CN109777044B - Electromagnetic shielding composite material based on graphene honeycomb structure and preparation method and application thereof - Google Patents
Electromagnetic shielding composite material based on graphene honeycomb structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an electromagnetic shielding composite material based on a graphene honeycomb structure, and belongs to the field of electromagnetic shielding. The paint comprises the following components in parts by mass: 1.1-2.6 parts by weight of honeycomb structure graphene, 100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent. The honeycomb walls of the electromagnetic shielding composite material are formed by penetrating graphene, the structure arrangement is uniform, a complete conductive path is formed, electromagnetic waves can be subjected to multiple reflection, scattering, absorption and other processes in the honeycomb after entering the honeycomb structure, the structure can greatly improve multiple adsorption, reflection and scattering of the electromagnetic waves in the material, the path of the electromagnetic waves in the material is prolonged, the 'transmission, absorption and dispersion' functions of the electromagnetic waves in the structure are realized more easily, and the conductive and electromagnetic shielding performance of the composite material is improved. In addition, the honeycomb structure graphene in the invention is in a state close to a hollow state, so that the weight of the material can be obviously reduced.
Description
Technical Field
The invention relates to the technical field of electromagnetic shielding, in particular to an electromagnetic shielding composite material based on a graphene honeycomb structure and a preparation method and application thereof.
Background
The epoxy resin has the advantages of high tensile strength and Young modulus, good solvent resistance, low cost and the like, and is one of main matrix materials for manufacturing the polymer-based electromagnetic shielding composite material. Compared with the traditional metal-based electromagnetic shielding material, the carbon filler/polymer-based composite material has the advantages of low density, high conductivity, corrosion resistance, easy processing and the like, and is one of the most ideal electromagnetic shielding materials at present. Compared with other carbon materials, the graphene has the characteristics of large specific surface area, excellent electron transmission performance and the like, and has wide application prospects in the fields of sensors, nano-electronic devices and the like.
However, due to strong van der waals force between graphene sheets and contact resistance between sheets, irreversible stacking or aggregation between sheets is caused, and properties such as excellent electrical mechanics are seriously inhibited. And the graphene is made into a three-dimensional porous structure, so that the problems can be effectively solved. Although the commonly used three-dimensional structure has many excellent properties, the graphene sheets are partially oriented or almost parallel to each other to form an anisotropic layered structure, which affects the electrical conductivity and electromagnetic shielding properties.
Disclosure of Invention
In view of this, the present invention provides an electromagnetic shielding composite material based on a graphene honeycomb structure, and a preparation method and an application thereof. The electromagnetic shielding composite material provided by the invention has high conductivity and excellent electromagnetic shielding performance.
In order to achieve the above object, the present invention provides the following technical solutions:
an electromagnetic shielding composite material based on a graphene honeycomb structure comprises the following components in parts by mass:
1.1-2.6 parts by weight of honeycomb structure graphene, 100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent.
Preferably, the graphene with the honeycomb structure is in a honeycomb hexagon shape.
Preferably, the side length of the honeycomb hexagon is 0.5 mm.
Preferably, the curing agent is EK 3402.
The invention also provides a preparation method of the electromagnetic shielding composite material in the technical scheme, which comprises the following steps:
immersing an aluminum oxide honeycomb plate into a graphene oxide solution, performing ultrasonic treatment, and then performing freeze drying to obtain a graphene oxide-aluminum honeycomb plate composite structure;
etching an alumina honeycomb plate in the graphene oxide-aluminum honeycomb plate composite structure by using dilute hydrochloric acid, and then drying to obtain graphene oxide with a honeycomb structure;
annealing the graphene oxide with the honeycomb structure in a hydrogen/argon mixed atmosphere to obtain graphene with the honeycomb structure;
and mixing epoxy resin and a curing agent in a water bath, pouring the obtained mixture into the honeycomb-structure graphene, and then sequentially exhausting and curing to obtain the electromagnetic shielding composite material.
Preferably, the graphene oxide in the graphene oxide solution is prepared by a modified Hummers method through concentrated sulfuric acid, potassium permanganate, hydrogen peroxide and water.
Preferably, the volume fraction of hydrogen in the hydrogen/argon mixed atmosphere is 5%.
Preferably, the annealing temperature is 450-800 ℃, and the annealing time is 1-2 h.
Preferably, the heating rate of heating to the annealing temperature is 2-5 ℃/min.
The invention also provides the application of the electromagnetic shielding composite material in the technical scheme in the field of electromagnetic shielding.
The invention provides an electromagnetic shielding composite material based on a graphene honeycomb structure, which comprises the following components in parts by mass: 1.1-2.6 parts by weight of honeycomb structure graphene, 100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent. The honeycomb walls of the electromagnetic shielding composite material are formed by penetrating graphene, the structure arrangement is uniform, a complete conductive path is formed, electromagnetic waves can be subjected to multiple reflection, scattering, absorption and other processes in the honeycomb after entering the honeycomb structure, the structure can greatly improve multiple adsorption, reflection and scattering of the electromagnetic waves in the material, the path of the electromagnetic waves in the material is prolonged, the 'transmission, absorption and dispersion' functions of the electromagnetic waves in the structure are realized more easily, and the conductive and electromagnetic shielding performance of the composite material is improved. In addition, the honeycomb structure graphene in the invention is in a state close to a hollow state, so that the weight of the material can be obviously reduced. The data of the embodiment shows that the electromagnetic shielding effectiveness of the electromagnetic shielding composite material provided by the invention is improved to 20-38 dB from 1dB of pure epoxy resin, and the conductivity is 13.2-40.2S/m.
Drawings
Fig. 1 is a scanning electron microscope image of the graphene with the honeycomb structure prepared by the invention.
Detailed Description
The invention provides an electromagnetic shielding composite material based on a graphene honeycomb structure, which comprises the following components in parts by mass:
1.1-2.6 parts by weight of honeycomb structure graphene, 100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent.
According to the invention, the honeycomb walls of the graphene with the honeycomb structure are formed by penetrating the graphene, the structure is uniformly arranged, a complete conductive path is formed, and electromagnetic waves can be subjected to multiple reflection, scattering, absorption and other processes in the honeycomb after entering the honeycomb structure. In addition, the honeycomb structure graphene in the invention is in a state close to a hollow state, so that the weight of the material can be obviously reduced.
In the present invention, the graphene having a honeycomb structure is preferably a honeycomb hexagon.
In the present invention, the side length of the honeycomb hexagon is preferably 0.5 mm.
In the present invention, the curing agent is preferably EK 3402. The source of the curing agent is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the structural formula of the EK3402 is as follows:
in the present invention, the structural formula of the epoxy resin is as follows:
the invention also provides a preparation method of the electromagnetic shielding composite material in the technical scheme, which comprises the following steps:
immersing an aluminum oxide honeycomb plate into a graphene oxide solution, performing ultrasonic treatment, and then performing freeze drying to obtain a graphene oxide-aluminum honeycomb plate composite structure;
etching an alumina honeycomb plate in the graphene oxide-aluminum honeycomb plate composite structure by using dilute hydrochloric acid, and then drying to obtain graphene oxide with a honeycomb structure;
annealing the graphene oxide with the honeycomb structure in a hydrogen/argon mixed atmosphere to obtain graphene with the honeycomb structure;
and mixing epoxy resin and a curing agent in a water bath, pouring the obtained mixture into the honeycomb-structure graphene, and then sequentially exhausting and curing to obtain the electromagnetic shielding composite material.
According to the invention, an alumina honeycomb plate is immersed in a graphene oxide solution for ultrasonic treatment and then is subjected to freeze drying, so that a graphene oxide-aluminum honeycomb plate composite structure is obtained.
In the present invention, the Graphene Oxide (GO) in the graphene oxide solution is preferably prepared by a modified Hummers method using concentrated sulfuric acid, potassium permanganate, hydrogen peroxide, and water. The invention does not specially limit the concrete mode of the improved Hummers method, and adopts a mode known by persons skilled in the art, specifically, for example, natural graphite flakes are added into 8% concentrated sulfuric acid, stirred, diluted and filtered, and then the product is added into 98% concentrated sulfuric acid, and KMnO is added under the ice bath condition4Stirring, heating, stirring, adding deionized water, stirring, and adding H2O2(ii) a And sequentially adding deionized water and concentrated hydrochloric acid, standing and centrifuging to obtain Graphene Oxide (GO).
In the present invention, said H2O2Preferably slowly, dropwise.
In the present invention, the KMnO4Preferably, the addition is carried out slowly in small amounts, preferably over a period of 15 min.
The preparation method of the graphene oxide solution is not particularly limited, and a method well known to those skilled in the art can be adopted. In the present invention, the concentration of graphene oxide in the graphene oxide solution is preferably 5, 10, 15 and 20 g/L.
The power and time of the ultrasonic treatment are not particularly limited, and the graphene oxide in the graphene oxide solution can be loaded on the surface of the alumina honeycomb plate.
In the present invention, the freeze-drying is preferably performed in a freeze-dryer, and the freeze-drying time is preferably 48 to 72 hours.
After the graphene oxide-aluminum honeycomb plate composite structure is obtained, the aluminum oxide honeycomb plate in the graphene oxide-aluminum honeycomb plate composite structure is etched by dilute hydrochloric acid, and then the aluminum oxide honeycomb plate is dried to obtain the graphene oxide (GH) with the honeycomb structure. In the invention, the mass ratio of the graphene oxide to the dilute hydrochloric acid in the graphene oxide-aluminum honeycomb plate composite structure is preferably 1:10, and the concentration of the dilute hydrochloric acid is preferably 1.5 mol/L.
After the dilute hydrochloric acid etching is completed, the present invention preferably washes the resulting dilute hydrochloric acid etching product with deionized water to neutrality.
In the invention, the drying is preferably freeze drying, the freeze drying is preferably carried out in a freeze dryer, and the freeze drying time is preferably 48-72 h.
After obtaining the graphene oxide with the honeycomb structure, annealing the graphene oxide with the honeycomb structure in a hydrogen/argon mixed atmosphere to obtain graphene (rGH) with the honeycomb structure.
In the present invention, the volume fraction of hydrogen in the hydrogen/argon mixed atmosphere is preferably 5%.
In the invention, the annealing temperature is preferably 450-800 ℃, more preferably 600-800 ℃, and the annealing time is preferably 1-2 h.
In the present invention, the rate of temperature rise to the annealing temperature is preferably 2 to 5 ℃/min, and more preferably 3 to 4 ℃/min.
After the graphene with the honeycomb structure is obtained, epoxy resin and a curing agent are mixed in a water bath, the obtained mixture is poured into the graphene with the honeycomb structure, and then air suction and curing are sequentially carried out, so that the electromagnetic shielding composite material is obtained.
In the invention, the temperature of the water bath is preferably 70-100 ℃, and more preferably 80-90 ℃.
In the invention, the mixing is preferably mechanical stirring, the rotation speed of the mechanical stirring is preferably 200rpm, and the time of the mechanical stirring is preferably 20-40 min.
In the invention, the air extraction time is preferably 30-60 min, more preferably 40-50 min, and the air extraction is preferably carried out by a vacuum oven.
In the invention, the curing temperature is preferably 120 ℃, the curing time is preferably 5-7 h, and the curing is preferably carried out in an oven.
After the curing is finished, the invention preferably naturally cools the cured product to room temperature to obtain the electromagnetic shielding composite material.
The invention also provides the application of the electromagnetic shielding composite material in the technical scheme in the field of electromagnetic shielding.
The electromagnetic shielding composite material based on the graphene honeycomb structure, the preparation method and the application thereof provided by the invention are described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of the invention.
Example 1:
adding 0.5 weight part of natural graphite flake into 2 weight parts of 98% concentrated sulfuric acid, and stirring for 4 hours at 80 ℃; diluting and filtering, adding the product into 20 parts by weight of 98% concentrated sulfuric acid, and adding 1.5 parts by weight of KMnO under the ice bath condition4Stirring for 20min, heating to 35 ℃, and stirring for 2 h; adding 30 parts by weight of deionized water, stirring for 15min, and adding 5 parts by weight of H2O2(ii) a Then adding 100 parts by weight of deionized water and 10 parts by weight of 12mol/L concentrated hydrochloric acid in sequence, standing and centrifuging to obtain GO;
immersing an aluminum oxide honeycomb plate into GO solution, carrying out ultrasonic treatment for 30min, and standing for 48h to obtain a graphene oxide-aluminum honeycomb plate composite structure. Placing the obtained product in a freeze dryer for 48hrs, etching an alumina honeycomb plate by using 10 parts by weight of 1.5mol/L dilute hydrochloric acid, and washing the alumina honeycomb plate by using deionized water until the alumina honeycomb plate is neutral to obtain the graphene oxide (GH) with the honeycomb structure. Followed by lyophilization for 48hrs to obtain dried GH. GH is put at a speed of 2 ℃/min-1At a rate of 5% hydrogen/argon (v/v) atmosphere, at 450 ℃ for 2h, to obtain rGH;
100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent (EK3402) were mechanically stirred (200rpm) for 20min in a water bath at 70 ℃. The mixture was then poured into rGH and evacuated for 30min using a vacuum oven. And finally, curing for 5 hours in an oven at 120 ℃, and naturally cooling to room temperature to obtain the rGH/epoxy resin electromagnetic shielding composite material.
Through tests, the prepared graphene/epoxy resin electromagnetic shielding composite material with the honeycomb structure has the filler content of 0.9 wt%, the conductivity of 32.5S/m and the electromagnetic shielding performance of 25 dB.
Fig. 1 is a scanning electron microscope image of the graphene with the honeycomb structure prepared by the invention, and as can be seen from fig. 1, the graphene with the honeycomb structure prepared by the invention has a honeycomb hexagonal structure.
Example 2:
adding 1 weight part of natural graphite flake into 4 weight parts of 98% concentrated sulfuric acid, and stirring for 6 hours at 80 ℃; diluting and filtering, adding the product into 40 parts by weight of 98% concentrated sulfuric acid, and adding 3 parts by weight of KMnO under the ice bath condition4Stirring for 40min, heating to 35 ℃, and stirring for 2 h; adding 60 parts by weight of deionized water, stirring for 15min, and adding 10 parts by weight of H2O2(ii) a Sequentially adding 200 parts by weight of deionized water and 20 parts by weight of 12mol/L concentrated hydrochloric acid, standing and centrifuging to obtain GO;
and (3) immersing the alumina honeycomb plate into a GO solution, carrying out ultrasonic treatment for 30min, and standing for 48h to obtain the graphene oxide-aluminum honeycomb plate composite structure. And (3) placing the honeycomb structure in a freeze dryer for 72 hours, etching the alumina honeycomb plate by using 10 parts by weight of 1.5mol/L dilute hydrochloric acid, and washing the alumina honeycomb plate by using deionized water until the alumina honeycomb plate is neutral to obtain the graphene oxide (GH) with the honeycomb structure. Followed by lyophilization for 72hrs to obtain dried GH. Annealing GH at a rate of 5 ℃/min for 2h at 800 ℃ in a 5% hydrogen/argon (v/v) atmosphere to obtain rGH;
100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent (EK3402) were mechanically stirred (200rpm) for 40min at 100 ℃ in a water bath. The mixture was then poured into rGH and evacuated with a vacuum oven for 60 min. And finally, curing for 7 hours in an oven at 120 ℃, and naturally cooling to room temperature to obtain the rGH/epoxy resin electromagnetic shielding composite material.
Through tests, the prepared graphene/epoxy resin electromagnetic shielding composite material with the honeycomb structure has the filler content of 1.2 wt%, the conductivity of 40.2S/m and the electromagnetic shielding performance of 38 dB.
Example 3:
adding 1.5 parts by weight of natural graphite flakes into 6 parts by weight of 98% concentrated sulfuric acid, and stirring at 80 ℃ for 4 hours; diluting and filtering, adding the product into 60 parts by weight of 98% concentrated sulfuric acid, and adding 4.5 parts by weight of KMnO under the ice bath condition4Stirring for 30min, heating to 35 ℃, and stirring for 2 h; adding 30 parts by weight of deionized water, stirring for 15min, and adding 15 parts by weight of H2O2(ii) a Then sequentially adding 300 parts by weight of deionized water and 30 parts by weight of 12mol/L concentrated hydrochloric acid, standing and centrifuging to obtain GO;
and (3) immersing the alumina honeycomb plate into a GO solution, carrying out ultrasonic treatment for 30min, and standing for 48h to obtain the graphene oxide-aluminum honeycomb plate composite structure. Placing the obtained product in a freeze dryer for 48hrs, etching an alumina honeycomb plate by using 10 parts by weight of 1.5mol/L dilute hydrochloric acid, and washing the alumina honeycomb plate by using deionized water until the alumina honeycomb plate is neutral to obtain the graphene oxide (GH) with the honeycomb structure. Followed by lyophilization for 72hrs to obtain dried GH. Annealing GH at a rate of 3 ℃/min for 2h at 450 ℃ in a 5% hydrogen/argon (v/v) atmosphere to obtain rGH;
100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent (EK3402) were mechanically stirred (200rpm) for 30min in a water bath at 80 ℃. Then, the mixture was poured into rGH obtained in step (b) and evacuated for 40min with a vacuum oven. And finally, curing for 6 hours in an oven at 120 ℃, and naturally cooling to room temperature to obtain the rGH/epoxy resin electromagnetic shielding composite material.
Through tests, the prepared graphene/epoxy resin electromagnetic shielding composite material with the honeycomb structure has the filler content of 1.7 wt%, the conductivity of 31.3S/m and the electromagnetic shielding performance of 33 dB.
Example 4:
adding 2 parts by weight of natural graphite flakes into 8 parts by weight of 98% concentrated sulfuric acid, and stirring for 6 hours at 80 ℃; diluting and filtering, adding the product into 80 parts by weight of 98% concentrated sulfuric acid, and adding 6 parts by weight of KMnO under the ice bath condition4Stirring for 30min, heating to 35 deg.C, and stirring for 2 hrs; adding 120 parts by weight of deionized water, stirring for 15min, and adding 20 parts by weight of H2O2(ii) a Then adding 400 parts by weight of deionized water and 40 parts by weight of 12mol/L concentrated hydrochloric acid in sequence, standing and centrifuging to obtain GO;
and (3) immersing the alumina honeycomb plate into a GO solution, carrying out ultrasonic treatment for 30min, and standing for 48h to obtain the graphene oxide-aluminum honeycomb plate composite structure. And (3) placing the honeycomb structure in a freeze dryer for 72 hours, etching the alumina honeycomb plate by using 10 parts by weight of 1.5mol/L dilute hydrochloric acid, and washing the alumina honeycomb plate by using deionized water until the alumina honeycomb plate is neutral to obtain the graphene oxide (GH) with the honeycomb structure. Followed by lyophilization for 48hrs to obtain dried GH. Annealing GH at a rate of 4 ℃/min for 2h at 450 ℃ in a 5% hydrogen/argon (v/v) atmosphere to obtain rGH;
100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent (EK3402) were mechanically stirred (200rpm) in a water bath at 90 ℃ for 35 min. The mixture was then poured into rGH and evacuated for 50min using a vacuum oven. And finally, curing for 6.5h in an oven at 120 ℃, and naturally cooling to room temperature to obtain the rGH/epoxy resin electromagnetic shielding composite material.
Through tests, the prepared graphene/epoxy resin electromagnetic shielding composite material with the honeycomb structure has the filler content of 2.0 wt%, the conductivity of 13.2S/m and the electromagnetic shielding performance of 20 dB.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The electromagnetic shielding composite material based on the graphene honeycomb structure is characterized by comprising the following components in parts by mass:
1.1-2.6 parts by weight of honeycomb structure graphene, 100 parts by weight of epoxy resin and 26.5 parts by weight of curing agent;
the preparation method of the electromagnetic shielding composite material comprises the following steps:
immersing an aluminum oxide honeycomb plate into a graphene oxide solution, performing ultrasonic treatment, and then performing freeze drying to obtain a graphene oxide-aluminum honeycomb plate composite structure;
etching an alumina honeycomb plate in the graphene oxide-aluminum honeycomb plate composite structure by using dilute hydrochloric acid, and then drying to obtain graphene oxide with a honeycomb structure;
annealing the graphene oxide with the honeycomb structure in a hydrogen/argon mixed atmosphere to obtain graphene with the honeycomb structure;
and mixing epoxy resin and a curing agent in a water bath, pouring the obtained mixture into the honeycomb-structure graphene, and then sequentially exhausting and curing to obtain the electromagnetic shielding composite material.
2. The electromagnetically shielding composite as claimed in claim 1, wherein said graphene of honeycomb structure is a honeycomb hexagon.
3. The electromagnetically shielding composite as claimed in claim 2, wherein said honeycomb hexagon has a side length of 0.5 mm.
4. The electro-magnetic shielding composite of claim 1, wherein the curing agent is EK 3402.
5. The method for preparing the electromagnetic shielding composite material according to any one of claims 1 to 4, comprising the steps of:
immersing an aluminum oxide honeycomb plate into a graphene oxide solution, performing ultrasonic treatment, and then performing freeze drying to obtain a graphene oxide-aluminum honeycomb plate composite structure;
etching an alumina honeycomb plate in the graphene oxide-aluminum honeycomb plate composite structure by using dilute hydrochloric acid, and then drying to obtain graphene oxide with a honeycomb structure;
annealing the graphene oxide with the honeycomb structure in a hydrogen/argon mixed atmosphere to obtain graphene with the honeycomb structure;
and mixing epoxy resin and a curing agent in a water bath, pouring the obtained mixture into the honeycomb-structure graphene, and then sequentially exhausting and curing to obtain the electromagnetic shielding composite material.
6. The preparation method according to claim 5, wherein the graphene oxide in the graphene oxide solution is prepared by a modified Hummers method using concentrated sulfuric acid, potassium permanganate, hydrogen peroxide and water.
7. The method according to claim 5, wherein the volume fraction of hydrogen in the hydrogen/argon mixed atmosphere is 5%.
8. The preparation method according to claim 5, wherein the annealing temperature is 450-800 ℃, and the annealing time is 1-2 h.
9. The method according to claim 5 or 8, wherein a temperature rise rate of raising the temperature to the annealing temperature is 2 to 5 ℃/min.
10. Use of the electromagnetically shielding composite as claimed in any one of claims 1 to 4 in the field of electromagnetic shielding.
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