CN107760028B - Light-propelled graphene composite material film and preparation method and application thereof - Google Patents
Light-propelled graphene composite material film and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a photo-propulsion graphene composite material film and a preparation method and application thereof, and belongs to the technical field of polyimide material photo-propulsion. The graphene polyimide composite material prepared by the invention has the following characteristics: the material has high conductivity; the material has high strength and high thermal stability; the material has light driving performance and can be driven under the irradiation of visible light, and the light source is laser, short-arc xenon and the like or simulated sunlight and sunlight; the sample in the form of a composite material is driven and lifted under illumination from a light source.
Description
Technical Field
The invention relates to a photo-propulsion graphene composite material film and a preparation method and application thereof, and belongs to the technical field of polyimide material photo-propulsion.
Background
Spacecraft is an important tool for exploring the universe for human beings, and the problem of a power source is that the human beings cannot walk farther. Almost all aviation and aerospace flights at present adopt the technology of obtaining driving force by spraying burning chemical substances, sending a carrier into a preset space orbit and realizing the on-orbit operation of the carrier, mainly liquid and solid chemical propulsion. With the wide expansion of the scope and depth of the utilization and exploration of the space of human beings, the human beings also start a new round of space exploration heat tide marked by deep space exploration, and the traditional chemical propulsion cannot meet the requirement of the space in the future. The energy density is low, a large amount of fuel is required to be carried by chemical propulsion, the fuel carried by the liquid and solid rocket engines accounts for more than 90% of the total weight at present, the effective load only accounts for 1-1.5%, the chemical propulsion efficiency is low, the reliability is low, and the like, a large amount of fuel is consumed, the spacecraft cannot be accelerated to a sufficient speed, and the deep space exploration requirement cannot be met. Compared with the traditional chemical propulsion, the most outstanding advantage of the graphene optical propulsion is that the aircraft can be driven by the irradiation of sunlight when the spacecraft flies in the atmosphere without carrying fuel. Under the combined action of a macroscopic material special morphology structure and a graphene self special electronic structure, the graphene material developed by experts such as Chenyongsheng professor of the southern Kai university can effectively drive to fly under the irradiation of various light sources including sunlight, and the obtained driving force is more than 1000 times of the traditional light pressure.
The solar sail film material generally uses plastic film as a substrate, and the reflecting surface is covered with an aluminum layer, and the emitting surface is covered with a chromium layer. Most plastic film materials are low in light propulsion efficiency and small in obtained driving force, so that the solar sail spacecraft is required to be huge in overall size, the sail area can reach hundreds of square meters or even thousands of square meters, and the solar sail spacecraft is often provided with huge rotational inertia and inconvenient to launch and control the posture of the spacecraft. Because the light driving pressure of the graphene material is large, the graphene material is used as a thin film sail material, so that the driving force is greatly improved, the sail area is reduced, and the control of launching and spacecraft postures is facilitated. The invention discloses a light-driven graphene polyimide film material prepared from graphene, binary anhydride and diamine, and solves the problems of small light driving force, large area, spacecraft attitude control and the like of a film sail.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects of the prior art are overcome, and the light-propelled graphene composite material film, the preparation method and the application thereof are provided.
The technical solution of the invention is as follows:
the light-propelled graphene composite material film comprises the following components in percentage by mass: 10-50: 100.
a preparation method of a light-propelled graphene composite material film comprises the following steps:
1) uniformly dispersing modified graphene in an organic solvent after stirring and ultrasonic treatment to obtain an organic dispersion liquid of the graphene;
2) at the temperature of 40-60 ℃, pyromellitic dianhydride and 4, 4' -diaminodiphenyl ether are placed in a dimethylacetamide solvent for polymerization reaction to obtain a polyamic acid glue solution A with the solid content of 15-30 wt%;
3) placing 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride and p-phenylenediamine in a dimethylacetamide solvent for polymerization reaction at 40-60 ℃ to obtain a polyamic acid glue solution B with a solid content of 15-30 wt%;
4) mixing the organic dispersion liquid of the graphene obtained in the step 1), the polyamic acid glue solution A obtained in the step 2) and the polyamic acid glue solution B obtained in the step 3) to obtain a polyamic acid composite glue solution; wherein, the content of the graphene accounts for 10-30 wt% of the total amount of solid matters in the polyamic acid composite glue solution;
5) adding pyromellitic dianhydride into the polyamic acid composite glue solution obtained in the step 4) at the temperature of 40-60 ℃ to enable the viscosity of the polyamic acid composite glue solution to be 300-350 pa.s;
6) defoaming the polyamic acid composite glue solution obtained in the step 5), preparing the defoamed polyamic acid composite glue solution into a film through a tape casting process, and finally sending the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain the photo-propelled graphene polyimide film.
In the step 1), the preparation method of the modified graphene comprises the following steps:
i, dispersing graphene oxide prepared by a Hummers method in ethanol, stirring, and performing ultrasonic treatment to fully disperse the graphene oxide to obtain a graphene oxide ethanol solution with the concentration of 1-2 mg/ml;
ii, adding the graphene oxide ethanol solution obtained in the step i into a high-pressure thermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into a preheated oven at 180-200 ℃, carrying out high-temperature solvothermal reaction for 16-20 hours, stopping the reaction, cooling to room temperature, taking out the graphene material filled with ethanol, and putting the graphene material into a container;
iii, replacing the solvent in the graphene material filled with the ethanol obtained in the step ii with deionized water to obtain the graphene material filled with the deionized water;
iv, carrying out freeze drying on the graphene material filled with the deionized water obtained in the step iii at the temperature of-50 ℃ to-60 ℃;
v, calcining the graphene material subjected to freeze drying treatment in the step iv at a high temperature of 800-1000 ℃ for 1-2 hours in an inert atmosphere or a vacuum environment to obtain a graphene material;
vi, putting the graphene material obtained in the step v into a dopamine aqueous solution with the pH value of 8 and the concentration of 2mg/ml, forming a polydopamine thin layer on the surface of the graphene, and filtering and vacuum drying the polydopamine thin layer to obtain the modified graphene.
In the step 1), the organic solvent is N, N-dimethylformamide, dimethylacetamide or N-methylpyrrolidone;
in the step 1), the mass relationship between the modified graphene and the organic solvent is 1-2 mg/ml;
in the step 2), the molar ratio of pyromellitic dianhydride to 4, 4' -diaminodiphenyl ether is 1: 1.006-1.015;
in the step 3), the molar ratio of 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride to p-phenylenediamine is 1: 1.006-1.015;
in the step 3), the 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride can also be phthalic anhydride, trimellitic anhydride or tetrabromophthalic anhydride;
in the step 4), the mass ratio of the organic dispersion liquid of the graphene to the polyamic acid glue solution A to the amic acid glue solution B is as follows: 1-5: 1: 1-3;
in the step 6), the temperature of the biaxial stretching treatment is 150-200 ℃, the stretching ratio of the transverse stretching to the longitudinal stretching is 1.10-1.25, the temperature of the imidization treatment is 360-400 ℃, the time of the imidization treatment is 3-4 minutes, the temperature of the setting treatment is 180-250 ℃, and the time of the setting treatment is 2-3 minutes.
Advantageous effects
1) The technical problem to be solved is to provide a preparation method of a light-propelled graphene composite material film, and the light-propelled graphene composite material film prepared by the method has the performance advantages of high strength, high stability, high electrical strength, light driving and the like. The technology is an upgrading and upgrading of a graphene optical propulsion technology in a spacecraft propulsion system, the service life and the performance of an in-orbit spacecraft are improved, the cost of the existing spacecraft is reduced, and remarkable economic benefits are created.
2) The graphene polyimide composite material prepared by the invention has high strength, high stability, high electrical strength and optical driving performance.
3) The graphene polyimide composite material prepared by the invention has the following characteristics: the material has high conductivity; the material has high strength and high thermal stability; the material has light driving performance and can be driven under the irradiation of visible light, and the light source is laser, short-arc xenon and the like or simulated sunlight and sunlight; the sample in the form of a composite material is driven and lifted under illumination from a light source.
4) The light-driven operation should place the material in a vacuum environment, place the light source in the vacuum environment, or add a light-transmitting window structure on the device, use a quartz light-transmitting material in the local part of the vacuum device, so as to introduce the light to be irradiated;
5) the prepared graphene polyimide film has the performance advantages of high strength, high thermal stability, optical drive and the like, and the optical drive graphene polyimide material is used for conductive materials, space vehicles, optical drive devices or devices and solar sail materials.
6) The preparation method of the graphene/polyimide composite material film comprises the following steps: the preparation method comprises the steps of placing pyromellitic dianhydride and 4,4 ' -diaminodiphenyl ether in a dimethylacetamide solvent for polymerization reaction to obtain a polyamide acid glue solution A, placing 3,3 ', 4,4 ' -benzophenone tetracarboxylic dianhydride (or phthalic anhydride, trimellitic anhydride and tetrabromophthalic anhydride) and p-phenylenediamine in a dimethylacetamide solvent for polymerization reaction to obtain a polyamide acid glue solution B, mixing the polyamide acid glue solution A and the polyamide acid glue solution B to prepare a graphene dispersion solution, fully dispersing the graphene dispersion solution in a polybasic polyamide acid glue solution to obtain a polyamide acid composite glue solution, preparing the polyamide acid composite glue solution into a film through a tape casting process, and finally feeding the film into an imidization furnace for treatment to obtain the polyimide film. The graphene/polyimide composite material film prepared by the method has the performance advantages of high strength, high stability, high conductivity, optical drive and the like.
Drawings
FIG. 1 is a diagram of a photo-driven phenomenon of a graphene polyimide composite material under the action of laser;
FIG. 2 shows a solar sail model made of graphene polyimide composite.
Detailed Description
The graphene/polyimide composite material film is prepared by placing an organic dispersion solution of anhydride, 4' -diaminodiphenyl ether, p-phenylenediamine and graphene in a dimethylacetamide solvent for polymerization, wherein the content of graphene accounts for 10-30 wt% of the total amount of solids in a polyamic acid composite glue solution, and preferably, the mass ratio of graphene to polyamic acid glue is 10-30: 100.
The acid anhydride is one or a mixture of more of pyromellitic dianhydride, 3 ', 4, 4' -benzophenone tetracarboxylic dianhydride, phthalic anhydride, trimellitic anhydride and tetrabromophthalic anhydride.
A method of preparing the light-advanced graphene composite film of claim 1, comprising the steps of:
(1) dispersing modified graphene in an organic solvent, and uniformly dispersing the graphene in the organic solvent through stirring and ultrasonic treatment to obtain an organic dispersion liquid of the graphene;
(2) under the condition of 40-60 ℃, pyromellitic dianhydride and 4,4 '-diaminodiphenyl ether are placed in a dimethylacetamide solvent for polymerization reaction, the molar ratio of pyromellitic dianhydride to 4, 4' -diaminodiphenyl ether is 1: 1.006-1.015, and a polyamic acid glue solution A with the solid content of 15-30 wt% is obtained;
(3) placing 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride (or phthalic anhydride, trimellitic anhydride and tetrabromophthalic anhydride) and p-phenylenediamine in a dimethylacetamide solvent for polymerization at 40-60 ℃, wherein the molar ratio of the 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride to the p-phenylenediamine is 1: 1.006-1.015, and obtaining a polyamic acid glue solution B with the solid content of 15-30 wt%;
(4) mixing the modified graphene organic dispersion liquid, the polyamide acid glue solution A and the polyamide acid glue solution B according to a weight ratio of 1-5: 1: 1-3 to obtain a polyamic acid composite glue solution, wherein the content of graphene accounts for 10-30 wt% of the total solid content in the polyamic acid composite glue solution, and finally, the viscosity of the polyamic acid composite glue solution is controlled to be 300-350 pa.s by adding pyromellitic dianhydride at the temperature of 60 ℃;
(5) defoaming the polyamide acid composite glue solution, and then preparing the polyamide acid composite glue solution into a film by a tape casting process, which is characterized in that: and (3) carrying out biaxial stretching treatment at the temperature of 150-200 ℃, wherein the stretching ratio of transverse stretching to longitudinal stretching is 1.10-1.25, the imidization treatment at the temperature of 360-400 ℃ is carried out for 3-4 minutes, the setting treatment at the temperature of 180-250 ℃ is carried out for 2-3 minutes, and thus the photo-propelled graphene polyimide film is obtained.
The preparation method of the light-propelled graphene composite material film comprises the following steps:
(1) dispersing graphene oxide prepared by a Hummers method in ethanol, and stirring and ultrasonically treating the graphene oxide to fully disperse the graphene oxide to obtain a graphene oxide ethanol solution with the concentration of 1-2 mg/ml;
(2) pouring the dispersion liquid into a high-pressure thermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into a preheating oven at 180 ℃ for high-temperature solvothermal reaction for 16-20 hours, stopping the reaction, cooling to room temperature, taking out the graphene material filled with the reaction solvent, and putting the graphene material into a container;
(3) replacing the reaction solvent in the graphene material with deionized water;
(4) freeze-drying the graphene material filled with the deionized water at the temperature of-55 ℃;
(5) calcining the freeze-dried graphene material at a high temperature of 1000 ℃ for 1 hour in an inert atmosphere or a vacuum environment to obtain a graphene material;
(6) and carrying out surface modification on the prepared graphene material, modifying the graphene by using 2g/ml dopamine aqueous solution to form a polydopamine thin layer on the surface of the graphene, filtering, and drying in vacuum to obtain the modified graphene.
The graphene/polyimide composite material film has the performances of high strength, high stability, high conductivity, light drive and the like. The graphene/polyimide composite material film is placed in a vacuum environment, a light source is placed in the vacuum environment or a light-transmitting window is additionally arranged on the device for introduction, and under the action of light, sufficient driving force is provided and the graphene/polyimide composite material film is used as a propelling device of a space vehicle.
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
The preparation method of the functionalized graphene comprises the following steps:
1) dispersing graphene oxide prepared by a Hummers method in ethanol, and stirring and ultrasonically treating the graphene oxide to fully disperse the graphene oxide to obtain a graphene oxide ethanol solution with the concentration of 1 mg/ml;
2) pouring the dispersion liquid into a high-pressure thermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into a preheating oven at 180 ℃, carrying out high-temperature solvothermal reaction for 18 hours, stopping the reaction, cooling to room temperature, taking out the graphene material filled with the reaction solvent, and putting the graphene material into a container;
3) replacing the reaction solvent in the graphene material with deionized water;
4) freeze-drying the graphene material filled with the deionized water at the temperature of-55 ℃;
5) calcining the graphene material subjected to freeze drying treatment at a high temperature of 1000 ℃ for 1 hour in an inert atmosphere or a vacuum environment to prepare a light propulsion graphene material;
6) and uniformly dispersing the prepared graphene material into a dopamine aqueous solution with the pH value of 8 and the concentration of 2mg/ml to form a polydopamine thin layer, filtering, and drying in vacuum to obtain the modified graphene for later use.
The preparation method of the light-propelled graphene polyimide composite material comprises the following steps:
1) dispersing the modified graphene in a dimethylacetamide solvent, and fully dispersing the modified graphene in the dimethylacetamide solvent through stirring and ultrasonic treatment to obtain an organic dispersion liquid of graphene with the concentration of 1 mg/ml;
2) under the normal pressure condition that a kettle body at the temperature of 45 ℃ is filled with nitrogen, firstly, 4 '-diaminodiphenyl ether is dissolved in a dimethylformamide solvent, pyromellitic dianhydride is added for polymerization reaction, the reaction time is 4 hours, the molar ratio of the pyromellitic dianhydride to the 4, 4' -diaminodiphenyl ether is 1:1.008, and polyamic acid glue solution A with the solid content of 17% is obtained (the stirring speed in the whole reaction process is 100 r/min);
3) under the normal pressure condition that a kettle body at the temperature of 55 ℃ is filled with nitrogen, firstly, p-phenylenediamine is dissolved in a dimethylformamide solvent, then, 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride is added for polymerization reaction, the reaction time is 4.5 hours, the molar ratio of the 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride to the p-phenylenediamine is 1.008, and polyamide acid glue solution B with the solid content of 23 wt% is obtained (the stirring speed in the whole reaction process is 100 r/min);
4) mixing an organic dispersion liquid of graphene, a polyamic acid glue solution A and a polyamic acid glue solution B according to a weight ratio of 2: 1: 2.5 to obtain graphene poly polyamic acid glue solution (stirring speed 200r/min, time 1 h); the content of graphene accounts for 15 wt% of the total amount of solids in the polyamic acid composite glue solution, and finally, the viscosity of the polyamic acid composite glue solution is controlled to be 300pa.s by adding pyromellitic dianhydride at the temperature of 45 ℃;
5) defoaming the polyamide acid composite glue solution, preparing the polyamide acid composite glue solution into a film by a tape casting process, controlling the solid content of the film to be 43 wt%, and finally sending the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain the polyimide film, wherein the biaxial stretching treatment temperature is 175 ℃, the stretching ratio of transverse stretching to longitudinal stretching is 1.10 (transverse stretching is carried out after longitudinal stretching), the imidization treatment temperature is 360 ℃, the time is 4 minutes, and the sizing treatment temperature is 210 ℃, and the time is 2.5 minutes.
Example 2
1) Modified graphene was prepared according to the same method as in example 1, and was used.
2) The preparation method of the light-propelled graphene polyimide composite material comprises the following steps:
i, dispersing the modified graphene in a dimethylacetamide solvent, and fully dispersing the modified graphene in the dimethylacetamide solvent through stirring and ultrasonic treatment to obtain an organic dispersion liquid of graphene with the concentration of 1 mg/ml;
ii, under the normal pressure condition that the kettle body is filled with nitrogen at 50 ℃, dissolving 4,4 '-diaminodiphenyl ether in a dimethylformamide solvent, adding pyromellitic dianhydride to carry out polymerization reaction for 4 hours, wherein the molar ratio of the pyromellitic dianhydride to the 4, 4' -diaminodiphenyl ether is 1:1.007, and obtaining polyamic acid glue solution A with the solid content of 17% (the stirring speed in the whole reaction process is 100 r/min);
iii, under the normal pressure condition that the kettle body at the temperature of 55 ℃ is filled with nitrogen, firstly, dissolving p-phenylenediamine in a dimethylformamide solvent, then adding phthalic anhydride for polymerization reaction, wherein the reaction time is 4.5 hours, and the molar ratio of the phthalic anhydride to the p-phenylenediamine is 1.007, so that a polyamic acid glue solution B with the solid content of 23 wt% is obtained (the stirring speed in the whole reaction process is 100 r/min);
iv, mixing the organic dispersion liquid of the graphene, the polyamic acid glue solution A and the polyamic acid glue solution B according to a weight ratio of 3: 1: 2.5 to obtain graphene poly polyamic acid glue solution (stirring speed 200r/min, time 1 h); the content of graphene accounts for 20 wt% of the total amount of solids in the polyamic acid composite glue solution, and finally, the viscosity of the polyamic acid composite glue solution is controlled to be 300pa.s by adding pyromellitic dianhydride at the temperature of 45 ℃;
and v, defoaming the polyamide acid composite glue solution, preparing the polyamide acid composite glue solution into a film by a tape casting process, controlling the solid content of the film to be 43 wt%, and finally conveying the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain the polyimide film, wherein the biaxial stretching treatment temperature is 175 ℃, the stretching ratio of transverse stretching to longitudinal stretching is 1.10 (transverse stretching is carried out after longitudinal stretching), the imidization treatment temperature is 350 ℃, the time is 4 minutes, and the sizing treatment temperature is 200 ℃ and the time is 2.5 minutes.
Example 3
1) Modified graphene was prepared according to the same method as in example 1, and was used.
2) The preparation method of the light-propelled graphene polyimide composite material comprises the following steps:
i, dispersing the modified graphene in a dimethylacetamide solvent, and fully dispersing the modified graphene in the dimethylacetamide solvent through stirring and ultrasonic treatment to obtain an organic dispersion liquid of graphene with the concentration of 1 mg/ml;
ii, under the normal pressure condition that the kettle body is filled with nitrogen at 40 ℃, dissolving 4,4 '-diaminodiphenyl ether in a dimethylformamide solvent, adding pyromellitic dianhydride to carry out polymerization reaction for 4 hours, wherein the molar ratio of the pyromellitic dianhydride to the 4, 4' -diaminodiphenyl ether is 1:1.010, and obtaining a polyamic acid glue solution A with the solid content of 17% (the stirring speed in the whole reaction process is 100 r/min);
iii, under the normal pressure condition that the kettle body at 50 ℃ is filled with nitrogen, firstly, dissolving p-phenylenediamine in a dimethylformamide solvent, then adding tetrabromophthalic anhydride for polymerization reaction, wherein the reaction time is 4.5 hours, and the molar ratio of the tetrabromophthalic anhydride to the p-phenylenediamine is 1.010, thus obtaining polyamic acid glue solution B with the solid content of 23 wt% (the stirring speed in the whole reaction process is 100 r/min);
iv, mixing the organic dispersion liquid of the graphene, the polyamic acid glue solution A and the polyamic acid glue solution B according to a weight ratio of 4: 1: 2.5 to obtain graphene poly polyamic acid glue solution (stirring speed 200r/min, time 1 h); the content of graphene accounts for 30 wt% of the total amount of solids in the polyamic acid composite glue solution, and finally, the viscosity of the polyamic acid composite glue solution is controlled to be 300pa.s by adding pyromellitic dianhydride at the temperature of 45 ℃;
and v, defoaming the polyamide acid composite glue solution, preparing the polyamide acid composite glue solution into a film by a tape casting process, controlling the solid content of the film to be 40 wt%, and finally conveying the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain the polyimide film, wherein the biaxial stretching treatment temperature is 180 ℃, the stretching ratio of transverse stretching to longitudinal stretching is 1.10 (transverse stretching is carried out after longitudinal stretching), the imidization treatment temperature is 360 ℃, the time is 4 minutes, and the sizing treatment temperature is 210 ℃, and the time is 3.0 minutes.
Comparative example 1
The preparation method of the polyimide composite material comprises the following steps:
i, under the normal pressure condition that a kettle body at the temperature of 40 ℃ is filled with nitrogen, dissolving 4,4 '-diaminodiphenyl ether in a dimethylformamide solvent, adding pyromellitic dianhydride to carry out polymerization reaction for 4 hours, wherein the molar ratio of the pyromellitic dianhydride to the 4, 4' -diaminodiphenyl ether is 1:1.008, and obtaining polyamic acid glue solution A with the solid content of 17% (stirring speed of 100r/min in the whole reaction process);
ii, under the normal pressure condition that the kettle body at the temperature of 50 ℃ is filled with nitrogen, firstly, dissolving p-phenylenediamine in a dimethylformamide solvent, then adding tetrabromophthalic anhydride for polymerization reaction, wherein the reaction time is 4.5 hours, and the molar ratio of the tetrabromophthalic anhydride to the p-phenylenediamine is 1.008, so as to obtain polyamic acid glue solution B with the solid content of 23 wt% (the stirring speed in the whole reaction process is 100 r/min);
and iii, mixing the polyamic acid glue solution A and the polyamic acid glue solution B according to the weight ratio of 1: 2.5 to obtain a polybasic polyamic acid glue solution (stirring speed of 200r/min, time of 1 h); finally, under the condition of 45 ℃, the viscosity of the polyamic acid composite glue solution is controlled to be 300pa.s by adding pyromellitic dianhydride;
iv, defoaming the polyamic acid composite glue solution, preparing the polyamic acid composite glue solution into a film by a tape casting process, controlling the solid content of the film to be 40 wt%, and finally sending the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain the polyimide film, wherein the biaxial stretching treatment temperature is 180 ℃, the stretching ratio of transverse stretching to longitudinal stretching is 1.10 (transverse stretching is carried out after longitudinal stretching), the imidization temperature is 360 ℃, the time is 4 minutes, and the sizing treatment temperature is 210 ℃, and the time is 3.0 minutes.
The step of "fully dispersing" in the above embodiments adopts a process of firstly dispersing by using a high-speed disperser (1800-2500 r/min), and then dispersing for 100-180 s with the aid of ultrasonic waves.
The graphene polyimide composite material obtained in the embodiment 1-3 has a light propulsion performance. The material has quick and effective light propelling performance under the irradiation of different light sources.
As shown in fig. 1, the operation method of the light propulsion includes: a piece of graphene composite material is taken and placed in a vacuum degree of not higher than 10Pa, a light source is placed outside a vacuum environment, and a light-transmitting window structure is added on the device, so that the material to be irradiated is optically introduced.
Based on the light propulsion phenomenon, the graphene-based polyimide composite material can be used for manufacturing a solar sail with light driving performance, and a design prototype of the solar sail is shown in fig. 2.
The graphene/polyimide films prepared according to examples 1 to 3 were compared with comparative example 1, a conventional polyimide film currently on the market, in terms of performance, and the results are shown in the following table 1:
TABLE 1 graphene/polyimide film Properties
| Performance of | EXAMPLE 1 | EXAMPLE 2 | EXAMPLE 3 | Control 1 |
| Modulus GPa) | 4.0 | 3.8 | 3.7 | 2.5 |
| Tensile strength MPa) | 299 | 315 | 290 | 200 |
| Thermal stability 5% Td/. degree.C | 530 | 540 | 510 | 550 |
| Conductivity(s) | 5.89*10-6 | 8.0*10-6 | 5.89*10-6 | - |
| Whether or not light propulsion performance is present | Is that | Is that | Is that | Whether or not |
Compared with the conventional polyimide film, the graphene/polyimide film prepared by the invention has the advantages of high strength, high thermal stability, high conductivity, good light propelling performance and the like, and the graphene/polyimide film prepared by the invention has good flexibility and good bonding performance with copper foil.
It is understood that the examples and embodiments described herein are for illustrative purposes only and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this application.
Claims (1)
1. The light-propelled graphene composite material film is characterized in that: the composite material film comprises the following components in percentage by mass: 10-50: 100, respectively;
the preparation method of the light-propelled graphene composite material film comprises the following steps:
1) uniformly dispersing modified graphene in an organic solvent after stirring and ultrasonic treatment to obtain an organic dispersion liquid of the graphene;
2) at the temperature of 40-60 ℃, pyromellitic dianhydride and 4, 4' -diaminodiphenyl ether are placed in a dimethylacetamide solvent for polymerization reaction to obtain a polyamic acid glue solution A with the solid content of 15-30 wt%;
3) placing 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride and p-phenylenediamine in a dimethylacetamide solvent for polymerization reaction at 40-60 ℃ to obtain a polyamic acid glue solution B with a solid content of 15-30 wt%;
4) mixing the organic dispersion liquid of the graphene obtained in the step 1), the polyamic acid glue solution A obtained in the step 2) and the polyamic acid glue solution B obtained in the step 3) to obtain a polyamic acid composite glue solution; wherein, the content of the graphene accounts for 10-30 wt% of the total amount of solid matters in the polyamic acid composite glue solution;
5) adding pyromellitic dianhydride into the polyamic acid composite glue solution obtained in the step 4) at the temperature of 40-60 ℃ to enable the viscosity of the polyamic acid composite glue solution to be 300-350 pa.s;
6) preparing the polyamic acid composite glue solution obtained in the step 5) into a film to obtain a light-propelled graphene polyimide film;
in the step 6), the method for preparing the polyamic acid composite glue solution into the film comprises the following steps: firstly, defoaming polyamide acid composite glue solution, then preparing the defoamed polyamide acid composite glue solution into a film through a tape casting process, and finally sending the film into an imidization furnace for biaxial stretching, imidization and sizing treatment to obtain a photo-propelled graphene polyimide film;
in the step 1), the preparation method of the modified graphene comprises the following steps:
i, dispersing graphene oxide prepared by a Hummers method in ethanol, stirring, and performing ultrasonic treatment to fully disperse the graphene oxide to obtain a graphene oxide ethanol solution with the concentration of 1-2 mg/ml;
ii, adding the graphene oxide ethanol solution obtained in the step i into a high-pressure thermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into a preheated oven at 180-200 ℃, carrying out high-temperature solvothermal reaction for 16-20 hours, stopping the reaction, cooling to room temperature, taking out the graphene material filled with ethanol, and putting the graphene material into a container;
iii, replacing the solvent in the graphene material filled with the ethanol obtained in the step ii with deionized water to obtain the graphene material filled with the deionized water;
iv, carrying out freeze drying on the graphene material filled with the deionized water obtained in the step iii at the temperature of-50 ℃ to-60 ℃;
v, calcining the graphene material subjected to freeze drying treatment in the step iv at a high temperature of 800-1000 ℃ for 1-2 hours in an inert atmosphere or a vacuum environment to obtain a graphene material;
vi, putting the graphene material obtained in the step v into a dopamine aqueous solution with the pH value of 8 and the concentration of 2mg/ml, forming a polydopamine thin layer on the surface of graphene, and filtering and vacuum drying the polydopamine thin layer to obtain modified graphene;
in the step 1), the organic solvent is N, N-dimethylformamide, dimethylacetamide or N-methylpyrrolidone;
in the step 1), the relation between the modified graphene and the organic solvent is 1-2 mg/ml;
in the step 2), the molar ratio of pyromellitic dianhydride to 4, 4' -diaminodiphenyl ether is 1: 1.006-1.015;
in the step 3), the molar ratio of 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride to p-phenylenediamine is 1: 1.006-1.015;
in the step 3), the 3,3 ', 4, 4' -benzophenone tetracarboxylic dianhydride can also be phthalic anhydride, trimellitic anhydride or tetrabromophthalic anhydride;
in the step 4), the mass ratio of the organic dispersion liquid of the graphene to the polyamic acid glue solution A to the amic acid glue solution B is as follows: 1-5: 1: 1-3;
the temperature of the biaxial stretching treatment is 150-200 ℃, the stretching ratio of the transverse stretching to the longitudinal stretching is 1.10-1.25, the temperature of the imidization treatment is 360-400 ℃, the time of the imidization treatment is 3-4 minutes, the temperature of the setting treatment is 180-250 ℃, and the time of the setting treatment is 2-3 minutes.
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| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
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| CN105111476A (en) * | 2015-09-16 | 2015-12-02 | 安徽鑫柏格电子股份有限公司 | Preparation method for polyimide film |
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