CN112357915A - Graphene film with high heat conductivity and good buffering property for liquid crystal screen and preparation method thereof - Google Patents

Graphene film with high heat conductivity and good buffering property for liquid crystal screen and preparation method thereof Download PDF

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Publication number
CN112357915A
CN112357915A CN202011398739.4A CN202011398739A CN112357915A CN 112357915 A CN112357915 A CN 112357915A CN 202011398739 A CN202011398739 A CN 202011398739A CN 112357915 A CN112357915 A CN 112357915A
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graphene
film
graphene oxide
liquid crystal
temperature
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何大平
傅华强
王哲
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Wuhan Yannuoja Technology Co ltd
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Wuhan Yannuoja Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/198Graphene oxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/24Thermal properties

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a graphene film for a liquid crystal screen with high heat conductivity and good buffering property and a preparation method thereof, wherein the method comprises the following steps: step 1, preparing graphene oxide gel/suspension, and adding a foaming agent into the graphene oxide gel/suspension; and 2, uniformly stirring the gel/suspension liquid added with the foaming agent in the last step, preparing the graphene oxide film by a vacuum filtration, blade coating, spin coating or hydrothermal evaporation method, and drying the graphene oxide film. The graphene film prepared by the invention has a fluffy porous structure, can keep the excellent heat conduction performance of the graphene film, and can absorb energy by utilizing the buffer characteristic of deformation of the fluffy porous structure when being impacted, so that the graphene film has a certain mechanical protection effect when being applied to a liquid crystal screen and has good heat dissipation performance.

Description

Graphene film with high heat conductivity and good buffering property for liquid crystal screen and preparation method thereof
Technical Field
The invention relates to the field of novel material preparation, in particular to a graphene film for a liquid crystal display screen with high heat conductivity and good buffering property and a preparation method thereof.
Background
The liquid crystal screen is an important man-machine interaction component in the visual equipment, and the service life and the reliability in the service period of the liquid crystal screen determine the service performance of the equipment. However, a backlight source in the liquid crystal screen, such as a cold cathode fluorescent lamp, may generate a large amount of heat during the working process, and a circuit board near the screen may also generate a higher temperature, and if the heat cannot be led out in time, the heat will heat the liquid crystal screen, which may cause problems such as screen splash, code confusion, touch failure, and service life reduction of the screen, and may seriously affect the reliability of the screen, or even may cause liquid crystal burnout. Therefore, heat dissipation of the lcd is a problem to be solved. In addition, the structure of the lcd panel is usually a stacked structure of a polarizer, a liquid crystal sheet, a glass substrate, an electrode, a circuit board, a diffusion sheet, a backlight source, and the like, and the structure and the glass structure have a certain brittleness, so that it is urgently needed to improve the shock resistance of the structure.
The theoretical thermal conductivity of the graphene is as high as 5000W.m < -1 > K < -1 >, and the graphene has great application potential in the field of heat dissipation modules of electronic devices. However, for the heat dissipation of the liquid crystal display, the graphene is usually doped in a coating or a heat conducting interface material such as silicone grease, heat dissipation glue, etc., and then coated on the back plate of the liquid crystal display, so as to improve the heat dissipation performance. However, due to the shock resistance of the liquid crystal screen, the back of the screen is usually filled with foam or silicone layer, which makes heat difficult to be conducted out. If the graphene material can be invented, the high heat-conducting performance and the anti-seismic performance are considered, and the problem of contradiction between the anti-seismic and heat-dissipation processes of the liquid crystal screen is expected to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a graphene film for a liquid crystal display screen with high heat conductivity and good buffer property and a preparation method thereof.
The technical scheme for solving the technical problems is as follows:
the preparation method of the graphene film for the liquid crystal display screen with high heat conductivity and good buffering property comprises the following steps:
step 1, preparing graphene oxide gel/suspension, and adding a foaming agent into the graphene oxide gel/suspension;
step 2, uniformly stirring the gel/suspension added with the foaming agent in the previous step, preparing a graphene oxide film by a vacuum filtration, blade coating, spin coating or hydrothermal evaporation method, and drying the graphene oxide film;
further, the temperature of the hydrothermal evaporation warm water is between 30 ℃ and 100 ℃;
step 3, heating the graphene oxide film to reduce and foam the graphene oxide film to obtain the graphene oxide film with a porous structure, and regulating and controlling the pore diameter of the porous structure and the thickness of the graphene film by combining stress; in the foaming process, the environmental temperature is increased to the range of C to C +200 ℃, wherein C is the foaming temperature of the foaming agent;
in the temperature rising process, when the temperature is below 1000 ℃, the heating rate is 10 ℃/min to 100 ℃/min, when the temperature is above 1000 ℃, the heating rate is 1 ℃/min to 50 ℃/min, and the temperature is kept for 5min to 24h after reaching the foaming temperature of the foaming agent;
and 4, reducing the graphene oxide film with the porous structure through high-temperature annealing or a chemical reduction process to obtain the fluffy and porous graphene film.
Further, when high-temperature annealing is adopted in the step 4, the annealing temperature is 2000-3000 ℃, and the heat preservation time is 10 min-24 h.
Further, when a chemical reduction process is adopted in the step 4, the reduction is performed by a chemical reducing agent, wherein the chemical reducing agent is any one of hydriodic acid, sodium borohydride, sodium hypophosphite, sodium ascorbate and ethylenediamine.
Further, the foaming agent in the step 1 is a substance which can generate a large amount of gas through pyrolysis after being heated, the foaming agent is an inorganic foaming agent, an organic foaming agent or a physical foaming agent, and the concentration of the foaming agent is between 0.1mg/ml and 10 mg/ml.
Further, step 1 is carried out by gradient temperature drying, and the drying process is as follows: firstly drying for 0.1-48 h at 30-100 ℃, and then drying for 0.1-24h at 100-180 ℃, wherein the thickness of the dried graphene oxide film is between 100nm and 1 mm.
The invention has the beneficial effects that: the graphene film prepared by the invention has a fluffy porous structure, can keep the excellent heat conduction performance of the graphene film, and can absorb energy by utilizing the buffer characteristic of deformation of the fluffy porous structure when being impacted, so that the graphene film has a certain mechanical protection effect when being applied to a liquid crystal screen and has good heat dissipation performance.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of a graphene thin film prepared in example 1;
FIG. 2 is a macroscopic view of the front side of a liquid crystal screen and a back plate attached with a graphene film;
FIG. 3 shows a liquid crystal display panel using a graphene film for heat dissipation;
FIG. 4 is a report of reliability tests of Shenzhen Cin Sidekescience and technology Limited.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
In the embodiment, firstly, graphene oxide is mixed with ultrapure water to prepare graphene oxide gel with a solid content of 20 mg/ml; then preparing a graphene oxide film by coating with a scraper, drying the graphene oxide film at 60 ℃ for 24h, and drying the graphene oxide film at 100 ℃ for 2h under the air pressure environment of 0.1MPa to obtain the graphene oxide film with the thickness of about 50 μm; then, heating the graphene oxide film from room temperature to 300 ℃ and preserving the temperature for 12h for foaming process by applying 0.5MPa stress and adjusting the heating rate to be 20 ℃/min; and finally, reducing the graphene oxide film by high-temperature annealing at 2800 ℃ to obtain a final fluffy and porous graphene film, wherein a cross-sectional scanning electron microscope image of the final fluffy and porous graphene film is shown in fig. 1. As shown in fig. 2, the film is connected to the back plate of the lcd panel by a heat conductive adhesive (silver paste). The loose and porous film has good heat dissipation performance, the heat dissipation effect of the loose and porous film is shown in fig. 3, the reliability test report is provided by Shenzhen Cisco science and technology Limited, and as shown in fig. 4, the result shows that the addition of the prepared graphene film can effectively reduce the temperature of the front surface and the back surface of the liquid crystal screen, so that the loose and porous film has a good heat dissipation effect compared with the conventional graphite sheets in the market. In addition, the porous structure of the loose and porous graphene film is extruded when the loose and porous graphene film is under the action of impact force, so that energy can be absorbed, and the effects of shock resistance and buffering are achieved.
Example 2
In the embodiment, firstly, graphene oxide is mixed with ultrapure water to prepare graphene oxide gel with a solid content of 15mg/ml, and 0.1mg/ml sodium bicarbonate is added as a foaming agent to be uniformly mixed with the graphene oxide gel; preparing a graphene oxide film by spin coating, drying the graphene oxide film at 50 ℃ for 12h, drying the graphene oxide film at 80 ℃ for 4h, drying the graphene oxide film at 100 ℃ for 2h, and drying the graphene oxide film at 120 ℃ and 0.1MPa for 1h to obtain the graphene oxide film with the thickness of about 100 microns; then, heating the graphene oxide film from room temperature to 270 ℃ and preserving the temperature for 6 hours to carry out a foaming process by applying a stress of 0.2MPa and adjusting the heating rate to be 30 ℃/min; and finally, reducing the graphene oxide film by annealing at the high temperature of 2500 ℃ to obtain the final fluffy and porous graphene film. The loose and porous film has good heat dissipation performance, and plays a good role in shock resistance and buffering so as to protect the liquid crystal screen.
Example 3
In the embodiment, firstly, graphene oxide is mixed with ultrapure water to prepare a graphene oxide suspension with a solid content of 2mg/ml, and 0.5mg/ml carbon black is added and added as a foaming agent to be uniformly mixed with the graphene oxide suspension; then preparing a graphene oxide film through vacuum filtration, drying the graphene oxide film at 80 ℃ for 12h, and drying the graphene oxide film at 140 ℃ under the air pressure environment of 0.5MPa for 1h to obtain the graphene oxide film with the thickness of about 25 mu m; then, heating the graphene oxide film from room temperature to 1000 ℃ and preserving the temperature for 12h for foaming process by applying 0.1MPa stress and adjusting the heating rate to 50 ℃/min; and finally, chemically reducing by using hydroiodic acid to obtain the final fluffy and porous graphene film.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. The preparation method of the graphene film for the liquid crystal display screen with high heat conductivity and good buffering property is characterized by comprising the following steps of:
step 1, preparing graphene oxide gel/suspension, and adding a foaming agent into the graphene oxide gel/suspension;
step 2, uniformly stirring the gel/suspension liquid added with the foaming agent in the previous step to prepare a graphene oxide film, and drying the graphene oxide film;
step 3, heating the graphene oxide film to reduce and foam the graphene oxide film to obtain the graphene oxide film with a porous structure, and regulating and controlling the pore diameter of the porous structure and the thickness of the graphene film by combining stress; in the foaming process, the environmental temperature is increased to the range of C to C +200 ℃, wherein C is the foaming temperature of the foaming agent;
in the temperature rising process, when the temperature is below 1000 ℃, the heating rate is 10 ℃/min to 100 ℃/min, when the temperature is above 1000 ℃, the heating rate is 1 ℃/min to 50 ℃/min, and the temperature is kept for 5min to 24h after reaching the foaming temperature of the foaming agent;
and 4, reducing the graphene oxide film with the porous structure through high-temperature annealing or a chemical reduction process to obtain the fluffy and porous graphene film.
2. The method for preparing a graphene film for a liquid crystal display panel having high thermal conductivity and good buffer property according to claim 1, wherein the film-forming method in the step 2 is any one of blade coating, hydrothermal evaporation, vacuum filtration and spin coating.
3. The method for preparing a graphene film for a liquid crystal display with high thermal conductivity and good buffer property according to claim 1, wherein when high temperature annealing is adopted in the step 4, the annealing temperature is 2000 ℃ to 3000 ℃, and the heat preservation time is 10min to 24 h.
4. The method for preparing a graphene film for a liquid crystal display panel having high thermal conductivity and good buffer property according to claim 1, wherein the graphene film is reduced by a chemical reducing agent when a chemical reducing process is adopted in the step 4, wherein the chemical reducing agent is any one of hydriodic acid, sodium borohydride, sodium hypophosphite, sodium ascorbate and ethylenediamine.
5. The method for preparing a graphene film for a liquid crystal display panel having high thermal conductivity and good buffer property according to claim 1, wherein the foaming agent in the step 1 is an inorganic foaming agent, an organic foaming agent or a physical foaming agent, and the concentration of the foaming agent is between 0.1mg/ml and 10 mg/ml.
6. The method for preparing the graphene film for the liquid crystal display with high thermal conductivity and good buffering property according to claim 1, wherein the step 1 is drying at a gradient temperature, and the drying process comprises the following steps: firstly, drying for 0.1-48 h at 30-100 ℃, and then drying for 0.1-24h at 100-180 ℃, wherein the thickness of the dried graphene oxide film is between 100nm and 1 mm.
CN202011398739.4A 2020-12-02 2020-12-02 Graphene film with high heat conductivity and good buffering property for liquid crystal screen and preparation method thereof Pending CN112357915A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113387702A (en) * 2021-06-23 2021-09-14 浙江原邦材料科技有限公司 High-thermal-conductivity graphene composite heat dissipation film and preparation method thereof
CN114801421A (en) * 2022-04-27 2022-07-29 广东墨睿科技有限公司 Preparation method of graphene heat-conducting gasket

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN206005085U (en) * 2016-02-22 2017-03-08 深圳市欣恒坤科技有限公司 A kind of thermal conductivity graphene
JP2018026527A (en) * 2016-07-28 2018-02-15 ジャパンマテックス株式会社 Heat-dissipating material arranged by use of mixed graphite, and method for manufacturing the same
CN111234721A (en) * 2020-01-17 2020-06-05 新纶科技(常州)有限公司 Heat dissipation buffer film
CN111924830A (en) * 2020-09-18 2020-11-13 山东海科创新研究院有限公司 Preparation method of graphene heat-conducting film and product obtained by preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN206005085U (en) * 2016-02-22 2017-03-08 深圳市欣恒坤科技有限公司 A kind of thermal conductivity graphene
JP2018026527A (en) * 2016-07-28 2018-02-15 ジャパンマテックス株式会社 Heat-dissipating material arranged by use of mixed graphite, and method for manufacturing the same
CN111234721A (en) * 2020-01-17 2020-06-05 新纶科技(常州)有限公司 Heat dissipation buffer film
CN111924830A (en) * 2020-09-18 2020-11-13 山东海科创新研究院有限公司 Preparation method of graphene heat-conducting film and product obtained by preparation method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113387702A (en) * 2021-06-23 2021-09-14 浙江原邦材料科技有限公司 High-thermal-conductivity graphene composite heat dissipation film and preparation method thereof
CN114801421A (en) * 2022-04-27 2022-07-29 广东墨睿科技有限公司 Preparation method of graphene heat-conducting gasket

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