CN109897213B - Preparation method of flexible composite material for electromagnetic shielding - Google Patents
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Abstract
The invention discloses a preparation method of a flexible composite material for electromagnetic shielding, which belongs to the technical field of electromagnetic shielding, wherein the conductivity of a carbon nano tube is improved by gold plating to obtain the gold-plated carbon nano tube, then a CNTs-Au/sodium alginate sponge composite material with uniform thickness is prepared by a freeze drying method, then a PDMS flexible polymer is infiltrated by vacuum to form a multi-scale composite material, finally, graphene-PDMS coatings are coated on the upper surface and the lower surface of the multi-scale composite material, and finally, the flexible composite material for electromagnetic shielding with good flexibility, high conductivity and good electromagnetic shielding performance is prepared; the composite material prepared by the invention has excellent electromagnetic shielding performance, flexibility and ductility, and can be applied to the field of special electromagnetic radiation protection.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding, and particularly relates to a preparation method of a flexible composite material for electromagnetic shielding.
Background
With the rapid development of information technology, electronic products and electronic communication bring convenience to the life of people, but also bring troubles, such as electromagnetic radiation; increasingly serious electromagnetic radiation can generate electromagnetic interference, electromagnetic information leakage, electromagnetic environment pollution and other problems, so that more troubles are brought to people, and electromagnetic shielding is an important method for solving the problems.
At present, most of electromagnetic shielding materials in the market are made of metal materials, but the electromagnetic shielding materials are expensive in price and poor in flexibility, and cannot be applied to high-end electronic industry. With the development of industrialization in China, the development of a flexible composite material for electromagnetic shielding is very important.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a flexible composite material for electromagnetic shielding, which has good flexibility, high conductivity and good electromagnetic shielding performance.
The preparation method of the flexible composite material for electromagnetic shielding provided by the invention comprises the following steps:
(1) performing gold plating treatment on the carbon nano tube to obtain a gold-plated carbon nano tube, namely a CNTs-Au composite material;
(2) adding sodium alginate into the solution of the CNTs-Au composite material, uniformly mixing, defoaming, and freeze-drying to obtain the CNTs-Au/sodium alginate sponge composite material;
(3) performing PDMS vacuum infiltration on the CNTs-Au/sodium alginate sponge composite material obtained in the step (2), and curing to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (4) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with a required thickness, and then coating graphene-PDMS coatings on two sides of the substrate to obtain the flexible composite material for the electromagnetic shielding.
Preferably, in the step (1), the mass ratio of the carbon nanotubes to the gold is (75-50): (25-50).
Preferably, in the step (1), the gold plating treatment comprises the following specific steps:
s1, adding the carbon nano tube subjected to acid treatment into a PEI solution, and performing super-shock treatment;
s2, adding a chloroauric acid solution into the mixed solution obtained in the step S1, and uniformly stirring;
s3, placing the mixed solution obtained in the step S2 in a constant temperature environment of 60 ℃, stirring and reacting for 1h, adding deionized water for dilution after the reaction is finished, and filtering to obtain the gold-plated carbon nano tube.
Preferably, in the step (2), the mass ratio of the CNTs-Au to the sodium alginate sponge is (83.4-38.4): (16.6-61.6).
Preferably, in the step (2), the preparation process of the CNTs-Au/sodium alginate sponge composite material is as follows:
1) adding sodium alginate into a solution of the CNTs-Au composite material, and performing ultra-shock treatment;
2) defoaming the mixed solution obtained in the step 1) by adopting a vacuum stirring defoaming machine;
3) and (3) freeze-drying the defoamed mixed solution obtained in the step 2), wherein the freeze-drying temperature is below-60 ℃ and the time is 24-36 h, and fully dehydrating to obtain the CNTs-Au/sodium alginate sponge composite material.
Further, the mass concentration of the solution of the CNTs-Au composite material is 0.5-4 wt%.
Preferably, in step (3), the CNTs-Au/sodium alginate sponge composite is added to the excess PDMS, ensuring sufficient penetration of the PDMS into the pores of the sodium alginate sponge.
Preferably, in the step (3), the method specifically comprises the following steps: and in the vacuum infiltration process, controlling the vacuum degree to be lower than 5Pa, and the infiltration time to be 24h until the polymer PDMS infiltrates into the sponge body and all bubbles are eliminated, and then carrying out curing treatment, wherein the curing temperature is 120 ℃ and the curing time is 4 h.
Preferably, in the step (4), the graphene-PDMS coating is coated on both sides of the substrate by a spin coating method.
Preferably, in the step (4), the thickness of the graphene-PDMS coating is 20-200 μm.
Preferably, in the step (4), in the flexible composite material for electromagnetic shielding, the mass percentage of graphene is 1-5%.
The invention provides a preparation method of a flexible composite material for electromagnetic shielding, which comprises the steps of improving the conductivity of a carbon nano tube by gold plating to obtain a gold-plated carbon nano tube, preparing a CNTs-Au/sodium alginate sponge composite material with uniform thickness by a freeze drying method, infiltrating a PDMS flexible polymer into a PDMS to form a multi-scale composite material by vacuum, and finally coating graphene-PDMS coatings on the upper surface and the lower surface of the multi-scale composite material to finally prepare the flexible composite material for electromagnetic shielding with good flexibility, high conductivity and good electromagnetic shielding performance.
The invention realizes a preparation method of a CNTs-Au/sponge/PDMS/graphene multilayer flexible composite material, wherein the carbon nano tube forms a conductive network, so that the electromagnetic shielding performance is greatly improved, and good flexibility and ductility are obtained by compounding with PDMS; the graphene-PDMS coating is prepared by a spin coating method, so that the electromagnetic shielding performance is further improved; the composite material prepared by the invention has excellent electromagnetic shielding performance, flexibility and ductility, and can be widely applied to the field of special electromagnetic radiation protection.
The carbon nano tube adopted by the invention is a carbon homoisomer, has light weight, perfect connection of a six-ring structure, excellent mechanical property and electrochemical property; PDMS is a super-elastic plastic, has a large thermal expansion coefficient and excellent bearing capacity; the flexible composite material for electromagnetic shielding prepared by the specific process parameters of the invention has uniform components and high interfacial binding force among all layers of the composite film; the preparation method has the advantages of simple preparation process, low cost and low equipment requirement, and can be suitable for large-scale production.
The multi-layer film structure prepared by the preparation method of the flexible composite material for electromagnetic shielding can effectively cause multiple reflection, absorption and attenuation to electromagnetic waves, greatly optimizes the electromagnetic shielding performance of products by improving the conductive performance of the products, has good flexibility of the prepared finished products, can bear deformation in a larger range, has good anti-fatigue capability, and has wide application fields.
Drawings
FIG. 1 is an SEM photograph of acid-treated carbon nanotubes of example 1.
Fig. 2 is an SEM image of gold-plated carbon nanotubes of example 1.
FIG. 3 is an SEM picture of the cross section of the CNTs-Au/sodium alginate sponge composite material in example 1.
FIG. 4 is an SEM image of the cross section of the CNTs-Au/sodium alginate sponge/PDMS composite material in example 1.
FIG. 5 is a macroscopic view of the CNTs-Au/sodium alginate sponge/PDMS composite material in example 1.
FIG. 6 is a macroscopic view of the CNTs-Au/sponge/PDMS/graphene multi-layer flexible composite prepared in example 2.
FIG. 7 is an SEM image of the cross section of the CNTs/sodium alginate sponge composite material in comparative example 1.
FIG. 8 is an SEM image of the cross section of the CNTs/sodium alginate sponge/PDMS composite material in comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention. The experimental procedures described in the following examples are conventional unless otherwise specified, and the reagents and materials described therein are commercially available without further specification.
Example 1
Preparing raw materials:
chloroauric acid solution: preparing 100ml of chloroauric acid solution by 1g of chloroauric acid, and refrigerating the prepared chloroauric acid solution in dark.
PEI solution: 60ml PEI +40ml deionized water, the solution is heated in the process of ultra-vibration until the solution is clear, and the solution can be used after standing and cooling to the room temperature.
Carbon nanotube acid treatment: adding the carbon nano tube into mixed acid of concentrated nitric acid and concentrated sulfuric acid (1: 3v/v), carrying out reflux treatment at 120 ℃ for 3h, and washing, carrying out suction filtration and drying to obtain the carbon nano tube subjected to acid treatment.
The preparation method of the flexible composite material for electromagnetic shielding comprises the following steps:
(1) performing gold plating treatment on the carbon nano tube:
1.1) adding 0.1g of acid-treated carbon nano tube into 48ml of PEI solution, uniformly stirring, and carrying out 40KHz super-vibration for 5min and 60KHz super-vibration for 5 min;
1.2) adding 36ml of chloroauric acid solution into the mixed solution obtained in the step 1.1), and uniformly stirring;
1.3) placing the mixed solution obtained in the step 1.2) in a constant-temperature water bath kettle at 60 ℃, adjusting the stirring speed until the liquid level begins to generate vortex, reacting for 1h, adding 600ml of deionized water for dilution after the reaction is finished, and filtering to obtain gold-plated carbon nano tubes;
(2) preparing a CNTs-Au/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs-Au solution (with the mass concentration of 0.5 percent), and performing ultra-shaking for 10min at 40KHz to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the product;
(3) adding the CNTs-Au/sodium alginate sponge composite material into excessive PDMS, controlling the vacuum degree to be lower than 5Pa, controlling the infiltration time to be 24h until a sponge body is immersed into the polymer material and bubbles are completely eliminated, then carrying out curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and carrying out furnace cooling to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (3) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the thickness of the coatings is 20-200 mu m, and the spin coating process is 5000 r/40 s, so as to obtain the flexible composite material, wherein the content of graphene is controlled to be 1%.
Fig. 1 is an SEM image of the carbon nanotubes after the acid treatment in example 1, and fig. 2 is an SEM image of the gold-plated carbon nanotubes in example 1, which can be obtained by comparing fig. 1-2, and the Au-plated samples prepared by this method can achieve a plating rate of 60% or more and uniform plating.
FIG. 3 is an SEM image of the cross section of the composite material of CNTs-Au/sodium alginate sponge in example 1, FIG. 4 is an SEM image of the cross section of the composite material of CNTs-Au/sodium alginate sponge/PDMS in example 1, and it can be seen from FIGS. 3-4 that carbon nanotubes are embedded in PDMS to form a carbon nanotube network.
FIG. 5 is a macroscopic view of the composite material of CNTs-Au/sodium alginate sponge/PDMS in example 1, and it can be seen from FIG. 5 that PDMS is substantially fully filled in the sponge, and the surface of the sample has no bubbles and the morphology is good.
Example 2
The preparation method of the flexible composite material for electromagnetic shielding comprises the following steps:
(1) performing gold plating treatment on the carbon nano tube:
1.1) adding 0.1g of acid-treated carbon nano tube into 48ml of PEI solution, uniformly stirring, and carrying out 40KHz super-vibration for 5min and 60KHz super-vibration for 5 min;
1.2) adding 36ml of chloroauric acid solution into the mixed solution obtained in the step 1.1), and uniformly stirring;
1.3) placing the mixed solution obtained in the step 1.2) in a constant-temperature water bath kettle at 60 ℃, adjusting the stirring speed until the liquid level begins to generate vortex, reacting for 1h, adding 600ml of deionized water for dilution after the reaction is finished, and filtering to obtain gold-plated carbon nano tubes;
(2) preparing a CNTs-Au/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs-Au solution (the mass concentration is 1 percent), and performing ultra-vibration at 40KHz for 10min to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the product;
(3) adding the CNTs-Au/sodium alginate sponge composite material into excessive PDMS, controlling the vacuum degree to be lower than 5Pa, controlling the infiltration time to be 24h until a sponge body is immersed into the polymer material and bubbles are completely eliminated, then carrying out curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and carrying out furnace cooling to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (3) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the thickness of the coatings is 20-200 mu m, and the spin coating process is 5000 r/40 s, so as to obtain the CNTs-Au/sponge/PDMS/graphene multilayer flexible composite material, namely the flexible composite material, wherein the content of graphene is controlled to be 1%.
FIG. 6 is a macroscopic view of the CNTs-Au/sponge/PDMS/graphene multi-layer flexible composite material prepared in example 2, wherein the surface of the sample is flat and the size of the sample is controllable.
Example 3
The preparation method of the flexible composite material for electromagnetic shielding comprises the following steps:
(1) performing gold plating treatment on the carbon nano tube:
1.1) adding 0.1g of acid-treated carbon nano tube into 48ml of PEI solution, uniformly stirring, and carrying out 40KHz super-vibration for 5min and 60KHz super-vibration for 5 min;
1.2) adding 36ml of chloroauric acid solution into the mixed solution obtained in the step 1.1), and uniformly stirring;
1.3) placing the mixed solution obtained in the step 1.2) in a constant-temperature water bath kettle at 60 ℃, adjusting the stirring speed until the liquid level begins to generate vortex, reacting for 1h, adding 600ml of deionized water for dilution after the reaction is finished, and filtering to obtain gold-plated carbon nano tubes;
(2) preparing a CNTs-Au/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs-Au solution (with the mass concentration of 2 percent), and performing ultra-vibration at 40KHz for 10min to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 36 hours, and fully dehydrating to obtain the product;
(3) adding the CNTs-Au/sodium alginate sponge composite material into excessive PDMS, controlling the vacuum degree to be lower than 5Pa, controlling the infiltration time to be 24h until a sponge body is immersed into the polymer material and bubbles are completely eliminated, then carrying out curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and carrying out furnace cooling to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (3) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the thickness of the coatings is 20-200 mu m, and the spin coating process is 5000 r/40 s, so as to obtain the flexible composite material, wherein the content of graphene is controlled to be 3%.
Example 4
The preparation method of the flexible composite material for electromagnetic shielding comprises the following steps:
(1) performing gold plating treatment on the carbon nano tube:
1.1) adding 0.1g of acid-treated carbon nano tube into 48ml of PEI solution, uniformly stirring, and carrying out 40KHz super-vibration for 5min and 60KHz super-vibration for 5 min;
1.2) adding 36ml of chloroauric acid solution into the mixed solution obtained in the step 1.1), and uniformly stirring;
1.3) placing the mixed solution obtained in the step 1.2) in a constant-temperature water bath kettle at 60 ℃, adjusting the stirring speed until the liquid level begins to generate vortex, reacting for 1h, adding 600ml of deionized water for dilution after the reaction is finished, and filtering to obtain gold-plated carbon nano tubes;
(2) preparing a CNTs-Au/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs-Au solution (with the mass concentration of 4 percent), and performing ultra-vibration at 40KHz for 10min to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the product;
(3) adding the CNTs-Au/sodium alginate sponge composite material into excessive PDMS, controlling the vacuum degree to be lower than 5Pa, controlling the infiltration time to be 24h until a sponge body is immersed into the polymer material and bubbles are completely eliminated, then carrying out curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and carrying out furnace cooling to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (3) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the thickness of the coatings is 20-200 mu m, and the spin coating process is 5000 r/40 s, so as to obtain the flexible composite material, wherein the content of graphene is controlled to be 5%.
Comparative example 1
(1) Carrying out carbon nanotube acid treatment;
(2) preparing a CNTs/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs solution (with the mass concentration of 0.5 percent), and performing ultra-vibration at 40KHz for 10min to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the CNTs/sodium alginate sponge composite material, wherein a cross-section SEM picture is shown in FIG. 7;
(3) performing PDMS vacuum infiltration on the CNTs/sodium alginate sponge composite material, controlling the vacuum degree to be lower than 5Pa, and the infiltration time to be 24h until a sponge body sinks into the polymer material and bubbles are completely eliminated, then performing curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and performing furnace cooling to obtain the CNTs/sodium alginate sponge/PDMS composite material, wherein FIG. 8 is an SEM image of the cross section of the composite material;
(4) and (3) cutting the CNTs/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the spin coating process is 5000 r/40 s, so as to obtain a flexible composite material, and controlling the content of graphene to be 1%.
Comparative example 2
(1) Preparing a sodium alginate sponge material:
s1, adding 0.04g of sodium alginate into 4ml of deionized water, and performing 40KHz ultra-vibration for 10min to fully dissolve the sodium alginate;
s2, defoaming the mixed solution obtained in the step S1 by adopting a vacuum stirring defoaming machine;
s3, freeze-drying the defoamed mixed solution obtained in the step S2 at the temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the defoaming agent;
(2) performing PDMS vacuum infiltration on the sodium alginate sponge material, controlling the vacuum degree to be lower than 5Pa, and the infiltration time to be 24h until a sponge body sinks into the polymer material and bubbles are completely eliminated, then performing curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, and performing furnace cooling to obtain the sodium alginate sponge/PDMS composite material;
(3) and (3) cutting the sodium alginate sponge/PDMS composite material obtained in the step (2) into a sheet-shaped substrate with the thickness of 0.5mm, coating graphene-PDMS coatings on two sides of the substrate by a spin coating method, wherein the spin coating process is 5000 r/40 s, so as to obtain the flexible composite material, and controlling the content of graphene to be 1%.
Comparative example 3
(1) Performing gold plating treatment on the carbon nano tube:
1.1) adding 0.1g of acid-treated carbon nano tube into 48ml of PEI solution, uniformly stirring, and carrying out 40KHz super-vibration for 5min and 60KHz super-vibration for 5 min;
1.2) adding 36ml of chloroauric acid solution into the mixed solution obtained in the step 1.1), and uniformly stirring;
1.3) placing the mixed solution obtained in the step 1.2) in a constant-temperature water bath kettle at 60 ℃, adjusting the stirring speed until the liquid level begins to generate vortex, reacting for 1h, adding 600ml of deionized water for dilution after the reaction is finished, and filtering to obtain gold-plated carbon nano tubes;
(2) preparing a CNTs-Au/sodium alginate sponge composite material:
2.1) adding 0.04g of sodium alginate into 4ml of CNTs-Au solution (with the mass concentration of 0.5 percent), and performing ultra-shaking for 10min at 40KHz to fully dissolve the sodium alginate;
2.2) adopting a vacuum stirring defoaming machine to perform defoaming treatment on the mixed solution obtained in the step 2.1);
2.3) freeze-drying the mixed solution obtained in the step 2.2) after defoaming at the freeze-drying temperature of below-60 ℃ for 24 hours, and fully dehydrating to obtain the product;
(3) and (2) performing PDMS vacuum infiltration on the CNTs-Au/sodium alginate sponge composite material, controlling the vacuum degree to be lower than 5Pa, and the infiltration time to be 24h until the sponge body sinks into the polymer material and bubbles are completely eliminated, then performing curing treatment, wherein the curing temperature is 120 ℃, the curing time is 4h, performing furnace cooling, and cutting into a sheet-shaped substrate with the thickness of 0.5mm to obtain the flexible composite material.
The flexible composite materials prepared in the examples 1 to 4 and the comparative examples 1 to 3 are subjected to performance tests, and specific performances are shown in the following table:
table 1 shows the composition of the flexible composite material in each embodiment
Table 2 is a table of properties of the flexible composite material obtained in each embodiment
As can be seen from tables 1-2, the CNTs conductive network inside the polymer matrix is the main source of the electromagnetic shielding performance of the composite material, but also reduces the fracture elongation of the composite material; secondly, the CNTs are plated with gold, so that the electromagnetic shielding performance of the material can be greatly improved; the graphene coating can further improve the electromagnetic shielding performance of the composite material, and the flexibility of the material is not influenced; the high-content gold-plated CNTs and the graphene coating can effectively improve the electromagnetic shielding performance of the composite material, and finally the composite material still keeps good flexibility, so that the application range is wide.
Claims (10)
1. The preparation method of the flexible composite material for electromagnetic shielding is characterized by comprising the following steps:
(1) performing gold plating treatment on the carbon nano tube to obtain a gold-plated carbon nano tube, namely a CNTs-Au composite material;
(2) adding sodium alginate into the solution of the CNTs-Au composite material, uniformly mixing, defoaming, and freeze-drying to obtain the CNTs-Au/sodium alginate sponge composite material;
(3) performing PDMS vacuum infiltration on the CNTs-Au/sodium alginate sponge composite material obtained in the step (2), and curing to obtain the CNTs-Au/sodium alginate sponge/PDMS composite material;
(4) and (4) cutting the CNTs-Au/sodium alginate sponge/PDMS composite material obtained in the step (3) into a sheet-shaped substrate with a required thickness, and then coating graphene-PDMS coatings on two sides of the substrate to obtain the flexible composite material for the electromagnetic shielding.
2. The method for preparing the flexible composite material for electromagnetic shielding according to claim 1, wherein in the step (1), the mass ratio of the carbon nanotubes to the gold is (75-50): (25-50).
3. The method for preparing a flexible composite material for electromagnetic shielding according to claim 1 or 2, wherein in the step (1), the gold plating process comprises:
s1, adding the carbon nano tube subjected to acid treatment into a PEI solution, and performing super-shock treatment;
s2, adding a chloroauric acid solution into the mixed solution obtained in the step S1, and uniformly stirring;
s3, placing the mixed solution obtained in the step S2 in a constant temperature environment of 60 ℃, stirring and reacting for 1h, adding deionized water for dilution after the reaction is finished, and filtering to obtain the gold-plated carbon nano tube.
4. The preparation method of the flexible composite material for electromagnetic shielding according to claim 1, wherein in the step (2), the mass ratio of CNTs-Au to sodium alginate sponge (83.4-38.4): (16.6-61.6).
5. The method for preparing the flexible composite material for electromagnetic shielding according to claim 1 or 4, wherein in the step (2), the preparation process of the CNTs-Au/sodium alginate sponge composite material is as follows:
1) adding sodium alginate into a solution of the CNTs-Au composite material, and performing ultra-shock treatment;
2) defoaming the mixed solution obtained in the step 1) by adopting a vacuum stirring defoaming machine;
3) and (3) freeze-drying the defoamed mixed solution obtained in the step 2), wherein the freezing temperature is below-60 ℃, the freeze-drying time is 24-36 hours, and fully dehydrating to obtain the CNTs-Au/sodium alginate sponge composite material.
6. The preparation method of the flexible composite material for electromagnetic shielding according to claim 5, wherein the mass concentration of the solution of the CNTs-Au composite material is 0.5-4 wt%.
7. The method for preparing a flexible composite material for electromagnetic shielding according to claim 1, wherein in the step (3), the CNTs-Au/sodium alginate sponge composite material is added to the excess PDMS to ensure sufficient PDMS to permeate into the pores of the sodium alginate sponge.
8. The method for preparing the flexible composite material for electromagnetic shielding according to claim 1 or 7, wherein in the step (3), the method specifically comprises: and in the vacuum infiltration process, controlling the vacuum degree to be lower than 5Pa, and the infiltration time to be 24h until the polymer PDMS infiltrates into the sponge body and all bubbles are eliminated, and then carrying out curing treatment, wherein the curing temperature is 120 ℃ and the curing time is 4 h.
9. The method for preparing the flexible composite material for electromagnetic shielding according to claim 1, wherein in the step (4), the thickness of the graphene-PDMS coating is 20 to 200 μm.
10. The method for preparing the flexible composite material for electromagnetic shielding according to claim 1, wherein in the step (4), the graphene accounts for 1-5% by mass of the flexible composite material for electromagnetic shielding.
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| CN107041113B (en) * | 2017-05-04 | 2019-02-12 | 哈尔滨工业大学 | A method of it carries out compound preparing highly conductive high electromagnetic shielding flexible composite using graphene sponge and dimethyl silicone polymer |
| CN108003364B (en) * | 2017-11-24 | 2020-10-16 | 中南大学 | Flexible graphene-based composite membrane, preparation method thereof and application of flexible graphene-based composite membrane as electromagnetic shielding material |
| CN109320747B (en) * | 2018-09-25 | 2021-06-01 | 中南大学 | High-sensitivity flexible composite coating and preparation method thereof |
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