CN115160733A - Epoxy resin composite material, preparation method thereof, heat conducting fin and electronic device - Google Patents
Epoxy resin composite material, preparation method thereof, heat conducting fin and electronic device Download PDFInfo
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- CN115160733A CN115160733A CN202210847121.4A CN202210847121A CN115160733A CN 115160733 A CN115160733 A CN 115160733A CN 202210847121 A CN202210847121 A CN 202210847121A CN 115160733 A CN115160733 A CN 115160733A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
Abstract
The invention relates to the technical field of electronic packaging, in particular to an epoxy resin composite material, a preparation method thereof, a heat conducting sheet and an electronic device. The epoxy resin composite material comprises an epoxy resin matrix and a plurality of fluorinated graphene films positioned in the epoxy resin matrix, wherein the fluorinated graphene films are orderly arranged in an oriented manner along the thickness z direction of the epoxy resin matrix, the adjacent fluorinated graphene films are distributed at equal intervals of 0.03-0.1 mm along the length x direction of the epoxy resin matrix, the length x of the epoxy resin matrix is more than or equal to 1cm, and the adjacent fluorinated graphene films are distributed at equal intervals of 0.3-0.8 mm along the width y direction of the epoxy resin matrix. The thermal conductivity of the epoxy resin composite material is high.
Description
Technical Field
The invention relates to the technical field of electronic packaging, in particular to an epoxy resin composite material, a preparation method thereof, a heat conducting sheet and an electronic device.
Background
In the electronics industry, the packaging, design, and manufacture of Integrated Circuits (ICs) constitute the three major pillars of the IC industry. IC packaging is the bonding of packaging materials and semiconductor chips together to form a semiconductor-based electronic functional block device. The commonly used packaging materials mainly include metal-based packaging materials, ceramic packaging materials and plastic packaging materials. The ceramic packaging material and the metal-based packaging material are hermetically packaged, have the characteristic of high reliability, but are mainly used in the fields of aerospace, aviation and military due to high price; plastic packages are widely used in the consumer industry due to their low cost and high density. Up to now, 90% of semiconductor devices are packaged by plastic, and among them, epoxy resin packaging materials have the outstanding advantages of low shrinkage, good adhesion, good corrosion resistance, excellent electrical properties, lower cost, etc., and are commonly used plastic packaging materials, which account for more than 90% of plastic packaging materials. However, the epoxy resin encapsulating material has low thermal conductivity, and thus it is difficult to satisfy the heat dissipation requirement of the semiconductor chip.
Disclosure of Invention
Accordingly, there is a need for an epoxy resin composite material capable of improving thermal conductivity, a method for preparing the same, a thermally conductive sheet, and an electronic device.
The invention provides an epoxy resin composite material, which comprises an epoxy resin matrix and a plurality of fluorinated graphene films positioned in the epoxy resin matrix, wherein the fluorinated graphene films are orderly arranged along the thickness z direction of the epoxy resin matrix in an oriented manner, the adjacent fluorinated graphene films are distributed along the length x direction of the epoxy resin matrix at equal intervals of 0.03-0.1 mm, the length x of the epoxy resin matrix is more than or equal to 1cm, and the adjacent fluorinated graphene films are distributed along the width y direction of the epoxy resin matrix at equal intervals of 0.3-0.8 mm.
In one embodiment, the length of the epoxy resin matrix is 1cm ≦ x ≦ 15cm.
In one embodiment, it satisfies at least one of the following characteristics:
(1) Y is more than or equal to 1cm and less than or equal to 15cm;
(2) The thickness of the epoxy resin matrix is more than or equal to 2mm and less than or equal to 6mm.
In one embodiment, the height of the fluorinated graphene film is the same as the thickness z of the epoxy resin matrix, the thickness of the fluorinated graphene film is 10 μm to 25 μm, and the width of the fluorinated graphene film is 0.5mm to 1.5mm.
In one embodiment, the thermal conductivity of the epoxy resin composite material in the thickness direction is 8W/mK to 15W/mK.
In one embodiment, the fluorinated graphene film has a fluorine content of 45wt% to 65wt%.
In one aspect of the present invention, a method for preparing the epoxy resin composite material described above is further provided, which includes the following steps:
s100: forming a plurality of hollow structures which are distributed at equal intervals on the fluorinated graphene film, wherein the width of each hollow structure is 0.3-0.8 mm, and preparing the hollow fluorinated graphene film;
s200: forming an epoxy resin layer on the surface of the hollowed fluorinated graphene film, wherein the thickness of the epoxy resin layer is 0.03-0.1 mm;
s300: placing the hollow fluorinated graphene film prepared in the step S100 on the epoxy resin layer, and repeating the step S200;
s400: repeating the steps S100-S300 to obtain a laminated body with the fluorinated graphene film and the epoxy resin layer alternately laminated, wherein the thickness of the laminated body is more than or equal to 1cm; and
s500: the stack was cut and turned 90 °.
In one embodiment, the adjacent hollow structures are distributed at equal intervals of 0.5 mm-1.5 mm.
In one embodiment, the cutting in step S500 is equally spaced 2mm to 6mm cutting.
In another aspect of the present invention, there is further provided a thermally conductive sheet made of the epoxy resin composite material described above.
In another aspect of the present invention, an electronic device is provided, which includes the above-mentioned thermal conductive sheet and a chip, wherein the thermal conductive sheet is used for encapsulating the chip.
According to the epoxy resin composite material, the fluorinated graphene film is added into the epoxy resin matrix and is arranged in an oriented manner along the thickness direction of the epoxy resin matrix, and the distance between the fluorinated graphene film and the epoxy resin matrix in length and width is further regulated, so that the epoxy resin composite material has high thermal conductivity (at least more than 8W/mK) in the thickness direction, is very suitable for packaging a semiconductor element (such as a chip), can rapidly lead out the heat of the semiconductor element, and solves the problem of poor heat dissipation performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a hollow fluorinated graphene film prepared in one embodiment of the present invention;
FIG. 2 is a schematic structural view of a laminate produced in one embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an epoxy resin composite material produced in one embodiment of the present invention.
Description of reference numerals: 10. a fluorinated graphene film; 20. a hollow structure; 30. and an epoxy resin layer.
Detailed Description
Reference will now be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. Indeed, it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment, can be used on another embodiment to yield a still further embodiment.
It is therefore intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present invention are disclosed in or are apparent from the following detailed description. It is to be understood by one of ordinary skill in the art that the present discussion is a description of exemplary embodiments only, and is not intended as limiting the broader aspects of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
"orientation" means a preferred parallel alignment in a particular direction.
The invention provides an epoxy resin composite material, which comprises an epoxy resin matrix and a plurality of fluorinated graphene films positioned in the epoxy resin matrix, wherein the fluorinated graphene films are orderly oriented and arranged along the thickness z direction of the epoxy resin matrix, adjacent fluorinated graphene films are distributed at equal intervals of 0.03-0.1 mm along the length x direction of the epoxy resin matrix, the length x of the epoxy resin matrix is more than or equal to 1cm, and adjacent fluorinated graphene films are distributed at equal intervals of 0.3-0.8 mm along the width y direction of the epoxy resin matrix.
According to the epoxy resin composite material, the fluorinated graphene film is added into the epoxy resin matrix and is arranged in an oriented manner along the thickness direction of the epoxy resin matrix, and the distance between the fluorinated graphene film and the epoxy resin matrix in length and width is further regulated, so that the epoxy resin composite material has high thermal conductivity (at least more than 8W/mK) in the thickness direction, is very suitable for packaging a semiconductor element (such as a chip), can rapidly lead out the heat of the semiconductor element, and solves the problem of poor heat dissipation performance.
It is understood that the equal spacing between adjacent fluorinated graphene films is distributed from 0.03mm to 0.1mm, which means that the spacing between adjacent fluorinated graphene films may be any value between 0.03mm and 0.1mm, and for example, may be 0.04mm, 0.05mm, 0.06mm, 0.07mm, 0.08mm, or 0.09mm.
It is understood that the equal spacing between adjacent fluorinated graphene films is 0.3mm to 0.8mm in distribution, which means that the spacing between adjacent fluorinated graphene films can be any value between 0.3mm to 0.8mm, and for example, can also be 0.4mm, 0.5mm, 0.6mm, or 0.7mm.
In some embodiments, the epoxy resin matrix has a length of 1cm ≦ x ≦ 15cm, and may also be, for example, 2cm, 3cm, 4cm, 5cm, 6cm, 7cm, 8cm, 9cm, 10cm, 11cm, 12cm, 13cm, 14cm.
In some embodiments, the epoxy resin matrix has a width of 1cm ≦ y ≦ 15cm, and may also be 2cm, 3cm, 4cm, 5cm, 6cm, 7cm, 8cm, 9cm, 10cm, 11cm, 12cm, 13cm, 14cm.
In some embodiments, the thickness of the epoxy resin matrix is 2mm ≦ z ≦ 6mm, and may also be 3mm, 4mm, or 5mm, for example.
In some embodiments, the height of the fluorinated graphene film is the same as the thickness z of the epoxy matrix, i.e., the height of the fluorinated graphene film is from 2mm to 6mm.
In some embodiments, the fluorinated graphene film may have a thickness of 10 μm to 25 μm and a width of 0.5mm to 1.5mm.
In some embodiments, the thermal conductivity of the epoxy resin composite material in the thickness direction is 8W/mK to 15W/mK.
In some embodiments, the fluorine content of the fluorinated graphene film may be any known in the art, for example, the fluorine content in the fluorinated graphene film may be 45wt% to 65wt%.
The second object of the present invention is to provide a method for preparing the epoxy resin composite material, which comprises steps S100 to S500:
step S100: forming a plurality of hollow structures which are distributed at equal intervals on the fluorinated graphene film, wherein the width of each hollow structure is 0.3-0.8 mm, and preparing the hollow fluorinated graphene film;
in some embodiments, the shape of the fluorinated graphene film in step S100 is not limited, and may be, for example, a rectangle or a square.
In some embodiments, the fluorinated graphene film in step S100 may have a thickness of 10 to 25 μm and a length and a width of 1 to 15cm, respectively and independently.
In some embodiments, the adjacent hollow structures are distributed at equal intervals of 0.5mm to 1.5mm.
In some embodiments, the method for forming the plurality of hollow structures distributed at equal intervals is not limited, and for example, a laser cutting process may be selected.
Step S200: forming an epoxy resin layer on the surface of the hollow fluorinated graphene film, wherein the thickness of the epoxy resin layer is 0.03-0.1 mm;
in some embodiments, the method of forming the epoxy resin layer is not limited, and for example, a coating and curing process such as knife coating and heat curing may be selected. Specifically, a mixed solution formed by epoxy resin and a curing agent may be coated on the surface of the hollowed-out fluorinated graphene film, and then heated and cured. The curing agent may be any curing agent known in the art, and may be one or more of ethylenediamine, tetramethylenediamine, hexamethylenediamine, diaminodiphenylmethane, m-phenylenediamine, and phthalic anhydride, for example; the mass ratio of the epoxy resin to the curing agent may be any known ratio in the art, and may be, for example, (0.4 to 0.6): 1. in addition, the parameters of heating and curing are not limited, so that the mixed solution of the epoxy resin and the curing agent is subjected to curing and molding.
Step S300: placing the hollow fluorinated graphene film prepared in the step S100 on the epoxy resin layer, and repeating the step S200;
step S400: repeating the steps S100-S300 until a laminated body formed by alternately laminating the fluorinated graphene film and the epoxy resin layer is obtained, wherein the thickness of the laminated body is more than or equal to 1cm; and
step S500: the stack was cut and turned 90 °. The fluorinated graphene film can be orderly oriented and arranged in the thickness direction of the epoxy resin composite material by turning 90 degrees, so that the thermal conductivity of the epoxy resin composite material in the thickness direction is improved.
In some embodiments, the cuts in step S500 are equally spaced 2mm to 6mm cuts.
The third object of the present invention is to further provide a heat conducting sheet, which is made of the epoxy resin composite material.
A fourth object of the present invention is to provide an electronic device, which includes the above thermal conductive sheet and a chip, wherein the thermal conductive sheet is used for encapsulating the chip.
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 45wt%, a thickness of 25 μm, and a length and a width of 15cm on a laser cutting platform, controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (0.5 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10, so as to obtain the periodically hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.3mm and a length of 14cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a blade coater, and uniformly spraying a mixed solution of epoxy resin and ethylenediamine (mass ratio is 0.4;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the fluorinated graphene film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 15cm;
(5) Heating the laminated body prepared in the step (4) in an oven to cure the epoxy resin to form an epoxy resin composite material; and then cutting the epoxy resin composite material by using the multi-wire diamond at equal intervals of 2mm along the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 2mm as shown in figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 25 μm, a width of 1.5mm, and a height of 2mm, and the respective fluorinated graphene films 10 are arranged at an equal interval of 0.03mm in the x direction and at an equal interval of 0.3mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 15W/mK.
Example 2
This example is prepared substantially identically to example 1, except that: the content of fluorine in the fluorinated graphene film 10 is 65wt%, and the specific steps are as follows:
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 65wt%, a thickness of 25 μm, and a length and a width of 15cm on a laser cutting platform, controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (0.5 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10, so as to obtain the periodically hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.3mm and a length of 14cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a blade coater, and uniformly spraying a mixed solution of epoxy resin and tetramethylenediamine (mass ratio is 0.6;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the fluorinated graphene film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 15cm;
(5) Placing the laminated body prepared in the step (4) in an oven, and heating to cure the epoxy resin to form an epoxy resin composite material; and then cutting the epoxy resin composite material by using the multi-wire diamond at equal intervals of 2mm along the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 2mm as shown in figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 25 μm, a width of 1.5mm, and a height of 2mm, and the respective fluorinated graphene films 10 are arranged at an equal pitch of 0.03mm in the x direction and at an equal pitch of 0.3mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 14W/mK.
Example 3
This example is prepared substantially identically to example 2, except that: the fluorinated graphene films 10 have different thicknesses, and the specific steps are as follows:
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 65wt%, a thickness of 10 μm, and a length and a width of 15cm on a laser cutting platform, and controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (0.5 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10 to obtain the periodically hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.3mm and a length of 14cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a blade coater, and uniformly spraying a mixed solution of epoxy resin and m-phenylenediamine (the mass ratio is 0.5;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the fluorinated graphene film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 15cm;
(5) Placing the laminated body prepared in the step (4) in an oven, and heating to cure the epoxy resin to form an epoxy resin composite material; and then cutting the epoxy resin composite material by using the multi-wire diamond at equal intervals of 2mm along the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 2mm as shown in figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 10 μm, a width of 1.5mm, and a height of 2mm, and the respective fluorinated graphene films 10 are arranged at an equal interval of 0.03mm in the x direction and at an equal interval of 0.3mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 12W/mK.
Example 4
This example is prepared substantially identically to example 2, except that: the dimension parameters of the fluorinated graphene film 10, the thickness of the laminate in the step (4), and the thickness of the heat conducting sheet are different, and the specific steps are as follows:
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 65wt%, a thickness of 10 μm, and a length and a width of 10cm on a laser cutting platform, controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (2 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10, so as to obtain a periodic hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.8mm and a length of 6cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a knife coater, and uniformly spraying a mixed solution of epoxy resin and curing agent phthalic anhydride (mass ratio is 0.5;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the fluorinated graphene film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 10cm;
(5) Heating the laminated body prepared in the step (4) in an oven to cure the epoxy resin to form an epoxy resin composite material; and then, cutting the epoxy resin composite material by using the multi-wire diamond at equal intervals of 6mm in the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 6mm as shown in figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 10 μm, a width of 1.5mm, and a height of 2mm, and the respective fluorinated graphene films 10 are arranged at an equal pitch of 0.03mm in the x direction and at an equal pitch of 0.8mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 11W/mK.
Example 5
This example is prepared substantially identically to example 2, except that: the thickness of the epoxy resin layer 30 is different, and the specific steps are as follows:
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 65wt%, a thickness of 10 μm, and a length and a width of 10cm on a laser cutting platform, controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (2 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10, so as to obtain a periodic hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.8mm and a length of 6cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a blade coater, and uniformly spraying a mixed solution of epoxy resin and phthalic anhydride (mass ratio is 0.5;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the fluorinated graphene film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 10cm;
(5) Heating the laminated body prepared in the step (4) in an oven to cure the epoxy resin to form an epoxy resin composite material; and then, cutting the epoxy resin composite material by using multi-line diamonds at equal intervals of 6mm in the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 6mm as shown in the figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 10 μm, a width of 1.5mm, and a height of 6mm, and the fluorinated graphene films 10 are arranged at an equal interval of 0.06mm in the x direction and at an equal interval of 0.8mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 9W/mK.
Example 6
This example is prepared substantially identically to example 2, except that: the thickness of the epoxy resin layer 30 is different, and the specific steps are as follows:
(1) Tiling a square fluorinated graphene film 10 with a fluorine content of 65wt%, a thickness of 10 μm, and a length and a width of 10cm on a laser cutting platform, controlling a laser cutting device program to cut at equal intervals (1.5 mm) in a central region (2 cm away from an edge of the fluorinated graphene film 10) of the fluorinated graphene film 10, so as to obtain a periodic hollowed-out fluorinated graphene film 10 shown in fig. 1, wherein each hollowed-out structure 20 has a width of 0.8mm and a length of 6cm;
(2) Transferring the periodically hollowed fluorinated graphene film 10 prepared in the step (1) to a scraper coater, and uniformly spraying a mixed solution of epoxy resin and diaminodiphenylmethane (mass ratio is 0.4;
(3) Placing the fluorinated graphene film 10 prepared in the step (1) on the surface of the epoxy resin layer 30 formed in the step (2), and repeating the step (2) to form the epoxy resin layer 30 on the surface of the fluorinated graphene film 10;
(4) As shown in fig. 2, repeating the steps (1) to (3) yields a laminate in which the graphene fluoride film 10 and the epoxy resin layer 30 are alternately laminated, the thickness of the laminate being 10cm;
(5) Placing the laminated body prepared in the step (4) in an oven, and heating to cure the epoxy resin to form an epoxy resin composite material; and then, cutting the epoxy resin composite material by using the multi-wire diamond at equal intervals of 6mm in the thickness direction of the epoxy resin composite material, and turning the cut epoxy resin composite material by 90 degrees to obtain a plurality of epoxy resin composite materials with the thickness of 6mm as shown in figure 3. As can be seen from fig. 3, the interior of the epoxy resin composite material contains periodically arranged fluorinated graphene films 10 along the thickness direction thereof, each fluorinated graphene film 10 has a thickness of 10 μm, a width of 1.5mm, and a height of 6mm, and the respective fluorinated graphene films 10 are arranged at an equal pitch of 0.1mm in the x direction and at an equal pitch of 0.8mm in the y direction. The fluorinated graphene films 10 are covered with epoxy layers 20 between and on the surface. The thermal conductivity of the epoxy resin composite material is tested to be 8W/mK.
Comparative example 1
This comparative example was prepared substantially identically to example 1, except that: the width of the hollow structure is 1.5mm. The thermal conductivity of the epoxy resin composite material was measured to be 6.5W/mK.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The epoxy resin composite material is characterized by comprising an epoxy resin matrix and a plurality of fluorinated graphene films positioned in the epoxy resin matrix, wherein the fluorinated graphene films are orderly arranged along the thickness z direction of the epoxy resin matrix in an oriented manner, the adjacent fluorinated graphene films are distributed at equal intervals of 0.03-0.1 mm along the length x direction of the epoxy resin matrix, the length x of the epoxy resin matrix is not less than 1cm, and the adjacent fluorinated graphene films are distributed at equal intervals of 0.3-0.8 mm along the width y direction of the epoxy resin matrix.
2. The epoxy resin composite of claim 1, wherein the epoxy resin matrix has a length of 1cm ≦ x ≦ 15cm.
3. The epoxy resin composite according to claim 1, characterized in that it satisfies at least one of the following characteristics:
(1) The width y of the epoxy resin matrix is not less than 1cm and not more than 15cm;
(2) The thickness of the epoxy resin matrix is more than or equal to 2mm and less than or equal to 6mm.
4. The epoxy composite of claim 3, wherein the fluorinated graphene film has a height that is the same as the thickness z of the epoxy matrix, a thickness of 10 μm to 25 μm, and a width of 0.5mm to 1.5mm.
5. The epoxy resin composite according to claim 3, wherein the thermal conductivity in the thickness direction of the epoxy resin composite is 8W/mK to 15W/mK.
6. The epoxy resin composite according to any one of claims 1 to 5, wherein the fluorinated graphene film has a fluorine content of 45wt% to 65wt%.
7. A method for preparing an epoxy resin composite material according to any one of claims 1 to 6, comprising the steps of:
s100: forming a plurality of hollow structures which are distributed at equal intervals on the fluorinated graphene film, wherein the width of each hollow structure is 0.3-0.8 mm, and preparing the hollow fluorinated graphene film;
s200: forming an epoxy resin layer on the surface of the hollowed-out fluorinated graphene film, wherein the thickness of the epoxy resin layer is 0.03-0.1 mm;
s300: placing the hollow fluorinated graphene film prepared in the step S100 on the epoxy resin layer, and repeating the step S200;
s400: repeating the steps S100-S300 to obtain a laminated body with the fluorinated graphene film and the epoxy resin layer alternately laminated, wherein the thickness of the laminated body is more than or equal to 1cm; and
s500: the stack was cut and turned 90 °.
8. The preparation method of the epoxy resin composite material according to claim 7, wherein the adjacent hollow structures are distributed at equal intervals of 0.5 mm-1.5 mm; and/or
The cutting in step S500 is equal interval 2 mm-6 mm cutting.
9. A thermally conductive sheet, characterized by being produced from the epoxy resin composite material according to any one of claims 1 to 6.
10. An electronic device comprising the thermal conductive sheet according to claim 9 and a chip, wherein the thermal conductive sheet is used for encapsulating the chip.
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