CN101807690B - Preparation method of lithium ion battery ferric metasilicate lithium positive electrode material - Google Patents
Preparation method of lithium ion battery ferric metasilicate lithium positive electrode material Download PDFInfo
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- CN101807690B CN101807690B CN2010101483542A CN201010148354A CN101807690B CN 101807690 B CN101807690 B CN 101807690B CN 2010101483542 A CN2010101483542 A CN 2010101483542A CN 201010148354 A CN201010148354 A CN 201010148354A CN 101807690 B CN101807690 B CN 101807690B
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 38
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 230000005855 radiation Effects 0.000 claims abstract description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000006230 acetylene black Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 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
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 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 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 229940062993 ferrous oxalate Drugs 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 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
- YNQRWVCLAIUHHI-UHFFFAOYSA-L dilithium;oxalate Chemical compound [Li+].[Li+].[O-]C(=O)C([O-])=O YNQRWVCLAIUHHI-UHFFFAOYSA-L 0.000 claims description 2
- 229940116007 ferrous phosphate Drugs 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 229910000155 iron(II) phosphate Inorganic materials 0.000 claims description 2
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 claims description 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
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 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
- 239000013078 crystal Substances 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 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 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
Abstract
The invention provides a preparation method of a lithium ion battery ferric metasilicate lithium positive electrode material, which comprises the following steps: A. mixing basic raw materials of lithium source compounds, iron source compounds and silicon dioxide according to a mol ratio of Fi : Fe : Si = 2 : 1 : 1, adding heat conducting agents which account for 2 to 40 percent of the total mass of the basic raw materials, and carrying out grinding; and B. pressing ground materials into blocks after drying, placing the blocks into a crucible provided with active carbon, and then, placing the crucible into microwaves for radiation heating for 2 to 30 minutes to obtain the ferric metasilicate lithium positive electrode material. The positive electrode material prepared by the preparation method of the lithium ion battery ferric metasilicate lithium positive electrode material has the excellent microstructure, the grains are fine and are uniformly distributed, and the electrochemical performance is excellent. The invention has the advantages of simple preparation technology, short flow process, easy operation and low equipment investment, and can be widely used for the production of various lithium ion batteries.
Description
Technical field
The invention belongs to technical field of lithium-ion battery, specially refer to a kind of preparation method of anode material for lithium-ion batteries.
Background technology
Since Li/LiCoO
2Since the battery industryization; Lithium ion battery with its high-energy-density, high discharge voltage, specific capacity is big, self-discharge rate is low, memory-less effect and advantage such as pollution-free receive the extensive concern of countries in the world, especially iron is that positive electrode has aboundresources, low price, nontoxic, environmental friendliness, Heat stability is good, completeness advantages of higher.The iron of using at present is that positive electrode mainly contains LiFePO4 (LiFePO
4) and ferric metasilicate lithium (Li
2FeSiO
4).Since element silicon on earth content first in the element, the environment and the mankind all are safe from harm and Li
2FeSiO
4With respect to LiFePO
4Have cost of material cheaper, with advantages such as the compatibility of environment is better, so Li
2FeSiO
4Be expected to become the anode material for lithium-ion batteries of a new generation.
At present, the Li of bibliographical information
2FeSiO
4Typical preparation method have that high temperature solid-state is synthetic, sol-gel process and hydro thermal method etc.People such as A.Nyten are being raw material through high temperature solid-state method with lithium metasilicate, ferrous oxalate and tetraethoxysilane, mix the back at CO/CO
2The following 750 ℃ of reaction 24h high temperature of atmosphere have synthesized Li
2FeSiO
4/ C composite material.At 60 ℃, discharge and recharge at 2.0-3.7V with the 1/16C electric current, discharge capacity is 130mAh/g.People such as R.Dominko are dispersed in lithium hydroxide solution with silicon dioxide through ultrasonic assisting; Mix with solution of ferrous chloride then; More than 150 ℃ of isothermal reaction 72h, the powder that obtains is used the distilled water cyclic washing under Ar atmosphere, obtain Li after the drying in airtight autoclave
2FeSiO
4Powder, but the material electrochemical performance that obtains is relatively poor, discharges and recharges at 2.0-4.2V with 1/30C multiplying power electric current under the room temperature, and reversible capacity is about 91mAh/g.People such as R.Dominko are with mixture, the CH of ironic citrate, ferric nitrate
3COOLi and SiO
2Powder is a raw material, in ultrasonic water bath, prepares gel, through dry, grinds the back in obtaining Li behind the reaction 1h under 700 ℃ the inert atmosphere
2FeSiO
4, at 60 ℃, discharging and recharging at 2.0-3.8V with the 1/20C electric current, reversible capacity is about 110mAh/g, and shows cyclical stability preferably.
In the middle of the above-mentioned synthetic method; Traditional high temperature solid phase synthesis needs higher synthesis temperature; Obtain material grains and particle is big, be unfavorable for the raising of ferric metasilicate lithium chemical property, and hydro thermal method, sol-gel process are difficult to industrial applications; And it is low to obtain powder body material density, is unfavorable for improving the volume of battery energy density.Therefore, research and development have the Li of good electrical chemical property and higher density concurrently
2FeSiO
4The preparation method of/C positive electrode is for promoting Li
2FeSiO
4The research and development of positive electrode and industrialization process promote the development of lithium ion battery, electric motor car and related industry that significance is arranged.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of lithium ion battery ferric metasilicate lithium positive electrode material, the ferric metasilicate lithium positive electrode material that this preparation method is easy to industrialization, prepare is mutually even, and the generation cycle is short, saves energy consumption.
The preparation method of lithium ion battery ferric metasilicate lithium positive electrode material of the present invention comprises the steps:
A: 2: 1: 1 the ratio of mol ratio according to Li: Fe: Si is mixed basic material Li source compound, Fe source compound and silicon dioxide, and adds the thermal conducting agent that quality accounts for above-mentioned basic material gross mass 2%-40%, grinds;
B: the material after the grinding is pressed into bulk after drying, puts into the crucible that active carbon is housed, and again crucible is placed the microwave radiation heating 2~30 minutes, can make ferric metasilicate lithium positive electrode material.
The ferric metasilicate lithium positive electrode material electric conductivity that generates for making is better; In the said steps A; Also add the carbon-source cpd that quality accounts for basic material gross mass 0.1%-20% and grind, the ferric metasilicate lithium positive electrode material for preparing is like this coated by carbon, has improved conductivity.
For guaranteeing grinding effect, grind as dispersant with absolute ethyl alcohol in the said steps A.
Li source compound described in the steps A is one or more in lithium hydroxide, lithium carbonate, lithium oxalate, lithium acetate, lithium chloride, the lithium nitrate.
Fe source compound described in the steps A is one or more in ferrous oxalate, frerrous chloride, ferrous phosphate, the ferrous acetate.
Thermal conducting agent described in the steps A is one or more in acetylene black, active carbon, the graphite.
Carbon-source cpd described in the steps A is one or more in polyethylene, sucrose, glucose, the starch.
The prepared positive electrode of the preparation method of lithium ion battery ferric metasilicate lithium positive electrode material of the present invention has good microstructure, and particle is tiny and be evenly distributed, and its chemical property is good; Preparation technology is simple, flow process is short, processing ease, equipment investment are less, can be widely used in the production of all kinds of lithium ion batteries.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the ferric metasilicate lithium positive electrode material that coats of the carbon for preparing of embodiment, and wherein curve A is the collection of illustrative plates of embodiment 1, and curve B is the collection of illustrative plates of embodiment 2
Fig. 2 is the electron microscope scanning collection of illustrative plates of the ferric metasilicate lithium positive electrode material that coats of the carbon of embodiment 1 preparation;
Fig. 3 is the electron microscope scanning collection of illustrative plates of the ferric metasilicate lithium positive electrode material that coats of the carbon of embodiment 2 preparation;
Fig. 4 is that ferric metasilicate lithium positive electrode material that the carbon for preparing of embodiment coats is processed behind the button cell at the cycle performance collection of illustrative plates of constant current 0.1C, and wherein curve C is the collection of illustrative plates of embodiment 1, and curve D is the collection of illustrative plates of embodiment 2.
Embodiment
Specify the present invention below in conjunction with specific embodiment and accompanying drawing.
Embodiment 1:
Preparation method's step of the lithium ion battery ferric metasilicate lithium positive electrode material of present embodiment is following: with basic material Li
2CO
3, FeC
2O
42H
2O, SiO
2Mixed in 1: 1: 1 in molar ratio; Adding quality again is the carbon-source cpd sucrose of basic material quality 10% and the thermal conducting agent acetylene black that quality is basic material quality 0.5%, makes the abundant ground and mixed of dispersant with ethanol, and dry back depresses to the bulk that thickness is 1.5cm at 10MPa pressure; Place the crucible that active carbon is housed then; Again crucible is placed microwave oven, the low knot 5min that burns obtains the ferric metasilicate lithium positive electrode material that carbon coats.
Shown in the curve A among Fig. 1, the ferric metasilicate lithium positive electrode material that the carbon that present embodiment obtains coats is single ferric metasilicate lithium thing phase, and the crystal property of product is good.
As shown in Figure 2, the material particle size of the ferric metasilicate lithium positive electrode material that the carbon that present embodiment obtains coats is tiny, is about 100nm, and is evenly distributed.
Be test performance; The ferric metasilicate lithium positive electrode material that the above-mentioned carbon that obtains coats is processed battery; Its concrete steps are following: the material of gained is mixed according to mass ratio with conductive agent acetylene black, binding agent PVDF (Kynoar) respectively at 80: 10: 10, with NMP (1-Methyl-2-Pyrrolidone) this mixture is modulated into slurry, evenly be coated on the aluminium foil; 80 ℃ of vacuumize 24 hours makes Experimental cell and uses positive plate.With the lithium sheet is negative pole, and electrolyte is 1mol/LLiPF
6EC (ethyl carbonate ester)+DMC (dimethyl carbonate) (volume ratio 1: 1) solution, barrier film is the celgard2400 film, in being full of the glove box of argon gas atmosphere, is assembled into CR2025 type button cell.
Carry out the cycle performance test after being assembled into battery; Shown in the curve C among Fig. 4, reached 122mAh/g in the first discharge specific capacity of 0.1C, circulating, specific capacity is 120mAh/g after 20 times; Capability retention explains that near 98% this material has excellent cycle performance.
Embodiment 2:
Preparation method's step of the lithium ion battery ferric metasilicate lithium positive electrode material of present embodiment is following: with basic material LiOH, FeC
2O
42H
2O, SiO
2Mixed in 2: 1: 1 in molar ratio; Adding quality again is the coating glucose of basic material quality 10% and the thermal conducting agent active carbon that quality is basic material quality 0.5%, makes the abundant ground and mixed of dispersant with ethanol, and dry back depresses to the bulk that thickness is 1.3cm at 10MPa pressure; Place the crucible that active carbon is housed; Again crucible is placed microwave oven, the low knot 7min that burns obtains the ferric metasilicate lithium positive electrode material that carbon coats.
Shown in the curve B among Fig. 1, the ferric metasilicate lithium positive electrode material that the carbon that present embodiment obtains coats is single ferric metasilicate lithium thing phase, and the crystal property of product is good.
As shown in Figure 3, the material particle size of the ferric metasilicate lithium positive electrode material that the carbon that present embodiment obtains coats is tiny, is about 70nm, and is evenly distributed.
Method according to embodiment 1 is processed the ferric metasilicate lithium positive electrode material of the above-mentioned carbon coating that obtains battery and is carried out the cycle performance test, and shown in curve D among Fig. 4, the material first discharge specific capacity has reached 125mAh/g, and cycle performance is also fine.
Claims (5)
1. the preparation method of a lithium ion battery ferric metasilicate lithium positive electrode material is characterized in that comprising the steps:
A: 2: 1: 1 the ratio of mol ratio according to Li: Fe: Si is mixed basic material Li source compound, Fe source compound and silicon dioxide; And the adding quality accounts for the thermal conducting agent of above-mentioned basic material gross mass 2%-40%; The carbon-source cpd that quality accounts for basic material gross mass 0.1%-20% grinds, and described carbon-source cpd is one or more in polyethylene, sucrose, glucose, the starch;
B: the material after the grinding is pressed into bulk after drying, puts into the crucible that active carbon is housed, and again crucible is placed the microwave radiation heating 2~30 minutes, can make ferric metasilicate lithium positive electrode material.
2. the preparation method of lithium ion battery ferric metasilicate lithium positive electrode material according to claim 1 is characterized in that grinding as dispersant with absolute ethyl alcohol in the said steps A.
3. the preparation method of lithium ion battery ferric metasilicate lithium positive electrode material according to claim 1 and 2 is characterized in that the Li source compound described in the steps A is one or more in lithium hydroxide, lithium carbonate, lithium oxalate, lithium acetate, lithium chloride, the lithium nitrate.
4. the preparation method of lithium ion battery ferric metasilicate lithium positive electrode material according to claim 1 and 2 is characterized in that the Fe source compound described in the steps A is one or more in ferrous oxalate, frerrous chloride, ferrous phosphate, the ferrous acetate.
5. the preparation method of lithium ion battery ferric metasilicate lithium positive electrode material according to claim 1 and 2 is characterized in that the thermal conducting agent described in the steps A is one or more in acetylene black, active carbon, the graphite.
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CN102709561A (en) * | 2012-06-19 | 2012-10-03 | 中国科学院福建物质结构研究所 | Preparation method of carbon nano-Li2FeSiO4 composite cathode material |
CN103342369A (en) * | 2013-06-08 | 2013-10-09 | 合肥国轩高科动力能源股份公司 | Method for synthesizing silicate cathode material by taking rice husk as raw material |
CN104425819B (en) * | 2013-09-09 | 2016-06-29 | 国家纳米科学中心 | A kind of preparation method of the ferric metasilicate lithium as anode material for lithium-ion batteries |
CN110993923B (en) * | 2019-12-26 | 2021-11-23 | 湖北亿纬动力有限公司 | Carbon-coated auxiliary sodium-titanium double-doped lithium iron silicate positive electrode material and preparation method and application thereof |
CN111547731A (en) * | 2020-05-20 | 2020-08-18 | 西安工业大学 | Three-dimensional carbon nano tube composite lithium iron silicate microsphere and preparation method thereof |
CN112090382A (en) * | 2020-08-28 | 2020-12-18 | 江苏富矿智能科技有限公司 | Novel size mixing device for lithium ion battery production and size mixing method thereof |
CN114464790B (en) * | 2022-01-25 | 2023-06-02 | 四川金汇能新材料股份有限公司 | Pre-lithiated silica composite material, preparation method and application |
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