CN1903707A - Semiwet method of preparing lithium ferrous phosphate and its prepared lithium ferrous phosphate - Google Patents
Semiwet method of preparing lithium ferrous phosphate and its prepared lithium ferrous phosphate Download PDFInfo
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- CN1903707A CN1903707A CNA2006101114448A CN200610111444A CN1903707A CN 1903707 A CN1903707 A CN 1903707A CN A2006101114448 A CNA2006101114448 A CN A2006101114448A CN 200610111444 A CN200610111444 A CN 200610111444A CN 1903707 A CN1903707 A CN 1903707A
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- Prior art keywords
- compound
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- lithium
- suspension liquid
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Links
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 10
- 229940116007 ferrous phosphate Drugs 0.000 title claims description 9
- 229910000155 iron(II) phosphate Inorganic materials 0.000 title claims description 9
- 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 title claims description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 61
- 239000000725 suspension Substances 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 51
- 229910052742 iron Inorganic materials 0.000 claims abstract description 30
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000002482 conductive additive Substances 0.000 claims abstract description 15
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000010298 pulverizing process Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001386 lithium phosphate Inorganic materials 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 58
- 239000007788 liquid Substances 0.000 claims description 50
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 46
- 238000013019 agitation Methods 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 229910001416 lithium ion Inorganic materials 0.000 claims description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 238000000197 pyrolysis Methods 0.000 claims description 22
- 239000012298 atmosphere Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 17
- 230000002829 reductive effect Effects 0.000 claims description 17
- 238000005118 spray pyrolysis Methods 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 239000007774 positive electrode material Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 14
- 150000001722 carbon compounds Chemical class 0.000 claims description 13
- 239000002019 doping agent Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 239000003610 charcoal Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 10
- 150000002736 metal compounds Chemical class 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- -1 monometallic Chemical compound 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 5
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 5
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical group [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-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
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 4
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-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
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 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
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- LNOZJRCUHSPCDZ-UHFFFAOYSA-L iron(ii) acetate Chemical compound [Fe+2].CC([O-])=O.CC([O-])=O LNOZJRCUHSPCDZ-UHFFFAOYSA-L 0.000 claims description 2
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 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
- 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
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 150000002902 organometallic compounds Chemical class 0.000 claims description 2
- 125000002524 organometallic group Chemical group 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical group O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005275 alloying Methods 0.000 abstract 2
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 12
- 229910010710 LiFePO Inorganic materials 0.000 description 11
- 238000001816 cooling Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000003825 pressing Methods 0.000 description 7
- 239000010955 niobium Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 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 description 3
- 229930006000 Sucrose Natural products 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010908 decantation Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910007247 Li(CH3COO).2H2O Inorganic materials 0.000 description 2
- 229910015645 LiMn Inorganic materials 0.000 description 2
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 description 1
- 240000007762 Ficus drupacea Species 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 235000019698 starch Nutrition 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
- 229910052726 zirconium Inorganic materials 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)
Abstract
Description
Sample | 0.2C | 0.5C | 1C | 3C | 5C | 7C | 10C |
Embodiment 1 | 136 | 126 | 126 | 125 | 123 | 124 | 115 |
| 134 | 123 | 123 | 122 | 119 | 118 | - |
Embodiment 3 | 133 | 123 | 122 | 121 | 118 | 113 | - |
Embodiment 4 | 132 | 122 | 122 | 121 | 116 | 112 | - |
Embodiment 5 | 132 | 123 | 122 | 120 | 124 | 110 | - |
Claims (6)
Priority Applications (1)
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CNB2006101114448A CN100528745C (en) | 2006-08-18 | 2006-08-18 | Semiwet method of preparing lithium ferrous phosphate and its prepared lithium ferrous phosphate |
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CNB2006101114448A CN100528745C (en) | 2006-08-18 | 2006-08-18 | Semiwet method of preparing lithium ferrous phosphate and its prepared lithium ferrous phosphate |
Publications (2)
Publication Number | Publication Date |
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CN1903707A true CN1903707A (en) | 2007-01-31 |
CN100528745C CN100528745C (en) | 2009-08-19 |
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CNB2006101114448A Expired - Fee Related CN100528745C (en) | 2006-08-18 | 2006-08-18 | Semiwet method of preparing lithium ferrous phosphate and its prepared lithium ferrous phosphate |
Country Status (1)
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CN (1) | CN100528745C (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101604747B (en) * | 2009-07-07 | 2011-02-02 | 刘强 | Preparation method of lithium iron phosphate anode material |
CN102468489A (en) * | 2010-11-18 | 2012-05-23 | 芯和能源股份有限公司 | Method for producing lithium iron phosphate material and lithium iron phosphate powder produced thereby |
CN102479953A (en) * | 2010-11-25 | 2012-05-30 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery, method for manufacturing the same, and rechargeable lithium battery including the same |
CN102593428A (en) * | 2011-01-11 | 2012-07-18 | 同济大学 | Method for preparing cathode material of lithium ion battery |
CN102637853A (en) * | 2011-02-12 | 2012-08-15 | 同济大学 | Preparation method of lithium ion battery anode composite material |
CN101794880B (en) * | 2007-11-14 | 2012-09-12 | 中国科学院理化技术研究所 | Preparation method of positive-electrode porous material used by lithium ion battery |
CN103123969A (en) * | 2013-01-22 | 2013-05-29 | 北京大学 | Preparation method of nano LiMPO4 cathode material for lithium ion battery |
CN109336078A (en) * | 2012-08-10 | 2019-02-15 | 三星Sdi株式会社 | The manufacturing method of lithium metal phosphates |
-
2006
- 2006-08-18 CN CNB2006101114448A patent/CN100528745C/en not_active Expired - Fee Related
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101794880B (en) * | 2007-11-14 | 2012-09-12 | 中国科学院理化技术研究所 | Preparation method of positive-electrode porous material used by lithium ion battery |
CN101604747B (en) * | 2009-07-07 | 2011-02-02 | 刘强 | Preparation method of lithium iron phosphate anode material |
CN102468489A (en) * | 2010-11-18 | 2012-05-23 | 芯和能源股份有限公司 | Method for producing lithium iron phosphate material and lithium iron phosphate powder produced thereby |
CN102468489B (en) * | 2010-11-18 | 2014-02-19 | 芯和能源股份有限公司 | Method for producing lithium iron phosphate material and lithium iron phosphate powder produced thereby |
CN102479953A (en) * | 2010-11-25 | 2012-05-30 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery, method for manufacturing the same, and rechargeable lithium battery including the same |
US9705132B2 (en) | 2010-11-25 | 2017-07-11 | Samsung Sdi Co., Ltd. | Olivine oxide-containing positive active material for rechargeable lithium battery with improved electro-conductivity, rate characteristics and capacity characteristics, method for manufacturing the same, and rechargeable lithium battery including the same |
US10218001B2 (en) | 2010-11-25 | 2019-02-26 | Samsung Sdi Co., Ltd. | Olivine oxide-containing positive active material for rechargeable lithium battery with improved electro-conductivity, rate characteristics and capacity characteristics, method for manufacturing the same, and rechargeable lithium battery including the same |
CN102593428A (en) * | 2011-01-11 | 2012-07-18 | 同济大学 | Method for preparing cathode material of lithium ion battery |
CN102637853A (en) * | 2011-02-12 | 2012-08-15 | 同济大学 | Preparation method of lithium ion battery anode composite material |
CN109336078A (en) * | 2012-08-10 | 2019-02-15 | 三星Sdi株式会社 | The manufacturing method of lithium metal phosphates |
CN103123969A (en) * | 2013-01-22 | 2013-05-29 | 北京大学 | Preparation method of nano LiMPO4 cathode material for lithium ion battery |
Also Published As
Publication number | Publication date |
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CN100528745C (en) | 2009-08-19 |
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