CN104852045A - Method for preparing spherical lithium iron phosphate with high polymer lattice dispersion technology - Google Patents
Method for preparing spherical lithium iron phosphate with high polymer lattice dispersion technology Download PDFInfo
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- CN104852045A CN104852045A CN201410056887.6A CN201410056887A CN104852045A CN 104852045 A CN104852045 A CN 104852045A CN 201410056887 A CN201410056887 A CN 201410056887A CN 104852045 A CN104852045 A CN 104852045A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000006185 dispersion Substances 0.000 title claims 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 description 8
- 229920000642 polymer Polymers 0.000 title abstract 3
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 125000002091 cationic group Chemical group 0.000 claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 3
- 239000011574 phosphorus Substances 0.000 claims abstract description 3
- 229920002521 macromolecule Polymers 0.000 claims description 21
- 229910010707 LiFePO 4 Inorganic materials 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-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
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 5
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 4
- 229940062993 ferrous oxalate Drugs 0.000 claims description 4
- 150000002506 iron compounds Chemical class 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
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 4
- 150000002642 lithium compounds Chemical class 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 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 2
- 229920000858 Cyclodextrin Polymers 0.000 claims description 2
- 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 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 239000006230 acetylene black Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 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
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 238000005056 compaction Methods 0.000 abstract 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- 239000011651 chromium Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- -1 ferric phosphate lithium compound Chemical class 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- AQLLBJAXUCIJSR-UHFFFAOYSA-N OC(=O)C[Na] Chemical compound OC(=O)C[Na] AQLLBJAXUCIJSR-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 229920000333 poly(propyleneimine) Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing spherical lithium iron phosphate with a high polymer lattice dispersion technology. The method comprises the following steps: grinding a lithium source compound, an iron source compound and a phosphorus source compound in a ball mill, and performing heating treatment in a protective atmosphere to obtain a precursor; and grinding the precursor, a carbon source, a high polymer lattice reagent, an anion additive and a cationic additive in a mixed way in the ball mill, performing secondary calcination treatment in the protective atmosphere, and performing ball-milling crushing treatment to obtain a spherical lithium iron phosphate product. The spherical lithium iron phosphate prepared with the method disclosed by the invention has the advantages of high compaction density, excellent processing performance, high capacity, excellent cycle performance and the like. Moreover, the method is simple and easily-controllable in process, and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of ball shape ferric phosphate lithium compound, particularly a kind of macromolecule network dispersion technology prepares the method for spherical LiFePO 4.
Background technology
The advantages such as lithium ion battery is high with its voltage, energy density large, long service life, memory-less effect and operating temperature range are wide, be rapidly spread since appearance, be widely used in the portable equipments such as mobile phone, MP3, UPS, camera, notebook computer.And along with growth in the living standard in recent years, and warm for global environment in countries in the world, the thinking of environmental protection and energy saving, electric bicycle replaces traditional vehicles just gradually, the research and development of electric automobile have been put on the schedule of future work by each big country especially, and this proposes larger challenge to high power capacity, high-power lithium ion battery.
Positive electrode is an important component part of lithium ion battery, in lithium ion battery charge and discharge process, not only to be provided in positive and negative lithium intercalation compound back and forth embedding/de-required lithium, but also the lithium will undertaken required for negative material surface formation SEI film, therefore, the key point that a kind of high performance positive electrode has become restriction lithium battery industry development now how is researched and developed.
Numerous as LiCoO
2, LiNiO
2, LiMn
2o
4, LiFePO
4in positive electrode Deng lithium battery, there is the LiFePO4 of olivine structural, due to its abundant raw material source, the advantage such as cost is low, environmental friendliness, security performance are high, specific capacity is high, discharge platform is steady, thermal stability and cycle performance are excellent, become the emphasis of current countries in the world research.In LiFePO4 preparation technology in the past, how to improve its conductivity is a difficult problem always, constrains its development.
Summary of the invention
The present invention is directed to the problems referred to above, provide a kind of method of macromolecule network dispersion technology synthesizing spherical LiFePO4.The anion of the metal cation and improvement capacity that improve circulation is incorporated into LiFePO
4inside lattice, thus obtain the spherical LiFePO 4 of function admirable.Technical characterstic of the present invention is the peptizaiton utilizing macromolecule network agent, processes under the condition of high temperature to the surface of lithium iron phosphate particles, the spheric granules of formation rule.
Principle of the present invention adds Doped anions additive, cationic additive and macromolecule network agent in the precursor obtained in pre-burning, utilize the peptizaiton of macromolecule network agent under the high temperature conditions, process is continued to lithium iron phosphate particles, make the carbon source added can be distributed to homogenizing the surface of LiFePO4, the spheric granules of formation rule.
A kind of macromolecule network dispersion technology of the present invention prepares the method for spherical LiFePO 4, comprises the following steps:
1), by Li source compound, Fe source compound and P source compound in grinding in ball grinder 0.1 ~ 10 hour, obtain mixture, in protective atmosphere, mixture is obtained precursor in 4 ~ 30 hours in 300 ~ 600 DEG C of heat treated;
2), by precursor, carbon source, macromolecule network agent, anionic additive, cationic additive mixed grinding 0.2 ~ 10 hour in ball mill; in protective atmosphere, carry out secondary clacining process 4 ~ 30 hours in 400 ~ 900 DEG C again, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
Described macromolecule network agent is one or more in polyvinyl alcohol, carboxymethyl cellulose, polyethylene glycol and polyacrylamide.
Described lithium source is one or more of lithium compound, described source of iron is one or more of iron compound, described phosphorus source is one or more of phosphate cpd, described carbon source is one or more in glucose, vitamin c, cyclodextrin, acetylene black, described cationic additive is one or more in Zn, Mg, Al, Cr, Nd, Nb element, and described anionic additive is one or both in S, F element.
Described lithium compound is lithium carbonate, lithium dihydrogen phosphate; Described iron compound is ferrous oxalate, ferric orthophosphate, iron oxide; Described phosphate cpd is ammonium dihydrogen phosphate, lithium dihydrogen phosphate, phosphoric acid.
The protective atmosphere of described heating treatment step and secondary clacining treatment process is one or more in nitrogen, argon gas and hydrogen.
The spherical LiFePO 4 utilizing method of the present invention to prepare, have the advantages such as compacted density is high, processing characteristics is excellent, capacity is high, cycle performance is excellent, and technique is simple and easy to control, is applicable to large-scale industrial production.
Embodiment
Embodiment 1:
Be that 1:1:1 prepares burden by lithium carbonate, ferrous oxalate and ammonium dihydrogen phosphate according to Li:Fe:P mol ratio, in grinding in ball grinder mixing in 2 hours, in nitrogen atmosphere, mixture obtained precursor in 25 hours in 500 DEG C of heat treated.By precursor, macromolecule network agent PVAC polyvinylalcohol, zinc oxide ZnO and lithium fluoride LiF according to the weight ratio of 1:0.03:0.01:0.01 mixed grinding 2 hours in ball mill; in protective atmosphere, carry out secondary clacining process 25 hours in 800 DEG C again, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
Embodiment 2:
Be that 1:1:1 prepares burden by lithium carbonate, iron oxide and lithium dihydrogen phosphate according to Li:Fe:P mol ratio, in grinding in ball grinder mixing in 2 hours, in nitrogen atmosphere, mixture obtained precursor in 15 hours in 500 DEG C of heat treated.By precursor, macromolecule network agent polyethylene glycol PEG, aluminium oxide Al
2o
3with lithium fluoride LiF according to the weight ratio of 1:0.03:0.01:0.02 mixed grinding 2.5 hours in ball mill, then carry out secondary clacining process 25 hours in 800 DEG C in protective atmosphere, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
Embodiment 3:
Be that 1:1:1 prepares burden by lithium carbonate, ferric orthophosphate and ammonium dihydrogen phosphate according to Li:Fe:P mol ratio, in grinding in ball grinder mixing in 2 hours, in nitrogen atmosphere, mixture obtained precursor in 20 hours in 500 DEG C of heat treated.By precursor, macromolecule network agent carboxymethyl sodium cellulosate CMC, magnesium oxide MgO and lithium fluoride LiF according to the weight ratio of 1:0.03:0.02:0.01 mixed grinding 3 hours in ball mill; in protective atmosphere, carry out secondary clacining process 25 hours in 800 DEG C again, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
Embodiment 4:
Be that 1:1:1 prepares burden by lithium carbonate, ferrous oxalate and phosphoric acid according to Li:Fe:P mol ratio, in grinding in ball grinder mixing in 3 hours, in nitrogen atmosphere, mixture obtained precursor in 15 hours in 500 DEG C of heat treated.By precursor, macromolecule network agent polypropylene amine PAM, chromium oxide Cr
2o
3with lithium fluoride LiF according to the weight ratio of 1:0.03:0.02:0.02 mixed grinding 4 hours in ball mill, then carry out secondary clacining process 20 hours in 800 DEG C in protective atmosphere, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
Experimental example:
The spherical LiFePO 4 that embodiment 1 ~ embodiment 4 is prepared and lithium ion battery negative material Delanium, take vinylidene as pole plate binding agent, make positive plate and the negative plate of lithium ion battery respectively, take microporous polypropylene membrane as electrode diaphragm, with volume ratio dimethyl carbonate: diethyl carbonate: the lithium hexafluoro phosphate of the 1mol/L of ethylene carbonate=1:1:1 is that electrolyte is assembled into lithium ion battery.
Lithium ion anode material performance table prepared by table 1 embodiment
Note: capability retention refers to the ratio of the capacity after being recycled to 1000 times and initial capacity.
Because this method utilizes the peptizaiton of macromolecule network agent, under the condition of high temperature, the surface of lithium iron phosphate particles is processed, the spheric granules of formation rule.More regular than the lithium iron phosphate particles of conventional method synthesis, good sphericity, thus there is outstanding chemical property.
Claims (5)
1. macromolecule network dispersion technology prepares a method for spherical LiFePO 4, it is characterized in that comprising the following steps:
1), by Li source compound, Fe source compound and P source compound in grinding in ball grinder 0.1 ~ 10 hour, obtain mixture, in protective atmosphere, mixture is obtained precursor in 4 ~ 30 hours in 300 ~ 600 DEG C of heat treated;
2), by precursor, carbon source, macromolecule network agent, anionic additive, cationic additive mixed grinding 0.2 ~ 10 hour in ball mill; in protective atmosphere, carry out secondary clacining process 4 ~ 30 hours in 400 ~ 900 DEG C again, finally carry out ball mill crushing process and obtain spherical LiFePO4 product.
2. a kind of macromolecule network dispersion technology according to claim 1 prepares the method for spherical LiFePO 4, it is characterized in that: described macromolecule network agent is one or more in polyvinyl alcohol, carboxymethyl cellulose, polyethylene glycol and polyacrylamide.
3. a kind of macromolecule network dispersion technology according to claim 1 prepares the method for spherical LiFePO 4, it is characterized in that: described lithium source is one or more of lithium compound, described source of iron is one or more of iron compound, described phosphorus source is one or more of phosphate cpd, described carbon source is one or more in glucose, vitamin c, cyclodextrin, acetylene black, described cationic additive is one or more in Zn, Mg, Al, Cr, Nd, Nb element, and described anionic additive is one or both in S, F element.
4. a kind of macromolecule network dispersion technology according to claim 3 prepares the method for spherical LiFePO 4, it is characterized in that: described lithium compound is lithium carbonate, lithium dihydrogen phosphate; Described iron compound is ferrous oxalate, ferric orthophosphate, iron oxide; Described phosphate cpd is ferric orthophosphate, ammonium dihydrogen phosphate, lithium dihydrogen phosphate, phosphoric acid.
5. a kind of macromolecule network dispersion technology according to claim 1 prepares the method for spherical LiFePO 4, it is characterized in that: the protective atmosphere of described heating treatment step and secondary clacining treatment process is one or more in nitrogen, argon gas and hydrogen.
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| CN201410056887.6A CN104852045A (en) | 2014-02-19 | 2014-02-19 | Method for preparing spherical lithium iron phosphate with high polymer lattice dispersion technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099103A (en) * | 2016-08-24 | 2016-11-09 | 合肥国轩电池材料有限公司 | A kind of preparation method of low-cost and high-performance LiFePO 4 material |
| CN113745521A (en) * | 2021-09-05 | 2021-12-03 | 浙江大学 | A kind of preparation method and application of zinc electrode material capable of suppressing self-discharge |
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| US20130157133A1 (en) * | 2011-11-17 | 2013-06-20 | Brookhaven Science Associates, Llc | Process for Producing Defect-Free Lithium Metal Phosphate Electrode Materials |
| CN103441271A (en) * | 2013-08-16 | 2013-12-11 | 上海微纳科技有限公司 | Anion-cation double-doped lithium iron phosphate anode material and preparation method thereof |
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| CN106099103A (en) * | 2016-08-24 | 2016-11-09 | 合肥国轩电池材料有限公司 | A kind of preparation method of low-cost and high-performance LiFePO 4 material |
| CN113745521A (en) * | 2021-09-05 | 2021-12-03 | 浙江大学 | A kind of preparation method and application of zinc electrode material capable of suppressing self-discharge |
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