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Preparation method of self-supported three-dimensional graphene

A graphene, self-supporting technology, applied in the field of preparation of self-supporting three-dimensional graphene, can solve the problems of waste of resources, complicated preparation process, environmental pollution, etc., and achieve good foaming effect, improved current transmission capacity, and improved performance. Effect

Inactive Publication Date: 2015-12-09
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature (Z.Tang, S.Shen, J.Zhuang and X.Wang, Angew.Chem.Int.Ed., 2010, 49, 4603.) uses the method of reducing GO to prepare three-dimensional graphene, and the hydrophilic property of three-dimensional graphene is excellent However, the preparation of graphene oxide GO involves a series of dangerous drugs, the preparation process is relatively complicated, the process is rough, and it is easy to cause environmental pollution
In the literature (Z.Chen, W.Ren, L.Gao, B.Liu, S.PeiandH.-M.Cheng, NatureMater., 2011, 10, 424.), nickel foam is used to grow three-dimensional graphene, and then the nickel template is removed. Three-dimensional graphene can be obtained, and three-dimensional graphene with extremely thin thickness can be obtained, but the use of metal templates will inevitably cause a great waste of resources, and the cost is not conducive to industrialization
Literature (WangX, ZhangY, ZhiC, etal.Three-dimensional strutted graphene grown by substrate-freesu gar blowing for high-power-density supercapacitors. Naturecommunications, 2013, 4) used ammonium chloride foaming method to prepare three-dimensional graphene, without doping, its electrical transport performance is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Using hexamethylenetetramine as a foaming agent and glucose as a carbon source to prepare three-dimensional graphene, the first step is to mix hexamethylenetetramine and glucose, stir into a uniform powder, and the second step is to heat up to a specified temperature and keep it for a certain period of time to prepare Self-supporting three-dimensional graphene foam.

[0021] Step 1. Mix glucose and hexamethylenetetramine at a mass ratio of 1:0.5.

[0022] Step 3. Under an inert atmosphere, heat the mixed powder to 1000°C at 4°C / min, and keep it warm for 0.5h;

[0023] Step 4, after the reaction is finished, take out the sample.

[0024] The samples were characterized by SEM and EDS as figure 1 , 2 shown. The results show that, according to the process parameters of Example 1, a three-dimensional graphene with a pore diameter of about 100 um, good light transmission, and self-supported by a carbon skeleton can be obtained.

Embodiment 2

[0026] Three-dimensional graphene is prepared by using hexamethylenetetramine as a foaming agent. The first step is to mix the carbon source and the foaming agent, and the second step is to raise the temperature to a specified temperature and keep it for a certain period of time to prepare a self-supporting three-dimensional graphene foam.

[0027] Step 1, mix glucose and hexamethylenetetramine with a mass ratio of 1:1, and place in the furnace body;

[0028] Step 2. Under an inert atmosphere, heat the powder at 8°C / min to 1200°C and keep it warm for 2 hours;

[0029] Step 3, the reaction furnace is cooled to room temperature, and after the reaction is completed, the sample is taken out.

[0030] The samples were characterized by SEM and EDS as in case 1.

Embodiment 3

[0032] Three-dimensional graphene is prepared by using hexamethylenetetramine as a foaming agent. The first step is to mix the carbon source and the foaming agent, and the second step is to raise the temperature to a specified temperature and keep it for a certain period of time to prepare a self-supporting three-dimensional graphene foam.

[0033] Step 1, mix glucose and hexamethylenetetramine with a mass ratio of 1:2, and place in the furnace body;

[0034] Step 2. Under an inert atmosphere, heat the powder at 10°C / min to 1400°C and keep it warm for 5 hours;

[0035] Step 3, the reaction furnace is cooled to room temperature, and after the reaction is completed, the sample is taken out.

[0036] The samples were characterized by SEM and EDS as in case 1.

[0037] The invention adopts a chemical foaming method and uses small nitrogen-containing organic molecules as a foaming agent to prepare nitrogen-doped three-dimensional graphene. Compared with the original plan using am...

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Abstract

The invention discloses a preparation method of self-supported three-dimensional graphene. According to the preparation method, hexamethylene tetramine is taken as the foaming agent, glucose is taken as the carbon source, then the raw materials are heated to a certain temperature, the temperature is maintained for a while, then the raw materials are cooled to the room temperature to prepare the self-supported graphene, and the foaming effect can be controlled by changing the reaction temperature and the weight ratio of carbon source to foaming agent. Nitrogen-containing organic micromolecules are taken as the foaming agent, the foaming effect is very good for three-dimensional graphene preparation, moreover, nitrogen atoms are introduced into the graphene, the graphene is doped chemically, compared with that of un-doped graphene, the current transmission performance of chemically-doped graphene is prominently improved, and the practical application value is greatly improved.

Description

technical field [0001] The invention belongs to the field of nanometer material preparation, in particular to a method for preparing self-supporting three-dimensional graphene applicable to lithium ion batteries and supercapacitors. Background technique [0002] Graphene has superior electrical conductivity and a large specific surface area; the three-dimensional graphene derived from it inherits the advantages of graphene and obtains a large surface area through a three-dimensional structure. It is widely used in lithium batteries, supercapacitors and catalysis. Wide application prospects. [0003] The preparation methods of three-dimensional graphene mainly include methods based on reduced graphene oxide GO, metal template growth method and hexamethylenetetramine foaming method. Literature (Z.Tang, S.Shen, J.Zhuang and X.Wang, Angew.Chem.Int.Ed., 2010, 49, 4603.) uses the method of reducing GO to prepare three-dimensional graphene, and the hydrophilic property of three-di...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 曾海波吉建平严仲宋秀峰
Owner NANJING UNIV OF SCI & TECH
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