CN114853002A - Preparation method and application of high-order-degree graphite film - Google Patents
Preparation method and application of high-order-degree graphite film Download PDFInfo
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- CN114853002A CN114853002A CN202210521887.3A CN202210521887A CN114853002A CN 114853002 A CN114853002 A CN 114853002A CN 202210521887 A CN202210521887 A CN 202210521887A CN 114853002 A CN114853002 A CN 114853002A
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- C01B32/00—Carbon; Compounds thereof
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- C09K5/08—Materials not undergoing a change of physical state when used
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/24—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/28—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyamides
- D01F9/30—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds from polyamides from aromatic polyamides
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method and application of a high-order graphite film. According to the preparation method of the high-order-degree graphite film, aramid fibers are subjected to chemical cracking to obtain an aramid nanofiber dispersion liquid, the aramid nanofiber dispersion liquid is prepared into a film to obtain the aramid nanofiber film, and the aramid nanofiber film is subjected to carbonization and graphitization respectively to obtain the high-order-degree graphite film; the graphite film prepared by the method has the advantages of high graphitization degree, good flexibility, smooth surface, few internal wrinkle defects and larger grain size; the graphite film prepared by the method has ultrahigh conductivity (1.67 multiplied by 10) 6 S/m) and thermal diffusivity (724.5 mm) 2 S); the preparation method has simple technical processEasy operation, green environmental protection and large-scale production.
Description
Technical Field
The invention relates to the technical field of film material preparation, in particular to a preparation method and application of a high-order-degree graphite film.
Background
In recent years, a graphite material prepared by carbonizing an organic polymer material through graphitization has excellent physical and chemical properties, and the graphite material with the layered hexagonal carbon atom plane ordered stacking structure has the characteristics of light weight, good heat resistance, high electrical conductivity, strong heat conduction and the like, and has wide application prospects in the aspects of heat dissipation, electromagnetic shielding, energy storage and the like. However, the graphite materials obtained by graphitizing the high molecular organic materials reported in the prior art, such as polyimide, acrylic fiber and the like, have more wrinkle defects and lower crystallinity, so that the heat conduction and electric conduction performances of the high molecular organic materials are affected. The graphite material obtained by adding the nano-filler and improving the raw material preparation process can improve the physical and chemical properties of the graphite material, but the further application of the graphite material is limited due to the factors of complex preparation process, high cost and the like. Therefore, the selection of a proper polymer organic precursor is a necessary condition for preparing the high-performance graphitized carbon material.
Aramid fibers are widely applied in civil and defense directions due to high orientation degree, high crystallinity, excellent mechanical and flame-retardant properties, but single macroscopic aramid fibers are difficult to form a film in a self-assembly mode due to the properties of strong hydrophobicity, difficult dispersion and the like, so that the further application of the aramid fibers in new materials is limited. In recent years, researchers crack the intermolecular acting force and chemical bonds of aramid fibers into nano-sized aramid nanofibers through chemical action, the linear chain structure of the macroscopic aramid fibers with the alternate amide bonds and benzene rings is maintained, and the aramid nanofibers have high length-diameter ratio, more oxygen-containing functional groups and nano-sized effect. Therefore, the aramid nano fiber material is self-assembled into a film with a macroscopic structure by utilizing the emerging self-assembly technology, and the graphite material prepared by high graphitization is an ideal high molecular organic precursor. For example, the prior art discloses that an aramid nanofiber film is carbonized at a temperature of below 900 ℃ to obtain a carbonaceous material with certain conductive characteristics, however, the film has the defects of poor flexibility, rough surface, more internal defects, lower conductivity and the like. Therefore, further research is needed to obtain a high-performance film by regulating the preparation of the aramid nano-cellulose film.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a highly ordered graphite film and applications thereof, so as to solve the above problems or at least partially solve the above problems.
In a first aspect, the invention provides a preparation method of a high-order graphite film, which comprises the following steps:
subjecting aramid fibers to chemical cracking to obtain an aramid nanofiber dispersion liquid;
preparing the aramid nano-fiber dispersion liquid into a film to obtain an aramid nano-fiber film;
placing the obtained aramid fiber nanofiber membrane in inert gas for carbonization at 500-2000 ℃;
and (3) graphitizing the carbonized aramid fiber nanofiber membrane in inert gas at 2000-3000 ℃ to obtain the high-order-degree graphite membrane.
Preferably, the preparation method of the high-order graphite film comprises the following steps of chemically cracking the aramid fiber to obtain the aramid nanofiber dispersion liquid: adding aramid fibers into a DMSO (dimethyl sulfoxide) solvent or a mixed solvent of DMSO and water, adding KOH, and dispersing to obtain an aramid nanofiber dispersion liquid.
Preferably, in the preparation method of the high-order graphite film, the concentration of the aramid nanofiber dispersion liquid is 0.01-60 mg/mL.
Preferably, in the preparation method of the high-order graphite film, the thickness of the aramid nanofiber film is 1-150 μm.
Preferably, in the preparation method of the high-order graphite film, the carbonization time is 30-360 min; the graphitization time is 30-360 min.
Preferably, the preparation method of the high-order graphite film comprises the steps of putting the obtained aramid nano-fiber film in inert gas, heating the aramid nano-fiber film to 500-2000 ℃ at the speed of 1-15 ℃/min, and carbonizing the aramid nano-fiber film;
and (3) placing the carbonized aramid nano fiber membrane in inert gas, and heating to 2000-3000 ℃ at the speed of 1-15 ℃/min for graphitization.
Preferably, in the preparation method of the high-order graphite film, the flow rate of the inert gas is 10-800 ml/min in the carbonization and graphitization processes.
Preferably, the preparation method of the high-order graphite film further comprises the step of placing the graphitized aramid nanofiber film on a static pressure machine to be calendered under 20-50 Mpa for 1-3 hours, so that the high-order graphite film is obtained.
Preferably, the preparation method of the high-order graphite film is a method for preparing the aramid nano-fiber dispersion into a film, and the method comprises any one of a vacuum filtration method, a spin-coating method, a spraying method, a hydrothermal evaporation method and a scraper coating method;
wherein, the vacuum filtration method specifically comprises the following steps: filtering the aramid nano-fiber dispersion liquid in vacuum by using a filter membrane, and drying at 25-105 ℃ for 2-24 hours to obtain an aramid nano-fiber membrane;
the scraper coating method comprises the following specific steps: and (3) carrying out blade coating on the aramid nano-fiber dispersion liquid on a substrate, and drying for 2-24 h at the temperature of 25-105 ℃ to obtain the aramid nano-fiber membrane.
In a second aspect, the invention also provides application of the high-order graphite film prepared by the preparation method as a heat dissipation material, an electromagnetic shielding material and an energy storage material.
Compared with the prior art, the preparation method of the high-order graphite film has the following beneficial effects:
according to the preparation method of the high-order-degree graphite film, aramid fibers are subjected to chemical cracking to obtain an aramid nanofiber dispersion solution, the aramid nanofiber dispersion solution is prepared into a film to obtain the aramid nanofiber film, and the aramid nanofiber film is subjected to carbonization and graphitization respectively to obtain the high-order-degree graphite film; the graphite film prepared by the method has the advantages of high graphitization degree, good flexibility, smooth surface, few internal wrinkle defects and larger grain size; the graphite film prepared by the method has ultrahigh conductivity (1.67 multiplied by 10) 6 S/m) and thermal diffusivity (724.5 mm) 2 S); the preparation method has the advantages of simple and feasible technical process, environmental protection and large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is an optical photograph of a highly ordered graphite film prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of a highly ordered graphite film prepared in example 2 of the present invention;
FIG. 3 is a surface scanning electron microscope image of a highly ordered graphite film prepared in example 3 of the present invention;
FIG. 4 is a scanning electron microscope cross-sectional view of a highly ordered graphite film prepared in example 3 of the present invention;
FIG. 5 is a graph showing the thermal diffusion coefficient of the highly ordered graphite film prepared in example 3 of the present invention.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the application provides a preparation method of a high-order graphite film, which comprises the following steps:
s1, subjecting aramid fibers to chemical cracking to obtain an aramid nanofiber dispersion liquid;
s2, preparing the aramid nano-fiber dispersion liquid into a film to obtain an aramid nano-fiber film;
s3, placing the obtained aramid fiber nanofiber membrane in inert gas for carbonization at 500-2000 ℃;
and S4, graphitizing the carbonized aramid fiber nanofiber membrane in inert gas at 2000-3000 ℃ to obtain the high-order-degree graphite membrane.
In some embodiments, the chemical cracking of the aramid fiber to obtain the aramid nanofiber dispersion specifically comprises: adding aramid fibers into a DMSO (dimethyl sulfoxide) solvent or a mixed solvent of DMSO and water, adding KOH, and dispersing to obtain an aramid nanofiber dispersion liquid.
Specifically, 0.5-2 g of aramid fiber is added into 100-550 mL of DMSO (dimethyl sulfoxide) solvent, 1-2 g of KOH is added, and the aramid fiber and the KOH are uniformly mixed in a mechanical stirring mode, a magnetic stirring mode, an ultrasonic or homogeneous stirring mode and the like to obtain an aramid nanofiber dispersion liquid; or adding 0.5-2 g of aramid fiber into a mixed solvent consisting of 100-550 mL of DMSO (dimethyl sulfoxide) and 15-25 mL of water, adding 1-2 g of KOH, and uniformly mixing in a mechanical stirring mode, a magnetic stirring mode, an ultrasonic or homogeneous stirring mode and the like to obtain the aramid nanofiber dispersion liquid.
In some embodiments, the concentration of the aramid nanofiber dispersion is 0.01-60 mg/mL.
In some embodiments, the aramid nanofiber film has a thickness of 1 to 150 μm.
In some embodiments, the carbonization time is 30 to 360 min; the graphitization time is 30-360 min.
In some embodiments, the obtained aramid nanofiber membrane is placed in inert gas, and the temperature is raised to 500-2000 ℃ at the speed of 1-15 ℃/min for carbonization;
and (3) placing the carbonized aramid nano fiber membrane in inert gas, and heating to 2000-3000 ℃ at the speed of 1-15 ℃/min for graphitization.
Specifically, the inert gas includes nitrogen, argon, helium, and the like.
In some embodiments, the flow rate of the inert gas during carbonization and graphitization is 10 to 800 ml/min.
In some embodiments, the graphitized aramid nano fiber film is placed on a static pressure machine and is calendered for 1-3 hours under 20-50 Mpa, and the high-order-degree graphite film is obtained.
In some embodiments, the aramid nanofiber dispersion is prepared into a film by any one of a vacuum filtration method, a spin coating method, a spray coating method, a hydrothermal evaporation method, and a doctor blade coating method;
wherein, the vacuum filtration method specifically comprises the following steps: filtering the aramid nano-fiber dispersion liquid in vacuum by using a filter membrane, and drying at 25-105 ℃ for 2-24 hours to obtain an aramid nano-fiber membrane;
the scraper coating method comprises the following specific steps: and (3) carrying out blade coating on the aramid nano-fiber dispersion liquid on a substrate, and drying for 2-24 h at the temperature of 25-105 ℃ to obtain the aramid nano-fiber membrane.
In the above embodiment, after the aramid nanofiber membrane is prepared, the aramid nanofiber membrane needs to be peeled from the filtering membrane or the substrate, and the aramid nanofiber membrane can be peeled from the filtering membrane or the substrate by applying an external force.
Specifically, the aramid fiber is subjected to chemical cracking to obtain the aramid nanofiber dispersion liquid, and the aramid nanofiber dispersion liquid is prepared into a film by using a self-assembly technology, wherein the film forming method specifically comprises any one of a vacuum filtration method, a spin-coating method, a spraying method, a hydrothermal evaporation method and a scraper coating method.
Specifically, the substrate is a polytetrafluoroethylene substrate, and the aperture of the filter membrane is 0.2-0.25 μm.
According to the preparation method of the high-order-degree graphite film, aramid fibers are subjected to chemical cracking to obtain an aramid nanofiber dispersion liquid, the aramid nanofiber dispersion liquid is prepared into a film to obtain the aramid nanofiber film, and the aramid nanofiber film is subjected to carbonization and graphitization respectively to obtain the high-order-degree graphite film; the graphite film prepared by the method has the advantages of high graphitization degree, good flexibility, smooth surface, few internal wrinkle defects and larger grain size; the graphite film prepared by the method has ultrahigh conductivity (1.67 multiplied by 10) 6 S/m) and thermal diffusivity (724.5 mm) 2 S); the preparation method has the advantages of simple and feasible technical process, environmental protection and large-scale production.
Based on the same inventive concept, the high-order-degree graphite film prepared by the preparation method is applied as a heat dissipation material, an electromagnetic shielding material and an energy storage material.
The following further describes a method for producing a highly ordered graphite film according to the present invention with specific examples. This section further illustrates the present invention with reference to specific examples, which should not be construed as limiting the invention. The technical means employed in the examples are conventional means well known to those skilled in the art, unless otherwise specified. Reagents, methods and apparatus employed in the present invention are conventional in the art unless otherwise indicated.
Example 1
The embodiment of the application provides a preparation method of a high-order graphite film, which comprises the following steps:
s1, adding 1.0 short-cut aramid fiber into a mixed solvent consisting of 20mL of water and 500mL of DMSO, adding 1.5g of KOH, and stirring at room temperature for 4 hours to obtain a uniform, transparent and dark red aramid nanofiber dispersion liquid;
s2, subjecting the aramid nano-fiber dispersion liquid to vacuum filtration through a filter membrane with the aperture of 0.22 mu m, and drying at 60 ℃ for 6 hours to obtain an aramid nano-fiber membrane;
s3, placing the obtained aramid fiber nanofiber membrane in a tube furnace, heating to 1300 ℃ at a heating rate of 5 ℃/min in an argon atmosphere, preserving heat for 1h, and then naturally cooling to finish carbonization;
s4, placing the carbonized aramid fiber nanofiber membrane in a tubular furnace, heating to 2500 ℃ at a heating rate of 15 ℃/min in an argon atmosphere, preserving heat for 1h, and then naturally cooling in argon flow to complete graphitization;
and S5, finally, placing the graphitized aramid fiber nanofiber membrane on a static pressure machine, and calendering for 2 hours under 20Mpa to obtain the high-order-degree graphite membrane.
Example 2
The embodiment of the application provides a preparation method of a high-order graphite film, which comprises the following steps:
s1, adding 1.0 short-cut aramid fibers into 500mL of DMSO solvent, adding 1.5g of KOH, and stirring at room temperature for 7d to obtain a uniform, transparent and deep red aramid nanofiber dispersion liquid;
s2, subjecting the aramid nano-fiber dispersion liquid to vacuum filtration through a filter membrane with the aperture of 0.22 mu m, and drying at 60 ℃ for 6 hours to obtain an aramid nano-fiber membrane;
s3, placing the obtained aramid fiber nanofiber membrane in a tube furnace, heating to 1300 ℃ at a heating rate of 10 ℃/min in an argon atmosphere, preserving heat for 1h, and then naturally cooling to finish carbonization;
s4, placing the carbonized aramid fiber nanofiber membrane in a tubular furnace, heating to 2850 ℃ at a heating rate of 20 ℃/min in an argon atmosphere, preserving heat for 1h, and then naturally cooling in argon flow to complete graphitization;
and S5, finally, placing the graphitized aramid fiber nanofiber membrane on a static pressure machine, and calendering for 2 hours under 50Mpa to obtain the high-order-degree graphite membrane.
Example 3
The embodiment of the application provides a preparation method of a high-order graphite film, which comprises the following steps:
s1, adding 2.0 short-cut aramid fibers into 100mL of DMSO solvent, adding 1.5g of KOH, and stirring at room temperature for 8d to obtain a uniform, viscous and deep red aramid nanofiber dispersion liquid;
s2, coating the aramid nano-fiber dispersion liquid on a polytetrafluoroethylene substrate in a blade mode, and drying for 6 hours at the temperature of 80 ℃ to obtain an aramid nano-fiber film;
s3, placing the obtained aramid fiber nanofiber membrane in a tubular furnace, heating to 1600 ℃ at a heating rate of 10 ℃/min in an argon atmosphere, preserving heat for 1h, and then naturally cooling to finish carbonization;
s4, placing the carbonized aramid fiber nanofiber membrane in a tubular furnace, heating to 2850 ℃ at a heating rate of 10 ℃/min in an argon atmosphere, preserving heat for 2 hours, and then naturally cooling in argon flow to complete graphitization;
and S5, finally, placing the graphitized aramid fiber nanofiber membrane on a static pressure machine, and pressing and rolling for 2 hours under the pressure of 30Mpa to obtain the high-order-degree graphite membrane.
Comparative example 1
The comparative example provides a method of preparing a carbonized film, comprising the steps of:
s1, adding 1.0 short-cut aramid fiber into a mixed solvent consisting of 20mL of water and 500mL of DMSO, adding 1.5g of KOH, and stirring at room temperature for 4 hours to obtain a uniform, transparent and dark red aramid nanofiber dispersion liquid;
s2, subjecting the aramid nano-fiber dispersion liquid to vacuum filtration through a filter membrane with the aperture of 0.22 mu m, and drying at 60 ℃ for 6 hours to obtain an aramid nano-fiber membrane;
s3, placing the obtained aramid fiber nanofiber membrane in a tube furnace, heating to 1300 ℃ at a heating rate of 5 ℃/min in an argon atmosphere, preserving heat for 1h, then naturally cooling, and completing carbonization to obtain the carbonized membrane.
Performance testing
An optical picture of the highly ordered graphite film prepared in example 1 is shown in fig. 1.
The XRD pattern of the highly ordered graphite film prepared in example 2 is shown in FIG. 2.
As can be seen from fig. 2, the high ordered graphite film prepared in example 2 has a sharp and strong X-ray diffraction peak and the same interlayer spacing of 0.334nm as that of graphite.
FIG. 3 is a surface scanning electron micrograph of the highly ordered graphite film prepared in example 3, and FIG. 4 is a cross-sectional scanning electron micrograph of the highly ordered graphite film prepared in example 3.
As can be seen from fig. 3 to 4, the high-order graphite film prepared in example 3 has a relatively flat and particle-free surface, has a high degree of densification in the cross-sectional direction, and is arranged in parallel in a layered manner.
The high-order degree graphite film prepared in example 3 was tested for thermal diffusivity, as shown in fig. 5.
As can be seen from FIG. 5, the thermal diffusivity of the highly ordered graphite film prepared in example 3 is 724.5mm 2 /s。
The thickness, sheet resistance and conductivity data of the graphite film before and after calendering in example 2 were tested and the results are shown in table 1 below.
TABLE 1 thickness, sheet resistance, and conductivity data for graphite films before and after calendering in EXAMPLE 2
| Thickness (μm) | Square resistance (m omega) | Conductivity (S/m) | |
| Graphite film before rolling | 18 | 224 | 2.48×10 5 |
| Graphite film after rolling | 2.1 | 285 | 1.67×10 6 |
The carbonized film prepared by the method of comparative example 1 described above had poor flexibility, large surface roughness, and electric conductivity of only 2.45X 10 4 S/m。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of a high-order graphite film is characterized by comprising the following steps:
subjecting aramid fibers to chemical cracking to obtain an aramid nanofiber dispersion liquid;
preparing the aramid nano-fiber dispersion liquid into a film to obtain an aramid nano-fiber film;
placing the obtained aramid fiber nanofiber membrane in inert gas for carbonization at 500-2000 ℃;
and (3) graphitizing the carbonized aramid fiber nanofiber membrane in inert gas at 2000-3000 ℃ to obtain the high-order-degree graphite membrane.
2. The preparation method of the high-order graphite film according to claim 1, wherein the aramid fiber is subjected to chemical cracking to obtain an aramid nanofiber dispersion liquid, and specifically comprises the following steps: adding aramid fibers into a DMSO (dimethyl sulfoxide) solvent or a mixed solvent of DMSO and water, adding KOH, and dispersing to obtain an aramid nanofiber dispersion liquid.
3. The preparation method of the high-order graphite film according to claim 1, wherein the concentration of the aramid nanofiber dispersion liquid is 0.01-60 mg/mL.
4. The preparation method of the high-order graphite film according to claim 1, wherein the thickness of the aramid nanofiber film is 1-150 μm.
5. The method for preparing a highly ordered graphite film according to claim 1, wherein the carbonization time is 30 to 360 min; the graphitization time is 30-360 min.
6. The preparation method of the high-order graphite film according to claim 1, wherein the obtained aramid nanofiber film is put in inert gas and carbonized at a temperature rising rate of 1-15 ℃/min to 500-2000 ℃;
and (3) placing the carbonized aramid nano fiber membrane in inert gas, and heating to 2000-3000 ℃ at the speed of 1-15 ℃/min for graphitization.
7. The method of claim 1, wherein the inert gas is supplied at a flow rate of 10 to 800ml/min during the carbonization and graphitization.
8. The preparation method of the high-order graphite film as claimed in any one of claims 1 to 7, further comprising placing the graphitized aramid nanofiber film on a static pressure machine and rolling for 1-3 hours under 20-50 Mpa to obtain the high-order graphite film.
9. The method for preparing the high-order degree graphite film according to claim 1, wherein the aramid nanofiber dispersion is prepared into a film by any one of a vacuum filtration method, a spin-coating method, a spray-coating method, a hydrothermal evaporation method and a doctor blade coating method;
wherein, the vacuum filtration method specifically comprises the following steps: filtering the aramid nano-fiber dispersion liquid in vacuum by using a filter membrane, and drying at 25-105 ℃ for 2-24 hours to obtain an aramid nano-fiber membrane;
the scraper coating method comprises the following specific steps: and (3) carrying out blade coating on the aramid nano-fiber dispersion liquid on a substrate, and drying for 2-24 h at the temperature of 25-105 ℃ to obtain the aramid nano-fiber membrane.
10. The application of the high-order graphite film prepared by the preparation method according to any one of claims 1 to 9 as a heat dissipation material, an electromagnetic shielding material and an energy storage material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115571877A (en) * | 2022-09-30 | 2023-01-06 | 浙江中科玖源新材料有限公司 | Aramid fiber-based graphite film and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030064017A1 (en) * | 2001-05-22 | 2003-04-03 | Masayuki Tobita | Carbon fiber powder, a method of making the same, and thermally conductive composition |
| US20160059444A1 (en) * | 2014-08-29 | 2016-03-03 | Yanbo Wang | Production of highly conductive graphitic films from polymer films |
| CN106968128A (en) * | 2017-04-12 | 2017-07-21 | 株洲时代新材料科技股份有限公司 | A kind of soft graphite alkenyl extrusion coating paper and its preparation method and application |
| CN110205862A (en) * | 2019-06-10 | 2019-09-06 | 陕西科技大学 | A kind of preparation method of aramid nano-fiber self-reinforcing aramid fiber mica paper |
| CN111170316A (en) * | 2020-01-04 | 2020-05-19 | 松山湖材料实验室 | Preparation method of isotropic high-thermal-conductivity carbon nanofiber membrane and product thereof |
| CN111285352A (en) * | 2020-02-20 | 2020-06-16 | 陕西科技大学 | High-temperature carbonized aramid nanofiber conductive material and preparation method thereof |
| WO2021020922A1 (en) * | 2019-08-01 | 2021-02-04 | 코오롱인더스트리 주식회사 | Method for manufacturing graphite sheet |
| CN112409613A (en) * | 2020-11-19 | 2021-02-26 | 陕西科技大学 | Preparation method of aramid nanofiber dispersion liquid |
| CN113389080A (en) * | 2021-06-28 | 2021-09-14 | 陕西科技大学 | Aramid fiber modification method |
-
2022
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030064017A1 (en) * | 2001-05-22 | 2003-04-03 | Masayuki Tobita | Carbon fiber powder, a method of making the same, and thermally conductive composition |
| US20160059444A1 (en) * | 2014-08-29 | 2016-03-03 | Yanbo Wang | Production of highly conductive graphitic films from polymer films |
| CN106968128A (en) * | 2017-04-12 | 2017-07-21 | 株洲时代新材料科技股份有限公司 | A kind of soft graphite alkenyl extrusion coating paper and its preparation method and application |
| CN110205862A (en) * | 2019-06-10 | 2019-09-06 | 陕西科技大学 | A kind of preparation method of aramid nano-fiber self-reinforcing aramid fiber mica paper |
| WO2021020922A1 (en) * | 2019-08-01 | 2021-02-04 | 코오롱인더스트리 주식회사 | Method for manufacturing graphite sheet |
| CN111170316A (en) * | 2020-01-04 | 2020-05-19 | 松山湖材料实验室 | Preparation method of isotropic high-thermal-conductivity carbon nanofiber membrane and product thereof |
| CN111285352A (en) * | 2020-02-20 | 2020-06-16 | 陕西科技大学 | High-temperature carbonized aramid nanofiber conductive material and preparation method thereof |
| CN112409613A (en) * | 2020-11-19 | 2021-02-26 | 陕西科技大学 | Preparation method of aramid nanofiber dispersion liquid |
| CN113389080A (en) * | 2021-06-28 | 2021-09-14 | 陕西科技大学 | Aramid fiber modification method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115571877A (en) * | 2022-09-30 | 2023-01-06 | 浙江中科玖源新材料有限公司 | Aramid fiber-based graphite film and preparation method thereof |
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