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A kind of preparation method of sodium titanate/graphene composite negative electrode material for sodium ion battery

A graphene composite and sodium-ion battery technology, which is applied in battery electrodes, secondary batteries, circuits, etc., can solve the problem of poor electronic and ionic conductivity of sodium titanate, poor high-current discharge performance, and capacity must be fully utilized, etc. problems, to overcome the poor ionic conductivity, improve electronic conductivity, and facilitate storage and diffusion

Active Publication Date: 2017-02-22
LIAONING TECHNICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, the electronic conductivity and ionic conductivity of sodium titanate are poor, so the capacity must be fully utilized, and the high-current discharge performance is poor.

Method used

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  • A kind of preparation method of sodium titanate/graphene composite negative electrode material for sodium ion battery
  • A kind of preparation method of sodium titanate/graphene composite negative electrode material for sodium ion battery

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preparation example Construction

[0030] The preparation method of graphite oxide is as follows:

[0031] Take an appropriate amount of concentrated H with a mass fraction of 95-98% 2 SO 4 Add to the reaction vessel placed in the ice bath, start stirring, and add graphite and KMnO at 20-100rpm 4 React for 30-60 minutes; then raise the temperature of the reaction solution to 40±2°C, react for 30-60 minutes; then control the temperature of the reaction solution at 95-100°C, add deionized water to the solution for 30-60 minutes; then add an appropriate amount H with a mass fraction of 5% 2 o 2 Finally, the reaction solution was filtered, and the filter residue was washed with 5% HCl until there was no SO in the filtrate. 4 2- (with BaC1 2 solution detection); then use deionized water to wash the filter residue to neutrality, and vacuum filter to obtain paste-like graphite oxide;

[0032] Among them, graphite is natural flake graphite or artificial graphite, with a particle size of 0.04-30 μm; concentrated ...

Embodiment 1

[0034] 1. Take 10g of graphite oxide and add it to 50mL of absolute ethanol, then add 0.1g of γ-aminopropyltriethoxysilane, and conduct ultrasonic treatment at a constant temperature of 60°C for 30min to obtain a graphene oxide solution;

[0035] 2. Add 8g of tetraethyl titanate to 400mL of absolute ethanol, stir at 20-50rpm, add formic acid to adjust the pH of the solution to 5, then add the graphene oxide solution obtained in step 1, and mix evenly to obtain titanium-containing Graphene oxide solution; then take the sodium acetate aqueous solution containing 0.028mol sodium acetate, add the sodium acetate aqueous solution dropwise to the titanium-containing graphene oxide solution at a rate of 0.5mL / min, and stir the reaction at 20-50rpm 20min, and after standing still for 2h, wash with deionized water for 3 to 5 times, vacuum filter, and dry to obtain the composite precursor;

[0036] 3. Mix 10g of the composite precursor prepared in step 2 with 5mL of deionized water and 0...

Embodiment 2

[0041] 1. Take 10g of graphite oxide and add it to 200mL of absolute ethanol, then add 0.5g of γ-(2,3-glycidoxy)propyltrimethoxysilane, and conduct ultrasonic treatment at a constant temperature of 30°C for 240min to obtain graphene oxide solution;

[0042] 2. Add 32g of tetrabutyl titanate to 320mL of absolute ethanol, stir at 20-50rpm, add HCl to adjust the pH of the solution to 2, then add the graphene oxide solution obtained in step 1, and mix evenly to obtain titanium-containing Graphene oxide solution; Then get the sodium oxalate aqueous solution that contains 0.031mol sodium oxalate, with the drop rate of 3mL / min, the sodium oxalate aqueous solution is added dropwise in the graphene oxide solution containing titanium, at 20~ Stir and react at 50rpm for 60min, then let stand for 6h, wash with deionized water for 3 to 5 times, vacuum filter and dry to obtain a composite precursor;

[0043] 3. Take 10g of the composite precursor prepared in step 2, mix it with 15mL of dei...

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Abstract

The invention provides a preparation method of a sodium titanate / graphene composite cathode material of a sodium ion battery, which is used for solving the problems in the prior art that no sodium ion battery cathode material with excellent comprehensive performance is provided, and belongs to the field of sodium ion secondary batteries. The method comprises the steps of dispersing graphene oxide to obtain a graphene oxide solution, mixing the graphene oxide solution, a sodium-containing compound and a titanium-containing compound, carrying out reaction to obtain a composite precursor, mixing the composite precursor with a binder, carrying out atomizing drying and granulating to obtain a spherical composite precursor, and finally burning the spherical composite precursor in an inert atmosphere to obtain a micro-scale spherical sodium titanate / graphene composite cathode material. The composite cathode material has the advantages of high sodium storage capacity, long cycle life, good large-current discharge property, high compaction density and the like, and the requirement of the high-performance sodium ion battery for the comprehensive performance of the cathode material can be met.

Description

technical field [0001] The invention belongs to the field of sodium ion secondary batteries, in particular to a preparation method of sodium titanate / graphene composite negative electrode material for sodium ion batteries. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, high working voltage, small self-discharge, no pollution, and long cycle life. They have become the fastest-growing chemical power sources and are widely used in small mobile appliances such as mobile phones, notebook computers, and digital cameras. , and gradually develop into the fields of electric vehicles and aerospace. Sodium-ion battery is a battery system similar to lithium-ion battery. Because metal sodium is a metal element of the same family as lithium, its physical and chemical properties are relatively close, and metal sodium has a large reserve in the earth's crust and is the sixth most abundant element. Therefore, sodium-ion batteries The cost is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36
CPCH01M4/362H01M4/485H01M4/583H01M10/054Y02E60/10
Inventor 沈丁李红董伟杨绍斌王晓亮李思南张琴
Owner LIAONING TECHNICAL UNIVERSITY
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