JP2011500492A - Liイオン蓄電池用オルトリン酸鉄(III) - Google Patents
Liイオン蓄電池用オルトリン酸鉄(III) Download PDFInfo
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- JP2011500492A JP2011500492A JP2010529336A JP2010529336A JP2011500492A JP 2011500492 A JP2011500492 A JP 2011500492A JP 2010529336 A JP2010529336 A JP 2010529336A JP 2010529336 A JP2010529336 A JP 2010529336A JP 2011500492 A JP2011500492 A JP 2011500492A
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- iron
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- orthophosphate
- phosphoric acid
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- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 87
- 229910001416 lithium ion Inorganic materials 0.000 title claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 36
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000011541 reaction mixture Substances 0.000 claims abstract description 16
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical class [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 14
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical class O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 claims abstract description 5
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 claims abstract description 5
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims abstract description 4
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 15
- 150000002506 iron compounds Chemical class 0.000 claims description 14
- 239000007774 positive electrode material Substances 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000011164 primary particle Substances 0.000 claims description 8
- -1 Iron (II) compound Chemical class 0.000 claims description 7
- 239000010406 cathode material Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-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
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 2
- 229910010710 LiFePO Inorganic materials 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 150000004679 hydroxides Chemical class 0.000 abstract description 7
- 150000004677 hydrates Chemical class 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 10
- 239000007858 starting material Substances 0.000 description 10
- 229910000398 iron phosphate Inorganic materials 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 229910000358 iron sulfate Inorganic materials 0.000 description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000002411 adverse Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000002367 phosphate rock Substances 0.000 description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 238000012916 structural analysis Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000005955 Ferric phosphate Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- HGMOGXHCIWRNSL-UHFFFAOYSA-L [N+](=O)([O-])[O-].P(=O)([O-])([O-])O.[Fe+3] Chemical compound [N+](=O)([O-])[O-].P(=O)([O-])([O-])O.[Fe+3] HGMOGXHCIWRNSL-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 229910001463 metal phosphate Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- C01P2002/30—Three-dimensional structures
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Y10T428/00—Stock material or miscellaneous articles
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Abstract
【選択図】 図2a
Description
乾燥収量: 305 g
収率(%): 96.7
バルク密度: 920 g/l
乾燥収量: 124 g
収率(%): おおよそ93
バルク密度: 890 g/l
乾燥収量: 128 g
収率(%): ca. 96
バルク密度: 810 g/l
Claims (17)
- 一般式 FePO4 x nH2O (n ≦ 2.5) のオルトリン酸鉄(III)であって、該オルトリン酸鉄(III)は、水酸化物、酸化物、酸化水酸化物、酸化物の水和物、炭酸塩及び/水酸化炭酸塩から選択された鉄(II)化合物、鉄(III)化合物または鉄(II, III)混合化合物を、5%〜50%の範囲の濃度を有しているリン酸と反応せしめ、当該反応後に存在している鉄(II)を、酸化剤を添加することで鉄(III)に変換し、得られた反応混合物から固体状オルトリン酸鉄(III)を分離取得するプロセスで製造されるものであることを特徴とする該オルトリン酸鉄(III)。
- 上記鉄化合物とリン酸との反応を、50℃〜180℃の範囲の温度、好ましくは60℃〜150℃の範囲内の温度、特に好ましくは70℃〜120℃の範囲内の温度で行うことを特徴とする請求項1に記載の該オルトリン酸鉄(III)。
- 上記鉄化合物とリン酸との反応を、激しく攪拌しながら行うことを特徴とする請求項1又は2に記載の該オルトリン酸鉄(III)。
- 上記鉄化合物とリン酸との反応を、0.5分間〜120分間の期間、好ましくは1分間〜60分間の期間、特に好ましくは2分間〜30分間の期間行うことを特徴とする請求項1〜3のいずれか一に記載の該オルトリン酸鉄(III)。
- 上記鉄化合物とリン酸との反応を、8%〜23%の範囲内のリン酸濃度でもって行うことを特徴とする請求項1〜4のいずれか一に記載の該オルトリン酸鉄(III)。
- 存在する鉄(II)のすべてを酸化するのを、過酸化水素(H2O2)を添加することにより、あるいは、空気、純酸素又はオゾンを供給することにより行うものであることを特徴とする請求項1〜5のいずれか一に記載の該オルトリン酸鉄(III)。
- 上記反応混合物からの分離処理の後、当該オルトリン酸鉄(III)を昇温下及び/又は減圧下に乾燥せしめることを特徴とする請求項1〜6のいずれか一に記載の該オルトリン酸鉄(III)。
- メタストレング石II(metastrengite II)〔斜燐鉄鉱、フォスフォシデライト(phosphosiderite)〕結晶構造中に > 80 wt%の当該オルトリン酸鉄(III)、好ましくは > 90 wt%の当該オルトリン酸鉄(III)、特に好ましくは > 95 wt%の当該オルトリン酸鉄(III)が存在しているものであることを特徴とする請求項1〜7のいずれか一に記載の該オルトリン酸鉄(III)。
- 少なくとも一つの寸法において、それは < 1μmの平均一次粒子径、好ましくは < 500nmの平均一次粒子径、特に好ましくは <100nmの平均一次粒子径を有しているものであることを特徴とする請求項1〜8のいずれか一に記載の該オルトリン酸鉄(III)。
- それは、 > 600 g/lのバルク密度、好ましくは > 800 g/lのバルク密度、特に好ましくは > 1000 g/lのバルク密度を有しているものであることを特徴とする請求項1〜9のいずれか一に記載の該オルトリン酸鉄(III)。
- それは、ナトリウム含有量及びカリウム含有量がそれぞれ < 300 ppmであるものであることを特徴とする請求項1〜10のいずれか一に記載の該オルトリン酸鉄(III)。
- それは、 < 300 ppmの硫黄含有量を持つものであることを特徴とする請求項1〜11のいずれか一に記載の該オルトリン酸鉄(III)。
- それは、 < 100 ppmの硝酸塩含有量を持つものであることを特徴とする請求項1〜12のいずれか一に記載の該オルトリン酸鉄(III)。
- Liイオン蓄電池用LiFePO4正極材を製造するために請求項1〜13のいずれか一に記載の該オルトリン酸鉄(III)を使用することを特徴とする請求項1〜13のいずれか一に記載の該オルトリン酸鉄(III)の用途。
- 請求項1〜14のいずれか一に記載の該オルトリン酸鉄(III)を使用することを特徴とするLiイオン蓄電池用LiFePO4正極材。
- 請求項1〜13のいずれか一に記載の該オルトリン酸鉄(III)を製造することを特徴とするオルトリン酸鉄(III)の製造法。
- 請求項15に記載のLiFePO4正極材を有しているLiイオン蓄電池。
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DE102007049757A DE102007049757A1 (de) | 2007-10-16 | 2007-10-16 | Eisen(III)orthophosphat für Li-Ionen-Akkumulatoren |
PCT/EP2008/063348 WO2009050055A2 (de) | 2007-10-16 | 2008-10-06 | Eisen(iii)orthophosphat für li-ionen-akkumulatoren |
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JP2012518594A (ja) * | 2009-02-26 | 2012-08-16 | ケミスケ ファブリック ブデンヘイム ケージー | オルトリン酸鉄の製造 |
JP2013505193A (ja) * | 2009-09-18 | 2013-02-14 | エー123 システムズ, インコーポレイテッド | リン酸第二鉄およびその調製の方法 |
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US9954228B2 (en) | 2009-09-18 | 2018-04-24 | A123 Systems, LLC | High power electrode materials |
JP2011192500A (ja) * | 2010-03-15 | 2011-09-29 | Gs Yuasa Corp | 非水電解質二次電池 |
JP2014510005A (ja) * | 2011-01-25 | 2014-04-24 | ケミッシュ ファブリーク ブーデンハイム カーゲー | オルトリン酸鉄(iii)−炭素複合材 |
US9437868B2 (en) | 2011-01-25 | 2016-09-06 | Chemische Fabrik Budenheim Kg | Iron (III) orthophosphate-carbon composite |
JP2014203589A (ja) * | 2013-04-02 | 2014-10-27 | 旭化成株式会社 | 非水電解質二次電池用正極活物質及び非水電解質二次電池 |
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US20110117003A1 (en) | 2011-05-19 |
CA2698550A1 (en) | 2009-04-23 |
CA2698550C (en) | 2015-03-03 |
CN101821197B (zh) | 2013-07-10 |
US8609056B2 (en) | 2013-12-17 |
RU2479485C2 (ru) | 2013-04-20 |
RU2010119411A (ru) | 2012-01-27 |
BRPI0818660B1 (pt) | 2019-03-26 |
HK1147240A1 (en) | 2011-08-05 |
CN101821197A (zh) | 2010-09-01 |
JP5528346B2 (ja) | 2014-06-25 |
WO2009050055A2 (de) | 2009-04-23 |
EP2203383A2 (de) | 2010-07-07 |
KR101547137B1 (ko) | 2015-08-25 |
TWI457273B (zh) | 2014-10-21 |
DE102007049757A1 (de) | 2009-04-23 |
WO2009050055A3 (de) | 2009-06-04 |
TW200925107A (en) | 2009-06-16 |
EP2203383B1 (de) | 2016-07-20 |
ES2588030T3 (es) | 2016-10-28 |
KR20100083773A (ko) | 2010-07-22 |
BRPI0818660A2 (pt) | 2015-09-15 |
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