CN105047919B - Preparation method of lithium iron phosphate battery positive electrode material - Google Patents
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- H01M4/00—Electrodes
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- H01M2220/00—Batteries for particular applications
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- 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 iron phosphate battery positive electrode material. The method comprises the following steps: 1) preparing a lithium iron phosphate/graphene composite material by using a hydrothermal method for in-situ reaction; 2) granulating the lithium iron phosphate/graphene composite material to obtain particles of 1-10 microns; 3) and coating the graphene nanosheets on the compound by using a powder mixer, and mixing the compound electrode material and the binder to obtain the lithium battery anode material. The lithium iron phosphate/graphene composite material prepared by the method disclosed by the invention is uniform in graphene dispersion, the improvement of the conductivity of the lithium iron phosphate is facilitated, the prepared cathode material is good in conductivity and high in tap density, a large-capacity battery can be prepared, the preparation process disclosed by the invention is simple, the controllability is good, and the requirement of large-scale production can be met.
Description
Technical Field
The invention relates to a power lithium battery material, in particular to a preparation method of a lithium iron phosphate battery positive electrode material.
Background
The performance of the lithium ion battery mainly depends on anode and cathode materials, the lithium iron phosphate is a novel lithium ion battery anode material, the safety performance and the cycle life of the lithium ion battery are incomparable with those of other battery materials, the requirement of frequent charging and discharging of the electric vehicle is met, and the high-capacity lithium ion battery taking the lithium iron phosphate as the anode material is easier to be connected in series for use, so that higher power can be provided for the electric vehicle. In addition, the lithium iron phosphate has the advantages of no toxicity, no pollution, good safety performance, wide raw material source, low price, long service life and the like, and is an ideal anode material of a new generation of power lithium ion batteries.
The practical application of lithium iron phosphate is hindered by the disadvantages of low bulk density and poor conductivity. Researchers mix carbon materials such as conductive graphite in the material in order to improve the conductivity, so that the bulk density of the material is obviously reduced, and the tap density of the carbon-doped lithium iron phosphate is only 1.0-1.2 g/cm3The tap density of commercial lithium cobaltate is generally 2.0-2.4 g/cm3The low stacking density makes the volume specific capacity of the lithium iron phosphate greatly different from that of lithium cobaltate, and the prepared battery has larger volume and is difficult to be applied to practice; in addition, dopingThe conductive graphite of (2) is generally spherical, and forms a point contact with lithium iron phosphate, and the doping amount is large in order to form a good path, so that the volume of the lithium iron phosphate positive electrode material is large.
The ideal graphene is a carbon material with a single atomic layer, and most of graphene which can be industrially produced in a large scale is 1-10 atomic layers and is generally called as graphene nanosheet. The graphene nanosheets are used as the conductive material in the lithium iron phosphate lithium battery positive electrode material, so that the tap density of the lithium iron phosphate positive electrode material can be improved while the conductive performance of the lithium iron phosphate positive electrode material is ensured, the power density, the charging and discharging speed and the electric capacity of the lithium battery can be improved, and a foundation is laid for the practical application of the lithium iron phosphate lithium battery.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium iron phosphate battery positive electrode material, which solves the problems of low tap density and poor conductivity of the lithium iron phosphate positive electrode material and lays a foundation for further improving the performance of a lithium battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparing a lithium iron phosphate/graphene composite material:
a. preparing a lithium solution: dissolving a soluble lithium compound in deionized water to prepare a solution;
b. preparing a graphene dispersion liquid: uniformly dispersing graphene in deionized water through ultrasonic dispersion;
c. b, performing hydrothermal reaction, namely adding the solution obtained in the step a and the solution obtained in the step b into a magnetic stirring reaction kettle, adding ferrous sulfate and phosphoric acid according to the atomic ratio of L i, Fe and P being 1-3.5: 1, stirring, filtering, washing and drying to obtain a lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding a binder into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 micrometers;
3) preparing a lithium battery positive electrode material:
d. mixing the composite material particles obtained in the step 2) and the graphene nanosheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with a binder, homogenizing, drying, and then carrying out high-temperature vacuum treatment at 180-220 ℃.
According to the first preferable technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the soluble lithium compound is lithium acetate, lithium lactate, lithium nitrate, lithium carbonate, lithium citrate, lithium chloride or lithium oxalate.
According to the second preferable technical scheme of the preparation method of the lithium iron phosphate battery cathode material, the hydrothermal reaction is carried out at 100-200 ℃ for at least 3 h.
According to the third preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the mass ratio of the lithium iron phosphate to the graphene in the solution in the step c is 100: 1-1: 1.
According to the fourth preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the mass ratio of the lithium iron phosphate to the graphene in the solution in the step c is 20: 1.
According to the fifth preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the binder is sodium alginate, chitosan, sodium carboxymethylcellulose or polyacrylic acid.
According to the sixth preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the mass ratio of the binder in the step 2) to the lithium iron phosphate in the composite material is 1: 1-1: 50;
according to the seventh preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the mass ratio of the lithium iron phosphate to the graphene nanosheets in the composite material particles in the step d is 100: 1-1: 1.
According to the eighth preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, the mass ratio of the lithium iron phosphate to the graphene nanosheets in the composite material particles in the step d is 20: 1.
According to the ninth preferred technical scheme of the preparation method of the lithium iron phosphate battery positive electrode material, in the step e, the mass ratio of the binder to the lithium iron phosphate in the composite material is 1: 1-1: 50.
Compared with the closest prior art, the invention has the following advantages:
1) the lithium iron phosphate/graphene composite material prepared by the invention has the advantages that the graphene is uniformly distributed and coated on the surface of the composite material, so that the conductivity of the positive electrode material can be improved, the power density, the charging and discharging speed and the capacitance of a battery are improved, the using amount of the conductive material is reduced, the volume of the positive electrode material is reduced, and the discharge specific capacity is up to 169.5 mAh.g-1The specific capacity retention rate is more than 92% after 1000 cycles of 10C multiplying power;
2) the method adopts a granulation preparation process for the lithium iron phosphate/graphene composite material, improves the tap density of the anode material while ensuring the conductivity of the anode material, and reduces the volume of the conductive carbon material.
Detailed Description
The technical solution of the present invention is further described with reference to the following examples, but the scope of the present invention is not limited to the contents of the following examples.
Example 1
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 3.78g of lithium hydroxide (L iOH. H)2O, 0.09mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.1g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 15 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 160 ℃, reacting for 6 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
d. Mixing the composite material particles obtained in the step 2) and 0.05g of graphene nano sheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 200 ℃ to obtain the lithium ion battery electrode material.
Example 2
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 2.52g of lithium hydroxide (L iOH. H)2O, 0.06mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.05g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 20 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 150 ℃, reacting for 6 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
d. Mixing the composite material particles obtained in the step 2) and 0.05g of graphene nano sheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 200 ℃ to obtain the lithium ion battery electrode material.
Example 3
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 2.10g of lithium hydroxide (L iOH. H)2O, 0.05mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.05g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 15 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 150 ℃, reacting for 6 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
d. Mixing the composite material particles obtained in the step 2) and 0.05g of graphene nano sheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 200 ℃ to obtain the lithium ion battery electrode material.
Example 4
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparation ofLithium solution 3.78g of lithium hydroxide (L iOH. H)2O, 0.09mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.2g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 30 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in the stainless steel reaction kettle at 160 ℃, reacting for 8 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
d. Mixing the composite material particles obtained in the step 2) and 0.05g of graphene nano sheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 210 ℃ to obtain the lithium ion battery electrode material.
Example 5
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 3.78g of lithium hydroxide (L iOH. H)2O, 0.09mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.05g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 10 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the solution obtained in the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid(H3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 120 ℃, reacting for 12 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
d. Mixing the composite material particles obtained in the step 2) and 0.05g of graphene nano sheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 180 ℃ to obtain the lithium ion battery electrode material.
Comparative example 1
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 3.78g of lithium hydroxide (L iOH. H)2O, 0.09mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.1g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 15 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 160 ℃, reacting for 6 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) and (3) granulating the composite material: adding 1g of polyacrylic acid into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 microns;
3) preparation of lithium battery anode material
Mixing the lithium iron phosphate/graphene composite particles with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 200 ℃ to obtain the lithium ion battery electrode material.
Comparative example 2
A preparation method of a positive electrode material of a lithium iron phosphate battery comprises the following steps:
1) preparation of lithium iron phosphate/graphene composite material
a. Preparing a lithium solution by mixing 3.78g of lithium hydroxide (L iOH. H)2O, 0.09mol) is dissolved in 200ml of deionized water to prepare a lithium hydroxide solution;
b. preparing a graphene dispersion liquid: adding 0.1g of graphene nanosheet into 10ml of deionized water, and performing ultrasonic dispersion for 15 min;
c. hydrothermal reaction: adding the solution obtained in the step a and the step b into a magnetic stirring reaction kettle, uniformly stirring, and adding 2.97g of phosphoric acid (H)3PO499%, 0.03mol) and 8.34g of ferrous sulfate (FeSO)4·7H2O, 0.03mol), controlling the temperature in a stainless steel reaction kettle at 160 ℃, reacting for 6 hours, naturally cooling to normal temperature, pouring out the reaction liquid, filtering, washing and drying to obtain the lithium iron phosphate/graphene composite material;
2) preparation of lithium battery anode material
d. C, mixing the composite material obtained in the step c and 0.05g of graphene nanosheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with 1g of polyacrylic acid, adding a proper amount of water, stirring to prepare a slurry, coating the slurry on an aluminum foil current collector, drying, and performing high-temperature vacuum treatment at 200 ℃ to obtain the lithium ion battery electrode material.
The obtained positive electrode material is assembled into a 2025 button cell, the discharge capacity and the cycle performance of the button cell are tested within the voltage range of 2.5-4.2V, and the results are shown in Table 1 and implementedIn the examples, the discharge specific capacity of the obtained product is up to 169.5 mAh.g-1The specific capacity retention rate is more than 92% after 1000 cycles at the 10C rate, the combined action of graphene in the lithium iron phosphate/graphene composite material and the graphene nanosheet coated on the surface of the composite material is beneficial to improving the performance of the positive electrode material (comparative example 1 and comparative example 1), and the capacity and the cycle performance of the positive electrode material are improved by adopting a granulation process (comparative example 1 and comparative example 2).
TABLE 1
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (7)
1. A preparation method of a positive electrode material of a lithium iron phosphate battery is characterized by comprising the following steps:
1) preparing a lithium iron phosphate/graphene composite material:
a. preparing a lithium solution: dissolving a soluble lithium compound in deionized water to prepare a solution;
b. preparing a graphene dispersion liquid: uniformly dispersing graphene in deionized water through ultrasonic dispersion;
c. a step of hydrothermal reaction, which is to add the solution obtained in the step a and the step b into a reaction kettle at 100-200 ℃ under magnetic stirring, add ferrous sulfate and phosphoric acid according to an atomic ratio of L i, Fe and P being 1-3.5: 1:1, react for at least 3 hours, and then filter, wash and dry the mixture to obtain a lithium iron phosphate/graphene composite material, wherein the mass ratio of the lithium iron phosphate to the graphene in the solution is 20: 1;
2) and (3) granulating the composite material: adding a binder into the lithium iron phosphate/graphene composite material, and granulating to obtain particles with the particle size of 1-10 micrometers;
3) preparing a lithium battery positive electrode material:
d. mixing the composite material particles obtained in the step 2) and the graphene nanosheets in a powder mixer;
e. and d, mixing the lithium iron phosphate/graphene composite material coated with the graphene nanosheets obtained in the step d with a binder, homogenizing, drying, and then carrying out high-temperature vacuum treatment at 180-220 ℃.
2. The method for preparing the positive electrode material of the lithium iron phosphate battery as claimed in claim 1, wherein the soluble lithium compound is lithium acetate, lithium hydroxide, lithium nitrate, lithium carbonate, lithium chloride or lithium oxalate.
3. The method for preparing the positive electrode material of the lithium iron phosphate battery as claimed in claim 1, wherein the binder is sodium alginate, chitosan, sodium carboxymethylcellulose or polyacrylic acid.
4. The preparation method of the positive electrode material of the lithium iron phosphate battery as claimed in claim 1, wherein the mass ratio of the binder in the step 2) to the lithium iron phosphate in the composite material is 1: 1-1: 50.
5. The preparation method of the lithium iron phosphate battery positive electrode material as claimed in claim 1, wherein the mass ratio of the lithium iron phosphate to the graphene nanoplatelets in the composite material particles in the step d is 100: 1-1: 1.
6. The preparation method of the lithium iron phosphate battery positive electrode material as claimed in claim 5, wherein the mass ratio of the lithium iron phosphate to the graphene nanoplatelets in the composite material particles in the step d is 20: 1.
7. The preparation method of the positive electrode material of the lithium iron phosphate battery as claimed in claim 1, wherein the mass ratio of the binder in the step e to the lithium iron phosphate in the composite material is 1: 1-1: 50.
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| CN107394114A (en) * | 2017-07-05 | 2017-11-24 | 东莞中汽宏远汽车有限公司 | Anode material of lithium battery and preparation method thereof and lithium battery anode, lithium battery |
| CN107394139B (en) * | 2017-07-05 | 2020-06-16 | 东莞中汽宏远汽车有限公司 | Composite lithium battery positive electrode material and preparation method thereof, lithium battery positive electrode and lithium battery |
| CN107256960A (en) * | 2017-08-06 | 2017-10-17 | 长沙小新新能源科技有限公司 | A kind of composite positive pole, its preparation method and the lithium ion battery comprising the composite positive pole |
| CN107919462A (en) * | 2017-10-13 | 2018-04-17 | 苏州艾维科斯园林设备有限公司 | A kind of preparation process of the energy-efficient jetting machine of new energy lithium battery |
| CN114464809A (en) * | 2022-01-25 | 2022-05-10 | 牛墨石墨烯应用科技有限公司 | Graphene-coated lithium ion battery and preparation method thereof |
| CN116154152B (en) * | 2022-12-16 | 2023-12-26 | 贵州胜泽威化工有限公司 | Lithium iron phosphate battery positive electrode slurry and preparation method thereof |
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| CN102714306A (en) * | 2010-01-15 | 2012-10-03 | 丰田自动车株式会社 | Method for manufacturing composite positive electrode active material |
| CN102299336A (en) * | 2011-07-20 | 2011-12-28 | 彩虹集团公司 | Preparation method of lithium ion battery anode material lithium iron phosphate |
| CN104600292A (en) * | 2013-10-30 | 2015-05-06 | 北京万源工业有限公司 | Preparation method for carbon-graphene doubly modified lithium iron phosphate anode material |
| CN103872287A (en) * | 2014-03-20 | 2014-06-18 | 重庆工商大学 | Composite positive electrode material of graphene and lithium iron phosphate battery and preparation method thereof |
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