CN115367744A - Secondary-formed high-thermal-conductivity graphene thick film and preparation method thereof - Google Patents
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- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
- H05K7/20436—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing
- H05K7/20445—Inner thermal coupling elements in heat dissipating housings, e.g. protrusions or depressions integrally formed in the housing the coupling element being an additional piece, e.g. thermal standoff
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- C01B2204/32—Size or surface area
Abstract
The invention discloses a post-forming high-thermal-conductivity graphene thick film and a preparation method thereof, wherein the method comprises the following steps: obtaining a single-layer heat-conducting graphene film; sequentially attaching a plurality of single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying for 2-10 h to obtain a multilayer heat-conducting graphene film; pressurizing the multilayer heat-conducting graphene film for 12-36 h under the condition of 10-30 Mpa, and fully drying at the temperature of 40 ℃; and pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours under the conditions of protective gas at 300-400 ℃ and 10-30 Mpa to obtain the secondary formed high-heat-conducting graphene thick film. The preparation method simplifies the preparation process, avoids the use of various additives, and the obtained secondary-formed high-thermal-conductivity graphene thick film has the advantages of excellent traditional thermal and mechanical properties and the like, and has the characteristics of low process cost and contribution to large-scale preparation.
Description
Technical Field
The invention relates to the technical field of graphene heat dissipation composite materials, in particular to a secondary formed high-thermal-conductivity graphene thick film and a preparation method thereof.
Background
With the vigorous development of the semiconductor industry and the technical innovation of graphics card ray tracing and the like, the heat conduction material has more profound practical significance and future value. Taking the display card market as an example, the 1080Ti process of the highest-end consumer-grade display card in the market in 2016 is 16nm, the average full-load power consumption is 250W, the 3090Ti process of the consumer-grade flagship display card issued by Nvidia in 2022 in 1 month is 8nm, the average full-load power consumption is more than 450W, the full-load power consumption of part of 3090Ti with special specifications can even reach 516W, and the ultrahigh power consumption of the next generation 40-series flagship display card which is going to be marketed in 2023 is very likely to reach 800W. Along with the trend of continuous reduction of the manufacturing process of the electronic device chip and explosive rise of power, the heat dissipation capability of the electronic device is seriously examined. For example, for cellcept chips such as cellcept 888 and 8gen1 with high pass, the serious heating problem greatly affects the user experience, even results such as failure of the mobile phone hardware due to overheating. The improvement of heat conduction materials is taken as an important ring for improving the heat dissipation of electronic equipment, and is a scientific and technological hotspot and a consumption hotspot, and liquid gold is taken as a superior substitute product of heat conduction silicone grease to enter a consumption-level market. Nowadays, the heat dissipation capability of electronic products has become one of the important factors considered when consumers choose products, manufacturers pay more attention to the heat dissipation modules in mobile phones and computers, and the effective heat conduction area of the heat dissipation modules increases year by year. There are indications that the heat-dissipating military provision is underway.
Graphene has excellent thermal, optical, electrical and mechanical properties, and is one of the most popular carbon materials at present. In the aspect of heat conduction materials, graphene has extremely high application value, and a graphene heat conduction film with ultrahigh heat conduction coefficient (more than 1000W/mk) is an important solution for the heat dissipation problem of electronic equipment, so that the graphene heat conduction film can replace the current commercial polyimide film. The heat dissipation benefit of the heat-conducting film is basically proportional to the thickness of the heat-conducting film under the condition that the heat conductivity coefficient is not greatly reduced. Compared with the method of simply improving the heat conductivity coefficient, the method of improving the thickness of the heat-conducting film is a performance improvement mode with more cost performance. However, when the thickness of the thermal conductive film reaches millimeter order, if graphene is used as a main component, the thermal conductivity of the graphene thick film is generally in a lower value range due to factors such as difficult orientation. Due to the technical problem, a preparation process of the graphene thick film is rarely reported in the industry, and the preparation process is complex in steps, is not beneficial to large-scale production and needs to be optimized to obtain a more efficient production mode.
Disclosure of Invention
The invention provides a preparation method of a secondary formed high-thermal-conductivity graphene thick film, which comprises the following steps:
obtaining a single-layer heat-conducting graphene film;
sequentially attaching a plurality of single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying to obtain a multilayer heat-conducting graphene film;
primarily pressurizing the multilayer heat-conducting graphene film under the condition of 10-30 Mpa, and fully drying the multilayer heat-conducting graphene film at the temperature of 40 ℃;
and pressurizing the fully dried multilayer heat-conducting graphene film under the conditions of protective gas at 300-400 ℃ and 10-30 Mpa to obtain the secondary formed high heat-conducting graphene thick film.
Preferably, the single-layer heat-conducting graphene film is obtained by an expansion intercalation method.
Preferably, before a plurality of single-layer heat-conducting graphene films coated with the graphene oxide solution are sequentially attached and are kept stand and dried for 2-10 hours to obtain a multilayer heat-conducting graphene film, the method further comprises the following steps: fully cleaning the single-layer heat-conducting graphene film by using deionized water and ethanol; and uniformly coating the graphene oxide solution on the surface of the single-layer heat-conducting graphene film.
Preferably, the concentration of the graphene oxide solution is 5-15 mg/mL.
Preferably, the solvent of the graphene oxide solution is deionized water or 50% ethanol.
Preferably, the standing time is 2-10 h, the preliminary pressurizing time is 12-36 h, and the re-pressurizing time is 24h.
Preferably, the number of the tablets is 2-5.
Preferably, the protective gas is argon, helium or nitrogen.
Preferably, the purity of the protective gas is 99.999%.
The invention also provides a secondary formed high-thermal-conductivity graphene thick film, which is obtained by any one of the preparation methods, wherein the thickness of the secondary formed high-thermal-conductivity graphene thick film is 140-850 mu m, and the thermal conductivity is 660-1200W/mK.
According to the invention, the graphene oxide film is bonded by utilizing the self-assembly phenomenon of graphene oxide in the solvent evaporation process, the graphene oxide bonding process is a simple self-assembly process between carbon materials, the flow is simple, no other kinds of binders are involved, and the thickness is improved while most of the thermal conductivity of the graphene film is kept. According to the invention, surface modification treatment is not required to be carried out on a single-layer film, unnecessary preparation processes are simplified, the use of various additives is avoided, and the obtained high-thermal-conductivity graphene thick film has the advantages of excellent traditional thermal and mechanical properties and the like, and also has the characteristics of low process cost and contribution to large-scale preparation.
Drawings
Fig. 1 is a flow chart of a preparation method of a post-formed high thermal conductivity graphene thick film;
fig. 2 is an SEM image of the post-formed high thermal conductivity graphene thick film;
fig. 3 is an XPS energy spectrum of an overmolded graphene thick film with high thermal conductivity.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
S100, preparing the single-layer heat-conducting graphene film by using an expansion intercalation method, which comprises the following specific steps:
dispersing 20g of crystalline flake graphite in 1000mL of dimethylformamide, performing ultrasonic treatment for 10 minutes to form a dispersion, precipitating the dispersion for 2 hours, slowly adding a hydrogen peroxide solution until no bubbles are generated, slowly adding 50mL of 15% ammonium hydroxide solution to balance acidity to enable the pH value to be 8.0, and stirring for 1 hour by using a magnetic stirrer to form a primary dispersion suspension;
carrying out suction filtration on the primary dispersion suspension, adding 1000mL of deionized water after suction filtration, and fully mixing to enable the graphene sheets to form 0.5mg/mL of dispersion;
vacuum filtering the graphene sheet dispersion on a non-woven fabric with the aperture of 0.5 mu m to obtain a film;
drying the film for 12 hours at 40 ℃ by using infrared equipment, and then secondarily drying the film for 6 hours on a double-layer dryer at 120 ℃; carrying out thermal reduction on the dried film at 2600 ℃ for 0.5h, wherein the protective gas is argon, and the reducing gas is hydrogen;
compacting the graphite film subjected to the drying thermal reduction by using a precision calender under the hydraulic pressure of 30Mpa to obtain a single-layer heat-conducting graphene film, wherein the thickness of the single-layer heat-conducting graphene film is 70 mu m, and the heat conductivity coefficient is 1456W/mk;
fully cleaning 2 sheets of the single-layer graphene film by using deionized water and ethanol;
s200, uniformly coating a graphene oxide solution on the surface of a single-layer heat-conducting graphene film, wherein the concentration of the graphene oxide solution is 5mg/mL, and the solvent of the graphene oxide solution is deionized water or 50% ethanol;
attaching 2 single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying for 2 hours to obtain a multilayer heat-conducting graphene film;
s300, pressurizing the multilayer heat-conducting graphene film for 12 hours under the condition of 10Mpa, and fully drying the multilayer heat-conducting graphene film at the temperature of 40 ℃;
s400, pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours at 300 ℃ and 10Mpa under the protection of argon gas to obtain a secondary formed high heat-conducting graphene thick film, wherein the thickness of the secondary formed high heat-conducting graphene thick film is 145 mu m, and the heat conductivity coefficient is 1242W/mk.
Example 2
S100, preparing the single-layer heat-conducting graphene film by using an expansion intercalation method, which comprises the following specific steps:
dispersing 40g of flake graphite in 1000mL of chlorosulfonic acid, performing ultrasonic treatment for 20 minutes to form a dispersion, precipitating the dispersion for 3 hours, slowly adding a hydrogen peroxide solution until no bubbles are generated, slowly adding 100mL of a 15% ammonium hydroxide solution to balance acidity to make the pH value be 8.5, and stirring for 1 hour by using a magnetic stirrer to form a primary dispersed suspension;
carrying out suction filtration on the primary dispersion suspension, adding 1000mL of deionized water after suction filtration, and fully mixing to enable the graphene flakes to form a 1mg/mL dispersion;
vacuum filtering the graphene sheet dispersion on a non-woven fabric with the aperture of 2 mu m to obtain a film;
drying the film for 18 hours at 50 ℃ by using infrared equipment, and then secondarily drying the film for 8 hours on a double-layer dryer at 120 ℃; carrying out thermal reduction on the dried film at 2800 ℃ for 1h, wherein the protective gas is argon, and the reducing gas is hydrogen;
compacting the graphite film subjected to the drying thermal reduction by using a precision calender under the hydraulic pressure of 40Mpa to obtain a single-layer heat-conducting graphene film, wherein the thickness of the single-layer heat-conducting graphene film is 140 mu m, and the heat conductivity coefficient is 1284W/mk;
fully washing 3 sheets of the single-layer graphene film by using deionized water and ethanol;
s200, uniformly coating a graphene oxide solution on the surface of a single-layer heat-conducting graphene film, wherein the concentration of the graphene oxide solution is 10mg/mL, and the solvent of the graphene oxide solution is deionized water or 50% ethanol;
attaching 3 single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying for 6 hours to obtain a multilayer heat-conducting graphene film;
s300, pressurizing the multilayer heat-conducting graphene film for 24 hours under the condition of 20Mpa, and fully drying the multilayer heat-conducting graphene film at the temperature of 40 ℃;
s400, pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours at 350 ℃ and 20Mpa under the protection of argon gas to obtain a secondary formed high heat-conducting graphene thick film, wherein the thickness of the secondary formed high heat-conducting graphene thick film is 430 microns, and the heat conductivity coefficient is 894W/mk.
Example 3
S100, preparing the single-layer heat-conducting graphene film by using an expansion intercalation method, which comprises the following specific steps:
dispersing 20g of flake graphite in 1000mL of dimethylformamide, performing ultrasonic treatment for 30 minutes to form a dispersion, precipitating the dispersion for 4 hours, slowly adding a hydrogen peroxide solution until no bubbles are generated, slowly adding 50mL of 15% ammonium hydroxide solution to balance acidity to enable the pH value to be 8.0, and stirring for 1 hour by using a magnetic stirrer to form a primary dispersed suspension;
carrying out suction filtration on the primary dispersion suspension, adding 1000mL of deionized water after suction filtration, and fully mixing to enable the graphene sheets to form 0.5mg/mL of dispersion;
vacuum filtering the graphene sheet dispersion on a non-woven fabric with the aperture of 0.5 mu m to obtain a film;
drying the film for 12 hours at 40 ℃ by using infrared equipment, and then secondarily drying the film for 6 hours on a double-layer dryer at 120 ℃; carrying out thermal reduction on the dried film at 2700 ℃ for 1.5h, wherein the protective gas is argon and the reducing gas is hydrogen;
compacting the graphite film subjected to the drying thermal reduction by using a precision calender under the hydraulic pressure of 50Mpa to obtain a single-layer heat-conducting graphene film, wherein the thickness of the single-layer heat-conducting graphene film is 70 mu m, and the heat conductivity coefficient is 1473W/mk;
fully washing 4 sheets of the single-layer graphene film by using deionized water and ethanol;
s200, uniformly coating a graphene oxide solution on the surface of a single-layer heat-conducting graphene film, wherein the concentration of the graphene oxide solution is 15mg/mL;
attaching 4 single-layer heat-conducting graphene films coated with graphene oxide solution, standing and drying for 10 hours to obtain a multilayer heat-conducting graphene film, wherein the solvent of the graphene oxide solution is deionized water or 50% ethanol;
s300, pressurizing the multilayer heat-conducting graphene film for 36 hours under the condition of 30Mpa, and fully drying the multilayer heat-conducting graphene film at the temperature of 40 ℃;
s400, pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours at 400 ℃ and 30Mpa under the protection of argon gas to obtain a secondary formed high heat-conducting graphene thick film, wherein the thickness of the secondary formed high heat-conducting graphene thick film is 294 mu m, and the heat conductivity coefficient is 1081W/mk.
Example 4
S100, preparing the single-layer heat-conducting graphene film by using an expansion intercalation method, which comprises the following specific steps:
dispersing 60g of flake graphite in 1000mL of dimethylformamide, performing ultrasonic treatment for 30 minutes to form a dispersion, precipitating the dispersion for 4 hours, slowly adding a hydrogen peroxide solution until no bubbles are generated, slowly adding 75mL of 15% ammonium hydroxide solution to balance acidity to enable the pH value to be 9.0, and stirring for 1 hour by using a magnetic stirrer to form a primary dispersed suspension;
carrying out suction filtration on the primary dispersion suspension, adding 1000mL of deionized water after suction filtration, and fully mixing to enable the graphene sheets to form a 1.5mg/mL dispersion;
vacuum filtering the graphene sheet dispersion on a non-woven fabric with the aperture of 3 mu m to obtain a film;
drying the film for 18h by using infrared equipment at 40 ℃, and then secondarily drying the film for 12h on a double-layer dryer at 120 ℃; carrying out thermal reduction on the dried film at 2900 ℃ for 1h, wherein the protective gas is nitrogen, and the reducing gas is hydrogen;
compacting the graphite film subjected to the drying thermal reduction by using a precision calender under the hydraulic pressure of 50Mpa to obtain a single-layer heat-conducting graphene film, wherein the thickness of the single-layer heat-conducting graphene film is 210 mu m, and the heat conductivity coefficient is 1156W/mk;
fully cleaning 4 sheets of the single-layer graphene film by using deionized water and ethanol;
s200, uniformly coating a graphene oxide solution on the surface of a single-layer heat-conducting graphene film, wherein the concentration of the graphene oxide solution is 15mg/mL, and the solvent of the graphene oxide solution is deionized water or 50% ethanol;
attaching 4 single-layer heat-conducting graphene films coated with the graphene oxide solution, and standing and drying for 10 hours to obtain a multilayer heat-conducting graphene film;
s300, pressurizing the multilayer heat-conducting graphene film for 36 hours under the condition of 30Mpa, and fully drying at the temperature of 40 ℃;
s400, pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours at 400 ℃ and 30Mpa under the protection of argon gas to obtain a secondary formed high heat-conducting graphene thick film, wherein the thickness of the secondary formed high heat-conducting graphene thick film is 836 microns, and the heat conductivity coefficient is 668W/mk.
Example 5
S100, preparing the single-layer heat-conducting graphene film by using an expansion intercalation method, which comprises the following specific steps:
dispersing 20g of flake graphite in 1000mL of chlorosulfonic acid, performing ultrasonic treatment for 20 minutes to form a dispersion, precipitating the dispersion for 3 hours, slowly adding a hydrogen peroxide solution until no bubbles are generated, slowly adding 25mL of 15% ammonium hydroxide solution to balance acidity to make the pH value be 8.0, and stirring for 1 hour by using a magnetic stirrer to form a primary dispersed suspension;
carrying out suction filtration on the primary dispersion suspension, adding 1000mL of deionized water after suction filtration, and fully mixing to enable the graphene sheets to form 0.5mg/mL of dispersion;
vacuum filtering the graphene sheet dispersion on a non-woven fabric with the aperture of 1 mu m to obtain a film;
drying the film for 12 hours at 40 ℃ by using infrared equipment, and then secondarily drying the film for 6 hours on a double-layer dryer at 120 ℃; carrying out thermal reduction on the dried film at 3000 ℃ for 1h, wherein the protective gas is helium, and the reducing gas is hydrogen;
compacting the graphite film subjected to the drying thermal reduction by using a precision calender under the hydraulic pressure of 30Mpa to obtain a single-layer heat-conducting graphene film, wherein the thickness of the single-layer heat-conducting graphene film is 70 mu m, and the heat conductivity coefficient is 1479W/mk;
fully cleaning 5 sheets of the single-layer graphene film by using deionized water and ethanol;
s200, uniformly coating a graphene oxide solution on the surface of a single-layer heat-conducting graphene film, wherein the concentration of the graphene oxide solution is 10mg/mL, and the solvent of the graphene oxide solution is deionized water or 50% ethanol;
attaching 5 single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying for 8 hours to obtain a multilayer heat-conducting graphene film;
s300, pressurizing the multilayer heat-conducting graphene film for 18 hours under the condition of 20Mpa, and fully drying the multilayer heat-conducting graphene film at the temperature of 40 ℃;
s400, pressurizing the fully dried multilayer heat-conducting graphene film for 24 hours at 350 ℃ and 20Mpa under the protection of argon to obtain a secondary formed high heat-conducting graphene thick film, wherein the thickness of the secondary formed high heat-conducting graphene thick film is 369 microns, and the heat conductivity coefficient is 984W/mk.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of a post-forming high-thermal-conductivity graphene thick film is characterized by comprising the following steps:
obtaining a single-layer heat-conducting graphene film;
sequentially attaching a plurality of single-layer heat-conducting graphene films coated with the graphene oxide solution, standing and drying to obtain a multilayer heat-conducting graphene film;
primarily pressurizing the multilayer heat-conducting graphene film under the condition of 10-30 Mpa, and fully drying the graphene film at the temperature of 40 ℃;
and pressurizing the fully dried multilayer heat-conducting graphene film under the conditions of protective gas at 300-400 ℃ and 10-30 Mpa to obtain the secondary formed high heat-conducting graphene thick film.
2. The method for preparing an overmolded graphene thick film according to claim 1, wherein the single layer of thermally conductive graphene film is obtained by an expansion intercalation process.
3. The method for preparing an overmolded graphene thick film according to claim 1, wherein the steps of sequentially laminating a plurality of single-layer graphene films coated with graphene oxide solution, and standing and drying the laminated graphene films to obtain a multilayer graphene film further comprise: fully cleaning the single-layer heat-conducting graphene film by using deionized water and ethanol; and uniformly coating the graphene oxide solution on the surface of the single-layer heat-conducting graphene film.
4. The method for preparing an overmolded thick graphene film according to claim 1, wherein the concentration of the graphene oxide solution is 5-15 mg/mL.
5. The method for preparing an overmolded graphene thick film according to claim 4, wherein the solvent of the graphene oxide solution is deionized water or 50% ethanol.
6. The method for preparing an overmolded thick graphene film according to claim 1, wherein the standing time is 2-10 hours, the preliminary pressing time is 12-36 hours, and the re-pressing time is 24 hours.
7. The method for preparing an overmolded thick graphene film according to claim 1, wherein the number of sheets is 2 to 5.
8. The method for preparing an overmolded thick graphene film according to claim 1, wherein the protective gas is argon, nitrogen or helium.
9. The method for preparing a secondary formed graphene thick film with high thermal conductivity of claim 8, wherein the purity of the protective gas is 99.999%.
10. An overmolded thick graphene film, obtained by the preparation method of any one of claims 1 to 9, having a thickness of 140 to 850 μm and a thermal conductivity of 660 to 1200W/mK.
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| CN114536883A (en) * | 2022-01-26 | 2022-05-27 | 杭州热流新材料有限公司 | Preparation method of high-thermal-conductivity thick film with large-size graphene interface |
| CN114751404A (en) * | 2022-04-29 | 2022-07-15 | 上海大学 | High-thermal-conductivity graphene thick film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20130236715A1 (en) * | 2012-03-08 | 2013-09-12 | Aruna Zhamu | Graphene oxide gel bonded graphene composite films and processes for producing same |
| CN107140619A (en) * | 2017-05-27 | 2017-09-08 | 杭州高烯科技有限公司 | A kind of graphene thick film of high heat conduction and preparation method thereof |
| CN112760082A (en) * | 2021-02-23 | 2021-05-07 | 银河之星成都新能源有限公司 | High-thermal-conductivity graphene film and preparation method thereof |
| CN112969355A (en) * | 2021-04-22 | 2021-06-15 | 世星科技股份有限公司 | Graphene heat dissipation film and preparation method thereof |
| CN114381240A (en) * | 2022-01-26 | 2022-04-22 | 杭州热流新材料有限公司 | Preparation method of C/metal composite interface welding high-thermal-conductivity thick film |
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