CN110572997B - Preparation method of novel foam carbon electromagnetic shielding composite material - Google Patents
Preparation method of novel foam carbon electromagnetic shielding composite material Download PDFInfo
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Abstract
The invention discloses a novel foamThe preparation method of the carbon electromagnetic shielding composite material comprises the steps of pretreating melamine foam, carbonizing the melamine foam to prepare the foam carbon and preparing Fe3O4Reaction solution of nanoparticles, preparation of Fe3O4The mixed solution of the nano particles and the foam carbon is dried to obtain the prepared Fe3O4Nanoparticle/carbon foam composites. The invention relates to a preparation method of a novel foam carbon electromagnetic shielding composite material, which is prepared by mixing Fe3O4The nano particles are compounded with the soft foam carbon to obtain the flexible light electromagnetic shielding composite material with excellent electromagnetic shielding performance, so that Fe can be used3O4The nano particles are uniformly dispersed.
Description
Technical Field
The invention belongs to a preparation method of a foam carbon electromagnetic shielding composite material, and relates to a preparation method of a novel foam carbon electromagnetic shielding composite material.
Background
The progress in electronic technology and the rapid development of the information industry inevitably bring about the problem of electromagnetic wave radiation. Electromagnetic interference and radio frequency interference caused by electromagnetic wave radiation not only can cause the problems of electronic equipment failure, communication interruption, electromagnetic information leakage and the like, but also seriously endanger the living environment and health of human life. Therefore, the development of new and efficient electromagnetic shielding materials has gradually attracted much attention. At present, the major share of electromagnetic shielding materials in the market is mainly metals and their alloys, which have excellent electromagnetic shielding performance, but they are still limited by many defects in the using process, such as high density, poor corrosion resistance, high cost, etc. Therefore, the development of novel electromagnetic shielding materials with light weight, high efficiency, flexibility, corrosion resistance and low cost has become an important development direction in the field of electromagnetic shielding materials, and has very important practical significance and application value.
As a novel carbon material with a three-dimensional porous structure, the foam carbon has the advantages of low density, high strength, good conductivity, corrosion resistance, easy processing and forming and the like, and is considered to be one of ideal candidate materials of the next-generation electromagnetic shielding material. The electromagnetic shielding performance of the foam carbon is general, and has a certain gap from the performance requirement of the electromagnetic shielding material. The method for preparing the foam carbon composite material by compounding the proper second-phase material with the foam carbon is a main means for improving the electromagnetic shielding performance of the foam carbon and is one of the most effective methods for promoting the practical application of the foam carbon composite material. The transition metal oxide has wide application prospect in the field of electromagnetic shielding due to the characteristics of high magnetic conductivity, low cost, good biocompatibility, high saturation magnetization and the like, and is one of the materials commonly used for preparing the electromagnetic shielding composite material.
However, when the transition metal oxide nanoparticles are used as a filling material to prepare a composite material, the nanoparticles are easy to agglomerate in a matrix (especially a polymer), mainly because the nanoparticles have large specific surface area and large surface energy, are in a thermodynamically unstable state, and can be aggregated together under the action of intermolecular force such as van der waals force, and the like to generate agglomeration. The agglomeration phenomenon can reduce the interface bonding between the nanoparticles and the matrix material, and greatly weaken the reinforcing effect of the nanoparticles on the matrix. At present, common methods for solving the agglomeration problem of nano-particles or carbon nano-tubes in a foam carbon matrix mainly comprise an ultrasonic dispersion method, a ball milling method, a calendaring method, a stirring extrusion method, surfactant addition and the like, but the dispersion effects of the methods are general and the uniform dispersion of the nano-particles cannot be ensured.
Disclosure of Invention
The invention aims to provide a preparation method of a novel foam carbon electromagnetic shielding composite material, which is prepared by mixing Fe3O4The nano particles are compounded with the soft foam carbon to obtain the flexible light electromagnetic shielding composite material with excellent electromagnetic shielding performance and Fe3O4The nano particles are uniformly dispersed.
The technical scheme adopted by the invention is that the preparation method of the novel foam carbon electromagnetic shielding composite material is implemented according to the following steps:
step 1, pretreating melamine foam;
step 2, carbonizing the pretreated melamine foam obtained in the step 1, and then cooling to room temperature to obtain foam carbon;
step 3, preparing Fe3O4A reaction solution of nanoparticles;
step 4, measuring a certain amount of Fe prepared in step 33O4Measuring a certain amount of the carbon foam prepared in the step 2, and placing the measured carbon foam in Fe3O4Carrying out ultrasonic treatment on the solution in the reaction solution of the nano particles for 1-2 h, and adjusting the pH value of the solution to 9.5-10.5 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
step 5, drying the reaction mixed liquid prepared in the step 4 after ultrasonic cleaning to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
The present invention is also characterized in that,
the step 1 specifically comprises the following steps: the melamine foam is respectively subjected to ultrasonic cleaning by deionized water and absolute ethyl alcohol for 10-30 min, and then is dried in an oven at the temperature of 70-90 ℃ for 12-24 h.
The step 2 specifically comprises the following steps: placing the pretreated melamine foam obtained in step 1 in a tube furnace in N2Carrying out multi-section carbonization treatment under the protection of atmosphere, wherein in the first stage: heating the mixture from room temperature to 200 ℃, and preserving heat for 1-2 h; and a second stage: heating to 400 ℃, and preserving heat for 1-2 h; and a third stage: and (3) heating to the carbonization temperature, preserving the heat for 1-2 hours, then controlling the cooling rate, and cooling the sample to the room temperature to obtain the carbon foam.
And in the step 2, the heating rate and the cooling rate in the multi-stage carbonization treatment process of the melamine foam are both 3-5 ℃/min.
The carbonization temperature is 800-1000 ℃.
The step 3 specifically comprises the following steps: respectively dissolving certain mass of FeCl in deionized water3·6H2O and FeSO4·7H2O, adding a surface active agent PVP, and then magnetically stirring for 1-2 h to obtain uniform Fe3O4Reaction solution of nanoparticles.
FeCl3·6H2The concentration of O is 0.72mol/L, FeSO4·7H2The concentration of O was 0.39mol/L, the mass m of the surfactant PVP was adjusted to1Let FeCl3·6H2O、FeSO4·7H2Sum of mass of O m2，m1：m2＝1：10～1：12。
Measuring Fe in step 43O4The volume ratio of the reaction solution of the nano particles to the measured foam carbon is 5: 3-5: 1.
The step 5 specifically comprises the following steps: and (4) ultrasonically cleaning the reaction mixed liquid prepared in the step (4) in deionized water for 5-10 min, and then drying the reaction mixed liquid in a vacuum drying oven at the temperature of 90 ℃ for 12-24 h.
The invention has the beneficial effects that the invention selects Fe3O4The nano particles are used as a second phase material, the foam carbon is used as a matrix, the electromagnetic shielding performance of the foam carbon is enhanced through the synergistic optimization effect of dielectric loss and magnetic loss between the matrix and an addition phase, and the characteristics of flexibility and light weight of the foam carbon are added, so that the flexible light electromagnetic shielding composite material with excellent electromagnetic shielding performance is obtained; the preparation method of the invention makes Fe3O4The nano particles grow in situ on the surface of the foam carbon, so the method has excellent dispersibility, and simultaneously, the method has simple preparation process, low cost and no pollution.
Drawings
FIG. 1 shows Fe prepared in example 1 of the present invention3O4XRD (X-ray diffraction) pattern of nanoparticle/carbon foam composite;
FIG. 2 is a photograph and SEM (scanning electron microscope) picture of the carbon foam prepared in example 1 of the present invention;
FIG. 3 is Fe prepared in example 1 of the present invention3O4A micro-topography of the nanoparticle/carbon foam composite;
FIG. 4 Fe prepared in example 1 of the present invention3O4Electromagnetic shielding performance curve diagram of the nanometer particle/foam carbon composite material.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a novel foam carbon electromagnetic shielding composite material, which is implemented according to the following steps:
step 1, pretreating melamine foam; the method specifically comprises the following steps: respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 10-30 min, and then drying in an oven at the temperature of 70-90 ℃ for 12-24 h;
step 2, carbonizing the pretreated melamine foam obtained in the step 1, and then cooling to room temperature to obtain foam carbon; the method specifically comprises the following steps: placing the pretreated melamine foam obtained in step 1 in a tube furnace in N2Carrying out multi-section carbonization treatment under the protection of atmosphere, wherein in the first stage: heating the mixture from room temperature to 200 ℃, and preserving heat for 1-2 h; and a second stage: heating to 400 ℃, and preserving heat for 1-2 h; and a third stage: heating to a carbonization temperature, preserving heat for 1-2 hours, then controlling the cooling rate, and cooling the sample to room temperature to obtain foam carbon; wherein the heating rate and the cooling rate in the multi-stage carbonization treatment process of the melamine foam are both 3-5 ℃/min; the carbonization temperature is 800-1000 ℃;
step 3, preparing Fe3O4A reaction solution of nanoparticles; the method specifically comprises the following steps: respectively dissolving certain mass of FeCl in deionized water3·6H2O and FeSO4·7H2O, adding a surface active agent PVP, and then magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles; FeCl3·6H2The concentration of O is 0.72mol/L, FeSO4·7H2The concentration of O was 0.39mol/L, the mass m of the surfactant PVP was adjusted to1Let FeCl3·6H2O、FeSO4·7H2Sum of mass of O m2，m1：m2＝1：10～1：12。
Step 4, mixing the raw materials in a volume ratio of 5: 3-5: 1 measuring a certain amount of Fe prepared in the step 33O4Placing the measured foam carbon into Fe in the reaction solution of the nano particles and the foam carbon prepared in the step 23O4Carrying out ultrasonic treatment on the solution in the reaction solution of the nano particles for 1-2 h, and adjusting the pH value of the solution to 9.5-10.5 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
and 5, ultrasonically cleaning the reaction mixed liquid prepared in the step 4 in deionized water for 5-10 min, and then drying the reaction mixed liquid in a vacuum drying oven at the temperature of 90 ℃ for 12-24 h.
Example 1
Step 1, pretreating melamine foam:
respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 30min, and then drying the melamine foam in an oven at the temperature of 90 ℃ for 12 h;
step 2, placing the pretreated melamine foam obtained in the step 1 into a tube furnace, and performing reaction in N2Carrying out multi-stage carbonization treatment under the protection of atmosphere, heating to 200 ℃ from room temperature in the first stage, and keeping the temperature for 1-2 h; in the second stage, heating to 400 ℃, and keeping the temperature for 1-2 hours; finally, heating to 800 ℃, preserving the heat for 1-2 h, finally controlling the cooling rate, cooling the sample to room temperature, wherein the heating rate and the cooling rate are both 5 ℃/min, and preparing the foam carbon;
step 3, preparing Fe3O4Reaction solution of nanoparticles: 2.3g of FeCl was dissolved in 20ml of deionized water3·6H2O and 1.2g of FeSO4·7H2O, adding 0.3g of PVP (polyvinylpyrrolidone) as a surfactant, and magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles;
step 4, taking the foam carbon of 12cm obtained in the step 23Is placed in the step 3 to prepare Fe3O4Carrying out ultrasonic treatment on the solution in the reaction solution of the nano particles for 1-2 h, and adjusting the pH value of the solution to 9.5 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution; and 5, ultrasonically cleaning the reaction mixed solution prepared in the step 4 in deionized water for 5-10 min, and finally drying the sample in a vacuum drying oven at the temperature of 90 ℃ for 12-24h to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
Example 2
Step 1, pretreating melamine foam:
respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 30min, and then drying the melamine foam in an oven at the temperature of 90 ℃ for 12 h;
step 2, placing the pretreated melamine foam obtained in the step 1 into a tube furnace, and performing reaction in N2Carrying out multi-stage carbonization treatment under the protection of atmosphere, heating to 200 ℃ from room temperature in the first stage, and keeping the temperature for 1-2 h; in the second stage, heating to 400 ℃, and keeping the temperature for 1-2 hours; and finally, heating to 850 ℃, and preserving the heat for 1-2 hours. Finally, controlling the cooling rate, cooling the sample to room temperature, wherein the heating rate and the cooling rate are both 3 ℃/min, and preparing the foam carbon;
step 3, preparing Fe3O4Reaction solution of nanoparticles: 4.6g of FeCl was dissolved in 40ml of deionized water3·6H2O and 2.4g of FeSO4·7H2O, adding 0.73g of PVP (polyvinylpyrrolidone) as a surfactant, and magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles;
step 4, taking the foam carbon obtained in the step 2, wherein the volume of the foam carbon is 24cm3Is placed in the step 3 to prepare Fe3O4In the reaction solution of the nano particles, carrying out ultrasonic treatment on the solution for 1-2 h, and adjusting the pH value of the solution to 10 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
and 5, ultrasonically cleaning the reaction mixed solution prepared in the step 4 in deionized water for 5-10 min, and finally drying the sample in a vacuum drying oven at the temperature of 90 ℃ for 12-24h to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
Example 3
Step 1, pretreating melamine foam:
respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 30min, and then drying the melamine foam in an oven at the temperature of 90 ℃ for 12 h;
step 2, placing the pretreated melamine foam obtained in the step 1 into a tube furnace, and performing reaction in N2Multi-section carbon under the protection of atmosphereCarrying out chemical treatment, namely heating the mixture from room temperature to 200 ℃ in the first stage, and keeping the temperature for 1-2 h; in the second stage, heating to 400 ℃, and keeping the temperature for 1-2 hours; finally, heating to 900 ℃, preserving heat for 1-2 h, finally controlling the cooling rate, cooling the sample to room temperature, wherein the heating rate and the cooling rate are both 4 ℃/min, and preparing the foam carbon;
step 3, preparing Fe3O4Reaction solution of nanoparticles: 6.9g of FeCl was dissolved in 60ml of deionized water3·6H2O and 3.6g of FeSO4·7H2O, adding 1.05g of PVP (polyvinylpyrrolidone) as a surfactant, and magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles;
step 4, the volume of the carbon foam obtained in the step 2 is 36cm3Is placed in the step 3 to prepare Fe3O4In the reaction solution of the nano particles, carrying out ultrasonic treatment on the solution for 1-2 h, and adjusting the pH value of the solution to 10 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
and 5, ultrasonically cleaning the reaction mixed solution prepared in the step 4 in deionized water for 5-10 min, and finally drying the sample in a vacuum drying oven at the temperature of 90 ℃ for 12-24h to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
Example 4
Step 1, pretreating melamine foam:
respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 30min, and then drying the melamine foam in an oven at the temperature of 90 ℃ for 12 h;
step 2, placing the pretreated melamine foam obtained in the step 1 into a tube furnace, and performing reaction in N2Carrying out multi-stage carbonization treatment under the protection of atmosphere, heating to 200 ℃ from room temperature in the first stage, and keeping the temperature for 1-2 h; in the second stage, heating to 400 ℃, and keeping the temperature for 1-2 hours; and finally, heating to 1000 ℃, and preserving the heat for 1-2 hours. Finally, controlling the cooling rate, cooling the sample to room temperature, wherein the heating rate and the cooling rate are both 5 ℃/min, and preparing the foam carbon;
step 3, preparingPut Fe3O4Reaction solution of nanoparticles: 9.2g of FeCl were dissolved in 80ml of deionized water3·6H2O and 4.8g of FeSO4·7H2O, adding 1.4g of PVP (polyvinylpyrrolidone) as a surfactant, and magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles;
step 4, the volume of the carbon foam obtained in the step 2 is 48cm3Is placed in the step 3 to prepare Fe3O4Carrying out ultrasonic treatment on the solution in the reaction solution of the nano particles for 1-2 h, and adjusting the pH value of the solution to 10.5 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
and 5, ultrasonically cleaning the reaction mixed solution prepared in the step 4 in deionized water for 5-10 min, and finally drying the sample in a vacuum drying oven at the temperature of 90 ℃ for 12-24h to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
FIG. 1 shows Fe prepared in example 1 of the present invention3O4XRD (X-ray diffraction) spectrum of nano-particle/foam carbon composite material, and Fe contained in the composite material prepared by the pattern3O4。
FIG. 2 is a photograph and an SEM (scanning electron microscope) picture of the carbon foam prepared in example 1 of the present invention, and it can be seen from FIG. 2(a) that the carbon foam prepared by the present method has good flexibility, complete cell structure, clear ligament structure connecting cells and pores, and high cell density; the sample prepared from the surface of fig. 2(b) is flexible and can be bent largely without breaking.
FIG. 3 shows Fe prepared in example 1 of the present invention3O4The microscopic morphology of the nano-particle/foam carbon composite material can be observed, and Fe can be observed3O4The nanoparticles were successfully grown on the carbon foam ligament surface (fig. 3(b)) and dispersed uniformly.
FIG. 4 shows Fe prepared in example 1 of the present invention3O4The electromagnetic shielding performance of the nano particle/foam carbon composite material is that the total shielding effectiveness is highest within a wave band of 8-12.4 GHzCan reach 19dB, and the composite material prepared by the invention has good electromagnetic shielding performance.
Claims (2)
1. A preparation method of a novel foam carbon electromagnetic shielding composite material is characterized by comprising the following steps:
step 1, pretreating melamine foam;
respectively carrying out ultrasonic cleaning on melamine foam by using deionized water and absolute ethyl alcohol for 10-30 min, and then drying in an oven at the temperature of 70-90 ℃ for 12-24 h;
step 2, carbonizing the pretreated melamine foam obtained in the step 1, and then cooling to room temperature to obtain foam carbon;
placing the pretreated melamine foam obtained in step 1 in a tube furnace in N2Carrying out multi-section carbonization treatment under the protection of atmosphere, wherein in the first stage: heating the mixture from room temperature to 200 ℃, and preserving heat for 1-2 h; and a second stage: heating to 400 ℃, and preserving heat for 1-2 h; and a third stage: heating to a carbonization temperature, preserving heat for 1-2 hours, then controlling the cooling rate, and cooling the sample to room temperature to obtain foam carbon;
the temperature rise rate and the temperature drop rate in the multi-stage carbonization treatment process of the melamine foam are both 3-5 ℃/min, and the carbonization temperature is 800-1000 ℃;
step 3, preparing Fe3O4A reaction solution of nanoparticles;
respectively dissolving certain mass of FeCl in deionized water3·6H2O and FeSO4·7H2O, adding a surface active agent PVP, and then magnetically stirring for 1-2 h to obtain uniform Fe3O4A reaction solution of nanoparticles;
FeCl3·6H2the concentration of O is 0.72mol/L, FeSO4·7H2The concentration of O was 0.39mol/L, the mass m of the surfactant PVP was adjusted to1Let FeCl3·6H2O、FeSO4·7H2Sum of mass of O m2，m1：m2＝1：10～1：12；
Step 4, measuring a certain amount of Fe prepared in step 33O4Measuring a certain amount of the carbon foam prepared in the step 2, and placing the measured carbon foam in Fe3O4Carrying out ultrasonic treatment on the solution in the reaction solution of the nano particles for 1-2 h, and adjusting the pH value of the solution to 9.5-10.5 by using concentrated ammonia water in the ultrasonic process to obtain a reaction mixed solution;
measuring Fe3O4The volume ratio of the reaction solution of the nano particles to the measured foam carbon is 5: 3-5: 1;
step 5, drying the reaction mixed liquid prepared in the step 4 after ultrasonic cleaning to obtain the prepared Fe3O4Nanoparticle/carbon foam composites.
2. The preparation method of the novel foam carbon electromagnetic shielding composite material according to claim 1, wherein the step 5 specifically comprises the following steps: and (4) ultrasonically cleaning the reaction mixed liquid prepared in the step (4) in deionized water for 5-10 min, and then drying the reaction mixed liquid in a vacuum drying oven at the temperature of 90 ℃ for 12-24 h.
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