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Preparation method of highly ordered and compact graphene heat conduction film

A highly ordered, graphene technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of broken structure, low thermal and electrical conductivity, inapplicability, etc., to improve the density and size of GO film Thin, high thermal conductivity effect

Inactive Publication Date: 2020-11-10
深圳市展旺新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the miniaturization and integration of electronic products, the space constraints are getting higher and higher, and the use of large heat sinks is becoming more and more difficult. Therefore, heat sinks with thin dimensions, high thermal conductivity, and flexibility are required for effective heat management. Layer-suspended graphene has a high thermal conductivity exceeding 5000W / m·k, but it is not suitable for use as a heat dissipation material. The current industrialized flexible thermal conductive film mainly relies on flexible pyrolytic graphite or graphitized polyimide, the highest in-plane The thermal conductivity is 1950W / m·k
[0003] Graphene oxide is the oxide of graphene, because it introduces a large amount of oxygen-containing functional groups such as hydroxyl carboxyl groups on its surface and edge, it can exist stably in aqueous solution and polar solvent, and the solution prepared can be passed through various techniques (including vacuum). Filtration, spraying, rod coating, electrochemical deposition and shear alignment) are fabricated into thin films, but the oxidized graphene is destroyed by the structure of sp2 hybridized carbon, resulting in extremely low thermal conductivity and electrical conductivity, which can be removed by reduction These functional groups, especially high-temperature graphitization can restore the sp2 ene ring structure of graphene. Therefore, we propose a method for preparing a highly ordered and dense graphene thermal conductivity film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] S1, the 10mg / mL graphene oxide (GO) solution is centrifuged at a high speed of 25000rpm for 20min at a speed of 25000rpm, poured off the upper clear night, and concentrated to prepare about 50mg / mL of graphene oxide with a nematic phase liquid crystal;

[0030] S2. Add 0.5% reduced graphene oxide (rGO) powder into S1, grind for 10 minutes with a mortar and mix to prepare rGO / GO colloid;

[0031] S3. The colloid prepared in S2 was prepared into an rGO / GO film by tape casting method, and dried in a vacuum oven at 100°C for 2 hours;

[0032] S4. Put the film prepared in S3 into a quartz tube under an atmosphere of argon (200 sccm, 1 atm) at a heating rate of 1° C. / min, heat it up to 1000° C. for 2 hours, and then cool naturally.

[0033] S5. Graphitize the carbonized film of S4 in a graphite furnace, and raise the temperature to 3000° C. in three stages in an argon (200 L / hr) atmosphere.

[0034] The first stage is from normal temperature to 1200°C, the heating rate is 15...

Embodiment 2

[0039] S1, the 10mg / mL graphene oxide (GO) solution is centrifuged at a high speed of 25000rpm for 20min at a speed of 25000rpm, poured off the upper clear night, and concentrated to prepare about 50mg / mL of graphene oxide with a nematic phase liquid crystal;

[0040] S2. Add 1.5% reduced graphene oxide (rGO) powder into S1, grind for 10 minutes with a mortar and mix to prepare rGO / GO colloid;

[0041] S3. The colloid prepared in S2 was prepared into an rGO / GO film by tape casting method, and dried in a vacuum oven at 100°C for 2 hours;

[0042] S4. Put the film prepared in S3 into a quartz tube under an atmosphere of argon (200 sccm, 1 atm) at a heating rate of 1° C. / min, heat it up to 1000° C. for 2 hours, and then cool naturally.

[0043] S5. Graphitize the carbonized film of S4 in a graphite furnace, and raise the temperature to 3000° C. in three stages in an argon (200 L / hr) atmosphere.

[0044] The first stage is from normal temperature to 1200°C, the heating rate is 15...

Embodiment 3

[0049] S1. Centrifuge the 10 mg / mL graphene oxide (GO) solution at 25000 rpm for 20 min at high speed, pour off the supernatant, and concentrate to prepare about 50 mg / mL of graphene oxide with a nematic liquid crystal;

[0050] S2. Add 2.0% reduced graphene oxide (rGO) powder into S1, grind for 10 minutes with a mortar and mix to prepare rGO / GO colloid;

[0051] S3. The colloid prepared in S2 was prepared into an rGO / GO film by tape casting method, and dried in a vacuum oven at 100°C for 2 hours;

[0052] S4. Put the film prepared in S3 into a quartz tube under an atmosphere of argon (200 sccm, 1 atm) at a heating rate of 1° C. / min, heat it up to 1000° C., keep it for 2 hours, and then cool naturally.

[0053] S5. Graphitize the carbonized film of S4 in a graphite furnace, and raise the temperature to 3000° C. in three stages in an argon (200 L / hr) atmosphere.

[0054] The first stage is from normal temperature to 1200°C, the heating rate is 15°C / min; the second stage is 120...

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Abstract

The invention discloses a preparation method of a highly ordered and compact graphene heat conduction film. The preparation method comprises the following steps: S1, carrying out high-speed centrifugal concentration on a low-concentration graphene oxide (GO) solution to prepare nematic phase liquid crystal graphene oxide; S2, mixing reduced graphene oxide (rGO) powder with S1 to prepare colloid; and S3, preparing the rGO / GO film from the colloid in the S2. According to the preparation method of the highly ordered and compact graphene heat conduction film, a small part of rGO sheets with very small diameters are added to fill gaps in large GO sheet diameters before the film is prepared; in addition, pressure is applied after heat treatment or in the heat treatment process, so that the density of the GO film is further improved; besides, industrial mass production is guaranteed by adopting a mode of calendering treatment after heat treatment, and secondary high-temperature treatment is carried out on a sample after calendering treatment to repair defects in crystal lattices, so that the graphene heat-conducting film which is thin in size, high in heat conductivity and flexible is obtained; herein, the heat conductivity reaches up to 2025W / k.m, and the thickness of the film can be 2-100 microns.

Description

technical field [0001] The invention relates to the technical field of heat management materials, in particular to a method for preparing a highly ordered and dense graphene heat conduction film. Background technique [0002] With the miniaturization and integration of electronic products, the space constraints are getting higher and higher, and the use of large heat sinks is becoming more and more difficult. Therefore, heat sinks with thin dimensions, high thermal conductivity, and flexibility are required for effective heat management. Layer-suspended graphene has a high thermal conductivity exceeding 5000W / m·k, but it is not suitable for use as a heat dissipation material. The current industrialized flexible thermal conductive film mainly relies on flexible pyrolytic graphite or graphitized polyimide, the highest in-plane The thermal conductivity is 1950W / m·k. [0003] Graphene oxide is the oxide of graphene, because it introduces a large amount of oxygen-containing func...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192C01B32/194
CPCC01B32/192C01B32/194C01B2204/24C01B2204/32
Inventor 张世闯曾凡聪高金鸽张江杨亚敏曲勇威
Owner 深圳市展旺新材料科技有限公司