Method for preparing self-supporting three-dimensional porous graphene composite microsphere

A graphene composite and three-dimensional porous technology, which is applied in the field of preparation of self-supporting three-dimensional porous graphene composite microspheres, can solve the problem of the inability to use negative electrode materials for sodium-ion batteries, less research and development of modified electrode materials, and the specific surface area of ​​pure graphene. Large and other problems, to achieve the effect of reducing the first irreversible capacity, preventing agglomeration, and increasing the bulk density

Active Publication Date: 2015-05-06
江苏嘉明碳素新材料有限公司
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Problems solved by technology

However, due to the large specific surface area of ​​pure graphene, the first Coulombic efficiency is low, and the graphene sheets are prone to irreversible agglomeration due to the van der Waals force, resulting in poor cycle performance, and cannot be directly used as anode materials for sodium-ion batteries.
[0005] At this stage, there are few researches on the development of graphene-modified electrode materials for energy storage devices such as sodium-ion batteries.
In 2013, Wang et al. used graphene oxide and pyrrole as raw materials to synthesize a 2D porous doped carbon / graphene composite material through heat treatment and carbonization. The introduction of heteroatoms improved the electronic conductivity and capacity of the material; in 2014, Yan Yang et al. constructed a porous carbon / graphene nanocomposite material with a sandwich structure by ion thermal method. Although porous carbon guarantees Na + The reversible deintercalation of the graphene layer promotes the rapid transport of electrons, but there are still shortcomings such as large specific surface area leading to high irreversible capacity for the first time.

Method used

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preparation example Construction

[0031] The preparation method of graphite oxide is as follows:

[0032] 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;

[0033] Among them, graphite is natural flake graphite or artificial graphite, with a particle size of 0.04-30 μm; concentrated ...

Embodiment 1

[0035] 1. Take 10g of graphite oxide, add it to 50mL of absolute ethanol, then add 0.3g of surfactant sodium dodecylbenzenesulfonate, ultrasonically treat at 45°C for 240min, then filter, and dry the filter residue at 60°C to obtain Graphene oxide; then put the graphene oxide into a microwave oven with a power of 800W and a frequency of 2.45GHz, and perform a heat treatment for 30min in an Ar gas atmosphere to obtain graphene;

[0036] 2. Take 8g of graphene obtained in step 1, add 20mL of deionized water, stir evenly, then add 32g of activator NaOH and 1.6g of binder starch, stir to form a slurry, and then the inlet temperature is 150 ° C, the outlet temperature spray drying and granulation under the conditions of 90°C, spray pressure of 2MPa, and nozzle diameter of 0.4mm, to obtain micron-sized graphene microspheres containing activators;

[0037] 3. Dissolve 1g of petroleum pitch in 10mL of kerosene, then add 10g of graphene microspheres containing activator obtained in ste...

Embodiment 2

[0041] 1. Take 10g of graphite oxide, add it to 100mL of absolute ethanol, then add 0.15g of surfactant sodium lauryl sulfate, ultrasonically treat at 30°C for 150min, then filter, and dry the filter residue at 70°C to obtain graphite oxide Then put the graphene oxide into a microwave oven with a power of 600W and a frequency of 2.45GHz, and perform a 16min heat treatment in an Ar gas atmosphere to obtain graphene;

[0042] 2. Take 6g of graphene obtained in step 1, add 10mL of deionized water, stir evenly, then add 13g of activator KOH and 0.8g of binder glucose, stir to form a slurry, and then the inlet temperature is 130 ° C, the outlet temperature 80°C, spray pressure of 0.5MPa, and nozzle diameter of 0.7mm for spray drying and granulation to obtain micron-sized graphene microspheres containing activators;

[0043] 3. Dissolve 1g of petroleum pitch in 8mL of kerosene, then add 5g of graphene microspheres containing activator obtained in step 2, stir at 70rpm until evenly m...

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Abstract

The invention aims at less current research and development on graphene-modified electrode material for energy storage devices such as a sodium ion battery, provides a method for preparing a self-supporting three-dimensional porous graphene composite microsphere and belongs to the technical field of novel carbon materials. The method comprises the following steps of mixing graphene with water, an activator and a binder and stirring to obtain a slurry, carrying out spray-drying and granulating to obtain the graphene microsphere containing the activator; dissolving petroleum pitch in kerosene, adding the graphene microsphere, uniformly mixing and drying to obtain the carbon-precursor-coated graphene microsphere; and carrying out heat treatment on the microsphere to obtain the self-supporting three-dimensional porous graphene composite microsphere. The self-supporting three-dimensional porous graphene composite microsphere obtained by using the method has the characteristics of stable structure, high gap content, high bulk density and the like. The sodium ion battery prepared from the graphene composite microsphere has the advantages of high capacity, good high-current discharge performance, excellent cycle performance, large packing density and the like.

Description

technical field [0001] The invention belongs to the technical field of new carbon materials, and in particular relates to a preparation method of self-supporting three-dimensional porous graphene composite microspheres. Background technique [0002] As the newest member of carbon materials, graphene was prepared and discovered for the first time in 2004 by Geim et al., University of Manchester. The ideal graphene is a single-layer two-dimensional material composed of carbon atoms in a hexagonal honeycomb structure. It is the basic unit for constructing zero-dimensional fullerenes, one-dimensional carbon nanotubes, three-dimensional graphite and other carbon materials. Its unique structure makes it have excellent electrical, mechanical, thermal and optical properties, making graphene show great application potential in energy, electronics, medicine and other fields. [0003] At present, the preparation methods of graphene include micromechanical exfoliation method, epitaxial...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 沈丁董伟杨绍斌王晓亮王中将张佳民徐建波
Owner 江苏嘉明碳素新材料有限公司
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