CN114410223B - Graphene electromagnetic shielding coating and preparation method thereof - Google Patents
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- C09D5/24—Electrically-conducting paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08K2003/0806—Silver
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/085—Copper
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
Abstract
The invention provides a preparation method of a light broadband efficient electromagnetic shielding coating, which uses magnesium-thermal combustion synthesized graphene and a byproduct magnesium oxide powder thereof combined with silver-coated copper powder as a filler of the electromagnetic shielding coating, wherein in the preparation of the graphene, the combustion synthesized product does not need to be acid-washed, the graphene and the byproduct thereof are directly used as the filler, and the raw material of the electromagnetic shielding coating is dispersed by adopting a non-grinding medium, so that the prepared electromagnetic shielding coating has low volume of conductive filler, realizes the coordination and unification of high shielding efficiency, conductivity, low density and construction process of a coating, the shielding efficiency is more than or equal to 65dB (150 MHz-10 GHz), and the conductivity is as follows: sheet resistance is less than or equal to 400m omega, and surface density is as follows: less than or equal to 90g/m2.
Description
Technical Field
The invention relates to the technical field of electromagnetic shielding coatings, and particularly relates to a graphene electromagnetic shielding coating and a preparation method thereof.
Background
With the rapid development of the electronic information industry, communication equipment and electronic products are increasingly popularized, and the problem of interference of electromagnetic waves is increasingly serious, because an electric field and a magnetic field can be generated during the operation of electronic and electrical equipment, the intensive configuration and equipment devices thereof can form electromagnetic wave cross radiation, radiation pollution is caused, external electromagnetic interference is easily caused, the operation of the electronic and electrical equipment is seriously influenced, and instruments or equipment can generate errors, so that serious consequences are brought to the industry, families and military, therefore, the electromagnetic shielding coating with excellent shielding performance and simple manufacturing process becomes a hotspot of research.
The electromagnetic shielding coating is prepared from synthetic resin, conductive filler and solvent, and is coated on the surface of a base material to form a layer of cured film, so that the conductive shielding effect is achieved. Among the compositions of electromagnetic shielding coatings, the electromagnetic properties of the conductive filler are critical in determining the shielding properties of the coating. The electromagnetic shielding coating can be classified into 4 types of silver, copper, nickel and carbon based coatings according to the type of the conductive filler. The silver product has excellent conductivity and stability, low oxidation speed and high price, and is mainly used in the aerospace field with higher shielding requirements. Copper-based products have inferior electrical conductivity and good shielding effect, but poor oxidation resistance. The nickel product has conductivity, high price, high shielding effect and high oxidation resistance, and is the mainstream of the application of the electromagnetic shielding coating at present. The carbon products mainly use conductive graphite as a filler, and the products are low in price and poor in conductivity and are mostly applied at low end.
Graphene is an ideal conductive filler for electromagnetic shielding due to its high conductivity, high aspect ratio and low density. The high length-diameter ratio and the nanometer size of the coating enable the coating to obtain intentional electric conduction and electromagnetic shielding performance with small addition amount. In the preparation process of the graphene-based electromagnetic shielding coating or the conductive coating, in order to realize good dispersion of graphene in the coating, the traditional mechanical stirring can cause damage to the graphene, introduce defects and influence the conductivity of the graphene, and the ultrasonic mode can cause the characteristics of long dispersion time and low efficiency, so that a more efficient graphene dispersion mode is urgently needed on the premise of ensuring the complete quality of the graphene.
The invention patent CN10449010A discloses a preparation method of a polymer/graphene antistatic coating, wherein the antistatic problem of the coating is solved by adding 0.01-0.05 part of graphene into 100 parts of the polymer coating, but the problems of difficult dispersion and high cost of the graphene exist;
the invention patent CN110951369A discloses a coating for electromagnetic shielding, a preparation method and a use method thereof. The fillers are graphene, flaky silver-coated copper powder, spherical silver-coated copper powder and dendritic silver-coated copper powder, the addition amount of the fillers is 70-85%, but the content of the graphene in the fillers is ultrahigh by 50%, so that the cost of the coating is too high and the coating is dispersed efficiently;
the invention patent CN108129977A discloses a graphene composite conductive coating and a preparation method thereof, wherein graphene and copper powder and silver powder are used as conductive fillers, a magnetic stirrer is adopted for stirring and ultrasonic dispersion, so that graphene is damaged, defects are introduced, and the conductivity of the graphene is influenced, and an ultrasonic mode causes the characteristics of long dispersion time and low efficiency.
The carbon dioxide is adopted as the raw material to prepare the graphene through the magnesiothermic reduction reaction, and the prepared graphene has the characteristics of low price of the raw material, easiness in realization of scale production, high conductivity and few impurity functional groups on the surface of the graphene, so that attention is paid to the graphene in recent years. The invention patent CN106115675B reports a method for preparing mesoporous graphene by magnesium thermal heating. The patent proves that the prepared graphene has good capacitance performance and electrochemical stability, but the method needs to remove the magnesium oxide byproduct added and reacted by adopting a diluted acid solution washing mode, and on one hand, a large amount of hydrochloric acid and sulfuric acid are consumed in the subsequent treatment process, and on the other hand, impurity groups are introduced to the surface of the graphene in the acid washing process to reduce the conductivity of the graphene.
Aiming at the increasingly severe problems of electromagnetic pollution and electromagnetic interference, the series of problems of high density, high cost, poor efficiency and the like of the existing electromagnetic shielding coating, the design idea of the graphene modified electromagnetic shielding coating based on combustion synthesis is provided, the preparation method of the broadband light high-efficiency electromagnetic shielding coating is developed, and the technical problems that the wide-screen electromagnetic shielding, the high electrical conductivity and the low surface density of the coating are difficult to be considered are solved.
Disclosure of Invention
Aiming at the problems in the prior art, the application provides the graphene electromagnetic shielding coating, the coating adopts the mixed powder of graphene and magnesium oxide synthesized by combustion and silver-coated copper powder as the conductive composite filler, the volume concentration of the conductive filler of the coating is reduced, and the high shielding efficiency, the electric conductivity and the low density of the coating are realized.
The invention adopts the following technical scheme:
the light broadband efficient electromagnetic shielding coating is characterized by comprising a component A and a component B, wherein the component A comprises 60-70 parts by weight of epoxy resin, 0.5-1 part by weight of graphene and magnesium oxide mixed powder, 15-20 parts by weight of silver-coated copper powder, 0.5-1 part by weight of an auxiliary agent, 0.5-1 part by weight of a coupling agent and 5-7 parts by weight of a solvent; the component B is 20 to 30 parts of amine curing agent; the graphene and magnesium oxide mixed powder is a mixed product prepared through a combustion synthesis reaction, and the combustion synthesis reaction comprises the following steps: (1) mixing the raw materials in a mass ratio of 80-86:10-15 parts of nano magnesium oxide powder and magnesium powder are mixed to obtain a reactant, and the reactant is placed in a reaction kettle; (2) vacuumizing the reaction kettle, and filling carbon dioxide gas into the reaction kettle, wherein the pressure of the carbon dioxide gas is 0.5-1 MPa; (3) electrifying, heating and igniting the reactant by using a tungsten wire to initiate combustion synthesis reaction of magnesium powder and carbon dioxide; (4) and directly crushing the combustion synthesis product to obtain the graphene and magnesium oxide mixed powder, wherein the graphene and magnesium oxide mixed powder contains nanometer magnesium oxide powder with the dilution effect in a reactant.
Preferably, the particle size of the silver-coated copper powder is 10-14 μm; more preferably, the silver content in the silver-coated copper powder is 20wt%.
Preferably, the epoxy resin is epoxy modified silicone resin; the epoxy value of the epoxy resin is preferably 0.03 to 0.05.
Preferably, the auxiliary agent is one or two of an anti-settling agent and a defoaming agent.
Preferably, the anti-settling agent is selected from at least one of organic bentonite, amide wax and hydrogenated castor oil, and the antifoaming agent is selected from soybean lecithin.
Preferably, the solvent is selected from at least one of xylene, n-butanol, acetone, and cyclohexanone.
Preferably, the amine curing agent of the component B is at least one selected from polyamide, phenolic amine and polyether amine.
The invention also provides a preparation method of the electromagnetic shielding coating, which is characterized in that 60-70 parts of epoxy resin, 0.5-1 part of graphene and magnesium oxide powder, 15-20 parts of silver-coated copper powder, 0.5-1 part of auxiliary agent, 0.5-1 part of coupling agent and 5-7 parts of solvent are weighed and placed in a container to be uniformly mixed to obtain the component A; weighing 20-30 parts of amine curing agent as a component B; when in use, the component A and the component B are mixed evenly.
Preferably, the A component is mixed by high speed dispersion.
In the preparation of the graphene and the magnesium oxide powder, different from the conventional combustion synthesis reaction of graphene powder, the combustion synthesis product is not required to be subjected to acid washing and water washing, and the graphene synthesized by magnesium thermal combustion and the byproduct magnesium oxide thereof are used as the filler to prepare the high-performance electromagnetic shielding coating. The problems of the dispersibility of the graphene powder and the low-cost large-scale preparation are effectively solved.
According to the invention, the raw materials are dispersed without grinding media, so that on one hand, the silver-coated copper powder and the graphene powder are efficiently and uniformly mixed; on the other hand, mechanical damage of a silver coating on the surface of the copper powder is avoided, and structural integrity is ensured; the stability of the process is improved, and the high-efficiency dispersion is realized.
According to the invention, graphene synthesized by combustion and flaky silver-coated copper powder are used as a composite filler of the electromagnetic shielding coating, a synergistic electromagnetic shielding mechanism of the high-quality high-conductivity graphene and the silver-coated copper powder under the action of electromagnetic waves is exerted, the volume concentration of the conductive filler of the coating is reduced through formula optimization design, the high shielding efficiency, the conductivity, the low density and the coordination and unification of the construction process of the coating are realized, the shielding efficiency is more than or equal to 65dB (150 MHz-10 GHz), and the conductivity is as follows: sheet resistance is less than or equal to 400m omega, and surface density is as follows: less than or equal to 90g/m2.
The silver-coated copper/graphene composite material provided by the invention has double functions of high conductivity and magnetic conductivity, and when the silver-coated copper/graphene composite material is added into a coating, the electromagnetic shielding coating has high conductivity and electromagnetic shielding effect under the condition of low filler content, and the problems of light weight and high efficiency of the coating are solved. The surface protective coating composition provided by the invention has high electromagnetic shielding effectiveness and low-density and high-performance performances, and when the surface protective coating composition is coated on the surface of a base material, the high-efficiency wide-screen electromagnetic shielding effectiveness is provided under the condition of low density.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 shows SEM images of combustion-synthesized graphene powder and magnesium oxide powder as a byproduct thereof in example 1;
FIG. 2 shows a schematic diagram of the dispersion without milling media;
fig. 3 shows SEM images of silver-coated copper powder in examples 1 and 2.
Detailed Description
In order to make the technical solutions and technical effects of the present patent clearer, the following describes in detail specific embodiments of the present patent with reference to examples.
In order to more clearly illustrate the present invention, the present invention is further described below with reference to preferred embodiments and the accompanying drawings. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
The preparation method of the graphene and magnesium oxide filler comprises the following steps:
firstly, weighing a proper amount of nano magnesium oxide and magnesium powder, and uniformly mixing, wherein the mass ratio of the nano magnesium oxide to the metal magnesium powder is 7:1, filling the mixed powder into a reaction kettle, vacuumizing a reaction device, then filling carbon dioxide gas, wherein the pressure of the carbon dioxide gas is 0.5MPa, electrifying, heating and igniting a reactant by using a tungsten wire, automatically and continuously burning the reactant until the reactant is completely burnt and synthesized to obtain a mixed product of graphene and magnesium oxide, crushing the mixed product of the graphene and the magnesium oxide to obtain the high-conductivity graphene filler, wherein the SEM is shown in figure 1, and the microstructure of the powder is displayed among the magnesium oxide powder and distributed with the graphene. The magnesium oxide powder effectively prevents the graphene from agglomerating.
Preparing electromagnetic shielding paint:
the light broadband high-efficiency electromagnetic shielding coating consists of a component A and a component B, the contents of the components are shown in the following table 1 according to weight, wherein silver-coated copper powder with the particle size of 10-14 mu m and the silver content of 20wt% is adopted.
TABLE 1 content of each component of the electromagnetic shielding paint in example 1
And dispersing the raw materials in the component A in a container without grinding media to obtain the component A. When in use, the component A and the component B are weighed and mixed evenly to obtain the electromagnetic shielding coating.
The slurry is uniformly coated on an ABS base layer by a spraying method, the shielding effectiveness of the ABS base layer is tested, and the shielding effectiveness is shown in table 2 through detection, so that the shielding effectiveness is not less than 65dB (150 MHz-10 GHz), and the conductivity is as follows: sheet resistance is less than or equal to 400m omega, and surface density is as follows: less than or equal to 70g/m 2 。
Table 2 shielding effectiveness test results
Example 2
The preparation method of the graphene filler comprises the following steps:
firstly weighing a proper amount of nano magnesium oxide and magnesium powder, uniformly mixing, wherein the mass ratio of the nano magnesium oxide to the metal magnesium powder is 61, putting the mixed powder into a reaction kettle, vacuumizing a reaction device, then filling carbon dioxide gas, wherein the pressure of the carbon dioxide gas is 1.0MPa, electrifying, heating and igniting a reactant by using a tungsten wire, automatically and continuously burning the reactant until completely burning and synthesizing reaction is carried out after ignition, obtaining a mixed product of graphene and magnesium oxide, and crushing the mixed product of graphene and magnesium oxide to obtain the high-conductivity graphene filler.
Preparing electromagnetic shielding paint:
the light broadband high-efficiency electromagnetic shielding coating consists of a component A and a component B, the contents of the components are shown in Table 3 according to weight, wherein silver-coated copper powder with the particle size of 10-14 mu m and the silver content of 20wt% is adopted.
Table 3 contents of respective components of the electro-magnetic shielding coating material in example 2
And dispersing all the raw materials in the component A in a container without grinding media to obtain the component A. When in use, the component A and the component B are weighed and mixed evenly to obtain the electromagnetic shielding coating.
The slurry is uniformly coated on the ABS base layer by a spraying method, and the detection shows that the shielding effectiveness is more than or equal to 65dB (150 MHz-10 GHz), the conductivity is less than or equal to 400m omega, and the surface density is as follows: less than or equal to 70g/m 2 。
In examples 1 and 2, the raw materials of the component a are dispersed and mixed without using a grinding medium in the preparation method of the electromagnetic shielding coating, and the dispersion principle is shown in fig. 2. In examples 1 and 2, silver-coated copper powder having a particle size of 10 to 14 μm and a silver content of 20wt% was used, and the SEM image thereof is shown in FIG. 3. The epoxy value of the epoxy resin in example 1 and example 2 was 0.04.
Claims (10)
1. The light broadband efficient electromagnetic shielding coating is characterized by comprising a component A and a component B, wherein the component A comprises 60-70 parts by weight of epoxy resin, 0.5-1 part by weight of graphene and magnesium oxide mixed powder, 15-20 parts by weight of silver-coated copper powder, 0.5-1 part by weight of an auxiliary agent, 0.5-1 part by weight of a coupling agent and 5-7 parts by weight of a solvent; the component B is 20 to 30 parts of amine curing agent; the graphene and magnesium oxide mixed powder is a mixed product prepared by a combustion synthesis reaction, and the combustion synthesis reaction comprises the following steps: (1) mixing the raw materials in a mass ratio of 80-86:10-15 parts of nano magnesium oxide powder and magnesium powder are mixed to obtain a reactant, and the reactant is placed in a reaction kettle; (2) vacuumizing the reaction kettle, and filling carbon dioxide gas into the reaction kettle, wherein the pressure of the carbon dioxide gas is 0.5-1 MPa; (3) electrifying, heating and igniting the reactant by using a tungsten wire to initiate combustion synthesis reaction of magnesium powder and carbon dioxide; (4) directly crushing a combustion synthesis product to obtain the graphene and magnesium oxide mixed powder, wherein the graphene and magnesium oxide mixed powder comprises nano magnesium oxide powder with a diluting effect in a reactant, the shielding effectiveness of the coating is not less than 65dB under the condition of 150MHz-10GHz, and the conductivity is as follows: sheet resistance is less than or equal to 400m omega, and surface density is as follows: less than or equal to 90g/m 2 ；
The particle size of the silver-coated copper powder is 10-14 mu m; the silver content in the silver-coated copper powder is 20wt%.
2. The electromagnetic shielding coating of claim 1, wherein the epoxy resin is an epoxy-modified silicone resin.
3. The electro-magnetic shielding paint of claim 2, wherein the epoxy value of the epoxy resin is 0.03 to 0.05.
4. The electromagnetic shielding paint according to any one of claims 1 to 3, wherein the auxiliary agent is one or both of an anti-settling agent and an antifoaming agent.
5. The electro-magnetic shielding coating of claim 4, wherein the anti-settling agent is selected from at least one of organic bentonite, amide wax and hydrogenated castor oil, and the antifoaming agent is selected from soy lecithin.
6. The electro-magnetic shielding paint as claimed in claim 1, wherein the solvent is at least one selected from the group consisting of xylene, n-butanol, acetone and cyclohexanone.
7. The electromagnetic shielding paint according to claim 1, wherein the amine curing agent of the component B is at least one selected from the group consisting of polyamide, phenalkamine and polyetheramine.
8. The preparation method of the electromagnetic shielding coating material according to claim 1, characterized by weighing 60-70 parts by weight of epoxy resin, 0.5-1 part by weight of mixed powder of graphene and magnesium oxide, 15-20 parts by weight of silver-coated copper powder, 0.5-1 part by weight of auxiliary agent, 0.5-1 part by weight of coupling agent, and 5-7 parts by weight of solvent, and uniformly mixing in a container to obtain a component A; weighing 20-30 parts of amine curing agent as a component B; when in use, the component A and the component B are mixed uniformly.
9. The method for preparing an electromagnetic shielding paint as claimed in claim 8, wherein the component A is dispersed at a high speed during the mixing.
10. The method for preparing an electromagnetic shielding paint according to claim 8 or 9, wherein the component A is dispersed without using a grinding medium during mixing.
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