CN109825053A - A kind of preparation method of thermally conductive PC film - Google Patents
A kind of preparation method of thermally conductive PC film Download PDFInfo
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- CN109825053A CN109825053A CN201811619189.7A CN201811619189A CN109825053A CN 109825053 A CN109825053 A CN 109825053A CN 201811619189 A CN201811619189 A CN 201811619189A CN 109825053 A CN109825053 A CN 109825053A
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Abstract
The present invention relates to PC films, disclose a kind of preparation method of thermally conductive PC film, solving existing preparation method need to be using graphene oxide as raw material, graphene oxide need to be restored again, complex process and the big problem that consumes energy, it includes the following steps, organic solvent is added in the PC of 0.4-0.6 parts of mass fractions and is mixed, PC/ organic solvent solution is obtained after PC is completely dissolved；The graphene of 0.1-0.6 parts of mass fractions is added into the resulting PC/ organic solvent solution of S1, obtains into film liquid after mixing；By the resulting upper surface for being coated on film forming plate at film liquid, film liquid is evaporated into when organic solvent and is being formed a film on plate not in flowing, the film forming plate with film liquid coating is obtained；The resulting film forming plate with film liquid coating is placed into heat drying in baking oven；Film forming plate after oven drying is cooling, after it is cooled to room temperature, molding film is taken off from film forming plate upper surface, obtains thermally conductive PC film, preparation method is simple, produces strong operability in batches.
Description
Technical field
The present invention relates to PC film, in particular to a kind of preparation method of thermally conductive PC film.
Background technique
Polycarbonate, abbreviation PC are the general name of a kind of high-molecular compound in strand containing carbonic ester, melt
Intensity is high, has good transparent, also with higher tensile strength, bending strength, elongation and a rigidity, resistance to ag(e)ing,
Excellent electrical properties, water absorption rate is low, so that the film as made from PC material is used widely in various industries field.
But since the heating conduction of pure PC material is poor, the PC film used in the electronic device or cooling module of fever is needed
It is modified or improves.A certain amount of graphene is mixed into existing production method in PC film, it is excellent conducive to graphene
Heat conduction and heat radiation performance, auxiliary PC film heat dissipation.
Such as Chinese patent that application publication number is CN105731435B " a kind of high tensile flexible graphene composite heat conduction film and
Preparation method ", it discloses a kind of preparation methods of graphene composite heat conduction film, comprising the following steps:
(1) graphene oxide by 1 mass parts average-size greater than 100 μm and the organic polymer of 0.01-1 mass parts are configured to
Concentration is 6-30mg/mL graphene oxide water solution, and the auxiliary agent of mass fraction 0.1-5% is added in the solution, and the auxiliary agent is
Degradable inorganic salts or degradable small organic molecule at 2500 DEG C at 2500 DEG C；After ultrasonic disperse, it is poured on mold
It is dried into graphene oxide membrane on plate, is then restored with reducing agent；
(2) graphene film after reduction is first warming up to 500-800 under atmosphere of inert gases with the rate of 0.1-1 DEG C/min
DEG C, keep the temperature 0.5-2h；
(3) it is warming up to 1000-1300 DEG C with the rate of 1-3 DEG C/min under atmosphere of inert gases, keeps the temperature 0.5-3h；
(4) it is warming up to 2500-3000 DEG C with the rate of 5-8 DEG C/min under atmosphere of inert gases, keeps the temperature 0.5-4h, Temperature fall
After porous graphene film can be obtained；
(5) super flexible high thermal conductivity graphene film can be obtained by suppressing graphene film under high pressure.
Disadvantage is that being added by graphene oxide as raw material, need again to restore graphene oxide after film forming, and
And also soak being needed to operate, there is inconvenience for batch production in complex process and energy consumption is big.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of preparation method of thermally conductive PC film,
Preparation method is simple and convenient, is not necessarily to redox graphene, produces strong operability in batches.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of thermally conductive PC film, includes the following steps,
S1: the PC of the 0.4-0.6 mass fraction organic solvent that 1 mass fraction is added is mixed, is dissolved completely in PC organic molten
The PC/ organic solvent solution that concentration range is 40wt%-60wt% is obtained after in agent；
S2: the graphene of 0.07-0.6 parts of mass fractions being added into the resulting PC/ organic solvent solution of S1, after mixing
To at film liquid；
S3: by the resulting upper surface for being coated on film forming plate at film liquid S2, it is flat in film forming that film liquid is evaporated into organic solvent
On plate not in flowing, the film forming plate with film liquid coating is obtained；
S4: the resulting film forming plate with film liquid coating of S3 is placed into baking oven, the dry 4-6h at 80-100 DEG C；
S5: the film forming plate after oven drying in S4 is cooling, after it is cooled to room temperature, work is used from film forming plate upper surface
Tool takes molding film off, obtains thermally conductive PC film.
By using above-mentioned technical proposal, after PC is dissolved in organic appearance solvent, then directly to disperse graphene in PC/ organic
Solvent solution is formed into film liquid, is constantly volatilized at organic solvent in film liquid, and the PC of original dissolution in organic solvent is gradually precipitated,
The PC of precipitation is dispersed in into film liquid, and the PC being precipitated volatilizees and gradually coated graphite alkene with organic solvent, so that PC
With graphene stable bond, remaining organic solvent is removed finally by baking oven, and heats and further strengthens the thin film strength of PC,
Thermally conductive PC film is obtained, there is good heat conductivity, the high advantage of intensity, and preparation method is simple and convenient, is not necessarily to oxygen reduction fossil
Black alkene produces strong operability in batches.
The present invention is further arranged to: the organic solvent is tetrahydrofuran, acetone, methylene chloride, chloroform, neighbour two
One of chlorobenzene.
By using above-mentioned technical proposal, PC all has preferably in tetrahydrofuran, acetone, methylene chloride, chloroform
Dissolubility, and recovery can be precipitated, while the low boiling point of tetrahydrofuran, acetone, methylene chloride, chloroform, it is volatile, it is mentioning
High efficiency, and make in S3 that organic solvent content is few in film liquid coating, avoid organic solvent a large amount of in S4 drying course
It is precipitated from film liquid coating and reduces PC film product intensity.
The present invention is further arranged to: the organic solvent is methylene chloride.
By using above-mentioned technical proposal, the polarity of methylene chloride and chloroform is small compared with tetrahydrofuran, acetone, is conducive to
Graphene disperses in PC/ organic solvent solution, while methylene chloride boiling point is low compared with chloroform, and volatilization is fast, and permeability is strong, easily
It is removed from PC film.
The present invention is further arranged to: when the PC mixed dissolution, the mass ratio of the PC and methylene chloride is 0.4-0.6
∶ 1。
By using above-mentioned technical proposal, when the mass ratio of PC and methylene chloride is 0.4-0.6: 1, PC/ methylene chloride is molten
The viscosity of liquid is small, is easy to shake dispersion after graphene is added, graphene agglomerate is avoided to agglomerate；The quality of PC and methylene chloride simultaneously
Higher than for 0.4-0.6: 1, PC concentration, cooperation methylene chloride quickly volatilizees, and film liquid coating forms block, and it is dynamic to film to reduce film forming liquid stream
Film forming is precipitated convenient for PC in the influence of liquid coating layer thickness distribution, and the PC film cavity formed after PC is precipitated is few, and the PC formed is thick
Degree is stablized at film liquid coating thickness relationship, is convenient for test and production control PC film thickness,
The present invention is further arranged to: it is described at graphene quality in film liquid be PC mass 1/4-2/3.
By using above-mentioned technical proposal, so that the 1/4-2/3 that graphene quality is PC mass is similarly in film forming coatings,
It avoids the very few heat-conducting effect of graphene poor, and avoids graphene excessively and make that film forming coatings internal bond is poor, intensity is low and is difficult into
Film.
The present invention is further arranged to: it is characterized in that, at film liquid coating method using first in film-forming plates upper surface in S3
Film liquid is added dropwise into, then strikes off to obtain with scraper plate or scraping blade.
By using above-mentioned technical proposal, roller coating or brushing are difficult to controlling at film liquid liquid layer thickness for coating；Paint roller and painting
Outside brush is exposed to, organic solvent is volatile, and PC particle or sheet body is easily precipitated at film liquid with what is be brushed in paint roller, leads into film liquid and applies
Cloth is uneven；
And spraying method improving to some extent at the control of film liquid liquid layer thickness to coating, but controlling extent is difficult；At film liquid towards at
Film plate sprays to be formed in spray process, and the drop of atomization is small, and large specific surface area, organic solvent is volatile, partly soluble PC
It is precipitated in advance and forms small PC particle, so that PC and graphene binding force are poor, thermally conductive PC film strength is poor；
And use and be added dropwise at film liquid, then in the mode struck off with scraper plate or scraping blade, it is on the one hand easy to control at film liquid liquid layer thickness
Precisely, on the other hand before film forming drop goes out, at film liquid sealed storage, reduce organic solvent volatilization, avoid being precipitated PC particle or
Sheet body, while for the PC of drop precipitation is added dropwise compared with drop, amount of precipitation is few, because being uniformly distributed in drop, avoids the production of PC particle
Raw possibility, convenient at film liquid film-forming and the raising thermally conductive PC film strength of product.
The present invention is further arranged to: the film forming plate is the sheet glass or quartz plate that surface smooth treatment is crossed.
By using above-mentioned technical proposal, the plate material that forms a film is silicate or silica, and the surface for the plate that forms a film is easy
The water in air is adsorbed, and forms silicone hydroxyl；Silicone hydroxyl can form hydrogen bond with methylene chloride, so that methylene chloride infiltration film forming is flat
The surface of plate and driving is spread on film forming plate at film liquid, convenient for forming a film at film liquid；It volatilizees simultaneously at organic solvent in film liquid
And after by baking oven removing remaining organic solvent, the binding force of PC be precipitated and the plate that forms a film is poor, is convenient for the thermally conductive PC film of finished product
It takes off.
In conclusion the invention has the following advantages:
1. making PC be first dissolved in organic solvent, then coated graphite alkene is precipitated, so that PC is steady with graphene using the principle of solution modeling
It is fixed to combine, remaining organic solvent is removed finally by baking oven, and heat and further strengthen the thin film strength of PC, obtains thermally conductive PC
Film has good heat conductivity, the high advantage of intensity, and preparation method is simple and convenient, is not necessarily to redox graphene, and batch is raw
Produce strong operability；
It is struck off using first be added dropwise in film-forming plates upper surface at film liquid, then with scraper plate or scraping blade in 2.S3 at film liquid coating method
Arrive, on the one hand at film liquid liquid layer thickness it is easy to control precisely, on the other hand reduce organic solvent volatilization, avoid be precipitated PC particle
Or PC sheet body or PC particle generate, convenient at film liquid film-forming and the raising thermally conductive PC film strength of product.
3. film forming plate is the sheet glass or quartz plate that surface smooth treatment is crossed, the water in air is easily adsorbed on surface, and
Formed silicone hydroxyl so that methylene chloride infiltration film forming plate surface and drive at film liquid film forming plate on spread, convenient at
Film liquid film forming；After removing remaining organic solvent at organic solvent volatilization in film liquid and by baking oven simultaneously, PC be precipitated and film forming
The binding force of plate is poor, takes off convenient for the thermally conductive PC film of finished product.
Specific embodiment
Embodiment one,
A kind of preparation method of thermally conductive PC film, includes the following steps,
S1: organic solvent is added in the PC of 0.4-0.6 parts of mass fractions and is mixed, is obtained after PC is dissolved completely in organic solvent
PC/ organic solvent solution；
S2: the graphene of 0.07-0.6 parts of mass fractions being added into the resulting PC/ organic solvent solution of S1, after mixing
To at film liquid；
S3: by the resulting upper surface for being coated on film forming plate at film liquid S2, it is flat in film forming that film liquid is evaporated into organic solvent
On plate not in flowing, the film forming plate with film liquid coating is obtained；
S4: the resulting film forming plate with film liquid coating of S3 is placed into baking oven, the dry 6h at 80 DEG C；
S5: the film forming plate after oven drying in S4 is cooling, after it is cooled to room temperature, work is used from film forming plate upper surface
Tool takes molding film off, obtains thermally conductive PC film.
It is struck off using first be added dropwise in film-forming plates upper surface at film liquid, then with scraper plate or scraping blade in S3 at film liquid coating method
It obtains, the thermally conductive PC film thickness of gained is 50-100 μm.
Organic solvent is methylene chloride, and film forming plate is glass slide.
Thermally conductive PC film is prepared according to above-mentioned preparation method, obtains embodiment 1A-1E, the dosage of each raw material is as follows.
| Embodiment 1A | Embodiment 1B | Embodiment 1C | Embodiment 1D | Embodiment 1E | |
| PC/g | 8 | 10 | 10 | 12 | 10 |
| Organic solvent/g | 20 | 20 | 20 | 20 | 20 |
| Graphene/g | 2 | 3 | 6 | 8 | 5 |
Embodiment 1A-1E obtains molding thermally conductive PC film, carries out thermal coefficient to resulting thermally conductive PC film, stretches
The test of performance, test result is as follows.
Comparative example one is set to comparative example three simultaneously.
Comparative example one,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1C, difference place is, PC dosage is 10g,
Graphene dosage is 0g.
Thermally conductive PC film resulting to comparative example one carries out the test of thermal coefficient, tensile property, and test result is as follows.
| Performance | Thermal coefficient (w/mk) | Tension failure rate (%) | Tensile strength (MPa) |
| Comparative example one | 0.22 | 25 | 50 |
Comparative example two,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1A, difference place is that graphene dosage is
2g changes PC dosage, to obtain the preparation method of comparative example 2A-2F, prepares thermally conductive PC film, preparation knot by corresponding preparation method
Fruit is as follows.
Comparative example three,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1C, difference place is, PC dosage is 12g,
Change graphene dosage, to obtain the preparation method of comparative example 3A-3F, prepares thermally conductive PC film by corresponding preparation method, prepare
As a result as follows.
By comparative example two and comparative example three it is found that when organic solvent is methylene chloride, quality when PC is mixed with methylene chloride
Than being preferably 0.4-0.6: 1, and graphene dosage is preferably the 1/4-2/3 of PC mass, in order to product film forming.
Embodiment two,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment one, difference place is, organic solvent four
Hydrogen furans, obtains embodiment 2A-2E, and the dosage embodiment 1A-1E of each raw material corresponds equal.
Embodiment 2A-2E obtains molding thermally conductive PC film, carries out thermal coefficient, insulation to resulting thermally conductive PC film
The test of intensity, tensile property, test result is as follows.
Embodiment three,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment one, difference place is, organic solvent third
Ketone, obtains embodiment 3A-3E, and the dosage embodiment 1A-1E of each raw material corresponds equal.
Embodiment 3A-3E obtains molding thermally conductive PC film, carries out thermal coefficient, insulation to resulting thermally conductive PC film
The test of intensity, tensile property, test result is as follows.
Example IV,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment one, difference place is, organic solvent three
Chloromethanes, obtains embodiment 4A-4E, and the dosage embodiment 1A-1E of each raw material corresponds equal.
Embodiment 4A-4E obtains molding thermally conductive PC film, carries out thermal coefficient, insulation to resulting thermally conductive PC film
The test of intensity, tensile property, test result is as follows.
Example IV,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment one, difference place is, organic solvent is neighbour
Dichloro-benzenes, obtains embodiment 5A-5E, and the dosage embodiment 1A-1E of each raw material corresponds equal.
Embodiment 4A-4E obtains molding thermally conductive PC film, carries out thermal coefficient, insulation to resulting thermally conductive PC film
The test of intensity, tensile property, test result is as follows.
Embodiment six,
A kind of preparation method of thermally conductive PC film uses roller coating at film liquid coating method in S3 based on the basis of embodiment 1C.
The thermally conductive PC film surface of gained finished product has hole sunken and protrusion.
Embodiment seven,
A kind of preparation method of thermally conductive PC film is used at film liquid coating method in S3 and is brushed based on the basis of embodiment 1C.
| Performance | Thermal coefficient (w/mk) | Tension failure rate (%) | Tensile strength (MPa) |
| Embodiment seven | 11.68 | 7 | 105 |
Embodiment eight,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1C, film forming plate is quartz slide.
Comparative example four,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1C, film forming plate is metal copper plate.Gained finished product
Thermally conductive PC film can not completely be taken off.
Comparative example five,
A kind of preparation method of thermally conductive PC film, based on the basis of embodiment 1C, film forming plate is PE plate.Gained finished product is thermally conductive
PC film can not be taken off.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (7)
1. a kind of preparation method of thermally conductive PC film, which is characterized in that include the following steps,
S1: the PC of the 0.4-0.6 mass fraction organic solvent that 1 mass fraction is added is mixed, is dissolved completely in PC organic molten
The PC/ organic solvent solution that concentration range is 40wt%-60wt% is obtained after in agent；
S2: the graphene of 0.07-0.6 parts of mass fractions being added into the resulting PC/ organic solvent solution of S1, after mixing
To at film liquid；
S3: by the resulting upper surface for being coated on film forming plate at film liquid S2, the film forming plate with film liquid coating is obtained；
S4: the resulting film forming plate with film liquid coating of S3 is placed into baking oven, the dry 4-6h at 80-100 DEG C；
S5: the film forming plate after oven drying in S4 is cooling, after it is cooled to room temperature, work is used from film forming plate upper surface
Tool takes molding film off, obtains thermally conductive PC film.
2. a kind of preparation method of thermally conductive PC film according to claim 1, which is characterized in that the organic solvent is four
One of hydrogen furans, acetone, methylene chloride, chloroform, o-dichlorohenzene.
3. a kind of preparation method of thermally conductive PC film according to claim 2, which is characterized in that the organic solvent is two
Chloromethanes.
4. a kind of preparation method of thermally conductive PC film according to claim 3, which is characterized in that the PC mixed dissolution
When, the mass ratio of the PC and methylene chloride is 0.4-0.6:1.
5. a kind of preparation method of thermally conductive PC film according to claim 3, which is characterized in that described at graphite in film liquid
Alkene quality is the 1/4-2/3 of PC mass.
6. a kind of preparation method of thermally conductive PC film according to claim 3, which is characterized in that at film liquid coating side in S3
Formula strikes off to obtain using first be added dropwise in film-forming plates upper surface at film liquid, then with scraper plate or scraping blade.
7. a kind of preparation method of thermally conductive PC film according to claim 3, which is characterized in that the film forming plate is table
The sheet glass or quartz plate that face smooth treatment is crossed.
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| CN101381511A (en) * | 2008-10-24 | 2009-03-11 | 南开大学 | Mono-layer graphite and polymer compound material and preparation and application thereof |
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| KR20150033517A (en) * | 2013-09-24 | 2015-04-01 | (주)유민에쓰티 | Weak acidic solution leak detection apparatus |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381511A (en) * | 2008-10-24 | 2009-03-11 | 南开大学 | Mono-layer graphite and polymer compound material and preparation and application thereof |
| CN103122075A (en) * | 2013-03-19 | 2013-05-29 | 苏州格瑞丰纳米科技有限公司 | High heat-conducting thin graphene-based composite material, as well as preparation method and application thereof |
| KR20150033517A (en) * | 2013-09-24 | 2015-04-01 | (주)유민에쓰티 | Weak acidic solution leak detection apparatus |
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Application publication date: 20190531 |