CN114214042A - Application of graphene film as high-temperature-resistant thermal interface material or heat dissipation film material - Google Patents
Application of graphene film as high-temperature-resistant thermal interface material or heat dissipation film material Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F21V29/00—Protecting lighting devices from thermal damage; Cooling or heating arrangements specially adapted for lighting devices or systems
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Abstract
The invention relates to the technical field of new materials and application thereof, in particular to application of a graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material. The graphene film has excellent heat conductivity in the in-plane direction and the vertical plane direction: the in-plane thermal conductivity is 400-1500W/mK, and the vertical plane thermal conductivity is 10-180W/mK; the graphene film has good flexibility and excellent heat conductivity, and is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material which has high heat conductivity in the plane and the vertical plane and is all-carbon high-temperature-resistant. The prepared graphene film has high crystallization quality and flexibility, and has excellent heat conductivity in the in-plane direction and the vertical plane direction. The graphene film is of an all-carbon structure with high crystallization quality, can be stably used in an air environment below 800 ℃, and has great application potential in the field of thermal management.
Description
Technical Field
The invention relates to the technical field of new materials and application thereof, in particular to application of a graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material.
Background
The graphene serving as a new material has excellent heat-conducting property, and the heat-conducting coefficient is as high as 5300W m-1K-1Much higher than carbon nanotubes and diamond. In addition, the graphene is a honeycomb-shaped perfect lattice formed by a single layer of carbon atoms, and has high structural stability and chemical stability. Therefore, graphene has great application potential in the field of thermal management.
With the miniaturization and integration of electronic devices, the power density of electronic devices has increased dramatically, and the heat dissipation of electronic devices is becoming a bottleneck restricting the performance improvement thereof. The heat dissipation film material is more and more widely applied to various electronic devices, especially portable devices such as mobile phones, flat panels, notebooks and the like. Because the graphite/graphene material has thermal conductivity far higher than that of a metal material and good flexibility, the current commercial heat dissipation films mainly comprise two types, namely a graphite film prepared by taking polyimide (which is strictly required as a raw material and is produced mainly in Japan and has a neck risk) as a precursor and a graphene film prepared by taking graphene oxide as a raw material. The polyimide is used as a precursor, a film with the thickness of below 50 micrometers can be generally prepared, the preparation process has strict requirements on raw materials, and the high-end polyimide precursor film is mainly produced by foreign enterprises such as Japan and has neck clamping risk. Dangerous chemicals such as potassium permanganate and concentrated sulfuric acid are generally involved in the preparation process of the graphene oxide, the preparation process is complex, chemical impurities and products are difficult to separate after mixing, and the difficulty in removing the impurities is high. Meanwhile, due to the existence of a large number of defects such as surface functional groups, even if the subsequent complex reduction process is carried out, the heat conduction and the electric conductivity of the alloy are still not ideal. Especially, the thermal conductivity is two to three orders of magnitude lower than that of the intrinsic graphene due to the damaged crystal lattice. Meanwhile, the two types of film preparation processes both require a slow heating carbonization process for more than ten hours and a subsequent ultrahigh temperature graphitization process for more than eight hours (the temperature is generally more than 2800 ℃, which consumes very much energy).
In addition, the heat-resistant high-performance thermal interface material which is very important and cannot be overcome always remains in the field of thermal management. The traditional metal material and ceramic material have higher heat-conducting property, but can not be directly used as a thermal interface material due to higher hardness. Although the polymer-based thermal interface material can provide good interface contact, the thermal conductivity of the polymer-based thermal interface material is poor, and the general thermal conductivity is 10W m-1K-1Below, and due to the presence of the polymeric matrix material, it withstands temperatures generally below 150 ℃; while the conventional graphite/graphene-based film material has good flexibility and high-temperature resistance, the conventional graphite/graphene-based film material has the characteristics of highly oriented (along the plane direction) structure and anisotropic heat conduction. The thermal conductivity of the thermal interface material is much lower than 10W m in the required vertical plane-1K-1Generally at 5W m-1K-1The following are completely unsatisfactory for application.
As described above, the two major types of graphite/graphene films have problems that are difficult to overcome in terms of preparation process and application performance. Therefore, the bottleneck problem is overcome, and the high-temperature-resistant high-performance graphene film material is developed to be applied to the fields of heat dissipation film materials and heat conduction interface materials, and has important significance.
Disclosure of Invention
The invention aims to provide an application of a graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material, wherein the graphene film material has high temperature resistance and excellent heat conduction performance in a plane and a vertical plane direction, solves the problem that the two types of graphite/graphene films are difficult to overcome in preparation process and application performance at present, and can be applied to the fields of heat dissipation film materials and heat conduction interface materials.
The technical scheme of the invention is as follows:
the graphene film has excellent heat conductivity in the in-plane direction and the vertical plane direction: the in-plane thermal conductivity is 400-1500W/mK, and the vertical plane thermal conductivity is 10-180W/mK; the graphene film has good flexibility and excellent heat conductivity, and is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material which has high heat conductivity in the plane and the vertical plane and is all-carbon high-temperature resistant; the high-temperature-resistant thermal interface material is an all-carbon heat conduction gasket which can be stably used in a high-temperature environment and can resist the temperature in the air to be more than 800 ℃; the heat dissipation film material is a graphene heat dissipation film with adjustable thickness.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, and the preparation method of the graphene film comprises the following steps:
(1) heating the reaction furnace cavity to a set temperature of 600-1200 ℃ under the protective atmosphere of carrier gas;
(2) placing a three-dimensionally communicated porous metal matrix with high porosity and high density into a constant-temperature area of a cavity of the reaction furnace, introducing reducing gas, and preserving heat for 0-60 min;
(3) introducing mixed atmosphere of carbon source gas, reducing gas and carrier gas into the cavity of the reaction furnace, and catalytically growing graphene on the surface of the porous metal substrate; the flow ratio of the carbon source gas, the reducing gas and the carrier gas in the mixed atmosphere is 1: (0-80): (0-100), and the reaction time is 1-120 min;
(4) cooling the porous metal matrix in a carrier gas protective atmosphere, and taking out the porous metal matrix to obtain a three-dimensionally communicated high-density graphene skeleton structure growing on the porous metal matrix;
(5) removing the porous metal matrix by using a metal etching liquid to obtain three-dimensional porous graphene;
(6) and pressing the obtained three-dimensional porous graphene to form a graphene film.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, in the step (1), the carrier gas protective atmosphere is one or a mixture of more than two of argon, nitrogen and helium, the set temperature is 900-1100 ℃, and the reaction in the step (3) is carried out at the set temperature to grow the graphene.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, and in the step (2), the porous metal matrix is IIIPorous alloy formed by one or more than two of communicated porous nickel, porous copper, porous iron, porous cobalt, porous silver, porous gold, porous platinum and porous titanium with high porosity and high density; the porosity of the porous metal matrix is 210-4000 PPI, and the surface density is 0.5-6.5 g/cm3。
In the step (3), the carbon source gas is one or more than two of methane, ethane, ethylene and acetylene, the reducing gas is one or two of hydrogen and ammonia, and the carrier gas is one or more than two of argon, nitrogen and helium.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, and in the step (4), the carrier gas protective atmosphere is one or a mixture of more than two of argon, nitrogen and helium.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, and in the step (5), the metal etching liquid is one or a mixed aqueous solution of more than two of hydrochloric acid, sulfuric acid, nitric acid, ammonium persulfate and ferric chloride.
The graphene film is applied as a high-temperature-resistant thermal interface material or a heat dissipation film material, in the step (6), the three-dimensional porous graphene is pressed into a film in an extrusion or rolling mode, and the pressure is 0.2-300 MPa.
The method can regulate and control the thickness, the pores and the form of the prepared porous graphene by selecting different porous metal matrixes and/or regulating and controlling the temperature and the reaction atmosphere growth parameters in the reduction reaction; the thickness range of the prepared graphene film is 10-1000 mu m, and the density of the graphene film is 0.8-2.2 g/cm3(ii) a The graphene film is of a three-dimensional full-connected structure, and due to the catalytic activity of the porous metal matrix, the graphene film which is not required to be graphitized and has excellent crystallization quality is obtained: the Raman spectrum of the graphene film is characterized, the characteristic peak of the graphene is obvious and has no defect peak (D peak); the X-ray diffraction pattern of the graphene film is characterized, the characteristic diffraction peak of the graphene is obvious, the peak position is 26.5 degrees, and the half degreeThe height and width are 0.102 degrees, and no peak position shift and miscellaneous peaks exist.
The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material shows that the graphene film can endure the temperature in the air of more than 800 ℃ when being used as the high-temperature-resistant thermal interface material or the heat dissipation film material.
The design mechanism of the invention is as follows:
the method takes three-dimensionally communicated porous metal with high porosity and high density as a template, and utilizes a chemical vapor deposition process to catalytically grow a graphene layer on the surface of the metal template under the conditions of proper temperature and atmosphere. And removing the metal substrate to obtain the three-dimensionally communicated porous graphene skeleton. Pressing the three-dimensional graphene skeleton into a flexible film by applying pressure. The thickness, the pore space and the like of the graphene film can be regulated and controlled by regulating and controlling preparation parameters. The invention has simple process and low production cost. The prepared graphene film has high crystallization quality and flexibility, and has excellent heat conductivity in the in-plane direction and the vertical plane direction. The graphene film is of an all-carbon structure with high crystallization quality, and can be stably used in an air environment below 800 ℃.
The invention has the following advantages and beneficial effects:
1. the method takes the three-dimensionally communicated height as a substrate template to catalyze and grow the graphene. The shape and thickness of the prepared graphene can be regulated and controlled by regulating and controlling the type and the growth parameters, so that different application requirements are met.
2. All reactants and reaction liquid except inert carrier gas can be recycled, harmful waste gas and waste liquid are not generated in the whole process, and the preparation method is low-carbon and environment-friendly.
3. Due to the high reaction temperature and the catalytic activity of the transition metal matrix, the graphene film prepared by the method has the crystallization quality which is comparable to that of the mechanically exfoliated eigen-state graphene. The Raman spectrum shows that the characteristic peak of the graphene is obvious and has no defect peak (D peak). The XRD result shows that the graphene film has obvious characteristic diffraction peak, 26.5 degrees of peak position, 0.102 degree of full width at half maximum and no peak position shift and impurity peak. Therefore, the graphene film is excellent in thermal conductivity.
4. The thermal weight loss result shows that the graphene film can tolerate the temperature of 800 ℃ in the air. Therefore, the material is different from the traditional heat-conducting interface material (the heat conductivity is generally below 10W/mK, and the temperature resistance is generally below 150 ℃), and can be used as a high-performance high-temperature-resistant (the heat conductivity is above 10W/mK, and the temperature resistance is above 800 ℃) thermal interface material.
5. The heat conductivity of the traditional heat dissipation film material in the vertical plane direction is very low and is far lower than 10W m-1K-1Typically at 5Wm-1K-1The temperature difference gradient in the direction vertical to the plane of the radiating film is obvious, heat is difficult to be effectively transferred in the whole radiating film material, and the performance of the radiating performance of the material is seriously influenced. The heat dissipation film material prepared by the invention has the heat conductivity of more than 10W/mK in the vertical plane direction, and has better heat dissipation performance compared with the traditional heat dissipation film material.
6. The invention has simple process, easy amplification and mass production, does not need to go through the processes of carbonization and graphitization which are time and energy consuming (the carbonization process generally needs dozens of hours for slow temperature rise, the temperature of the subsequent graphitization process needs more than 2800 ℃ and takes more than eight hours), and has low production cost.
7. The graphene film material provided by the invention does not appear in the prior art, has positive technical effects and application, and has great application potential in the field of thermal management.
Drawings
Fig. 1 is a photomicrograph of a graphene film.
Fig. 2 is a photomicrograph (surface) of a graphene film.
Fig. 3 is a photomicrograph (side) of a graphene film.
Fig. 4 is a raman spectrum of a graphene film.
Fig. 5 is an XRD characteristic peak of the graphene film. In the figure, the abscissa 2 θ represents the diffraction angle (degree) and the ordinate Intensity represents the relative Intensity (a.u.).
Fig. 6 is a thermogravimetric plot of graphene membrane.
Fig. 7 is a photograph of a thermal interface application scene of a high-power LED street lamp.
FIG. 8 is a schematic view of a device for testing the cooling effect of a thermal interface material. In the figure, 1, an infrared thermal imager, 2, an LED street lamp, 3, a radiator, 4, an environment temperature monitor, 5 and a thermal interface.
FIG. 9 is a schematic view of a device for testing the heat dissipation effect of a heat dissipation film material. In the figure, 6, an infrared thermometer, 7, a ceramic heating sheet, 8, a heat dissipation film, 9, an environment temperature monitor, 10 and a constant voltage and constant current power supply.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples. The thermal conductivity of the prepared graphene film was tested by using LFA 467 flash method thermal conductivity instrument (the instrument is widely used in domestic electronic product manufacturing enterprises and scientific research units at present, and the test is performed according to ASTM E1461 standard).
Example 1:
in this example, the cavity of the reactor was heated to 1000 ℃ under a nitrogen atmosphere, and a constant temperature zone of the cavity of the reactor was filled with a solution having a porosity of 500PPI and an areal density of 2.5g/cm3Introducing hydrogen into the three-dimensionally communicated porous nickel with high porosity and high density, keeping the temperature for 10min, wherein the flow of the hydrogen is 600sccm, and the function of introducing the hydrogen firstly is as follows: removing the oxide layer on the surface of the substrate; and (2) continuously introducing a mixed gas of ethylene and hydrogen, wherein the flow rate of the mixed gas is 620sccm, and the flow rate ratio of the ethylene to the hydrogen in the mixed gas is 1: and 30, reacting for 30min, and catalytically growing graphene on the surface of the three-dimensionally communicated high-porosity high-density porous nickel base.
Taking out the three-dimensionally communicated high-density graphene skeleton growing on the porous metal substrate in a nitrogen protective atmosphere, putting the three-dimensionally communicated high-density graphene skeleton into 3mol/L hydrochloric acid aqueous solution (etching solution), preserving heat for 60min at 80 ℃, completely removing nickel in the graphene skeleton, taking out the graphene skeleton, cleaning and drying to obtain the three-dimensionally communicated hollow graphene skeleton structure. And (3) placing the graphene framework in a tablet press die, and applying pressure of 30MPa to obtain the graphene membrane.
As shown in fig. 1, the macrostructure of the graphene film is shown in fig. 2 and fig. 3, which are respectively the micrographs of the surface and the side surface of the graphene film, and it can be seen from the figure that the graphene film has a three-dimensionally connected microstructure.
As shown in fig. 4, it can be seen from the raman spectrum of the obtained sample that the graphene prepared by the method has high crystalline quality due to the high reaction temperature and the catalytic activity of the metal matrix. The Raman spectrum shows that the characteristic peak of the graphene is obvious and has no defect peak (D peak).
As shown in fig. 5, the XRD result can see that the graphene film has a distinct graphene characteristic diffraction peak, a peak position of 26.5 degrees, a full width at half maximum of 0.102 degrees, and no peak position shift and no miscellaneous peak.
As shown in fig. 6, the thermal weight loss results show that the material can withstand a temperature of 800 ℃ in air, and thus has excellent thermal conductivity. The thickness of the prepared graphene film is 100 mu m, and the density is 1.5g/cm3The in-plane thermal conductivity was 910W/mK, and the vertical-plane thermal conductivity was 42W/mK.
In the following embodiments, the shape of the hollow graphite film after the metal substrate is etched is substantially the same as that of embodiment 1 in terms of raman spectrum, XRD, and thermogravimetric results, which are not described again.
Example 2:
heating the cavity of the reaction furnace to 1000 ℃ under the protection of argon, adding 800PPI with porosity and 3.5g/cm of surface density into the constant-temperature area of the cavity of the reaction furnace3The three-dimensional communicated high-porosity high-density porous copper is introduced with hydrogen, the flow of the hydrogen is 500sccm, and the hydrogen is introduced firstly: removing the oxide layer on the surface of the substrate; and continuously introducing a mixed gas of methane and hydrogen, wherein the flow rate of the mixed gas is 510sccm, and the flow rate ratio of the methane to the hydrogen in the mixed gas is 1: and (3) reacting for 50min, and catalytically growing graphene on the surface of the three-dimensionally communicated high-porosity high-density porous copper substrate.
Taking out the three-dimensionally communicated high-density graphene skeleton growing on the porous metal substrate in a nitrogen protective atmosphere, putting the three-dimensionally communicated high-density graphene skeleton into 2mol/L sulfuric acid aqueous solution (etching solution), preserving heat for 120min at 80 ℃, completely removing copper in the graphene skeleton, taking out the graphene skeleton, cleaning and drying to obtain the three-dimensionally communicated hollow graphene skeleton structure. Placing the graphene skeleton under pressureAnd applying 40MPa pressure in a sheet machine die to obtain the graphene film. The thickness of the prepared graphene film is 120 mu m, and the density is 1.8g/cm3The in-plane thermal conductivity was 830W/mK, and the vertical-plane thermal conductivity was 60W/mK.
Example 3:
heating the cavity of the reaction furnace to 1100 ℃ under the protection of argon, adding 1100PPI with porosity of 1100 and surface density of 5.1g/cm into the constant-temperature zone of the cavity of the reaction furnace3The three-dimensional communicated porous nickel with high porosity and high density is introduced with hydrogen, the flow of the hydrogen is 500sccm, and the hydrogen is introduced firstly: removing the oxide layer on the surface of the substrate; and continuously introducing a mixed gas of methane, hydrogen and argon, wherein the flow rate of the mixed gas is 1010sccm, and the flow ratio of the methane to the hydrogen in the mixed gas is 1: and (3) reacting for 70min for 50min, and catalytically growing graphene on the surface of the three-dimensionally communicated high-porosity high-density porous nickel base.
Taking out the three-dimensionally communicated high-density graphene skeleton growing on the porous metal substrate in a nitrogen protective atmosphere, putting the three-dimensionally communicated high-density graphene skeleton into 3mol/L hydrochloric acid aqueous solution (etching solution), preserving heat for 90min at 80 ℃, completely removing nickel in the graphene skeleton, taking out the graphene skeleton, cleaning and drying to obtain the three-dimensionally communicated hollow graphene skeleton structure. And (3) placing the graphene framework in a tablet press die, and applying 80MPa pressure to obtain the graphene membrane. The obtained graphene film has a thickness of 155 μm and a density of 1.95g/cm3The in-plane thermal conductivity was 1030W/mK, and the vertical-plane thermal conductivity was 30W/mK.
Example 4:
heating the cavity of the reaction furnace to 1100 ℃ under the protection of argon, adding 1550PPI with the porosity of 5.3g/cm into the constant-temperature area of the cavity of the reaction furnace3The three-dimensional communicated porous nickel-copper alloy with high porosity and high density is introduced with hydrogen, the flow of the hydrogen is 500sccm, and the hydrogen is introduced firstly: removing the oxide layer on the surface of the substrate; and continuously introducing a mixed gas of methane, hydrogen and argon, wherein the flow rate of the mixed gas is 1010sccm, and the flow ratio of the methane to the hydrogen in the mixed gas is 1: 50, the reaction time is 80min, and the three-dimensional connected high-porosity high-density porous nickel-copper alloyAnd catalytically growing graphene on the surface of the gold substrate.
Taking out the three-dimensionally communicated high-density graphene framework growing on the porous metal substrate in a nitrogen protective atmosphere, putting the three-dimensionally communicated high-density graphene framework into 3mol/L hydrochloric acid aqueous solution (etching solution), preserving heat for 110min at 80 ℃, completely removing nickel-copper alloy in the graphene framework, taking out the graphene framework, cleaning and drying to obtain the three-dimensionally communicated hollow graphene framework structure. And (3) placing the graphene framework in a tablet press die, and applying 180MPa pressure to obtain the graphene membrane. The thickness of the prepared graphene film is 105 mu m, and the density is 2.1g/cm3The in-plane thermal conductivity is 1248W/mK and the vertical in-plane thermal conductivity is 35W/mK.
Example 5:
heating the cavity of the reaction furnace to 1050 ℃ under the nitrogen protection atmosphere, adding a constant temperature zone of the cavity of the reaction furnace with a porosity of 950PPI and an area density of 4.2g/cm3The three-dimensional communicated porous cobalt with high porosity and high density is introduced with hydrogen, the flow of the hydrogen is 500sccm, and the hydrogen is introduced firstly: removing the oxide layer on the surface of the substrate; and continuously introducing a mixed gas of methane, hydrogen and argon, wherein the flow rate of the mixed gas is 1010sccm, and the flow ratio of the methane to the hydrogen in the mixed gas is 1: and 50, reacting for 60min, and catalytically growing graphene on the surface of the three-dimensionally communicated high-porosity high-density porous cobalt base body.
Taking out the three-dimensionally communicated high-density graphene skeleton growing on the porous metal substrate in a nitrogen protective atmosphere, putting the three-dimensionally communicated high-density graphene skeleton into 3mol/L hydrochloric acid aqueous solution (etching solution), preserving heat for 110min at 80 ℃, completely removing cobalt in the graphene skeleton, taking out the graphene skeleton, cleaning and drying to obtain the three-dimensionally communicated hollow graphene skeleton structure. And (3) placing the graphene framework in a tablet press die, and applying pressure of 90MPa to obtain the graphene membrane. The thickness of the prepared graphene film is 115 mu m, and the density is 1.74g/cm3The in-plane thermal conductivity of the material is 945W/mK, and the vertical-plane thermal conductivity of the material is 48W/mK.
Application example 1:
the graphene film described in example 2 is applied to a thermal interface (position shown by arrow in the figure) between a high-power LED street lamp (heat source) and a heat sink shown in fig. 7 as a thermal interface material, and the temperature reduction effect of the material is evaluated by testing the highest temperature at the center point of the LED street lamp by using the device shown in fig. 8.
As shown in fig. 8, the device for testing the cooling effect of the thermal interface material comprises: the LED street lamp comprises an infrared thermal imager 1, an LED street lamp 2 (heat source), a radiator 3, an ambient temperature monitor 4 and the like, wherein the radiator 3 is arranged at the bottom of the LED street lamp 2, a thermal interface material is arranged at a thermal interface 5 between the radiator 3 and the LED street lamp 2, the infrared thermal imager 1 is arranged above the LED street lamp 2, and the ambient temperature is tested through the ambient temperature monitor 4.
Under constant power, the lower the surface temperature of the LED street lamp is, the lower the thermal interface material can better reduce the thermal interface contact resistance, and the cooling effect is more excellent. The equipment is stably operated for 15min at the room temperature of 24.5 ℃, and the temperature is stable. And measuring the highest temperature of the central point of the LED street lamp to be 50.5 ℃. Since the cooling test conditions in the comparative examples described later are consistent, they are not described again.
Application comparative example 1:
a commercial thermal pad having a thickness of 0.5mm and a nominal thermal conductivity of 10W/mK was applied to the thermal interface shown in fig. 7. Under the test condition consistent with the application example 1, the highest temperature of the center point of the LED street lamp is measured to be 62.6 ℃.
The graphene film material disclosed by the invention is used as a thermal interface material, and has a more excellent cooling effect compared with a traditional commercial heat-conducting gasket material. Meanwhile, the graphene film material can resist the high temperature of 800 ℃ in the air. The material has wide application prospect as a high-performance high-temperature-resistant (the thermal conductivity is more than 10W/mK, and the temperature resistance is more than 800 ℃) thermal interface material.
Application example 2:
the graphene film described in example 4 was applied to heat dissipation of electronic devices as a heat dissipation film material, and a heat dissipation effect test was performed using the apparatus shown in fig. 9.
As shown in fig. 9, the device for testing the heat dissipation effect of the heat dissipation film material comprises an infrared thermometer 6, a ceramic heating sheet 7, a heat dissipation film 8, an ambient temperature monitor 9, a constant voltage and constant current power supply 10, and the like, wherein the heat dissipation film 8 is attached to the back surface of the ceramic heating sheet 7, the infrared thermometer 6 is arranged above the ceramic heating sheet 7, the ceramic heating sheet 7 is connected with the constant voltage and constant current power supply 10 through a circuit, and the ambient temperature is tested through the ambient temperature monitor 9.
Wherein the area of the ceramic heating sheet is 1cm multiplied by 1cm, and the resistance is about 18 omega. The heating current used was about 0.3A. The equipment is stably operated for 15min at the room temperature of 24.5 ℃, and the temperature is stable. The surface temperature of the ceramic heating sheet is measured to be about 320 ℃ under the condition of not adding any heat dissipation film. And (3) after the heat dissipation film with the thickness of 3cm multiplied by 3cm is pasted on the back surface of the ceramic heating sheet, the surface temperature of the ceramic heating sheet is measured to be 84.4 ℃. Since the cooling test conditions in the comparative examples described later are consistent, they are not described again.
Application comparative example 2:
after the ceramic heating sheet is pasted with the same area and thickness and the nominal thermal conductivity is 1200W/mK, the surface temperature of the ceramic heating sheet is measured to be 93.1℃ under the same test condition.
Because the heat conductivity of the traditional heat dissipation film material in the vertical plane direction is very low and is far lower than 10W m-1K-1Generally at 5W m-1K-1The temperature difference gradient in the direction vertical to the plane of the radiating film is obvious, heat is difficult to be effectively transferred in the whole radiating film material, and the performance of the radiating performance of the material is seriously influenced. The heat dissipation film material prepared by the invention has the heat conductivity of more than 10W/mK in the vertical plane direction, and has better heat dissipation performance compared with the traditional heat dissipation film material. Experiments show that the graphene film material provided by the invention is used as a heat dissipation film material, and has a more excellent heat dissipation effect compared with a traditional commercial heat dissipation film material.
In conclusion, the graphene film disclosed by the invention is controllable in form and thickness, high in crystallization quality, excellent in heat conductivity, simple in preparation method and process, recyclable and reusable in most raw materials, and low in preparation cost. The examples provided above for the preparation of the graphene film are only for illustration and should not be considered as limiting the scope of the present invention, and any method of equivalent substitution or modification according to the technical solution of the present invention and the inventive concept thereof should be covered within the scope of the present invention.
Claims (10)
1. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material is characterized in that the graphene film has excellent heat conductivity in the in-plane direction and the vertical plane direction: the in-plane thermal conductivity is 400-1500W/mK, and the vertical plane thermal conductivity is 10-180W/mK; the graphene film has good flexibility and excellent heat conduction performance, and is applied as a high-temperature resistant thermal interface material or a heat dissipation film material which has excellent heat conduction performance in the plane and the vertical plane and is all-carbon high-temperature resistant; the high-temperature-resistant thermal interface material is an all-carbon heat conduction gasket which can be stably used in a high-temperature environment and can resist the temperature in the air to be more than 800 ℃; the heat dissipation film material is a graphene heat dissipation film with adjustable thickness.
2. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 1, wherein the preparation method of the graphene film comprises the following steps:
(1) heating the reaction furnace cavity to a set temperature of 600-1200 ℃ under the protective atmosphere of carrier gas;
(2) placing a three-dimensionally communicated porous metal matrix with high porosity and high density into a constant-temperature area of a cavity of the reaction furnace, introducing reducing gas, and preserving heat for 0-60 min;
(3) introducing mixed atmosphere of carbon source gas, reducing gas and carrier gas into the cavity of the reaction furnace, and catalytically growing graphene on the surface of the porous metal substrate; the flow ratio of the carbon source gas, the reducing gas and the carrier gas in the mixed atmosphere is 1: (0-80): (0-100), and the reaction time is 1-120 min;
(4) cooling the porous metal matrix in a carrier gas protective atmosphere, and taking out the porous metal matrix to obtain a three-dimensionally communicated high-density graphene skeleton structure growing on the porous metal matrix;
(5) removing the porous metal matrix by using a metal etching liquid to obtain three-dimensional porous graphene;
(6) and pressing the obtained three-dimensional porous graphene to form a graphene film.
3. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (1), the protective atmosphere of carrier gas is one or a mixture of more than two of argon, nitrogen and helium, the set temperature is 900-1100 ℃, and the reaction in the step (3) to grow graphene is carried out at the set temperature.
4. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (2), the porous metal matrix is a porous alloy formed by one or more than two of three-dimensionally connected porous nickel, porous copper, porous iron, porous cobalt, porous silver, porous gold, porous platinum and porous titanium with high porosity and high density; the porosity of the porous metal matrix is 210-4000 PPI, and the surface density is 0.5-6.5 g/cm3。
5. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (3), the carbon source gas is one or more than two of methane, ethane, ethylene and acetylene, the reducing gas is one or two of hydrogen and ammonia, and the carrier gas is one or more than two of argon, nitrogen and helium.
6. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (4), the carrier gas protective atmosphere is one or a mixture of more than two of argon, nitrogen and helium.
7. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (5), the metal etching solution is one or a mixed aqueous solution of more than two of hydrochloric acid, sulfuric acid, nitric acid, ammonium persulfate and ferric chloride.
8. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 2, wherein in the step (6), the three-dimensional porous graphene is pressed into a film by means of extrusion or rolling, and the pressure is 0.2-300 MPa.
9. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to any one of claims 2 to 8, wherein the method can regulate and control the thickness, the pores and the morphology of the prepared porous graphene by selecting different porous metal substrates and/or regulating and controlling the temperature in the reduction reaction and the growth parameters of the reaction atmosphere; the thickness range of the prepared graphene film is 10-1000 mu m, and the density of the graphene film is 0.8-2.2 g/cm3(ii) a The graphene film is of a three-dimensional full-connected structure, and due to the catalytic activity of the porous metal matrix, the graphene film which is not required to be graphitized and has excellent crystallization quality is obtained: the Raman spectrum of the graphene film is characterized, the characteristic peak of the graphene is obvious and has no defect peak (D peak); the X-ray diffraction pattern of the graphene film is characterized in that the characteristic diffraction peak of the graphene is obvious, the peak position is 26.5 degrees, the full width at half maximum is 0.102 degree, and no peak position shift and miscellaneous peaks exist.
10. The application of the graphene film as a high-temperature-resistant thermal interface material or a heat dissipation film material according to claim 9, wherein the thermal weight loss result shows that the graphene film can withstand a temperature of more than 800 ℃ in the air when being used as the high-temperature-resistant thermal interface material or the heat dissipation film material.
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