CN108726505A - A kind of carbon nanotube heat conduction film and its manufacturing method - Google Patents
A kind of carbon nanotube heat conduction film and its manufacturing method Download PDFInfo
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- CN108726505A CN108726505A CN201810736301.9A CN201810736301A CN108726505A CN 108726505 A CN108726505 A CN 108726505A CN 201810736301 A CN201810736301 A CN 201810736301A CN 108726505 A CN108726505 A CN 108726505A
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- carbon nanotube
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
Abstract
The present invention provides a kind of preparation methods of carbon nanotube heat conduction film.The present invention is compound with polyimide fiber by carbon nanotube by high-voltage electrostatic spinning, both the excellent heat conduction of carbon nanotube and electric conductivity had been remained, the good mechanical performance of polyimide fiber and heat resistance, radiance, chemical stability, humidity resistance are remained again, the advantages of making full use of the two, the carbon nanotube heat conduction film being prepared have excellent heat conductivility and mechanical performance.Embodiment the experimental results showed that, the thermal coefficient of carbon nanotube heat conduction film provided by the invention is 1500W/mk or so, and the carbon nanotube heat conduction film can bear the counterweight of 500g and not break up, and will not be broken when bending angle is 90~180 °.
Description
Technical field
The present invention relates to Heat Conduction Material technical fields, and in particular to a kind of carbon nanotube heat conduction film and its manufacturing method.
Background technology
21 century is information big data epoch and electronic technology development epoch.Electronic product also becomes more and more frivolous.
Although the internal structure power density of electronic product improves, the heat generated during its use is difficult to come out,
Constantly accumulation forms high temperature to heat.High temperature influences whether the stability of electronic product operation, substantially reduces its service life.Cause
This, has higher requirement to Electronic Product Core component heat sink material at present.
In recent years, carbon nano tube compound material is the new hot spot of Heat Conduction Material research.The carbon reported in the prior art is received
Mitron film is typically compound by carbon nanotube and common paper fiber (such as lumber fibre), and common paper fiber generally existing hardness
Problem low, flexibility is poor, and non-refractory, easy cracking, have certain limitation in practical applications.
Invention content
The purpose of the present invention is to provide a kind of carbon nanotube heat conduction film and its manufacturing method, use are provided by the invention
The carbon nanotube heat conduction film that method is prepared has excellent heat conductivility and mechanical performance.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preparation methods of carbon nanotube heat conduction film, include the following steps：
It carries out discongesting processing after polyimide fiber is mixed with water, gained, which is discongested polyimide fiber, is impregnated in polyamides
In imide resin solution, shear treatment is carried out after gained dipping polyimide fiber is mixed with water, obtains polyimide fiber
Dispersion liquid；
Shear treatment is carried out after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube, gained is spun
Silk dispersion liquid carries out high-voltage electrostatic spinning, obtains carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is subjected to charing process, graphitization processing and rolling successively, is obtained
Carbon nanotube heat conduction film.
Preferably, the carbon nanotube is the multi-walled carbon nanotube of crystal whisker-shaped.
Preferably, the polyimide fiber and the mass ratio of carbon nanotube are 1：(1~3).
Preferably, the mass concentration of polyimide resin is 1.5~2.5% in the polyimide resin solution.
Preferably, the dispersion liquid of the carbon nanotube includes carbon nanotube, aqueous dispersion and water；The carbon nanotube
The mass concentration of carbon nanotube is 0.5~1.5% in dispersion liquid, and the mass concentration of aqueous dispersion is 0.025~0.075%.
Preferably, the operating parameter of the high-voltage electrostatic spinning is：Using 18# syringe needles, between spinning head and receiving screen
Distance is 14~16cm, and electrostatic pressure is 10~25KV.
Preferably, the charing process includes the following steps：
650~750 DEG C are warming up to 5~20 DEG C/min, keeps the temperature 40~150min；
Continue to be warming up to 850~1200 DEG C with 5~10 DEG C/min, keeps the temperature 5~10h.
Preferably, the graphitization processing includes the following steps：
In protective atmosphere, 2000~2800 DEG C are warming up to 10~20 DEG C/min, keeps the temperature 5~30h.
The present invention provides the carbon nanotube heat conduction films that preparation method described in above-mentioned technical proposal is prepared.
Preferably, the thickness of the carbon nanotube heat conduction film is 5~25 μm, and density is 0.1~0.6g/cm3。
The present invention provides a kind of preparation methods of carbon nanotube heat conduction film, include the following steps：By polyimides fibre
Dimension carries out discongesting processing after mixing with water, and gained, which is discongested polyimide fiber, to be impregnated in polyimide resin solution, by institute
It must impregnate after polyimide fiber is mixed with water and carry out shear treatment, obtain polyimide fiber dispersion liquid；By polyamides Asia
Amine fiber dispersion carries out shear treatment after being mixed with the dispersion liquid of carbon nanotube, and gained spinning dispersion liquid is carried out high-pressure electrostatic
Spinning obtains carbon nanotube-polyimide fiber film；The carbon nanotube-polyimide fiber film is subjected to charcoal successively
Change processing, graphitization processing and rolling obtain carbon nanotube heat conduction film.The present invention is by high-voltage electrostatic spinning by carbon nanotube
Compound with polyimide fiber, the two uniformly overlaps in recombination process, forms network-like structure, it is excellent both to have remained carbon nanotube
Different heat conduction and electric conductivity, and remain the good mechanical performance of polyimide fiber and heat resistance, radiance, chemistry
Stability, humidity resistance, the advantages of both making full use of, the carbon nanotube heat conduction film being prepared has excellent thermal conductivity
Energy and mechanical performance.Embodiment the experimental results showed that, the thermal coefficient of carbon nanotube heat conduction film provided by the invention is
1500W/mk or so, and the carbon nanotube heat conduction film can bear the counterweight of 500g and not break up, in bending angle
It will not be broken when being 90~180 °.
In addition, preparation method provided by the invention is easy to operate, it is convenient for large-scale production.
Specific implementation mode
The present invention provides a kind of preparation methods of carbon nanotube heat conduction film, include the following steps：
It carries out discongesting processing after polyimide fiber is mixed with water, gained, which is discongested polyimide fiber, is impregnated in polyamides
In imide resin solution, shear treatment is carried out after gained dipping polyimide fiber is mixed with water, obtains polyimide fiber
Dispersion liquid；
Shear treatment is carried out after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube, gained is spun
Silk dispersion liquid carries out high-voltage electrostatic spinning, obtains carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is subjected to charing process, graphitization processing and rolling successively, is obtained
Carbon nanotube heat conduction film.
The present invention carries out discongesting processing after mixing polyimides (PI) fiber with water, and gained is discongested polyimide fiber
It is impregnated in polyimide resin solution, carries out shear treatment after gained dipping polyimide fiber is mixed with water, gathered
Imide fiber dispersion liquid.In the present invention, the length of the polyimide fiber is preferably 4~6mm, more preferably 5mm.This
Invention does not have the source of the polyimide fiber special restriction, using commercial goods well known to those skilled in the art
?.In the present invention, the mass ratio of the polyimide fiber and water is preferably 1：(50~150), more preferably 1:100.
The present invention handles not special restriction for described discongest, using the technical side well known to those skilled in the art for discongesting processing
Case；In the present invention, the time for discongesting processing is preferably 15~30min.
In the present invention, in the polyimide resin solution mass concentration of polyimide resin be preferably 1.5~
2.5%, more preferably 2%.In the present invention, the solvent in the polyimide resin solution is preferably water.The present invention for
The not special restriction of the dipping, using the technical solution of dipping well known to those skilled in the art；In the present invention,
The dipping preferably carries out at room temperature, and the time of the dipping is preferably 0.5~1h.In the present invention, the polyimides
Resin has cementation, discongests polyimide fiber using polyimide resin solution dipping, the polyamides can be kept sub-
The structural intergrity of amine fiber.
In the present invention, the mass ratio of the dipping polyimide fiber and water is preferably 1：(100~500), more preferably
It is 1：(200~400).In the present invention, in the present invention, the rotating speed of the shear treatment is preferably 3800~4200r/min；
The time of the shear treatment is preferably 30~50min.
After obtaining polyimide fiber dispersion liquid, the present invention is by point of the polyimide fiber dispersion liquid and carbon nanotube
Shear treatment is carried out after dispersion liquid mixing, gained spinning dispersion liquid is subjected to high-voltage electrostatic spinning, obtains carbon nanotube-polyimides
Fiber membrane.In the present invention, preferably 2~5 μm of the length of the carbon nanotube, diameter preferably 30~150nm.In the present invention
In, the carbon nanotube is preferably according to document (Sun X G, Qiu Z W, Chen L, et al.Industrial synthesis
of Whisker carbon nanotubes[C]//Materials Science Forum.Trans Tech
Publications Ltd.,2016,852:514) method disclosed in is prepared；Be prepared in this way is straight line
Type high-purity high-crystallinity carbon nanotube.In the present invention, the polyimide fiber and the mass ratio of carbon nanotube are preferably
1：(1~3), more preferably 1：2.
In the present invention, the dispersion liquid of the carbon nanotube preferably includes carbon nanotube, aqueous dispersion and water；The carbon
The mass concentration of carbon nanotube is preferably 0.5~1.5% in the dispersion liquid of nanotube, and more preferably 1%；The matter of aqueous dispersion
It is preferably 0.025~0.075% to measure concentration, and more preferably 0.03~0.05%.Kind of the present invention for the aqueous dispersion
Class does not have special restriction, specific such as lauryl sodium sulfate using aqueous dispersion well known to those skilled in the art.
The present invention does not have the preparation method of the dispersion liquid of the carbon nanotube special restriction, using known to those skilled in the art
Material dispersion technical solution；Carbon nanotube is preferably carried out ball milling 1 by the present invention under the conditions of 200~400r/min
~2h carries out supersound process and shear treatment, obtains carbon nanotube successively after mixing gained carbon nanotube with second alcohol and water
Dispersion liquid.In the present invention, the time of the supersound process is preferably 1~2h；Power of the present invention for the supersound process
There is no special restriction, using power well known to those skilled in the art.In the present invention, the rotating speed of the shear treatment
Preferably 3800~4200r/min；The time of the shear treatment is preferably 1~2h.
At the shearing that the present invention carries out after being mixed with the dispersion liquid of carbon nanotube for the polyimide fiber dispersion liquid
The rotating speed of reason is preferably 3800~4200r/min；The time of the shear treatment is preferably 1~2h.
In the present invention, the operating parameter of the high-voltage electrostatic spinning is preferably：Using 18# syringe needles, spinning head and reception
The distance between screen is 14~16cm, and electrostatic pressure is 10~25KV.In an embodiment of the present invention, specifically by spinning dispersion liquid
It is placed in metering pump, using 18# syringe needles, control the distance between spinning head and receiving screen are 14~16cm, and capillary connection is high
The anode of voltage generator, receiving screen connect the cathode of high-voltage generator；The electrostatic pressure for applying 10~25KV on syringe needle, into
Horizontal high voltage electrostatic spinning；Spinning dispersion liquid is sprayed by spinning head, collects on receiving screen that obtain carbon nanotube-poly- after 4~6h
Imide fiber film.In the present invention, the carbon nanotube-polyimide fiber film thickness preferably≤30 μm.
The present invention uses high-voltage electrostatic spinning technology, and the fibrousness of polyimide fiber can be made to refine, and without activity
Group will not be crosslinked and be connected between fiber；So that carbon nanotube is uniformly overlapped with polyimide fiber simultaneously, is formed network-like
Structure the advantages of both making full use of, makes the carbon nanotube heat conduction film being prepared have excellent heat conductivility and machinery
Performance.
After obtaining carbon nanotube-polyimide fiber film, the present invention is by the carbon nanotube-polyimide fiber film
Charing process, graphitization processing and rolling are carried out successively, obtain carbon nanotube heat conduction film.The present invention is preferably by the carbon nanometer
Pipe-polyimide fiber film, which is placed in tube furnace, carries out charing process；In the present invention, the charing process preferably include with
Lower step：
650~750 DEG C are warming up to 5~20 DEG C/min, keeps the temperature 40~150min；
Continue to be warming up to 850~1200 DEG C with 5~10 DEG C/min, keeps the temperature 5~10h.
The present invention removes the impurity such as nitrogen, hydrogen, the oxygen in carbon nanotube-polyimide fiber film member by charing process
Element only leaves carbonaceous film.
Gained film after charing process is preferably placed in graphitizing furnace and carries out graphitization processing by the present invention；In the present invention
In, the graphitization processing preferably includes following steps：
In protective atmosphere, 2000~2800 DEG C are warming up to 10~20 DEG C/min, keeps the temperature 5~30h.
The present invention does not have special restriction for the protective gas type for providing the protective atmosphere, using art technology
Protective gas known to personnel, it is specific such as argon gas or nitrogen.
The present invention changes the crystal structure of carbon by graphitization processing, improves the electrical and thermal conductivity performance of carbon nano-tube film.
The present invention is for the not special restriction of the rolling, using the technical side of rolling well known to those skilled in the art
Case.In an embodiment of the present invention, specifically the film after graphitization processing is rolled using twin rollers.
The present invention provides the carbon nanotube heat conduction films that any one of above-mentioned technical proposal preparation method is prepared.
In the present invention, the thickness of the carbon nanotube heat conduction film is preferably 5~25 μm, more preferably 10~20 μm；Density is preferred
For 0.1~0.6g/cm3, more preferably 0.2~0.4g/cm3。
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
It carries out discongesting processing 30min after 0.5g polyimide fibers (length 5mm) are mixed with 50mL water, gained is dredged
Solution polyimide fiber is impregnated in 1h in the polyimide resin solution that 100mL mass concentrations are 2%, and gained dipping polyamides is sub-
Amine fiber carries out shear treatment 40min after being mixed with 100mL water under the conditions of 4000r/min, obtains polyimide fiber dispersion
Liquid；
The multi-walled carbon nanotube for weighing 0.5g crystal whisker-shapeds carries out ball milling 1.5h under the conditions of 220r/min, by the carbon after ball milling
Nanotube carries out supersound process 1h after being mixed with 50mL water and 0.025g lauryl sodium sulfate, under the conditions of 4000r/min into
Row shear treatment 1h, obtains the dispersion liquid of carbon nanotube；
It is carried out under the conditions of 4000r/min after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube
Gained spinning dispersion liquid is placed in metering pump by shear treatment 1h, using 18# syringe needles, is controlled between spinning head and receiving screen
Distance is 15cm, and capillary connects the anode of high-voltage generator, and receiving screen connects the cathode of high-voltage generator, on syringe needle
Apply the electrostatic pressure of 25KV, carries out high-voltage electrostatic spinning；Spinning dispersion liquid is sprayed by spinning head, is collected on receiving screen after 5h
Obtain carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is placed in tube furnace and carries out charing process, specifically with 10 DEG C/
Min is warming up to 700 DEG C, keeps the temperature 2h；Continue to be warming up to 1100 DEG C with 8 DEG C/min, keep the temperature 8h, after be cooled to room temperature after take
Go out；Gained film after charing process is placed in graphitizing furnace and carries out graphitization processing, specifically under nitrogen protection, with 15
DEG C/min is warming up to 2600 DEG C, keep the temperature 25h, after be cooled to room temperature after take out；Using twin rollers to institute after graphitization processing
It obtains film to be rolled, obtains carbon nanotube heat conduction film.
The thickness of carbon nanotube heat conduction film manufactured in the present embodiment is 15 μm, and density is about 0.375g/cm3。
Counterweight is hung in the lower section of carbon nanotube heat conduction film manufactured in the present embodiment, as a result, it has been found that the aromatic carbon nanotube
Heat conduction film can bear the counterweight of 500g and not break up, and show good intensity；In addition, carbon manufactured in the present embodiment is received
Mitron heat conduction film will not be broken when bending angle is 90~180 °, show good flexibility.
Meanwhile conducting performance test is carried out to carbon nanotube heat conduction film manufactured in the present embodiment, the results show that this implementation
The thermal coefficient of carbon nanotube heat conduction film prepared by example is 1500W/mk or so.
Embodiment 2
It carries out discongesting processing 15min after 0.25g polyimide fibers (length 5mm) are mixed with 25mL water, by gained
It discongests polyimide fiber and is impregnated in 0.5h in the polyimide resin solution that 50mL mass concentrations are 2%, gained is impregnated poly-
Imide fiber carries out shear treatment 35min after being mixed with 90mL water under the conditions of 4000r/min, obtains polyimide fiber point
Dispersion liquid；
The multi-walled carbon nanotube for weighing 0.75g crystal whisker-shapeds carries out ball milling 2h under the conditions of 220r/min, by the carbon after ball milling
Nanotube carries out supersound process 1.5h after being mixed with 75mL water and 0.0375g lauryl sodium sulfate, under the conditions of 4000r/min
Shear treatment 1h is carried out, the dispersion liquid of carbon nanotube is obtained；
It is carried out under the conditions of 4000r/min after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube
Gained spinning dispersion liquid is placed in metering pump by shear treatment 1h, using 18# syringe needles, is controlled between spinning head and receiving screen
Distance is 15cm, and capillary connects the anode of high-voltage generator, and receiving screen connects the cathode of high-voltage generator, on syringe needle
Apply the electrostatic pressure of 25KV, carries out high-voltage electrostatic spinning；Spinning dispersion liquid is sprayed by spinning head, is collected on receiving screen after 5h
Obtain carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is placed in tube furnace and carries out charing process, specifically with 5 DEG C/
Min is warming up to 700 DEG C, keeps the temperature 100min；Continue to be warming up to 1000 DEG C with 5 DEG C/min, keep the temperature 7h, after be cooled to room temperature after
It takes out；Gained film after charing process is placed in graphitizing furnace and carries out graphitization processing, specifically under nitrogen protection, with 10
DEG C/min is warming up to 2000 DEG C, keep the temperature 20h, after be cooled to room temperature after take out；Using twin rollers to institute after graphitization processing
It obtains film to be rolled, obtains carbon nanotube heat conduction film.
The thickness of carbon nanotube heat conduction film manufactured in the present embodiment is 13 μm, and density is about 0.310g/cm3。
According to the method for embodiment 1 to the heat conductivility and mechanical performance of carbon nanotube heat conduction film manufactured in the present embodiment
It is tested, it is as a result almost the same with embodiment 1.
Embodiment 3
It carries out discongesting processing 30min after 0.5g polyimide fibers (length 5mm) are mixed with 50mL water, gained is dredged
Solution polyimide fiber is impregnated in 1h in the polyimide resin solution that 100mL mass concentrations are 2%, and gained dipping polyamides is sub-
Amine fiber carries out shear treatment 40min after being mixed with 100mL water under the conditions of 4000r/min, obtains polyimide fiber dispersion
Liquid；
The multi-walled carbon nanotube for weighing 1g crystal whisker-shapeds carries out ball milling 2.5h under the conditions of 220r/min, and the carbon after ball milling is received
Mitron carries out supersound process 2h after being mixed with 100mL water and 0.05g lauryl sodium sulfate, is carried out under the conditions of 4000r/min
Shear treatment 1h obtains the dispersion liquid of carbon nanotube；
It is carried out under the conditions of 4000r/min after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube
Gained spinning dispersion liquid is placed in metering pump by shear treatment 2h, using 18# syringe needles, is controlled between spinning head and receiving screen
Distance is 15cm, and capillary connects the anode of high-voltage generator, and receiving screen connects the cathode of high-voltage generator, on syringe needle
Apply the electrostatic pressure of 25KV, carries out high-voltage electrostatic spinning；Spinning dispersion liquid is sprayed by spinning head, is collected on receiving screen after 5h
Obtain carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is placed in tube furnace and carries out charing process, specifically with 15 DEG C/
Min is warming up to 700 DEG C, keeps the temperature 2.5h；Continue to be warming up to 1200 DEG C with 10 DEG C/min, keep the temperature 10h, after be cooled to room temperature after
It takes out；Gained film after charing process is placed in graphitizing furnace and carries out graphitization processing, specifically under nitrogen protection, with 20
DEG C/min is warming up to 2800 DEG C, keep the temperature 30h, after be cooled to room temperature after take out；Using twin rollers to institute after graphitization processing
It obtains film to be rolled, obtains carbon nanotube heat conduction film.
The thickness of carbon nanotube heat conduction film manufactured in the present embodiment is 20 μm, and density is about 0.392g/cm3。
According to the method for embodiment 1 to the heat conductivility and mechanical performance of carbon nanotube heat conduction film manufactured in the present embodiment
It is tested, it is as a result almost the same with embodiment 1.
As seen from the above embodiment, carbon nanotube heat conduction film provided by the invention has excellent heat conductivility and machinery
Performance；In addition, preparation method provided by the invention is easy to operate, it is convenient for large-scale production.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon nanotube heat conduction film, includes the following steps：
It carries out discongesting processing after polyimide fiber is mixed with water, gained, which is discongested polyimide fiber, is impregnated in polyimides
In resin solution, shear treatment is carried out after gained dipping polyimide fiber is mixed with water, obtains polyimide fiber dispersion
Liquid；
Shear treatment is carried out after the polyimide fiber dispersion liquid is mixed with the dispersion liquid of carbon nanotube, by gained spinning point
Dispersion liquid carries out high-voltage electrostatic spinning, obtains carbon nanotube-polyimide fiber film；
The carbon nanotube-polyimide fiber film is subjected to charing process, graphitization processing and rolling successively, carbon is obtained and receives
Mitron heat conduction film.
2. preparation method according to claim 1, which is characterized in that the carbon nanotube is the multi-wall carbon nano-tube of crystal whisker-shaped
Pipe.
3. preparation method according to claim 1 or 2, which is characterized in that the polyimide fiber and carbon nanotube
Mass ratio is 1：(1~3).
4. preparation method according to claim 1, which is characterized in that polyimides tree in the polyimide resin solution
The mass concentration of fat is 1.5~2.5%.
5. preparation method according to claim 1 or 2, which is characterized in that the dispersion liquid of the carbon nanotube includes that carbon is received
Mitron, aqueous dispersion and water；The mass concentration of carbon nanotube is 0.5~1.5% in the dispersion liquid of the carbon nanotube, aqueous
The mass concentration of dispersant is 0.025~0.075%.
6. preparation method according to claim 1, which is characterized in that the operating parameter of the high-voltage electrostatic spinning is：It adopts
With 18# syringe needles, the distance between spinning head and receiving screen are 14~16cm, and electrostatic pressure is 10~25KV.
7. preparation method according to claim 1, which is characterized in that the charing process includes the following steps：
650~750 DEG C are warming up to 5~20 DEG C/min, keeps the temperature 40~150min；
Continue to be warming up to 850~1200 DEG C with 5~10 DEG C/min, keeps the temperature 5~10h.
8. preparation method according to claim 1, which is characterized in that the graphitization processing includes the following steps：
In protective atmosphere, 2000~2800 DEG C are warming up to 10~20 DEG C/min, keeps the temperature 5~30h.
9. the carbon nanotube heat conduction film that any one of claim 1~8 preparation method is prepared.
10. carbon nanotube heat conduction film according to claim 9, which is characterized in that the carbon nanotube heat conduction film
Thickness is 5~25 μm, and density is 0.1~0.6g/cm3。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869291A (en) * | 2005-05-23 | 2006-11-29 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
| KR20130099273A (en) * | 2012-02-09 | 2013-09-06 | 이성균 | Functional polyimide fiber |
| CN105542458A (en) * | 2016-01-19 | 2016-05-04 | 北京化工大学 | High-strength high-toughness polyimide resin matrix composite and preparation method thereof |
| CN105696116A (en) * | 2014-11-24 | 2016-06-22 | 北京化工大学 | Preparation method of novel high-heat conduction carbon fibers |
| CN106638114A (en) * | 2015-11-02 | 2017-05-10 | 北京化工大学 | Polyimide paper and preparation method thereof |
-
2018
- 2018-07-06 CN CN201810736301.9A patent/CN108726505B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869291A (en) * | 2005-05-23 | 2006-11-29 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
| KR20130099273A (en) * | 2012-02-09 | 2013-09-06 | 이성균 | Functional polyimide fiber |
| CN105696116A (en) * | 2014-11-24 | 2016-06-22 | 北京化工大学 | Preparation method of novel high-heat conduction carbon fibers |
| CN106638114A (en) * | 2015-11-02 | 2017-05-10 | 北京化工大学 | Polyimide paper and preparation method thereof |
| CN105542458A (en) * | 2016-01-19 | 2016-05-04 | 北京化工大学 | High-strength high-toughness polyimide resin matrix composite and preparation method thereof |
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