comprises glucose, sucrose, lactose, phenolic resin, graphene, carbon nano tubes and graphite; the doping element is a compound containing one or more of Zn, zr, cr, mo, pd, si, al, V, ti and F; the dispersant comprises one or more of methanol, ethanol, propanol, diethyl ether, propylene oxide, ethylene glycol monomethyl ether, polyethylene, polypropylene and universal dispersant.
5. The method for producing modified lithium iron phosphate according to claim 3 or 4, characterized in that: in the step 1, a Fe source, an M source and a P source are added into a dispersing agent according to the proportion of 20-70% of solid content; in the step 4, the Li source, the C source and the doping metal are put into a sufficient amount of dispersant, and after the primary precursor is added, the Li source, the C source, the doping metal and the primary precursor have solid contents of 20-70%.
6. The method for producing modified lithium iron phosphate according to claim 3 or 4, characterized in that: in the step 2 and the step 4, the sand grinding treatment is performed under the conditions that the ball-to-material ratio is 1 to 1, the stirring speed is 100rpm to 1000rpm, and ultrasonic waves are added.
7. The method for producing modified lithium iron phosphate according to claim 3 or 4, characterized in that: calcining for 1-10 h in the step 3, sintering for 6-15 h in the step 5, and crushing and sieving the sintered materials.
8. The method for preparing modified lithium iron phosphate according to claim 3 or 4, wherein: and (3) adding a pH regulator and/or a buffer solution in the step (2) for grinding treatment, and carrying out coprecipitation for 5-80 h until the particle morphology reaches the preset morphology.
9. The method for preparing modified lithium iron phosphate according to claim 8, wherein the method comprises the following steps: the pH regulator comprises one or more of hydrochloric acid, sulfuric acid, acetic acid, sodium hydroxide, sodium bicarbonate and ammonia water; the buffer solution comprises one or more of phosphate buffer, borate buffer and boric acid buffer.
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Denomination of invention: Preparation method of modified lithium iron phosphate Granted publication date: 20230331 Pledgee: Ningxiang sub branch of Bank of Changsha Co.,Ltd. Pledgor: Hunan Pengbo New Material Co.,Ltd. Registration number: Y2024980011784 |