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Method for preparing graphene-loaded Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material

A technology of ferric hydroxyphosphate and lithium ion battery, applied in the field of electrochemistry, can solve problems such as poor conductivity, and achieve the effect of excellent electrochemical performance

Active Publication Date: 2017-06-13
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However with LiFePO 4 and FePO 4 Similarly, the electrical conductivity of this material is poor, and the currently synthesized Fe 1.5 (PO 4 )OH, cycle stability needs to be improved

Method used

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  • Method for preparing graphene-loaded Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material
  • Method for preparing graphene-loaded Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material
  • Method for preparing graphene-loaded Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material

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preparation example Construction

[0024] A method for preparing a graphene-loaded iron hydroxyphosphate hollow octahedral lithium-ion battery positive electrode material, comprising the following steps:

[0025] 1) Dissolve commercially available graphene oxide in deionized water to form a solution of 1 to 5 mg / mL, and use an ultrasonic generator to sonicate for 2 to 6 hours at a power of 300 W to form a uniformly dispersed graphene oxide suspension, denoted as A ;

[0026] 2) Put analytically pure soluble ferrous salt (ferrous sulfate, ferrous chloride, etc.), urea, ammonium dihydrogen phosphate or diammonium hydrogen phosphate in a molar ratio of 1:1:0.5~1:1:5 Add to the mixed solution of deionized water and ethylene glycol (or glycerin), the volume ratio of water and ethylene glycol (or glycerin) is 5:1~5:5, stir for 10min-30min, then add to the suspension In A, configure mixed solution B, the concentration of iron salt in mixed solution B is 0.05-0.5mol / L, and the concentration of graphene oxide is 0.5-2....

Embodiment 1

[0031] 1) Dissolve commercially available graphene oxide in deionized water to form a solution of 1 mg / mL, and use an ultrasonic generator to sonicate for 3 hours at a power of 300 W to form a uniformly dispersed suspension of graphene oxide, which is designated as A;

[0032] 2) Add the analytically pure soluble ferrous ferrous salt ferrous sulfate, urea, and ammonium dihydrogen phosphate in a molar ratio of 1:1:0.5 to the mixed solution of deionized water and ethylene glycol, and the water and ethylene glycol The volume ratio is 5:1, stirred for 10 minutes, and then added to the suspension A to form a mixed solution. The concentration of iron salt is 0.05mol / L, and the concentration of graphene oxide is 0.5mg / mL, which is recorded as B ;

[0033] 3) Pour the mixed solution B prepared above into a microwave hydrothermal reactor with a filling degree of 60%, then seal the reactor, put it into a microwave hydrothermal reactor, and control the heating rate at 5°C / min. The react...

Embodiment 2

[0039] 1) Dissolve commercially available graphene oxide in deionized water to form a solution of 5 mg / mL, and use an ultrasonic generator to sonicate for 2 hours at a power of 300 W to form a uniformly dispersed suspension of graphene oxide, which is designated as A;

[0040] 2) Add analytically pure soluble ferrous ferrous salt ferrous sulfate, urea, and ammonium dihydrogen phosphate in a molar ratio of 1:1:1 to a mixed solution of deionized water and glycerin, and the volume ratio of water and glycerin is 5 : 3, stirred for 20min, then joined in the suspension A, configured into a mixed solution, the concentration of iron salt was 0.5mol / L, and the concentration of graphene oxide was a solution of 2.5mg / mL, denoted as B;

[0041] 3) Pour the mixed solution B prepared above into a microwave hydrothermal reactor with a filling degree of 40%, then seal the reactor, put it into a microwave hydrothermal reactor, and control the heating rate at 10°C / min. The reaction temperature ...

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Abstract

The invention discloses a method for preparing a graphene-loaded Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material. The method comprises the following steps: dissolving commercially available graphene oxide in deionized water; performing ultrasonic treatment to form turbid liquid A in which graphene oxide is uniformly dispersed; adding analytically pure soluble bivalent ferrous salts, urea and ammonium dihydrogen phosphate or diammonium hydrogen phosphate into a mixed solution of deionized water and ethylene glycol or glycerin, stirring and adding the mixture into the turbid liquid A to prepare a mixed solution B; carrying out microwave reaction on the mixed solution B so as to obtain a product C; and finally, performing centrifugal collection on the product C, washing, performing freeze drying, thereby obtaining the Fe1.5(PO4)OH hollow octahedron lithium ion battery positive electrode material in in-situ growth on the graphene surface. According to the method disclosed by the invention, the time is short, the reaction is fast, the yield is high, raw material price is low and the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry, and in particular relates to a preparation method of a graphene-loaded iron hydroxyphosphate hollow octahedral lithium-ion battery cathode material. Background technique [0002] Due to the advantages of high energy density, long service life, and environmental friendliness, lithium-ion batteries have become a research hotspot in recent years and have been successfully commercialized. In order to develop the next generation of more efficient Li-ion battery materials that can be applied to electric vehicles and large-scale energy storage devices, it is a key factor to be able to find a cathode material with excellent electrochemical performance. LiFePO 4 It is cheap, environmentally friendly, has good structural stability and thermal stability, and is compatible with most electrolytes. It has become a new generation of positive lithium-ion cathode materials with the most development and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/48H01M4/62
CPCH01M4/48H01M4/625Y02E60/10
Inventor 李嘉胤齐慧黄剑锋曹丽云党欢程娅伊马萌李春光
Owner SHAANXI UNIV OF SCI & TECH
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