CN110128792A - A kind of hot interface composites and its preparation method and application - Google Patents
A kind of hot interface composites and its preparation method and application Download PDFInfo
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- CN110128792A CN110128792A CN201910481765.4A CN201910481765A CN110128792A CN 110128792 A CN110128792 A CN 110128792A CN 201910481765 A CN201910481765 A CN 201910481765A CN 110128792 A CN110128792 A CN 110128792A
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Abstract
The present invention provides a kind of hot interface composites and its preparation method and application, and the hot interface composites include carbon fiber skeleton, and fill and coat the macromolecule matrix of the carbon fiber skeleton；Carbon fiber in the carbon fiber skeleton is along single-orientated arrangement.The carbon fiber aligned in the present invention sets up passage of heat in the vertical direction of hot interface composites, and carbon fiber is contacted with each other in the direction, is connected, the whole interface resistance for reducing material, substantially increases thermal conductivity outside the face of hot interface composites；And mutual coordinated between carbon fiber skeleton and macromolecule matrix, make hot interface composites that there are the mechanical performances such as high glass-transition temperature and good intensity, toughness.Hot interface composites provided by the invention are thermally conductive and mechanical performance is excellent, and preparation method is simple, easily operated, are a kind of novel heat-conducting materials with large-scale industrial production prospect.
Description
Technical field
The invention belongs to technical field of polymer composite materials, and in particular to a kind of hot interface composites and its preparation side
Method and application.
Background technique
The micromation of electronic component and high integration while assigning more multi-functional electronic product, higher efficiency,
So that the operating power of unit volume is significantly promoted in electronic product, serious heat dissipation problem is thus brought.Electronics member device
The dissipation heat of part can directly result in the raising of electronic equipment temperature and the increase of thermal stress, to the reliable operation of microelectronic device
Property causes to seriously threaten.The most important heat dissipation design of electronic component is to dissipate chip and substrate, substrate by thermal interfacial material
Hot systems connection, industry generally believe future electronic product development bottleneck be not hardware itself and cooling system design, and
It is that can prepare effective thermal interfacial material.Therefore, it in order to solve the structure heat dissipation problem of electric/electronic device, develops new
There is type the thermal interfacial material of excellent heat conductivity performance to become the research hotspot of International Electrical electronic field, research and develop thermal interfacial material
Main thought is that design polymer and a variety of heat fillings interact to form composite material.
CN102286207A discloses a kind of thermoplastic polymer based thermal conductive composite and preparation method thereof, described thermally conductive
Composite material includes polymer thermoplastic matrix, heat filling and auxiliary heat conduction material, and wherein polymer thermoplastic matrix is poly-
Diphenyl sulfide, acrylonitrile-butadiene-styrene copolymer, nylon, polyethylene, polycarbonate, polyvinyl chloride, polypropylene, polyphenyl second
At least one of high molecular materials such as alkene or silicon rubber, auxiliary heat conduction material are the heat incompatible with polymer thermoplastic matrix
Thermoplastic polymer, heat filling are selected from graphite, carbon nanotube, carbon black, silicon nitride, boron nitride, aluminium oxide, magnesia, copper powder, aluminium
The volume ratio of at least one of powder or magnesium powder, polymer thermoplastic matrix and auxiliary heat conduction material is (50~95): (5~
50), heat filling accounts for 5~40wt% of polymer thermoplastic matrix.
CN103665772A discloses a kind of preparation of the carbon nano pipe array compliant thermal interface material of composite epoxy resin
Method, the composite material with carbon nano-pipe array column be thermally conductive skeleton, it is compound with epoxy resin, and be added toughener improve stretch it is tough
Property, it polishes on surface and exposes carbon nanotube pipe end as hot interfacial contact layer；Wherein the average caliber of carbon nano pipe array is
It 80nm, is highly 0.4~1mm, toughener is dibutyl phthalate.The thermal interfacial material obtained by the preparation method
With good heating conduction and certain soft tensile toughness, it can be bonded hot interface, help interface heat dissipation.
Khan M.F.Shahil etc. has studied the application of single-layer graphene and multi-layer graphene in thermal interfacial material, grinds
Study carefully show the loading of single-layer graphene and multi-layer graphene in the material be 2% volume fraction when, the thermal interfacial material of preparation
Thermal coefficient can achieve 14W/ (mK)；In addition, using graphene and silver-colored micrometer/nanometer particle as mixing heat dissipation filler and ring
Epoxy resin-based bluk recombination, the loading for obtaining mixing heat dissipation filler is the thermal interfacial material of 5% volume fraction, thermal coefficient phase
Than that can increase by 500% (Khan M.F.Shahil, et al.Solid State in silver-epoxy resin thermal interfacial material
Communications,2012,152(15):1331).Tang Bo etc. reports raising of the graphene to epoxy resin heating conduction
And Related Mechanism, it was demonstrated that graphene can significantly improve the thermal conductivity of epoxy resin, can will when graphene content is 15%
The thermal conductivity of epoxy resin is improved to 24 times；The functional group of graphene surface can effectively reduce between graphene and epoxy resin
Interface contact heat resistance rate promotes the phonon modes between graphene and epoxy resin more to match (Tang Bo etc., graphene-based epoxy
The preparation of resin compounded thermal interfacial material and hot property [J], silicate journal, 2017,45,126).
However in the prior art, there are processing difficulties, cost for the thermal interfacial material based on compound powder type heat filling
The problems such as high, and compound powder ratio is high, the often mechanical property reduction, poor toughness, not corrosion-resistant of the material of good heat conductivity；
The thermal interfacial material that carbon nanotube is added is had excellent performance, but carbon nanotube preparation process is complicated, at high cost, is not suitable for industrialization and answers
With；Graphene has anisotropic heating conduction, therefore the hot interface material based on graphene as a kind of two-dimentional Heat Conduction Material
Material shows thermal conductivity in preferable face, but thermal conductivity is low outside face, it is difficult to realize heat dissipation performance outside good face.
Based on this, develop a kind of heat dissipation performance it is excellent, especially perfect heat-dissipating outside face, at low cost, mechanical performance is high, suitable
The hot interface composites of suitable industrial application, are this field urgent problems to be solved.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of thermal interfacial material and preparation method thereof and answer
With carbon fiber skeleton is the skeleton structure for playing conductive force in the thermal interfacial material, and carbon fiber makes along single-orientated arrangement
Thermal interfacial material has excellent heating conduction, and especially aligning direction in carbon fiber has the characteristics that high thermal conductivity outside face；It is high
Molecular matrix and carbon fiber skeleton interact, and provide good mechanical strength and processing performance for thermal interfacial material.
In order to achieve that object of the invention, the invention adopts the following technical scheme:
In a first aspect, the present invention provides hot interface composites, the hot interface composites include carbon fiber skeleton, with
And fill and coat the macromolecule matrix of the carbon fiber skeleton；Carbon fiber in the carbon fiber skeleton is along single-orientated row
Column.
In hot interface composites provided by the invention, carbon fiber skeleton is thermally conductive the filling out for undertaking major heat conduction effect
Material, wherein carbon fiber not only has the intrinsic intrinsic property such as the high thermal conductivity of carbon material, high temperature resistant, corrosion-resistant, but also has both fiber
Therefore on the one hand high intensity, high tenacity and the processing performance of material can be played excellent based on the skeleton structure that carbon fiber is constructed
Heating conduction, reduce the interface resistances of hot interface composites, on the other hand as between filler and macromolecule matrix mutually
Coordinated, the effect of activeness and quietness is played to macromolecule matrix, to improve the intensity, toughness of hot interface composites entirety
Etc. mechanical performances.More importantly carbon fiber takes along single in the carbon fiber skeleton of hot interface composites of the present invention
To aligning, passage of heat is being set up along carbon fiber axial direction, and carbon fiber contacts with each other in the axial direction, phase
Even, the interface resistance of material is changed into carbon fiber-carbon fiber from carbon fiber-macromolecule matrix, reduces the whole boundary of material
Face thermal resistance substantially increases thermal conductivity outside the face of hot interface composites.In conclusion hot Interface composites material provided by the invention
Material passes through the mutual cooperation of carbon fiber skeleton and macromolecule matrix, has excellent heating conduction and mechanical performance, especially has
Outside face the characteristics of high thermal conductivity.
Preferably, the material of the macromolecule matrix is thermosetting polymer；
Preferably, the thermosetting polymer is selected from epoxy resin, phenolic resin, polyurethane, polyimides, Lauxite
In organic siliconresin any one or at least two combination, further preferably epoxy resin；
It preferably, is the percent by volume of the macromolecule matrix in terms of 100% by the hot interface composites total volume
It is 80~99%, such as 81%, 83%, 85%, 87%, 89%, 90%, 93%, 85%, 97%, 99% or 100%, and
Specific point value between above-mentioned point value, as space is limited and for concise consideration, range packet described in the present invention no longer exclusive list
The specific point value included.
In hot interface composites provided by the invention, macromolecule matrix is selected primarily based upon its mechanical performance and chemistry
Consider of both stability.The material of the macromolecule matrix selected in the present invention is thermosetting polymer, has mechanical strength
Well, the mechanical performances such as toughness is high, processing performance is good, and chemical property is stablized, and corrosion-resistant, high temperature resistant can be with carbon fiber bone
Frame complements each other to form the thermal conductive composite material haveing excellent performance.The present invention has further screened asphalt mixtures modified by epoxy resin in a preferred approach
Rouge, epoxy resin density is low, corrosion-resistant, chemical property is stable, elastic good, can satisfy hot interface composites for high score
The performance requirement of subbase body.
Preferably, the diameter of the carbon fiber is 1~15 μm, such as 2 μm, 4 μm, 5 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μ
M, the specific point value between 13 μm, 14 μm or 15 μm and above-mentioned point value, as space is limited and for concise consideration, the present invention
The no longer specific point value that includes of range described in exclusive list, further preferably 9~12 μm.
Preferably, the length of the carbon fiber be 50~300 μm, such as 55 μm, 60 μm, 65 μm, 70 μm, 80 μm, 90 μm,
It is specific between 100 μm, 130 μm, 150 μm, 170 μm, 190 μm, 200 μm, 250 μm, 270 μm or 300 μm and above-mentioned point value
Point value, as space is limited and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes, further
Preferably 150~200 μm.
In hot interface composites of the present invention, carbon fiber aligns the carbon fiber skeleton constructed and is to provide thermal conductivity
The key point of energy, the scale of carbon fiber will affect the overall performance of material.If the scale of carbon fiber is limited beyond the present invention
Range, when length is less than 50 μm, the draw ratio of carbon fiber is low, and it is unobvious to align the skeleton structure order to be formed,
Good passage of heat can not be upwardly formed in carbon fiber axle, it is difficult to heating conduction outside high face is provided for material；Its length is big
When 300 μm, the draw ratio of carbon fiber is too big, it is difficult to provide mechanical support upwards in carbon fiber axle and form it into stable skeleton
Structure, so that stable carbon fiber skeleton structure can not be constructed.
It preferably, is in terms of 100% by the hot interface composites total volume, the percent by volume of the carbon fiber is 1
~20%, for example, 2%, 3%, 5%, 7%, 9%, 10%, 13%, 15%, 17%, 19% or 20% and above-mentioned point value it
Between specific point value, as space is limited and for concise consideration, range described in the present invention no longer exclusive list includes specific
Value, further preferably 3~15%.
The percent by volume that carbon fiber is defined in hot interface composites provided by the invention is 1~20%, if being lower than
1%, then the ratio of heat filling carbon fiber is too low in material, and carbon fiber can not play good heat-conducting effect, has material not
Standby heating conduction；If the percent by volume of carbon fiber is higher than 20%, the carbon fiber skeleton structure density for causing to be formed can be made too big, bone
Porosity in frame is low, and enough macromolecule matrixes can not be filled in skeleton, to make the integrated machine of hot interface composites
Tool performance is poor, is unfavorable for later period application.
Preferably, the carbon fiber is the carbon fiber Jing Guo surface-functionalized processing；
Preferably, the carbon fiber is the carbon fiber handled by surface hydrophilicity.
It preferably, further include binder in the hot interface composites；
Preferably, the binder is hydrophilic agglomerant；
Preferably, the hydrophilic agglomerant is cellulosic binder, polyvinyl alcohol binder or alpha-cyanoacrylate
Esters binder；
Preferably, the cellulosic binder is sodium carboxymethylcellulose and/or hydroxyethyl cellulose；
Preferably, the mass ratio of the binder and carbon fiber be (1~5): 1, for example, 1.1:1,1.3:1,1.5:1,
1.8:1,2:1,2.3:1,2.5:1,2.8:1,3:1,3.3:1,3.5:1,3.8:1,4:1,4.3:1,4.5:1,4.8:1 or 4.9:
1。
In heretofore described hot interface composites, to obtain stable carbon fiber skeleton structure, need in carbon fiber
Binder is added when preparing in skeleton, is connected between binder and carbon fiber based on intermolecular interactions such as hydrogen bonds, makes to construct
Carbon fiber skeleton structure it is stronger, be conducive to hot interface composites next step preparation and subsequent applications.
On the other hand, the present invention provides a kind of preparation method of hot interface composites as described above, the preparation side
Method the following steps are included:
(1) preparation of carbon fiber skeleton: the aqueous solution of carbon fiber and binder is mixed to get carbon fiber suspension, then
By carbon fiber suspension freezing, drying, the carbon fiber skeleton of the carbon fiber along single-orientated arrangement is obtained；
(2) preparation of hot interface composites: liquid polymer is mixed with the carbon fiber skeleton that step (1) obtains, and is taken out
Filter, solidification, obtain the hot interface composites.
Preferably, step (1) described carbon fiber is the carbon fiber Jing Guo surface-functionalized processing；
Preferably, the surface-functionalized processing is that hydrophily is handled；
Preferably, the method for the hydrophily processing includes corona treatment and/or acidification.
Carbon fiber skeleton in hot interface composites of the present invention is lyophilized by carbon fiber water solution, is
Make carbon fiber favorable dispersibility in water, be evenly distributed, do not generate reunion or sedimentation, obtains well dispersed outstanding of carbon fiber
Supernatant liquid, carbon fiber of the present invention need to handle by surface hydrophilicity, including corona treatment and/or acid solution processing, make
The surface of carbon fiber keeps it evenly dispersed in water with hydrophilic radicals such as-OH.
Preferably, in step (1) the carbon fiber suspension carbon fiber percent by volume be 1~20%, such as 2%,
3%, the tool between 4%, 5%, 7%, 9%, 10%, 13%, 15%, 17%, 18%, 19% or 20% and above-mentioned point value
Body point value, as space is limited and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the preparation condition of step (1) the carbon fiber suspension is to be stirred under vacuum mixing；
Preferably, it is described be stirred under vacuum mixing revolving speed be 1500~2500rpm, such as 1600rpm, 1700rpm,
Tool between 1800rpm, 1900rpm, 2000rpm, 2100rpm, 2300rpm, 2400rpm or 2500rpm and above-mentioned point value
Body point value, as space is limited and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, it is described be stirred under vacuum mixing time be 10~30min, such as 12min, 14min, 15min, 17min,
Specific point value between 19min, 20min, 22min, 24min, 25min, 27min, 28min or 29min and above-mentioned point value,
As space is limited and for concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the temperature of step (1) described freezing be 0~-250 DEG C, such as -5 DEG C, -10 DEG C, -15 DEG C, -20 DEG C, -
30 DEG C, -50 DEG C, -70 DEG C, -100 DEG C, -130 DEG C, -150 DEG C, -180 DEG C, -200 DEG C, -210 DEG C, -230 DEG C or -250 DEG C, with
And the specific point value between above-mentioned point value, as space is limited and for concise consideration, range described in the present invention no longer exclusive list
Including specific point value.
Preferably, the method for step (1) described freezing is liquid nitrogen frozen.
Carbon fiber skeleton in hot interface composites of the present invention is lyophilized by carbon fiber water solution, institute
It states in preparation method and now disperses carbon fiber in the aqueous solution of binder, mix well to carry out after obtaining the suspension of carbon fiber
The method of cooling freezing, the cooling freezing is preferably liquid nitrogen frozen；Under the cryogenic conditions lower than 0 DEG C in carbon fiber suspension
Water flash freeze, in freezing process, ice grow up caused by extruding force adjust the orientation of carbon fiber, carbon fiber
It ties up direction under the action of extruding force along ice growth and forms vertical single-orientated arrangement, to build carbon fiber vertical
The ordered structure of the axial orientation arrangement of direction, i.e. carbon fiber；Meanwhile carbon fiber is in contact with each other in vertical direction, connects, structure
Build up the passage of heat of vertical direction.And then the ice in system is dried and removed, obtain the skeleton knot of the single-orientated arrangement of carbon fiber
Structure.
Preferably, step (1) drying is vacuum freeze-drying；
Preferably, the time of step (1) described drying be 10~30h, such as 12h, 14h, 15h, 17h, 20h, 22h,
For 24 hours, the specific point value between 26h, 28h or 30h and above-mentioned point value, as space is limited and for concise consideration, the present invention is not
The specific point value that range described in exclusive list includes again.
Preferably, step (2) the mixed method are as follows: the carbon fiber skeleton that step (1) obtains is completely immersed in liquid
In polymer；
It preferably, further include curing agent and catalyst in step (2) described liquid polymer；
Preferably, the temperature of step (2) described suction filtration be 30~50 DEG C, such as 31 DEG C, 33 DEG C, 35 DEG C, 37 DEG C, 39 DEG C,
Specific point value between 40 DEG C, 42 DEG C, 44 DEG C, 45 DEG C, 47 DEG C, 48 DEG C or 50 DEG C and above-mentioned point value, as space is limited and for
Concise consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, step (2) is described filters as vacuum filtration；
Preferably, the time of the vacuum filtration be 2~4h, such as 2.1h, 2.3h, 2.5h, 2.7h, 2.9h, 3h,
Specific point value between 3.3h, 3.5h, 3.8h or 4h and above-mentioned point value, as space is limited and for concise consideration, the present invention
The no longer specific point value that includes of range described in exclusive list.
During the preparation process, the method for first passing through freeze-drying has obtained carbon fiber to hot interface composites of the present invention
Then skeleton structure immerses carbon fiber skeleton structure in liquid polymer, polymer is sufficient filling with into carbon fiber skeleton structure
Gap among, and carbon coated fiber skeleton, and then solidify and obtain macromolecule matrix.Carbon fiber skeleton structure is being immersed into liquid
Be filtered by vacuum after in polymer, be on the one hand to reach molding purpose, be on the other hand vacuum filtration can to the greatest extent can
Polymer and carbon fiber skeleton can be allowed to come into full contact with and be packed into the inside of entire carbon fiber skeleton, do not destroying carbon fiber skeleton
Make the associativity between carbon fiber and macromolecule matrix more preferable under the premise of structure.
Preferably, step (2) the cured method is to be heating and curing；
Preferably, the temperature being heating and curing is 100~250 DEG C, such as 110 DEG C, 130 DEG C, 150 DEG C, 170 DEG C, 190
DEG C, 200 DEG C, 210 DEG C, 220 DEG C, 240 DEG C or the specific point value between 250 DEG C and above-mentioned point value, as space is limited and for letter
Bright consideration, the specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the time being heating and curing be 0.5~7h, such as 0.7h, 0.8h, 1h, 1.3h, 1.5h, 1.7h,
Specific point value between 1.9h, 2h, 2.3h, 2.5h, 2.8h, 3h, 4h, 5h, 6h or 6.5h and above-mentioned point value, as space is limited
And for concise consideration, specific point value that range described in the present invention no longer exclusive list includes.
Preferably, the preparation method specifically includes the following steps:
(1) preparation of carbon fiber skeleton: surface hydrophilicity treated carbon fiber is mixed with the aqueous solution of binder,
10~30min of Vacuum Mixture under the conditions of 1500~2500rpm of revolving speed obtains the carbon that the percent by volume of carbon fiber is 1~20%
Fibrous suspension；Then by the carbon fiber suspension liquid nitrogen frozen, 10~30h of vacuum drying, carbon fiber is obtained along single
The carbon fiber skeleton of orientations；
(2) the carbon fiber skeleton that step (1) obtains the preparation of hot interface composites: is completely immersed in liquid polymer
In, it then places it in vacuum oven, 2~4h is filtered by vacuum under the conditions of 30~50 DEG C；Then in 100~250 DEG C of items
Be heating and curing 0.5~7h under part, obtains the hot interface composites.
On the other hand, the present invention provides a kind of electronic component, includes hot boundary as described above in the electronic component
Plane materiel material.
On the other hand, the present invention provides a kind of electronic equipment, includes electronics member device as described above in the electronic equipment
Part.
Compared with the existing technology, the invention has the following advantages:
It include carbon fiber skeleton and macromolecule matrix, carbon in carbon fiber skeleton in hot interface composites provided by the invention
Fiber is aligned along single-orientated, sets up passage of heat in vertical direction, and carbon fiber contacts with each other, even in the direction
It connects, reduces the whole interface resistance of material, substantially increase thermal conductivity outside the face of hot interface composites；And carbon fiber bone
Mutual coordinated between frame and macromolecule matrix makes hot interface composites have high glass-transition temperature and good
The mechanical performances such as intensity, toughness.Hot interface composites provided by the invention are thermally conductive and mechanical performance is excellent, preparation method letter
It is single, easily operated, it is a kind of novel heat-conducting material with large-scale industrial production prospect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of hot interface composites in the embodiment of the present invention 1, wherein " hot-fluid " represents heat edge
The transmitting of direction shown in arrow, " high temperature " represents the contact surface of hot interface composites and heating device, and " low temperature " represents hot interface
Far from the face of heating device in composite material；
Fig. 2 is the scanning electron microscope (SEM) photograph of carbon fiber skeleton in the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph in the section of hot interface composites in the embodiment of the present invention 1.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Epoxy resin used in the embodiment of the present invention 1~15 is Jiangsu Tai Teer new material Science and Technology Ltd. TTA
21S, epoxide equivalent are 128~145；Curing agent is methyl hexahydrophthalic anhydride, and catalyst N, N- bis- Jia Ji Benzyl amine, binder is hydroxyl
Ethyl cellulose is purchased from Shanghai Aladdin company；Carbon fiber powder be purchased from Shanghai Li Shuo company, average length be 180 μm,
Average diameter is 10 μm, and the surface hydrophilicity processing method of carbon fiber is acidification.
Embodiment 1
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 20min under the conditions of revolving speed 2000rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
Vacuum drying for 24 hours, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in epoxy resin,
Then it places it in vacuum oven, 3h is filtered by vacuum under the conditions of 40 DEG C；Then gradient increased temperature solidify, successively 120 DEG C,
1h, 2h, 2h are heated respectively under the conditions of 160 DEG C, 200 DEG C, obtain the hot interface composites.
Step (1) obtains carbon fiber along single-orientated arrangement by the method for liquid nitrogen frozen and vacuum freeze-drying in the present embodiment
Carbon fiber skeleton, polymer is mixed in step (2) with carbon fiber skeleton then and is filtered, is solidified, is obtained polymer-based
Body and the compound hot interface composites of carbon fiber skeleton, illustratively, the structural schematic diagram of the hot interface composites is such as
Shown in Fig. 1." hot-fluid " represents heat and transmits along direction shown in arrow in Fig. 1, and " high temperature " represents hot interface composites and heat dissipation
The contact surface of device, " low temperature " represent the face in hot interface composites far from radiating element.
The carbon fiber skeleton obtained with scanning electron microscope (SEM) testing procedure (1), obtained scanning electron microscope (SEM) photograph is as schemed
Shown in 2, from figure 2 it can be seen that the carbon fiber in carbon fiber skeleton is along single-orientated ordered arrangement；Use scanning electron microscope
Hot interface composites are tested, obtain the scanning electron microscope (SEM) photograph in its section as shown in figure 3, from figure 3, it can be seen that rodlike substance is
Carbon fiber is epoxy resin-base around carbon fiber, and carbon fiber is scattered in macromolecule matrix, hot interface provided in this embodiment
Composite material has good out-of-plane orientation structure.
Embodiment 2
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 10min under the conditions of revolving speed 1500rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
It is dried in vacuo 12h, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in epoxy resin,
Then it places it in vacuum oven, 2h is filtered by vacuum under the conditions of 30 DEG C；Then gradient increased temperature solidify, successively 120 DEG C,
1h, 2h, 2h are heated respectively under the conditions of 160 DEG C, 200 DEG C, obtain the hot interface composites.
Embodiment 3
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 15min under the conditions of revolving speed 1800rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
It is dried in vacuo 20h, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in epoxy resin,
Then it places it in vacuum oven, 2.5h is filtered by vacuum under the conditions of 35 DEG C；Then gradient increased temperature solidifies, successively 120
DEG C, 160 DEG C, heat 1h, 2h, 2h respectively under the conditions of 200 DEG C, obtain the hot interface composites.
Embodiment 4
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 25min under the conditions of revolving speed 2300rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
It is dried in vacuo 30h, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in epoxy resin,
Then it places it in vacuum oven, 3.5h is filtered by vacuum under the conditions of 45 DEG C；Then gradient increased temperature solidifies, successively 120
DEG C, 160 DEG C, heat 1h, 2h, 2h respectively under the conditions of 200 DEG C, obtain the hot interface composites.
Embodiment 5
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 30min under the conditions of revolving speed 2500rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
It is dried in vacuo 36h, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in epoxy resin,
Then it places it in vacuum oven, 4h is filtered by vacuum under the conditions of 50 DEG C；Then gradient increased temperature solidify, successively 120 DEG C,
1h, 2h, 2h are heated respectively under the conditions of 160 DEG C, 200 DEG C, obtain the hot interface composites.
Embodiment 6
The present embodiment provides a kind of hot interface composites, specific preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: by the water-soluble of surface hydrophilicity treated 0.8g carbon fiber powder and binder
Liquid mixing adds suitable quantity of water to be made into 3mL suspension, and first magneton stirs, then Vacuum Mixture 20min under the conditions of revolving speed 2000rpm,
Obtain the carbon fiber suspension that the percent by volume of carbon fiber is 12%；Then by the carbon fiber suspension liquid nitrogen frozen,
It is dried in vacuo 25h, obtains the carbon fiber skeleton of the carbon fiber along single-orientated arrangement；
(2) the carbon fiber skeleton that step (1) obtains the preparation of hot interface composites: is completely immersed in the phenolic aldehyde of base catalysis
It in resin prepolymer, then places it in vacuum oven, 3.5h is filtered by vacuum under the conditions of 40 DEG C；Then in 180 DEG C of items
Be heating and curing 2h under part, obtains the hot interface composites.
Embodiment 7
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 0.4g.
Embodiment 8
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 0.6g.
Embodiment 9
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 1.0g.
Embodiment 10
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 1.2g.
Embodiment 11
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 0.07g.
Embodiment 12
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 0.05g.
Embodiment 13
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 1.3g.
Embodiment 14
The present embodiment the difference from embodiment 1 is that, in step (1) carbon fiber powder be 1.5g.
Embodiment 15
The present embodiment the difference from embodiment 1 is that, the carbon fiber in step (1) is handled without surface hydrophilicity.
Embodiment 16
The present embodiment the difference from embodiment 1 is that, in step (1) average length of carbon fiber be 500 μm.
Comparative example 1
This comparative example provides a kind of hot interface composites, specific preparation method the following steps are included:
Surface hydrophilicity treated 6g carbon fiber powder is mixed with the aqueous solution of binder, suitable quantity of water is added to be made into 3mL
Suspension, first magneton stirring, then Vacuum Mixture 30min under the conditions of revolving speed 2500rpm, obtains the percent by volume of carbon fiber
For 12% carbon fiber suspension；Then by the carbon fiber suspension liquid nitrogen frozen, vacuum drying 36h, the heat is obtained
Interface composites.
Comparative example 2
This comparative example provides a kind of hot interface composites, specific preparation method the following steps are included:
It will be placed in a vacuum drying oven in liquid-state epoxy resin, 4h be filtered by vacuum under the conditions of 50 DEG C；Then 100~
Be heating and curing 0.5~3h under the conditions of 250 DEG C, obtains the hot interface composites.
Comparative example 3
This comparative example mention the difference from embodiment 1 is that, the carbon fiber suspension vacuum drying oven in step (1) is successively
1h, 2h, 2h are heated respectively under the conditions of 120 DEG C, 160 DEG C, 200 DEG C, obtain the carbon fiber skeleton of carbon fiber random arrangement.
Comparative example 4
This comparative example mention the difference from embodiment 1 is that, the carbon nanotube of the quality such as carbon fiber Wesy in step (1) is replaced
It changes.
Performance test methods: the performance test of hot interface composites of the present invention is carried out with reference to the prior art, such as
With reference to Xiaoliang Zeng, et al.Small, 2015,11 (46), 6250-6213.
(1) Determination of conductive coefficients:
Steady state method measures the thermally conductive standard test method of vertical direction, and test equipment is the survey of LW-9389TIM resistance conductivity
Measure instrument, specific steps are as follows: hot interface composites are placed between instrument stick, stable hot-fluid is established by component；Then
The temperature in ammeter item is monitored along its length in two or more sites；Leap is calculated according to obtained temperature reading
The temperature difference at interface, and it is used to determine the thermal coefficient at interface.
(2) thermal expansion coefficient is tested:
Thermo-mechanical analysis method (TMA test), test equipment are thermomechanical analyzer (402 F1 of Model TMA
Hyperion, Netzsch), the thermal expansion coefficient (CTE) of hot interface composites is measured in 25~300 DEG C of temperature ranges.
(3) glass transition temperature is tested:
Thermo-mechanical analysis method (TMA test), test equipment are thermomechanical analyzer (402 F1 of Model TMA
Hyperion, Netzsch), the thermal dilatometry of hot interface composites is measured in 25~300 DEG C of temperature ranges, it is swollen by heat
Glass transition temperature is calculated in inflection point in swollen curve.
According to above method testing example 1~15, comparative example 1~4 provide hot interface composites thermal coefficient,
Thermal expansion coefficient and glass transition temperature, test result are as shown in table 1:
Table 1
It can be seen that from the data of table 1 when the percent by volume of carbon fiber in hot interface composites is limited in the present invention
1~20% range in when, the heat transfer efficiencies of hot interface composites, glass transition temperature are with carbon fiber percent by volume
Increase and be gradually increased, thermal expansion coefficient is gradually reduced with the increase of carbon fiber percent by volume, it was demonstrated that provided by the invention
Hot interface composites have excellent heating conduction and mechanical performance, especially have the characteristics that high thermal conductivity outside face.When hot interface
Arrangement mode of the percent by volume of carbon fiber beyond the framework of the present definition or carbon fiber is random arrangement in composite material
When, hot interface composites do not have good heating conduction；In addition, carbon fiber of the present invention is replaced with other of equivalent
When two-dimentional carbon material (such as carbon nanotube), the thermally conductive skeleton of carbon of ordered arrangement is unable to get according to the technique that the present invention limits,
It is unable to get the hot interface composites with excellent heat conducting performance.
The Applicant declares that the present invention is explained by the above embodiments hot interface composites provided by the invention and its system
Standby and application process, but the invention is not limited to above-mentioned processing steps, that is, do not mean that the present invention must rely on
Stating processing step could implement.It should be clear to those skilled in the art, any improvement in the present invention, to the present invention
The equivalence replacement of selected raw material and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention
Within the open scope.
Claims (10)
1. a kind of hot interface composites, which is characterized in that the hot interface composites include carbon fiber skeleton, and filling
And coat the macromolecule matrix of the carbon fiber skeleton；Carbon fiber in the carbon fiber skeleton is along single-orientated arrangement.
2. hot interface composites according to claim 1, which is characterized in that the material of the macromolecule matrix is thermosetting
Property polymer；
Preferably, the thermosetting polymer is selected from epoxy resin, phenolic resin, polyurethane, polyimides, Lauxite or has
In machine silicone resin any one or at least two combination, further preferably epoxy resin；
It preferably, is in terms of 100% by the hot interface composites total volume, the percent by volume of the macromolecule matrix is 80
~99%.
3. hot interface composites according to claim 1 or 2, which is characterized in that the diameter of the carbon fiber is 1~15
μm, preferably 9~12 μm；
Preferably, the length of the carbon fiber is 50~300 μm, further preferably 150~200 μm；
Preferably, by the hot interface composites total volume it is in terms of 100% that the percent by volume of the carbon fiber is 1~
20%, further preferably 3~15%；
Preferably, the carbon fiber is the carbon fiber Jing Guo surface-functionalized processing；
Preferably, the carbon fiber is the carbon fiber handled by surface hydrophilicity.
4. described in any item hot interface composites according to claim 1~3, which is characterized in that the hot Interface composites material
It further include binder in material；
Preferably, the binder is hydrophilic agglomerant；
Preferably, the hydrophilic agglomerant is cellulosic binder, polyvinyl alcohol binder or cyanoacrylate
Binder；
Preferably, the cellulosic binder is sodium carboxymethylcellulose and/or hydroxyethyl cellulose；
Preferably, the mass ratio of the binder and carbon fiber is (1~5): 1.
5. a kind of preparation method of such as described in any item hot interface composites of Claims 1 to 4, which is characterized in that described
Preparation method the following steps are included:
(1) preparation of carbon fiber skeleton: being mixed to get carbon fiber suspension for the aqueous solution of carbon fiber and binder, then by institute
The freezing of carbon fiber suspension, drying are stated, the carbon fiber skeleton of the carbon fiber along single-orientated arrangement is obtained；
(2) preparation of hot interface composites: liquid polymer is mixed with the carbon fiber skeleton that step (1) obtains, and filters, is solid
Change, obtains the hot interface composites.
6. preparation method according to claim 5, which is characterized in that step (1) carbon fiber is by function of surface
Change the carbon fiber of processing；
Preferably, the surface-functionalized processing is that hydrophily is handled；
Preferably, the method for the hydrophily processing includes corona treatment and/or acidification；
Preferably, the percent by volume of carbon fiber is 1~20% in step (1) the carbon fiber suspension；
Preferably, the preparation condition of step (1) the carbon fiber suspension is to be stirred under vacuum mixing；
Preferably, the revolving speed for being stirred under vacuum mixing is 1500~2500rpm；
Preferably, the time for being stirred under vacuum mixing is 10~30min；
Preferably, the temperature of step (1) described freezing is 0~-250 DEG C；
Preferably, the method for step (1) described freezing is liquid nitrogen frozen；
Preferably, step (1) drying is vacuum freeze-drying；
Preferably, the time of step (1) described drying is 10~30h.
7. preparation method according to claim 5 or 6, which is characterized in that step (2) the mixed method are as follows: will walk
Suddenly the carbon fiber skeleton that (1) obtains is completely immersed in liquid polymer；
It preferably, further include curing agent and catalyst in step (2) described liquid polymer；
Preferably, the temperature of step (2) described suction filtration is 30~50 DEG C；
Preferably, step (2) is described filters as vacuum filtration；
Preferably, the time of the vacuum filtration is 2~4h；
Preferably, step (2) the cured method is to be heating and curing；
Preferably, the temperature being heating and curing is 100~250 DEG C；
Preferably, the time being heating and curing is 0.5~7h.
8. according to the described in any item preparation methods of claim 5~7, which is characterized in that the preparation method specifically include with
Lower step:
(1) preparation of carbon fiber skeleton: surface hydrophilicity treated carbon fiber is mixed with the aqueous solution of binder, in revolving speed
10~30min of Vacuum Mixture under the conditions of 1500~2500rpm obtains the carbon fiber that the percent by volume of carbon fiber is 1~20%
Suspension；Then by the carbon fiber suspension liquid nitrogen frozen, 10~30h of vacuum drying, carbon fiber is obtained along single-orientated
The carbon fiber skeleton of arrangement；
(2) preparation of hot interface composites: the carbon fiber skeleton that step (1) obtains is completely immersed in liquid polymer, so
After place it in vacuum oven, under the conditions of 30~50 DEG C be filtered by vacuum 2~4h；Then add under the conditions of 100~250 DEG C
0.5~7h of heat cure obtains the hot interface composites.
9. a kind of electronic component, which is characterized in that comprising as described in any one of Claims 1 to 4 in the electronic component
Thermal interfacial material.
10. a kind of electronic equipment, which is characterized in that include electronic component as claimed in claim 9 in the electronic equipment.
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