CN105226274A - A kind of preparation method of LiFePO4/graphene composite material of graphene uniform dispersion - Google Patents
A kind of preparation method of LiFePO4/graphene composite material of graphene uniform dispersion Download PDFInfo
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The present invention relates to the preparation method of the LiFePO4/graphene composite material of a kind of graphene uniform dispersion, comprise the following steps: undertaken pre-dispersedly obtaining slurry by ferric lithium phosphate precursor, with identical dispersant solution, shitosan dispersant is added to Graphene and carries out ultrasonicly pre-dispersedly obtaining Graphene slurry.The alkene slurry of extra-fine grinding admixed graphite again and ferric lithium phosphate precursor slurry, realize Graphene slurry and ferric lithium phosphate precursor slurry is miscible, dry through fast spraying, obtains LiFePO4/graphene composite material after calcining.Present invention process process is simple, be easy to realize suitability for industrialized production, the LiFePO4 obtained/graphene composite material electrochemical performance, especially the powder resistance rate of material obtains and effectively reduces, polarization reduces, coulombic efficiency obviously promotes first, is with a wide range of applications in power lithium-ion battery field.
Description
Technical field
The present invention relates to electrochemical material preparation and new energy field, particularly relate to the preparation method of the LiFePO4/graphene composite material of a kind of graphene uniform dispersion.
Background technology
Along with increasingly sharpening of energy crisis, new renewable resource is all being found in the whole world, and renewable resource such as solar energy, wind energy, tidal energy, geothermal energy etc. have the advantages that region drinks timeliness.Make full use of these resources, need intelligent grid or large-scale energy-storage system.Lithium ion battery has good application prospect as energy storage electromotive force.On the other hand, the exhaustion day by day of fossil energy forces people to develop hybrid electrically or pure electric vehicle, and its core component battery becomes research emphasis.Lithium ion is its higher energy density compared with other batteries, good fail safe and longer useful life and to be standbyly popular.
LiFePO 4 material is as anode material for lithium-ion batteries, and the advantage such as, Heat stability is good moderate with its abundant raw material, cheap, environmental protection, operating voltage, causes the extensive concern of people.But the poorly conductive of LiFePO 4 material, lithium ion diffusion rate is slow, and lithium iron phosphate dynamic battery can not meet the demand of market to electric motor car high current charge-discharge.Graphene, as a kind of novel two-dimension nano materials, is the Two Dimensional Free state atomic crystal of the unique existence found at present.Graphene due to its special nanostructure and excellence physical and chemical performance and show huge application potential in fields such as electronics, optics, catalysis, energy storage.Field of lithium ion battery, Many researchers is by carrying out compound to promote the conductivity etc. of electrode material by grapheme material and existing battery material system.
Patent CN103855391A discloses fluorophosphoric acid iron lithium/graphene composite material and its preparation method and application.Obtain ferric phosphate after preparing precursor powder calcining by Fe source compound and phosphate compounds grinding, by ferric phosphate and graphite oxide, lithium fluoride through ground and mixed, after calcining, obtain fluorophosphoric acid iron lithium/graphene composite material.Patent CN103872287A discloses a kind of grapheme lithium iron phosphate battery anode composite material and preparation method thereof, high-temperature solid phase reaction method is first utilized to prepare carbon-coated LiFePO 4 for lithium ion batteries positive electrode, again carbon-coated LiFePO 4 for lithium ion batteries material and grapheme material are carried out ball milling dispersion with alcohol or pure water for dispersant, cool grinding after the oven dry of 60-120 degree and obtain grapheme lithium iron phosphate battery anode composite material.Patent CN101562248A discloses lithium ion battery anode material lithium iron phosphate of a kind of Graphene compound and preparation method thereof.By 0.1-2.5% Graphene and the abundant mixed calcining of graphene oxide of nano-grade lithium iron phosphate pure phase powder and LiFePO4 weight ratio or iron content, lithium and phosphate radical are fully mixed rear calcining according to certain mol proportion and by the raw material of LiFePO4 weight ratio 0.5-5% Graphene or graphene oxide.Above-mentioned patent has a common feature, Graphene or graphene oxide and LiFePO 4 material and ferric lithium phosphate precursor are carried out simple ball milling be dry mixed or add absolute ethyl alcohol, pure water ball milling mixes.Dry powder ball milling inherently exists and is difficult to homodisperse feature.Consider that Graphene has specific area large, be easy to the feature of reuniting, therefore common wet ball grinding is also difficult to well disperse Graphene.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method of the LiFePO4/graphene composite material providing a kind of graphene uniform to disperse.
Following technical scheme is adopted in order to solve the problems of the technologies described above the present invention:
A preparation method for the LiFePO4/graphene composite material of graphene uniform dispersion, comprises the following steps:
(1) be 0.5% ~ 3.5% take dispersant and be dissolved in deionized water and prepare dispersant solution according to dispersant mass fraction, according to mol ratio Li:Fe=, (0.98 ~ 1.0 (2): 1 takes ferric phosphate raw material and lithium source joins in dispersant solution again, the solid content controlling slurry is 25% ~ 45%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry;
(2) water soluble chitosan is taken, being dissolved in dispersant mass fraction is in the dispersant solution of 0.5% ~ 3.5%, obtain shitosan dispersant blend solution, wherein the mass concentration of shitosan is 0.5% ~ 2%, taking graphene powder again joins in above-mentioned chitosan solution, the mass concentration controlling Graphene is 3% ~ 5%, after ultrasonic disperse, namely obtain Graphene slurry;
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 0.5% ~ 2% of theoretical LiFePO4 output adds according to Graphene content, after extra-fine grinding is about 30min, slurry spraying dry obtains presoma;
(4) presoma of above-mentioned acquisition is placed in 350 ~ 500 DEG C of insulation 3h under inert atmosphere protection, namely 700 ~ 750 DEG C of insulation 10h obtain LiFePO4/graphene composite material.
Preferably, the dispersant in step (1) is one in polyvinylpyrrolidone, polyvinyl alcohol or both combinations, and the molecular weight of polyvinylpyrrolidone, polyvinyl alcohol is 50000 to 80000.
Preferably, the lithium source in step (1) is the combination of a kind of in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride or at least two kinds.
Preferably, the deacetylation of the shitosan in step (2) is 50% ~ 60%, and the molecular weight of shitosan is 80000 ~ 100000.
Preferably, the inert gas in step (4) is one or more in helium, nitrogen and argon gas.
The invention has the beneficial effects as follows: present invention process process is simple, be easy to realize suitability for industrialized production, the LiFePO4 obtained/graphene composite material electrochemical performance, especially the powder resistance rate of material obtains and effectively reduces, polarization reduces, coulombic efficiency obviously promotes first, is with a wide range of applications in power lithium-ion battery field.Undertaken pre-dispersedly obtaining slurry by ferric lithium phosphate precursor, with identical dispersant solution, shitosan dispersant is added to Graphene and carries out ultrasonicly pre-dispersedly obtaining Graphene slurry.The alkene slurry of extra-fine grinding admixed graphite again and ferric lithium phosphate precursor slurry, realize Graphene slurry and ferric lithium phosphate precursor slurry is miscible, dry through fast spraying, obtains LiFePO4/graphene composite material after calcining.Wherein used dispersant and shitosan not only play good dispersion effect to ferric lithium phosphate precursor, Graphene, and it is also the carbon source of LiFePO 4 material preparation process.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of LiFePO4/graphene composite material that embodiment 3 obtains;
Fig. 2 be embodiment 3 with LiFePO4/graphene composite material 0.2C multiplying power of obtaining in the LiFePO4/graphene composite material obtained and comparative example under to discharge curve comparison figure, wherein, a is by being obtained LiFePO4/graphene composite material in embodiment 3, and b is the LiFePO4/graphene composite material obtained in comparative example.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
(1) be 0.5% take PVP and be dissolved in deionized water and prepare PVP solution according to PVP mass fraction, appropriate ferric phosphate raw material is taken again and lithium carbonate joins in PVP solution according to mol ratio Li:Fe=0.98:1, the solid content controlling slurry is 45%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry.
(2) take appropriate water soluble chitosan, being dissolved in mass fraction is in the PVP solution of 0.5%, obtains shitosan, PVP blend solution.Wherein the mass concentration of shitosan is 0.5%, then takes appropriate graphene powder and join in above-mentioned shitosan, PVP solution, and the mass concentration controlling Graphene is 3%, after ultrasonic disperse, namely obtain Graphene slurry.
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment and carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 0.5% of theoretical LiFePO4 output adds according to Graphene content.After extra-fine grinding is about 30min, slurry spraying dry obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 350 degree of insulation 3h under inert atmosphere protection, namely 700 insulation 10h obtain LiFePO4/graphene composite material.
The powder resistance rate of this composite material is 80 Ω ﹒ cm, and button electrical testing first coulombic efficiency is 97.5%.
Embodiment 2
(1) be 1.5% take PVA and be dissolved in deionized water and prepare PVA solution according to PVA mass fraction, appropriate ferric phosphate raw material is taken again and lithium hydroxide joins in PVA solution according to mol ratio Li:Fe=1.0:1, the solid content controlling slurry is 35%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry.
(2) take appropriate water soluble chitosan, being dissolved in mass fraction is in the PVA solution of 1.5%, obtains shitosan, PVA blend solution.Wherein the mass concentration of shitosan is 1.0%, then takes appropriate graphene powder and join in above-mentioned shitosan, PVA solution, and the mass concentration controlling Graphene is 3.5%, after ultrasonic disperse, namely obtain Graphene slurry.
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment and carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 1.5% of theoretical LiFePO4 output adds according to Graphene content.After extra-fine grinding is about 30min, slurry spraying dry obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 400 degree of insulation 3h under inert atmosphere protection, namely 710 insulation 10h obtain LiFePO4/graphene composite material.
The powder resistance rate of this composite material is 42.1 Ω ﹒ cm, and button electrical testing first coulombic efficiency is 98.2%.
Embodiment 3
(1) be 2.0% take PVP and be dissolved in deionized water and prepare PVP solution according to PVP mass fraction, appropriate ferric phosphate raw material is taken again and lithium carbonate joins in PVP solution according to mol ratio Li:Fe=1.01:1, the solid content controlling slurry is 40%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry.
(2) take appropriate water soluble chitosan, being dissolved in mass fraction is in the PVP solution of 2.0%, obtains shitosan, PVP blend solution.Wherein the mass concentration of shitosan is 1.5%, then takes appropriate graphene powder and join in above-mentioned shitosan, PVP solution, and the mass concentration controlling Graphene is 4.5%, after ultrasonic disperse, namely obtain Graphene slurry.
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment and carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 1.5% of theoretical LiFePO4 output adds according to Graphene content.After extra-fine grinding is about 30min, slurry spraying dry obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 450 degree of insulation 3h under inert atmosphere protection, namely 730 insulation 10h obtain LiFePO4/graphene composite material.
The powder resistance rate of this composite material is 26.9 Ω ﹒ cm, and button electrical testing first coulombic efficiency is 99.6%.
Embodiment 4
(1) be 3.5% take PVA and be dissolved in deionized water and prepare PVA solution according to PVA mass fraction, appropriate ferric phosphate raw material is taken again and lithium hydroxide joins in PVA solution according to mol ratio Li:Fe=1.02:1, the solid content controlling slurry is 25%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry.
(2) take appropriate water soluble chitosan, being dissolved in mass fraction is in the PVA solution of 3.5%, obtains shitosan, PVA blend solution.Wherein the mass concentration of shitosan is 2%, then takes appropriate graphene powder and join in above-mentioned shitosan, PVA solution, and the mass concentration controlling Graphene is 5%, after ultrasonic disperse, namely obtain Graphene slurry.
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment and carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 2% of theoretical LiFePO4 output adds according to Graphene content.After extra-fine grinding is about 30min, slurry spraying dry obtains presoma.
(4) presoma of above-mentioned acquisition is placed in 500 degree of insulation 3h under inert atmosphere protection, namely 750 insulation 10h obtain LiFePO4/graphene composite material.
The powder resistance rate of this composite material is 35.7 Ω ﹒ cm, and button electrical testing first coulombic efficiency is 98.9%.
Comparative example
(1) take in appropriate ferric phosphate raw material and lithium carbonate deionized water according to mol ratio Li:Fe=1.01:1, the solid content controlling slurry is 40%, joins in Ball-stirring mill, carries out grinding stir process and obtain ferric lithium phosphate precursor slurry.
(2) be that 1.5% of theoretical LiFePO4 output takes appropriate graphene powder according to Graphene content, join in ferric lithium phosphate precursor slurry.After extra-fine grinding is about 30min, slurry spraying dry obtains presoma.
(3) presoma of above-mentioned acquisition is placed in 450 degree of insulation 3h under inert atmosphere protection, namely 730 insulation 10h obtain LiFePO4/graphene composite material.
The powder resistance rate of this composite material is 339.5 Ω ﹒ cm, and button electrical testing first coulombic efficiency is 95.4%.
Button electricity makes and test
The composite material obtained in embodiment 3 and comparative example is all assembled into 2016 type button cells and carries out charge-discharge performance test.According to quality than active material (positive electrode): acetylene black: binding agent (PVDF)=80:10:10, add NMP, prepare anode sizing agent, be evenly coated on aluminium foil and obtain anode pole piece, employing metal lithium sheet is cathode pole piece, 1mol/LLiPF
6being dissolved in ethylene carbonate (EC)+dimethyl carbonate (DMC) (volume ratio is 1: 1) is electrolyte, and Celgard2300 film is barrier film, assembles in argon gas glove box.Button electricity carries out charge-discharge test in 2.0V ~ 4.0V voltage range.From above-described embodiment and comparative example's test result, the LiFePO4/graphene composite material adopting the method for this patent to prepare has lower powder resistance rate and higher coulombic efficiency first.From the contrast first charge-discharge curve of Fig. 2 obviously, compared with comparative example, the composite material button electrical testing that embodiment 3 obtains has higher specific discharge capacity, higher coulombic efficiency first, less mean voltage difference, illustrate this composite material have evenly conductive network, this is dispersed relevant with its graphene conductive network.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (5)
1. a preparation method for the LiFePO4/graphene composite material of graphene uniform dispersion, is characterized in that: comprise the following steps:
(1) be 0.5% ~ 3.5% take dispersant and be dissolved in deionized water and prepare dispersant solution according to dispersant mass fraction, according to mol ratio Li:Fe=, (0.98 ~ 1.0 (2): 1 takes ferric phosphate raw material and lithium source joins in dispersant solution again, the solid content controlling slurry is 25% ~ 45%, join in Ball-stirring mill, carry out grinding stir process and obtain ferric lithium phosphate precursor slurry;
(2) water soluble chitosan is taken, being dissolved in dispersant mass fraction is in the dispersant solution of 0.5% ~ 3.5%, obtain shitosan dispersant blend solution, wherein the mass concentration of shitosan is 0.5% ~ 2%, taking graphene powder again joins in above-mentioned chitosan solution, the mass concentration controlling Graphene is 3% ~ 5%, after ultrasonic disperse, namely obtain Graphene slurry;
(3) the ferric lithium phosphate precursor slurry in Ball-stirring mill and Graphene slurry are all transferred in extra-fine grinding equipment carry out extra-fine grinding dispersion treatment, the addition of Graphene slurry is that 0.5% ~ 2% of theoretical LiFePO4 output adds according to Graphene content, after extra-fine grinding is about 30min, slurry spraying dry obtains presoma;
(4) presoma of above-mentioned acquisition is placed in 350 ~ 500 DEG C of insulation 3h under inert atmosphere protection, namely 700 ~ 750 DEG C of insulation 10h obtain LiFePO4/graphene composite material.
2. the preparation method of the LiFePO4/graphene composite material of graphene uniform dispersion according to claim 1, it is characterized in that: the dispersant in step (1) is one in polyvinylpyrrolidone, polyvinyl alcohol or both combinations, and the molecular weight of polyvinylpyrrolidone, polyvinyl alcohol is 50000 to 80000.
3. the preparation method of the LiFePO4/graphene composite material of graphene uniform according to claim 1 dispersion, is characterized in that: the lithium source in step (1) is the combination of a kind of in lithium carbonate, lithium hydroxide, lithium acetate, lithium fluoride or at least two kinds.
4. the preparation method of the LiFePO4/graphene composite material of graphene uniform dispersion according to claim 1, it is characterized in that: the deacetylation of the shitosan in step (2) is 50% ~ 60%, the molecular weight of shitosan is 80000 ~ 100000.
5. the preparation method of the LiFePO4/graphene composite material of graphene uniform according to claim 1 dispersion, is characterized in that: the inert gas in step (4) is one or more in helium, nitrogen and argon gas.
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Cited By (9)
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CN106299360A (en) * | 2016-11-08 | 2017-01-04 | 浙江瑞邦科技有限公司 | A kind of LiFePO4/graphene composite material and its preparation method and application |
CN106711447A (en) * | 2016-12-19 | 2017-05-24 | 重庆汉岳科技发展有限公司 | Preparation method of compound graphene lithium battery positive electrode material |
CN107845792A (en) * | 2017-10-20 | 2018-03-27 | 深圳市毓丰新材料有限公司 | A kind of LiFePO4 with loose structure/graphene composite lithium ion battery positive electrode |
CN108179627A (en) * | 2017-12-28 | 2018-06-19 | 泉州迪特工业产品设计有限公司 | A kind of graphene dress materials and its manufacturing method |
CN108417801A (en) * | 2018-03-07 | 2018-08-17 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
CN110176599A (en) * | 2019-07-10 | 2019-08-27 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
CN110429277A (en) * | 2019-06-28 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability |
CN111293294A (en) * | 2020-02-22 | 2020-06-16 | 电子科技大学 | Method for synthesizing lithium iron phosphate/graphene composite material by template method in one step |
CN112694078A (en) * | 2020-12-29 | 2021-04-23 | 陕西煤业化工技术研究院有限责任公司 | Graphene-coated lithium iron phosphate composite material and preparation method thereof |
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CN106299360A (en) * | 2016-11-08 | 2017-01-04 | 浙江瑞邦科技有限公司 | A kind of LiFePO4/graphene composite material and its preparation method and application |
CN106299360B (en) * | 2016-11-08 | 2019-01-29 | 浙江瑞邦科技有限公司 | A kind of LiFePO4/graphene composite material and its preparation method and application |
CN106711447A (en) * | 2016-12-19 | 2017-05-24 | 重庆汉岳科技发展有限公司 | Preparation method of compound graphene lithium battery positive electrode material |
CN107845792A (en) * | 2017-10-20 | 2018-03-27 | 深圳市毓丰新材料有限公司 | A kind of LiFePO4 with loose structure/graphene composite lithium ion battery positive electrode |
CN108179627A (en) * | 2017-12-28 | 2018-06-19 | 泉州迪特工业产品设计有限公司 | A kind of graphene dress materials and its manufacturing method |
CN108417801A (en) * | 2018-03-07 | 2018-08-17 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
CN110429277A (en) * | 2019-06-28 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of the lithium iron phosphate positive material of high-pressure solid high rate capability |
CN110176599A (en) * | 2019-07-10 | 2019-08-27 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene In-situ reaction lithium iron phosphate positive material and preparation method thereof |
CN111293294A (en) * | 2020-02-22 | 2020-06-16 | 电子科技大学 | Method for synthesizing lithium iron phosphate/graphene composite material by template method in one step |
CN111293294B (en) * | 2020-02-22 | 2022-04-22 | 电子科技大学 | Method for synthesizing lithium iron phosphate/graphene composite material by template method in one step |
CN112694078A (en) * | 2020-12-29 | 2021-04-23 | 陕西煤业化工技术研究院有限责任公司 | Graphene-coated lithium iron phosphate composite material and preparation method thereof |
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