CN107804843B - A kind of preparation process of uniform high heat conduction graphite film coiled material - Google Patents
A kind of preparation process of uniform high heat conduction graphite film coiled material Download PDFInfo
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Abstract
The present invention relates to a kind of heat conduction membrane material applied to the electric terminal such as fields such as computer, mobile phone, LCD TV, the preparation processes of particularly a kind of high performance uniform high heat conduction graphite film coiled material of large scale.Its step are as follows：By polyimide film coiling, through being carbonized, being carbonized in advance, silicon carbide/graphene oxide dispersion spraying, graphitization are handled with calendering technology, obtain continuous large-sized artificial uniform high heat conduction graphite film coiled material.The present invention can prepare the ultra-thin artificial conduction graphite film that plane thermal conductivity can reach 1400 ~ 1900W/ (mk), thickness is 10 ~ 50um.The defects of being caused present invention improves the scuffing in coiled material graphite film preparation process at this stage and heat shrinkable unevenness and out-of-flatness problem, graphitization temperature and time are reduced while ensureing performance；And due to being bonded to each other sintering without graphite paper, reduce the transfering process of graphite paper before and after sintering, greatly simplify calendering, cross cutting and terminal film coating process, improve the utilization rate of graphite film coiled material.
Description
Technical field
The present invention relates to a kind of heat dissipation membrane material applied to the electric terminal such as fields such as computer, mobile phone and LCD TV,
The preparation process of particularly a kind of high performance uniform high heat conduction graphite film coiled material of large scale.
Background technology
At present, various types of electric terminals, such as laptop, LCD TV, tablet computer, smart mobile phone etc.,
The function of these equipment is stronger and stronger, and the less and less heat dissipation problem for causing to be difficult to avoid of size is more and more significant, this is main
It is that the calorific value of electric terminal is increasing or heat generating spot is increasingly concentrated.How heat dissipation problem is solved, be all electronics
The technical barrier that terminal production firm is faced.Using the electrographite film Heat Conduction Material that polyimide film is prepared as raw material, because
Its distinctive low-density and high thermal conductivity coefficient become the preferred material that hyundai electronics class product solves heat dissipation heat conduction technology.But
Due to the limitation of prior art processes, electrographite film is concentrated mainly on the research and development and production of flake graphite film, and production capacity is low, unfavorable
In the cross cutting and film process in later stage, production efficiency is constantly in low state, therefore how efficiently to give birth to practical efficiency
The continuous graphite film coiled material of output is into instantly popular subject.Three kinds of rulers can occur during carburizing sintering for polyimide film
Very little variation is broadly divided into the contraction of planar dimension, the dimensional contraction of thickness direction and the expansion of graphitizing process thickness direction, especially
It is that it is easy to appear free warpages and Folding Deformation and broken hole etc. due to heat shrinkable unevenness for carbonation stage polyimide film
Other defect causes the flatness of whole graphite film very low and reduces product fine rate, influence the operation of subsequent handling with
The promotion of production capacity.And since polyimide film graphitizing process backbone structure orientation is more complicated, graphitization temperature
It is very high, it generally requires and reaches 3000 ~ 3300 DEG C, increase manufacturing cost to a certain extent and equipment loss, limit artificial
The fast development of graphite film.
Also have successively at this stage correlative study team and manufacturer start to concentrate on the research of coiled material artificial stone ink film with
Production, such as middle stone, Suzhou lattice are excellent, maple and Dongguan letter hundred million etc. are expanded in Shanghai.Though certain achievement is achieved, most of producer
It is required for being bonded to each other with flexible graphite paper in graphite film preparation and is carbonized and is graphitized, however flexible graphite paper is often
It is broken in graphitizing process by huge tension, it is difficult to accomplish effectively to reuse, this preparation method undoubtedly increases
The process that graphite paper shifts before and after sintering and material and cost of labor.Coiled material graphite film is most of at present all can be in carbonization and graphite
Led to the problem of in change different degrees of scuffing and flatness be low, graphitization not exclusively and other defect, cause to roll
Process can not avoid the appearance of defective products, and row such as lightning line, bubble, fisheye, cut and the problem of fracture occur, influence most often
Whole performance and appearance and scrap.This is also that most of producer does not solve the problems, such as from technique yet, so as to limit high heat conduction
The continuity of performance artificial stone ink film and the promotion of breadth size, constrain the further development of artificial stone ink film production capacity.
For background above and problem, it can solve in existing graphite film manufacturing method that there are production capacities there is an urgent need to one kind
It is low, complex procedures are of high cost, shrink uneven poor flatness, a kind of uniform height for the problems such as continuity and breadth are size-constrained processed is led
The preparation method of hot graphite film coiled material.
Invention content
The purpose of the present invention is to provide a kind of preparation processes of uniform high heat conduction graphite film coiled material, can effectively reduce stone
Inkization temperature and graphitization time reduce the loss of graphitizing furnace.
To reach this purpose, the present invention specifically uses following technical scheme.
A kind of preparation process of uniform high heat conduction graphite film coiled material, includes the following steps.
Step（1）It is pre- between layers by string pendulum coiling mode coiling by polyimide film slitting into specified breadth
Stay the polyimides film coiled material of uniform gap.
Step（2）By step（1）Heat preservation 0.5 when middle polyimides film coiled material is warming up to 200 ~ 250 DEG C with 2 ~ 3 DEG C/min ~
1h, then while being warming up to 300 ~ 450 DEG C with 1 ~ 2 DEG C/min, keep the temperature 2 ~ 4h, and cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa environment in, with 5 ~ 7 DEG C/min's
Then heating rate is warming up to 650 ~ 750 DEG C from room temperature to 0.5 ~ 1h is kept the temperature at 500 ~ 550 DEG C with 0.5 ~ 1.5 DEG C/min
0.5 ~ 1.5h of Shi Baowen, then while being warming up to 900 DEG C ~ 1200 DEG C with 1 ~ 2 DEG C/min, keep the temperature 1 ~ 2h, and cooled to room temperature obtains
Be carbonized coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide/graphene oxide dispersion is protected in argon gas
Environment with the heating rate of 4 ~ 8 DEG C/min from room temperature to 1000 DEG C, is then warming up to 1700 ~ 1800 DEG C with 3 ~ 4 DEG C/min
0.5 ~ 1h is kept the temperature, then 2000 ~ 2200 DEG C of heat preservation 0.5h ~ 1h, 2300 ~ 2400 DEG C of heat preservation 0.5h ~ 1h are warming up to 1 ~ 2 DEG C/min,
1 ~ 3h is kept the temperature when being finally warming up to 2650 ~ 2850 DEG C with 1 ~ 2 DEG C/min, cooled to room temperature obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
A kind of preferred embodiment of preparation process as above-mentioned uniform high heat conduction graphite film coiled material：The string pendulum coiling side
Formula is the soft filament using 0.1 ~ 0.5mm of diameter, as coiling machine is attached to coiling on polyimide film, after coiling is completed
Take out flexible cord.
A kind of preferred embodiment of preparation process as above-mentioned uniform high heat conduction graphite film coiled material：Carrying out step（1）When
It is synchronous to carry out static elimination and dust removal process.
A kind of preferred embodiment of preparation process as above-mentioned uniform high heat conduction graphite film coiled material：Silicon carbide/the oxygen
Graphite alkene dispersion liquid concentration is 1wt% ~ 5wt%.
A kind of preferred embodiment of preparation process as above-mentioned uniform high heat conduction graphite film coiled material：Silicon carbide dispersion is warp
High temperature pre-oxidation treatment and the nanometer silicon carbide particle of silane coupling agent modification are scattered in by supersound process in DMAC solvents, oxygen
Graphite alkene dispersion liquid is graphene oxide ultrasonic disperse in DMAC solvents.
Beneficial effects of the present invention are.
String pendulum coiling mode coiling is used in the present invention as the coiled material of uniform gap between layers, can ensure polyamides Asia
Amine film coiled material does not generate moderate finite deformation and fracture while carbonation stage radial contraction has enough shrink spaces, can be with
The graphitization stage is reduced due to squeezing bonding or fracture caused by polyimides graphite film puffing foaming, improves the flat of integral membrane
Whole degree and acceptance rate reduce coiling mutual with graphite paper and the process and cost of transfer.
Pre- carbonization treatment is carried out to polyimides film coiled material before being carbonized in the present invention, can effectively remove former film may contain
Some moisture and impurity etc. further improve the degree of imidisation of polyimide film so that carbonation stage heat shrinkable is more
Uniformly, the graphite film that graphitized ordered degree is high, defect is few can be obtained.
Silicon carbide/graphene oxide is sprayed to polyimides carbonized film in the present invention, is capable of providing polyimides graphitization
Degree increases carbon content, plays induction graphitizing, obtains defect and lacks the artificial stone ink film of excellent performance, and can reduce stone
Inkization temperature and graphitization time, so as to reduce the loss of graphitizing furnace.
In conclusion wrinkle, buckling deformation and the flatness that present invention process can slow down carbonation stage graphite film are low
The problem of, improve quality and efficiency that Delanium membrane pressure is prolonged；The temperature and time in graphitization stage can be reduced, is improved poly-
Acid imide film degree of graphitization is prepared more preferably perfect uniform high heat conduction graphite film coiled material, can largely be improved most
The breadth of whole graphite film product meets the more project demands of client.
Specific embodiment
Embodiment 1.
Step（1）It is layer by string pendulum coiling mode coiling by the polyimide film slitting of thickness 25um into specified breadth
The polyimides film coiled material of uniform gap is reserved between layer, it is synchronous to carry out static elimination and dust removal process.
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 0.5h, then with 2 when being warming up to 200 DEG C with 3 DEG C/min
DEG C/min keeps the temperature 2h when being warming up to 400 DEG C, cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa carbide furnace in, with 6 DEG C/min's
0.5h is kept the temperature when heating rate is from room temperature to 500 DEG C, keeps the temperature 0.5h when being then warming up to 650 DEG C with 1.5 DEG C/min, then with
2 DEG C/min keeps the temperature 1h when being warming up to 900 DEG C, cooled to room temperature obtains carbonization coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；Spraying is by pre-
A concentration of 1.5wt% of silicon carbide dispersion of oxidation processes.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide in the graphitizing furnace of argon gas protection environment,
With the heating rate of 6 DEG C/min from room temperature to 1000 DEG C, 1800 DEG C of heat preservation 0.5h are then warming up to 4 DEG C/min, then with 2
DEG C/min be warming up to 2000 DEG C heat preservation 0.5h, 2300 DEG C heat preservation 0.5h, keep the temperature 1h when being finally warming up to 2800 DEG C with 2 DEG C/min,
Cooled to room temperature obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
Through measuring its mean coefficient of heat conductivity as 1805W/ (mk), averag density reaches the conduction graphite film that above-mentioned technique obtains
To 2.1g/cm3, thickness is 10um ± 1um.
Embodiment 2.
Step（1）It is layer by string pendulum coiling mode coiling by the polyimide film slitting of thickness 38um into specified breadth
The polyimides film coiled material of uniform gap is reserved between layer, it is synchronous to carry out static elimination and dust removal process.
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 0.5h, then with 2 when being warming up to 200 DEG C with 3 DEG C/min
DEG C/min keeps the temperature 2h when being warming up to 380 DEG C, cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa carbide furnace in, with 6 DEG C/min's
0.5h is kept the temperature when heating rate is from room temperature to 500 DEG C, keeps the temperature 0.5h when being then warming up to 650 DEG C with 1.5 DEG C/min, then with
2 DEG C/min keeps the temperature 1h when being warming up to 900 DEG C, cooled to room temperature obtains carbonization coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；Spraying is by pre-
A concentration of 1wt% of silicon carbide dispersion of oxidation processes.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide in the graphitizing furnace of argon gas protection environment,
With the heating rate of 6 DEG C/min from room temperature to 1000 DEG C, 1800 DEG C of heat preservation 0.5h are then warming up to 4 DEG C/min, then with 2
DEG C/min be warming up to 2200 DEG C heat preservation 0.5h, 2400 DEG C heat preservation 0.5h, keep the temperature 1h when being finally warming up to 2650 DEG C with 2 DEG C/min,
Cooled to room temperature obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
Through measuring its mean coefficient of heat conductivity as 1705W/ (mk), averag density reaches the conduction graphite film that above-mentioned technique obtains
To 2.05g/cm3, thickness is 17um ± 1um.
Embodiment 3.
Step（1）It is layer by string pendulum coiling mode coiling by the polyimide film slitting of thickness 38um into specified breadth
The polyimides film coiled material of uniform gap is reserved between layer, it is synchronous to carry out static elimination and dust removal process.
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 0.5h, then with 2 when being warming up to 250 DEG C with 3 DEG C/min
DEG C/min keeps the temperature 2h when being warming up to 380 DEG C, cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa carbide furnace in, with 4 DEG C/min's
0.5h is kept the temperature when heating rate is from room temperature to 500 DEG C, 1h is kept the temperature when being then warming up to 650 DEG C with 1.5 DEG C/min, then with 2
DEG C/min keeps the temperature 1h when being warming up to 1000 DEG C, cooled to room temperature obtains carbonization coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；Spraying is by pre-
A concentration of 2.5wt% of silicon carbide dispersion of oxidation processes.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide in the graphitizing furnace of argon gas protection environment,
With the heating rate of 6 DEG C/min from room temperature to 1000 DEG C, 1800 DEG C of heat preservation 0.5h are then warming up to 4 DEG C/min, then with 2
DEG C/min be warming up to 2200 DEG C heat preservation 0.5h, 2400 DEG C heat preservation 0.5h, keep the temperature 1h when being finally warming up to 2850 DEG C with 2 DEG C/min,
Cooled to room temperature obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
Through measuring its mean coefficient of heat conductivity as 1905W/ (mk), averag density reaches the conduction graphite film that above-mentioned technique obtains
To 2.12g/cm3, thickness is 17um ± 1um.
Embodiment 4.
Step（1）It is layer by string pendulum coiling mode coiling by the polyimide film slitting of thickness 60um into specified breadth
The polyimides film coiled material of uniform gap is reserved between layer, it is synchronous to carry out static elimination and dust removal process.
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 1h when being warming up to 250 DEG C with 3 DEG C/min, then with 2 DEG C/
Min keeps the temperature 2.5h when being warming up to 400 DEG C, cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa carbide furnace in, with 6 DEG C/min's
0.5h is kept the temperature when heating rate is from room temperature to 500 DEG C, keeps the temperature 0.5h when being then warming up to 650 DEG C with 1 DEG C/min, 750 DEG C
Shi Baowen 0.5h, then while being warming up to 1100 DEG C with 1.5 DEG C/min, keep the temperature 1h, and cooled to room temperature obtains carbonization coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；Spraying is by pre-
A concentration of 3wt% of silicon carbide dispersion of oxidation processes.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide in the graphitizing furnace of argon gas protection environment,
With the heating rate of 6 DEG C/min from room temperature to 1000 DEG C, 1800 DEG C of heat preservation 0.5h are then warming up to 3 DEG C/min, then with 2
DEG C/min be warming up to 2200 DEG C heat preservation 1h, 2400 DEG C heat preservation 1h, keep the temperature 1.5h when being finally warming up to 2800 DEG C with 2 DEG C/min, from
It is so cooled to room temperature, obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
Through measuring its mean coefficient of heat conductivity as 1510W/ (mk), averag density reaches the heat dissipation graphite film that above-mentioned technique obtains
To 1.89 g/cm3, thickness is 32um ± 1um.
Embodiment 5.
Step（1）It is layer by string pendulum coiling mode coiling by the polyimide film slitting of thickness 75um into specified breadth
The polyimides film coiled material of uniform gap is reserved between layer, it is synchronous to carry out static elimination and dust removal process.
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 1h when being warming up to 250 DEG C with 3 DEG C/min, then with 2 DEG C/
Min keeps the temperature 2.5h when being warming up to 450 DEG C, cooled to room temperature obtains pre- carbonization coiled material.
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa carbide furnace in, with 6 DEG C/min's
0.5h is kept the temperature when heating rate is from room temperature to 550 DEG C, keeps the temperature 0.5h when being then warming up to 650 DEG C with 1 DEG C/min, 750 DEG C
Shi Baowen 0.5h, then while being warming up to 1200 DEG C with 1.5 DEG C/min, keep the temperature 1h, and cooled to room temperature obtains carbonization coiled material.
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；Spraying is by pre-
A concentration of 5wt% of silicon carbide dispersion of oxidation processes.
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide in the graphitizing furnace of argon gas protection environment,
With the heating rate of 6 DEG C/min from room temperature to 1000 DEG C, 1800 DEG C of heat preservation 0.5h are then warming up to 3 DEG C/min, then with 2
DEG C/min is warming up to 2200 DEG C of heat preservation 1h, 2400 DEG C of heat preservation 1h, and 2h is kept the temperature when being finally warming up to 2800 DEG C with 2 DEG C/min, it is natural
It is cooled to room temperature, obtains graphitization coiled material.
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the big ruler of the uniform continuity of thickness
Very little high heat conduction graphite film coiled material.
Through measuring its mean coefficient of heat conductivity as 1405W/ (mk), density reaches the heat dissipation graphite film that above-mentioned technique obtains
1.79 g/cm3, thickness is 50um ± 1um.
The basic principle and key feature of the present invention have been described in detail above in association with real case.The technical staff of the industry
Reason is not it will be appreciated that the present invention is limited by the above embodiment, and the above embodiment described in specification with only illustrating this hair
Bright basic principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Variation will be included in the claimed scope of the invention with improving, and claimed range of the invention is by appended claims
And its equivalent thereof.
Claims (4)
1. a kind of preparation process of uniform high heat conduction graphite film coiled material, includes the following steps：
Step（1）It is equal to reserve between layers by string pendulum coiling mode coiling by polyimide film slitting into specified breadth
The polyimides film coiled material in even gap；
Step（2）By step（1）Middle polyimides film coiled material keeps the temperature 0.5 ~ 1h when being warming up to 200 ~ 250 DEG C with 2 ~ 3 DEG C/min,
2 ~ 4h is kept the temperature when being warming up to 300 ~ 450 DEG C again with 1 ~ 2 DEG C/min, cooled to room temperature obtains pre- carbonization coiled material；
Step（3）By step（2）In be carbonized in advance coiled material absolute pressure be 10 ~ 30pa environment in, with the liter of 5 ~ 7 DEG C/min
Warm rate is from room temperature to 0.5 ~ 1h of heat preservation at 500 ~ 550 DEG C, when being then warming up to 650 ~ 750 DEG C with 0.5 ~ 1.5 DEG C/min
1 ~ 2h is kept the temperature when keeping the temperature 0.5 ~ 1.5h, then 900 DEG C ~ 1200 DEG C are warming up to 1 ~ 2 DEG C/min, cooled to room temperature obtains carbon
Change coiled material；
Step（4）By step（3）Middle carbonization coiled material surface spraying silicon carbide/graphene oxide dispersion；
Step（5）By step（4）The carbonization coiled material of middle surface spraying silicon carbide/graphene oxide dispersion is in argon gas protection ring
Border with the heating rate of 4 ~ 8 DEG C/min from room temperature to 1000 DEG C, is then warming up to 1700 ~ 1800 DEG C with 3 ~ 4 DEG C/min
0.5 ~ 1h is kept the temperature, then 2000 ~ 2200 DEG C of heat preservation 0.5h ~ 1h, 2300 ~ 2400 DEG C of heat preservation 0.5h ~ 1h are warming up to 1 ~ 2 DEG C/min,
1 ~ 3h is kept the temperature when being finally warming up to 2650 ~ 2850 DEG C with 1 ~ 2 DEG C/min, cooled to room temperature obtains graphitization coiled material；
Step（6）By step（5）Middle graphitization coiled material is delayed through cold-pressed steel roll-in obtains the uniform continuity large scale volume of thickness
Fill high heat conduction graphite film；
The string pendulum coiling mode is the soft filament using 0.1 ~ 0.5mm of diameter, as coiling machine is attached to polyimides
Coiling on film, coiling take out flexible cord after completing.
2. a kind of preparation process of uniform high heat conduction graphite film coiled material according to claim 1, it is characterised in that：Into
Row step（1）When synchronize and carry out static elimination and dust removal process.
3. a kind of preparation process of uniform high heat conduction graphite film coiled material according to claim 1, it is characterised in that：It is described
A concentration of 1wt% ~ 5wt% of silicon carbide/graphene oxide dispersion.
4. a kind of preparation process of uniform high heat conduction graphite film coiled material according to claim 1 or 3, it is characterised in that：
Silicon carbide dispersion is the nanometer silicon carbide particle through high temperature pre-oxidation treatment and silane coupling agent modification by supersound process point
It dissipates in DMAC solvents, graphene oxide dispersion is graphene oxide ultrasonic disperse in DMAC solvents.
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Address after: 215200 Wujiang 168 economic and Technological Development Zone, Suzhou, Jiangsu Patentee after: Suzhou Shihua new material Polytron Technologies Inc Address before: 215200 Wujiang 168 economic and Technological Development Zone, Suzhou, Jiangsu Patentee before: Suzhou Shihua New Material Technology Co., Ltd. |