CN115643733A - Graphene composite copper heat-conducting film and preparation method thereof - Google Patents
Graphene composite copper heat-conducting film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene composite copper heat-conducting film and a preparation method thereof, wherein the preparation method comprises the following steps: adding graphene oxide into water and stirring to obtain graphene oxide slurry; adding a copper sulfate solution into the graphene oxide slurry to obtain graphene oxide/copper sulfate composite slurry; coating the graphene oxide-copper sulfate composite slurry on a substrate; sequentially feeding the base material into a tunnel bin and a tunnel furnace which are filled with hydrogen iodide steam to obtain a fluffy graphene composite nano copper film; firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace, and then placing the carbonization furnace and the graphitization furnace to obtain a heat-treated fluffy graphene composite nano copper film; and placing the fluffy graphene composite nano copper film subjected to heat treatment in a vacuum high-temperature hot-pressing sintering furnace. By updating the formula and the process, copper is attached to the surface of the graphene and fills and covers gaps among graphene sheets, so that the thermal conductivity of the graphene heat-conducting film in the thickness direction is improved.
Description
Technical Field
The invention belongs to the technical field of preparation of heat-conducting films, and particularly relates to a graphene composite copper heat-conducting film and a preparation method thereof.
Background
This section provides background information related to the present disclosure only and is not necessarily prior art.
With the development of mobile phones towards high performance and miniaturization, the heat productivity of chips is larger and is limited by narrow space, and heat is easy to gather to form hot spots, so that the chips cannot normally work, and therefore materials with higher transverse heat conductivity are adopted for carrying out uniform heating. For 4G mobile phones, the material is usually an artificial graphite heat dissipation film, which is prepared from a polyimide film as a raw material through carbonization, graphitization and calendaring processes. The artificial graphite radiating film is limited by polyimide film raw materials, has limited thickness (less than 100 mu m) and cannot deal with higher heat productivity of 5G mobile phone chips. Due to the difference of the process and the raw materials, the graphene heat dissipation film breaks through the limitation of thickness, and can meet the requirement of even heating of a 5G mobile phone chip, so that the graphene heat dissipation film is widely applied.
The graphene heat-conducting film is prepared from graphene oxide serving as a raw material by adopting processes of pulping, coating, carbonizing, graphitizing and rolling. Because the graphene oxide contains rich oxygen-containing functional groups, the graphene oxide is very easy to disperse in water to obtain stable high-solid-content slurry. In the slurry coating process, the graphene oxide is self-assembled into oriented arrangement through the hydrogen bond between sheets and the van der waals force action. At a higher temperature, the graphene oxide is reduced to graphene, and then the graphene oxide is graphitized to repair crystal lattices and is calendered to improve the density, so that the graphene heat-conducting film with oriented graphene arrangement is finally obtained. Since graphene is a thermally conductive anisotropic material, its two-dimensional plane direction has ultrahigh thermal conductivity (theoretically 5300W/(m · K)), but its thermal conductivity is low perpendicular to the two-dimensional plane direction, lower than 20W/(m · K). Therefore, the graphene thermal conductive film with the oriented graphene arrangement has high in-plane thermal conductivity, but the thermal conductivity is low in the thickness direction, generally < 10W/(m · K), which results in that the excellent horizontal thermal conductivity of the graphene thermal conductive film cannot be fully exerted.
Disclosure of Invention
In view of the above problems, a first aspect of the present invention provides a method for preparing a graphene composite copper thermal conductive film, including:
pulping: adding graphene oxide into water and stirring to obtain graphene oxide slurry;
compounding: adding a copper sulfate solution into the graphene oxide slurry to obtain graphene oxide/copper sulfate composite slurry;
coating: coating the graphene oxide-copper sulfate composite slurry on a substrate;
reduction: sequentially feeding the base material into a tunnel bin and a tunnel furnace which are filled with hydrogen iodide steam to obtain a fluffy graphene composite nano copper film;
and (3) heat treatment: firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace, and then placing the carbonization furnace and the graphitization furnace to obtain a heat-treated fluffy graphene composite nano copper film;
vacuum hot pressing: and (3) placing the fluffy graphene composite nano copper film subjected to heat treatment in a vacuum high-temperature hot-pressing sintering furnace at 1400-1800 ℃, wherein the pressure is 10-100 tons, and the vacuumizing pressing time is 10-30min.
And mixing the copper sulfate solution and the graphene oxide slurry, coating the mixture on a substrate to complete reduction, heat treatment and vacuum hot pressing, so that the graphene oxide is reduced into graphene in a tunnel cabin of hydrogen iodide steam, the copper sulfate is reduced into nano copper in the tunnel cabin of the hydrogen iodide steam and is attached to the surface of the graphene, and the water is continuously evaporated in a tunnel furnace. The graphene crystal lattices are repaired in a carbonization furnace and a graphitization furnace, heteroatoms in the fluffy graphene composite nano copper film are removed to obtain a heat-treated fluffy graphene composite nano copper film, the nano copper is in a molten state through vacuum hot pressing, under the action of pressure and vacuum, air in the heat-treated fluffy graphene composite nano copper film is discharged, the distance between graphene sheets is reduced, the nano copper in the molten state can enter the space between the graphene sheets, and the graphene composite copper heat-conducting film is obtained after cooling.
By updating the formula and the process, the copper sulfate solution is converted into nano copper to be introduced, and the copper is attached to the surface of the graphene and fills and covers gaps among graphene sheets through compounding, reduction, heat treatment and vacuum hot pressing.
In some embodiments of the invention, the graphene oxide slurry has a solid content of 2wt% to 6wt%.
In some embodiments of the invention, the copper sulfate solution has a concentration of 0.01 to 0.1mol/L.
In some embodiments of the present invention, the mass ratio of copper in the copper sulfate solution to graphene in graphene oxide is 1:0.2-1.
In some embodiments of the invention, the temperature in the tunnel furnace is 70 ℃ to 90 ℃, the temperature in the carbonization furnace is 1300 ℃ to 1500 ℃, the time in the carbonization furnace is 2 to 6 hours, the temperature in the graphitization furnace is 2850 ℃ to 3000 ℃, and the time in the carbonization furnace is 6 to 10 hours.
The second aspect of the invention provides a graphene composite copper heat conduction film, which is obtained by the preparation method of the graphene composite copper heat conduction film in any one of the above technical schemes.
The graphene composite copper heat-conducting film of the embodiment of the invention has the same beneficial effects as the graphene composite copper heat-conducting film prepared by the preparation method of the graphene composite copper heat-conducting film in any one of the technical schemes, and is not repeated herein.
In some embodiments of the present invention, the mass ratio of copper to graphene in the graphene composite copper thermal conductive film is 1:0.2-1.
In some embodiments of the present invention, in the graphene composite copper thermal conductive film, the copper occupies the surface of the graphene and the gaps between the sheets.
In some embodiments of the present invention, the thickness of the graphene composite copper thermal conductive film is 50-300 μm.
In some embodiments of the present invention, the thickness direction thermal conductivity of the graphene composite copper thermal conductive film is 50-100W/(m · K), and the in-plane thermal conductivity is 1100-1600W/(m · K).
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a flowchart of a method for manufacturing a graphene composite copper thermal conductive film according to an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It is to be understood that the terminology used herein is for the purpose of describing particular example embodiments only, and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" may be intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprises," "comprising," "including," and "having" are inclusive and therefore specify the presence of stated features, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and/or groups thereof.
Although the terms first, second, third, etc. may be used herein to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms may be only used to distinguish one element, component, region, layer or section from another region, layer or section. Terms such as "first," "second," and other numerical terms when used herein do not imply a sequence or order unless clearly indicated by the context. Thus, a first element, component, region, layer or section discussed below could be termed a second element, component, region, layer or section without departing from the teachings of the example embodiments.
For convenience of description, spatially relative terms, such as "inner", "outer", "lower", "below", "upper", "above", and the like, may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. Such spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" or "over" the other elements or features. Thus, the example term "in 8230 \8230; below" may include both upper and lower orientations. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the application of other processes and/or the use of other materials.
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
As shown in fig. 1, a first aspect of the present invention provides a method for preparing a graphene composite copper thermal conductive film, including:
pulping: adding graphene oxide into water and stirring to obtain graphene oxide slurry;
compounding: adding a copper sulfate solution into the graphene oxide slurry to obtain graphene oxide/copper sulfate composite slurry;
coating: coating the graphene oxide-copper sulfate composite slurry on a substrate;
reduction: sequentially feeding the base material into a tunnel bin and a tunnel furnace which are filled with hydrogen iodide steam to obtain a fluffy graphene composite nano copper film;
and (3) heat treatment: firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace, and then placing the carbonization furnace and the graphitization furnace to obtain a heat-treated fluffy graphene composite nano copper film;
vacuum hot pressing: and (3) placing the fluffy graphene composite nano copper film subjected to heat treatment in a vacuum high-temperature hot-pressing sintering furnace at 1400-1800 ℃, wherein the pressure is 10-100 tons, and the vacuumizing pressing time is 10-30min.
And mixing the copper sulfate solution and the graphene oxide slurry, coating the mixture on a substrate to complete reduction, heat treatment and vacuum hot pressing, so that the graphene oxide is reduced into graphene in a tunnel cabin of hydrogen iodide steam, the copper sulfate is reduced into nano copper in the tunnel cabin of the hydrogen iodide steam and is attached to the surface of the graphene, and the water is continuously evaporated in a tunnel furnace. The graphene lattice is repaired in a carbonization furnace and a graphitization furnace, heteroatoms in the fluffy graphene composite nano copper film are removed to obtain a fluffy graphene composite nano copper film subjected to heat treatment, the nano copper is in a molten state through vacuum hot pressing at last, under the action of pressure and vacuum, air inside the fluffy graphene composite nano copper film subjected to heat treatment is discharged, the distance between graphene sheet layers is reduced, the nano copper in the molten state can enter the space between the graphene sheet layers, and the graphene composite copper heat-conducting film is obtained after cooling.
By updating the formula and the process, the copper sulfate solution is converted into nano copper to be introduced, and the copper is attached to the surface of the graphene and fills and covers gaps among graphene sheets through compounding, reduction, heat treatment and vacuum hot pressing.
In some embodiments of the invention, the graphene oxide slurry has a solid content of 2wt% to 6wt%.
In some embodiments of the invention, the concentration of the copper sulfate solution is 0.01 to 0.1mol/L.
In some embodiments of the invention, the mass ratio of copper in the copper sulfate solution to graphene in the graphene oxide is 1:0.2-1.
In some embodiments of the invention, the temperature in the tunnel furnace is 70 ℃ to 90 ℃, the temperature in the carbonization furnace is 1300 ℃ to 1500 ℃, the time in the carbonization furnace is 2 to 6 hours, the temperature in the graphitization furnace is 2850 ℃ to 3000 ℃, and the time in the carbonization furnace is 6 to 10 hours.
The following description will be given of preparing an electrothermal film composed of graphene/polyurethane composite films according to a comparative example and preparing a graphene composite copper heat-conducting film according to different examples:
example one
Pulping: adding graphene oxide into water, and stirring in a double-planet vacuum stirrer to obtain graphene oxide slurry with the solid content of 6 wt%;
compounding: adding a copper sulfate solution with the concentration of 0.05mol/L into the graphene oxide slurry according to the mass ratio of copper to graphene being 1.2, and fully stirring to obtain graphene oxide/copper sulfate composite slurry;
coating: coating the graphene oxide/copper sulfate composite slurry on a base material;
reduction: firstly, feeding a base material into a tunnel bin filled with hydrogen iodide steam, reducing graphene oxide into graphene, reducing copper sulfate into nano copper to be attached to the surface of the graphene, feeding the base material into a tunnel furnace at the temperature of 70 ℃, and evaporating water to obtain a fluffy graphene composite nano copper film;
and (3) heat treatment: firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace for treatment at 1300 ℃ for 4h, then treating in a graphitization furnace at 3000 ℃ for 10h, repairing graphene lattices, and removing heteroatoms to obtain the fluffy graphene composite nano copper film after heat treatment;
vacuum hot pressing: and (3) feeding the fluffy graphene composite nano copper film subjected to the heat treatment into a vacuum high-temperature hot-pressing sintering furnace, and vacuumizing and pressing for 30min at 1400 ℃ and 100 tons of pressure. Under the action of pressure and vacuum, air in the fluffy graphene composite nano copper film after heat treatment is discharged, the distance between graphene sheet layers is reduced, gaps between the sheet layers are filled and covered by molten copper, and the graphene composite copper heat-conducting film is obtained after cooling.
According to the test of the graphene composite copper conducting film by a thermogravimetric analyzer, the mass ratio of copper to graphene is 1:0.2, the thickness is 50 μm measured by a thickness gauge, the thermal conductivity in the thickness direction is 100W/(m.K) measured by a laser thermal conductivity tester, and the in-plane thermal conductivity is 1600W/(m.K).
Example two
Pulping: adding graphene oxide into water, and stirring in a double-planet vacuum stirrer to obtain graphene oxide slurry with the solid content of 2 wt%;
compounding: adding a copper sulfate solution with the concentration of 0.1mol/L into the graphene oxide slurry according to the mass ratio of 1;
coating: coating the graphene oxide/copper sulfate composite slurry on a base material;
reduction: firstly, feeding a base material into a tunnel bin filled with hydrogen iodide steam, reducing graphene oxide into graphene, reducing copper sulfate into nano copper to be attached to the surface of the graphene, feeding the base material into a tunnel furnace at the temperature of 90 ℃, and evaporating water to obtain a fluffy graphene composite nano copper film;
and (3) heat treatment: firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace for treatment at 1500 ℃ for 4h, then treating in a graphitization furnace at 3000 ℃ for 6h, repairing graphene lattices, and removing heteroatoms to obtain the fluffy graphene composite nano copper film after heat treatment;
vacuum hot pressing: and (3) feeding the fluffy graphene composite nano copper film subjected to the heat treatment into a vacuum high-temperature hot-pressing sintering furnace, and vacuumizing and pressing for 10min at 1800 ℃ under 50 tons of pressure. Under the action of pressure and vacuum, air in the fluffy graphene composite nano copper film after heat treatment is discharged, the distance between graphene sheet layers is reduced, gaps between the sheet layers are filled and covered by molten copper, and the graphene composite copper heat-conducting film is obtained after cooling.
According to the test of the graphene composite copper conducting film by a thermogravimetric analyzer, the mass ratio of copper to graphene is 1:1, the thickness is 300 μm measured by a thickness gauge, the thermal conductivity in the thickness direction is 50W/(mK) measured by a laser thermal conductivity tester, and the in-plane thermal conductivity is 1100W/(mK).
Comparative example one (graphene composite carbon fiber heat-conducting film, compare with example one)
Step 1: adding a certain amount of graphite oxide into deionized water for dispersion to prepare slurry with the solid content of 6wt%, and stirring in a double-planet vacuum stirrer to obtain uniformly dispersed graphene oxide slurry;
step 2, adding 1 part of high-thermal-conductivity carbon fiber powder into 20 parts of concentrated sulfuric acid, acidifying for 2 hours to acidify and activate the surface of the carbon fiber, and washing and drying to obtain acidified fiber powder;
step 3, adding high-thermal-conductivity carbon fiber powder accounting for 5% of graphene oxide content into the slurry, wherein the diameter of carbon fiber is about 7 microns, and the length of the carbon fiber is 50 microns, and fully mixing the carbon fiber powder and the slurry in a double-planet vacuum mixer for 2 hours to obtain graphene oxide/carbon fiber composite slurry;
step 4, coating the composite slurry obtained in the step 3 on a coating machine to form a film, and drying the film to obtain a graphene oxide/carbon fiber composite film;
step 5, treating the obtained composite membrane for 4 hours at 1300 ℃, and then treating the composite membrane for 10 hours at 3000 ℃ in a graphitization furnace to complete graphitization to obtain a graphene membrane;
and 6, further vacuumizing and pressing the obtained graphene film for 30min under the pressure of 100 tons to obtain the high-thermal-conductivity graphene/carbon fiber composite heat-conducting film with the thickness of 50 micrometers, wherein the in-plane direction thermal conductivity coefficient can reach 1200W/(m.K), and the vertical direction thermal conductivity coefficient can reach 30W/(m.K).
Comparative example two (graphene composite thermal conductive film, compare with example one)
Step 1: adding a certain amount of graphite oxide into deionized water for dispersion to prepare slurry with the solid content of 6wt%, and stirring in a double-planet vacuum stirrer to obtain uniformly dispersed graphene oxide slurry;
step 2, coating the graphene oxide slurry obtained in the step 1 on a coating machine to form a film, and drying the film to obtain a graphene oxide film;
step 3, treating the obtained graphene oxide film at 1300 ℃ for 4h, and then treating the graphene oxide film in a graphitization furnace at 3000 ℃ for 10h to complete graphitization to obtain a graphene film;
and 4, further vacuumizing and pressing the obtained graphene film for 30min under the pressure of 100 tons to obtain the high-thermal-conductivity graphene heat-conducting film with the thickness of 50 microns, wherein the in-plane thermal conductivity coefficient can reach 1550W/(m.K), and the vertical thermal conductivity coefficient can reach 5W/(m.K).
As can be seen from the comparison between the first example, the second example, the first comparative example and the second comparative example, the in-plane thermal conductivity of the samples is not much different, but the thickness direction thermal conductivity of the first example and the second example is greatly improved compared with that of the first comparative example and the second comparative example. Through analyzing the mass ratio of copper to graphene in the final sample, it can be seen that the introduction of copper plays a decisive role in the improvement of the thermal conductivity in the thickness direction.
The second aspect of the invention provides a graphene composite copper heat-conducting film, which is obtained by the preparation method of the graphene composite copper heat-conducting film in any one of the technical schemes.
The graphene composite copper heat-conducting film of the embodiment of the invention has the same beneficial effects as the graphene composite copper heat-conducting film prepared by the preparation method of the graphene composite copper heat-conducting film in any one of the technical schemes, and is not repeated herein.
In some embodiments of the present invention, the mass ratio of copper to graphene in the graphene composite copper thermal conductive film is 1:0.2-1.
In some embodiments of the present invention, in the graphene composite copper thermal conductive film, copper occupies the gaps between graphene sheets. The copper is attached to the surface of the graphene and fills and covers gaps among graphene sheets, and the copper has good thermal conductivity, so that the thermal conductivity of the graphene heat-conducting film in the thickness direction is improved, and the in-plane thermal conductivity is kept.
In some embodiments of the present invention, the thickness of the graphene composite copper thermal conductive film is 50-300 μm.
In some embodiments of the present invention, the graphene composite copper thermal conductive film has a thickness direction thermal conductivity of 50 to 100W/(m · K) and an in-plane thermal conductivity of 1100 to 1600W/(m · K).
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of a graphene composite copper heat conduction film is characterized by comprising the following steps:
pulping: adding graphene oxide into water and stirring to obtain graphene oxide slurry;
compounding: adding a copper sulfate solution into the graphene oxide slurry to obtain graphene oxide/copper sulfate composite slurry;
coating: coating the graphene oxide-copper sulfate composite slurry on a substrate;
reduction: sequentially feeding the base material into a tunnel bin and a tunnel furnace which are filled with hydrogen iodide steam to obtain a fluffy graphene composite nano copper film;
and (3) heat treatment: firstly, placing the fluffy graphene composite nano copper film in a carbonization furnace, and then placing the carbonization furnace and the graphitization furnace to obtain a heat-treated fluffy graphene composite nano copper film;
vacuum hot pressing: and (3) placing the fluffy graphene composite nano copper film subjected to heat treatment in a vacuum high-temperature hot-pressing sintering furnace at 1400-1800 ℃, wherein the pressure is 10-100 tons, and the vacuumizing pressing time is 10-30min.
2. The preparation method of the graphene composite copper heat conduction film according to claim 1, wherein the solid content of the graphene oxide slurry is 2wt% to 6wt%.
3. The method for preparing the graphene composite copper heat-conducting film according to claim 1, wherein the concentration of the copper sulfate solution is 0.01-0.1mol/L.
4. The method for preparing the graphene composite copper heat-conducting film according to claim 1, wherein the mass ratio of copper in the copper sulfate solution to graphene in the graphene oxide is 1:0.2-1.
5. The method for preparing the graphene composite copper heat-conducting film according to claim 1, wherein the temperature in the tunnel furnace is 70 ℃ to 90 ℃, the temperature in the carbonization furnace is 1300 ℃ to 1500 ℃, the time in the carbonization furnace is 2 to 6 hours, the temperature in the graphitization furnace is 2850 ℃ to 3000 ℃, and the time in the carbonization furnace is 6 to 10 hours.
6. A graphene composite copper heat-conducting film obtained by the method for preparing a graphene composite copper heat-conducting film according to any one of claims 1 to 5.
7. The graphene composite copper heat conduction film according to claim 6, wherein the mass ratio of copper to graphene in the graphene composite copper heat conduction film is 1:0.2-1.
8. The graphene composite copper thermal conductive film according to claim 7, wherein in the graphene composite copper thermal conductive film, the copper occupies voids between the graphene sheets.
9. The graphene composite copper heat conduction film according to claim 6, wherein the thickness of the graphene composite copper heat conduction film is 50-300 μm.
10. The graphene composite copper heat-conducting film according to claim 6, wherein the graphene composite copper heat-conducting film has a thickness direction thermal conductivity of 50-100W/(m-K) and an in-plane thermal conductivity of 1100-1600W/(m-K).
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