CN115011072A - Epoxy resin composite heat conducting fin and preparation method thereof - Google Patents
Epoxy resin composite heat conducting fin and preparation method thereof Download PDFInfo
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- CN115011072A CN115011072A CN202210800473.4A CN202210800473A CN115011072A CN 115011072 A CN115011072 A CN 115011072A CN 202210800473 A CN202210800473 A CN 202210800473A CN 115011072 A CN115011072 A CN 115011072A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a preparation method of an epoxy resin composite heat conducting sheet, which is characterized by comprising the following steps: mixing fluorinated graphene, epoxy resin, a curing agent and an organic solvent to prepare epoxy resin mixed dispersion liquid; and (3) defoaming the epoxy resin mixed dispersion liquid in vacuum, then placing the epoxy resin mixed dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, removing the organic solvent, crosslinking and curing the epoxy resin, cutting the epoxy resin in the thickness direction, and reversing the epoxy resin for 90 degrees to prepare the epoxy resin composite heat conducting sheet. According to the preparation method of the epoxy resin composite heat conducting fin, the fluorinated graphene and the epoxy resin are used as raw materials and matched with the action of the magnetic field, so that the fluorinated graphene is arranged in an oriented manner, the heat conducting performance of the epoxy resin is further effectively improved, and the prepared epoxy resin composite heat conducting fin has high heat conductivity. The material is used as a semiconductor chip packaging material, so that the heat conduction of the chip can be accelerated, and the heat dissipation problem of the chip can be solved.
Description
Technical Field
The invention relates to the technical field of functional sheet materials, in particular to an epoxy resin composite heat conducting sheet and a preparation method thereof.
Background
In the electronics industry, the Integrated Circuit (IC) industry primarily involves the packaging, design, and manufacture of integrated circuits. The packaging of integrated circuits refers to the bonding of semiconductor chips and packaging materials together to form semiconductor chip-based electronic functional block devices. The packaging material mainly comprises a metal-based packaging material, a ceramic packaging material and a plastic packaging material. The metal-based packaging material and the ceramic packaging material are hermetically packaged, have high reliability and high price, and are mainly used in the fields of aviation, aerospace and military; plastic packaging materials are widely used in the civil field due to their advantages in terms of cost and density. Currently, approximately 90% of semiconductor chips employ plastic encapsulation materials. The epoxy resin accounts for more than 90% of the plastic packaging material due to the outstanding advantages of low shrinkage, good cohesiveness, good corrosion resistance, excellent electrical property, lower cost and the like. With the increase of the integration degree of the semiconductor chip, the heat productivity of the semiconductor chip in the using process is larger and larger, which puts higher demands on the heat conducting performance of the packaging material.
There is a technique related to modifying an epoxy resin with a thermally conductive filler to improve the thermal conductivity of the epoxy resin. The heat-conducting filler serves as a heat-conducting node in the epoxy resin composite material, so that the thermal resistance of an interface is reduced, a heat-conducting network for transferring heat is formed, and the heat-conducting property of the material is further improved. The fluorinated graphene has high thermal conductivity, the theoretical thermal conductivity of the fluorinated graphene can reach 1800W/mK, and the fluorinated graphene is an insulating material. Therefore, when the epoxy resin is used as the heat conducting filler, the insulation requirement of the chip packaging material can be met, and meanwhile, the heat conductivity of the epoxy resin can be obviously improved. However, the thermal conductivity of the fluorinated graphene modified epoxy resin prepared by the traditional method is still low, and the increasing heat dissipation requirements of the semiconductor chip are difficult to meet.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for producing an epoxy resin composite heat conductive sheet capable of having high heat conductive properties.
The preparation method of the epoxy resin composite heat-conducting sheet provided by the embodiment of the invention comprises the following steps:
mixing fluorinated graphene, epoxy resin, a curing agent and an organic solvent to prepare a fluorinated graphene epoxy resin mixed dispersion liquid;
and (2) carrying out vacuum defoaming on the fluorinated graphene epoxy resin mixed dispersion liquid, then placing the dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, removing the organic solvent, crosslinking and curing the epoxy resin, cutting the epoxy resin in the thickness direction, and reversing the epoxy resin by 90 degrees to prepare the epoxy resin composite heat conducting sheet.
In one embodiment, the fluorinated graphene is a sheet-structured fluorinated graphene with the number of layers being 5-20; and/or the flake diameter of the fluorinated graphene is 5-20 microns.
In one embodiment, the fluorine content of the fluorinated graphene is 45 wt% to 65 wt%.
In one embodiment, the mass ratio of the fluorinated graphene to the epoxy resin is 1: (1-3); and/or the epoxy value of the epoxy resin is 0.25-0.45.
In one embodiment, the organic solvent comprises one or more of ethanol, diethyl ether, isopropanol, and acetone.
In one embodiment, the curing agent is one or more of ethylenediamine, tetramethylenediamine, hexamethylenediamine, diaminodiphenylmethane, m-phenylenediamine, and phthalic anhydride; and/or the mass ratio of the curing agent to the epoxy resin is (0.4-0.6): 1.
in one embodiment, the magnetic field has a strength of 25 Tesla to 50 Tesla.
In one embodiment, the magnetic field is applied by a magnetic field orienting device, and the magnetic field orienting device comprises a power supply (1), two coils (2) and (3) which are connected with the power supply and distributed at intervals, an electric heating plate (4) positioned between the two coils (2) and (3), and a mold (5) placed on the electric heating plate (4); the two coils (2) and (3) have the same radius and are arranged oppositely; the central connecting line of the two coils (2) and (3) is superposed with the central axis of the mould (5); when the orientation treatment is performed, the epoxy resin mixed dispersion liquid is placed in a molding groove of the mold (5).
The invention provides an epoxy resin composite heat conducting sheet, which is prepared by the preparation method of the epoxy resin composite heat conducting sheet.
In one embodiment, the thickness of the epoxy resin composite heat conducting sheet is 2-6 mm; and/or the vertical thermal conductivity of the epoxy resin composite heat conducting sheet is 4W/m.degree to 8W/m.degree.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the preparation method of the epoxy resin composite heat conducting fin, the fluorinated graphene and the epoxy resin are used as raw materials and matched with the action of the magnetic field, so that the fluorinated graphene is arranged in an oriented manner, the heat conducting performance of the epoxy resin is further effectively improved, and the prepared epoxy resin composite heat conducting fin has high heat conductivity. The material is used as a semiconductor chip packaging material, so that the heat conduction of the chip can be accelerated, and the heat dissipation problem of the chip can be solved.
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FIG. 1 is a schematic view of a magnetic field orienting device;
reference numerals:
1: a power source; 2 and 3: a coil; 4: an electric hot plate; 5: and (5) molding.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The following is a description of preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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.
Reference herein to numerical intervals is deemed to be continuous, unless otherwise stated, and includes both the minimum and maximum values of that range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
The temperature parameter herein is not particularly limited, and is allowed to be either constant temperature treatment or treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
An embodiment provides a preparation method of a graphene composite heat conducting sheet, which comprises the following steps:
S110: and mixing the fluorinated graphene, the epoxy resin, the curing agent and the organic solvent to prepare the fluorinated graphene-epoxy resin mixed dispersion liquid.
In one example, the fluorinated graphene and the epoxy resin are added into the organic solvent, and the mixture is stirred in vacuum until the mixture is uniformly dispersed, then the curing agent is added, and the mixture is stirred in vacuum again to prepare the fluorinated graphene epoxy resin mixed dispersion liquid.
In one example, the fluorinated graphene is a sheet-structured fluorinated graphene having 5 to 20 layers. In some specific examples, the number of layers of the fluorinated graphene is 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, or 20 layers.
In one example, the fluorinated graphene has a sheet diameter of 5 to 20 micrometers, and may be, for example, 5 to 6 micrometers, 7 micrometers, 8 micrometers, 9 micrometers, 10 micrometers, 11 micrometers, 12 micrometers, 13 micrometers, 14 micrometers, 15 micrometers, 16 micrometers, 17 micrometers, 18 micrometers, 19 micrometers, or 20 micrometers.
In one example, the fluorinated graphene has a fluorine content of 45 wt% to 65 wt%. In some specific examples, the content of elemental fluorine may be 45 wt%, 46 wt%, 47 wt%, 48 wt%, 49 wt%, 50 wt%, 51 wt%, 52 wt%, 53 wt%, 54 wt%, 55 wt%, 56 wt%, 57 wt%, 58 wt%, 59 wt%, 60 wt%, 61 wt%, 62 wt%, 63 wt%, 64 wt%, or 65 wt%.
In one example, the mass ratio of the fluorinated graphene to the epoxy resin is 1: (1-3). In some specific examples, the mass ratio of the fluorinated graphene to the epoxy resin may be 1: 1. 1: 1.5, 1: 2. 1: 2.5 or 1: 3.
in one example, the organic solvent includes one or more of ethanol, diethyl ether, isopropanol, and acetone.
In one example, the curing agent is one or more of ethylenediamine, tetramethylenediamine, hexamethylenediamine, diaminodiphenylmethane, m-phenylenediamine, and phthalic anhydride.
In one example, the mass ratio of the curing agent to the epoxy resin is (0.4-0.6): 1. in some specific examples, the mass ratio of curing agent to epoxy resin may be 0.4: 1. 0.42: 1. 0.46: 1. 0.5: 1. 0.53: 1. 0.56: 1. 0.58: 1 or 0.6: 1.
in one example, the epoxy value of the epoxy resin is 0.25 to 0.45. In some specific examples, the epoxy value of the epoxy resin may be 0.25, 0.27, 0.29, 0.31, 0.33, 0.35, 0.37, 0.39, 0.41, 0.43, or 0.45.
S120: and (3) defoaming the epoxy resin mixed dispersion liquid in vacuum, then placing the epoxy resin mixed dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, removing the organic solvent, crosslinking and curing the epoxy resin, cutting the epoxy resin in the thickness direction, and reversing the epoxy resin for 90 degrees to prepare the epoxy resin composite heat conducting sheet.
In one example, the magnetic field has a strength of 25 tesla to 50 tesla, and specifically, the magnetic field has a strength of 25 tesla, 26 tesla, 27 tesla, 28 tesla, 29 tesla, 30 tesla, 31 tesla, 32 tesla, 33 tesla, 34 tesla, 35 tesla, 36 tesla, 37 tesla, 38 tesla, 39 tesla, 40 tesla, 41 tesla, 42 tesla, 43 tesla, 44 tesla, 45 tesla, 46 tesla, 47 tesla, 48 tesla, 49 tesla, 50 tesla, and preferably, the magnetic field has a strength of 30 tesla to 40 tesla.
In one example, the magnetic field is applied by a magnetic field orienting device, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5.
In one example, the two sides of the electric heating plate 4 are provided with fixing brackets, and the fixing brackets are provided with fixing grooves which are electrically connected with a power supply.
In one example, when the two coils 2 and 3 are energized, a magnetic field is formed along the direction of the line connecting the centers of the two coils, and the magnetic field passes through a mold 5 which is arranged on an electric heating plate 4 and is filled with epoxy resin mixed dispersion liquid.
In one example, under the action of a magnetic field, the graphene is arranged along the direction of the magnetic field, i.e., in the horizontal direction.
In one example, when the electric heating plate is electrified and heated, the solvent is volatilized, and the epoxy resin is crosslinked and cured, so that the epoxy resin composite material in the horizontal orientation arrangement is obtained.
In one example, the mold 5 is made of stainless steel and has a molding groove, and the surface of the molding groove is plated with fluorine.
In one example, after the organic solvent is removed and the epoxy resin is cross-linked and cured, the method further includes the step of cutting the epoxy resin composite heat conduction sheet in the thickness direction.
In one example, the epoxy resin composite material is cut at equal intervals in the thickness direction and then inverted by 90 °.
In one example, the preparation method of the epoxy resin composite heat conducting sheet comprises the following steps:
1. mixing the laminated structure fluorinated graphene and epoxy resin with the number of layers of 5-20 and the sheet diameter of 5-20 microns with one or more organic solvents of ethanol, diethyl ether, isopropanol and acetone, stirring in vacuum until the mixture is uniformly dispersed, and adding one or more curing agents of ethylenediamine, tetramethylenediamine, hexamethylenediamine, diaminodiphenylmethane, m-phenylenediamine and phthalic anhydride to obtain the fluorinated graphene epoxy resin mixed dispersion liquid.
The fluorine content of the fluorinated graphene is 45 wt% -65 wt%.
The mass ratio of the fluorinated graphene to the epoxy resin is 1: (1-3).
The mass ratio of the curing agent to the epoxy resin is (0.4-0.6): 1.
the epoxy value of the epoxy resin is 0.25-0.45.
2. Transferring the graphene fluoride epoxy resin mixed dispersion liquid to a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, enabling the graphene fluoride to be arranged in an oriented mode along the horizontal direction under the action of a magnetic field with the strength of 25-50 Tesla, heating to enable the solvent to be completely volatilized, crosslinking and curing the epoxy resin, and demolding to obtain the graphene fluoride epoxy resin composite material.
The magnetic field is applied by a magnetic field orienting device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 is superposed with the central axis of the mould 5. After the two coils 2 and 3 are electrified, a magnetic field is formed along the central connection line direction of the two coils, and the magnetic field passes through a die 5 which is positioned on an electric hot plate 4 and is provided with graphene epoxy resin mixed dispersion liquid. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are arranged on the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine.
3. And cutting the fluorinated graphene epoxy resin composite material at equal intervals along the thickness direction, and then reversing the material for 90 degrees to prepare the epoxy resin composite heat conducting sheet.
An embodiment also provides an epoxy resin composite heat conducting sheet prepared by the preparation method of the epoxy resin composite heat conducting sheet.
In one example, the thickness of the epoxy resin composite heat conducting sheet is 2 mm to 6 mm.
In one example, the epoxy resin composite heat conducting sheet has a vertical heat conductivity of 4W/m.degree to 8W/m.degree.
According to the preparation method of the epoxy resin composite heat conducting sheet, fluorinated graphene and epoxy resin are used as raw materials, and the fluorinated graphene is arranged in an oriented mode under the action of a magnetic field, so that the heat conducting performance of the epoxy resin is improved more effectively, and the prepared epoxy resin composite heat conducting sheet has high heat conductivity. The material is used as a semiconductor chip packaging material, so that the heat conduction of the chip can be accelerated, and the heat dissipation problem of the chip can be solved.
The following are specific examples.
Example 1: preparation of epoxy resin composite heat-conducting fin
The preparation method of the epoxy resin composite heat-conducting fin comprises the following steps:
1. mixing 20 layers of lamellar structure fluorinated graphene with the diameter of 20 microns, epoxy resin and ethanol, stirring in vacuum until the mixture is uniformly dispersed, and adding curing agent ethylenediamine to obtain a fluorinated graphene epoxy resin mixed dispersion liquid with the solid content of 50 wt%;
The fluorine content of the fluorinated graphene is 45 wt%.
The mass ratio of the fluorinated graphene to the epoxy resin is 1: 3.
the epoxy value of the epoxy resin was 0.25.
The mass ratio of the curing agent to the epoxy resin is 0.4: 1.
2. transferring the graphene fluoride epoxy resin mixed dispersion liquid to a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, enabling the graphene fluoride to be arranged in an oriented mode along the horizontal direction under the action of a magnetic field with the strength of 25 Tesla, then heating for 6 hours at the temperature of 60 ℃, then heating for 4 hours at the temperature of 120 ℃, enabling the solvent to be completely volatilized, and enabling the epoxy resin to be crosslinked and cured, and demoulding to obtain the graphene fluoride epoxy resin composite material.
The magnetic field is applied by a magnetic field orientation device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 coincides with the central axis of the mould 5. After the two coils 2 and 3 are electrified, a magnetic field is formed along the central connection line direction of the two coils, and the magnetic field passes through a die 5 which is positioned on an electric hot plate 4 and is provided with graphene epoxy resin mixed dispersion liquid. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are formed in the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine.
3. And (3) cutting the fluorinated graphene epoxy resin composite material at equal intervals of 2 mm in the thickness direction, and then reversing the cut material by 90 degrees to obtain the fluorinated graphene epoxy resin composite heat conducting sheet with the thickness of 2 mm.
Example 2: preparation of epoxy resin composite heat-conducting fin
The preparation method of the epoxy resin composite heat-conducting fin comprises the following steps:
1. mixing 5 layers of fluorinated graphene with a lamellar structure and a sheet diameter of 5 microns, epoxy resin and acetone, stirring in vacuum until the mixture is uniformly dispersed, and adding hexamethylene diamine serving as a curing agent to obtain a fluorinated graphene epoxy resin mixed dispersion liquid with a solid content of 50 wt%;
the fluorine content of the fluorinated graphene is 65 wt%.
The mass ratio of the fluorinated graphene to the epoxy resin is 1: 1.
the epoxy value of the epoxy resin was 0.45.
The mass ratio of the curing agent to the epoxy resin is 0.6: 1.
2. transferring the graphene fluoride epoxy resin mixed dispersion liquid to a magnetic field orientation device, carrying out orientation treatment in the horizontal direction, enabling the graphene fluoride to be arranged in an oriented mode along the horizontal direction under the action of a magnetic field with the strength of 50 Tesla, then heating for 6 hours at the temperature of 60 ℃, then heating for 4 hours at the temperature of 120 ℃, enabling the solvent to be completely volatilized, and enabling the epoxy resin to be crosslinked and cured, and demoulding to obtain the graphene fluoride epoxy resin composite material.
The magnetic field is applied by a magnetic field orienting device shown in fig. 1, which comprises a power supply 1, two coils 2 and 3 connected with the power supply and distributed at intervals, an electric heating plate 4 positioned between the two coils 2 and 3, and a mold 5 placed on the electric heating plate 4; the two coils 2 and 3 have the same radius and are arranged oppositely; the central connecting line of the two coils 2 and 3 coincides with the central axis of the mould 5. Two coils 2 and 3 can form the magnetic field along two coil central connecting line directions after the circular telegram, and the magnetic field is through being equipped with graphite alkene epoxy mixed dispersion's mould 5 on lieing in electric plate 4. The two sides of the electric heating plate 4 are provided with fixing supports, fixing grooves are arranged on the fixing supports, and the fixing grooves are electrically connected with a power supply. The die 5 is made of stainless steel and is provided with a forming groove, and the surface of the forming groove is plated with fluorine.
3. And (3) cutting the fluorinated graphene epoxy resin composite material at equal intervals of 6 mm in the thickness direction, and then reversing the cut material by 90 degrees to obtain the fluorinated graphene epoxy resin composite heat conducting sheet with the thickness of 6 mm.
Comparative example 1
1. Mixing 20 layers of lamellar structure fluorinated graphene with the diameter of 20 microns, epoxy resin and ethanol, stirring in vacuum until the mixture is uniformly dispersed, and adding curing agent ethylenediamine to obtain a fluorinated graphene epoxy resin mixed dispersion liquid with the solid content of 50 wt%;
The fluorine content of the fluorinated graphene is 45 wt%.
The mass ratio of the fluorinated graphene to the epoxy resin is 1: 3.
the epoxy value of the epoxy resin was 0.25.
The mass ratio of the curing agent to the epoxy resin is 0.4: 1.
2. heating the graphene fluoride epoxy resin mixed dispersion liquid at 60 ℃ for 6 hours, heating at 120 ℃ for 4 hours to completely volatilize the solvent and crosslink and solidify the epoxy resin, and demolding to obtain the graphene fluoride epoxy resin composite material.
3. And (3) cutting the fluorinated graphene epoxy resin composite material at equal intervals of 2 mm in the thickness direction, and then reversing the cut material by 90 degrees to obtain the fluorinated graphene epoxy resin composite heat conducting sheet with the thickness of 2 mm.
Comparative example 2
1. Mixing 5 layers of fluorinated graphene with a lamellar structure and a sheet diameter of 5 microns, epoxy resin and acetone, stirring in vacuum until the mixture is uniformly dispersed, and adding hexamethylene diamine serving as a curing agent to obtain a fluorinated graphene epoxy resin mixed dispersion liquid with a solid content of 50 wt%;
the fluorine content of the fluorinated graphene is 65 wt%.
The mass ratio of the fluorinated graphene to the epoxy resin is 1: 1.
the epoxy value of the epoxy resin was 0.45.
The mass ratio of the curing agent to the epoxy resin is 0.6: 1.
2. heating the graphene fluoride epoxy resin mixed dispersion liquid at 60 ℃ for 6 hours, heating at 120 ℃ for 4 hours to completely volatilize the solvent and crosslink and solidify the epoxy resin, and demolding to obtain the graphene fluoride epoxy resin composite material.
3. And (3) cutting the fluorinated graphene epoxy resin composite material at equal intervals of 6 mm in the thickness direction, and then reversing the cut material by 90 degrees to obtain the fluorinated graphene epoxy resin composite heat conducting sheet with the thickness of 6 mm.
The fluorinated graphene epoxy resin composite heat conducting sheet prepared in the examples 1 to 2 and the comparative examples 1 to 2 was subjected to thickness and heat conductivity coefficient tests, and the test results are shown in the following table 1. Wherein, the test standard of the thermal conductivity test is ASTM E1461.
TABLE 1 thickness and thermal conductivity test results
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 more specific and detailed, but not construed 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 should be subject to the appended claims.
Claims (10)
1. The preparation method of the epoxy resin composite heat-conducting fin is characterized by comprising the following steps of:
mixing fluorinated graphene, epoxy resin, a curing agent and an organic solvent to prepare a fluorinated graphene epoxy resin mixed dispersion liquid;
and (2) carrying out vacuum defoaming on the fluorinated graphene epoxy resin mixed dispersion liquid, then placing the dispersion liquid in a magnetic field, carrying out orientation treatment in the horizontal direction, removing the organic solvent, crosslinking and curing the epoxy resin, cutting the epoxy resin in the thickness direction, and reversing the epoxy resin by 90 degrees to prepare the epoxy resin composite heat conducting sheet.
2. The method for preparing an epoxy resin composite heat conducting sheet according to claim 1, wherein the fluorinated graphene is a sheet-structured fluorinated graphene having 5 to 20 layers; and/or the sheet diameter of the fluorinated graphene is 5-20 micrometers.
3. The method for preparing an epoxy resin composite heat conductive sheet according to claim 2, wherein the fluorine element content of the fluorinated graphene is 45 wt% to 65 wt%.
4. The method for preparing the epoxy resin composite heat conducting sheet according to claim 1, wherein the mass ratio of the fluorinated graphene to the epoxy resin is 1: (1-3); and/or the epoxy value of the epoxy resin is 0.25-0.45.
5. The method for preparing an epoxy resin composite heat conducting sheet according to claim 1, wherein the organic solvent includes one or more of ethanol, diethyl ether, isopropyl alcohol and acetone.
6. The method for preparing an epoxy resin composite heat conductive sheet according to claim 1, wherein the curing agent is one or more of ethylenediamine, tetramethylenediamine, hexamethylenediamine, diaminodiphenylmethane, m-phenylenediamine, and phthalic anhydride; and/or the mass ratio of the curing agent to the epoxy resin is (0.4-0.6): 1.
7. the method of claim 1, wherein the magnetic field has a strength of 25 tesla to 50 tesla.
8. The method for preparing an epoxy resin composite heat conducting sheet according to any one of claims 1 to 7, wherein the magnetic field is applied by a magnetic field orienting device comprising a power supply (1), two coils (2) and (3) connected to the power supply and spaced apart from each other, an electric heating plate (4) disposed between the two coils (2) and (3), and a mold (5) disposed on the electric heating plate (4); the two coils (2) and (3) have the same radius and are arranged oppositely; the central connecting line of the two coils (2) and (3) is superposed with the central axis of the mould (5); when the orientation treatment is performed, the epoxy resin mixed dispersion liquid is placed in a molding groove of the mold (5).
9. An epoxy resin composite heat-conducting sheet, characterized by being produced by the method for producing an epoxy resin composite heat-conducting sheet according to any one of claims 1 to 8.
10. The epoxy resin composite heat conductive sheet according to claim 9, wherein the thickness of the epoxy resin composite heat conductive sheet is 2 to 6 mm; and/or the vertical thermal conductivity of the epoxy resin composite heat conducting sheet is 4W/m.degree to 8W/m.degree.
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