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Method for preparing graphene material at high temperature and high pressure

A high-temperature and high-pressure, graphene technology is applied in the field of high-temperature and high-pressure preparation of graphene materials, and high-temperature and high-pressure sintering to prepare graphene materials with different thicknesses and special shapes, which can solve the problems of no graphene materials and achieve good repeatability and suitable for The effect of industrial production

Inactive Publication Date: 2014-06-25
JILIN JIANZHU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, people have also carried out a lot of research work on the research of carbon materials under high pressure, but so far there is no method and product for preparing graphene materials under high temperature and high pressure.

Method used

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  • Method for preparing graphene material at high temperature and high pressure
  • Method for preparing graphene material at high temperature and high pressure
  • Method for preparing graphene material at high temperature and high pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] See attached figure 1 , the method for preparing graphene material at high temperature and high pressure of the present invention may further comprise the steps:

[0022] Step 1: Pre-press the powdered adamantane to obtain bulk adamantane;

[0023] Step 2: Put the block-like adamantane obtained in Step 1 into the cavity of the synthesis module, then put it into high-temperature and high-pressure equipment, and then sinter it. The pressure value is 500MPa and the temperature is 1050°C. 30 minutes, the heating rate is 5 degrees per minute;

[0024] Step 3: The bulk adamantane sintered in step 2 is subjected to pressure relief cooling and demoulding treatment to obtain spherical graphene materials, wherein the pressure relief cooling is carried out slowly.

[0025] See attached figure 2 , Carry out Raman spectrum measurement to the spherical graphene material prepared above, the result shows that the samples are all graphene. Among them, peak D appears at 1270-1273cm ...

Embodiment 2

[0027] See attached image 3 , The difference between this embodiment and Embodiment 1 is that under the conditions of pressure 500 MPa and temperature 1050° C., the heating rate is 25 degrees per minute, and the heat preservation and pressure sintering is 30 minutes.

[0028] Raman spectrum measurement was performed on the rod-shaped graphene material obtained by the above sintering, and the results showed that the samples were all graphene. Among them, peak D appears at 1270-1273cm -1 , G peak appears at 1580-1581cm -1 , the 2D peak appears at 2700cm -1 nearby. Compared with the G peak, the D peak is only about 1 / 3 of the G peak, indicating that graphene has fewer defects. Meanwhile, the 2D peak is more than 2 times that of the G peak. A scanning electron microscope (SEM) of the sample revealed that the rod-like material is composed of graphene. The diameter of the rod-shaped graphene is between 0.3-2um, the length is between 0.4-15um, the diameter of the surface pores...

Embodiment 3

[0030] See attached Figure 4 The difference between the present embodiment and the first embodiment is that adamantane is used as raw material, under the conditions of pressure 500MPa and temperature 1050°C, the heating rate is above 60°C per minute, and the heat preservation and pressure sintering is carried out for 30 minutes.

[0031] Carry out Raman spectrum measurement to the above-mentioned prepared flake graphene material, the result shows that the samples are all graphene. Among them, peak D appears at 1270-1273cm -1 , G peak appears at 1580-1581cm -1 , the 2D peak appears at 2700cm -1 nearby. Compared with the G peak, the D peak is only about 1 / 3 of the G peak, indicating that graphene has fewer defects. Meanwhile, the 2D peak is more than 2 times that of the G peak. A scanning electron microscope (SEM) of the sample revealed that the sheet-like material is composed of graphene. The area of ​​sheet-like graphene is 0.3-10um, that is, between single-layer, two-l...

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Abstract

The invention discloses a method for preparing graphene material at high temperature and high pressure and belongs to the technical field of carbon material, and the method is used for solving the problems of the prior art and achieving preparation of graphene. The method comprises the following steps; pre-pressing a solid organism with carbon so as to obtain a block raw material; putting the block raw material into a mold chamber, and performing heat preservation and pressure maintaining for more than 10 minutes, wherein the heating rate is 5 DEG C per minute; further releasing the pressure, cooling, demolding and treating to obtain the graphene material. The value of the pressure P in the step of performing heat preservation and pressure maintaining ranges from 400MPa to 20000MPa, and the temperature T ranges from 900 DEG C to 1600 DEG C. By virtue of high temperature and high pressure, the particle size, thickness and surface opening slit size of spherical, bar-shaped and flake graphene are precisely controlled; the defects of the spherical, bar-shaped and flake graphene are precisely controlled; the method is environmental-friendly as no acid, alkali or toxic and harmful reagents are used; multiple graphene materials prepared by using the method are good in repeatability and applicable to industrial production.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and relates to a method for preparing graphene materials under high temperature and high pressure, in particular to a process method for preparing graphene materials with different thicknesses and special shapes by firing under high temperature and high pressure. Background technique [0002] Graphene is a planar film composed of carbon atoms with sp2 hybrid orbitals forming a hexagonal honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. At present, the preparation of graphene mainly includes the following methods: mechanical separation method, graphite oxide reduction method, SiC pyrolytic epitaxial growth method and chemical vapor deposition method. Among them, the mechanical separation method peels the single-layer graphite sheet from the graphite crystal by mechanical force. The single-layer graphite sheet obtained by this method is relatively comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 刘亚冰秦鹤秦杰明
Owner JILIN JIANZHU UNIVERSITY
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