CN111040222A - Preparation method of graphene electromagnetic shielding film - Google Patents
Preparation method of graphene electromagnetic shielding film Download PDFInfo
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- CN111040222A CN111040222A CN201911314741.6A CN201911314741A CN111040222A CN 111040222 A CN111040222 A CN 111040222A CN 201911314741 A CN201911314741 A CN 201911314741A CN 111040222 A CN111040222 A CN 111040222A
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
Abstract
The invention belongs to the field of electronic devices and radio application, and particularly relates to a preparation method of a graphene electromagnetic shielding film for electronic devices and radio parts. Preparing graphene dispersion liquid by taking high-conductivity intrinsic graphene powder as a raw material, adopting a needle injection centrifugal membrane preparation method, injecting the graphene dispersion liquid into the surface of a membrane forming substrate by using an injection needle, moving the injection needle according to a set area so as to obtain a set graphene dispersion liquid film, spreading the graphene dispersion liquid film on the membrane forming substrate, utilizing centrifugal force and shearing force generated by a rotary drum to directionally arrange graphene sheets, and heating and drying the graphene dispersion liquid film so as to obtain the graphene electromagnetic shielding membrane. The method of the invention firstly applies the needle injection centrifugal membrane making method to the field of electromagnetic shielding membrane material manufacture, has high efficiency in the preparation process, and can realize the industrial production of high-performance electromagnetic shielding membrane materials.
Description
Technical Field
The invention belongs to the field of electronic devices and radio application, and particularly relates to a preparation method of a graphene electromagnetic shielding film for electronic devices and radio parts.
Background
The rapid development of electronic equipment has led to more and more serious electromagnetic pollution, which generates great interference to the stable operation of precise electronic equipment, and the protection by using high-performance electromagnetic shielding materials becomes a main way for protecting precise electronic devices from interference. In highly integrated portable electronic devices, the shielding material is required to have not only an excellent electromagnetic shielding effect but also comprehensive properties such as ultra-thin, ultra-light, and high thermal conductivity.
Due to the characteristics of high electrical conductivity and a sheet structure of the two-dimensional material represented by graphene, the layered thin film material formed by directional assembly of graphene not only has excellent electromagnetic shielding performance, but also has the characteristics of low density and high thermal conductivity, and is a recognized novel material with excellent electromagnetic shielding performance at present. However, graphene electromagnetic shielding materials reported at present are all prepared by using graphene oxide as a raw material, and high conductivity and good electromagnetic shielding performance can be obtained only by performing high-temperature graphitization treatment, so that the preparation process is complex, the period is long, and the graphitization cost is high, and therefore, a new method for preparing a graphene electromagnetic shielding film at low cost and high efficiency is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene electromagnetic shielding film, which is characterized in that intrinsic graphene with high crystallization quality is used as a raw material, the intrinsic graphene film is prepared by a centrifugal film-making method, and the intrinsic graphene film with a special layered structure is prepared by optimizing a centrifugal film-making process, so that the intrinsic graphene film has excellent electromagnetic shielding performance and related comprehensive performance.
The technical scheme of the invention is as follows:
a preparation method of a graphene electromagnetic shielding film comprises the steps of preparing graphene dispersion liquid by taking high-conductivity intrinsic graphene powder as a raw material, adopting a needle injection centrifugal film-making method, injecting the graphene dispersion liquid into the surface of a film-forming substrate by using an injection needle, moving the injection needle according to a set area so as to obtain a set graphene dispersion liquid film, spreading the graphene dispersion liquid film on the film-forming substrate, utilizing centrifugal force and shearing force generated by a rotary drum to directionally arrange graphene sheets, and heating and drying the graphene dispersion liquid film so as to obtain the graphene electromagnetic shielding film; wherein the inner diameter range of the rotary drum is 10-1000 mm, and the rotating speed range of the rotary drum is 10-10000 rpm; the inner diameter of the needle adopted by the needle injection centrifugal membrane preparation method is 10 mu m-1 cm, the moving speed range of the needle is 10 mm/min-1000 mm/min, the flow rate of the graphene dispersion liquid is 1 ml/min-100 ml/min, and the heating and drying temperature is 50-150 ℃.
According to the preparation method of the graphene electromagnetic shielding film, intrinsic graphene is high-crystalline-quality graphene, the sheet diameter size range of the intrinsic graphene is 0.1-500 mu m, the sheet thickness range is 0.34-10 nm, the carbon content of the graphene is more than 80 wt%, and the powder conductivity range of the graphene is as follows: 1 to 10000S/cm.
According to the preparation method of the graphene electromagnetic shielding film, preferably, the sheet diameter size range of intrinsic graphene is 1-50 mu m, the sheet thickness range is 0.34-3.4 nm, the carbon content of graphene is more than 95 wt%, and the powder conductivity range of graphene is 100-5000S/cm.
According to the preparation method of the graphene electromagnetic shielding film, intrinsic graphene powder is prepared into graphene dispersion liquid through a solvent and a dispersing agent, the concentration range of graphene is 0.01-50 mg/ml, and the concentration range of the dispersing agent is 0.005-50 mg/ml.
According to the preparation method of the graphene electromagnetic shielding film, the preferable concentration range of graphene is 0.1-5 mg/ml, and the concentration range of a dispersing agent is 0.05-10 mg/ml.
According to the preparation method of the graphene electromagnetic shielding film, a solvent comprises one or more than two mixed solvents of water, ethanol, acetone, ethyl acetate, N-methyl pyrrolidone, N-dimethylformamide, xylene and hexane, and a dispersing agent comprises one or more than two mixed dispersing agents of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium deoxycholate and pyrenebutyric acid.
According to the preparation method of the graphene electromagnetic shielding film, the diameter range of the rotary drum is preferably 100-500 mm, and the rotating speed range of the rotary drum is preferably 500-5000 rpm.
The preparation method of the graphene electromagnetic shielding film is preferably characterized in that the inner diameter of a needle used in the needle injection centrifugal film preparation method is 100-0.5 mm, the moving speed range of the needle is 100-600 mm/min, the flow rate of a graphene dispersion liquid is 10-60 ml/min, and the heating and drying temperature is 80-120 ℃.
According to the preparation method of the graphene electromagnetic shielding film, a film forming matrix is a fluoroplastic release film, a polyethylene terephthalate film, a polytetrafluoroethylene film, an aluminum foil, a copper foil, a polyethylene film or a polyimide film.
The technical principle of the invention is as follows:
the invention provides a needle-injection-based centrifugal membrane-making method for preparing a graphene electromagnetic shielding membrane based on the Chinese patent with the publication number of 110274803A, and particularly relates to a method for preparing a graphene electromagnetic shielding membrane based on a needle-injection centrifugal membrane-making method.
The invention has the advantages and beneficial effects that:
1. the method of the invention firstly applies the needle injection centrifugal membrane making method to the field of electromagnetic shielding, has high efficiency in the preparation process, and can realize the industrial production of high-performance electromagnetic shielding membrane materials.
2. The preparation method realizes the preparation of graphene films with different thicknesses, and has an adjustable range of 1-1000 microns.
3. The graphene electromagnetic shielding film prepared by the invention has a highly oriented structure and a multiple reflection effect on electromagnetic waves, so that the graphene electromagnetic shielding film has excellent shielding performance.
Drawings
Fig. 1 is a schematic diagram of a principle of preparing graphene electromagnetic shielding by using a needle injection centrifugal membrane preparation method. In the figure, 1 is a rotary roller, 2 is a film forming substrate, 3 is a graphene film, and 4 is an injection needle.
Detailed Description
In the specific implementation process, high-conductivity intrinsic graphene powder is used as a raw material to prepare a graphene dispersion liquid, and the graphene dispersion liquid is prepared into a graphene film with a special layered structure by adopting an injection centrifugal film preparation technology and optimizing film preparation parameters, so that the graphene film has excellent electromagnetic shielding performance and related comprehensive performance. Wherein the "special layered structure" means: the graphene sheet layers are directionally arranged and stacked along the film direction to form a film, and the arrangement angle of the graphene sheet layers along the graphene film direction is within 0-20 degrees. The electromagnetic shielding effectiveness of the graphene electromagnetic shielding film is 30-150 dB, the conductivity range of the graphene electromagnetic shielding film is 100-5000S/cm, and the thickness of the graphene electromagnetic shielding film is 1-1000 mu m.
As shown in fig. 1, first, the film formation substrate 2 is attached to the inner wall of the rotary drum 1, the rotary drum 1 and the film formation substrate 2 are rotated at a set rotation speed, the rotary drum 1 and the film formation substrate 2 are heated at a set temperature by a heating device, and graphene is arranged into a set graphene dispersion liquid through a solvent and a dispersant. Injecting the graphene dispersion liquid into the surface of the film forming substrate 2 by using an injection needle 4, moving the injection needle 4 according to a set area, so as to obtain a set graphene dispersion liquid film, spreading the graphene dispersion liquid film on the film forming substrate 2, directionally arranging graphene sheets by using centrifugal force and shearing force generated by a rotary drum 1, heating and drying the graphene dispersion liquid film, thereby obtaining a highly-oriented graphene film 3, and applying the highly-oriented graphene film to the field of electromagnetic shielding. Wherein, the "high orientation" of the highly oriented graphene film means: the graphene sheet layers are directionally arranged and stacked along the film direction to form a film, and the arrangement angle of the graphene sheet layers along the graphene film direction is within 0-20 degrees.
The drawings and examples of the present invention are intended to describe the embodiments of the present invention in further detail, and the following three examples are illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1.
In this embodiment, the used film-forming base material is a fluoroplastic release film, a rotating drum with an inner diameter of 100mm and a length of 100mm is adopted, the rotating speed of the rotating drum is 2000rpm, an injection needle adopts an inner diameter of 200 μm, the moving speed of the needle is 600mm/min, the moving distance is 80mm, the concentration of graphene in the used graphene dispersion liquid is 2.5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 100 wt% of the graphene. The flow rate of the graphene dispersion liquid is 30ml/min, the repeated scanning times are 500 times, the heating and drying temperature is 100 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 2000S/cm, and the electromagnetic shielding efficiency is 90 dB.
Example 2.
In this embodiment, the used film-forming base material is a fluoroplastic release film, a rotating drum with an inner diameter of 230mm and a length of 150mm is adopted, the rotating speed of the rotating drum is 1500rpm, an injection needle adopts an inner diameter of 200 μm, the moving speed of the needle is 500mm/min, the moving distance is 140mm, the concentration of graphene in the used graphene dispersion liquid is 2.5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 100 wt% of the graphene. The flow rate of the graphene dispersion liquid is 20ml/min, the repeated scanning times are 500 times, the heating and drying temperature is 90 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 1600S/cm, and the electromagnetic shielding effectiveness is 80 dB.
Example 3.
In this embodiment, the used film-forming base material is a fluoroplastic release film, a rotating drum with an inner diameter of 330mm and a length of 200mm is adopted, the rotating speed of the rotating drum is 1000rpm, an injection needle adopts an inner diameter of 260 μm, the moving speed of the needle is 300mm/min, the moving distance is 180mm, the concentration of graphene in the used graphene dispersion liquid is 2.5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 100 wt% of the graphene. The flow rate of the graphene dispersion liquid is 10ml/min, the repeated scanning times are 400 times, the heating and drying temperature is 80 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 1500S/cm, and the electromagnetic shielding effectiveness is 70 dB.
Example 4.
In this embodiment, the used film-forming base material is a fluoroplastic release film, a rotating drum with an inner diameter of 500mm and a length of 400mm is adopted, the rotating speed of the rotating drum is 500rpm, an injection needle adopts an inner diameter of 500 μm, the moving speed of the needle is 200mm/min, the moving distance is 300mm, the concentration of graphene in the used graphene dispersion liquid is 5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 50 wt% of graphene. The flow rate of the graphene dispersion liquid is 40ml/min, the repeated scanning times are 200 times, the heating and drying temperature is 110 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 1000S/cm, and the electromagnetic shielding efficiency is 50 dB.
Example 5.
In this embodiment, the used film-forming base material is a polyethylene terephthalate film, a rotating drum with an inner diameter of 500mm and a length of 400mm is adopted, the rotating speed of the rotating drum is 800rpm, an injection needle adopts an inner diameter of 500 μm, the moving speed of the needle is 200mm/min, the moving distance is 350mm, the concentration of graphene in the used graphene dispersion liquid is 5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 50 wt% of the graphene. The flow rate of the graphene dispersion liquid is 50ml/min, the repeated scanning times are 100 times, the heating and drying temperature is 120 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 1200S/cm, and the electromagnetic shielding effectiveness is 55 dB.
Example 6.
In this embodiment, the used film-forming base material is a polyethylene terephthalate film, a rotating drum with an inner diameter of 1000mm and a length of 500mm is adopted, the rotating speed of the rotating drum is 500rpm, an injection needle adopts an inner diameter of 1000 μm, the moving speed of the needle is 100mm/min, the moving distance is 450mm, the concentration of graphene in the used graphene dispersion liquid is 5mg/ml, the dispersion solvent is water, the dispersant is polyvinylpyrrolidone, and the dosage of the dispersant is 50 wt% of the graphene. The flow rate of the graphene dispersion liquid is 60ml/min, the repeated scanning times are 100 times, the heating and drying temperature is 130 ℃, the thickness of the prepared graphene film is 40 mu m, the conductivity is 1000S/cm, and the electromagnetic shielding efficiency is 50 dB.
The above 6 examples are further illustrative of the present invention, and several changes and modifications can be made in each electrolysis step without departing from the principle of the present invention, and should be construed as the protection scope of the present invention.
Claims (9)
1. A preparation method of a graphene electromagnetic shielding film is characterized in that high-conductivity intrinsic graphene powder is used as a raw material to prepare a graphene dispersion liquid, a needle injection centrifugal film-making method is adopted, the graphene dispersion liquid is injected onto the surface of a film-forming substrate by using an injection needle, the injection needle is moved according to a set area, so that a set graphene dispersion liquid film is obtained and spread on the film-forming substrate, graphene sheets are directionally arranged by using centrifugal force and shearing force generated by a rotary drum, and the graphene dispersion liquid film is heated and dried, so that the graphene electromagnetic shielding film is obtained; wherein the inner diameter range of the rotary drum is 10-1000 mm, and the rotating speed range of the rotary drum is 10-10000 rpm; the inner diameter of the needle adopted by the needle injection centrifugal membrane preparation method is 10 mu m-1 cm, the moving speed range of the needle is 10 mm/min-1000 mm/min, the flow rate of the graphene dispersion liquid is 1 ml/min-100 ml/min, and the heating and drying temperature is 50-150 ℃.
2. The preparation method of the graphene electromagnetic shielding film according to claim 1, wherein the intrinsic graphene is high-crystalline-quality graphene, the sheet diameter size of the intrinsic graphene is 0.1-500 μm, the sheet thickness is 0.34-10 nm, the carbon content of the intrinsic graphene is more than 80 wt%, and the powder conductivity of the intrinsic graphene is in the following range: 1 to 10000S/cm.
3. The preparation method of the graphene electromagnetic shielding film according to claim 2, wherein preferably, the intrinsic graphene has a sheet diameter size ranging from 1 to 50 μm, a sheet thickness ranging from 0.34 to 3.4nm, a graphene carbon content of more than 95 wt%, and a powder conductivity ranging from 100 to 5000S/cm.
4. The preparation method of the graphene electromagnetic shielding film according to claim 1, wherein the intrinsic graphene powder is prepared into a graphene dispersion liquid through a solvent and a dispersant, the concentration range of graphene is 0.01-50 mg/ml, and the concentration range of the dispersant is 0.005-50 mg/ml.
5. The method for preparing a graphene electromagnetic shielding film according to claim 4, wherein the concentration of the graphene is preferably in the range of 0.1 to 5mg/ml, and the concentration of the dispersing agent is preferably in the range of 0.05 to 10 mg/ml.
6. The method for preparing a graphene electromagnetic shielding film according to claim 4 or 5, wherein the solvent includes but is not limited to one or more mixed solvents of water, ethanol, acetone, ethyl acetate, N-methyl pyrrolidone, N-dimethylformamide, xylene and hexane, and the dispersant includes but is not limited to one or more mixed dispersants of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium deoxycholate and pyrenebutyric acid.
7. The method for preparing a graphene electromagnetic shielding film according to claim 1, wherein preferably, the diameter of the rotating drum is in a range of 100 to 500mm, and the rotating speed of the rotating drum is in a range of 500 to 5000 rpm.
8. The method for preparing a graphene electromagnetic shielding film according to claim 1, wherein preferably, the inner diameter of the needle used in the needle injection centrifugal film-making method is 100 μm to 0.5mm, the moving speed range of the needle is 100mm/min to 600mm/min, the flow rate of the graphene dispersion liquid is 10ml/min to 60ml/min, and the heating and drying temperature is 80 ℃ to 120 ℃.
9. The method for preparing a graphene electromagnetic shielding film according to claim 1, wherein the film forming substrate is a fluoroplastic release film, a polyethylene terephthalate film, a polytetrafluoroethylene film, an aluminum foil, a copper foil, a polyethylene film or a polyimide film.
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Cited By (5)
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| CN112341848A (en) * | 2020-11-05 | 2021-02-09 | 上海理工大学 | Graphene coating and preparation method of graphene conductive corrosion-resistant coating |
| CN112456480A (en) * | 2020-12-02 | 2021-03-09 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Graphene membrane material, preparation method and application thereof |
| CN112691558A (en) * | 2020-12-02 | 2021-04-23 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Preparation method and system of membrane material |
| CN114213849A (en) * | 2021-12-07 | 2022-03-22 | 佛山(华南)新材料研究院 | Insulating heat-conducting gasket and preparation method thereof |
| CN115125726A (en) * | 2022-05-25 | 2022-09-30 | 浙江理工大学 | Graphene fiber felt with directional electromagnetic shielding function and preparation method thereof |
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| CN114213849A (en) * | 2021-12-07 | 2022-03-22 | 佛山(华南)新材料研究院 | Insulating heat-conducting gasket and preparation method thereof |
| CN115125726A (en) * | 2022-05-25 | 2022-09-30 | 浙江理工大学 | Graphene fiber felt with directional electromagnetic shielding function and preparation method thereof |
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