Preparation method of graphene-based lithium iron phosphate positive electrode material

A technology of alkenyl iron phosphate lithium and positive electrode materials, which is applied in the direction of positive electrodes, battery electrodes, active material electrodes, etc., can solve the problems of reducing the mass of effective active materials, affecting the diffusion of lithium ions, and uneven morphology, so as to achieve improved Dispersion and uniformity, the effect of reducing energy consumption

Pending Publication Date: 2022-03-11
湖北华烯新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1) LiFePO 4 The electronic conductivity of (10 -9 S / cm) is low, much smaller than LiCoO 2 (10 -3 S / cm) and LiMnO 2 (10 - 5 S / cm) conductivity, which seriously affects the diffusion of lithium ions
[0004] 2) In LiFePO 4 In the process of preparation and synthesis, it is easy to produce Fe 2+ Oxidation of the active material reduces the mass of the effective active material, resulting in high irreversible capacity and poor cycle performance of the material.
[0005] 3) Industrial production is mainly based on the solid phase method. The disadvantage of this method is that the prepared material has a large particle size and uneven shape, which is not conducive to the infiltration of the electrolyte and the diffusion of lithium ions.
However, these studies are limited to the use of graphene as a raw material, which is added when the lithium iron phosphate cathode material is used to prepare the precursor, which cannot solve the problems inherent in the production of graphene products, such as complex preparation processes, high energy consumption, and difficulty in dispersing in the precursor.

Method used

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  • Preparation method of graphene-based lithium iron phosphate positive electrode material
  • Preparation method of graphene-based lithium iron phosphate positive electrode material
  • Preparation method of graphene-based lithium iron phosphate positive electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh ferrous sulfate heptahydrate to dissolve and be mixed with a solution, then add graphene oxide slurry and stir evenly, the amount of graphene oxide added is 5% of the produced ferric phosphate quality, and the molar ratio of Fe:P is 1:1.1 before stirring Add ammonium hydrogen phosphate solution under the condition of stirring, adjust the pH to 2.0-2.5 with ammonia water, then add surfactant OP-10 (non-ionic surfactant alkylphenol polyoxyethylene ether) and add hydrogen peroxide under the condition of stirring, at 70- Iron phosphate was precipitated by reaction at 80°C. The resulting iron phosphate was washed with water, filtered, and vacuum-dried at 100°C. The dried sample was calcined at 500°C for 4 hours, cooled and ground to form a graphene oxide-iron phosphate composite material.

[0037] Mix the above composite material with lithium carbonate according to the molar ratio of Fe:Li of 1:1.01, add 10% glucose accounting for the mass of lithium iron phosphate, dis...

Embodiment 2

[0041] Weigh ferrous sulfate heptahydrate to dissolve and prepare a solution, then add graphene oxide slurry and stir evenly, the amount of graphene oxide added is 10% of the produced ferric phosphate quality, and the molar ratio of Fe:P is 1:1.1 before stirring Add ammonium hydrogen phosphate solution under low temperature, adjust the pH to 2.0-2.5 with ammonia water, then add surfactant OP-10, add hydrogen peroxide under stirring conditions, react and precipitate iron phosphate at 70-80°C, and remove the generated iron phosphate Washed with water, filtered, and vacuum-dried at 100°C, the dried sample was calcined at 500°C for 4 hours, cooled and ground to form a graphene oxide-iron phosphate composite material.

[0042] Mix the above-mentioned composite material with lithium carbonate according to the molar ratio of Fe:Li of 1:1.01, add glucose accounting for 7% of the mass of lithium iron phosphate, disperse in water at high speed, ball mill for 4 hours, take out the mixture...

Embodiment 3

[0044] Take the iron phosphate slurry before washing and mix it with the graphene oxide slurry. The amount of graphene oxide added is 2% of the mass of iron phosphate. The mixture is washed, filtered, and vacuum-dried at 100°C. Calcined for 4 hours, cooled and ground to form a graphene oxide-iron phosphate composite material.

[0045] Mix the above composite material with lithium carbonate according to the molar ratio of Fe:Li of 1:1.03, add 10% glucose accounting for the mass of lithium iron phosphate, disperse in water at high speed, ball mill for 4 hours, take out the mixture and dry it in vacuum at 100°C, and grind it to make precursor, and finally the precursor in N 2 In a reducing atmosphere, pre-sinter at 300°C for 4 hours, heat up to 700°C for 10 hours, and cool to room temperature with the furnace, then grind to obtain a graphene-based lithium iron phosphate cathode material.

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Abstract

The invention discloses a preparation method of a graphene-based lithium iron phosphate positive electrode material, and belongs to the technical field of manufacturing of power type lithium ion batteries. The preparation method comprises the following steps: by using graphene oxide as a graphene source, uniformly mixing the graphene oxide with an iron source solution for preparing iron phosphate in the preparation process of iron phosphate, carrying out a co-precipitation reaction with phosphoric acid, ammonium phosphate or ammonium dihydrogen phosphate, washing, filtering and drying a reaction product, and then calcining and grinding to prepare the graphene oxide-iron phosphate composite material; the preparation method comprises the following steps: taking graphene as an iron source for producing a lithium iron phosphate positive electrode material, grinding and uniformly dispersing the iron source, lithium carbonate and glucose in a ball mill, drying to prepare a precursor of lithium iron phosphate, pre-sintering for 3-6 hours at 250-500 DEG C in a reducing atmosphere of H2 / Ar / N2 and the like, heating to 600-800 DEG C, continuously sintering for 6-12 hours, and cooling along with a furnace to obtain the graphene-based lithium iron phosphate positive electrode material. According to the preparation method, the dispersity and uniformity of graphene in the positive electrode material can be improved, and the defect that graphene is difficult to disperse in water in the preparation process of the positive electrode material is overcome.

Description

technical field [0001] The invention relates to a preparation method of a graphene-based lithium iron phosphate cathode material, which is used in the technical field of manufacturing power lithium ion batteries. Background technique [0002] With the expansion of lithium-ion batteries in practical applications, the performance of cathode materials directly determines the development of lithium-ion batteries. LiFePO with olivine structure 4 Cathode materials, due to the wide source of raw materials, low price, environmental friendliness, high specific capacity and voltage platform, have gradually become the protagonists of lithium-ion battery cathode materials. Compared with other cathode materials, LiFePO 4 It has relatively high safety and is more suitable as a power source for large power batteries. But LiFePO 4 As the application of large-scale power ion battery materials, there are still the following problems to be solved: [0003] 1) LiFePO 4 The electronic cond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M4/62H01M10/0525
CPCH01M4/366H01M4/583H01M4/5825H01M4/625H01M10/0525H01M2004/028Y02E60/10
Inventor 奉辉
Owner 湖北华烯新材料有限公司
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