CN108384034A - A kind of PET/ graphenes heat conducting film and preparation method thereof - Google Patents
A kind of PET/ graphenes heat conducting film and preparation method thereof Download PDFInfo
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The present invention relates to grapheme material application and preparation field, a kind of PET/ graphenes heat conducting film and preparation method thereof is disclosed.The present invention uses graphene quantum dot as additive in a creative way, compared to existing high molecular surfactant and dispersant, new impurity, which will not be introduced, reduces heat conductivility, graphene quantum dot itself has good heat conductivility, the thermal emissivity rate that heat conducting film can be increased substantially improves the heat dissipation performance of heat conducting film.Graphene quantum dot is added in PET/ graphene heat conducting films can also effectively reduce the cohesion between graphene, improve stability of the graphene in heat radiation coating, keep it evenly dispersed in the slurry, and the harmful substance of harmful to human and environment is not will produce in radiation processes, environmentally protective, the thermal diffusion coefficient for the PET/ graphene composite material heat conducting film graphenes being prepared is 7~10 cm2/ S, thermal coefficient are 1000~1300 W/mk.
Description
Technical field
The present invention relates to grapheme material application and preparation field, more particularly, to a kind of PET/ graphenes heat conducting film and
Preparation method.
Background technology
For electronic product, effectively heat dissipation is used for the longevity to all parts to obtain lower operating temperature
Life and the speed of service will produce extremely important influence.With the continuous development of science and technology and progressive, especially computer chip is more
Coring has become mainstream, and the speed of service is constantly accelerated, and power also increases, and effective heat dissipation plays its speed of service
Very important effect.Currently, heat dissipation main product in the market is graphite-like heat conducting film, however, its heat dissipation performance is much
The radiating requirements that can not meet electronics and IT products radiating element become the heat dissipation bottleneck of most electronic product.
Graphene be it is a kind of arranged according to hexagon by carbon atom and carbon molecules made of being connected with each other, structure
It is highly stable, it is presently found most thin, maximum intensity, a kind of strongest novel nano-material of electrical and thermal conductivity performance.Graphene
Thermal coefficient is up to 5000W/mK, can be obtained extensively in fields such as coating, electronics, space flight military project, new energy, new materials
Using.Therefore, graphene is prepared graphene heat conducting film as main heat sink medium becomes research hotspot.
Existing graphene heat conducting film typically directly uses graphene as basis material, due to being easy between graphene
Cohesion, causes it to disperse in the slurry uneven, so that the heat conductivility of heat conducting film is bad.In order to reduce graphene it
Between cohesion, improve stability of the graphene in heat conducting film, it usually needs addition polyethylene wax, polyvinyl chloride, polyethylene pyrrole
The chemicals such as pyrrolidone are as dispersant or surfactant, although adding above-mentioned chemicals can subtract to a certain extent
Cohesion between few graphene, but, harmful to human and environment readily volatilized in radiation processes using chemicals.
Invention content
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of preparations of PET/ graphenes heat conducting film
Method.Add graphene quantum dot in the PET/ graphenes heat conducting film, effectively reduce the cohesion between graphene, make its
It is uniformly dispersed in slurry, and then improves the heat dissipation performance of heat conducting film, new impurity will not be introduced in radiation processes, it is environmentally protective.
Another object of the present invention is to provide a kind of PET/ graphenes heat conducting films.
The present invention is achieved by the following technical solutions：
A kind of preparation method of PET/ graphenes heat conducting film, includes the following steps：
S1. graphene slurry is prepared：
S11., graphene quantum dot, graphene and solvent are carried out to mixed grinding, shearing, ultrasonic work(under ultrasonication
Rate is 1000~1200W, and the time is 40~60min, obtains composite slurry material；
S12. it after Lauxite, curing agent and carbon nanotube being added into composite slurry made from step S11, is stirred
It mixes, rotating speed is 1000~1200rpm, and mixing time is 2~4h, obtains graphene heat dissipation slurry；
S13. heat-conducting metal powder, antifoaming agent and antioxidant is added in the graphene heat dissipation slurry that step S12 is obtained,
It is sufficiently stirred, rotating speed is 1200~1500rpm, and mixing time is 2~3h, after mixing up to graphene heat radiation coating；
Wherein, in step S1, the graphene heat dissipation slurry is made of following parts by weight of component：6~12 parts of graphene,
50~70 parts of Lauxite, 12~30 parts of graphene quantum dot, 2~5 parts of heat-conducting metal powder, 3~6 parts of carbon nanotube, solvent 12
1~5 part of~24 parts, 5~8 parts of curing agent, 12~16 parts of antifoaming agent and antioxidant；
S2.PET film coronas：Sided corona treatment is carried out using 30 μ m thick PET of corona machine pair；
S3. desk-top coating machine is used to be coated on mixed uniformly graphene heat dissipation slurry at corona in a manner of hanging painting
On the PET film managed, scraper height is 10~50mm；
S4. processing is dried in the coated PET films of step S3；
S5. it uses two pairs of rollers roll squeezer to carry out hot rolling processing to dried PET film, obtains PET base graphene heat conduction
Film；
S6. the PET base graphene heat conducting films after handling rolling carry out cutting edge and handle to obtain the consistent PET/ stones of size
Black alkene heat conducting film.
Further, in step S1, the graphene slurry is made of following parts by weight of component：8~12 parts of graphene,
60~65 parts of Lauxite, 18~30 parts of graphene quantum dot, 3~4 parts of heat-conducting metal powder, 3~5 parts of carbon nanotube, solvent 18
2~4 parts of~24 parts, 6~8 parts of curing agent, 12~15 parts of antifoaming agent and antioxidant.
Further, in step S1, the size of the graphene quantum dot is 2~4nm；
Further, in step S1, the heat-conducting metal powder is any one in copper powder, silver powder and aluminium powder, granularity 5
~10 μm；Purity >=96wt% of the carbon nanotube, ash content≤0.4wt%, specific surface area are 100~200m2/g。
PET bases graphene heat conducting film provided by the invention is by by heat conduction such as graphene, carbon nanotube and heat-conducting metal powder
The effect of be combineding with each other of material, the heat conduction network chain that the heat that heat source generates can be formed by above-mentioned three rapidly and evenly pass
The graphene for being diffused into film coated surface is led, surface graphene again rapidly gives out heat in the form of convection current, infra-red radiation
It goes, to achieve the effect that heat source temperature is greatly lowered.
Further, the curing agent is any one in ammonium chloride, ethylenediamine and vinyl triamine.
Further, the antifoaming agent is any one in silicone emulsion, organosiloxane, polypropylene glycerol aether.
Further, the solvent is any one in water, ethyl alcohol, isopropanol, butanone.
Further, the antioxidant is any one in ascorbic acid and sodium sulfite.
Further, the discharge power of corona machine is 0.3KVA~1.5KVA, 100~500 r/min of rotating speed in step S2.
Further, it refers to the dry 12h in 60 DEG C of vacuum drying chamber to be dried described in step S4.
Further, the upper mold temperature of the processing of heat rolling described in step S5 stabilizes to 80~110 DEG C, and lower die temperature is steady
It is set to 80~110 DEG C, rotating speed is 30~100r/min.
PET/ graphene heat conducting films are prepared in a kind of preparation method of above-mentioned PET/ graphenes heat conducting film.
Further, the thermal diffusion coefficient of the PET/ graphene composite materials heat conducting film is 7~10cm2/ S, heat conduction system
Number is 1000~1300W/mk.
Compared with prior art, the invention has the advantages that：
The present invention uses graphene quantum dot as additive in a creative way, compares existing high molecular surfactant
And dispersant, will not introduce new impurity reduces heat conductivility.Meanwhile graphene quantum dot itself has good thermal conductivity
Can, the thermal emissivity rate of heat conducting film can be increased substantially, the heat dissipation performance of heat conducting film is improved.In PET/ graphene heat conducting films
Graphene quantum dot, which is added, can also effectively reduce the cohesion between graphene, improve stability of the graphene in heat radiation coating,
Keep it evenly dispersed in the slurry, and the harmful substance of harmful to human and environment is not will produce in radiation processes, it is environmentally protective.
The present invention is using Lauxite as film forming matter, by Heat Conduction Materials such as graphene, carbon nanotube, heat-conducting metal powder
It is dispersed in film so that form contact and interaction between Heat Conduction Material, netted or chain structure shape is formed in system
State so that PET/ graphene heat conducting films form heat conduction network chain, and the heat conduction to which PET/ graphene heat conducting films be greatly improved dissipates
Hot property.
The present invention around graphene radiate slurry, technique is optimized, specifically to rolling pressure, coating thickness,
Solvent type and slurry viscosity are adjusted, and the heat conductivility of PET/ graphene heat conducting films, and energy are greatly improved
Realize large-scale production.
The thermal diffusion coefficient for the PET/ graphene heat conducting film graphenes that the present invention is prepared is 7~10cm2/ S, heat conduction
Coefficient is 1000~1300W/ (mk).
Specific implementation mode
It is further illustrated the present invention with reference to specific embodiment.Following embodiment is only illustrative examples, not structure
At inappropriate limitation of the present invention, the multitude of different ways that the present invention can be limited and be covered by invention content is implemented.Unless special
Do not mentionlet alone bright, reagent, compound and the equipment that the present invention uses is the art conventional reagent, compound and equipment.
Embodiment 1
A kind of preparation method of graphene heat dissipation slurry of the present embodiment, includes the following steps：
S1., graphene quantum dot, graphene and solvent are carried out to mixed grinding, shearing, ultrasonic power under ultrasonication
Composite slurry material is obtained for 1000W, time 60min；
S2. it after Lauxite, curing agent and carbon nanotube being added into composite slurry made from step S1, is stirred,
Rotating speed is 1000~1200rpm, and mixing time is 2~4h, obtains graphene heat dissipation slurry；
S3. heat-conducting metal powder, anti-oxidation and antifoaming agent is added in the graphene heat dissipation slurry that step S2 is obtained, fully
Stirring, rotating speed are 1200~1500rpm, and mixing time is 2~3h, after mixing up to graphene heat radiation coating.
Wherein, the mass fraction group of above-mentioned each component becomes：6 parts of graphene, 50 parts of Lauxite, 25 parts of auxiliary agent, graphite
12 parts of alkene quantum dot, 5 parts of heat-conducting metal powder, 3 parts of carbon nanotube, 12 parts of solvent, 5 parts of curing agent, 16 parts of antifoaming agent and anti-oxidation
1 part of agent.
The size of the graphene quantum dot is 2~4nm；The heat-conducting metal powder is arbitrary in copper powder, silver powder and aluminium powder
One kind, granularity are 5~10 μm；Purity >=95wt% of the carbon nanotube, ash content≤0.2wt%, specific surface area be 100~
200m2/g。
Further, the curing agent is any one in ammonium chloride, ethylenediamine and vinyl triamine.
Further, the antifoaming agent is any one in silicone emulsion, organosiloxane, polypropylene glycerol aether.
Further, the solvent is any one in water, ethyl alcohol, isopropanol, butanone.
Further, the antioxidant is any one in ascorbic acid and sodium sulfite.
Embodiment 2
With reference to the preparation method of embodiment 1, difference lies in step S1, ultrasonic power 1200W, time 40min；
The mass fraction group of wherein each component becomes：12 parts of graphene, 70 parts of Lauxite, 35 parts of auxiliary agent, graphene quantum dot 30
Part, 2 parts of heat-conducting metal powder, 6 parts of carbon nanotube, 24 parts of solvent, 8 parts of curing agent, 12 parts of antifoaming agent and 5 parts of antioxidant.
Embodiment 3
With reference to the preparation method of embodiment 1, difference lies in step S1, ultrasonic power 1100W, time 50min；
The mass fraction group of wherein each component becomes：8 parts of graphene, 60 parts of Lauxite, 18 parts of graphene quantum dot, heat-conducting metal
4 parts of 4 parts of powder, 4 parts of carbon nanotube, 18 parts of solvent, 6 parts of curing agent, 15 parts of antifoaming agent and antioxidant compositions.
Embodiment 4
With reference to the preparation method of embodiment 3, difference lies in the mass fraction groups of each component to become：9 parts of graphene, ureaformaldehyde
65 parts of resin, 24 parts of graphene quantum dot, 3 parts of heat-conducting metal powder, 5 parts of carbon nanotube, 20 parts of solvent, 6 parts of curing agent, defoaming
2 parts of 15 parts of agent and antioxidant.
Comparative example 1
This comparative example provides a kind of graphene heat radiation coating, the difference is that, the graphene dissipates with embodiment 4
Hot slurry is free of graphene quantum dot.
Comparative example 2
This comparative example provides a kind of graphene heat radiation coating, the difference is that, the graphene dissipates with embodiment 4
Hot coating is free of heat-conducting metal powder.
Comparative example 3
This comparative example provides a kind of graphene heat radiation coating, the difference is that, the graphene dissipates with embodiment 4
Hot coating not carbon nanotubes.
To the thermal conductivity of the graphene heat radiation coating of Examples 1 to 4 and comparative example 1~3, adhesive force, infrared emittance
It is detected with physicochemical properties such as hardness, wherein thermal conductivity is detected with reference to GB/T3651-2008, and adhesive force is with reference to GB/
T9286-98 is detected using hundred lattice testers, and infrared emittance is detected with reference to international endorsement ASTMC1371 standards,
Hardness is shown in Table 1 with reference to GB/T6739-1996, specific testing result.
1 physicochemical property test result of table
Embodiment 5
The present embodiment provides a kind of preparation methods of PET/ graphene composite materials heat conducting film, include the following steps：
S1. the graphene that selection example 4 is prepared radiates slurry as raw material；
S2.PET film coronas：Sided corona treatment is carried out using 30 μ m thick PET of corona machine pair, the discharge power of corona machine is
1KVA, rotating speed 300r/min；
S3. desk-top coating machine is used to be coated on mixed uniformly graphene heat dissipation slurry at corona in a manner of hanging painting
On the PET film managed, scraper height is 30mm；
S4. processing is dried in the coated PET films of step S3, it is dry specifically in 60 DEG C of vacuum drying chamber
12h；
S5. two pairs of rollers roll squeezer is used to carry out hot rolling processing to dried PET film, upper mold temperature in hot rolling process
100 DEG C are stabilized to, lower die temperature stabilizes to 100 DEG C, rotating speed 60r/min, obtains PET base graphene heat conducting films；
S6. the PET base graphene heat conducting films after handling rolling carry out cutting edge and handle to obtain the consistent PET/ stones of size
Black alkene heat conducting film.
Embodiment 6
The present embodiment provides a kind of preparation methods of PET/ graphene composite materials heat conducting film, include the following steps：
S1. the graphene that selection example 4 is prepared radiates slurry as raw material；
S2.PET film coronas：Sided corona treatment is carried out using 30 μ m thick PET of corona machine pair, the discharge power of corona machine is
0.3KVA, rotating speed 100r/min；
S3. desk-top coating machine is used to be coated on mixed uniformly graphene heat dissipation slurry at corona in a manner of hanging painting
On the PET film managed, scraper height is 10mm；
S4. processing is dried in the coated PET films of step S3, it is dry specifically in 60 DEG C of vacuum drying chamber
12h；
S5. two pairs of rollers roll squeezer is used to carry out hot rolling processing to dried PET film, upper mold temperature in hot rolling process
80 DEG C are stabilized to, lower die temperature stabilizes to 80 DEG C, rotating speed 30r/min, obtains PET base graphene heat conducting films；
S6. the PET base graphene heat conducting films after handling rolling carry out cutting edge and handle to obtain the consistent PET/ stones of size
Black alkene heat conducting film.
Embodiment 7
The present embodiment provides a kind of preparation methods of PET/ graphene composite materials heat conducting film, include the following steps：
S1. the graphene that selection example 4 is prepared radiates slurry as raw material；
S2.PET film coronas：Sided corona treatment is carried out using 30 μ m thick PET of corona machine pair, the discharge power of corona machine is
1.5KVA, rotating speed 500r/min；
S3. desk-top coating machine is used to be coated on mixed uniformly graphene heat dissipation slurry at corona in a manner of hanging painting
On the PET film managed, scraper height is 50mm；
S4. processing is dried in the coated PET films of step S3, it is dry specifically in 60 DEG C of vacuum drying chamber
12h；
S5. two pairs of rollers roll squeezer is used to carry out hot rolling processing to dried PET film, upper mold temperature in hot rolling process
110 DEG C are stabilized to, lower die temperature stabilizes to 110 DEG C, rotating speed 100r/min, obtains PET base graphene heat conducting films；
S6. the PET base graphene heat conducting films after handling rolling carry out cutting edge and handle to obtain the consistent PET/ stones of size
Black alkene heat conducting film.
Comparative example 4
This comparative example is substantially the same manner as Example 5, the difference is that, it is prepared using comparative example 1 in step S1
Graphene radiates slurry for raw material.
Comparative example 5
This comparative example is substantially the same manner as Example 5, the difference is that, it is prepared using comparative example 2 in step S1
Graphene radiates slurry for raw material.
Comparative example 6
This comparative example is substantially the same manner as Example 5, the difference is that, it is prepared using comparative example 3 in step S1
Graphene radiates slurry for raw material.
The PET/ graphene heat conducting film thermal properties that embodiment 5~7 and comparative example 4~6 are prepared are surveyed
Examination, it is specific as shown in table 2：
Table 2
The present invention illustrates the detailed process equipment and processing step of the present invention, art technology by above-described embodiment
Personnel are not it should be appreciated that the present invention is limited by above-described embodiment, and the above embodiments and description only describe this hairs
Bright principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, this is to this
It is for field technology personnel it will be apparent that these changes and improvements all fall within the protetion scope of the claimed invention.
Claims (9)
1. a kind of preparation method of PET/ graphenes heat conducting film, which is characterized in that include the following steps：
S1. graphene heat dissipation slurry is prepared：
S11., graphene quantum dot, graphene and solvent are carried out to mixed grinding, shearing under ultrasonication, ultrasonic power is
1000 ~ 1200 W, time are 40 ~ 60 min, obtain composite slurry material；
S12. it after Lauxite, curing agent and carbon nanotube being added into composite slurry material made from step S11, is stirred
It mixes, rotating speed is 1000 ~ 1200 rpm, and mixing time is 2 ~ 4 h, obtains graphene heat dissipation slurry initial product；
S13. heat-conducting metal powder, antifoaming agent and anti-oxidation are added in graphene that step S12 is obtained heat dissipation slurry initial product
Agent is sufficiently stirred, and rotating speed is 1200 ~ 1500 rpm, and mixing time is 2 ~ 3 h, after mixing up to graphene heat dissipation slurry；
Wherein, in step S1, the graphene heat dissipation slurry is made of following parts by weight of component：6 ~ 12 parts of graphene, ureaformaldehyde tree
50 ~ 70 parts of fat, 12 ~ 30 parts of graphene quantum dot, 2 ~ 5 parts of heat-conducting metal powder, 3 ~ 6 parts of carbon nanotube, 12 ~ 24 parts of solvent, solidification
1 ~ 5 part of 5 ~ 8 parts of agent, 12 ~ 16 parts of antifoaming agent and antioxidant；
S2.PET film coronas：Sided corona treatment is carried out using 30 μ m thick PET of corona machine pair；
S3. use desk-top coating machine that mixed uniformly graphene heat dissipation slurry is coated on what sided corona treatment was crossed in a manner of hanging painting
On PET film, scraper height is 10 ~ 50 mm；
S4. processing is dried in the coated PET films of step S3；
S5. it uses two pairs of rollers roll squeezer to carry out hot rolling processing to dried PET film, obtains PET base graphene heat conducting films；
S6. the PET base graphene heat conducting films after handling rolling carry out cutting edge and handle to obtain the consistent PET/ graphenes of size
Heat conducting film.
2. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that in step S1, the stone
Black alkene slurry is made of following parts by weight of component：8 ~ 12 parts of graphene, 60 ~ 65 parts of Lauxite, graphene quantum dot 18 ~ 30
Part, 3 ~ 4 parts of heat-conducting metal powder, 3 ~ 5 parts of carbon nanotube, 18 ~ 24 parts of solvent, 6 ~ 8 parts of curing agent, 12 ~ 15 parts of antifoaming agent and oxygen
2 ~ 4 parts of agent.
3. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that in step S1, the stone
The size of black alkene quantum dot is 2 ~ 4 nm.
4. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that described to lead in step S1
Thermometal powder is any one in copper powder, silver powder and aluminium powder, and granularity is 5 ~ 10 μm；
Purity >=96wt% of the carbon nanotube, ash content≤0.4wt%, specific surface area are 100~200m2/g。
5. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that corona machine in step S2
Discharge power is 0.3 KVA ~ 1.5 KVA, 100 ~ 500r/min of rotating speed.
6. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that dry described in step S4
Processing refers to the dry 12h in 60 DEG C of vacuum drying chamber.
7. the preparation method of PET/ graphenes heat conducting film according to claim 1, which is characterized in that heat rolling described in step S5
The upper mold temperature of pressure processing stabilizes to 80 ~ 110 DEG C, and lower die temperature stabilizes to 80 ~ 110 DEG C, and rotating speed is 30 ~ 100 r/min.
8. the PET/ graphene heat conduction that a kind of preparation method of any one of claim 1 ~ 7 PET/ graphenes heat conducting film obtains
Film.
9. PET/ graphenes heat conducting film according to claim 8, the thermal diffusion coefficient of the PET/ graphenes heat conducting film is 7~
10 cm2/ S, thermal coefficient are 1000~1300 W/mk.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251733A (en) * | 2018-09-19 | 2019-01-22 | 北京沃杰知识产权有限公司 | A kind of graphene composite material heat conducting film and preparation method thereof |
| CN109968845A (en) * | 2019-04-30 | 2019-07-05 | 山东华滋自动化技术股份有限公司 | A kind of manufacture craft of safeguard film for cellular phone |
| CN109968846A (en) * | 2019-04-30 | 2019-07-05 | 山东华滋自动化技术股份有限公司 | A kind of graphene coating process |
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