CN108485206A - A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application - Google Patents
A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application Download PDFInfo
- Publication number
- CN108485206A CN108485206A CN201810281686.4A CN201810281686A CN108485206A CN 108485206 A CN108485206 A CN 108485206A CN 201810281686 A CN201810281686 A CN 201810281686A CN 108485206 A CN108485206 A CN 108485206A
- Authority
- CN
- China
- Prior art keywords
- graphene
- interfacial material
- composite heat
- raw material
- heat interfacial
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08L63/10—Epoxy resins modified by unsaturated compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention relates to a kind of composite heat interfacial material of graphene-containing and preparation method thereof, applications.The first aspect of the invention provides a kind of composite heat interfacial material of graphene-containing, and the composite heat interfacial material of the graphene-containing prepares raw material, in parts by weight, includes at least following raw material：100 parts of epoxy vinyl ester resin；50~100 parts of vinylsiloxane rubber；100~130 parts of graphite；1~10 part of graphene.The second aspect of the invention provides a kind of preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：(1) epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added in toluene solvant, reaction temperature are increased to 80 DEG C, reaction obtains product after 3 hours；(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then sizing material is subjected to tension and compression, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
Description
Technical field
The invention belongs to Heat Conduction Material fields, more particularly it relates to a kind of composite heat interfacial material of graphene-containing
Material and preparation method thereof, application.
Background technology
Heat-conducting interface material is also interface Heat Conduction Material.It is a kind of material being commonly used to IC package and electronic radiation, it is main
It is used to fill up the hole of the microvoid and surface irregularity that are generated when two kinds of material engagements or contact, reduces heat transfer resistance,
Improve heat dissipation performance.
Traditional heat-conducting interface material is mainly with heat conduction particle filled polymer or grease, composition thermal grease conduction, heat conduction
A few class boundary materials such as adhesive, heat conductive rubber and phase-change material.Its filler packing volume requires very big (about 70%), Cai Nengda
It is 1~5W/ (mK) to thermal coefficient at room temperature.Thus for the demand of better interface Heat Conduction Material and more high thermal conductivity fillers
It is increasingly urgent to.
But the conductor thermal conductivity of most of high molecular material is relatively low.So general use fills one into high molecular material
The heat filling of a little roads good in thermal property, prepares Polymer composite heat conduction material.Heat filling mainly include metal powder such as Al,
Cu, Ag etc., metal oxide such as Al2O3, MgO etc., nitride such as BN etc. and carbon material such as carbon black, graphite, carbon fiber, carbon are received
Mitron etc..
Thus, it is also very desirable to by the improvement of formula and technique, to obtain a kind of composite heat interfacial material of graphene-containing
Material.
Invention content
To solve the above-mentioned problems, the first aspect of the invention provides a kind of composite heat interfacial material of graphene-containing
Material, the composite heat interfacial material of the graphene-containing prepare raw material, in parts by weight, include at least following raw material：
As a kind of preferred technical solution in the present invention, the preparation of the composite heat interfacial material of the graphene-containing is former
Material includes at least following raw material in parts by weight：
As a kind of preferred technical solution in the present invention, the preparation of the composite heat interfacial material of the graphene-containing is former
Material includes at least following raw material in parts by weight：
As a kind of preferred technical solution of the present invention, the graphite is crystalline flake graphite.
As a kind of preferred technical solution of the present invention, the graphene is modified graphene.
As a kind of preferred technical solution of the present invention, the composite heat interfacial material of the graphene-containing prepares raw material
Further include vinyl norbornene base capped polyimides.
As a kind of preferred technical solution of the present invention, the epoxy vinyl ester resin and vinyl norbornene base
Weight ratio between capped polyimides is 100：(1~8).
As a kind of preferred technical solution of the present invention, the composite heat interfacial material of the graphene-containing prepares raw material
Further include functionalized multi-wall carbonnanotubes.
The second aspect of the invention provides a kind of preparation method of the thermal interfacial material of graphene-containing, include at least with
Lower step：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The third aspect of the invention provides a kind of graphene heat conductive pad, and the graphene heat conductive pad contains stone by above-mentioned
The thermal interfacial material of black alkene is prepared.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to following detailed description.
Specific implementation mode
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention
The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim be closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to the element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
Singulative includes that plural number discusses object, unless the context clearly dictates otherwise." optional " or it is " arbitrary
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, and it is specific to indicate that the present invention is not limited to this
Quantity further includes the modified part of the acceptable change without lead to related basic function close to the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, approximate
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, range limits can be with
Combination and/or exchange, these ranges include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. occurrence number) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the apparent purport of the quantity refers to singulative.
" polymer " means the polymerizable compound prepared by the monomer by the identical or different type of polymerization.Generic term
" polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " copolymer ".
" copolymer " means the polymer prepared by polymerizeing at least two different monomers.Generic term " copolymer " includes
(it is general with term " terpolymer " for term " copolymer " (its generally to refer to the polymer prepared by two kinds of different monomers)
To refer to the polymer prepared by three kinds of different monomers).It also includes the polymerization manufactured by polymerization four or more monomer
Object." blend " means the polymerization that two or more polymer is formed by mixing jointly by physics or chemical method
Object.
To solve the above-mentioned problems, the first aspect of the invention provides a kind of composite heat interfacial material of graphene-containing
Material, the composite heat interfacial material of the graphene-containing prepare raw material, in parts by weight, include at least following raw material：
In a preferred embodiment, the composite heat interfacial material of the graphene-containing prepares raw material, with weight
Part meter, includes at least following raw material：
In a preferred embodiment, the composite heat interfacial material of the graphene-containing prepares raw material, with weight
Part meter, includes at least following raw material：
Epoxy vinyl ester resin
Epoxy vinyl ester resin in the application is commercially available acquisition, is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s.
Vinylsiloxane rubber
Vinylsiloxane rubber in the application is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available obtains
, it is purchased from Ningbo Dao Ruo organosilicons Co., Ltd.
Graphite
Graphite in the application is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd.
Graphene
Graphene in the application is commercially available to be obtained by self-control.
In a preferred embodiment, the graphene is modified graphene.
In a preferred embodiment, it is modified to be that graphene first passes through dopamine for the modified graphene, obtains
Dopamine modified graphene；Then dopamine modified graphene is modified again with the silane coupling agent containing double bond again.
After term " modified graphene " refers to dopamine modified graphene, by the silane coupling agent containing double bond to more
Bar amine modified graphene is modified.
Wherein, amino is obtained in dopamine to connect with the carboxyl on graphene, DOPA amine layer is obtained on the surface of graphene,
Then the hydroxyl in DOPA amine layer is attached again with the silane coupling agent containing double bond, obtains modified graphene.
In a preferred embodiment, in the dopamine modified graphene, the weight between dopamine and graphene
Measuring ratio is：1：1.
In a preferred embodiment, the weight ratio between the silane coupling agent and graphene containing double bond
For：1：5.
The silane coupling agent containing double bond is vinyl three (2- methoxy ethoxies) silane.
In a preferred embodiment, the preparation method of the modified graphene is：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
In a preferred embodiment, the raw material for preparing of the composite heat interfacial material of the graphene-containing further includes second
Alkenyl norbornene base capped polyimides.
In a preferred embodiment, the epoxy vinyl ester resin and vinyl norbornene base block polyamides
Weight ratio between imines is 100：(1~8).
In the application, the vinyl norbornene base capped polyimides are commercially available acquisition, are purchased from Yangzhong City Lutao rubber
Mould Co., Ltd.
The second aspect of the invention provides a kind of preparation method of the thermal interfacial material of graphene-containing, include at least with
Lower step：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
In a preferred embodiment, the initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
The third aspect of the invention provides a kind of graphene heat conductive pad, and the graphene heat conductive pad contains stone by above-mentioned
The thermal interfacial material of black alkene is prepared.
Hereinafter, the present invention is explained in more detail by embodiment, it should be appreciated that these embodiments are only
It is exemplary and not restrictive.If raw materials used to be all commercially available without other explanations.
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
Embodiment 1 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 2
Embodiment 2 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 3
Embodiment 3 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 4
Embodiment 4 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 5
Embodiment 5 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) that the epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added to toluene is molten
In agent, reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 6
Embodiment 6 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) epoxy vinyl ester resin of corresponding parts by weight, vinylsiloxane rubber, vinyl norbornene base are blocked poly-
Acid imide and initiator are added in toluene solvant, reaction temperature are increased to 100 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then by sizing material
Tension and compression are carried out, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Embodiment 7
Embodiment 7 provides a kind of composite heat interfacial material of graphene-containing, the composite heat interfacial material of the graphene-containing
Material prepares raw material, in parts by weight, includes at least following raw material：
The epoxy vinyl ester resin is purchased from Wuxi City Pin Hua Chemical Co., Ltd.s；
The vinylsiloxane rubber is methyl vinyl silicone rubber, and the methyl vinyl silicone rubber is commercially available acquisition, purchase
In Ningbo Dao Ruo organosilicons Co., Ltd；
The graphite is crystalline flake graphite, and the crystalline flake graphite is purchased from Qingdao day and reaches graphite Co., Ltd；
The graphene is modified graphene；
The preparation method of the modified graphene at least includes the following steps：
(1) Dopamine hydrochloride of the graphene of 100g and 100g are added in blender, then add 300mL three are sweet
The ethanol solution of alcoholic solution and 200mL is adopted after being then stirred by ultrasonic 12 hours at room temperature and is washed with deionized 3 times, second
After alcohol washs 3 times, dopamine modified graphene is obtained；
(2) the dopamine modified graphene obtained in step (1) is dissolved in the deionized water of 100mL, is then added
Vinyl three (2- methoxy ethoxies) silane of 15mL, is then stirred at room temperature 24 hours, adopts and be washed with deionized 3 times
Afterwards, modified graphene is obtained.
The preparation method of the thermal interfacial material of graphene-containing, at least includes the following steps：
(1) epoxy vinyl ester resin of corresponding parts by weight, vinylsiloxane rubber, vinyl norbornene base are blocked poly-
Acid imide and initiator are added in toluene solvant, reaction temperature are increased to 100 DEG C, reaction obtains product after 3 hours；
(2) graphite, graphene, functionalized multi-wall carbonnanotubes are added in the product into step (1) to be mixed,
Obtain sizing material；Then sizing material is subjected to tension and compression, rolls and cuts, obtain the thermal interfacial material of graphene-containing.
The initiator is benzoyl peroxide；
Weight ratio between the epoxy vinyl ester resin and benzoyl peroxide is 100：1.
Comparative example 1
Specific formula is with embodiment 5, the difference lies in that preparing in raw material for the composite heat interfacial material of graphene-containing is not wrapped
Include epoxy vinyl ester resin.
Comparative example 2
Specific formula is with embodiment 5, the difference lies in that preparing in raw material for the composite heat interfacial material of graphene-containing is not wrapped
Include vinylsiloxane rubber.
Comparative example 3
Specific formula is with embodiment 5, the difference lies in that not including epoxy vinyl ester resin and vinyl silicon rubber simultaneously
Glue.
Comparative example 4
Specific formula is with embodiment 5, the difference lies in that modified graphene is changed to graphene.
Comparative example 5
Specific formula is with embodiment 5, the difference lies in that modified graphene is changed to graphene oxide.
Comparative example 6
Specific formula is with embodiment 5, the difference lies in that modified graphene is changed to ammonification graphene.
Comparative example 7
Specific formula is with embodiment 5, the difference lies in that modified graphene is changed to carboxylated graphene.
Comparative example 8
Specific formula is with embodiment 5, the difference lies in that modified graphene is changed to dopamine modified graphene, i.e., not
It needs using containing the silane coupler modified of double bond.
Comparative example 9
Specific formula is with embodiment 5, the difference lies in that dopamine modified graphene is replaced with dopamine and graphene
It is simply mixed.
Comparative example 10
Specific formula is with embodiment 7, the difference lies in that functionalized multi-wall carbonnanotubes are replaced with single-walled carbon nanotube.
Comparative example 11
Specific formula is with embodiment 7, the difference lies in that functionalized multi-wall carbonnanotubes are replaced with amination multi wall carbon
Pipe.
Comparative example 12
Specific formula is with embodiment 7, the difference lies in that functionalized multi-wall carbonnanotubes are replaced with carbon fiber.
Performance test：
It is longitudinal to carry out test for the film that composite heat interfacial material in embodiment and comparative example is cut into the thickness of 3mm
Thermal conductivity；Longitudinal thermal conductivity measuring apparatus：LFA467, NETZSCH, Germany；Measurement standard：ASTM E1461.
Compression ratio：Measuring apparatus：UTM, 5567A, Instron, the U.S.；Measurement standard：GB1040-92.
Specific test result is shown in Table 1：
1 performance evaluation of table
The composite heat interfacial material of graphene-containing in the application has higher thermal conductivity and compression ratio, meanwhile, also have
There is lower conductivity, there is extraordinary insulation performance.Its working environment used can make between -55~125 DEG C
It can be up to 10 years or more with the service life, thus, provide the advantageous effect of the application.
Example above-mentioned is merely illustrative, some features of the feature for explaining the disclosure.The attached claims
It is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is that the attached claims are not illustrated the present invention
Feature exemplary selectional restriction.And the progress in science and technology will be formed language express inaccuracy due to and not
The possible equivalent or son being presently considered are replaced, and these variations also should in the conceived case be interpreted by appended
Claim covers.
Claims (10)
1. a kind of composite heat interfacial material of graphene-containing, which is characterized in that the composite heat interfacial material of the graphene-containing
Raw material is prepared, in parts by weight, includes at least following raw material：
2. the composite heat interfacial material of graphene-containing as described in claim 1, which is characterized in that the graphene-containing it is compound
Thermal interfacial material prepares raw material, in parts by weight, includes at least following raw material：
3. the composite heat interfacial material of graphene-containing as claimed in claim 2, which is characterized in that the graphene-containing it is compound
Thermal interfacial material prepares raw material, in parts by weight, includes at least following raw material：
4. the composite heat interfacial material of the graphene-containing as described in claims 1 to 3 any one, which is characterized in that the stone
Ink is crystalline flake graphite.
5. the composite heat interfacial material of the graphene-containing as described in claims 1 to 3 any one, which is characterized in that the stone
Black alkene is modified graphene.
6. the composite heat interfacial material of graphene-containing as described in claim 1, which is characterized in that the graphene-containing it is compound
The raw material for preparing of thermal interfacial material further includes vinyl norbornene base capped polyimides.
7. the composite heat interfacial material of graphene-containing as claimed in claim 6, which is characterized in that the epoxy vinyl ester tree
Weight ratio between fat and vinyl norbornene base capped polyimides is 100：(1~8).
8. the composite heat interfacial material of graphene-containing as described in claim 1, which is characterized in that the graphene-containing it is compound
The raw material for preparing of thermal interfacial material further includes functionalized multi-wall carbonnanotubes.
9. the preparation method of the composite heat interfacial material of the graphene-containing as described in claim 1~8 any one, feature exist
In at least including the following steps：
(1) epoxy vinyl ester resin, vinylsiloxane rubber and initiator of corresponding parts by weight are added in toluene solvant,
Reaction temperature is increased to 80 DEG C, reaction obtains product after 3 hours；
(2) addition graphite, graphene are mixed in the product into step (1), obtain sizing material；Then sizing material is carried out
Tension and compression are rolled and are cut, and obtain the thermal interfacial material of graphene-containing.
10. a kind of graphene heat conductive pad, which is characterized in that the graphene heat conductive pad passes through claim 1~8 any one institute
The composite heat interfacial material for the graphene-containing stated is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810281686.4A CN108485206A (en) | 2018-04-02 | 2018-04-02 | A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810281686.4A CN108485206A (en) | 2018-04-02 | 2018-04-02 | A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108485206A true CN108485206A (en) | 2018-09-04 |
Family
ID=63317953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810281686.4A Pending CN108485206A (en) | 2018-04-02 | 2018-04-02 | A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108485206A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327515A (en) * | 2014-10-20 | 2015-02-04 | 中国科学院金属研究所 | Graphene-containing silicon rubber heat-conducting composite material and preparation method thereof |
| CN104910625A (en) * | 2014-03-12 | 2015-09-16 | 江苏麒祥高新材料有限公司 | Preparation method of heat conduction silicone rubber interface material containing graphene |
| CN105860131A (en) * | 2016-04-29 | 2016-08-17 | 杭州华纳化工有限公司 | Application of graphene nano hybrid material as heat-resistant stabilizer of polymer |
| CN106633916A (en) * | 2016-12-26 | 2017-05-10 | 中国科学院宁波材料技术与工程研究所 | Graphene based heat-conducting interface material and preparation method thereof |
-
2018
- 2018-04-02 CN CN201810281686.4A patent/CN108485206A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910625A (en) * | 2014-03-12 | 2015-09-16 | 江苏麒祥高新材料有限公司 | Preparation method of heat conduction silicone rubber interface material containing graphene |
| CN104327515A (en) * | 2014-10-20 | 2015-02-04 | 中国科学院金属研究所 | Graphene-containing silicon rubber heat-conducting composite material and preparation method thereof |
| CN105860131A (en) * | 2016-04-29 | 2016-08-17 | 杭州华纳化工有限公司 | Application of graphene nano hybrid material as heat-resistant stabilizer of polymer |
| CN106633916A (en) * | 2016-12-26 | 2017-05-10 | 中国科学院宁波材料技术与工程研究所 | Graphene based heat-conducting interface material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5497458B2 (en) | Thermally conductive resin composition | |
| US11739245B2 (en) | Thermally conductive polyorganosiloxane composition | |
| TWI378968B (en) | Epoxy resin composition and semiconductor device | |
| TWI462968B (en) | A heat dissipating material and a semiconductor device using the same | |
| CN102337033B (en) | Additive high-thermal-conductivity organic silicon electronic pouring sealant and preparation method thereof | |
| CN111394056B (en) | High-thermal-conductivity organic silicon gap filler | |
| JP6969729B2 (en) | A method for producing a liquid epoxy resin composition, a semiconductor encapsulant, a semiconductor device, and a liquid epoxy resin composition. | |
| CN106661191A (en) | Composition for heat-dissipation members, heat-dissipation member, electronic device, and heat-dissipation-member production method | |
| JP5889303B2 (en) | Downhole well communication cable | |
| CN107915973A (en) | Thermoplasticity heat-conductive resin composition and preparation method thereof | |
| TW200428603A (en) | Thermally-conductive epoxy resin molded article and method of producing the same | |
| CN105754342A (en) | Low-viscosity heat conducting silicone grease and preparation method thereof | |
| CN106833509A (en) | A kind of heat conduction organosilicon rubber battery casting glue and preparation method thereof | |
| CN106661331A (en) | A single crystal alumina filled die attach paste | |
| CN110709474A (en) | Thermally conductive polyorganosiloxane composition | |
| JP6981001B2 (en) | Heat-dissipating device using heat-conducting sheet and heat-conducting sheet | |
| CN106496886A (en) | Thermal interface material | |
| CN114316328B (en) | High-thermal-conductivity insulating radiating fin for new energy battery and preparation method thereof | |
| CN107325782A (en) | A kind of bi-component casting glue and preparation method thereof | |
| JP2017014445A (en) | Aluminum nitride composite filler and resin composition containing the same | |
| CN108485206A (en) | A kind of composite heat interfacial material of graphene-containing and preparation method thereof, application | |
| TW201930454A (en) | Epoxy resin composition for sealing ball grid array package, epoxy resin cured product and electronic component device | |
| CN107880842A (en) | Flexible heat-conducting pad and preparation method thereof | |
| TWI664231B (en) | Resin composition, cast product for sensor, and temperature sensor using same | |
| US20210147633A1 (en) | Surface treatment agent for thermally conductive polyorganosiloxane composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180904 |