CN109251733A - A kind of graphene composite material heat conducting film and preparation method thereof - Google Patents
A kind of graphene composite material heat conducting film and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of graphene composite material heat conducting film and preparation method thereof, the raw material of the graphene composite material heat conducting film includes graphene, cerium zirconium sosoloid, the ceria of lanthana modification, V2O5, dispersing agent, coupling agent, heat stabilizer and solvent, the present invention joined the ceria and V of cerium zirconium sosoloid, lanthana modification in raw graphite alkene2O5, the cohesion between graphene can be effectively reduced, thermal conductivity and mechanical stretch intensity of the graphene in heat radiation coating are improved, in addition, the ceria and V of cerium zirconium sosoloid, lanthana modification2O5Addition enable to form netted or chain structure form in the inside of graphene composite material heat conducting film so that graphene heat conducting film forms thermally conductive network chain, so that the heating conduction of graphene heat conducting film be greatly improved.
Description
Technical field
The present invention relates to technical field of graphene, and in particular to a kind of graphene composite material heat conducting film and its preparation side
Method.
Background technique
Graphene (Graphene) is a kind of new material of individual layer laminated structure being made of carbon atom, is one kind by carbon
Atom is with sp2The hexangle type of hybridized orbit composition is in the flat film of honeycomb lattice, the two-dimentional material of only one carbon atom thickness
Material.
Due to the special construction of graphene, researcher pays close attention to always the exploitation to graphene Related product, graphene
Multiple use also increasingly shows.Wherein, with the graphene heat conducting film of the capacity of heat transmission, also known as thermal conductivity graphene piece, become in recent years
Carry out the novel heat conduction and heat radiation material of emerging one kind, is applied to electronics, communication, illumination, aviation and defence and military extensively
Etc. many fields.The performances such as graphene heat conducting film thermal coefficient with higher, lower thermal resistance and lighter in weight, it is thermally conductive
Coefficient is higher than carbon nanotube and diamond；Its thermal resistance is lower than aluminium, copper；It is low that its weight also compares aluminium, copper；In addition, graphene is led
Hotting mask surface can be combined with other materials such as metal, plastic cement, adhesive stickers to meet more design functions and needs, Ke Yigen
It needs to carry out graphene heat conducting film cutting cutting according to true form, thus there is very big market potential.
For example, Chinese patent literature CN104232027A discloses a kind of preparation method of graphene heat conducting film, the technology
In the raw material of graphene heat conducting film include: graphene, functionalization graphene, stabilizer and solvent, preparation method first will
Graphene oxide or the graphene being modified by the macromolecule matrixes material such as polyvinyl alcohol, polystyrene and cellulose, i.e.,
Functionalization graphene is dispersed in solvent with graphene, graphene oxide and stabilizer, obtains mixed slurry, then will
Above-mentioned mixed slurry, by film and matrix separation, finally obtains graphene heat conducting film after roller process.But above-mentioned technology is made
Graphene heat conducting film thermal coefficient it is to be improved.Therefore, a kind of graphene heat conducting film of high thermal conductivity coefficient is researched and developed, to meet
To high thermal conductivity coefficient heat conducting film demand in the fields such as electronics, communication, illumination, aviation and defence and military, this is for art technology
It is a technical problem urgently to be resolved for personnel.
Summary of the invention
The present invention provides a graphene composite material heat conducting film, which has high thermal conductivity system
Number.Furthermore the present invention further provides preparation methods.
The present invention solves the technical solution that above-mentioned technical problem uses are as follows:
The first aspect of the present invention provides a kind of graphene composite material heat conducting film comprising following raw material: stone
Black 35~50 parts by weight of alkene, 5~8 parts by weight of cerium zirconium sosoloid, 2~6 parts by weight of ceria of lanthana modification, V2O53~8
Parts by weight, 3~6 parts by weight of dispersing agent, 5~10 parts by weight of coupling agent, 4~9 parts by weight of heat stabilizer, 20~30 weight of solvent
Part.
In above-mentioned graphene composite material heat conducting film, the ceria of the lanthana modification the preparation method is as follows: system
Standby solubility lanthanum salt solution, and be impregnated on ceria, dry, roasting obtains the ceria of lanthana modification.
Preferably, the dispersing agent is hexenyl bis-stearamides or glyceryl tristearate；The coupling agent is 3- ammonia
Propyl trimethoxy silicane or gamma-mercaptopropyltriethoxysilane；The heat stabilizer is mono-tert-butyl malonate or double propylene
Sour fourth diester；The solvent is ethyl alcohol.
Preferably, the soluble lanthanum salt is lanthanum nitrate；The drying temperature for completing the ceria after dipping is 70
~90 DEG C, preferably 80~85 DEG C, the time be 2~4h, maturing temperature be 260~400 DEG C, preferably 300~350 DEG C, the time be 2~
3h。
Second aspect of the present invention provides the preparation method of above-mentioned graphene composite material heat conducting film, includes the following steps:
(1) graphene is prepared:
After mixing by crystalline graphite powder and intercalator sodium carbonate, using mechanical lapping mode, mixing presoma is obtained；
The mixing presoma is mixed with organic solvent, sequentially adds the poly-dopamine and dispersion modified through sulfhydrylation hydroxyethyl starch
Agent is handled in ultrasonic generator after mixing evenly, obtains graphene；
(2) graphene made from (1) the step of selected parts by weight and cerium zirconium sosoloid, the lanthana of selected parts by weight are changed
Ceria, the V of property2O5, dispersing agent, coupling agent, heat stabilizer and solvent carry out mixed grinding, shearing under ultrasonication, surpass
Acoustical power is 1000~1200W, and the time is 40~60min, obtains composite slurry slurry；
(3) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(4) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on sided corona treatment mistake in a manner of hanging painting
PET film on, scraper height be 10~50mm；
(5) the coated PET film of the step (4) is dried；
(6) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film；
(7) it carries out cutting edge to the PET base graphene heat conducting film after rolling processing and handles to obtain graphene composite material to lead
Hotting mask.
Preferably, in the step (1), the mass ratio of the crystalline graphite powder and the intercalator sodium carbonate is 1:5；Institute
Stating dispersing agent is neopelex；The crystalline graphite powder and the poly- DOPA modified through sulfhydrylation hydroxyethyl starch
Amine, the dispersing agent mass ratio be 1:10:80.
Preferably, in step (5), the temperature of the drying is 50~80 DEG C, and the time is 12~18h, preferably 15h.
Preferably, in step (6), the upper mold temperature of the heat rolling processing stabilizes to 80~110 DEG C, preferably 90 DEG C, under
Mould temperature stabilizes to 80~110 DEG C, preferably 90~100 DEG C, and revolving speed is 30~100r/min.
Third aspect present invention provides the graphene composite material heat conducting film that above-mentioned preparation method is prepared.
Above-mentioned technical proposal of the invention has the advantages that
(1) graphene composite material heat conducting film of the present invention, including graphene, cerium zirconium sosoloid, lanthana modification
Ceria, V2O5, dispersing agent, coupling agent, heat stabilizer and solvent, the present invention joined in raw graphite alkene cerium zirconium solid solution
The ceria and V of body, lanthana modification2O5, the cohesion between graphene can be effectively reduced, graphene is improved and is radiating
Thermal conductivity and mechanical stretch intensity in coating, in addition, the ceria and V of cerium zirconium sosoloid, lanthana modification2O5Addition
It enables to form netted or chain structure form in the inside of graphene composite material heat conducting film, so that graphene heat conducting film shape
At thermally conductive network chain, so that the heating conduction of graphene heat conducting film be greatly improved.After measured, graphene produced by the present invention is multiple
The thermal coefficient of condensation material heat conducting film is 1800~2300W/mK.
(2) preparation method of graphene composite material heat conducting film of the present invention, wherein headed by the preparation method of graphene
Graphite powder is uniformly mixed with intercalator first, using mechanical lapping mode, obtains mixing presoma, it then will be before mixing obtained
It drives body to mix with organic solvent, sequentially adds the poly-dopamine modified through sulfhydrylation hydroxyethyl starch, dispersing agent, stir evenly
Afterwards, it is ultrasonically treated, obtains graphite ene product.The preparation method of graphene of the present invention uses relatively mild through mercapto
The poly-dopamine and dispersing agent of base hydroxyethyl starch modification are removed, wherein sulfhydrylation hydroxyethyl starch is modified poly- more
Bar amine, has a special surface-active, the strong adsorption capacity shown, can π-between the benzene ring structure of graphite
Pi-electron cloud generates absorption, so that the outermost graphene of natural graphite is fallen in solvent from graphite substrate, by constantly heavy
This multiple process, hardly destroys the chemical bonding structure of graphene.
(3) preparation method of graphene composite material heat conducting film of the present invention, using suitable temperature to coating after
PET/ graphene film be dried, control solvent is volatilized with slowly speed, prevents graphene film layer from occurring empty
The phenomenon that hole；Meanwhile the present invention adjusts upper mold temperature, lower die temperature and the revolving speed to heat rolling, reduces in graphene film
Gap between graphene sheet layer improves the density of graphene heat conducting film, improves heat transfer efficiency.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.In addition, below
Technical characteristic involved in described different embodiments of the present invention as long as they do not conflict with each other can be mutual
In conjunction with.
Embodiment 1
Present embodiments provide a kind of preparation method of graphene:
(1) preparation for the poly-dopamine modified through sulfhydrylation hydroxyethyl starch
The hydroxyethyl starch 1g that molecular weight is 25000Da, ethoxy degree of substitution is 0.5 is taken to be dissolved in 10mL deionized water,
Then stirring sequentially adds 1.2g sodium hydroxide and 1.5g monoxone and forms reaction system to dissolving, and by the reaction system in
Reaction 5h is carried out at 100 DEG C, stops reaction, and cold room temperature processed pours into reaction system in 20mL methanol, stirs, and centrifugation obtains white
Color precipitating, the as hydroxyethyl starch of carboxylated；
It takes the hydroxyethyl starch of 0.8g carboxylated obtained above to be dissolved in 10mL deionized water, 250mg1- (3- bis- is added
Methylaminopropyl) -3- ethyl-carbodiimide hydrochloride, 75mgN- HOSu NHS and 150mg 2- (two sulphur of pyridine)-second
Amine hydrochlorate forms reaction system, this reaction system is stirred to react 30h in 30 DEG C, is centrifuged, and takes supernatant using molecular cut off
It is bag filter deionized water dialysis 3 days of 3500Da, freeze-drying obtains hydroxyethyl starch -2- (two sulphur of pyridine)；
It takes hydroxyethyl starch -2- made from 0.5g above-mentioned steps (two sulphur of pyridine) to be dissolved in 10mL dimethyl sulfoxide, is added
420mg dithiothreitol (DTT) is stirred at room temperature reaction for 24 hours under nitrogen protection, then uses molecular cut off for the dialysis of 3500Da
Bag deionized water dialysis 3 days, freeze-drying, obtains sulfhydrylation hydroxyethyl starch；
It takes 40mg poly-dopamine to be dispersed in 10mL deionized water, stirs ultrasound 30min, sodium hydroxide adjusting pH, which is added, is
10, it is then slowly added to the stirring of sulfhydrylation hydroxyethyl starch side made from 200mg above-mentioned steps, after addition, at room temperature
It is stirred to react 30h, to remove unreacted sulfhydrylation hydroxyethyl starch, the molecular cut off of above-mentioned super filter tube is for ultrafiltration
100kDa, ultrafiltration revolving speed are 4000 revs/min, obtain the poly-dopamine modified by sulfhydrylation hydroxyethyl starch；
(2) preparation of graphene
1g crystalline graphite powder is uniformly mixed with 5g intercalator sodium carbonate and carries out mechanical horizontal grinding 50h, grinding is finished, obtained
To mixing presoma；
Above-mentioned mixing presoma is mixed with 250mL methanol, it is obtained through sulfhydrylation then to sequentially add 10g step (1)
The poly-dopamine of hydroxyethyl starch modification, 80g neopelex carry out ultrasound with ultrasonic generator after mixing evenly
Processing, ultrasonic time 1h, ultrasonic power 300W obtain graphene then through washing, centrifugation, 50 DEG C of dryings.
Embodiment 2
Present embodiments provide a kind of graphene composite material heat conducting film, including following raw material:
Graphene 35g, cerium zirconium sosoloid 8g, lanthana modification ceria 2g, V2O58g, hexenyl bis-stearamides
3g, gamma-mercaptopropyltriethoxysilane 10g, mono-tert-butyl malonate 4g, ethyl alcohol 30g；
The ceria of lanthana modification in the present embodiment the preparation method is as follows:
It prepares mass concentration and is the lanthanum nitrate aqueous solution of 10t%, and be impregnated on ceria, two after impregnating will be completed
Cerium oxide obtains the ceria of lanthana modification in 90 DEG C of dry 2h, and in 260 DEG C of maturing temperature 3h；Wherein mass concentration
It is 1:5 for the lanthanum nitrate aqueous solution of 10t% and the mass ratio of ceria；
The present embodiment additionally provides the preparation method of above-mentioned graphene composite material heat conducting film:
(1) take graphene made from 35g embodiment 1 and 8g cerium zirconium sosoloid, 2g lanthana modification ceria,
8gV2O5, 3g hexenyl bis-stearamides, 10g gamma-mercaptopropyltriethoxysilane, 4g mono-tert-butyl malonate and 30g ethyl alcohol exist
Mixed grinding, shearing are carried out under ultrasonication, ultrasonic power 1000W, time 60min obtain composite slurry slurry；
(2) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(3) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on sided corona treatment mistake in a manner of hanging painting
PET film on, scraper height be 10mm；
(4) the coated PET film of the step (3) is dried to 18h at 50 DEG C；
(5) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film,
The upper mold temperature of heat rolling processing stabilizes to 80 DEG C, and lower die temperature stabilizes to 110 DEG C, revolving speed 30r/min；
(6) it carries out cutting edge to the PET base graphene heat conducting film after rolling processing and handles to obtain graphene composite material to lead
Hotting mask.
Embodiment 3
Present embodiments provide a kind of graphene composite material heat conducting film, including following raw material:
Graphene 50g, cerium zirconium sosoloid 5g, lanthana modification ceria 6g, V2O53g, glyceryl tristearate 6g,
3- aminopropyl trimethoxysilane 5g, double acrylic acid fourth diester 9g, ethyl alcohol 20g；
The ceria of lanthana modification in the present embodiment the preparation method is as follows:
It prepares mass concentration and is the lanthanum nitrate aqueous solution of 10t%, and be impregnated on ceria, two after impregnating will be completed
Cerium oxide obtains the ceria of lanthana modification in 70 DEG C of dry 4h, and in 400 DEG C of maturing temperature 2h；Wherein mass concentration
It is 1:5 for the lanthanum nitrate aqueous solution of 10t% and the mass ratio of ceria；
The present embodiment additionally provides the preparation method of above-mentioned graphene composite material heat conducting film:
(1) take graphene made from 50g embodiment 1 and 5g cerium zirconium sosoloid, 6g lanthana modification ceria,
3gV2O5, 6g glyceryl tristearate, 5g 3- aminopropyl trimethoxysilane, the bis- acrylic acid fourth diester of 9g and 20g ethyl alcohol are super
Sound effect is lower to carry out mixed grinding, shearing, and ultrasonic power 1200W, time 40min obtain composite slurry slurry；
(2) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(3) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on sided corona treatment mistake in a manner of hanging painting
PET film on, scraper height be 50mm；
(4) the coated PET film of the step (3) is dried to 12h at 80 DEG C；
(5) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film,
The upper mold temperature of heat rolling processing stabilizes to 110 DEG C, and lower die temperature stabilizes to 80 DEG C, revolving speed 100r/min；
(6) it carries out cutting edge to the PET base graphene heat conducting film after rolling processing and handles to obtain graphene composite material to lead
Hotting mask.
Embodiment 4
Present embodiments provide a kind of graphene composite material heat conducting film, including following raw material:
Graphene 40g, cerium zirconium sosoloid 7g, lanthana modification ceria 4g, V2O55g, hexenyl bis-stearamides
4g, 3- aminopropyl trimethoxysilane 8g, double acrylic acid fourth diester 6g, ethyl alcohol 25g；
The ceria of lanthana modification in the present embodiment the preparation method is as follows:
It prepares mass concentration and is the lanthanum nitrate aqueous solution of 10t%, and be impregnated on ceria, two after impregnating will be completed
Cerium oxide obtains the ceria of lanthana modification in 80 DEG C of dry 3h, and in 350 DEG C of maturing temperature 2.5h；Wherein quality is dense
Degree is the lanthanum nitrate aqueous solution of 10t% and the mass ratio of ceria is 1:5；
The present embodiment additionally provides the preparation method of above-mentioned graphene composite material heat conducting film:
(1) take graphene made from 40g embodiment 1 and 7g cerium zirconium sosoloid, 4g lanthana modification ceria,
5gV2O5, 4g hexenyl bis-stearamides, 8g 3- aminopropyl trimethoxysilane, the bis- acrylic acid fourth diester of 6g and 25g ethyl alcohol exist
Mixed grinding, shearing are carried out under ultrasonication, ultrasonic power 1200W, time 40min obtain composite slurry slurry；
(2) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(3) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on sided corona treatment mistake in a manner of hanging painting
PET film on, scraper height be 50mm；
(4) the coated PET film of the step (3) is dried to 15h at 80 DEG C；
(5) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film,
The upper mold temperature of heat rolling processing stabilizes to 90 DEG C, and lower die temperature stabilizes to 100 DEG C, revolving speed 50r/min；
(6) it carries out cutting edge to the PET base graphene heat conducting film after rolling processing and handles to obtain graphene composite material to lead
Hotting mask.
Embodiment 5
Present embodiments provide a kind of graphene composite material heat conducting film, including following raw material:
Graphene 45g, cerium zirconium sosoloid 6g, lanthana modification ceria 3g, V2O57g, hexenyl bis-stearamides
4g, gamma-mercaptopropyltriethoxysilane 9g, mono-tert-butyl malonate 5g, ethyl alcohol 23g；
The ceria of lanthana modification in the present embodiment the preparation method is as follows:
It prepares mass concentration and is the lanthanum nitrate aqueous solution of 10t%, and be impregnated on ceria, two after impregnating will be completed
Cerium oxide obtains the ceria of lanthana modification in 90 DEG C of dry 2h, and in 260 DEG C of maturing temperature 3h；Wherein mass concentration
It is 1:5 for the lanthanum nitrate aqueous solution of 10t% and the mass ratio of ceria；
The present embodiment additionally provides the preparation method of above-mentioned graphene composite material heat conducting film:
(1) take graphene made from 45g embodiment 1 and 6g cerium zirconium sosoloid, 3g lanthana modification ceria,
7gV2O5, 4g hexenyl bis-stearamides, 9g gamma-mercaptopropyltriethoxysilane, 5g mono-tert-butyl malonate and 23g ethyl alcohol exist
Mixed grinding, shearing are carried out under ultrasonication, ultrasonic power 1100W, time 50min obtain composite slurry slurry；
(2) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(3) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on sided corona treatment mistake in a manner of hanging painting
PET film on, scraper height be 30mm；
(4) the coated PET film of the step (3) is dried to 16h at 70 DEG C；
(5) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film,
The upper mold temperature of heat rolling processing stabilizes to 100 DEG C, and lower die temperature stabilizes to 90 DEG C, revolving speed 70r/min；
(6) it carries out cutting edge to the PET base graphene heat conducting film after rolling processing and handles to obtain graphene composite material to lead
Hotting mask.
Experimental example 1
Calculate the thermal coefficient of graphene composite material heat conducting film made from embodiment 2~5:
(1) calculates the thermal coefficient of graphene heat conducting film made from each embodiment according to the following formula,
K=α iCp ρ 0 (1),
Wherein, K is thermal coefficient, and α i is the thermal diffusion coefficient of sample, and Cp is the specific heat at constant pressure of test sample, and ρ 0 is to survey
The density of test agent；The thermal coefficient of the graphene heat conducting film of each embodiment measured is as shown in table 1.
The thermal coefficient of graphene heat conducting film made from 1 embodiment 2~5 of table
| The thermal coefficient (W/mK) of graphene heat conducting film | |
| Embodiment 2 | 2000 |
| Embodiment 3 | 2300 |
| Embodiment 4 | 1900 |
| Embodiment 5 | 1800 |
As shown in Table 1, the heating conduction of graphene heat conducting film produced by the present invention is preferable.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. a kind of graphene composite material heat conducting film, which is characterized in that it includes following raw material: 35~50 weight of graphene
Measure part, 5~8 parts by weight of cerium zirconium sosoloid, 2~6 parts by weight of ceria of lanthana modification, V2O53~8 parts by weight, dispersing agent
3~6 parts by weight, 5~10 parts by weight of coupling agent, 4~9 parts by weight of heat stabilizer, 20~30 parts by weight of solvent.
2. graphene composite material heat conducting film according to claim 1, which is characterized in that the dioxy of the lanthana modification
Change cerium the preparation method is as follows:
Soluble lanthanum salt solution is prepared, and is impregnated on ceria, dry, roasting obtains the ceria of lanthana modification.
3. graphene composite material heat conducting film according to claim 1 or 2, which is characterized in that
The dispersing agent is hexenyl bis-stearamides or glyceryl tristearate；
The coupling agent is 3- aminopropyl trimethoxysilane or gamma-mercaptopropyltriethoxysilane；
The heat stabilizer is mono-tert-butyl malonate or double acrylic acid fourth diester；
The solvent is ethyl alcohol.
4. graphene composite material heat conducting film according to claim 2, which is characterized in that the solubility lanthanum salt is nitric acid
Lanthanum；It is described complete dipping after ceria drying temperature be 70~90 DEG C, the time be 2~4h, maturing temperature be 260~
400 DEG C, the time is 2~3h.
5. a kind of preparation method of the described in any item graphene composite material heat conducting films of Claims 1 to 4, which is characterized in that
Include the following steps:
(1) graphene is prepared:
After mixing by crystalline graphite powder and intercalator sodium carbonate, using mechanical lapping mode, mixing presoma is obtained；By institute
It states mixing presoma to mix with organic solvent, sequentially adds the poly-dopamine modified through sulfhydrylation hydroxyethyl starch and dispersing agent,
After mixing evenly, it is handled in ultrasonic generator, obtains graphene；
(2) by the cerium zirconium sosoloids of graphene made from (1) the step of selected parts by weight and selected parts by weight, lanthana modification
Ceria, V2O5, dispersing agent, coupling agent, heat stabilizer and solvent carry out mixed grinding, shearing, ultrasonic function under ultrasonication
Rate is 1000~1200W, and the time is 40~60min, obtains composite slurry slurry；
(3) sided corona treatment PET film corona: is carried out to 30 μ m thick PET using corona machine；
(4) use desk-top coating machine that mixed uniformly composite slurry slurry is coated on what sided corona treatment was crossed in a manner of hanging painting
On PET film, scraper height is 10~50mm；
(5) the coated PET film of the step (4) is dried；
(6) hot rolling processing is carried out to dried PET film using to roller roll squeezer, obtains PET base graphene heat conducting film；
(7) cutting edge is carried out to the PET base graphene heat conducting film after rolling processing to handle to obtain graphene composite material heat conducting film.
6. the preparation method of graphene composite material heat conducting film according to claim 5, which is characterized in that the step
(1) in,
The mass ratio of the crystalline graphite powder and the intercalator sodium carbonate is 1:5；
The dispersing agent is neopelex；
The mass ratio of the crystalline graphite powder and the poly-dopamine modified through sulfhydrylation hydroxyethyl starch, the dispersing agent is
1:10:80.
7. the preparation method of graphene composite material heat conducting film according to claim 5 or 6, which is characterized in that step (5)
In, the temperature of the drying is 50~80 DEG C, and the time is 12~18h.
8. the preparation method of graphene composite material heat conducting film according to claim 7, which is characterized in that in step (6),
The upper mold temperature of the heat rolling processing stabilizes to 80~110 DEG C, and lower die temperature stabilizes to 80~110 DEG C, and revolving speed is 30~
100r/min。
9. a kind of graphene composite material heat conducting film that the described in any item preparation methods of claim 5~8 are prepared.
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| CN110759336A (en) * | 2019-11-11 | 2020-02-07 | 董影影 | Preparation method of graphene and graphene |
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