CN107022194A - A kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material and preparation method - Google Patents
A kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material and preparation method Download PDFInfo
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Abstract
By heat conduction main body, graphene of expanded graphite it is enhanced thermal conduction body the invention discloses a kind of preparation method of multiple dimensioned Carbon Materials/silicon rubber composite material, using organic silicon rubber as flexible substrate, the interface Heat Conduction Material of better performances is obtained by kneading, degassing, shaping and solidification.Heat conductivity is 0.68 ~ 2.98W/mK, and modulus of compressibility is less than 1.2MPa（Provide compressive deformation ε=30%）.Raw material of the present invention is cheap to be easy to get, and technique is simple, and performance is stable, is adapted to large-scale production.
Description
Technical field
The present invention relates to a kind of interface Heat Conduction Material, led more particularly to a kind of multiple dimensioned Carbon Materials/silicon rubber interface
Hot material and preparation method.
Background technology
Power device (processor, chip etc.) in electronic equipment is usually associated with the generation of heat in normal work.
These heats need to transmit to outside by forms such as heat transfer, convection current, radiation from power device in time, otherwise accumulative heat
A series of problems, such as slack-off speed of service of electronic equipment, less reliable, service life shorten can be caused.And electronic equipment compared with
High integrated level make it that the effect of heat management and thermal design in its design process is more and more important.Heat from power device to dissipate
During hot device transmission, a series of solid/solid contact interface is crossed over.From the point of view of microcosmic angle, between these solids
Contact interface have it is many it is microcosmic on it is uneven, it is this it is microcosmic on roughness be formed a considerable number of thermal contact resistance
(contact thermal resistance)。
In the electronic device, interface Heat Conduction Material (thermal interface materials) is filled in solid circle
Between face, and apply certain normal pressure to it.Interface Heat Conduction Material is deformed upon, and has made up uneven on microcosmic, is reached
To the purpose for reducing, eliminating interface resistance.Therefore interface Heat Conduction Material needs to have concurrently excellent compression deformation ability and higher
Thermal conductivity.Bernd Weidenfeller are by the fillers such as iron oxide, mica, copper powder, short glass fiber and methyl ethylene
The compound thermal conductivity for improving composite of silicon rubber.Research shows, when the volume fraction of mica is 30%, the heat of composite
Conductance can be improved from 0.7W/mK to 2.5W/mK.Certain the thermal conductive silicon rubber produced with DOW CORNING (Dow Corning) company
Exemplified by glue, basic material is dimethyl silicone polymer, and heat conduction particle is BN ceramic particles.When heat conduction particle percentage by weight reaches
When 88%, thermal conductivity is 4W/mK.
The filler that filled-type interface Heat Conduction Material is typically used for metallic particles, metal oxide particle, ceramic particle,
Metallic fiber, carbon fiber, CNT etc., heat conductivility is improved by the contact between filler.When the loading of filler is less than
When 20%, thermal conductivity factor is very low and increasess slowly, because not interconnected between filler under low loading, it is necessary to increase filling
Amount can just form network structure using the filler of Nano grade.The filler of Nano grade easily exists in Blending Processes
Agglomeration, improves the compatibility between filler and matrix by surface modification, to reduce the reunion journey of filler in the base
Degree.When loading is more than certain value, thermal conductivity factor increases very fast.Therefore traditional interface Heat Conduction Material needs higher loading
To form more contact points to realize the higher capacity of heat transmission or be equipped with by rational level and form more passages of heat.
But from actual processing angle, larger loading causes system viscosity to rise, the difficulty of mixing and sulfuration process is added
Degree, and higher loading can cause the reduction of the mechanical properties such as the compression deformation ability of composite.In addition, higher filling
Amount causes material cost increase.
The content of the invention
It is an object of the invention to provide a kind of low loading, low excess effusion value, inexpensive multiple dimensioned Carbon Materials/silicon rubber circle
Face Heat Conduction Material and preparation method.
Developed the present invention be directed to filling kind and filler form.Lee G W, Shenogina N have found sheet
The filler of structure has relatively low excess effusion value than chondritic, and heat conduction main body expanded graphite of the present invention is by nano level
Lamellar structure piles up composition, and lamellar structure is thinner (as shown in Figure 1) than traditional inorganic filler size, bigger specific surface area
(specific surface area of expanded graphite is different and different with expansion multiple, and the expanded graphite specific surface area scope of document report is
10-70cm2/g：Expanded graphite specific surface area prepared by the present invention is 32.9464m2/ g, and the conduction that common Heat Conduction Material is used
A diameter of 1-3.6 μm of silver powder, specific surface area is 0.78-3.2m2/ g) make the overlapped probability for forming thermal conducting path of its lamella knot
It is higher, therefore the heat conduction network of UNICOM is easily formed under smaller compactedness；The heat conductivility of expanded graphite in itself will simultaneously
It is higher than conventional filler.In addition, larger-size expanded graphite can be in structure shape with the less graphene of size (as shown in Figure 2)
Form complementary in state, form the structure that similar level is matched somebody with somebody, less graphene can as UNICOM's expanded graphite bridge so that
Excess effusion value is reduced to a certain extent.
Conventional filler particle diameter is thinner, agglomeration it is more obvious, it is necessary to by coupling agent etc. to filler carry out surface modification with
Improve compatibility or dispersion effect.And the main stuffing expanded graphite and enhanced thermal conduction body graphene and silicon rubber that the present invention is used
Matrix has good compatibility, therefore need not be modified, and its nanoscale twins can be scattered in matrix material well.
From cost angle analysis, technique of the present invention inherits traditional blending technology, simple production process.Its
Secondary, the present invention is that can reach traditional accessible heat conductivility of larger loading by relatively low loading；And main stuffing
Expanded graphite is cheap and easy to get, and two kinds of factors cause the holistic cost of interface Heat Conduction Material of the present invention to be the 1/4 of traditional material cost
Or it is lower.
In addition, relatively low loading can ensure that composite largely inherits the compression performance of base material, loading
It is smaller, performance of the compression performance closer to base material.This is also obtained interface Heat Conduction Material of the invention than traditional interface heat conduction
One of advantage of material.
To achieve these goals, the present invention is adopted the technical scheme that：
The preparation method of a kind of multiple dimensioned Carbon Materials/silicon rubber compound interface Heat Conduction Material, first by heat filling and silicon
Rubber resin is blended, and is molded after processing is de-gassed to the mixture after blending, and shaped article finally is carried out into heat
Crosslinking curing, obtains interface Heat Conduction Material.
Multiple dimensioned Carbon Materials/silicon rubber interface the Heat Conduction Material of the present invention, its mass percent matches composition and is：
Expanded graphite：2.0-28.0wt.%
Graphene：0.15-6.0wt.%
Organic silicon rubber：70.0-95wt.%
It is preferred that, mass percent proportioning composition is：
Expanded graphite：2.0-20.0wt.%
Graphene：0.15-5.5wt.%
Organic silicon rubber：76.5-95wt.%
The expansion multiple of the expanded graphite is 100-500ml/g；
Described graphene is that piece footpath size is 2-5 μm；
Described graphene content should in 0.15-6.0%, when content is less than 0.15%, graphene sheet layer do not reach with it is swollen
Swollen graphite forms multi-level bridging arrangement；When content is more than 6.0%, because graphene has higher specific surface area, itself and tree
The composite effect of fat is poor；
Described organic silicon rubber resin is mainly two-component silicones, is made up of, refers mainly to crosslinking agent its pre-polymerization liquid
Two-component methyl silicon resin, two-component methyl vinyl silicone, one kind in two-component methyl phenyl vinyl polysiloxane or
It is several.
The preparation method of the multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material of the present invention, including step are as follows：
(1) it will be placed in after graphene and bi-component organic silicon rubber pre-polymerization liquid premix in blending equipment and 10-60min be blended；
(2) expanded graphite is gradually added into the mixture that step (1) is obtained, continues that 30-150min is blended；
(3) mixture for obtaining step (2) is de-gassed under processing, -0.06~-0.09MPa pressure and keeps 30-
120min；
(4) mixture obtained using coating machine or mould to step (3) is molded；
(5) compound after shaping is solidified into 20-120min in 80-120 DEG C, obtains multiple dimensioned Carbon Materials/silicon rubber circle
Face Heat Conduction Material.
Blending in the step (2) refers to carry out the one or more in pressurization blending, vacuum blending, normal pressure blending
Combination.The blending equipment used is in screw extruder, vacuum kneading machine, vacuum pressed kneading machine, vacuum pressed stirred tank
One or more be applied in combination.
The present invention has the following advantages that compared with prior art
1) heat filling has nano level lamellar structure, and specific surface area is bigger than conventional filler, and (expanded graphite compares surface
For 10-70m2/ g, and traditional common micro-scaled filler is generally several m2/ g), the probability that lamella overlaps each other/contacted under identical loading
It is higher, heat conduction network can be formed under smaller loading.
2) traditional filler is matched somebody with somebody using the filler progress level of different-grain diameter, so that heat conduction network is more readily formed；It is of the invention then
Carry out level using the expanded graphite of multi-disc Rotating fields and the graphene of few lamellar structure and match somebody with somebody, form complementation is formed in structure, is held
More passages of heat are easily formed, as shown in Figure 4.
3) production technology inherits traditional blending technology；And relatively low loading causes raw material with relatively low filler price
Holistic cost is the 1/4 even lower of conventional filler cost.
4) filler need not carry out surface modification to improve dispersiveness of the filler in matrix, and it has good with silicone rubber matrix
Compatibility.
5) traditional interface Heat Conduction Material needs higher filler loading just to reach higher heat conductivility, and compared with
High loading causes the compression performance of composite to reduce, and one of main performance of interface Heat Conduction Material is to need well
Compression deformation ability.The loading of the present invention is smaller, the good compression property of multiple material, respectively less than 1.2MPa (regulation compressive deformation ε=
30%), thermal conductivity factor scope is 0.68-2.98W/mK.
Therefore find the multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material of the invention prepared with higher by contrasting
Cost performance, disclosure satisfy that heat conduction demand of the conventional electronic component to boundary material.
Brief description of the drawings
Fig. 1 is expanded graphite lamellar structure SEM figures of the present invention.
Fig. 2 is graphene film Rotating fields TEM figures of the present invention.
Fig. 3 be the present invention by filler of expanded graphite/graphene with using 100nm aluminum oxide being filler to thermal conductivity in document
The influence of energy.
A figures are traditional multiscale transform particulate filler passage of heat schematic diagram in Fig. 4, and B figures are that multiple dimensioned Carbon Materials of the invention are led
Passage of heat schematic diagram.
Embodiment
Specific embodiment is described in further details to the present invention below, but does not constitute any limitation of the invention.
Embodiment 1：
1) the dimethyl siloxane pre-polymerization liquid of two-component methyl silicon resin and crosslinking agent are pressed 10：1 ratio is mixed, and is had
Expansion multiple is 250ml/g expanded graphite by machine silicone rubber solution, the graphene and organic silicon rubber solution in 2.3 μm of piece footpaths
With 4.8%：0.17%：95% mass ratio weighs standby；
2) kneading 15min in being placed in after graphene and organic silicon rubber solution premix under vacuum kneading machine vacuum condition.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue kneading 30min under vacuum condition.
4) by step 3) obtained mixture is de-gassed under processing, -0.085MPa pressure and keeps 60min.
5) use coating machine that the compound after degassing is prepared into thin slice of the thickness for 1.0mm.
6) by the compound after shaping in solidifying 45min at 110 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity can
Up to 0.68W/mK, modulus of compressibility is 0.53MPa.
Embodiment 2：
1) the methyl vinyl silicone pre-polymerization liquid of two-component methyl vinyl silicone and crosslinking agent are pressed 8:1 ratio
Mix, obtain organic silicon rubber solution, by expansion multiple be 250ml/g expanded graphite, the graphene in 3.5 μm of piece footpaths with it is organic
Silicone rubber solution is with 6.2%：0.5%：93.3% mass ratio weighs standby；
2) it will be placed in after graphene and organic silicon rubber solution premix in vacuum pressed stirred tank and stir 10min.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue to stir 30min, vacuum (-
0.085MPa) with each 15min of (0.8MPa) mixing time with pressure.
4) by step 3) obtained mixture goes out to carry out degassing process after kettle, and 120min is kept under -0.07MPa pressure.
5) use mould that the compound after degassing is prepared into thin slice of the thickness for 1.0mm.
6) by mould in solidifying 60min at 100 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity is up to 0.96W/m
K, modulus of compressibility is 0.69MPa.
Embodiment 3：
1) the dimethyl siloxane pre-polymerization liquid of two-component dimethyl-silicon resin and crosslinking agent are pressed 10:1 ratio is mixed, and is obtained
To organic silicon rubber solution.Be 300ml/g expanded graphite by expansion multiple, graphene, the organic silicon rubber in 3.5 μm of piece footpaths it is molten
Liquid is with 11.6%：1.15%：87.2% mass ratio weighs standby；
2) kneading 30min under vacuum condition will be placed in vacuum kneading machine after graphene and organic silicon rubber solution premix.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue kneading 60min under vacuum condition.
4) by step 3) carry out keeping 60min under degassing process, -0.09MPa pressure after the discharging of obtained mixture.
5) use mould that the compound after degassing is prepared into thickness for thin slice thick 2.0mm.
6) by mould in solidifying 60min at 100 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity is up to 1.33W/m
K, modulus of compressibility is 0.61MPa.
Embodiment 4：
1) the dimethyl siloxane pre-polymerization liquid of two-component dimethyl-silicon resin and crosslinking agent are pressed 10:1 ratio is mixed, and is obtained
To organic silicon rubber solution.Be 300ml/g expanded graphite by expansion multiple, graphene, the organic silicon rubber in 3.5 μm of piece footpaths it is molten
Liquid is with 11.5%：2.30%：86.2% mass ratio weighs standby；
2) kneading 40min under vacuum condition will be placed in vacuum kneading machine after graphene and organic silicon rubber solution premix.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue kneading 60min under vacuum condition.
4) by step 3) carry out keeping 75min under degassing process, -0.09MPa pressure after the discharging of obtained mixture.
5) use coating machine that the compound after degassing is prepared into thin slice of the thickness for 1.0mm.
6) by the compound after shaping in solidifying 120min at 80 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity can
Up to 1.75W/mK, modulus of compressibility is 0.77MPa.
Embodiment 5：
1) the methyl phenyl vinyl siloxanes pre-polymerization liquid of two-component methyl phenyl vinyl polysiloxane is pressed with crosslinking agent
8:1 ratio is mixed, and obtains organic silicon rubber solution.Be 300ml/g expanded graphite by expansion multiple, the stone in 3.3 μm of piece footpaths
Black alkene, organic silicon rubber solution are with 16%：3.69%：80.3% mass ratio weighs standby；
2) kneading 40min under vacuum condition will be placed in vacuum kneading machine after graphene and organic silicon rubber solution premix.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue kneading 90min under vacuum condition.
4) by step 3) carry out keeping 120min under degassing process, -0.09MPa pressure after the discharging of obtained mixture.
5) use coating machine that the compound after degassing is prepared into thin slice of the thickness for 1.5mm.
6) by the compound after shaping in solidifying 120min at 80 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity can
Up to 2.37W/mK, modulus of compressibility is 0.92MPa.
Embodiment 6：
1) the methyl phenyl vinyl siloxanes pre-polymerization liquid of two-component methyl phenyl vinyl polysiloxane is pressed with crosslinking agent
8:1 ratio is mixed, and obtains organic silicon rubber solution.Be 300ml/g expanded graphite by expansion multiple, the stone in 3.3 μm of piece footpaths
Black alkene, organic silicon rubber solution are with 18%：5.5%：76.5% mass ratio weighs standby；
2) kneading 40min under vacuum condition will be placed in vacuum kneading machine after graphene and organic silicon rubber solution premix.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue kneading 135min under vacuum condition.
4) by step 3) carry out keeping 120min under degassing process, -0.09MPa pressure after the discharging of obtained mixture.
5) use coating machine that the compound after degassing is prepared into thin slice of the thickness for 1.5mm.
6) by the compound after shaping in solidifying 120min at 80 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity can
Up to 2.98W/mK, modulus of compressibility is 1.15MPa.Fig. 3 be expanded graphite/graphene and aluminum oxide respectively as filler to compound
The influence of thermal conductivity of material.
Comparative example：
1) the dimethyl siloxane pre-polymerization liquid of two-component methyl silicon resin and crosslinking agent are pressed 10:1 ratio is mixed, and is obtained
Organic silicon rubber solution.It is 300ml/g expanded graphite by expansion multiple, organic silicon rubber solution is with 2.3%：97.7% matter
Amount is more standby than weighing；
2) it will be placed in after graphene and organic silicon rubber pre-polymerization liquid premix in stirred tank and stir 15min.
3) expanded graphite is gradually added into step 2) in obtained mixture, continue to stir 45min.
4) by step 3) obtained mixture is de-gassed under processing, -0.085MPa pressure and keeps 60min.
5) use coating machine that the compound after degassing is prepared into thin slice of the thickness for 1.5mm.
6) by the compound after shaping in solidifying 30min at 120 DEG C, interface heat-conductive composite material is obtained.Its thermal conductivity is
0.33W/mK, modulus of compressibility is 0.48MPa.
By the contrast of comparative example and embodiment it can be found that can be to heat conduction after addition graphene formation Multi-scale model
Performance is significantly improved.
The boundary material that each embodiment that the present invention is provided is obtained, with relatively low loading, higher heat conductivility,
Excellent compression deformation ability.Composite is led respectively as filler with nano aluminium oxide by Fig. 3 expanded graphites/graphene
The influence of hot property, it can be found that when aluminum oxide is as filler, the following heat conductivility of volume content 25% is almost very low, surpasses
Larger growth just occurs when 25%；And expanded graphite/graphene system then reaches aluminum oxide 30% 4.8%/0.17%
The thermal conductivity factor of loading, and gradually increase with the increase of volume content.Illustrate to obtain as filler using expanded graphite/graphene
To interface Heat Conduction Material there is relatively low excess effusion value and higher heat conductivility.
Embodiments of the invention are the foregoing is only, and ratio is to limit the present invention, it is all in the spirit and principles in the present invention
Within, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (9)
1. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material, it is characterised in that mass percent, which is constituted, is：
Expanded graphite： 2.0-28.0 wt.%
Graphene： 0.15-6.0 wt.%
Organic silicon rubber： 70.0-95 wt.%.
2. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 1, it is characterised in that quality percentage
It is than composition：
Expanded graphite： 2.0-20.0 wt.%
Graphene： 0.15-5.5 wt.%
Organic silicon rubber： 76.5-95 wt.%.
3. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 1, it is characterised in that the expansion
The expansion multiple of graphite is 100-500ml/g.
4. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 1, it is characterised in that described stone
Black alkene is that piece footpath size is 2-5 μm.
5. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 1, it is characterised in that described has
Machine silicone rubber resina is two-component silicones, is made up of its pre-polymerization liquid with crosslinking agent.
6. a kind of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 5, it is characterised in that described is double
Component methyl silicon resin is two-component methyl vinyl silicone, one kind in two-component methyl phenyl vinyl polysiloxane or several
Kind.
7. a kind of preparation side of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as described in claim any one of 1-6
Method, it is characterised in that as follows including step：
(1) it will be placed in after graphene and bi-component organic silicon rubber pre-polymerization liquid premix in blending equipment and 10-60min be blended；
(2) expanded graphite is gradually added into the mixture that step (1) is obtained, continues that 30-150min is blended；
(3) mixture for obtaining step (2) is de-gassed under processing, -0.06~-0.09MPa pressure and keeps 30-120min；
(4) mixture obtained using coating machine or mould to step (3) is molded；
(5) compound after shaping is solidified into 20-120min in 80-120 DEG C, obtains multiple dimensioned Carbon Materials/silicon rubber interface and lead
Hot material.
8. a kind of preparation method of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 7, its feature exists
Blending in the step (2) is to carry out one or more kinds of combinations in pressurization blending, vacuum blending, normal pressure blending.
9. a kind of preparation method of multiple dimensioned Carbon Materials/silicon rubber interface Heat Conduction Material as claimed in claim 7, its feature exists
In blending equipment be screw extruder, vacuum kneading machine, vacuum pressed kneading machine, vacuum pressed stirred tank in one kind or
Multiple combinations are used.
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| CN108329893A (en) * | 2018-03-11 | 2018-07-27 | 深圳市驭晟新能源科技有限公司 | A kind of compliant thermal interface phase transformation compound foil material and preparation method thereof |
| CN114784307A (en) * | 2022-03-29 | 2022-07-22 | 广东氢发新材料科技有限公司 | Graphene-reinforced expanded graphite/polyimide-polyether ether ketone composite bipolar plate and preparation method thereof |
| CN114784307B (en) * | 2022-03-29 | 2023-11-17 | 广东氢发新材料科技有限公司 | Graphene reinforced expanded graphite/polyimide-polyether-ether-ketone composite bipolar plate and preparation method thereof |
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