CN102760879A - 具有稳定低温性能的纳米磷酸亚铁锂/碳复合物的制备方法 - Google Patents
具有稳定低温性能的纳米磷酸亚铁锂/碳复合物的制备方法 Download PDFInfo
- Publication number
- CN102760879A CN102760879A CN2012102695839A CN201210269583A CN102760879A CN 102760879 A CN102760879 A CN 102760879A CN 2012102695839 A CN2012102695839 A CN 2012102695839A CN 201210269583 A CN201210269583 A CN 201210269583A CN 102760879 A CN102760879 A CN 102760879A
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- Prior art keywords
- lithium
- carbon
- source
- compound
- phosphate
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- 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.)
- Granted
Links
- 150000001722 carbon compounds Chemical class 0.000 title claims abstract description 5
- 238000000034 method Methods 0.000 title abstract description 11
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 25
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 229920002521 macromolecule Polymers 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 230000002829 reductive effect Effects 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229940062993 ferrous oxalate Drugs 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 7
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 7
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 235000015165 citric acid Nutrition 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
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-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 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229940116007 ferrous phosphate Drugs 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229910000155 iron(II) phosphate Inorganic materials 0.000 claims description 4
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 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 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 235000001727 glucose Nutrition 0.000 claims description 2
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 2
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 30
- 239000002245 particle Substances 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 14
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 14
- 238000007599 discharging Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910010710 LiFePO Inorganic materials 0.000 description 24
- 238000001816 cooling Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 238000003837 high-temperature calcination Methods 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Images
Classifications
-
- 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
Abstract
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CN201210269583.9A CN102760879B (zh) | 2012-08-01 | 2012-08-01 | 具有稳定低温性能的纳米磷酸亚铁锂/碳复合物的制备方法 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016149297A (ja) * | 2015-02-13 | 2016-08-18 | 三井造船株式会社 | リチウム二次電池の正極活物質の製造方法 |
CN108461739A (zh) * | 2018-03-23 | 2018-08-28 | 枣庄学院 | 一种高性能锂离子电池负极材料Fe7S8/C的制备方法 |
CN109148836A (zh) * | 2017-06-19 | 2019-01-04 | 中天新兴材料有限公司 | 碳包覆磷酸铁锂正极材料及其制备方法 |
CN109920989A (zh) * | 2019-03-01 | 2019-06-21 | 沈阳国科金能科技有限公司 | 一种三层碳包覆复合磷酸铁锂正极材料的制备方法 |
CN111326725A (zh) * | 2020-03-05 | 2020-06-23 | 青海民族大学 | 一种锂离子有机正极材料、制备方法及应用 |
CN112151804A (zh) * | 2020-09-27 | 2020-12-29 | 广州大学 | 一种基于普鲁士蓝类似物的碳包覆过渡金属氧化物及其制备方法和应用 |
Citations (4)
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JP2003292309A (ja) * | 2002-01-31 | 2003-10-15 | Nippon Chem Ind Co Ltd | リチウム鉄リン系複合酸化物炭素複合体、その製造方法、リチウム二次電池正極活物質及びリチウム二次電池 |
US20120058039A1 (en) * | 2010-03-02 | 2012-03-08 | Guiqing Huang | HIGH PERFORMANCE CATHODE MATERIAL LiFePO4, ITS PRECURSORS AND METHODS OF MAKING THEREOF |
CN102496711A (zh) * | 2011-12-13 | 2012-06-13 | 海门容汇通用锂业有限公司 | 一种高比表面积微米级磷酸亚铁锂的制造方法 |
CN102522546A (zh) * | 2011-12-27 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | 纳米锂离子电池级正极材料磷酸亚铁锂的制备方法 |
-
2012
- 2012-08-01 CN CN201210269583.9A patent/CN102760879B/zh active Active
Patent Citations (4)
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JP2003292309A (ja) * | 2002-01-31 | 2003-10-15 | Nippon Chem Ind Co Ltd | リチウム鉄リン系複合酸化物炭素複合体、その製造方法、リチウム二次電池正極活物質及びリチウム二次電池 |
US20120058039A1 (en) * | 2010-03-02 | 2012-03-08 | Guiqing Huang | HIGH PERFORMANCE CATHODE MATERIAL LiFePO4, ITS PRECURSORS AND METHODS OF MAKING THEREOF |
CN102496711A (zh) * | 2011-12-13 | 2012-06-13 | 海门容汇通用锂业有限公司 | 一种高比表面积微米级磷酸亚铁锂的制造方法 |
CN102522546A (zh) * | 2011-12-27 | 2012-06-27 | 江苏中电长迅能源材料有限公司 | 纳米锂离子电池级正极材料磷酸亚铁锂的制备方法 |
Non-Patent Citations (2)
Title |
---|
QUANQI CHEN等: "Electrochemical performance of electrospun LiFePO4/C submicrofibers composite cathode material for lithium ion batteries", 《ELECTROCHIMICA ACTA》 * |
刘学武等: "Synthesis of Sub-micrometer Lithium Iron Phosphate Particles Using Supercritical Hydrothermal Method for Lithium Ion Batteries", 《J.SH ANGHAIJIAOTONG U NIV.》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2016149297A (ja) * | 2015-02-13 | 2016-08-18 | 三井造船株式会社 | リチウム二次電池の正極活物質の製造方法 |
CN109148836A (zh) * | 2017-06-19 | 2019-01-04 | 中天新兴材料有限公司 | 碳包覆磷酸铁锂正极材料及其制备方法 |
CN108461739A (zh) * | 2018-03-23 | 2018-08-28 | 枣庄学院 | 一种高性能锂离子电池负极材料Fe7S8/C的制备方法 |
CN109920989A (zh) * | 2019-03-01 | 2019-06-21 | 沈阳国科金能科技有限公司 | 一种三层碳包覆复合磷酸铁锂正极材料的制备方法 |
CN109920989B (zh) * | 2019-03-01 | 2022-01-14 | 沈阳国科金能科技有限公司 | 一种三层碳包覆复合磷酸铁锂正极材料的制备方法 |
CN111326725A (zh) * | 2020-03-05 | 2020-06-23 | 青海民族大学 | 一种锂离子有机正极材料、制备方法及应用 |
CN112151804A (zh) * | 2020-09-27 | 2020-12-29 | 广州大学 | 一种基于普鲁士蓝类似物的碳包覆过渡金属氧化物及其制备方法和应用 |
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