CN110258106B - Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene - Google Patents
Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene Download PDFInfo
- Publication number
- CN110258106B CN110258106B CN201910657184.1A CN201910657184A CN110258106B CN 110258106 B CN110258106 B CN 110258106B CN 201910657184 A CN201910657184 A CN 201910657184A CN 110258106 B CN110258106 B CN 110258106B
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- fiber fabric
- electromagnetic shielding
- type flexible
- shielding material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
A preparation method of a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nano-particles and graphene relates to a preparation method of an electromagnetic shielding material. The invention solves the problems that the traditional preparation method of the existing electromagnetic shielding composite material 'mixing-molding' influences the flexibility of the composite material, some non-environment-friendly chemical reagents are involved, and the distribution of active ingredients and the construction of a specific micro-morphology are difficult to accurately control, so that the shielding performance is difficult to improve. The preparation method comprises the following steps: firstly, preparing a carbon fiber fabric; secondly, preparing a metal nickel nanoparticle/carbon fiber fabric composite material by magnetron sputtering; and thirdly, carrying out plasma enhanced chemical vapor deposition. The invention is used for preparing the electromagnetic shielding material.
Description
Technical Field
The invention relates to a preparation method of an electromagnetic shielding material.
Background
In recent years, the wide use of radio frequency devices in many fields such as communications and medical treatment has caused large-scale electromagnetic pollution, which not only interferes with the normal operation of precision equipment, but also poses a great threat to human health. Therefore, the development of novel environment-friendly, light and high-performance electromagnetic shielding materials has significant research significance. The active ingredients of the electromagnetic shielding material can be roughly classified into three types, i.e., magnetic materials (e.g., carbonyl iron, iron oxide, etc.), dielectric materials (e.g., carbon materials, etc.), and conductive polymers (e.g., polypyrrole, polyaniline, etc.). Carbon materials have been widely used in the field of electromagnetic shielding because of their advantages such as high electrical conductivity, strong oxidation resistance, high thermal stability, and light weight. The graphene is a novel carbon material, and has high specific surface area, high aspect ratio and high conductivity, so that the graphene is favorable for obtaining high polarization amount and polarization loss when being used as an electromagnetic shielding material. In addition, compared with electromagnetic shielding materials such as metal or polymer, graphene materials generally have good flexibility, significantly lower density and excellent processability, and can meet the requirements as an electromagnetic shielding layer of current portable electronic devices. Due to the fact that the cost of graphene is high, in order to better utilize the graphene in the field of electromagnetic shielding, the amount of graphene used in a mode of doping the graphene and a matrix material is obviously less (namely the cost is lower) than that used in a mode of directly preparing a single-component graphene product, and the preparation mode is more flexible. In the preparation method of the graphene-based electromagnetic shielding composite material, "hybrid-molding" is a simple and very common method, i.e., mixing an active material such as graphene into a polymer matrix, and then performing processes such as polymerization and molding. However, this method usually affects the flexibility of the composite material and involves some non-environmental chemicals, and many polymer matrices (e.g., polyvinylidene fluoride, epoxy, polyvinyl alcohol, etc.) used in this method are insulating, i.e., do not have significant responsiveness to electromagnetic fields. In addition, it is difficult to accurately control the distribution of the active ingredients and to construct a specific micro-morphology in this manner, both of which have been shown to have important effects on electromagnetic shielding performance.
Disclosure of Invention
The invention provides a preparation method of a sandwich type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nano particles and graphene, aiming at solving the problems that the traditional preparation method of the existing electromagnetic shielding composite material through mixing-molding affects the flexibility of the composite material, some non-environment-friendly chemical reagents are involved, and the distribution of active ingredients and the construction of a specific micro morphology are difficult to accurately control, so that the shielding performance is difficult to improve.
A preparation method of a sandwich type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nano particles and graphene is carried out according to the following steps:
firstly, preparing a carbon fiber fabric:
placing a container filled with a biomass fiber fabric in a high-temperature pyrolysis device, introducing inert gas into the high-temperature pyrolysis device for 1-60 min, raising the temperature of the high-temperature pyrolysis device to 200-2000 ℃ at a temperature raising rate of 0.1-10 ℃/min under the protection of the inert gas, preserving the temperature for 0.1-10 h at the temperature of 200-2000 ℃, and then lowering the temperature of the high-temperature pyrolysis device from 200-2000 ℃ to room temperature at a temperature lowering rate of 0.1-10 ℃/min to obtain a carbon fiber fabric;
secondly, preparing the metal nickel nanoparticle/carbon fiber fabric composite material by magnetron sputtering:
placing a carbon fiber fabric in magnetron sputtering equipment, firstly fixing a nickel target material on a cathode, fixing the carbon fiber fabric on an anode of a sample platform, controlling the distance between the nickel target material and the carbon fiber fabric to be 1-100 mm, then forcibly pumping the pressure in a reaction chamber of the magnetron sputtering equipment to be 0.001-1 Pa, introducing argon at the flow rate of 1-100 sccm, and finally sputtering under the conditions that the sputtering power is 10-1000W and the rotation speed of the sample platform is 1-100 rpm until the thickness of a sputtered metal nickel nanoparticle layer is 100-10000 nm to obtain a metal nickel nanoparticle/carbon fiber fabric composite material;
thirdly, plasma enhanced chemical vapor deposition:
firstly, placing the metal nickel nanoparticle/carbon fiber fabric composite material in plasma enhanced chemical vapor deposition equipment, forcibly pumping the pressure in a reaction chamber of the plasma enhanced chemical vapor deposition equipment to 1 Pa-100 Pa, and then introducing mixed gas of methane and hydrogen at the flow rate of 1 sccm-100 sccm;
the flow rate ratio of methane to hydrogen in the mixed gas of methane and hydrogen is 3 (1.5-2.5);
secondly, depositing for 0.1 to 10 hours under the condition that the radio frequency power is 10 to 1000W, and taking out the material deposited on one surface;
thirdly, repeating the step three and the step two for 1 time to obtain the material with two deposited surfaces;
fourthly, repeating the material subjected to double-sided deposition for 0 to 4 times according to the third step to obtain the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nano particles and the graphene;
the thickness of the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metal nickel nano particles and the graphene is more than 0.62 mm.
The invention has the beneficial effects that:
the interlayer type flexible electromagnetic shielding material prepared by the invention based on the carbon fiber fabric, the metallic nickel nano particles and the graphene has excellent conductivity which can reach 625S m-1。
The interlayer type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nano particles and the graphene has an interlayer type multi-dimensional heterostructure, so that the synergistic effect of all components in the electromagnetic shielding process is facilitated, and the total electromagnetic shielding efficiency can reach 50.6 dB.
The prepared sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene has the characteristics of high flexibility (bending, folding and twisting), light weight and ultrathin thickness, and the density of the material is as low as 113mg/cm3Its thickness is as low as 0.65 mm.
The invention provides a preparation method of a sandwich type flexible electromagnetic shielding material based on carbon fiber fabrics, metal nickel nano particles and graphene.
Drawings
FIG. 1 is a scanning electron microscope image of a carbon fiber fabric prepared in one step one of the examples;
FIG. 2 is a scanning electron microscope image of a metallic nickel nanoparticle/carbon fiber fabric composite material prepared in step two of the example;
fig. 3 is a scanning electron microscope image of the interlayer type flexible electromagnetic shielding material based on carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first embodiment;
fig. 4 is an X-ray diffraction diagram, wherein 1 is a sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first example, and 2 is an X-ray diffraction standard card of metallic nickel;
fig. 5 is a graph of electromagnetic shielding efficiency versus electromagnetic wave frequency for a sandwich-type flexible electromagnetic shielding material based on a carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first embodiment, where 1 is total electromagnetic shielding efficiency, 2 is electromagnetic absorption loss, and 3 is electromagnetic reflection loss;
fig. 6 is a graph of bending effect of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment;
fig. 7 is a folding effect diagram of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment;
fig. 8 is a diagram illustrating the twisting effect of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment.
Detailed Description
The first embodiment is as follows: the embodiment provides a preparation method of a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nanoparticles and graphene, which is carried out according to the following steps:
firstly, preparing a carbon fiber fabric:
placing a container filled with a biomass fiber fabric in a high-temperature pyrolysis device, introducing inert gas into the high-temperature pyrolysis device for 1-60 min, raising the temperature of the high-temperature pyrolysis device to 200-2000 ℃ at a temperature raising rate of 0.1-10 ℃/min under the protection of the inert gas, preserving the temperature for 0.1-10 h at the temperature of 200-2000 ℃, and then lowering the temperature of the high-temperature pyrolysis device from 200-2000 ℃ to room temperature at a temperature lowering rate of 0.1-10 ℃/min to obtain a carbon fiber fabric;
secondly, preparing the metal nickel nanoparticle/carbon fiber fabric composite material by magnetron sputtering:
placing a carbon fiber fabric in magnetron sputtering equipment, firstly fixing a nickel target material on a cathode, fixing the carbon fiber fabric on an anode of a sample platform, controlling the distance between the nickel target material and the carbon fiber fabric to be 1-100 mm, then forcibly pumping the pressure in a reaction chamber of the magnetron sputtering equipment to be 0.001-1 Pa, introducing argon at the flow rate of 1-100 sccm, and finally sputtering under the conditions that the sputtering power is 10-1000W and the rotation speed of the sample platform is 1-100 rpm until the thickness of a sputtered metal nickel nanoparticle layer is 100-10000 nm to obtain a metal nickel nanoparticle/carbon fiber fabric composite material;
thirdly, plasma enhanced chemical vapor deposition:
firstly, placing the metal nickel nanoparticle/carbon fiber fabric composite material in plasma enhanced chemical vapor deposition equipment, forcibly pumping the pressure in a reaction chamber of the plasma enhanced chemical vapor deposition equipment to 1 Pa-100 Pa, and then introducing mixed gas of methane and hydrogen at the flow rate of 1 sccm-100 sccm;
the flow rate ratio of methane to hydrogen in the mixed gas of methane and hydrogen is 3 (1.5-2.5);
secondly, depositing for 0.1 to 10 hours under the condition that the radio frequency power is 10 to 1000W, and taking out the material deposited on one surface;
thirdly, repeating the step three and the step two for 1 time to obtain the material with two deposited surfaces;
fourthly, repeating the material subjected to double-sided deposition for 0 to 4 times according to the third step to obtain the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nano particles and the graphene;
the thickness of the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metal nickel nano particles and the graphene is more than 0.62 mm.
The beneficial effects of the embodiment are as follows:
first, the interlayer-type flexible electromagnetic shielding material prepared by the embodiment based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene has excellent conductivity, and the conductivity of the interlayer-type flexible electromagnetic shielding material can reach 625S m-1。
The interlayer type flexible electromagnetic shielding material based on the carbon fiber fabric, the metal nickel nanoparticles and the graphene prepared by the embodiment has an interlayer type multi-dimensional heterostructure, the synergistic effect of all components in the electromagnetic shielding process is facilitated, and the total electromagnetic shielding efficiency can reach 50.6 dB.
Thirdly, the sandwich type flexible electromagnetic shielding material prepared by the embodiment based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene has high flexibility (bendable, foldable and twistable), light weight and ultra-thin characteristicsSex, its density is as low as 113mg cm-3Its thickness is as low as 0.65 mm.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the biomass fiber fabric in the step one is a bamboo fiber fabric, a cotton fiber fabric, a hemp fiber fabric or a regenerated spinning fiber fabric. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the purity of the nickel target material in the second step is 90.00-99.99%. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the purity of the argon in the step two is 90.00-99.99%. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the purity of the methane in the third step is 90.00-99.99%; the purity of the hydrogen in the third step is 90.00-99.99%. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: placing the container filled with the biomass fiber fabric in a high-temperature pyrolysis device, introducing inert gas into the high-temperature pyrolysis device for 30-60 min, raising the temperature of the high-temperature pyrolysis device to 200-1000 ℃ at a temperature raising rate of 5-10 ℃/min under the protection of the inert gas, preserving the temperature for 1-10 h at the temperature of 200-1000 ℃, and then lowering the temperature of the high-temperature pyrolysis device from 200-1000 ℃ to room temperature at a temperature lowering rate of 5-10 ℃/min to obtain the carbon fiber fabric. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and secondly, controlling the distance between the nickel target material and the carbon fiber fabric to be 60-100 mm, then forcibly pumping the pressure in a reaction chamber of the magnetron sputtering equipment to be 0.003-1 Pa, and then introducing argon at the flow rate of 11-100 sccm. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and finally, sputtering under the conditions that the sputtering power is 100W-1000W and the rotating speed of the sample stage is 20 rpm-100 rpm. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: in the third step, the pressure in the reaction cavity of the plasma enhanced chemical vapor deposition equipment is firstly forcibly pumped to 50 Pa-100 Pa. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and thirdly, depositing for 1-10 h under the condition that the radio frequency power is 200-1000W. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of a sandwich type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nano particles and graphene is carried out according to the following steps:
firstly, preparing a carbon fiber fabric:
placing the container filled with the biomass fiber fabric in a high-temperature pyrolysis device, introducing inert gas into the high-temperature pyrolysis device for 30min, heating the temperature of the high-temperature pyrolysis device to 1000 ℃ at a heating rate of 5 ℃/min under the protection of the inert gas, preserving the heat for 1h at the temperature of 1000 ℃, and then cooling the temperature of the high-temperature pyrolysis device from 1000 ℃ to room temperature at a cooling rate of 5 ℃/min to obtain the carbon fiber fabric;
secondly, preparing the metal nickel nanoparticle/carbon fiber fabric composite material by magnetron sputtering:
placing a carbon fiber fabric in magnetron sputtering equipment, firstly fixing a nickel target material on a cathode, fixing the carbon fiber fabric on an anode of a sample platform, controlling the distance between the nickel target material and the carbon fiber fabric to be 60mm, then forcibly pumping the pressure in a reaction chamber of the magnetron sputtering equipment to 0.003Pa, introducing argon at the flow rate of 11sccm, and finally sputtering under the conditions that the sputtering power is 100W and the rotation speed of the sample platform is 20rpm until the thickness of a sputtered metal nickel nanoparticle layer is 500nm to obtain a metal nickel nanoparticle/carbon fiber fabric composite material;
thirdly, plasma enhanced chemical vapor deposition:
firstly, placing a metal nickel nanoparticle/carbon fiber fabric composite material in plasma enhanced chemical vapor deposition equipment, forcibly pumping the pressure in a reaction chamber of the plasma enhanced chemical vapor deposition equipment to 50Pa, and then introducing mixed gas of methane and hydrogen;
the flow rate of methane in the mixed gas of methane and hydrogen is 8.4sccm, and the flow rate of hydrogen is 5.6 sccm;
depositing for 1h under the condition that the radio frequency power is 200W, and taking out the material deposited on one surface;
thirdly, repeating the step three and the step two for 1 time on the other side of the material with one side deposited to obtain the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nano particles and the graphene;
the thickness of the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metal nickel nano particles and the graphene is 0.65 mm.
The biomass fiber fabric in the step one is a cotton fiber fabric.
And the purity of the nickel target material in the second step is 99.99%.
And the purity of the argon in the second step is 99.99%.
The purity of the methane in the step three is 99.99 percent; the purity of the hydrogen in the third step is 99.99%.
FIG. 1 is a scanning electron microscope image of a carbon fiber fabric prepared in one step one of the examples; as can be seen from the figure, the surface of the carbon fiber is relatively rough, which is beneficial to the mechanical interlocking effect between the metal nanoparticles deposited by magnetron sputtering and the surface of the carbon fiber, so as to enhance the interface adhesion between the metal nanoparticles and the surface of the carbon fiber.
FIG. 2 is a scanning electron microscope image of a metallic nickel nanoparticle/carbon fiber fabric composite material prepared in step two of the example; it can be observed from the figure that the original rough surface of the carbon fiber becomes uniform after the deposition of the metallic nickel nanoparticles.
Fig. 3 is a scanning electron microscope image of the interlayer type flexible electromagnetic shielding material based on carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first embodiment; from the figure, it can be observed that a large amount of compact dandelion-like graphene is successfully grown on the surface of the metal nickel nanoparticle/carbon fiber fabric composite material.
Fig. 4 is an X-ray diffraction diagram, wherein 1 is a sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first example, and 2 is an X-ray diffraction standard card of metallic nickel; as can be seen from the figure, the composite material contains the components of metallic nickel by comparing the X-ray diffraction standard cards of metallic nickel. In addition, the X-ray diffraction signal at 26.7 ° also indicates that the composite material contains graphene.
The interlayer type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment is used for electromagnetic shielding performance, and the test and calculation processes are as follows:
firstly, fixing a sandwich type flexible electromagnetic shielding material which is 22.9mm multiplied by 10.2mm multiplied by 0.65mm and is based on carbon fiber fabric, metal nickel nano particles and graphene on a sample table;
secondly, testing S parameters by using a PNA-X N5244a type network analyzer based on a waveguide method, wherein the testing range is 8.2 GHz-12.4 GHz;
third, total electromagnetic Shielding Effectiveness (SE)total) Electromagnetic absorption loss (SE)A) And electromagnetic reflection loss (SE)T) Calculated by the following formula:
SEtotal(dB)＝-10log[|S21|2]
SER＝-10log(1-|S11|2)
SEA＝-10log[|S21|2/(1-|S11|2)]
fig. 5 is a graph of electromagnetic shielding efficiency versus electromagnetic wave frequency for a sandwich-type flexible electromagnetic shielding material based on a carbon fiber fabric, metallic nickel nanoparticles and graphene prepared in the first embodiment, where 1 is total electromagnetic shielding efficiency, 2 is electromagnetic absorption loss, and 3 is electromagnetic reflection loss; as can be seen from the figure, the electromagnetic shielding material has excellent electromagnetic shielding performance, the total electromagnetic shielding efficiency can reach 50.6dB, and in addition, the electromagnetic absorption loss of the electromagnetic shielding material can reach 29.7dB which is higher than the electromagnetic reflection loss (20.9dB), which shows that the absorption loss of the electromagnetic shielding material is dominant in the electromagnetic shielding effect.
Fig. 6 is a graph of bending effect of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment; fig. 7 is a folding effect diagram of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment; fig. 8 is a diagram illustrating the twisting effect of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment; as can be seen, the composite material has high flexibility and can be bent, folded and distorted.
The interlayer type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene prepared in the first embodiment is tested by adopting a four-probe resistivity tester (model RTS-8, Guangzhou four-probe science and technology Co., Ltd.), and the conductivity can reach 625S m-1。
The volume and the mass of the interlayer type flexible electromagnetic shielding material prepared in the first embodiment and based on the carbon fiber fabric, the metallic nickel nano particles and the graphene are measured, and the density is calculated to be as low as 113mg/cm3And the thickness is as low as 0.65 mm.
Claims (10)
1. A preparation method of a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nanoparticles and graphene is characterized by comprising the following steps:
firstly, preparing a carbon fiber fabric:
placing a container filled with a biomass fiber fabric in a high-temperature pyrolysis device, introducing inert gas into the high-temperature pyrolysis device for 1-60 min, raising the temperature of the high-temperature pyrolysis device to 200-2000 ℃ at a temperature raising rate of 0.1-10 ℃/min under the protection of the inert gas, preserving the temperature for 0.1-10 h at the temperature of 200-2000 ℃, and then lowering the temperature of the high-temperature pyrolysis device from 200-2000 ℃ to room temperature at a temperature lowering rate of 0.1-10 ℃/min to obtain a carbon fiber fabric;
secondly, preparing the metal nickel nanoparticle/carbon fiber fabric composite material by magnetron sputtering:
placing a carbon fiber fabric in magnetron sputtering equipment, firstly fixing a nickel target material on a cathode, fixing the carbon fiber fabric on an anode of a sample platform, controlling the distance between the nickel target material and the carbon fiber fabric to be 1-100 mm, then forcibly pumping the pressure in a reaction chamber of the magnetron sputtering equipment to be 0.001-1 Pa, introducing argon at the flow rate of 1-100 sccm, and finally sputtering under the conditions that the sputtering power is 10-1000W and the rotation speed of the sample platform is 1-100 rpm until the thickness of a sputtered metal nickel nanoparticle layer is 100-10000 nm to obtain a metal nickel nanoparticle/carbon fiber fabric composite material;
thirdly, plasma enhanced chemical vapor deposition:
firstly, placing the metal nickel nanoparticle/carbon fiber fabric composite material in plasma enhanced chemical vapor deposition equipment, forcibly pumping the pressure in a reaction chamber of the plasma enhanced chemical vapor deposition equipment to 1 Pa-100 Pa, and then introducing mixed gas of methane and hydrogen at the flow rate of 1 sccm-100 sccm;
the flow rate ratio of methane to hydrogen in the mixed gas of methane and hydrogen is 3 (1.5-2.5);
secondly, depositing for 0.1 to 10 hours under the condition that the radio frequency power is 10 to 1000W, and taking out the material deposited on one surface;
thirdly, repeating the step three and the step two for 1 time to obtain the material with two deposited surfaces;
fourthly, repeating the material subjected to double-sided deposition for 0 to 4 times according to the third step to obtain the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nano particles and the graphene;
the thickness of the sandwich type flexible electromagnetic shielding material based on the carbon fiber fabric, the metal nickel nano particles and the graphene is more than 0.62 mm.
2. The method for preparing a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nanoparticles and graphene according to claim 1, wherein the biomass fiber fabrics in the step one are bamboo fiber fabrics, cotton fiber fabrics, hemp fiber fabrics or regenerated spinning fiber fabrics.
3. The method for preparing a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nanoparticles and graphene according to claim 1, wherein the purity of the nickel target material in the second step is 90.00% -99.99%.
4. The method for preparing a sandwich-type flexible electromagnetic shielding material based on carbon fiber fabrics, metallic nickel nanoparticles and graphene according to claim 1, wherein the purity of the argon gas in the second step is 90.00-99.99%.
5. The method for preparing the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1, wherein the purity of the methane in the third step is 90.00% -99.99%; the purity of the hydrogen in the third step is 90.00-99.99%.
6. The preparation method of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1 is characterized in that in the first step, the container containing the biomass fiber fabric is placed in a high-temperature pyrolysis device, inert gas is introduced into the high-temperature pyrolysis device for 30-60 min, the temperature of the high-temperature pyrolysis device is increased to 200-1000 ℃ at a heating rate of 5-10 ℃/min under the protection of the inert gas, the temperature is kept for 1-10 h at the temperature of 200-1000 ℃, and then the temperature of the high-temperature pyrolysis device is reduced to room temperature from 200-1000 ℃ at a cooling rate of 5-10 ℃/min to obtain the carbon fiber fabric.
7. The preparation method of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1, characterized in that in the second step, the distance between the nickel target material and the carbon fiber fabric is controlled to be 60mm to 100mm, then the internal pressure of the reaction chamber of the magnetron sputtering device is forcibly pumped to 0.003Pa to 1Pa, and then argon gas is introduced at a flow rate of 11sccm to 100 sccm.
8. The method for preparing the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1, wherein sputtering is finally performed in the second step under the conditions that the sputtering power is 100W-1000W and the rotation speed of the sample stage is 20 rpm-100 rpm.
9. The preparation method of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1 is characterized in that in the third step, the internal pressure of a reaction chamber of plasma enhanced chemical vapor deposition equipment is firstly forcibly pumped to 50-100 Pa.
10. The preparation method of the sandwich-type flexible electromagnetic shielding material based on the carbon fiber fabric, the metallic nickel nanoparticles and the graphene according to claim 1, characterized in that in the third step, the deposition is performed for 1 to 10 hours under the condition that the radio frequency power is 200 to 1000W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910657184.1A CN110258106B (en) | 2019-07-19 | 2019-07-19 | Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910657184.1A CN110258106B (en) | 2019-07-19 | 2019-07-19 | Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110258106A CN110258106A (en) | 2019-09-20 |
| CN110258106B true CN110258106B (en) | 2021-07-09 |
Family
ID=67927401
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910657184.1A Active CN110258106B (en) | 2019-07-19 | 2019-07-19 | Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110258106B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787971B (en) * | 2019-11-28 | 2022-06-14 | 江西邦力达科技股份有限公司 | High-heat-conduction near-infrared electromagnetic shielding film |
| CN112135372B (en) * | 2020-09-08 | 2022-03-25 | 大连理工大学 | Color carbon fiber heat management device with structural color gradient and preparation method thereof |
| CN112608506B (en) * | 2020-12-22 | 2022-11-15 | 聊城大学 | Preparation method of metal nanowire coating/polymer composite material with low contact resistance |
| CN112875647B (en) * | 2021-02-07 | 2022-10-28 | 天津理工大学 | Method for producing hydrogen by catalysis at room temperature |
| CN113088913B (en) * | 2021-04-13 | 2022-03-29 | 安徽工程大学 | Carbon fiber modification method and product thereof |
| CN114539974A (en) * | 2022-02-21 | 2022-05-27 | 厦门大学 | Method for preparing magnetic metal @ graphene wave-absorbing material based on chemical vapor deposition method |
| CN114633531A (en) * | 2022-03-01 | 2022-06-17 | 浙江工业大学 | Preparation method of anisotropic heat-conducting electromagnetic shielding nylon composite film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5952249A (en) * | 1996-12-17 | 1999-09-14 | Textron Systems Corporation | Amorphous carbon-coated carbon fabric wet friction material |
| CN103225203A (en) * | 2013-05-09 | 2013-07-31 | 西北工业大学 | Preparation method of carbon fiber-graphene oxide-carbon nanotube multi-scale reinforcement |
| CN107938323A (en) * | 2018-01-03 | 2018-04-20 | 北京北方国能科技有限公司 | A kind of graphene carbon fiber, its preparation method and its application |
-
2019
- 2019-07-19 CN CN201910657184.1A patent/CN110258106B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5952249A (en) * | 1996-12-17 | 1999-09-14 | Textron Systems Corporation | Amorphous carbon-coated carbon fabric wet friction material |
| CN103225203A (en) * | 2013-05-09 | 2013-07-31 | 西北工业大学 | Preparation method of carbon fiber-graphene oxide-carbon nanotube multi-scale reinforcement |
| CN107938323A (en) * | 2018-01-03 | 2018-04-20 | 北京北方国能科技有限公司 | A kind of graphene carbon fiber, its preparation method and its application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110258106A (en) | 2019-09-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110258106B (en) | Preparation method of sandwich type flexible electromagnetic shielding material based on carbon fiber fabric, metal nickel nanoparticles and graphene | |
| Lei et al. | Electrically conductive gradient structure design of thermoplastic polyurethane composite foams for efficient electromagnetic interference shielding and ultra-low microwave reflectivity | |
| Luo et al. | A double crosslinking MXene/cellulose nanofiber layered film for improving mechanical properties and stable electromagnetic interference shielding performance | |
| Fang et al. | Layer-structured silver nanowire/polyaniline composite film as a high performance X-band EMI shielding material | |
| Qing et al. | Multiwalled carbon nanotubes–BaTiO3/silica composites with high complex permittivity and improved electromagnetic interference shielding at elevated temperature | |
| Bizhani et al. | Double percolated MWCNTs loaded PC/SAN nanocomposites as an absorbing electromagnetic shield | |
| CN109591391B (en) | Low-reflection high-shielding gradient structure foam material | |
| CN108573763B (en) | Preparation method of wire and cable conductor, graphene-coated metal powder and conductor | |
| Zhou et al. | Mechanical, dielectric and microwave absorption properties of FeSiAl/Al2O3 composites fabricated by hot-pressed sintering | |
| Zhou et al. | Comparison in dielectric and microwave absorption properties of SiC coated carbon fibers with PyC and BN interphases | |
| Deng et al. | Controllable graphitization degree of carbon foam bulk toward electromagnetic wave attenuation loss behavior | |
| Zhang et al. | Asymmetric multilayered MXene-AgNWs/cellulose nanofiber composite films with antibacterial properties for high-efficiency electromagnetic interference shielding | |
| Fang et al. | Metal–organic framework-derived carbon/carbon nanotubes mediate impedance matching for strong microwave absorption at fairly low temperatures | |
| CN108929542B (en) | Polydimethylsiloxane/graphene flexible composite film with negative dielectric constant and preparation method thereof | |
| Aïssa et al. | Nanoelectromagnetic of a highly conductive 2D transition metal carbide (MXene)/Graphene nanoplatelets composite in the EHF M-band frequency | |
| Hu et al. | Investigation into electrical conductivity and electromagnetic interference shielding effectiveness of silicone rubber filled with Ag-coated cenosphere particles | |
| CN103087386A (en) | Preparation method of low-percolation graphene/macromolecule electromagnetism shielding material | |
| KR20160133711A (en) | Method for preparation of high concentrated carbon nanotube/graphene dispersion | |
| CN109735826A (en) | A kind of graphene/copper composite material and its preparation method and application | |
| Pu et al. | Hydrothermal synthesis of N-doped graphene/Fe2O3 nanocomposite for supercapacitors | |
| Kim et al. | Transparent and flexible electromagnetic interference shielding film using ITO nanobranches by internal scattering | |
| Zou et al. | Efficient electromagnetic interference shielding of flexible Ag microfiber sponge/polydimethylsiloxane composite constructed by blow spinning | |
| Wu et al. | Lightweight and flexible PAN@ PPy/MXene films with outstanding electromagnetic interference shielding and joule heating performance | |
| CN114133739B (en) | Silicone rubber wave-absorbing composite material and preparation method thereof | |
| CN114150496A (en) | Flexible nanofiber membrane with electromagnetic shielding and piezoresistive sensing performances and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |