CN114148044A - Graphene composite heat-conducting gasket and preparation method thereof - Google Patents

Graphene composite heat-conducting gasket and preparation method thereof Download PDF

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Publication number
CN114148044A
CN114148044A CN202111404548.9A CN202111404548A CN114148044A CN 114148044 A CN114148044 A CN 114148044A CN 202111404548 A CN202111404548 A CN 202111404548A CN 114148044 A CN114148044 A CN 114148044A
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graphene
foam film
adhesive
conducting
gasket
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CN114148044B (en
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石燕军
葛翔
李峰
卢静
李壮
周步存
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Changzhou Fuxi Technology Co Ltd
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Changzhou Fuxi Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0004—Cutting, tearing or severing, e.g. bursting; Cutter details
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/04—Punching, slitting or perforating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/08—Impregnating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/32—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed at least two layers being foamed and next to each other
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0064—Smoothing, polishing, making a glossy surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/04—Punching, slitting or perforating
    • B32B2038/047—Perforating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2266/00—Composition of foam
    • B32B2266/04—Inorganic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/51—Elastic

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  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Sealing Material Composition (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention provides a preparation method of a graphene composite heat conduction gasket, which comprises the following steps: carrying out laser drilling on the graphene heat-conducting foam film; impregnating the perforated graphene heat-conducting foam film with a first adhesive; stacking the impregnated graphene heat-conducting foam film layers into a mold, and applying pressure to joint adjacent graphene heat-conducting foam films; uniformly coating a second adhesive on the periphery of the pressed graphene heat conduction foam film to completely coat the multilayer graphene heat conduction foam film into a block, wherein the curing temperature of the second adhesive is lower than that of the first adhesive; cutting the cured and molded block into sheets along a stacking direction; carrying out hot-press molding on the sheet; carrying out surface polishing treatment on the sheet subjected to hot press molding; and trimming the edge of the polished sheet, and removing the second adhesive coated on the edge to obtain the graphene composite heat-conducting gasket. The invention also provides a gasket. The invention has low thermal resistance and high resilience.

Description

Graphene composite heat-conducting gasket and preparation method thereof
Technical Field
The invention belongs to the technical field of heat conduction and heat dissipation, and particularly relates to a graphene composite heat conduction gasket and a preparation method thereof.
Background
A heat conducting gasket, a high performance gap-filling heat conducting material, is mainly used for the transfer interface between electronic equipment and a heat sink or a product housing. The graphene has good heat-conducting property and can be used as a reinforcing material of a heat-conducting gasket. The heat-conducting gasket prepared by the graphene heat-conducting film mainly has two modes: firstly, stacking and bonding graphene heat-conducting films layer by layer through an adhesive, and then cutting the graphene heat-conducting films into heat-conducting gaskets so as to arrange the graphene heat-conducting films along the thickness direction; secondly, the graphene heat-conducting film is changed into longitudinal arrangement from the plane direction in a wrinkling mode, and then the graphene heat-conducting film is coated with an adhesive to form an integral structure.
Although the graphene heat-conducting film adopted by the two modes obtains higher heat conductivity coefficient, the prepared heat-conducting gasket has higher hardness due to the compact structure of the graphene heat-conducting film, and the application thermal resistance of the gasket is obviously improved; secondly, the graphene heat-conducting film has a smooth surface, and can be well combined with an adhesive only by performing surface roughening treatment such as nano coating or rough polishing; in addition, the internal graphite-like structure of the graphene heat-conducting film easily causes layering, and influences the overall mechanical stability.
Disclosure of Invention
Aiming at one or more problems in the prior art, the invention provides a preparation method of a graphene composite heat conduction gasket, which comprises the following steps:
carrying out laser drilling on the graphene heat-conducting foam film;
impregnating the perforated graphene heat-conducting foam film with a first adhesive;
stacking the impregnated graphene heat-conducting foam film layers into a mold, and applying pressure to joint adjacent graphene heat-conducting foam films;
uniformly coating a second adhesive on the periphery of the pressed graphene heat conduction foam film to completely coat the multilayer graphene heat conduction foam film into a block, wherein the curing temperature of the second adhesive is lower than that of the first adhesive;
cutting the cured and molded block into sheets along a stacking direction;
carrying out hot-press molding on the sheet;
carrying out surface polishing treatment on the sheet subjected to hot press molding;
and trimming the edge of the polished sheet, and removing the second adhesive coated on the edge to obtain the graphene composite heat-conducting gasket.
Optionally, in the step of performing laser drilling on the graphene heat-conducting foam film, a plurality of through holes are formed in the graphene heat-conducting foam film, the diameter of each through hole is 30-300 μm and is lower than 30 μm, so that the up-down through effect is poor, and the first adhesive impregnation effect is poor; if the thickness is more than 300 μm, the mechanical property of the graphene thermal conductive foam film is reduced due to large pores, and the graphene thermal conductive foam film is easy to crack, and preferably 50-200 μm.
Optionally, the average center spacing of the plurality of through holes is 100-600 μm, and if the average center spacing is lower than 100 μm, the through holes are too dense, and the graphene heat-conducting foam film is easy to crack; above 600 μm, the thickness is too loose to affect the penetration effect, preferably 200-500 μm.
Optionally, in the step of impregnating the perforated graphene thermal conductive foam film with the first adhesive, the first adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin, or organic silica gel.
Optionally, the first adhesive is a silicone, preferably a liquid silicone.
Optionally, the liquid silicone gum is one or more of polydimethylsiloxane, α, ω -dihydroxypolydimethylsiloxane, polydiphenylsiloxane, α, ω -dihydroxypolymethyl (3,3, 3-trifluoropropyl) siloxane, cyanosiloxysilane, or α, ω -diethylpolydimethylsiloxane.
Optionally, the viscosity of the first adhesive is 50-800mPa · s, the viscosity is lower than 50mPa · s, and the mechanical property of the colloid is relatively poor, so that the mechanical property of the whole gasket is affected; above 800 mPas, the viscosity is too high, the fluidity is poor, and the impregnation is not easy, so that a large amount of air exists inside the foam film, which affects the overall mechanical properties, and preferably 100-600 mPas.
Optionally, first gluing agent adopts the organic silica gel of heating curing mode, opens to place (in 3 months) can not solidify under normal atmospheric temperature, only can slowly solidify under the heating environment, and the higher solidification of temperature is faster, ensures that first gluing agent is in the liquid state when sample cutting technology, and when through hot pressing technology, first gluing agent can play the effect of impregnating again to utilize hot pressing temperature to solidify, thereby guarantee that the impregnating adhesive has better impregnation effect.
Optionally, in the step of stacking the impregnated graphene heat-conducting foam film layers into a mold, applying pressure to attach the films to each other, the graphene heat-conducting foam film is cut into sheets with the same size, and the sheets are stacked layer by layer and placed into the mold.
Optionally, in the step of uniformly coating the second adhesive on the periphery of the compressed graphene heat-conducting foam film, the second adhesive is mainly distributed on the surface of the foam film block to play a role in shaping and fixing, so that the foam film block is prevented from being scattered in cutting, hot-pressing and polishing processes, and cutting formability is ensured, and the second adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel, preferably epoxy resin.
Optionally, the epoxy resin is cured by heating, that is, when the graphene heat conduction foam film is stacked, shaped and cured, the second adhesive is cured by heating or at normal temperature, taking preparation efficiency into consideration, the heat-curable epoxy resin can be selected, preferably, the epoxy resin is cured by heating at 50 ℃, and the curing temperature of the second adhesive is too high, so that curing of the internal impregnating adhesive is easily caused, and the secondary impregnating effect of the second adhesive is influenced during a later-stage hot-pressing process.
Optionally, the viscosity of the second adhesive is 10000-; above 200000 mPas, the viscosity is too high, the bubble-discharging ability is poor, and the workability is poor, preferably 30000-150000 mPas.
Optionally, in the step of cutting the solidified and shaped block into sheets along the stacking direction, the cutting mode is linear cutting, laser cutting, ultrasonic cutting, blade cutting or freezing cutting, and preferably, the thickness of the cut sheet is 0.2-1 mm.
Optionally, the step of hot press forming the sheet includes: and limiting the sheet by using the die and heating and curing the sheet.
Alternatively, the applied pressure is 0.1-1.0MPa, preferably 0.3-0.8 MPa.
Optionally, the curing temperature is 100-160 ℃, preferably 120-150 ℃.
Optionally, the step of performing surface polishing treatment on the sheet after the hot press forming includes: the polishing mode adopts contact polishing or non-contact polishing equipment.
Optionally, in the step of performing laser drilling on the graphene thermal conductive foam film, the thermal conductivity of the graphene thermal conductive foam film is not less than 100W/(m · K), and if the thermal conductivity of the graphene thermal conductive foam film is less than 100, the thermal conductivity of the final gasket is too low, and is preferably not less than 150W/(m · K).
Optionally, the thickness of the graphene heat-conducting foam film is 100-300 μm, and the thickness is lower than 100 μm, so that the strength is low, and the preparation is not facilitated; the thickness is higher than 300 μm, the impregnating adhesive is not easy to enter the interior, the interior combination is poor, and the delamination is easy, and preferably, the thickness of the graphene heat-conducting foam film is 150-250 μm.
Optionally, the graphene thermal conductive foam film has a density of 0.05-0.20g/cm3Density lower than 0.05g/cm3The graphene heat-conducting foam film is easy to crack; the density is higher than 0.20g/cm3The pores are smaller, the impregnated adhesive cannot enter the interior of the graphene foam, and the thickness of the graphene heat-conducting foam film is preferably 0.08-0.15g/cm3。
Optionally, the graphene heat-conducting foam film is composed of graphene hole walls and pores, the graphene is of a layered structure, certain pores exist between layers, the graphene random structure is an isotropic material, the final heat-conducting gasket has a poor directional heat-conducting effect, and the average pore diameter of pores inside the graphene heat-conducting foam film is 10-50 μm, preferably 15-30 μm.
According to another aspect of the present invention, there is provided a graphene composite thermal conductive gasket, including a multi-layer graphene thermal conductive foam film and an adhesive, the multi-layer graphene thermal conductive foam film being arranged along a thickness direction, the multi-layer graphene thermal conductive foam film having a plurality of through holes, the graphene thermal conductive foam film having a ratio of 10 wt.% to 50 wt.%, and a ratio of less than 10 wt.% resulting in poor thermal conductivity due to too little graphene; above 50 wt.%, the thermally conductive pad is easily delaminated due to too little adhesive, and the mechanical properties are poor.
Optionally, the graphene thermal conductive foam film accounts for 15 wt.% to 35 wt.%, and when the graphene thermal conductive foam film accounts for 15 wt.% to 35 wt.%, the content of the adhesive in the system is relatively high, and the adhesive plays a role in bonding and providing a network structure in the system, so that the mechanical properties of the gasket, including the strength and the compression resilience, are favorably improved.
According to the preparation method of the graphene composite heat conduction gasket, the heat conduction gasket is prepared by compounding the low-density graphene heat conduction foam film and the adhesive, and the obtained graphene composite heat conduction gasket has the characteristics of high strength, high resilience, high heat conduction in the thickness direction and low heat resistance.
According to the invention, the graphene heat-conducting foam membrane after laser drilling is soaked by a first adhesive, then the graphene heat-conducting foam membrane is stacked layer by using a mould and is pressed and attached, then a second adhesive is coated on the periphery of a graphene heat-conducting foam membrane sample block to wrap the graphene heat-conducting foam membrane sample block, so that the graphene heat-conducting foam membrane sample block plays a role in bonding and fixing, the graphene heat-conducting foam membrane sample block is cut into sheets along the stacking direction after the second adhesive is completely cured, finally the sheets are subjected to hot-pressing treatment and surface polishing to obtain the heat-conducting gasket, and graphene sheet layers in the heat-conducting gasket are arranged along the thickness direction, so that the heat-conducting gasket has a good heat conductivity coefficient.
The first adhesive is an adhesive used in an impregnation process, is called as an impregnation adhesive for short, is low in viscosity, good in fluidity and low in hardness after being cured, has good adhesive property on a graphene material, and has good mechanical property; the second adhesive is an adhesive coated around the massive foam film, is called as a bonding adhesive for short, is high in viscosity, general in fluidity, high in hardness and high in strength after being cured, has good bonding performance on graphene materials, and can play a role in fixing the structure.
The graphene composite heat-conducting gasket can control the thickness of the gasket according to a cutting process, and can meet application requirements of various thicknesses; graphene sheet layers in the graphene heat-conducting foam film are vertically arranged along the thickness direction, so that the heat-conducting gasket has a high heat-conducting coefficient in the thickness direction; after the hot pressing process, adhesives are distributed in the foam films and between layers, so that the heat-conducting gasket has excellent mechanical property, good resilience, high strength and difficult layering; after the surface polishing process, the roughness of the surface of the gasket is reduced, the surface state is improved, and the bonding degree of the surface of the gasket and the substrate is good, so that lower thermal resistance is obtained, and the overall heat conducting performance is improved.
Drawings
Fig. 1 is a schematic view of a flow chart of a method for preparing a graphene composite thermal conductive gasket according to the present invention;
fig. 2 is an SEM image of the graphene thermal conductive foam film according to the present invention;
fig. 3 is a photograph of the graphene composite thermal pad according to the present invention;
fig. 4 is an SEM image of the graphene composite thermal pad according to the present invention;
fig. 5 is a cross-sectional view of the graphene composite thermal pad according to the present invention.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
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 may recognize applications of other processes and/or uses of other materials.
Fig. 1 is a schematic view of a flowchart of a method for manufacturing a graphene composite thermal pad according to the present invention, and as shown in fig. 1, the method for manufacturing a graphene composite thermal pad includes:
step S1, performing laser drilling on the graphene thermal conductive foam film (shown in fig. 2);
step S2, impregnating the perforated graphene heat-conducting foam film through the first adhesive, wherein the graphene heat-conducting foam film is not calendered, has a rough surface and a low density, has large pores inside and is beneficial to impregnation of the first adhesive;
step S3, stacking the impregnated graphene heat-conducting foam film layers into a mold, and applying pressure to joint adjacent graphene heat-conducting foam films;
step S4, uniformly coating a second adhesive on the periphery of the pressed graphene heat conduction foam film to completely coat the multilayer graphene heat conduction foam film into a block, wherein the curing temperature of the second adhesive is lower than that of the first adhesive;
step S5, cutting the cured and molded block into sheets along the stacking direction;
step S6, performing hot press molding on the sheet;
step S7, carrying out surface polishing treatment on the sheet after hot press molding;
and step S8, trimming the edges of the polished sheet, and removing the second adhesive coated on the edges to obtain the graphene composite heat-conducting gasket.
In one embodiment, in step S1, forming a plurality of through holes in the graphene thermal conductive foam film, wherein the diameter of the through holes is 30-300 μm, preferably 50-200 μm; the center average distance of the plurality of through holes is 100-. Punch from top to bottom graphite alkene heat conduction foam membrane through laser beam to can form a large amount of through-holes, make first gluing agent permeate into the inside interlayer of foam membrane from the hole more easily, thereby improve the inside cohesion of foam membrane, be favorable to improving the mechanical properties of gasket, the through-hole number is decided by aperture and hole interval, the aperture is the diameter of through-hole, the hole interval is close two through-hole edges to the interval at edge, a plurality of through-holes belong to array distribution.
Preferably, the thermal conductivity of the graphene thermal conductive foam film is not less than 100W/(m · K), and more preferably not less than 150W/(m · K).
Preferably, the thickness of the graphene thermal conductive foam film is 100-300 μm, and further preferably, the thickness of the graphene thermal conductive foam film is 150-250 μm.
Preferably, the density of the graphene heat-conducting foam film is 0.05-0.20g/cm3Further preferably, the thickness of the graphene heat-conducting foam film is 0.08-0.15g/cm3。
As shown in fig. 2, the graphene thermal conductive foam film is a low-density graphene thermal conductive foam film, the internal monolithic layer is well oriented, and the pores between sheets are large, preferably, the average pore diameter of the pores inside the graphene thermal conductive foam film is 10 to 50 μm, and further preferably, the average pore diameter is 15 to 30 μm.
In one embodiment, in step S2, the first adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin, or organic silica gel; preferably, the first adhesive is organic silica gel, and further, preferably liquid organic silica gel; preferably, the liquid silicone gum is one or more of polydimethylsiloxane, alpha, omega-dihydroxypolydimethylsiloxane, polydiphenylsiloxane, alpha, omega-dihydroxypolymethyl (3,3, 3-trifluoropropyl) siloxane, cyanosiloxysilane, or alpha, omega-diethylpolydimethylsiloxane; preferably, the viscosity of the first adhesive is 50 to 800 mPas, and more preferably 100 to 600 mPas.
Preferably, the first adhesive is organic silica gel in a heating and curing mode.
In one embodiment, in step S3, the graphene thermal conductive foam film is cut into sheets with uniform size, and the sheets are stacked layer by layer and placed in a mold.
In one embodiment, in step S4, the second adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel, preferably epoxy resin, further preferably, the epoxy resin is cured by heating, and further preferably, the epoxy resin is cured by heating at 50 ℃; preferably, the viscosity of the second adhesive is 10000-.
In one embodiment, in step S5, the cutting method is not particularly limited, and linear cutting, laser cutting, ultrasonic cutting, blade cutting, freezing cutting, etc. may be adopted; the thickness of the slices is not particularly required, and the slices are cut according to specific requirements, and are generally the thickness which is conventionally used, such as 0.2-1 mm.
In one embodiment, step S6 includes: utilize the mould to carry out spacing and heat curing to the sheet, hot briquetting, utilize the mould to control gasket thickness, and heat the pressurization solidification shaping to it, reach hot pressing technology effect, for example, the gasket of 0.3 mm's thickness is required, then select the cutting sheet of 0.4mm thickness (the thickness after the pre-compaction is 75% before the pre-compaction), place on the mould, adjust spacing size to 0.3mm, select suitable pressure and temperature to carry out hot briquetting technology to it, because spacing influence like this gasket thickness after the hot pressing is 0.3 mm.
Preferably, the applied pressure is 0.1-1.0MPa, preferably 0.3-0.8MPa, and the pressure is lower than 0.1MPa, so that the effect of leveling the surface of the gasket cannot be achieved due to too low pressure; if the pressure is higher than 1.0MPa, the graphene sheet layers in the vertical direction inside the gasket are easily seriously extruded and deformed due to overlarge pressure, so that the heat-conducting property is influenced, and the gasket is also extruded and cracked due to the overlarge pressure; the curing temperature is selected to be 100-160 ℃, preferably 120-150 ℃, if the curing temperature is lower than 100 ℃, the curing of the impregnating glue is easy to slow, the whole curing effect is influenced, if the temperature is higher than 160 ℃, the curing reaction is too violent due to too high temperature, the product is easy to crack, and if the temperature is higher than 200 ℃, the product is easy to age and damage, and the forming is poor.
In one embodiment, in step S7, the polishing process and the polishing equipment are not particularly limited, and contact polishing and non-contact polishing equipment can be used, so as to reduce the surface roughness, improve the adhesion between the gasket and the substrate when in use, and facilitate reducing the thermal interface resistance without damaging the integrity of the gasket. The polishing treatment reduces the surface roughness of the material, because the surface roughness has a greater influence on the thermal resistance, the greater the surface roughness, the higher the thermal resistance and the poorer the heat dissipation effect for the same gasket, and preferably the roughness Rz of the gasket is less than 5 um.
The method adopts the low-density graphene heat-conducting foam film and the adhesive to prepare the heat-conducting gasket in a compounding manner; the gasket is prepared by adopting the low-density foam film, and the impregnation glue is more favorably permeated into the foam film by matching with the laser drilling process, so that the overall mechanical properties including compression resilience and mechanical strength are improved; the second adhesive is coated around the stacked, pressurized and attached foam membrane blocks to play a role in shaping and fixing, so that the frame scattering phenomenon in the cutting process is prevented; because the first adhesive adopts a 50 ℃ low-temperature curing process and the curing temperature required by the first adhesive is higher, the first adhesive is in an uncured state when the first adhesive is cured, and is in a semi-flowing state only by means of the early low-temperature curing process; after the graphene heat conduction foam film is subjected to slicing, a hot pressing process is used, so that the first adhesive in a semi-flowing state permeates the interior of the graphene heat conduction foam film for the second time, the existence of a large amount of adhesives inside and outside the graphene heat conduction foam film is ensured, air holes (air) in the graphene heat conduction foam film are reduced, the first adhesive forms a continuous phase as far as possible, the graphene heat conduction foam film is integrally coated, and the integral mechanical property is improved; graphene sheet layers in the graphene heat-conducting foam film are vertically arranged along the thickness direction, so that the heat-conducting gasket has a high heat-conducting coefficient in the thickness direction; during the hot pressing process, part of the second adhesive is extruded and distributed on the surface of the gasket, and an extremely thin adhesive layer is formed after curing, so that the interface thermal resistance of the gasket is increased, and the overall heat dissipation performance is influenced.
Fig. 3 is a photograph of the graphene composite heat conduction gasket of the present invention, fig. 4 is an SEM image of the graphene composite heat conduction gasket of the present invention, and fig. 5 is a cross-sectional view of the graphene composite heat conduction gasket of the present invention, as shown in fig. 3 to 5, the graphene composite heat conduction gasket includes a multi-layer graphene heat conduction foam film and an adhesive, the multi-layer graphene heat conduction foam film has a plurality of through holes, and the graphene heat conduction foam film accounts for 10 wt.% to 50 wt.%.
Preferably, the graphene thermal conductive foam film accounts for 15-35 wt.%.
As shown in fig. 4, the graphene composite heat-conducting pad of the present invention has a smooth surface after polishing and grinding, and is favorable for bonding with a heat dissipation device, and reducing interface thermal resistance.
As shown in fig. 5, the graphene sheet layer of the graphene composite heat conduction gasket of the present invention has a cut slope along the thickness direction, so as to improve the compression resilience, and has a high heat conduction performance in the thickness direction.
The thermal resistance and the compression amount of the graphene composite heat-conducting gasket (with the thickness of 0.2 mm) under 10-100psi are shown in the following table 1:
TABLE 1
Pressure (Psi) 10 20 40 60 80 100
Thermal resistance (K.cm)2/W) 0.108 0.086 0.067 0.059 0.056 0.053
Amount of compression (%) 10.4 20.1 36.7 49.2 60.7 70.2
Under the conventional use environment (40psi), the thermal resistance of the graphene composite heat conduction gasket is low and is only 0.067K-cm2The compression amount is relatively good, and reaches 36.7%, the compression amount is the amount of the gasket which can be compressed under a certain pressure, generally, the better the compression performance of the gasket is, the better the bonding with the base material is, and the lower the thermal resistance is. The compression amount of the graphene composite heat-conducting gasket can reach 70%, so that the joint degree between the gasket and a device is facilitated, and the heat dissipation performance of the device is improved.
In order to embody the contrast effect, in the following specific embodiment, the thermal conductivity coefficient of the thermal conductive gasket under the condition of 40psi is tested through ASTM D5470, the thermal resistance is applied, the compression resilience performance of the thermal conductive gasket under the condition of 50% strain is tested through ASTM D575, compression resilience means that the gasket can cause a large compression amount after being stressed, deformation occurs, when the force is removed, the gasket can rebound, the rebound degree is the compression resilience performance, because the device has the performances of expansion with heat and contraction with cold and shaking in the using process, the gap between the gasket and the device can be changed, in order to adapt to the phenomenon, the gasket is required to have good compression resilience performance.
Example 1:
in this embodiment, the graphene thermal conductive foam film accounts for 12 wt.%, and the adhesive accounts for 88 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 205W/(m.K);
the thickness of the graphene heat-conducting foam film is 300 mu m, and the density is 0.19g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 50 micrometers;
the hole diameter of the punched graphene heat-conducting foam film is 300um, and the hole distance is 500 um;
the first adhesive is heating curing organic silica gel with the viscosity of 800mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 200000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 1.0MPa, and the curing temperature is 100 ℃;
polishing and grinding the gasket by adopting contact type polishing equipment, and selecting a 500-mesh polishing disc;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 45W/(m.K), the roughness Rz of 4.559um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000121
Figure BDA0003371830000000131
example 2:
in the embodiment, the ratio of the graphene heat-conducting foam film is 20 wt.%, and the ratio of the adhesive is 80 wt.%; the thermal conductivity coefficient of the graphene thermal conductive foam film is 225W/(m.K);
the thickness of the graphene heat-conducting foam film is 150 mu m, and the density is 0.11g/cm3；
The average pore diameter of internal pores of the graphene heat-conducting foam film is 30 mu m;
the aperture of the punched hole of the graphene heat-conducting foam film is 100um, and the hole spacing is 300 um;
the first adhesive is heating curing organic silica gel with the viscosity of 500mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 100000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.5MPa, and the curing temperature is 150 ℃;
polishing and grinding the gasket by adopting contact type polishing equipment, and selecting a 500-mesh polishing disc;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 73W/(m.K), the roughness Rz of 4.109um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000132
example 3:
in this embodiment, the graphene thermal conductive foam film accounts for 35 wt.%, and the adhesive accounts for 65 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 145W/(m.K);
the thickness of the graphene heat-conducting foam film is 200 mu m, and the density is 0.08g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 20 micrometers;
the hole diameter of the punched graphene heat-conducting foam film is 200um, and the hole interval is 350 um;
the first adhesive is heating curing organic silica gel with the viscosity of 200mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 50000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, pressure 0.3MPa, curing temperature 120 ℃;
polishing and grinding the gasket by adopting contact type polishing equipment, and selecting a 500-mesh polishing disc;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 52W/(m.K), the roughness Rz of 3.585um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000141
example 4:
in the embodiment, the graphene heat-conducting foam film accounts for 50 wt.%, and the adhesive accounts for 50 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 155W/(m.K);
the thickness of the graphene heat-conducting foam film is 180 mu m, and the density is 0.13g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 25 mu m;
the hole diameter of the punched graphene heat-conducting foam film is 80 microns, and the hole spacing is 200 microns;
the first adhesive is heating curing organic silica gel with the viscosity of 350mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 30000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.6MPa, and the curing temperature is 140 ℃;
polishing and grinding the gasket by adopting contact type polishing equipment, and selecting a 500-mesh polishing disc;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 85W/(m.K), the roughness Rz of 3.211um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000151
example 5:
in the embodiment, the graphene heat-conducting foam film accounts for 25 wt.%, and the adhesive accounts for 75 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 165W/(m.K);
the thickness of the graphene heat-conducting foam film is 250 mu m, and the density is 0.15g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 40 mu m;
the aperture of the punched hole of the graphene heat-conducting foam film is 150um, and the hole spacing is 400 um;
the first adhesive glue is heating curing organic silica gel with the viscosity of 600mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 150000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.8MPa, and the curing temperature is 125 ℃;
what polishing is used, what is the surface roughness and other parameters after polishing?
Polishing and grinding the gasket by adopting contact type polishing equipment, and selecting a 500-mesh polishing disc;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 50W/(m.K), the roughness Rz of 3.850um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000152
comparative example 1:
in the comparative example, the graphene heat-conducting foam film accounts for 40 wt.%, and the adhesive accounts for 60 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 165W/(m.K);
the thickness of the graphene heat-conducting foam film is 250 mu m, and the density is 0.15g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 40 mu m;
the aperture of the punched hole of the graphene heat-conducting foam film is 150um, and the hole spacing is 400 um;
the impregnating adhesive is heating curing organic silica gel with the viscosity of 600mPa & s;
the adhesive is heating curing type epoxy resin, the viscosity is 150000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.8MPa, and the curing temperature is 250 ℃;
in the hot pressing process in the comparative example, the temperature is too high, so that the gasket is cracked and layered and cannot be molded.
Comparative example 2:
in the comparative example, the graphene heat-conducting foam film accounts for 50 wt.%, and the adhesive accounts for 50 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 155W/(m.K);
the thickness of the graphene heat-conducting foam film is 180 mu m, and the density is 0.13g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 25 mu m;
the hole diameter of the punched graphene heat-conducting foam film is 80 microns, and the hole spacing is 200 microns;
the impregnating adhesive is heating curing organic silica gel with the viscosity of 3000mPa & s;
the adhesive is heating curing type epoxy resin, the viscosity is 30000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.6MPa, and the curing temperature is 140 ℃;
through tests, the thermal conductivity coefficient of the sample is 70W/(m.K), and the application thermal resistance and the compression resilience of the samples with different thicknesses are as follows:
Figure BDA0003371830000000161
because the dipping glue in the comparative example has too high viscosity, the dipping effect in the foam film is poor, and a large number of air holes exist in the foam film, the heat-conducting property of the gasket is finally reduced, and the application thermal resistance is increased; because the foam film has poor impregnation effect, the impact on the compression resilience performance of the gasket is large, and the compression resilience is seriously reduced.
Comparative example 3:
in the comparative example, the graphene heat-conducting foam film accounts for 20 wt.%, and the adhesive accounts for 80 wt.%;
the thermal conductivity coefficient of the graphene thermal conductive foam film is 255W/(m.K);
the thickness of the graphene heat-conducting foam film is 150 mu m, and the density is 0.41g/cm3；
The average pore diameter of the internal pores of the graphene heat-conducting foam film is 5 mu m;
the aperture of the punched hole of the graphene heat-conducting foam film is 100um, and the hole spacing is 300 um;
the impregnating adhesive is heating curing organic silica gel with the viscosity of 500mPa & s;
the adhesive is heating curing type epoxy resin, the viscosity is 100000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 0.5MPa, and the curing temperature is 150 ℃;
through tests, the thermal conductivity coefficient of the sample is 85W/(m.K), and the application thermal resistance and the compression resilience of the samples with different thicknesses are as follows:
Figure BDA0003371830000000171
the graphene heat-conducting foam film adopted in the comparative example has higher density, so that the internal pores are smaller, the impregnation effect of the impregnating compound is poorer, and a large number of air holes exist in the impregnating compound; but the foam film is densified, so that the overall heat-conducting property and the application thermal resistance are not greatly changed; but has a large influence on the compression resilience performance of the gasket, and the compression resilience is seriously reduced.
Comparative example 4:
in the comparative example, the graphene heat-conducting foam film accounts for 95 wt%, and the adhesive accounts for 5 wt%;
the thermal conductivity coefficient of the graphene thermal conductive foam film is 400W/(m.K);
the thickness of the graphene heat-conducting foam film is 1000 mu m, and the density is 0.88g/cm3；
The average pore diameter of internal pores of the graphene heat-conducting foam film is 100 microns;
the aperture of the punched hole of the graphene heat-conducting foam film is 100um, and the hole spacing is 300 um;
the impregnating adhesive is heating curing organic silica gel with the viscosity of 100mPa & s;
the adhesive is heating curing type epoxy resin, the viscosity is 300000mPa & s, and the curing temperature is 80 ℃;
hot pressing process, wherein the pressure is 2.0MPa, and the curing temperature is 150 ℃;
through tests, the thermal conductivity coefficient of the sample is 295W/(m.K), and the application thermal resistance and the compression resilience performance of the samples with different thicknesses are as follows:
Figure BDA0003371830000000181
although the thermal resistance of the gasket was only 0.07K-cm lower under the 40psi pressure test2The compression amount is only 10%, and the compression resilience performance is 40.2%, so that in the actual use process of the gasket, due to the unevenness of the surface of the device, the bonding degree between the gasket and the device is extremely poor, the actual use effect is not good, and the expected heat dissipation effect cannot be achieved.
Because the graphene heat-conducting foam film adopted in the comparative example has a large proportion, the internal adhesive is less, the internal bonding force is weak, the overall strength of the gasket is relatively poor, and the long-term service life of the gasket is influenced.
Comparative example 5:
in this embodiment, the graphene thermal conductive foam film accounts for 12 wt.%, and the adhesive accounts for 88 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 205W/(m.K);
the thickness of the graphene heat-conducting foam film is 300 mu m, and the density is 0.19g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 50 micrometers;
the graphene heat-conducting foam film is not perforated;
the first adhesive is heating curing organic silica gel with the viscosity of 800mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 200000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, wherein the pressure is 1.0MPa, and the curing temperature is 100 ℃;
because the comparative example does not adopt laser drilling, no impregnating compound enters the gasket, so that the overall mechanical property is poorer, and when the gasket is polished and polished, the gasket is cracked and scattered, namely, the mechanical property of the gasket cannot maintain the polishing and polishing process, and the experiment fails.
Comparative example 6:
in this embodiment, the graphene thermal conductive foam film accounts for 35 wt.%, and the adhesive accounts for 65 wt.%;
the thermal conductivity of the graphene thermal conductive foam film is 145W/(m.K);
the thickness of the graphene heat-conducting foam film is 200 mu m, and the density is 0.08g/cm3；
The average pore diameter of pores in the graphene heat-conducting foam film is 20 micrometers;
the hole diameter of the punched graphene heat-conducting foam film is 200um, and the hole interval is 350 um;
the first adhesive is heating curing organic silica gel with the viscosity of 200mPa & s;
the second adhesive is heating curing type epoxy resin, the viscosity is 50000mPa & s, and the curing temperature is 50 ℃;
hot pressing process, pressure 0.3MPa, curing temperature 120 ℃;
polishing and grinding are not carried out on the gasket;
through tests, the obtained graphene composite heat conduction gasket has the heat conductivity coefficient of 52W/(m.K), the roughness Rz of 22.125um, and the application thermal resistance and the compression resilience of the graphene composite heat conduction gasket with different thicknesses are as follows:
Figure BDA0003371830000000191
tests show that the unpolished and polished gasket has poor surface state and high roughness value (Rz is more than 20um), so that the interface thermal resistance of the gasket is high, the application thermal resistance is high, and the heat dissipation effect is poor.
The heat conductivity coefficient is taken as reference, the current heat conductivity coefficient is more than or equal to 30W/(m.K), namely the high heat conductivity gasket can be called as a high heat conductivity gasket, which is only a reference meaning, and the current specific requirements for application of thermal resistance and compression rebound are that the gasket is 0.2mm thick, the thermal resistance (pressure 40psi) is less than or equal to 0.12 (K.cm)2/W), compression resilience performance is more than or equal to 80 percent. The gasket is mainly applied to the fields of 5G communication, high-power chips and electric automobiles. If the thermal resistance is too high (more than 0.12), the heat dissipation effect is poor, and the heat dissipation of the whole heat dissipation system is affected, mainly the shadowThe heat dissipation effect of the chip is affected, so that the service life of the chip is reduced, and the use effect is influenced; because cooling system is in cold and hot exchange's state for a long time, the gap that leads to the gasket to fill also can be because cold and hot exchange changes, grow or the phenomenon that diminishes can appear in the gap, consequently, it changes along with the change in gap to need the gasket, just so need the gasket have good compression resilience performance, can adapt to the change of environment, and when the compression resilience of gasket < 80%, the change in unable adaptation environment gap, lead to the gasket to reduce with the laminating degree of upper and lower substrate, the heat can't conduct out through the gasket like this, influence holistic radiating effect, influence cooling system's life-span even.
The preparation method of the graphene composite heat-conducting gasket adopts a process of hot pressing after dipping and slicing, improves the dosage of the adhesive while ensuring the content of graphene in the gasket, reduces cavities (air) in the foam film, enables the adhesive to form a continuous phase as much as possible, integrally coats the foam film, and improves the mechanical properties of the whole body, including the mechanical strength and the compression resilience of the gasket.
The polishing process for the surface of the graphene composite heat-conducting gasket is beneficial to reducing the surface roughness, and is beneficial to improving the joint degree of the surface of the gasket and a substrate, reducing the interface thermal resistance and improving the overall heat-conducting performance in the actual use process.
As described above, according to the embodiments of the present invention, various changes and modifications can be made by those skilled in the art without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.

Claims (10)

1. A preparation method of a graphene composite heat conduction gasket is characterized by comprising the following steps:
carrying out laser drilling on the graphene heat-conducting foam film;
impregnating the perforated graphene heat-conducting foam film with a first adhesive;
stacking the impregnated graphene heat-conducting foam film layers into a mold, and applying pressure to joint adjacent graphene heat-conducting foam films;
uniformly coating a second adhesive on the periphery of the pressed graphene heat conduction foam film to completely coat the multilayer graphene heat conduction foam film into a block, wherein the curing temperature of the second adhesive is lower than that of the first adhesive;
cutting the cured and molded block into sheets along a stacking direction;
carrying out hot-press molding on the sheet;
carrying out surface polishing treatment on the sheet subjected to hot press molding;
and trimming the edge of the polished sheet, and removing the second adhesive coated on the edge to obtain the graphene composite heat-conducting gasket.
2. The preparation method according to claim 1, wherein in the step of performing laser drilling on the graphene thermal conductive foam film, a plurality of through holes are formed in the graphene thermal conductive foam film, and the diameter of the through holes is 30-300 μm, preferably 50-200 μm; the center average distance of the plurality of through holes is 100-.
3. The preparation method according to claim 1, wherein in the step of impregnating the perforated graphene thermal conductive foam film with the first adhesive, the first adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel; preferably, the first adhesive is organic silica gel, more preferably liquid organic silica gel, and still more preferably organic silica gel adopting a heating curing mode; preferably, the liquid silicone gum is one or more of polydimethylsiloxane, alpha, omega-dihydroxypolydimethylsiloxane, polydiphenylsiloxane, alpha, omega-dihydroxypolymethyl (3,3, 3-trifluoropropyl) siloxane, cyanosiloxysilane, or alpha, omega-diethylpolydimethylsiloxane; preferably, the viscosity of the first adhesive is 50 to 800 mPas, and more preferably 100 to 600 mPas.
4. The preparation method according to claim 1, wherein in the step of stacking the impregnated graphene heat-conducting foam film layers into a mold, applying pressure to attach the films to each other, the graphene heat-conducting foam film is cut into sheets with consistent sizes, and the sheets are stacked into the mold layer by layer.
5. The preparation method according to claim 1, wherein in the step of uniformly coating the second adhesive around the pressed graphene thermal conductive foam film, the second adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel, preferably epoxy resin, further preferably the epoxy resin is cured by heating, and further preferably the epoxy resin is cured by heating at 50 ℃; preferably, the viscosity of the second adhesive is 10000-.
6. The method according to claim 1, wherein in the step of cutting the solidified and shaped block into sheets along the stacking direction, the cutting is performed by linear cutting, laser cutting, ultrasonic cutting, blade cutting or freezing cutting, and preferably, the thickness of the cut sheet is 0.2-1 mm.
7. The method according to claim 1, wherein the step of hot press forming the sheet includes: limiting the sheet by using a die, and heating and curing the sheet, wherein the applied pressure is preferably 0.1-1.0MPa, and more preferably 0.3-0.8 MPa; preferably, the curing temperature is 100 to 160 ℃, and more preferably 120 to 150 ℃.
8. The production method according to claim 1, wherein the step of subjecting the hot press-molded sheet to surface polishing treatment comprises: the polishing mode adopts contact polishing or non-contact polishing equipment.
9. The preparation method according to claim 1, wherein in the step of laser drilling the graphene thermal conductive foam film, the thermal conductivity of the graphene thermal conductive foam film is not less than 100W/(m-K), preferably not less than 150W/(m-K); or/and
the thickness of the graphene heat-conducting foam film is 100-300 μm, preferably, the thickness of the graphene heat-conducting foam film is 150-250 μm; or/and
the density of the graphene heat-conducting foam film is 0.05-0.20g/cm3Preferably, the thickness of the graphene heat-conducting foam film is 0.08-0.15g/cm3(ii) a Or/and
the average pore diameter of pores inside the graphene heat-conducting foam membrane is 10-50 μm, and preferably, the average pore diameter is 15-30 μm.
10. The graphene composite heat conduction gasket is characterized by comprising a multi-layer graphene heat conduction foam film and an adhesive, wherein the multi-layer graphene heat conduction foam film is arranged along the thickness direction, a plurality of through holes are formed in the multi-layer graphene heat conduction foam film, the graphene heat conduction foam film accounts for 10-50 wt.%, and preferably the graphene heat conduction foam film accounts for 15-35 wt.%.
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CN115637425A (en) * 2022-10-17 2023-01-24 北京科技大学 Diamond hollow pipeline foam reinforced framework aluminum-based composite material and preparation method thereof
CN115637425B (en) * 2022-10-17 2024-06-07 北京科技大学 Diamond hollow pipeline foam reinforced skeleton aluminum-based composite material and preparation method thereof

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