CN113510979B - Graphene composite heat conduction gasket and preparation method thereof - Google Patents

Graphene composite heat conduction gasket and preparation method thereof Download PDF

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Publication number
CN113510979B
CN113510979B CN202110801374.3A CN202110801374A CN113510979B CN 113510979 B CN113510979 B CN 113510979B CN 202110801374 A CN202110801374 A CN 202110801374A CN 113510979 B CN113510979 B CN 113510979B
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graphene
foam film
adhesive
heat
graphene foam
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CN113510979A (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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • B32B38/0036—Heat treatment
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • B32B2038/0076—Curing, vulcanising, cross-linking
    • 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
    • B32B2307/70—Other properties
    • B32B2307/72—Density

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  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Thermal Sciences (AREA)
  • Sealing Material Composition (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)

Abstract

The invention provides a graphene composite heat conducting gasket which comprises a multilayer graphene foam film and an adhesive, wherein the multilayer graphene foam film is arranged along the thickness direction in a sheet mode, and the graphene foam film accounts for 50-95 wt.%. The invention also provides a preparation method, which comprises the following steps: stacking the graphene foam film layers, putting the graphene foam film layers into a mold, and applying pressure to enable the films to be tightly attached; uniformly coating the adhesive on the periphery of the pressed graphene heat-conducting foam film to completely coat the multilayer graphene heat-conducting foam film into a block; curing and molding the block, and cutting the block into sheets along the stacking direction; dipping the cut sheet into the dipping glue, taking out, and carrying out hot press molding on the taken-out sheet; and trimming the edges of the formed sheet, and removing the adhesive bonding area at the edges to obtain the graphene composite heat-conducting gasket. The heat conducting gasket has low density, high heat conductivity in the thickness direction and low heat resistance.

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, after being stacked and bonded layer by layer through an adhesive, the graphene heat-conducting film is cut into heat-conducting gaskets, so that the graphene heat-conducting film is arranged along the thickness direction, for example, patent document WO2019235983a 1; secondly, the graphene thermal conductive film is changed from a plane direction to a longitudinal arrangement in a manner of folding, and then is coated with an adhesive, so that the graphene thermal conductive film becomes an integral structure, for example, patent document CN 110491845A.
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 (WO2019235983A1 and WO2019235986A 1); 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 graphene composite heat conduction gasket, which comprises a multilayer graphene foam film and an adhesive, wherein the multilayer graphene foam film is arranged along the thickness direction, and the graphene foam film accounts for 50-95 wt.%.
Optionally, the graphene foam film is 60-90 wt.%.
Optionally, the bottom cushion block is made of graphite felt, graphite block or carbon felt, and preferably, the thickness of the bottom cushion block is between 10mm and 100 mm.
Optionally, the thermal conductivity of the graphene foam film is greater than or equal to 50W/(m · K), preferably greater than or equal to 100W/(m · K).
Optionally, the thickness of the graphene foam film is 50-1000 μm, and preferably, the thickness of the graphene foam film is 300-500 μm.
Optionally, theThe density of the graphene foam film is 0.10-0.90g/cm 3 Preferably, the thickness of the graphene foam film is 0.20-0.70g/cm 3 。
Optionally, the graphene foam film is composed of graphene pore walls and pores, the graphene is a layered structure, the pores exist between layers, and the average pore diameter of the pores inside the layered structure of the graphene is 10-100 μm, preferably, the average pore diameter is 15-50 μm.
Optionally, the adhesive comprises an adhesive glue and an impregnating glue, the adhesive glue is coated on the adhesive on the periphery of the graphene foam film, the impregnating glue is used for impregnating a sheet formed by cutting after the multilayer graphene foam film is adhered, the viscosity of the adhesive glue is higher than that of the impregnating glue, and the flowability of the impregnating glue is higher than that of the adhesive glue.
Optionally, the adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel, preferably, the adhesive is epoxy resin; the viscosity of the epoxy resin is 5000-300000 mPas, preferably 10000-250000 mPas.
Optionally, the impregnating adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel; preferably, the adhesive is organic silica gel; preferably, the impregnating glue is 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 impregnating adhesive has a viscosity of 50 to 1000 mPas, preferably 100-500 mPas.
According to another aspect of the present invention, a preparation method of a graphene composite thermal conductive gasket is provided, including:
stacking the graphene foam film layers, putting the graphene foam film layers into a mold, and applying pressure to enable the films to be tightly attached;
uniformly coating the adhesive on the periphery of the pressed graphene heat-conducting foam film to completely coat the multilayer graphene heat-conducting foam film into a block;
curing and molding the block, and cutting the block into sheets along the stacking direction;
dipping the cut sheet into the dipping glue, taking out, and carrying out hot press molding on the taken-out sheet;
and trimming the edges of the formed sheet, and removing the adhesive bonding area at the edges to obtain the graphene composite heat-conducting gasket.
Optionally, in the step of stacking the graphene thermal conductive foam film layers into a mold, applying pressure to make the films tightly fit with each other, the graphene 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 adhesive around the pressed graphene heat conduction foam film to completely coat the multi-layer graphene heat conduction foam film into a block, the adhesive is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel, preferably, the adhesive is epoxy resin; the viscosity of the epoxy resin is 5000-300000mPa & s, preferably 10000-250000mPa & s; the adhesive is cured by heating or at normal temperature, preferably, the adhesive is heat-curable epoxy resin and is cured by heating at 80 ℃.
Optionally, in the step of solidifying and forming the block to be cut into the sheet material 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 0.25-5 mm.
Optionally, in the step of dipping the cut sheet in an immersion glue, the immersion glue is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin or organic silica gel; preferably, the impregnating glue is organic silica gel; preferably, the impregnating glue is 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 impregnating adhesive has a viscosity of 50 to 1000 mPas, preferably 100-500 mPas.
Optionally, in the step of performing hot press molding on the taken out sheet, the hot press molding is performed, the thickness of the gasket is controlled by using a mold, and the taken out sheet is subjected to heating and pressurizing curing molding, wherein the applied pressure is 0.1-2.0MPa, and preferably 0.3-1.5 MPa; the curing temperature is 150 ℃ or lower, preferably 120 ℃ or lower.
The graphene heat-conducting gasket prepared by compounding the graphene foam film and the adhesive has the characteristics of low density, high heat conduction in the thickness direction, low heat resistance and the like.
The graphene composite heat-conducting gasket disclosed by the invention is low in density, the thickness of the gasket can be controlled according to a cutting process, and the application requirements of various thicknesses can be met; graphene sheet layers in the graphene 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 graphene composite heat-conducting gasket has excellent mechanical properties and is not easy to delaminate; in addition, after the hot pressing process, the softness of the gasket is improved, and the bonding degree between the surface of the gasket and the base material is good in the actual use process, so that lower thermal resistance is obtained, and the overall heat-conducting performance is improved.
According to the preparation method of the graphene composite heat conduction gasket, the graphene heat conduction foam films are stacked layer by using a mold, are pressed and attached, are coated on the periphery of the foam film sample block by using an adhesive, are wrapped and play a role in bonding and fixing, are cut into sheets along the lamination direction after the adhesive is completely cured, and are subjected to hot pressing treatment after being impregnated by the adhesive to obtain the heat conduction gasket, wherein the graphene sheets in the heat conduction gasket are arranged along the thickness direction, and the graphene foam films are not calendered, have rough surfaces and low density, have flat pores inside and are well combined with the adhesive.
The adhesive has two types, one type is an adhesive coated on the periphery of the massive foam film, and is called an adhesive for short, the adhesive is high in viscosity, general in fluidity, high in hardness and high in strength after being cured, has good adhesive property on a graphene material, and can play a role in fixing a structure; the second is an adhesive used in the dipping process, which is called dipping adhesive for short, and the dipping adhesive has the advantages of low viscosity, good fluidity, low hardness after curing, good adhesive property to the graphene material and good mechanical property.
Drawings
Fig. 1 is a photograph of a graphene composite thermal pad according to the present invention;
fig. 2 is an SEM image of the graphene composite thermal pad according to the present invention;
fig. 3 is a photo of a sheet cut along the stacking direction after the block is cured and formed in the method for manufacturing the graphene composite thermal conductive gasket 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 are used in the orientations and positional relationships indicated in the drawings, which are merely for convenience of description and simplicity of description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed 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" and "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, specific example components and arrangements are described below. Of course, they are merely examples and are not intended to limit the present invention. Moreover, the present invention may repeat reference numerals and/or reference letters in the various examples, which have been repeated for purposes of simplicity and clarity and do not in themselves 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.
In an embodiment, as shown in fig. 1 and 2, the present invention provides a graphene composite thermal pad, which is composed of a plurality of graphene foam films and an adhesive, the graphene foam films are arranged in a thickness direction, the ratio of the graphene foam films is 50wt.% to 95wt.%, preferably 60wt.% to 90wt.%, the ratio of the graphene foam films is less than 50wt.%, the thermal pad has poor thermal conductivity due to too little graphene, and the ratio of the graphene foam films is higher than 95wt.%, the thermal pad is easy to delaminate due to too little adhesive, and the mechanical properties are poor, as can be seen from a cross-sectional view of the graphene composite thermal pad in fig. 2, graphene sheet layers are arranged in the thickness direction, and the graphene composite thermal pad has high thermal conductivity in the thickness direction.
In one embodiment, the graphene foam film has a thermal conductivity of 50W/(m · K) or more, preferably 100W/(m · K) or more, and less than 50 results in too low a thermal conductivity of the final gasket.
In one embodiment, the thickness of the graphene foam film is 50-1000 μm, preferably 300-500 μm, and the thickness is less than 50 μm, so that the strength is low and the preparation is not facilitated; the thickness is higher than 1000 μm, so that the impregnating adhesive is not easy to enter the interior, the interior combination is poor, and the delamination is easy.
In one embodiment, the graphene foam film has a density of 0.10-0.90g/cm 3 Preferably 0.20 to 0.70g/cm 3 Density lower than 0.10g/cm 3 The graphene foam film is easy to crack; density higher than 0.90g/cm 3 And the pores are less, and the impregnating adhesive cannot enter the interior of the graphene foam.
In one embodiment, the graphene foam film is composed of graphene hole walls and graphene pores, the graphene is in a layered structure, certain pores exist among layers, the graphene random stacking structure is an isotropic material, and the final heat conducting gasket is poor in directional heat conducting effect.
Preferably, the average pore diameter of pores inside the graphene laminated structure is 10-100 μm, preferably 15-50 μm, and if the average pore diameter is lower than 10 μm, the pores are too small to influence the entering of the adhesive; if the thickness is larger than 100 mu m, the graphene foam film is too fluffy and has poor mechanical property, and the preparation of the gasket is not facilitated.
In one embodiment, a method for preparing a graphene composite thermal pad is provided, which includes:
a) punching the graphene heat-conducting foam film into sheets with consistent sizes, stacking the sheets layer by layer and putting the sheets into corresponding dies, and applying pressure to make the films tightly attached to each other;
b) uniformly coating the bonding glue on the periphery of the pressed foam film to completely coat the foam film into a block;
c) solidifying and molding the block, and cutting the block into sheets along the stacking direction, as shown in FIG. 3;
d) dipping the cut sheet into the dipping glue, taking out, and carrying out hot press molding on the sheet;
e) trimming the edges of the formed sheet, removing the adhesive bonding area at the edges, and obtaining the heat conducting gasket prepared by compounding the graphene foam film and the adhesive, as shown in fig. 1 and 2.
In the step b), the adhesive is mainly distributed on the surface of the graphene foam film block body to play a role in shaping and fixing, so that the foam film block body is prevented from scattering during a cutting process, and the cutting formability is ensured;
examples of the binder include epoxy resins, phenol resins, furfural resins, polyurethanes, acrylic resins, and silicone resins; from the viewpoint of adhesiveness, hardness, strength, and cutting molding effect, epoxy resin is preferable; the viscosity of the epoxy resin is 5000-300000mPa & s, preferably 10000-250000mPa & s, the viscosity is lower than 5000mPa & s, the permeability is too good, and the epoxy resin can easily penetrate into the foam film layers, so that the mechanical property of the gasket is influenced; above 300000 mPas, the viscosity is too high, the bubble removing ability is poor, and the workability is poor;
when the graphene foam film is laminated, shaped and cured, the adhesive can be cured by heating or curing at normal temperature, and in consideration of preparation efficiency, a heating curing type epoxy resin can be selected and cured by heating at 80 ℃;
in step c), the cutting method is not particularly limited, and examples thereof include wire cutting, laser cutting, ultrasonic cutting, blade cutting, and freeze cutting; the thickness of the slice has no special requirement, and the slice is cut according to the specific requirement, and is generally the conventional thickness, such as 0.25-5 mm;
in step d), examples of the impregnating adhesive include epoxy resin, phenol resin, furfural resin, polyurethane, acrylic resin, organic silica gel, and the like; silicone rubber is preferable from the viewpoints of compressibility, compression resilience, hardness, caulking effect, and the like; the organic silica gel is preferably liquid organic silica gel; examples of the liquid silicone gum include polydimethylcyclosiloxane, polydimethylsiloxane, α, ω -dihydroxypolydimethylsiloxane, polydiphenylsiloxane, α, ω -dihydroxypolymethyl (3,3, 3-trifluoropropyl) siloxane, cyanosiloxysilane, α, ω -diethylpolydimethylsiloxane, and the like;
the viscosity of the impregnating adhesive is 50-1000mPa & s, preferably 100 & lt 500mPa & s, the viscosity is lower than 50mPa & s, and the mechanical property of the colloid is relatively poor, so that the overall mechanical property of the gasket is influenced; above 1000mPa · s, the viscosity is too high, the fluidity is poor, the gasket is not easy to be impregnated, and the surface of the gasket is easy to have too many glue layers to influence the heat-conducting property;
hot press molding, namely controlling the thickness of the gasket by using a mold, heating, pressurizing, curing and molding the gasket, wherein the applied pressure is 0.1-2.0MPa, preferably 0.3-1.5MPa, and is lower than 0.1MPa, so that the leveling effect of the surface of the gasket cannot be achieved due to too low pressure; if the pressure is higher than 2.0MPa, the graphene sheet layer in the vertical direction in the gasket is 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 preferably 150 ℃ or lower, more preferably 120 ℃ or lower, and if it is higher than 150 ℃, the curing reaction is too severe due to the excessively high temperature, and the product is liable to crack.
The heat-conducting gasket is prepared by compounding the graphene foam film and the adhesive; the bonding adhesive is coated around the foam film blocks after stacking, pressurizing and laminating, so that the forming and fixing effects can be achieved, the frame scattering phenomenon in the cutting process can be prevented, and the influence on the overall heat-conducting performance caused by the fact that a large amount of bonding adhesive enters between foam film layers can be avoided; graphene sheet layers in the graphene 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 hot press molding, most of the impregnating adhesive is extruded and distributed on the surface of the gasket, and a small amount of adhesive is distributed inside and between each layer of foam film under the action of hot pressing to play a certain role in bonding and fixing, so that the heat conducting gasket is integrally formed after being cured, the mechanical property of the heat conducting gasket is improved, and the heat conducting gasket is not easy to delaminate; due to the hot pressing process, the flatness of the surface of the gasket is improved, the extremely thin adhesive layer is attached, the softness of the gasket is improved due to the low-stress adhesive, and in the actual use process, the improvement of the attaching degree of the surface of the gasket and a base material is facilitated, the interface thermal resistance is reduced, and the overall heat conducting performance is improved; the glue layer on the surface of the gasket solves the problems of powder falling and slag falling on the surface, and improves the reliability of the gasket.
In the following specific examples and comparative examples, the thickness of the graphene composite heat conduction gasket prepared by compounding the graphene foam film and the adhesive is 0.3mm, 1mm, 2mm or 3 mm; the thermal conductivity and the applied thermal resistance of the thermal conductive gasket under the condition of 40psi are tested by ASTM D5470.
Example 1:
in this embodiment, the graphene foam film accounts for 50wt.%, and the adhesive accounts for 50 wt.%;
the thermal conductivity coefficient of the graphene foam film is 50W/(m.K);
the thickness of the graphene foam film is 50 mu m, and the density is 0.12g/cm 3 ；
The average pore diameter of pores inside the graphene foam membrane is 10 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 5000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 1000mPa & s;
hot pressing process, wherein the pressure is 0.1MPa, and the curing temperature is 150 ℃;
the thermal conductivity of the sample is 22W/(m K) through testing, and the applied thermal resistances of the samples with different thicknesses are shown in the following table 1:
TABLE 1
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.65
1.00 0.98
2.00 1.51
3.00 1.88
Example 2:
in this embodiment, the graphene foam film accounts for 95wt.%, and the adhesive accounts for 5 wt.%;
the thermal conductivity coefficient of the graphene foam film is 400W/(m.K);
the thickness of the graphene foam film is 1000 mu m, and the density is 0.88g/cm 3 ；
The average pore diameter of internal pores of the graphene foam membrane is 100 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 300000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 50mPa & s;
hot pressing process, pressure 2.0MPa, curing temperature normal temperature;
the thermal conductivity of the sample is tested to be 305W/(m K), and the applied thermal resistances of the samples with different thicknesses are shown in the following table 2:
TABLE 2
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.07
1.00 0.10
2.00 0.13
3.00 0.16
Example 3:
in this example, the graphene foam film accounts for 60wt.%, and the adhesive accounts for 40 wt.%;
the thermal conductivity coefficient of the graphene foam film is 100W/(m.K);
the thickness of the graphene foam film is 300 mu m, and the density is 0.31g/cm 3 ；
The average pore diameter of pores in the graphene foam film is 20 micrometers;
the adhesive is heating curing type epoxy resin, the viscosity is 10000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 100mPa & s;
hot pressing process, pressure 0.3MPa, curing temperature 80 ℃;
the thermal conductivity of the sample is 55W/(m K) through testing, and the applied thermal resistance of the samples with different thicknesses is shown in the following table 3:
TABLE 3
Figure GDA0003240581790000101
Figure GDA0003240581790000111
Example 4:
in this embodiment, the graphene foam film accounts for 90wt.%, and the adhesive accounts for 10 wt.%;
the thermal conductivity coefficient of the graphene foam film is 200W/(m.K);
the thickness of the graphene foam film is 400 mu m, and the density is 0.22g/cm 3 ；
The average pore diameter of internal pores of the graphene foam membrane is 30 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 250000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 500mPa & s;
hot pressing process, wherein the pressure is 1.5MPa, and the curing temperature is 120 ℃;
the thermal conductivity of the sample is 160W/(m K) through testing, and the applied thermal resistance of the samples with different thicknesses is shown in the following table 4:
TABLE 4
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.12
1.00 0.16
2.00 0.23
3.00 0.29
Example 5:
in this embodiment, the graphene foam film accounts for 85 wt.%, and the adhesive accounts for 15 wt.%;
the thermal conductivity coefficient of the graphene foam film is 250W/(m.K);
the thickness of the graphene foam film is 500 mu m, and the density is 0.39g/cm 3 ；
The average pore diameter of pores inside the graphene foam membrane is 50 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 200000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 800mPa & s;
hot pressing process, pressure 0.5MPa, curing temperature 100 ℃;
the thermal conductivity of the sample is 205W/(m K) through testing, and the applied thermal resistances of the samples with different thicknesses are shown in the following table 5:
TABLE 5
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.15
1.00 0.18
2.00 0.23
3.00 0.28
Example 6:
in this embodiment, the graphene foam film accounts for 70 wt.%, and the adhesive accounts for 30 wt.%;
the thermal conductivity coefficient of the graphene foam film is 150W/(m.K);
the thickness of the graphene foam film is 350 mu m, and the density is 0.50g/cm 3 ；
The average pore diameter of pores in the graphene foam film is 70 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 50000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 300mPa & s;
hot pressing process, wherein the pressure is 1.0MPa, and the curing temperature is 50 ℃;
through testing, the thermal conductivity of the sample is 93W/(m K), and the applied thermal resistances of the samples with different thicknesses are shown in the following table 6:
TABLE 6
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.26
1.00 0.34
2.00 0.43
3.00 0.55
Example 7:
in the embodiment, the ratio of the graphene foam film is 80 wt.%, and the ratio of the adhesive is 20 wt.%;
the thermal conductivity of the graphene foam film is 350W/(m.K);
the thickness of the graphene foam film is 600 mu m, and the density is 0.75g/cm 3 ；
The average pore diameter of pores inside the graphene foam membrane is 60 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 100000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 600mPa & s;
hot pressing process, wherein the pressure is 1.2MPa, and the curing temperature is 60 ℃;
the thermal conductivity of the sample is 235W/(m K) through testing, and the applied thermal resistances of the samples with different thicknesses are shown in the following table 7:
TABLE 7
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 0.17
1.00 0.20
2.00 025
3.00 0.28
Comparative example 1:
in the comparative example, the graphene foam film accounts for 85 wt.%, and the adhesive accounts for 15 wt.%;
the thermal conductivity coefficient of the graphene foam film is 250W/(m.K);
the thickness of the graphene foam film is 500 mu m, and the density is 0.39g/cm 3 ；
The average pore diameter of pores in the graphene foam film is 50 micrometers;
the adhesive is heating curing type epoxy resin, the viscosity is 200000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 800mPa & s;
hot pressing process, wherein the pressure is 3.0MPa, and the curing temperature is 100 ℃;
in the hot pressing process in the comparative example, the gasket is cracked and layered due to overlarge pressure, and cannot be molded. When the pressure is lower than 0.1MPa, the effect of leveling the surface of the gasket cannot be achieved due to too low pressure; the pressure is higher than 2.0MPa, and the graphene sheet layer in the vertical direction in the gasket is 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 overlarge pressure.
Comparative example 2:
in the comparative example, the graphene foam film accounts for 80 wt.%, and the adhesive accounts for 20 wt.%;
the thermal conductivity coefficient of the graphene foam film is 350W/(m.K);
the thickness of the graphene foam film is 600 mu m, and the density is 0.75g/cm 3 ；
The average pore diameter of pores inside the graphene foam membrane is 60 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 100000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 600mPa & s;
hot pressing process, wherein the pressure is 1.2MPa, and the curing temperature is 200 ℃;
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 3:
in the comparative example, the graphene foam film accounts for 60wt.%, and the adhesive accounts for 40 wt.%;
the thermal conductivity coefficient of the graphene foam film is 100W/(m.K);
the thickness of the graphene foam film is 300 mu m, and the density is 0.31g/cm 3 ；
The average pore diameter of pores in the graphene foam film is 20 micrometers;
the adhesive is heating curing type epoxy resin, the viscosity is 10000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 3000mPa & s;
hot pressing process, pressure 0.3MPa, curing temperature 80 ℃;
the thermal conductivity of the sample is 41W/(m K) through testing, and the applied thermal resistance of the samples with different thicknesses is shown in the following table 8:
TABLE 8
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 1.53
1.00 1.67
2.00 1.97
3.00 2.20
Because the dipping glue viscosity is too high and the dipping effect is poor in the comparative example, the dipping glue on the surface of the sample is too large, and the surface glue layer is too thick, so that the heat-conducting property of the sample is obviously reduced, and the application thermal resistance is obviously improved.
Comparative example 4:
in the comparative example, the graphene foam film accounts for 30 wt.%, and the adhesive accounts for 70 wt.%;
the thermal conductivity coefficient of the graphene foam film is 200W/(m.K);
the thickness of the graphene foam film is 400 mu m, and the density is 0.22g/cm 3 ；
The average pore diameter of the inner pores of the graphene foam membrane is 30 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 250000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 500mPa & s;
hot pressing process, wherein the pressure is 1.5MPa, and the curing temperature is 120 ℃;
through testing, the thermal conductivity of the sample is 48W/(m K), and the applied thermal resistances of the samples with different thicknesses are shown in the following table 9:
TABLE 9
Thickness (mm) Using thermal resistance (Kcm) 2 /W)
0.30 1.27
1.00 1.40
2.00 1.64
3.00 1.84
The proportion of the graphene foam film adopted in the comparative example is too low, so that the content of silica gel is too high, the heat-conducting property of the sample is obviously reduced, and the application thermal resistance is obviously improved.
Comparative example 5:
in the comparative example, the ratio of the graphene foam film to the adhesive is 97 wt.%, and the ratio of the adhesive to the adhesive is 3 wt.%;
the thermal conductivity coefficient of the graphene foam film is 150W/(m.K);
the thickness of the graphene foam film is 350 mu m, and the density is 0.50g/cm 3 ；
The average pore diameter of pores in the graphene foam film is 70 mu m;
the adhesive is heating curing type epoxy resin, the viscosity is 50000mPa & s, and the curing temperature is 80 ℃;
the impregnating adhesive is liquid silica gel with the viscosity of 300mPa & s;
hot pressing process, wherein the pressure is 1.0MPa, and the curing temperature is 50 ℃;
because the adhesive dosage in this comparison example is too little, lead to the mechanical properties of gasket relatively poor, cracking, layering phenomenon appear easily at last, can't the shaping.
In the embodiment of the invention, the adopted liquid silica gel is taken as a representative of the adhesive, and other types of adhesives are also applicable.
According to the invention, the process that the adhesive is only adhered and fixed around the block body is used, so that the content of the adhesive in the whole gasket is reduced, the whole graphene occupation ratio is improved, and the heat-conducting property is improved; the hot press molding process is beneficial to improving the mechanical property of the gasket heat-conducting gasket and ensuring the moldability; the surface flatness of the gasket is good, the surface is soft, and in the actual use process, the bonding degree between the surface of the gasket and the substrate is favorably improved, the interface thermal resistance is reduced, and the integral heat-conducting property is improved; the glue layer on the surface of the gasket solves the problems of powder falling and slag falling on the surface, and improves the reliability of the gasket.
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 (20)

1. A preparation method of a graphene composite heat conduction gasket is characterized by comprising the following steps:
stacking the graphene foam film layers, putting the graphene foam film layers into a mold, and applying pressure to enable the films to be tightly attached;
uniformly coating adhesive glue around the pressed graphene heat-conducting foam film to completely coat the multilayer graphene heat-conducting foam film into a block, wherein the adhesive glue is epoxy resin, and the viscosity of the epoxy resin is 5000-300000mPa & s;
curing and molding the block, and cutting the block into sheets along the stacking direction;
dipping the cut sheet material into dipping glue, taking out, and carrying out hot press molding on the taken-out sheet material, wherein the dipping glue has the viscosity of 50-1000mPa & s;
and trimming the edges of the formed sheet, and removing the adhesive bonding area at the edges to obtain the graphene composite heat-conducting gasket, wherein the graphene foam film accounts for 50-95 wt.%.
2. The method according to claim 1, wherein the viscosity of the epoxy resin is 10000-250000 mPas.
3. The method according to claim 1, wherein the adhesive is cured by heating or by ambient temperature.
4. The preparation method according to claim 3, wherein the adhesive is a heat-curable epoxy resin and is cured by heating at 80 ℃.
5. The method according to claim 1, wherein in the step of solidifying and forming the block body and cutting the block body into sheets along the stacking direction, the cutting is performed by linear cutting, laser cutting, ultrasonic cutting or freezing cutting.
6. The method of claim 1, wherein the cut sheet has a thickness of 0.25 to 5 mm.
7. The method according to claim 1, wherein the step of impregnating the cut sheet with an impregnating compound, wherein the impregnating compound is one or more of epoxy resin, phenolic resin, furfural resin, polyurethane, acrylic resin, and silicone.
8. The method according to claim 7, wherein the impregnating gel is a silicone gel.
9. The method of claim 8, wherein the impregnating gel is a liquid silicone gel.
10. The method of claim 9, wherein the liquid silicone gum is one or more of polydimethylsiloxane, α, ω -dihydroxypolydimethylsiloxane, and α, ω -dihydroxypolymethyl (3,3, 3-trifluoropropyl) siloxane.
11. The production method according to claim 1, wherein the impregnating agent has a viscosity of 100-500 mPa-s.
12. The manufacturing method according to claim 1, wherein in the step of hot press forming the taken out sheet, the hot press forming is performed by controlling the thickness of the gasket by using a die, and the taken out sheet is subjected to heat and pressure curing forming with an applied pressure of 0.1 to 2.0 MPa; the curing temperature is below 150 ℃.
13. The production method according to claim 12, wherein the applied pressure is 0.3 to 1.5 MPa; the curing temperature is below 120 ℃.
14. The method for preparing the graphene foam film according to claim 1, wherein the graphene foam film accounts for 60-90 wt.%.
15. The production method according to claim 1, wherein the graphene foam film has a thermal conductivity of not less than 50W/(m-K).
16. The production method according to claim 15, wherein the thermal conductivity of the graphene foam film is not less than 100W/(m-K).
17. The preparation method according to claim 1, wherein the graphene foam film has a density of 0.10-0.90g/cm 3 。
18. The method of claim 17, wherein the method comprisesThe thickness of the graphene foam film is 0.20-0.70g/cm 3 。
19. The preparation method of claim 1, wherein the graphene foam membrane is composed of graphene pore walls and pores, the graphene is in a layered structure, the pores exist between layers, and the average pore diameter of the pores inside the layered graphene structure is 10-100 μm.
20. The method of claim 19, wherein the average pore size is 15 to 50 μm.
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