CN105514066B - A kind of compound infrared radiation heat-conducting film of graphene and preparation method thereof - Google Patents
A kind of compound infrared radiation heat-conducting film of graphene and preparation method thereof Download PDFInfo
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Abstract
The invention discloses compound infrared radiation heat-conducting films of a kind of graphene and preparation method thereof, it is characterised in that：It is that the compound infrared radiating coating of graphene is provided in substrate.The present invention utilizes the good infra-red radiation ability of the compound infrared radiant material of graphene and capacity of heat transmission, film obtained is respectively provided with good capacity of heat transmission on the direction for be parallel and perpendicular to substrate, so that heat is able to rapidly be transferred in radiating element or environment from heating position, improve heat conduction efficiency, hot localised points in abatement apparatus reduce the temperature gradient on heat conduction path.The present invention makes simple and convenient, and the rapid thermal conduction of Highgrade integration and heating equipment to electronic device provides powerful support.
Description
Technical field
The present invention relates to a kind of High-performance heat conduction materials, are particularly a kind of compound infrared radiation heat-conducting film of graphene and its system
Make method.
Technical background
With the Highgrade integration of electronic product, arithmetic speed and operation frequency are higher and higher, and electronic device often exists
The local substantial amounts of thermal conductivity of generation causes local temperature excessively high, so that electronic device disabler is even destroyed by damage property, contracts
Short electronic device service life.Modern electronic product is lightening, it is required that too big, too heavy, the electronics device that radiator can not be done
Part also tends to the limitation due to structure and shape so that can not usually be contacted directly between heating device and radiating element, seriously
Affect radiating rate and efficiency.In addition, heat is required to be transferred to preferable position in time in terms of traditional heating equipment,
And the heat that current heating equipment generates mainly carries out heat conveying by the contact conduction of heat and cross-ventilation heat-conducting mode,
Inefficiency, temperature gradient is big, and heat transmission is uneven, is badly in need of improving the conduction efficiency of heat.
Therefore how heat transfer, thermal convection current progress heat transfer efficiency to be made good use of maximumlly simultaneously, exploitation heat radiation
The important directions made great efforts as those skilled in the art.
The content of the invention
In view of this, the object of the present invention is to provide compound infrared radiation heat-conducting film of a kind of graphene and preparation method thereof,
It is intended to make heat conducting film that there is excellent infrared radiation property and heat dissipation performance.
The purpose of the present invention is what is be achieved through the following technical solutions：
The compound infrared radiation heat-conducting film of graphene of the present invention, feature are：The compound infrared radiation heat-conducting of graphene
Film is that the compound infrared radiating coating of graphene is provided in substrate；The compound infrared radiating coating of graphene is by base
It graphene coated compound infrared radiation coating and then is formed by curing on bottom；The compound infrared radiation coating of graphene is by conduct
The graphene and filler of infrared radiant material, dispersant, binding agent and solvent mixing are formed.
Specifically, each raw material for forming the compound infrared radiation coating of the graphene is by the composition of mass parts：
5~60 parts of graphene；
0~50 part of filler；
1~10 part of dispersant；
5~50 parts of binding agent；
40~90 parts of solvent；
Gross mass part of each raw material is 100 parts.
Wherein, the filler for bortz powder, aluminium oxide, graphite, carbon pipe, titanium oxide, chromium oxide, iron oxide, zirconium oxide,
At least one of silica, zirconium nitride, aluminium nitride, boron nitride, carborundum, zirconium boride and zirconium English powder are preferably bortz powder.
The dispersant is neopelex, lauryl sodium sulfate, cetyl trimethylammonium bromide, 16
Alkyl trimethyl ammonium chloride, polyvinylpyrrolidone (such as PVP K30, polyvinylpyrrolidone K60, polyethylene
Pyrrolidones K90), at least one of tween and sodium carboxymethylcellulose, be preferably sodium dodecyl benzene sulfonate.
The binding agent is epoxy resin, polyvinyl alcohol, LA133, butadiene-styrene rubber (SBR), heat conductive silica gel, polyurethane tree
At least one of fat, polyacrylic resin, phosphate-based inorganic binder and silicate organic binder bond are preferably epoxy
Resin.
The solvent is water, N-Methyl pyrrolidone (NMP), ethyl acetate, propyl acetate, butyl acetate, acetone, first
At least one of alcohol, ethyl alcohol, ethylene glycol and propyl alcohol are preferably water.
The substrate be aluminium foil, copper foil, polyethylene, polypropylene, polyvinyl chloride, polystyrene, ceramics, glass or silicon chip,
Preferably copper foil or aluminium foil.
The production method of the above-mentioned compound infrared radiation heat-conducting film of graphene, includes the following steps：
(1) the compound infrared radiation coating of graphene is prepared：By proportioning by graphene, filler, dispersant, binding agent and solvent
Simultaneously 1~5h of ultrasonic disperse is mixed, obtains mixed slurry；Then room temperature for the first time is carried out to the mixed slurry using high shear to emulsify,
Emulsification rotating speed is 10000~26000rpm, and the time is 3~12h；Slurry after first emulsifying is put into wet-milling in spherical grinder again
Slurry after grinding is crossed 150~300 mesh sieves by 3~30h；It finally reuses high shear and carries out secondary room temperature breast to crossing strained pulp
Change, emulsification rotating speed is 10000~26000rpm, and the time is 2~5h, that is, obtains the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated in substrate, in an oven 60~
200 DEG C of 5~10min of baking are formed by curing thickness in 3~100 μm of the compound infrared radiating coating of graphene, that is, obtain graphene
Compound infrared radiation heat-conducting film.
Preferably, it 2h, first emulsifying time is that 6h, emulsification rotating speed are that the time of ultrasonic disperse, which is, in step (1)
16000rpm, the wet-milling time for for 24 hours, sieve mesh number be 200 mesh, the second emulsifying time be 3h, emulsification rotating speed be 16000rpm, step
Suddenly baking temperature is 100 DEG C in (2), baking time is that 8min, the compound infrared radiating coating of graphene are 10 μm.
Compared with prior art, beneficial effects of the present invention are embodied in：
The present invention is obtained using the good infra-red radiation ability of the compound infrared radiant material of graphene and capacity of heat transmission
Film is respectively provided with good capacity of heat transmission on the direction for be parallel and perpendicular to substrate so that heat is able to rapidly from fever
Position is transferred in radiating element or environment, improves heat conduction efficiency, and hot localised points in abatement apparatus reduce heat conduction path
On temperature gradient.The present invention makes simple and convenient, the rapid thermal conduction of Highgrade integration and heating equipment to electronic device
Provide powerful support.
The compound infrared radiation heat-conducting film of graphene made by the present invention not only has good capacity of heat transmission, but also has
There is good infrared emanation ability, so as to heat conduction efficiency height, the advantage having a wide range of application.
Description of the drawings
Fig. 1 is the structure diagram of the compound infrared radiation heat-conducting film of graphene of the present invention.
Figure label：1 is the compound infrared radiating coating of graphene, and 2 be substrate.
Specific embodiment
Embodiment 1
The compound infrared radiation heat-conducting film of the present embodiment following steps for manufacturing graphene：
(1) 10 parts of graphenes, 5 parts of bortz powders, 2 parts of neopelexes, 10 parts of epoxy resin and 73 parts of water are taken
Mixing carries out ultrasonic disperse 2h and obtains mixed slurry；Then room temperature for the first time is carried out to mixed slurry using high shear to emulsify, emulsification turns
Speed is 16000rpm, time 6h；Slurry after first emulsifying is put into spherical grinder wet-milling for 24 hours again, by slurry after grinding
Cross 200 mesh sieves；It finally reusing high shear and carries out secondary room temperature emulsification to crossing strained pulp, emulsification rotating speed is 16000rpm, when
Between for 3h, that is, obtain the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated on 20 μm of copper foils, in an oven
100 DEG C of baking 8min, are formed by curing graphene compound infrared radiating coating of the thickness at 10 μm, that is, it is compound infrared to obtain graphene
Radiate heat conducting film.
After tested, the thermal conductivity factor (horizontal direction) of gained heat conducting film be 1940W/mk, thermal conductivity factor (vertical direction)
For 580W/mk.
Embodiment 2
The compound infrared radiation heat-conducting film of the present embodiment following steps for manufacturing graphene：
(1) 20 parts of graphenes, 8 parts of aluminium oxide, 5 parts of neopelexes, 15 parts of epoxy resin and 52 parts of water is taken to mix
It closes, carries out ultrasonic disperse 2h and obtain mixed slurry；Then room temperature for the first time is carried out to mixed slurry using high shear to emulsify, emulsifies rotating speed
For 16000rpm, time 8h；Slurry after first emulsifying is put into spherical grinder wet-milling for 24 hours again, by slurry mistake after grinding
200 mesh sieves；It finally reuses high shear and carries out secondary room temperature emulsification to crossing strained pulp, emulsification rotating speed is 16000rpm, the time
For 4h, that is, obtain the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated on 20 μm of copper foils, in an oven
100 DEG C of baking 8min, are formed by curing graphene compound infrared radiating coating of the thickness at 10 μm, that is, it is compound infrared to obtain graphene
Radiate heat conducting film.
After tested, the thermal conductivity factor (horizontal direction) of gained heat conducting film be 1890W/mk, thermal conductivity factor (vertical direction)
For 560W/mk.
Embodiment 3
The compound infrared radiation heat-conducting film of the present embodiment following steps for manufacturing graphene：
(1) 10 parts of graphenes, 5 parts of carborundum, 3 parts of neopelexes, 10 parts of epoxy resin and 72 parts of water is taken to mix
It closes, carries out ultrasonic disperse 2h and obtain mixed slurry；Then room temperature for the first time is carried out to mixed slurry using high shear to emulsify, emulsifies rotating speed
For 16000rpm, time 6h；Slurry after first emulsifying is put into spherical grinder wet-milling for 24 hours again, by slurry mistake after grinding
200 mesh sieves；It finally reuses high shear and carries out secondary room temperature emulsification to crossing strained pulp, emulsification rotating speed is 16000rpm, the time
For 3h, that is, obtain the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated on 30 μm of aluminium foils, in an oven
120 DEG C of baking 10min, are formed by curing graphene compound infrared radiating coating of the thickness at 15 μm, that is, it is compound red to obtain graphene
External radiation heat conducting film.
After tested, the thermal conductivity factor (horizontal direction) of gained heat conducting film be 1900W/mk, thermal conductivity factor (vertical direction)
For 560W/mk.
Embodiment 4
The compound infrared radiation heat-conducting film of the present embodiment following steps for manufacturing graphene：
(1) 15 parts of graphenes, 6 parts of boron nitride, 6 parts of hexadecyltrimethylammonium chlorides, 20 parts of epoxy resin and 53 parts are taken
NMP is mixed, and is carried out ultrasonic disperse 2h and is obtained mixed slurry；Then room temperature for the first time is carried out to mixed slurry using high shear to emulsify, breast
Change rotating speed is 16000rpm, time 6h；Slurry after first emulsifying is put into spherical grinder wet-milling for 24 hours again, after grinding
Slurry crosses 200 mesh sieves；It finally reuses high shear and carries out secondary room temperature emulsification to crossing strained pulp, emulsification rotating speed is
16000rpm, time 3h obtain the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated on 30 μm of aluminium foils, in an oven
120 DEG C of baking 10min, are formed by curing graphene compound infrared radiating coating of the thickness at 15 μm, that is, it is compound red to obtain graphene
External radiation heat conducting film.
After tested, the thermal conductivity factor (horizontal direction) of gained heat conducting film be 1920W/mk, thermal conductivity factor (vertical direction)
For 530W/mk.
Embodiment 5
The compound infrared radiation heat-conducting film of the present embodiment following steps for manufacturing graphene：
(1) 10 parts of graphenes, 5 parts of iron oxide, 3 parts of PVP K30s, 10 parts of butadiene-styrene rubber and 72 parts of NMP are taken
Mixing carries out ultrasonic disperse 3h and obtains mixed slurry；Then room temperature for the first time is carried out to the mixed slurry using high shear to emulsify, breast
Change rotating speed is 16000rpm, time 8h；Slurry after first emulsifying is put into spherical grinder wet-milling for 24 hours again, after grinding
Slurry crosses 200 mesh sieves；It finally reuses high shear and carries out secondary room temperature emulsification to crossing strained pulp, emulsification rotating speed is
16000rpm, time 3h obtain the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated on 30 μm of aluminium foils, in an oven
120 DEG C of baking 10min, are formed by curing graphene compound infrared radiating coating of the thickness at 10 μm, that is, it is compound red to obtain graphene
External radiation heat conducting film.
After tested, the thermal conductivity factor (horizontal direction) of gained heat conducting film be 1960W/mk, thermal conductivity factor (vertical direction)
For 550W/mk.
Claims (6)
1. a kind of production method of the compound infrared radiation heat-conducting film of graphene, it is characterised in that：
The compound infrared radiation heat-conducting film of graphene is that the compound infrared radiating coating of graphene is provided in substrate；The stone
The black compound infrared radiating coating of alkene is by the graphene coated compound infrared radiation coating in substrate and then is formed by curing；Institute
The compound infrared radiation coating of graphene is stated by the graphene as infrared radiant material and filler, dispersant, binding agent and solvent
Mixing is formed；Each raw material for forming the compound infrared radiation coating of the graphene is by the composition of mass parts：
5~20 parts of graphene；
0~8 part of filler；
1~10 part of dispersant；
5~50 parts of binding agent；
40~73 parts of solvent；
Gross mass part of each raw material is 100 parts；
The production method of the compound infrared radiation heat-conducting film of graphene, includes the following steps：
(1) the compound infrared radiation coating of graphene is prepared：Graphene, filler, dispersant, binding agent and solvent are mixed by proportioning
And 1~5h of ultrasonic disperse, obtain mixed slurry；Then room temperature for the first time is carried out to the mixed slurry using high shear to emulsify, emulsification
Rotating speed is 10000~26000rpm, and the time is 3~12h；Again by slurry after first emulsifying be put into wet-milling 3 in spherical grinder~
Slurry after grinding is crossed 150~300 mesh sieves by 30h；It finally reuses high shear and carries out secondary room temperature emulsification to crossing strained pulp,
Emulsification rotating speed is 10000~26000rpm, and the time is 2~5h, that is, obtains the compound infrared radiation coating of graphene；
(2) the compound infrared radiation coating of graphene that step (1) is obtained is coated in substrate, 60~200 DEG C in an oven
5~10min of baking is formed by curing graphene compound infrared radiating coating of the thickness at 3~100 μm, that is, it is compound red to obtain graphene
External radiation heat conducting film.
2. production method according to claim 1, it is characterised in that：The filler for bortz powder, aluminium oxide, graphite,
Carbon pipe, titanium oxide, chromium oxide, iron oxide, zirconium oxide, silica, zirconium nitride, aluminium nitride, boron nitride, carborundum, zirconium boride and
At least one of zirconium English powder.
3. production method according to claim 1, it is characterised in that：The dispersant is neopelex, ten
Sodium dialkyl sulfate, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, polyvinylpyrrolidone, tween and
At least one of sodium carboxymethylcellulose.
4. production method according to claim 1, it is characterised in that：The binding agent for epoxy resin, polyvinyl alcohol,
LA133, butadiene-styrene rubber, heat conductive silica gel, polyurethane resin, polyacrylic resin, phosphate-based inorganic binder and silicate
At least one of organic binder bond.
5. production method according to claim 1, it is characterised in that：The solvent is water, N-Methyl pyrrolidone, acetic acid
At least one of ethyl ester, propyl acetate, butyl acetate, acetone, methanol, ethyl alcohol, ethylene glycol and propyl alcohol.
6. production method according to claim 1, it is characterised in that：The substrate is aluminium foil, copper foil, polyethylene, poly- third
Alkene, polyvinyl chloride, polystyrene, ceramics, glass or silicon chip.
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