Preparation method of highly oriented pyrolytic graphite

A technology of pyrolytic graphite and pyrolytic graphite plate, which is applied in the field of preparation of new carbon materials, can solve the problems that the performance parameters are not as good as single crystal graphite, and the degree of crystal orientation is not high.

Active Publication Date: 2021-05-18
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The internal structure of pyrolytic graphite on the market is not high in crystallographic orientation, and its performance parameters are not as good as single crystal graphite. With the continuous development of equipment and devices, the performance requirements of pyrolytic graphite are getting higher and higher, and the preparation of pyrolytic graphite is on the way. Towards highly oriented pyrolytic graphite similar to single crystal graphite

Method used

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  • Preparation method of highly oriented pyrolytic graphite

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Experimental program
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Effect test

Embodiment 1

[0021] (1) Soak a rectangular and circular graphite substrate in the pretreatment solution. After soaking for 30 minutes, take it out, dry it, and then put it in a chemical vapor deposition furnace. Methane and nitrogen, the gas flow ratio is 1:2, and a 1mm pyrolytic graphite plate is deposited on the surface of the graphite substrate;

[0022] The pretreatment liquid is composed of methyltrichlorosilane, triethanolamine, and ethanol in a volume ratio of 0.5:1:20;

[0023] (2) When the pyrolytic graphite plate is cooled to 700°C, put it into a magnetic field with a magnetic field strength of 10000A / m and a magnetic field frequency of 130Hz, and take it out when the temperature drops to 150°C;

[0024] (3) Cut the pyrolytic graphite plate into square pyrolytic graphite pieces of 30*30*1mm, place the pyrolytic graphite pieces in a high-temperature and high-pressure furnace, and pass in argon gas, under the conditions of a pressure of 30MPa and a temperature of 3000°C Next, heat...

Embodiment 2

[0026] (1) Soak a rectangular and circular graphite substrate in the pretreatment solution. After soaking for 30 minutes, take it out and dry it, and then put it in a chemical vapor deposition furnace. Methane and nitrogen, the gas flow ratio is 1:2, and a 1mm pyrolytic graphite plate is deposited on the surface of the graphite substrate;

[0027] (2) When the pyrolytic graphite plate is cooled to 750°C, put it into a magnetic field with a magnetic field strength of 8000A / m and a magnetic field frequency of 120Hz, and take it out when the temperature drops to 100°C;

[0028] (3) Cut the pyrolytic graphite plate into square pyrolytic graphite pieces of 30*30*1mm, place the pyrolytic graphite pieces in a high-temperature and high-pressure furnace, and pass in argon gas, under the conditions of a pressure of 30MPa and a temperature of 3500°C Next, heat-treat the pyrolytic graphite, and the heat-treatment time is 100 minutes.

Embodiment 3

[0030] (1) Soak a rectangular and circular graphite substrate in the pretreatment solution. After soaking for 30 minutes, take it out, dry it, and then put it in a chemical vapor deposition furnace. Methane and nitrogen, the gas flow ratio is 1:2, and a 1.5mm pyrolytic graphite plate is deposited on the surface of the graphite substrate;

[0031] The pretreatment liquid is composed of methyltrichlorosilane, triethanolamine, and ethanol in a volume ratio of 0.5:1:20;

[0032] (2) When the pyrolytic graphite plate is cooled to 700°C, put it into a magnetic field with a magnetic field strength of 12000A / m and a magnetic field frequency of 150Hz, and take it out when the temperature drops to 150°C;

[0033] (3) Cut the pyrolytic graphite plate into square pyrolytic graphite pieces of 30*30*1mm, place the pyrolytic graphite small pieces in a high-temperature and high-pressure furnace, and pass in argon gas under the conditions of a pressure of 30MPa and a temperature of 2500°C Nex...

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Abstract

The invention belongs to the field of preparation of novel carbon materials, and particularly relates to a preparation method of highly oriented pyrolytic graphite. The method is realized by the following steps: firstly, soaking a graphite substrate in a pretreatment solution, taking out the graphite substrate, airing the graphite substrate, and then introducing methane and nitrogen by adopting a chemical deposition method to obtain a pyrolytic graphite plate; cooling the pyrolytic graphite plate to 700-750 DEG C, putting the pyrolytic graphite plate into a magnetic field, and taking out the pyrolytic graphite plate when the temperature is reduced to 100 DEG C; and taking out the pyrolytic graphite plate subjected to magnetic field treatment, putting the pyrolytic graphite plate into a high-pressure and high-temperature furnace, introducing inert gas, and carrying out heat treatment. According to the method, the graphite base material is pretreated, then the pyrolytic graphite is prepared through the chemical vapor deposition method; in the subsequent heat treatment process, the pyrolytic graphite easily forms the high-orientation pyrolytic graphite with the higher orientation degree, and the heat treatment time is relatively short, so that the high-orientation pyrolytic graphite with the higher quality is obtained with the lower cost; in addition, the graphite base material is subjected to magnetic field treatment in advance, so that the orientation degree of pyrolytic graphite is improved.

Description

technical field [0001] The invention belongs to the field of preparation of new carbon materials, and in particular relates to a preparation method of highly oriented pyrolytic graphite. Background technique [0002] Highly oriented pyrolytic graphite is a new type of graphite whose performance is close to that of single crystal graphite after high temperature treatment, referred to as HOPG. HOPG has a very high reflectivity for X-rays, it can eliminate the high background intensity caused by white light, fluorescent light and stray light in the X-ray tube, and clearly reveal the diffraction lines that are lost in the background intensity, thereby improving the performance of the instrument. sensitivity and precision. [0003] The internal structure of pyrolytic graphite on the market is not high in crystallographic orientation, and its performance parameters are not as good as single crystal graphite. With the continuous development of equipment and devices, the performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B28/14C30B29/02
CPCC30B28/14C30B29/02
Inventor 肖艳红
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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