CN1971981A - High charge-discharge magnification lithium iron phosphate material used for anode of lithium ion battery and its preparation method - Google Patents
High charge-discharge magnification lithium iron phosphate material used for anode of lithium ion battery and its preparation method Download PDFInfo
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- CN1971981A CN1971981A CNA2006101301656A CN200610130165A CN1971981A CN 1971981 A CN1971981 A CN 1971981A CN A2006101301656 A CNA2006101301656 A CN A2006101301656A CN 200610130165 A CN200610130165 A CN 200610130165A CN 1971981 A CN1971981 A CN 1971981A
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- lithium
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- lithium ion
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- 239000000463 material Substances 0.000 title claims abstract description 31
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title abstract description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title abstract 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 9
- 239000010452 phosphate Substances 0.000 claims abstract description 9
- 239000004020 conductor Substances 0.000 claims abstract description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 21
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 239000008139 complexing agent Substances 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000006258 conductive agent Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 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 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 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
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 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
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 238000013019 agitation Methods 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
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- 229960001484 edetic acid Drugs 0.000 claims description 2
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 2
- 229940062993 ferrous oxalate Drugs 0.000 claims description 2
- 239000008246 gaseous mixture Substances 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
- 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
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical compound [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229920000140 heteropolymer Polymers 0.000 description 1
- 230000002427 irreversible effect Effects 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
- 239000001301 oxygen Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Images
Classifications
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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
本发明涉及一种用于锂离子电池正极的高充放电倍率的磷酸铁锂材料及其制备方法。所述磷酸铁锂材料是将一定化学计量比的锂源化合物、铁源化合物、磷酸根源化合物及导电材料于30～90℃下经由溶胶－凝胶法制得前驱体。然后将所得前驱体在惰性或弱还原性气氛下，以1～30℃·min－1的速率升温，于100～450℃下预分解0.5～5h。在相同气氛下，以1～30℃·min－1的速率升温，于450～800℃煅烧2～24h，然后以1～30℃·min－1的速率或随炉自然冷却至室温，得目标产物。本发明制备磷酸铁锂材料的工艺简单，清洁无污染，适合工业化规模生产；得到的磷酸铁锂材料比容量高，循环稳定性好，其高倍率充放电性能尤其突出。The invention relates to a high charge and discharge rate lithium iron phosphate material used for the positive electrode of a lithium ion battery and a preparation method thereof. The lithium iron phosphate material is a precursor prepared by a sol-gel method at a temperature of 30-90° C. with a certain stoichiometric ratio of lithium source compound, iron source compound, phosphate source compound and conductive material. Then the obtained precursor is heated up at a rate of 1-30°C·min -1 under an inert or weakly reducing atmosphere, and pre-decomposed at 100-450°C for 0.5-5h. Under the same atmosphere, heat up at a rate of 1-30°C·min -1 , calcinate at 450-800°C for 2-24 hours, and then cool to room temperature at a rate of 1-30°C·min -1 or naturally with the furnace to obtain the target product. The preparation process of the lithium iron phosphate material in the invention is simple, clean and pollution-free, and is suitable for industrial scale production; the obtained lithium iron phosphate material has high specific capacity, good cycle stability, and particularly outstanding high-rate charge and discharge performance.
Description
Technical field
The invention belongs to the energy and material technical field.Be particularly related to LiFePO 4 material of a kind of high charge-discharge magnification that is used for lithium ion cell positive and preparation method thereof.
Background technology
1997, Goodenough found that the LiFePO4 with olivine structural can reversibly embed and deviate from lithium ion.From then on, LiFePO4 is considered to one of selectable electrode material of lithium ion battery.Primary Study shows that this material has lot of advantages: do not contain precious metal, raw material cheapness, resource are greatly abundant; Nontoxic, environmentally friendly; Operating voltage moderate (3.4V); Platform identity is good, under little electric current, has smooth charging/discharging voltage curve, and within the specific limits, its voltage accuracy even the stabilized voltage power supply that can match in excellence or beauty are a kind of desirable anode material for lithium-ion batteries; Big (the 170mAhg of theoretical capacity
-1), Stability Analysis of Structures, security performance splendid (O and P make material be difficult to analyse oxygen and decompose with the strong covalent bond strong bonded); High-temperature behavior and good cycle; Volume-diminished during charging, the bulk effect when cooperating with carbon negative pole material is good; Good with most of electrolyte system compatibilities, storge quality is good.But, because the electronic conductivity of LiFePO4 is low, cause high-rate discharge ability poor, actual specific capacity is low, and under the bigger situation of electric current, electrode polarization is serious, causes discharging and recharging irreversible degree and strengthens, and the electrochemistry capacitance loss is serious.This brings certain difficulty for the practicality of LiFePO4.
In order to improve the electronic conductivity of LiFePO4, the main method that adopts element doping and conductive agent to coat of most of both at home and abroad research.Wherein remarkable with the conductive agent covered effect, and be easy to industrialization.In addition, synthetic method also has certain influence to the performance of LiFePO4.
Summary of the invention
Purpose of the present invention is intended to solve the technical barrier of above-mentioned present stage, and LiFePO 4 material of a kind of high charge-discharge magnification that is used for lithium ion cell positive and preparation method thereof is provided.The LiFePO 4 material of this method preparation has significantly improved the big electric current application performance of LiFePO4.
Technical scheme of the present invention discloses a kind of LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive, it is characterized in that described LiFePO 4 material comprises: press atomic ratio Li: Fe: P=0.9-1.2: 1: 1 Li source compound, Fe source compound and phosphate radical source compound, and the quality percentage composition is polyethylene glycol or the polyethylene glycol oxide conductive agent of target product LiFePO4 5%-50%.
The invention also discloses a kind of preparation method of LiFePO 4 material of the above-mentioned high charge-discharge magnification that is used for lithium ion cell positive, it is characterized in that amount of substance according to Li source compound, Fe source compound, phosphate radical source compound is than the aqueous solution that under agitation is mixed with 0.7-0.8mol/L; The electric conducting material that adds the quality percentage composition 5%-50% of relative target product LiFePO4 then, under the 30-90 ℃ of temperature, add complexing agent concentration for by amount of substance than complexing agent: (lithium+iron)=obtained colloidal sol in 1: 1 or 2: 1, further transpiring moisture is to generating gel; With the gel porphyrize that generates, under inert or week reduction protection gas, with 1-30 ℃ of min
-1Speed be warming up to 100-450 ℃, keep 0.5-5h; Be warming up to 450 ~ 800 ℃ with identical heating rate again, keep 2-24h; With 1-30 ℃ of min
-1Speed or naturally cool to room temperature with stove; Product is taken out porphyrize, promptly get the target product LiFePO4.
Advantage of the present invention and good effect are: with described polymer is the electric conducting material presoma, and at high temperature portion of hot solves carbon simple substance, and other has the polymer of not pyrolysis to can be used as stock support.The material that the adding of this conductive agent obtains has higher specific capacity, well cyclical stability and very strong high power charging-discharging ability.Adding will obtain the high material of high rate performance than heteropolymer, add less polymer and can obtain the high material of electrochemistry capacitance.By the addition of telomerized polymer, can obtain being applicable to the material of practical situation, promptly stress capacity or multiplying power.
Description of drawings
The XRD test curve of Fig. 1 LiFePO4;
The cyclic voltammetry curve in first week of Fig. 2 LiFePO4;
The multiplying power discharging property curve of Fig. 3 LiFePO4.
Embodiment
LiFePO4 of the present invention through aqueous solution, adds into the sol/gel additive by Li source compound, Fe source compound, phosphate radical source compound and electric conducting material, obtains intermediate (presoma), protects sintering to form at last.The present invention adopts following raw material:
Li source compound: lithium chloride, lithium bromide, lithium sulfide, lithium carbonate, lithium nitrate, lithium acetate or lithium hydroxide;
Fe source compound: ferrous oxide, di-iron trioxide, ferric nitrate, ferrous oxalate or ferric oxalate;
Phosphate radical source compound: ammonium phosphate, diammonium hydrogen phosphate or ammonium dihydrogen phosphate;
Electric conducting material: mean molecule quantity is 1000～20000 polyethylene glycol or polyethylene glycol oxide;
The method for preparing LiFePO4 comprises following technical process:
Take by weighing a certain amount of Li source compound, Fe source compound and phosphate radical source compound, the ratio that makes the amount of atom is Li: Fe: P=0.9～1.2: 1: 1.Stir is solution or the suspension-turbid liquid that solvent or dispersant are mixed with above-mentioned raw materials 0.1～3moldm-3 with the deionized water down.Adding under 30～90 ℃, adds an amount of complexing agent with respect to the electric conducting material of target product LiFePO4 5%～50%, obtains colloidal sol, and further transpiring moisture is to generating gel.With the gel porphyrize that generates, under inert or week reduction protection gas, be warming up to 100～450 ℃ with the speed of 1～30 ℃ of min-1; keep 0.5～5h; be warming up to 450～800 ℃ with identical heating rate, keep 2～24h, naturally cool to room temperature with the speed of 1～30 ℃ of min-1 or with stove.Product is taken out porphyrize, promptly get the target product LiFePO4.
Complexing agent can be: citric acid, tartaric acid, vitamin C or ethylenediamine tetra-acetic acid;
Protection gas can be inert protective atmosphere as nitrogen or argon gas.Protection gas also can be restitutive protection's atmosphere as 1-10% hydrogen and nitrogen mixture or 1-10% hydrogen and argon gas gaseous mixture.The protection gas velocity is 0.1～10dm
3Min
-1
Embodiment
Now further understand content of the present invention and advantage with following embodiment:
Take by weighing FeC
2O
42H
2O 17.99g, LiOHH
2O 4.196g, (NH
4)
2HPO
413.21g, PEG (M=5000) 5g.Disperseing above-mentioned raw materials with the 200mL deionized water is suspension-turbid liquid, stirs down to add citric acid (C in 60 ℃
7H
8O
7H
2O) 42.02g.Continue to be stirred to the generation gel.The agate ball mill grinding of gained gel, the porcelain crucible of packing into.At flow velocity is 1dm
3Min
-199.999% argon gas stream in, with 3 ℃ of min
-1Speed be warming up to 300 ℃, keep 3h, be warming up to 700 ℃ with the phase same rate, keep 8h.Naturally cool to room temperature with stove, take out the product porphyrize and get described LiFePO4.
Claims (10)
1. LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive, it is characterized in that described LiFePO 4 material comprises: press atomic ratio Li: Fe: P=0.9-1.2: 1: 1 Li source compound, Fe source compound and phosphate radical source compound, and the quality percentage composition is polyethylene glycol or the polyethylene glycol oxide conductive agent of target product LiFePO4 5%-50%.
2. the LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive according to claim 1 is characterized in that described Li source compound is at least a in lithium chloride, lithium bromide, lithium sulfide, lithium carbonate, lithium nitrate, lithium acetate or the lithium hydroxide.
3. the LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive according to claim 1 is characterized in that described Fe source compound is at least a in ferrous oxide, di-iron trioxide, ferric nitrate, ferrous oxalate or the ferric oxalate.
4. the LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive according to claim 1 is characterized in that described phosphate radical source compound is at least a in ammonium phosphate, diammonium hydrogen phosphate or the ammonium dihydrogen phosphate.
5. the LiFePO 4 material that is used for the high charge-discharge magnification of lithium ion cell positive according to claim 1, the mean molecule quantity that it is characterized in that described electric conducting material polyethylene glycol or polyethylene glycol oxide is 1000-20000.
6. the preparation method of the LiFePO 4 material of the described high charge-discharge magnification that is used for lithium ion cell positive of a claim 1 is characterized in that amount of substance according to Li source compound, Fe source compound, phosphate radical source compound is than the aqueous solution that under agitation is mixed with 0.7-0.8mol/L; The electric conducting material that adds the quality percentage composition 5%-50% of relative target product LiFePO4 then, under the 30-90 ℃ of temperature, add complexing agent concentration for by amount of substance than complexing agent: (lithium+iron)=obtained colloidal sol in 1: 1 or 2: 1, further transpiring moisture is to generating gel; With the gel porphyrize that generates, under inert or week reduction protection gas, with 1-30 ℃ of min
-1Speed be warming up to 100-450 ℃, keep 0.5-5h; Be warming up to 450 ~ 800 ℃ with identical heating rate again, keep 2-24h; With 1-30 ℃ of min
-1Speed or naturally cool to room temperature with stove; Product is taken out porphyrize, promptly get the target product LiFePO4.
7. the preparation method of the LiFePO 4 material of the high charge-discharge magnification that is used for lithium ion cell positive according to claim 6, it is characterized in that: described complexing agent is citric acid, tartaric acid, vitamin C or ethylenediamine tetra-acetic acid.
8. according to the preparation method of the LiFePO 4 material of claim 6 or the 7 described high charge-discharge magnifications that are used for lithium ion cell positive, it is characterized in that: described inert protective atmosphere is: nitrogen or argon gas.
9. according to the preparation method of the LiFePO 4 material of claim 6 or the 7 described high charge-discharge magnifications that are used for lithium ion cell positive, it is characterized in that: described restitutive protection's atmosphere is: 1-10% hydrogen and nitrogen mixture or 1-10% hydrogen and argon gas gaseous mixture.
10. according to Claim 8 or the preparation method of the LiFePO 4 material of the 9 described high charge-discharge magnifications that are used for lithium ion cell positive, it is characterized in that: described protective atmosphere flow velocity is 0.1～10dm
3Min
-1
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| CNA2006101301656A CN1971981A (en) | 2006-12-14 | 2006-12-14 | High charge-discharge magnification lithium iron phosphate material used for anode of lithium ion battery and its preparation method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101867043A (en) * | 2010-06-28 | 2010-10-20 | 彩虹集团公司 | Method for preparing lithium ion battery anode material of LiFePO4/C |
| CN101985351A (en) * | 2010-09-30 | 2011-03-16 | 东南大学 | Method for preparing simple and cheap lithium-ion power battery anode materials |
| CN102097616A (en) * | 2011-01-11 | 2011-06-15 | 清华大学深圳研究生院 | Preparation method of high-energy and high-power density nano-scale lithium iron phosphate powder |
| CN102208686A (en) * | 2011-05-17 | 2011-10-05 | 江苏赛尔电池有限公司 | Power battery using double-network nano lithium iron phosphate as anode |
| CN102324494A (en) * | 2010-07-20 | 2012-01-18 | 上海大象能源科技有限公司 | Lithium iron phosphate/nano powder tube oxide composite cathode material and preparation method thereof |
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