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Preparation method of nanometer metallic oxide/graphene doped lithium iron phosphate electrode material

A nano-metal, lithium iron phosphate technology, applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of graphene sheets stacking each other in disorder, so as to improve the volumetric energy density, increase the specific surface area, excellent mechanical properties and The effect of electrochemical performance

Active Publication Date: 2011-09-14
河北中芯凤华科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, some people in China have modified lithium iron phosphate by doping graphene (such as patent CN101562248A and patent CN101752561A), but only a single graphene and lithium iron phosphate are composited. In the process of forming macro-aggregates of single-layer graphene in the heterogeneous process, the problem of disordered stacking and agglomeration of graphene sheets has not been solved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Disperse 19.2 mg of graphene oxide in 80 mL of deionized water and sonicate for 30 minutes, then add 20 mL of 0.002 mol / L titanium chloride solution and continue to sonicate for 30 minutes to mix graphene oxide and titanium chloride evenly. Under the condition of ultrasonic stirring, 20 wt% ammonia water was slowly added dropwise until the pH range was 8, and then 22.6 mg of sodium borohydride was added and stirred at 80° C. for 3 hours. The product was washed with deionized water, filtered and vacuum-dried at 40°C for 15 hours, then calcined at 400°C for 3 hours with argon as a protective gas and cooled to room temperature to obtain a nano-titanium dioxide / graphene composite material;

[0029] 2. Add lithium carbonate, ferrous oxalate, ammonium dihydrogen phosphate, nano-titanium dioxide / graphene composite material into ethanol in a molar ratio of 1:0.995:1:0.005, and mechanically ball mill and mix evenly. The ball mill speed is 300 rpm, and the ball mill Time 10 hour...

Embodiment 2

[0031] 1. Disperse 38.4mg of graphene oxide into 60mL of deionized water and sonicate for 40 minutes, then add 40mL of 0.004mol / L zinc chloride solution and continue to sonicate for 40 minutes to mix graphene oxide and zinc chloride evenly. Under the condition of ultrasonic stirring, 25% by weight of ammonia water was slowly added dropwise until the pH range was 8, and then 19.2 mg of sodium borohydride was added and stirred at 80° C. for 5 hours. The product was washed with deionized water and suction-filtered and vacuum-dried at 80°C for 20 hours, then calcined at 550°C for 5 hours with argon as a protective gas and cooled to room temperature to obtain a nano-zinc oxide / graphene composite material;

[0032] 2. Add lithium acetate, iron, ammonium dihydrogen phosphate, and nano-zinc oxide / graphene composite materials into deionized water in a molar ratio of 1:0.9:1:0.1 and mix them by mechanical ball milling. The ball milling speed is 2000 rpm. Time 15 hours. The mixed materi...

Embodiment 3

[0034] 1. Disperse 57.6 mg of graphene oxide into 60 mL of deionized water and sonicate for 30 minutes, then add 40 mL of 0.004 mol / L nickel chloride solution and continue to sonicate for 60 minutes to mix graphene oxide and nickel chloride evenly. Under the condition of ultrasonic stirring, 25% by weight of ammonia water was slowly added dropwise until the pH range was 9, and then 5.7 mg of hydrazine hydrate (85% by mass) was added and stirred at 100°C for 8 hours. The product was washed with deionized water and suction-filtered and vacuum-dried at 60°C for 24 hours, then calcined at 500°C for 8 hours with nitrogen as a protective gas and cooled to room temperature to obtain a nano-nickel oxide / graphene composite material;

[0035] 2. Add lithium hydroxide, ferrous sulfate, phosphoric acid, nano-nickel oxide / graphene composite material into acetone in a molar ratio of 1:0.95:1:0.05, and mechanically ball mill and mix evenly. The ball milling speed is 1000 rpm, and the ball mil...

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Abstract

The invention discloses a preparation method of a nanometer metallic oxide / graphene doped lithium iron phosphate electrode material. The method is characterized in that an ultrasonic dispersion method is used to disperse the graphene oxide into lamella, then the graphene oxide lamella is fully mixed with metal salt solution and then subjected to reduction, drying and calcination to prepare the nanometer metallic oxide / graphene composite material; and during the preparation process of lithium iron phosphate, the nanometer metallic oxide / graphene composite material together with lithium source, an iron source and a phosphorus source is added for in situ composing or the nanometer metallic oxide / graphene composite material and lithium iron phosphate are dispersed to alcohol solution for ultrasonic and ball-milling mixing so as to prepare the nanometer metallic oxide / graphene doped lithium iron phosphate electrode material. Through the nanometer metallic oxide modified graphene, the preparation method solves the problem that the grapheme is easy to agglomerate in the doping process with lithium iron phosphate, and the nanometer metallic oxide can reduce the grapheme amount and improve the volume energy density of the lithium iron phosphate, therefore, the preparation method has wide application prospects in the field of lithium ion battery positive electrode material.

Description

technical field [0001] The invention relates to a preparation method of a nanometer metal oxide / graphene-doped lithium iron phosphate electrode material, which belongs to the field of electrochemistry and new energy materials. Background technique [0002] Lithium-ion battery is a new type of energy storage battery developed after the 1970s. Due to the advantages of high energy, long life, low consumption, no pollution, no memory effect, small self-discharge, low internal resistance, high cost performance, and less pollution, lithium-ion batteries have shown great advantages in gradual application and are widely used Used in various fields such as mobile phones, notebook computers, camcorders, digital cameras, electric vehicles, energy storage, and aerospace. At present, lithium-ion battery cathode materials mainly include lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, and lithium iron phosphate. However, lithium cobalt oxide (LiCoO 2 ) poor safety p...

Claims

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Application Information

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IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 谭强强邱琳琳
Owner 河北中芯凤华科技发展有限公司
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