CN114316317A - Novel carbon fiber/polyimide composite material film and coating preparation method thereof - Google Patents
Novel carbon fiber/polyimide composite material film and coating preparation method thereof Download PDFInfo
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- CN114316317A CN114316317A CN202111513886.6A CN202111513886A CN114316317A CN 114316317 A CN114316317 A CN 114316317A CN 202111513886 A CN202111513886 A CN 202111513886A CN 114316317 A CN114316317 A CN 114316317A
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- polyimide
- carbon fiber
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- composite material
- film
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 65
- 239000004642 Polyimide Substances 0.000 title claims abstract description 42
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 35
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011248 coating agent Substances 0.000 title claims abstract description 29
- 238000000576 coating method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 13
- 239000007888 film coating Substances 0.000 claims abstract description 13
- 238000009501 film coating Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims description 16
- 239000011268 mixed slurry Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000004020 conductor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention belongs to a composite material preparation technology, and particularly relates to a carbon fiber/polyimide composite material film coating preparation method. The carbon fiber/polyimide composite material film coating preparation method comprises the steps of mixing and stirring carbon fiber/polyimide anhydride with a proper proportion in a vacuum environment, coating the mixture on a smooth surface, carrying out secondary heating, curing and forming, and taking down for use. The invention has the advantages that the technological parameters are easy to control through series improvement, the coating is more uniform, the polyimide film with large area and high smoothness can be processed and obtained, and the work is more efficient. The prepared polyimide film has light weight and good heating uniformity, can be used for heating and deicing the surface of an airplane, and has great practical application value.
Description
Technical Field
The invention belongs to a composite material preparation technology, and particularly relates to a carbon fiber/polyimide composite material film coating preparation method.
Background
Polyimide is a high molecular polymer with a main chain and containing imide rings, has high temperature resistance and good insulating property, and is widely applied to various industrial fields. Polyimide is generally used as an insulating film, but is rarely used in a heating device because of its insulating property.
In the field of aviation, under icing flight conditions, heating assemblies are needed to meet deicing requirements while minimizing weight. The existing airplane icing heating device is generally made of metal materials such as various heating wires, and has heavy mass and a narrow and limited heating area.
Disclosure of Invention
The purpose of the invention is: provides a novel carbon fiber/polyimide composite material film coating preparation method with light weight and large heating area.
In addition, the invention also discloses the polyimide film prepared by the method.
The technical scheme of the invention is as follows:
a carbon fiber/polyimide composite material film coating preparation method comprises the steps of mixing and stirring carbon fiber/polyimide anhydride with a proper proportion in a vacuum environment, coating the mixture on a smooth surface, carrying out secondary heating, curing and forming, and taking down for use.
The carbon fiber/polyimide composite material film coating preparation method comprises the following steps:
step 1: preparing carbon fiber/polyimide anhydride mixed slurry, wherein the proportion of the carbon fiber/polyimide anhydride mixed slurry and the polyimide anhydride mixed slurry is obtained according to the resistance requirement of a finished product;
step 2: the carbon fiber/polyimide anhydride mixed slurry is stirred in a vacuum environment, wherein the stirring speed is 1200-1800 r/min, and the stirring time is 45-60 min, so that under the condition of ensuring uniform stirring, the heating in the stirring process is avoided, the reaction is carried out in advance, and the subsequent film forming is not facilitated; the vacuum degree is not lower than-0.09 mPa in the stirring process, air is prevented from being mixed, bubbles are prevented from being generated, the coating quality is influenced, and the stirring is finished and the stirring is kept still for not less than 30min, so that the bubbles can be dissipated in the stirring process;
and step 3: uniformly coating the mixed slurry on a smooth surface by using coating equipment;
and 4, step 4: one-time heating
And drying the film for 60-80 minutes at the temperature of 80 +/-2 ℃ in a vacuum environment, and ensuring that the vacuum degree in the drying process is 0.65-0.75 standard atmospheric pressure so as to evaporate most of water, reduce the fluidity of the slurry and prepare for subsequent film forming.
And 5: second heating
Preheating by stages and heating to evaporate water vapor so as to concentrate the slurry and form a polyimide film;
step 6: taking out and cutting
And separating the formed polyimide film from the smooth surface, and cutting the polyimide film according to the requirement for use.
The smooth surface for coating is a quartz glass surface or a polyimide plastic surface so as to avoid reaction with polyimide and facilitate film separation.
The mass ratio of the carbon fiber to the polyimide anhydride is 100: 1-5, so that the formed film has proper resistance and can meet the deicing and heating requirements.
The mesh number of the carbon fibers is 500-1000, so that the film has good conductive uniformity.
The carbon fiber needs to be dried, the humidity is not more than 60%, the moisture is prevented from being mixed into the slurry, and the subsequent treatment difficulty is increased.
In the step 3, when coating is carried out, the coating speed is 10-20 mm/s, and the coating thickness is 550-700 mu m, so that the film is uniform in whole and has enough thickness, and the forming quality of the film is ensured.
And 5, during secondary heating, the specific process is as follows:
1) the temperature is raised to 80 ℃ at the rate of 2 ℃/min, and the temperature is kept for 45 min; integral first preheating is carried out, and integral heating uniformity is improved;
2) the temperature is 80 to 180 ℃, the heating rate is 2 ℃/min, and the temperature is kept for 60 min; the secondary preheating is combined with preheating process parameter control, so that the integral heating uniformity of the film can be effectively ensured, and the quality problems of film cracking, hole breaking and the like are reduced;
3) the temperature is increased at the rate of 2 ℃/min to 300 ℃, the temperature is kept for 180min, and water vapor is further evaporated to form a polyimide film;
4) and the film is naturally cooled along with the high-temperature box, so that the film is prevented from cracking.
The polyimide film is prepared by the carbon fiber/polyimide composite material film coating method, has the characteristics of large area and good flatness, can be used for heating an airborne deicing surface, and has comprehensive performance far superior to that of a conventional metal heating scheme.
The invention has the advantages and beneficial effects that: the novel polyimide film preparation process realizes mechanization and standardization of polyimide film preparation, and enables process monitoring variables to be more obvious and controllable. Through carrying out a series of improvements to it and making its parameter easily controlled, the coating is more even, can process the polyimide film who obtains large tracts of land, high planarization, and work is more high-efficient. The prepared polyimide film has light weight and good heating uniformity, can be used for heating and deicing the plane surface, and has great practical application value.
Drawings
FIG. 1 is a flow chart of a method for coating and preparing a carbon fiber/polyimide composite film according to the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples:
example 1
Step 1: and (5) preparing slurry. The preparation proportion (mass proportion) of the slurry is as follows: and recording the quality of the polyimide paste and the conductor, wherein the ratio of the polyimide paste to the conductor is 100: 2.
Step 2: stirring in vacuum. Setting the stirring speed at 1200r/min, the stirring time at 50 minutes, and the vacuum degree: -0.095 mPa.
After the stirring, the mixture was allowed to stand for 30 minutes.
And step 3: the mixed slurry is uniformly coated on a smooth surface using a coating apparatus. The coating speed was set at 20mm/s and the coating thickness was 580 um.
And 4, step 4: heating for one time. The temperature was set at 80 ℃ and the vacuum at 0.65 atm.
And 5: and (5) heating for the second time. Heating is carried out according to a heating program.
Step 6: taking out and cutting. Rectangular films cut to 60x350 square millimeters were tested.
Performance results
The cut polyimide film was measured to have a resistance of 1223 Ω, and recorded and stored. Using a four-probe type square resistance tester to randomly test five points on the polyimide film, and testing the square resistance values to be respectively: 8.78, 8.60, 8.52, 8.41 and 9.17(k omega), the resistance uniformity is good; and simultaneously, the thickness of the five points is measured by using an electronic thickness gauge: 49.7, 48.5, 45.8, 50.4, 46.7(um), thickness deviation less than 10 um. Therefore, the polyimide film can uniformly generate heat and has good deicing effect.
Example 2
Step 1: and (5) preparing slurry. The preparation proportion (mass proportion) of the slurry is as follows: and recording the quality of the polyimide paste and the conductor, wherein the ratio of the polyimide paste to the conductor is 100: 3.6.
Step 2: stirring in vacuum. Setting the stirring speed to be 1500r/min, the stirring time to be 50 minutes, and the vacuum degree: -0.1 mPa.
After the stirring, the mixture was allowed to stand for 30 minutes.
And step 3: the mixed slurry is uniformly coated on a smooth surface using a coating apparatus. The coating speed was set at 10mm/s and the coating thickness was 650 um.
And 4, step 4: heating for one time. The temperature was set at 80 ℃ and the vacuum at 0.7 atm.
And 5: and (5) heating for the second time. Heating is carried out according to a heating program.
Step 6: taking out and cutting. Rectangular films cut to 60x350 square millimeters were tested.
Performance results
The cut polyimide film was measured to have a resistance of 425 Ω, and recorded and stored. Using a four-probe type square resistance tester to randomly test five points on the polyimide film, and testing the square resistance values to be respectively: 2.88, 3.17, 2.87, 3.23 and 3.04(k omega), and the resistance uniformity is good; and simultaneously, the thickness of the five points is measured by using an electronic thickness gauge: 72.1, 64.2, 64.6, 62.6, 67.4(um), with thickness deviations of less than 10 um. Therefore, the polyimide film can uniformly generate heat and has good deicing effect.
In conclusion, the carbon fiber/polyimide composite film coating preparation method disclosed by the invention can be used for preparing polyimide films with different resistances by controlling the proportion and parameters, so that different deicing design requirements can be met.
Claims (9)
1. A carbon fiber/polyimide composite material film coating preparation method is characterized in that carbon fiber/polyimide anhydride with a proper proportion is mixed and stirred in a vacuum environment, then coated on a smooth surface, cured and formed after secondary heating, and then taken down for use.
2. The carbon fiber/polyimide composite material film coating preparation method according to claim 1, characterized by comprising the following steps:
step 1: preparing carbon fiber/polyimide anhydride mixed slurry, wherein the ratio of the carbon fiber/polyimide anhydride mixed slurry to the polyimide anhydride mixed slurry is adjusted according to the resistance requirement of a finished product;
step 2: stirring the carbon fiber/polyimide anhydride mixed slurry in a vacuum environment, wherein the stirring speed is 1200-1800 r/min, the stirring time is 45-60 min, the vacuum degree in the stirring process is not lower than-0.09 mPa, and the stirring is finished and the standing is not less than 30 min;
and step 3: uniformly coating the mixed slurry on a smooth surface by using coating equipment;
and 4, step 4: one-time heating
Drying for 60-80 minutes at 80 +/-2 ℃ in a vacuum environment, and ensuring that the vacuum degree in the drying process is 0.65-0.75 standard atmospheric pressure.
And 5: second heating
Evaporating the solvent by preheating and heating in stages to allow the slurry to react and form a polyimide film;
step 6: taking out and cutting
And separating the formed polyimide film from the smooth surface, and cutting the polyimide film according to the requirement for use.
3. The method for preparing carbon fiber/polyimide composite film coating according to claim 1, wherein the smooth surface for coating is quartz glass surface or polyimide plastic surface.
4. The coating preparation method of the carbon fiber/polyimide composite material film according to claim 1, wherein the mass ratio of the carbon fiber/polyimide anhydride is 1-5: 100.
5. the method for preparing the carbon fiber/polyimide composite film through coating according to claim 1, wherein in the step 3, the coating speed is 10-20 mm/s and the coating thickness is 550-700 μm.
6. The coating preparation method of the carbon fiber/polyimide composite material film according to claim 1, wherein the specific process of the secondary heating in the step 5 is as follows:
1) the temperature is raised to 80 ℃ at the rate of 2 ℃/min, and the temperature is kept for 45 min;
2) the temperature is 80 to 180 ℃, the heating rate is 2 ℃/min, and the temperature is kept for 60 min;
3) the temperature is increased at the rate of 2 ℃/min to be 180-300 ℃, and the temperature is kept for 180 min;
4) and naturally cooling along with the high-temperature box.
7. The coating preparation method of the carbon fiber/polyimide composite material film according to claim 1, wherein the mesh number of the carbon fiber is 500-1000.
8. The method for preparing carbon fiber/polyimide composite film coating according to claim 1, wherein the carbon fiber is dried and has a humidity of not more than 60%.
9. A polyimide film produced by the carbon fiber/polyimide composite film coating method according to any one of claims 1 to 8.
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| CN202111513886.6A CN114316317A (en) | 2021-12-10 | 2021-12-10 | Novel carbon fiber/polyimide composite material film and coating preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4394467A (en) * | 1981-06-22 | 1983-07-19 | Celanese Corporation | Sized carbon fibers capable of use with polyimide matrix |
| CN101733889A (en) * | 2009-11-23 | 2010-06-16 | 成都飞机工业（集团）有限责任公司 | Preparation method of thermoplastic polyimide-based composite material structural member-opening cover |
| JP2011046852A (en) * | 2009-08-28 | 2011-03-10 | Ube Industries Ltd | Polyimide precursor solution composition containing fine carbon fiber and polyimide film using the same |
| CN103467988A (en) * | 2013-10-10 | 2013-12-25 | 哈尔滨工业大学 | Polyimide/ carbon fiber X-ray window thin film and preparation method thereof |
| CN103694487A (en) * | 2013-12-13 | 2014-04-02 | 青岛海洋新材料科技有限公司 | Preparation method of carbon fiber-polyimide composite film |
| CN105542205A (en) * | 2015-12-29 | 2016-05-04 | 哈尔滨工业大学 | Preparation method of electrically-driven shape memory polyimide |
| CN106046784A (en) * | 2016-05-30 | 2016-10-26 | 江苏大学 | Strengthened and toughened polyimide composite film preparation method |
| JP2017066400A (en) * | 2015-09-29 | 2017-04-06 | 新日鉄住金化学株式会社 | Method for producing polyimide film |
-
2021
- 2021-12-10 CN CN202111513886.6A patent/CN114316317A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4394467A (en) * | 1981-06-22 | 1983-07-19 | Celanese Corporation | Sized carbon fibers capable of use with polyimide matrix |
| JP2011046852A (en) * | 2009-08-28 | 2011-03-10 | Ube Industries Ltd | Polyimide precursor solution composition containing fine carbon fiber and polyimide film using the same |
| CN101733889A (en) * | 2009-11-23 | 2010-06-16 | 成都飞机工业（集团）有限责任公司 | Preparation method of thermoplastic polyimide-based composite material structural member-opening cover |
| CN103467988A (en) * | 2013-10-10 | 2013-12-25 | 哈尔滨工业大学 | Polyimide/ carbon fiber X-ray window thin film and preparation method thereof |
| CN103694487A (en) * | 2013-12-13 | 2014-04-02 | 青岛海洋新材料科技有限公司 | Preparation method of carbon fiber-polyimide composite film |
| JP2017066400A (en) * | 2015-09-29 | 2017-04-06 | 新日鉄住金化学株式会社 | Method for producing polyimide film |
| CN105542205A (en) * | 2015-12-29 | 2016-05-04 | 哈尔滨工业大学 | Preparation method of electrically-driven shape memory polyimide |
| CN106046784A (en) * | 2016-05-30 | 2016-10-26 | 江苏大学 | Strengthened and toughened polyimide composite film preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 杨高峰;: "碳纤维/聚酰亚胺复合材料的合成及其性能研究", 橡塑技术与装备 * |
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Application publication date: 20220412 |