CN108070214A - A kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof - Google Patents
A kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof Download PDFInfo
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- CN108070214A CN108070214A CN201611011687.4A CN201611011687A CN108070214A CN 108070214 A CN108070214 A CN 108070214A CN 201611011687 A CN201611011687 A CN 201611011687A CN 108070214 A CN108070214 A CN 108070214A
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
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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
- C08L2312/00—Crosslinking
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Abstract
The invention discloses a kind of epoxy resin-matrix high heat-conductivity conducting composite materials and preparation method thereof, are prepared including following parts by weight raw material：30 60 parts of epoxy resin, 5 10 parts of vinyl butyl ether, 10 25 parts of polypyrrole, 25 parts of sodium sulfonate, 25 parts of nano aluminium oxide, 36 parts of carbon nano-fiber, 25 parts of nano-graphite, 13 parts of coupling agent, 15 parts of crosslinking agent；The present invention is made composite material have the advantages of heat conduction constant is big, and electric conductivity is high, is promoted application of the thermal conductivity composite material on rapid cooling electronic device is needed using polymer crosslinking and organic inorganic hybridization principle.
Description
Technical field
The present invention relates to field of electronic materials, and in particular to a kind of epoxy resin-matrix high heat-conductivity conducting composite material and its system
Preparation Method.
Background technology
The circuit design of electronic product becomes increasingly complex at present, in densification, trend toward miniaturization.These electronic and electrical equipments
Amount of heat can be generated, if these heats cannot discharge in time, accumulation to a certain extent will certainly be to the component of electronic apparatus
And equipment damages in itself.So the waste heat that must be generated is timely, is efficiently transferred in ambient enviroment.
Traditional metal material in heat dissipation industry, because the geometry of its product is very limited, and such radiator and electricity
Subcomponent surface is there are certain interval, so as to more and more easily be substituted by some thermal interfacial materials.
High molecular material electrical insulation capability is excellent, but thermal conductivity factor is very low, generally 0.2W/m.K, is only metal material
1 percent to one thousandth.There should be high heat conduction for some while the application scenario of conductive requirement is compared at present again
More conventional method is filler (metal, carbon etc.) of the addition with high thermal conductivity coefficient and high conductivity in polymer-based material.
But the material prepared in this way, since a large amount of additions of heat filling make the electric conductivity of composite material receive seriously
Damage, while the raising of thermal conductivity also not significantly, be generally hardly higher than 2W/m.K.It is dissipated for LED radiator, electric appliance
Hot device etc. needs the situation using radiator area flash heat transfer, if the thermal conductivity factor of material is small, in the longitudinal direction
Heat transfer with regard to extremely difficult, heat, which is all concentrated in the region of very little, to spread, and cause the effective area of radiator not have
It makes full use of, affects radiating efficiency.
The content of the invention
It is an object of the invention to overcome, thermal conductivity factor existing for existing thermal conductivity composite material is low, electric conductivity is poor
Defect provides a kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof；The present invention utilizes polymer crosslinking
With hybrid inorganic-organic principle, it is big to make it have thermal conductivity factor, the advantages of conducting electricity very well, promotes thermal conductivity material and exists
Need the application on the electronic device of rapid cooling.
In order to realize foregoing invention purpose, the present invention provides a kind of epoxy resin-matrix high heat-conductivity conducting composite material, bags
Following parts by weight raw material are included to be prepared：30-60 parts of epoxy resin, 5-10 parts of vinyl butyl ether, 10-25 parts poly-
Pyrroles, 2-5 parts of sodium sulfonate, 2-5 parts of nano aluminium oxide, 3-6 parts of carbon nano-fiber, 2-5 parts of nano-graphite, 1-3 parts
Coupling agent, 1-5 parts of crosslinking agent.
A kind of epoxy resin-matrix high heat-conductivity conducting composite material using the polymerization that is cross-linked with each other of gas chromatography, forms knot
Structure is stablized, the excellent polymer three-dimensional network structure of electric conductivity, while the hydridization difference thermal conductivity in three-dimensional net structure
Material, aluminium oxide-carbon fiber-graphite three form a three-dimensional radiation conductive structure, and electric conductivity and radiating rate increase, lead
Electrical conductivity can increase；Meanwhile three-dimensional net structure increases mechanical properties of polymer, operating temperature higher；The heat conduction is led
Composite use scope bigger, is conducive to the development of electronics industry.
Preferably, wherein the polymerization of epoxy resins degree is 200-500, the degree of polymerization is too big, and strand is too long, formation
It is poor that three-dimensional net structure is stablized, and composite material fusing point reduces；The degree of polymerization is too small, and strand is too short, is unfavorable for thermal conductivity material
Hydridization and insertion, thermal conductivity material disperse irregularly, it is possible to create agglomeration, product thermal conductivity reduce.
Preferably, wherein the polypyrrole degree of polymerization is 40-80, the degree of polymerization is too big, and strand is too long, the three-dimensional of formation
It is poor that network structure is stablized, and composite materials property reduces；The degree of polymerization is too small, and strand is too short, is unfavorable for thermal conductivity material
Hydridization and insertion, thermal conductivity material disperse irregularly, it is possible to create agglomeration, product thermal conductivity reduce.
Preferably, wherein the grain size of the nano aluminium oxide is 20-60 nanometers, grain size is too big, is unfavorable for thermal conductivity
The hydridization in three-dimensional net structure and insertion, thermal conductivity material of material are disperseed irregularly, it is possible to create agglomeration, production
Product thermal conductivity reduces, and grain size is too small, difficulties in dispersion, easily reunites.
Preferably, wherein a diameter of 2-5nm of the carbon nano-fiber, length 10-50nm, diameter and length are too
Greatly, the hydridization in three-dimensional net structure and insertion, thermal conductivity material for being unfavorable for thermal conductivity material are disperseed irregularly, can
Agglomeration can be generated, product thermal conductivity reduces, and a diameter of 2-5nm, length is too small for 10-50nm, difficulties in dispersion, holds
Easily reunite, it is difficult to the three-dimensional heat dissipation system of structure.
Preferably, wherein the grain size of the nano-graphite is 20-50 nanometers, grain size is too big, is unfavorable for thermal conductivity material
The hydridization in three-dimensional net structure and insertion, thermal conductivity material of material are disperseed irregularly, it is possible to create agglomeration, product
Thermal conductivity reduces, and grain size is too small, difficulties in dispersion, easily reunites.
Preferably, wherein the coupling agent is silane coupling agent, silane coupling agent imitates the coupling of thermal conductivity material
Fruit is best.
Preferably, a kind of epoxy resin-matrix high heat-conductivity conducting composite material is prepared including following parts by weight raw material
It forms：40-50 parts of epoxy resin, 5-8 parts of vinyl butyl ether, 15-20 parts of polypyrrole, 2-3 parts of sodium sulfonate, 2-3
Part nano aluminium oxide, 2-3 parts of carbon nano-fiber, 4-6 parts of nano-graphite, 1-2 parts of coupling agent, 2-3 parts of crosslinking agent.
In order to realize foregoing invention purpose, further, the present invention provides a kind of epoxy resin-matrix high heat-conductivity conductings to answer
The preparation method of condensation material, comprises the following steps：
（1）Nano aluminium oxide, carbon nano-fiber, nano-graphite are dispersed in vinyl butyl ether and form suspension；
（2）The suspension that step 1 is obtained is esterified with sodium sulfonate, coupling agent, coupling reaction, obtains the positive fourth of sodium sulfonate vinyl
Ether-ether hybridized mixed object；
（3）Sodium sulfonate vinyl butyl ether ester hybridized mixed object and epoxy resin, polypyrrole, crosslinking agent that step 2 obtains are mixed
Cross-linking reaction is carried out after conjunction, obtains epoxy resin-matrix high heat-conductivity conducting composite material.
A kind of preparation method of epoxy resin-matrix high heat-conductivity conducting composite material, first passes through vinyl by thermal conductivity material
N-butyl ether uniformly disperses out, and esterification and coupling agent is recycled to be coupled the ester of synthesis and thermal conductivity material, forms sulfonic acid
Sodium vinyl butyl ether ester hybridized mixed object, so that the arrangement of the uniform rule of thermal conductivity material is dispersed in three-dimensional net structure
In, it will not reunite, and aluminium oxide-carbon fiber-graphite three-dimensional radiation conductive structure is formed, electric conductivity and radiating rate increase,
Thermal conductivity increases；Finally by the crosslinking with other high molecular materials, the epoxy with three-dimensional net structure is formd
Resin base high heat-conductivity conducting composite material, increases mechanical properties of polymer, operating temperature higher；The epoxy resin-matrix height is led
The preparation method of thermal conductivity composite is simple, stablizes, is reliable, is suitble to the big rule of epoxy resin-matrix high heat-conductivity conducting composite material
Mould, industrialized production.
Preferably, the esterification reaction temperature is 120-150 DEG C, and reaction temperature is excessively high, and reaction is violent, and control is difficult, instead
Answer temperature too low, reaction speed is slow, and the production cycle is long.
Preferably, the reaction time of esterification is 2-5h, and the reaction time is long, and the production cycle is long, and efficiency is low, the reaction time
Too short, reaction is incomplete, and product thermal conductivity reduces.
Preferably, the cross-linking reaction temperature is 180-250 DEG C, and crosslinking temperature is excessively high, is crosslinked transition, the three dimensional network of formation
Network irregular structure, properties of product reduce, and crosslinking temperature is too low, and the reaction time is too long, and the production cycle is long.
Preferably, the time of the cross-linking reaction is 1-3h, and the reaction time is long, and the production cycle is long, and efficiency is low, during reaction
Between it is too short, reaction is incomplete, and product thermal conductivity reduces.
Compared with prior art, beneficial effects of the present invention：
1st, epoxy resin-matrix high heat-conductivity conducting composite material of the present invention contains three-dimensional net structure and aluminium oxide-carbon fiber-graphite
Three-dimensional radiation conductive structure has higher thermal conductivity.
2nd, the preparation method of epoxy resin-matrix high heat-conductivity conducting composite material of the present invention first passes through esterification and hydridization, recycles
Crosslinking, by thermal conductivity material Monodispersed in three-dimensional net structure system, dissipates into aluminium oxide-carbon fiber-graphite three-dimensional parallel
Thermal conducting structure, so as to add the radiating rate of composite material and electric conductivity.
3rd, the preparation method of epoxy resin-matrix high heat-conductivity conducting composite material of the present invention is simple, stablizes, is reliable, is suitble to epoxy
Extensive, the industrialized production of resin base high heat-conductivity conducting composite material.
Specific embodiment
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）The nano-graphite of the nano aluminium oxide of 3 parts by weight, the carbon nano-fiber of 5 parts by weight, 4 parts by weight is dispersed in 10 weights
It measures in the vinyl butyl ether of part and forms solution；
（2）Solution and the sodium sulfonate of 3 parts by weight that step 1 is obtained, the silane coupling agent of 2 parts by weight are under conditions of 120 DEG C
It is esterified, coupling reaction 5h, obtains sodium sulfonate vinyl butyl ether ester hybridized mixed object；
（3）The sodium sulfonate vinyl butyl ether ester hybridized mixed object and the degree of polymerization of 20 parts by weight that step 2 is obtained are 200 ring
Oxygen resin, the degree of polymerization of 5 parts by weight are 40 polypyrrole, are handed over after the crosslinking agent mixing of 2 parts by weight at a temperature of 180 DEG C
Connection reaction 3h, obtains epoxy resin-matrix high heat-conductivity conducting composite material.
Embodiment 2
（1）The nano-graphite of the nano aluminium oxide of 2 parts by weight, the carbon nano-fiber of 3 parts by weight, 6 parts by weight is dispersed in 5 weight
Solution is formed in the vinyl butyl ether of part；
（2）The solution that step 1 obtains and the sodium sulfonate of 2 parts by weight, the coupling agent of 1 parts by weight are carried out at a temperature of 150 DEG C
Esterification, coupling reaction 2h, obtain sodium sulfonate vinyl butyl ether ester hybridized mixed object；
（3）The sodium sulfonate vinyl butyl ether ester hybridized mixed object and the degree of polymerization of 15 parts by weight that step 2 is obtained are 500 ring
Oxygen resin, the degree of polymerization of 10 parts by weight are 80 polypyrrole, are carried out after the crosslinking agent mixing of 3 parts by weight at a temperature of 250 DEG C
Cross-linking reaction 1h obtains epoxy resin-matrix high heat-conductivity conducting composite material.
Embodiment 3
（1）The nano-graphite of the nano aluminium oxide of 2 parts by weight, the carbon nano-fiber of 3 parts by weight, 5 parts by weight is dispersed in 5 weight
Solution is formed in the vinyl butyl ether of part；
（2）Solution and the sodium sulfonate of 5 parts by weight, the coupling agent of 1 parts by weight that step 1 is obtained are esterified, coupling reaction, are obtained
Sodium sulfonate vinyl butyl ether ester hybridized mixed object；
（3）The sodium sulfonate vinyl butyl ether ester hybridized mixed object and the epoxy resin of 30 parts by weight that step 2 is obtained, 10 weight
The polypyrrole of part carries out cross-linking reaction after the crosslinking agent mixing of 1 parts by weight, obtains epoxy resin-matrix high heat-conductivity conducting composite material.
Embodiment 4
（1）The nano-graphite of the nano aluminium oxide of 5 parts by weight, the carbon nano-fiber of 5 parts by weight, 3 parts by weight is dispersed in 15 weights
It measures in the vinyl butyl ether of part and forms solution；
（2）Solution and the sodium sulfonate of 2 parts by weight, the coupling agent of 3 parts by weight that step 1 is obtained are esterified, coupling reaction, are obtained
Sodium sulfonate vinyl butyl ether ester hybridized mixed object；
（3）The sodium sulfonate vinyl butyl ether ester hybridized mixed object and the epoxy resin of 60 parts by weight that step 2 is obtained, 5 weight
The polypyrrole of part carries out cross-linking reaction after the crosslinking agent mixing of 1 parts by weight, obtains epoxy resin-matrix high heat-conductivity conducting composite material.
Claims (10)
1. a kind of thermal conductivity composite material, which is characterized in that be prepared including following parts by weight raw material：30-60 parts
Epoxy resin, 5-10 parts of vinyl butyl ether, 10-25 parts of polypyrrole, 2-5 parts of sodium sulfonate, 2-5 parts nano oxidized
Aluminium, 3-6 parts of carbon nano-fiber, 2-5 parts of nano-graphite, 1-3 parts of coupling agent, 1-5 parts of crosslinking agent.
2. thermal conductivity composite material according to claim 1, which is characterized in that the polymerization of epoxy resins degree is 200-
500。
3. thermal conductivity composite material according to claim 1, which is characterized in that the polypyrrole degree of polymerization is 40-80.
4. thermal conductivity composite material according to claim 1, which is characterized in that the grain size of the nano aluminium oxide is
20-60nm。
5. thermal conductivity composite material according to claim 1, which is characterized in that a diameter of 2- of the carbon nano-fiber
5nm, length 10-50nm.
6. thermal conductivity composite material according to claim 1, which is characterized in that the grain size of the graphite is 20-50nm.
7. thermal conductivity composite material according to claim 1, which is characterized in that prepared including following parts by weight raw material
It forms：40-50 parts of epoxy resin, 5-8 parts of vinyl butyl ether, 15-20 parts of polypyrrole, 2-3 parts of sodium sulfonate, 2-3
Part nano aluminium oxide, 2-3 parts of carbon nano-fiber, 4-6 parts of nano-graphite, 1-2 parts of coupling agent, 2-3 parts of crosslinking agent.
8. the preparation method of thermal conductivity composite material described in a kind of claim 1, which is characterized in that comprise the following steps：
（1）Nano aluminium oxide, carbon nano-fiber, nano-graphite are dispersed in vinyl butyl ether and form suspension；
（2）The suspension that step 1 is obtained is esterified with sodium sulfonate, coupling agent, coupling reaction, obtains the positive fourth of sodium sulfonate vinyl
Ether-ether hybridized mixed object；
（3）Sodium sulfonate vinyl butyl ether ester hybridized mixed object and epoxy resin, polypyrrole, crosslinking agent that step 2 obtains are mixed
Cross-linking reaction is carried out after conjunction, obtains epoxy resin-matrix high heat-conductivity conducting composite material.
9. preparation method according to claim 8, which is characterized in that esterification reaction temperature is 120-150 DEG C in step 2,
Time is 2-5h.
10. preparation method according to claim 8, which is characterized in that cross-linking reaction temperature is 180-250 DEG C in step 3,
Time is 1-3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611011687.4A CN108070214A (en) | 2016-11-17 | 2016-11-17 | A kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611011687.4A CN108070214A (en) | 2016-11-17 | 2016-11-17 | A kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108070214A true CN108070214A (en) | 2018-05-25 |
Family
ID=62163330
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611011687.4A Withdrawn CN108070214A (en) | 2016-11-17 | 2016-11-17 | A kind of epoxy resin-matrix high heat-conductivity conducting composite material and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN108070214A (en) |
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2016
- 2016-11-17 CN CN201611011687.4A patent/CN108070214A/en not_active Withdrawn
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