CN102244241B - 一种焦磷酸锂修饰的磷酸铁锂复合材料的制备方法 - Google Patents
一种焦磷酸锂修饰的磷酸铁锂复合材料的制备方法 Download PDFInfo
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- CN102244241B CN102244241B CN2011101431754A CN201110143175A CN102244241B CN 102244241 B CN102244241 B CN 102244241B CN 2011101431754 A CN2011101431754 A CN 2011101431754A CN 201110143175 A CN201110143175 A CN 201110143175A CN 102244241 B CN102244241 B CN 102244241B
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- lithium
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- pyrophosphoric acid
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- phosphate
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title abstract 3
- 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 title abstract 2
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 63
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 14
- 239000011574 phosphorus Substances 0.000 claims abstract description 14
- 238000012545 processing Methods 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 45
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 43
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 31
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 31
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 21
- 239000002243 precursor Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 10
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 6
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-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
- 238000001354 calcination Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229940062993 ferrous oxalate Drugs 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 4
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 claims description 4
- 238000003746 solid phase reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000005955 Ferric phosphate Substances 0.000 claims description 3
- 229940032958 ferric phosphate Drugs 0.000 claims description 3
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 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
- 229910000147 aluminium 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
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 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
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 28
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 28
- 239000010405 anode material Substances 0.000 abstract description 7
- 239000002002 slurry Substances 0.000 abstract 2
- 238000004804 winding Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 229910015645 LiMn Inorganic materials 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000010450 olivine Substances 0.000 description 2
- 229910052609 olivine Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- -1 pyrophosphoric acid lithium salts Chemical class 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910010710 LiFePO Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
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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)
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Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102683694A (zh) * | 2011-12-30 | 2012-09-19 | 南昌大学 | 一种水溶-干燥法制备LiFePO4/C复合正极材料的方法 |
CN103107332B (zh) * | 2013-01-24 | 2015-10-14 | 北大先行科技产业有限公司 | 一种磷酸铁锂正极材料及其制备方法 |
CN103280568B (zh) * | 2013-05-28 | 2016-03-02 | 宁德新能源科技有限公司 | 钛酸锂复合材料及其制备方法以及其应用 |
CN103441269B (zh) * | 2013-08-05 | 2016-08-17 | 北大先行科技产业有限公司 | 一种焦磷酸锂/碳包覆磷酸铁锂复合材料及其制备方法 |
CN106159204A (zh) * | 2016-07-21 | 2016-11-23 | 三峡大学 | 一种活性物质原位生长电极片及其制备方法 |
CN106058225A (zh) * | 2016-08-19 | 2016-10-26 | 中航锂电(洛阳)有限公司 | 核壳结构LiMn1‑xFexPO4正极材料及其制备方法、锂离子电池 |
CN109301174B (zh) * | 2017-07-24 | 2020-11-13 | 宁德时代新能源科技股份有限公司 | 正极材料及其制备方法及锂二次电池 |
CN108511715B (zh) * | 2018-03-27 | 2020-09-08 | 中南大学 | 一种表面包覆焦磷酸锂的锂离子电池三元材料、制备及其应用 |
CN110943206A (zh) * | 2018-09-25 | 2020-03-31 | 深圳市比亚迪锂电池有限公司 | 正极活性材料及其制备方法和含有该正极活性材料的电池 |
CN109244428B (zh) * | 2018-11-05 | 2022-06-14 | 桑顿新能源科技(长沙)有限公司 | 一种高镍三元材料的包覆改性方法 |
CN109659547B (zh) * | 2018-12-26 | 2020-11-13 | 泰州新滨江环保科技有限公司 | 一种用于锂电池的二元固溶体硼酸盐正极材料及制备方法 |
CN112635722B (zh) * | 2019-10-09 | 2022-04-15 | 北京卫蓝新能源科技有限公司 | 一种锂离子电池复合正极材料及制备方法 |
Citations (4)
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CN101200289A (zh) * | 2006-12-15 | 2008-06-18 | 中国电子科技集团公司第十八研究所 | 一种磷酸铁锂材料及其制备方法 |
CN101404328A (zh) * | 2008-10-30 | 2009-04-08 | 昆明理工大学 | 一种锂离子电池正极材料的制备方法 |
CN101519198A (zh) * | 2009-04-16 | 2009-09-02 | 丁建民 | 一种正极材料磷酸铁锂的制备方法 |
CN101950801A (zh) * | 2010-09-21 | 2011-01-19 | 新疆金盛科达有色金属新材料有限责任公司 | 一种锂离子电池正极材料LiFePO4/C的制备方法 |
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- 2011-05-31 CN CN2011101431754A patent/CN102244241B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101200289A (zh) * | 2006-12-15 | 2008-06-18 | 中国电子科技集团公司第十八研究所 | 一种磷酸铁锂材料及其制备方法 |
CN101404328A (zh) * | 2008-10-30 | 2009-04-08 | 昆明理工大学 | 一种锂离子电池正极材料的制备方法 |
CN101519198A (zh) * | 2009-04-16 | 2009-09-02 | 丁建民 | 一种正极材料磷酸铁锂的制备方法 |
CN101950801A (zh) * | 2010-09-21 | 2011-01-19 | 新疆金盛科达有色金属新材料有限责任公司 | 一种锂离子电池正极材料LiFePO4/C的制备方法 |
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