CN109880296B - Method for reversely designing negative dielectric material in metal mesh/epoxy resin composite material - Google Patents
Method for reversely designing negative dielectric material in metal mesh/epoxy resin composite material Download PDFInfo
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Abstract
The invention discloses a method for reversely designing a negative dielectric material in a metal mesh/epoxy resin composite material, which comprises the following steps of: step 1, putting a plurality of metal nets into acid solution with known concentration, and enabling the acid solution to respectively corrode the metal nets for different times; step 2, uniformly mixing the liquid epoxy resin and the organic solvent, adding the curing agent, and uniformly mixing to obtain a mixed solution; step 3, respectively immersing the metal nets corroded by the acid solution into the mixed solution to enable the epoxy resin to permeate into the metal nets; obtaining a metal mesh/epoxy resin composite material; step 4, drying the metal mesh/epoxy resin composite material under a vacuum condition; and 5, detecting the negative dielectric constant of the metal mesh/epoxy resin composite material dried in the step 4, if the negative dielectric constant does not meet the requirement, repeating the steps 1 to 4, and redesigning the time of the acid solution for corroding the metal mesh until the metal mesh/epoxy resin composite material with the negative dielectric constant meeting the requirement is prepared.
Description
Technical Field
The invention relates to the technical field of composite materials and the field of meta-materials, in particular to a method for reversely designing a negative dielectric material in a metal mesh/epoxy resin composite material.
Background
Negative dielectric materials have gained much attention in the last decade due to their new applications in plasmonic biosensing, dielectric constant enhancement, electromagnetic shielding, etc. In fact, the development of negative dielectric materials is closely related to metamaterials, and when the negative dielectric materials are combined with negative magnetic permeability materials, unique negative refraction can be realized. The metamaterial realizes the regulation and control of the electromagnetic performance by designing the shape (U-shaped, open resonance ring and fishing net) and arrangement mode of the periodic array. For a long time, the metamaterial is mainly researched in the fields of physical science and communication.
However, by controlling the chemical composition and microstructure of the material, modulation of negative electromagnetic parameters can also be achieved, and therefore, negative electromagnetic parameters are also of interest in conductor-insulator composites without a significant periodic structure. These studies have also greatly facilitated the development of negative dielectric materials in materials science and engineering. Typical material processing methods provide a more free and effective way for preparing negative dielectric materials, and the negative dielectric constant performance of the materials can be adjusted by controlling the chemical composition and microstructure of the materials. Theoretical analysis indicates that the negative dielectric constant is the result of a change in the microstructure of the material, during which free electrons in the conductive network oscillate. As the amount of conductive filler (metal or carbon material) in the composite increases, the filler contacts each other to form a conductive network, thereby forming a negative dielectric constant, which is a typical percolation phenomenon. The construction of a three-dimensional conductive network is the key to realizing a negative dielectric constant material.
Previous research has focused on designing negative dielectric materials by "additive manufacturing," i.e., by adding conductive particles to the matrix, when the content of the conductive phase exceeds but is still close to the percolation value, the conductive phase changes to a continuous phase and the dielectric constant becomes negative. However, due to the influence of percolation effect, the negative dielectric constant is very sensitive to the content of the conductive phase, and the precise regulation and control of the negative dielectric property are not easy to realize.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for easily regulating and controlling the negative dielectric property of a material, which has the advantages of simple and convenient process and low manufacturing cost and can accurately regulate and control the negative dielectric property of a composite material.
In order to achieve the above object, the present invention provides a method for reverse engineering a negative dielectric material in a metal mesh/epoxy composite material, comprising the steps of, step 1: putting a plurality of metal nets into an acid solution with known concentration, and enabling the acid solution to respectively corrode the metal nets for different times, wherein the time is limited by the fact that the metal nets are completely corroded by the acid solution; step 2: uniformly mixing liquid epoxy resin and an organic solvent, adding a curing agent, and uniformly mixing to obtain a mixed solution; and step 3: respectively immersing the metal mesh corroded by the acid solution into the mixed solution to enable epoxy resin to permeate into the metal mesh, so as to obtain a metal mesh/epoxy resin composite material; and 4, step 4: drying the metal mesh/epoxy resin composite material under a vacuum condition; and 5: and (4) detecting the negative dielectric constant of the metal mesh/epoxy resin composite material dried in the step (4), if the negative dielectric constant does not meet the requirement, repeating the steps (1) to (4), and redesigning the time for the metal mesh to be corroded by the acid solution until the metal mesh/epoxy resin composite material with the negative dielectric constant meeting the requirement is prepared.
Preferably, in step 1, the metal mesh comprises one of a nickel mesh, a copper mesh or an iron mesh.
Preferably, in step 1, the acid solution is a hydrochloric acid solution.
Preferably, in step 1, the mass fraction of hydrochloric acid in the hydrochloric acid solution is 18.5% -28.5%.
Preferably, in step 2, the organic solvent is ethanol.
Preferably, in the step 2, the temperature for mixing the liquid epoxy resin and the organic solvent is 40-60 ℃.
Preferably, in step 3, after the metal mesh is immersed in the mixed solution, the metal mesh is placed in a vacuum environment, so that the epoxy resin permeates into the metal mesh.
Preferably, in step 3, the metal mesh is placed in a vacuum environment for 1 to 3 hours.
Preferably, in step 4, the drying temperature is 120 ℃, and the drying time is 5 h.
Preferably, the method further comprises step 6: and (3) corroding the metal mesh by using an acid solution according to the corrosion time of the metal mesh with the negative dielectric constant meeting the requirement, and repeatedly preparing the metal mesh/epoxy resin composite material with the negative dielectric constant meeting the requirement according to the steps 2 to 4.
Has the advantages that:
(1) the method for reversely designing the negative dielectric material in the metal mesh/epoxy resin composite material has the advantages of simple process and low cost, can realize the mass production of products, and has good commercial prospect.
(2) The negative dielectric constant performance of the composite material is accurately regulated and controlled through reverse design, the negative dielectric constant value can be changed by changing the time for corroding the metal mesh with acid, and the regulation and control of the negative dielectric constant performance are simple.
(3) The metal mesh provides the composite with mechanical strength and is easily processed into the desired shape.
Drawings
Fig. 1 is a comparative graph of scanning electron micrographs of the nickel mesh in example 1 when it was not corroded and corroded for 10 hours, wherein (a) of fig. 1 is a graph of scanning electron micrographs of the nickel mesh when it was not corroded, and (b) of fig. 1 is a graph of scanning electron micrographs of the nickel mesh when it was corroded for 10 hours.
FIG. 2 is a graph showing the real part ε' of dielectric constant as a function of frequency for the nickel mesh/epoxy resin composite material of example 1.
Detailed Description
In order to make the specific processes and advantages of the present invention more apparent, the following detailed description is given with reference to specific examples. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present invention. The conditions employed in the examples may be further adjusted depending on the specific conditions, and the conditions not specified are generally those in the routine experiments.
The invention provides a method for preparing a negative dielectric material by a material reduction manufacturing method, which weakens an existing network by a chemical method or a material processing method so as to accurately control the value of a negative dielectric constant within a certain range.
According to the method for reversely designing the negative dielectric material in the metal mesh/epoxy resin composite material, the metal mesh with good chemical activity is selected, the metal mesh can react with acid, and the reverse design of the negative dielectric material can be realized by reducing the material, namely controlling the reaction time of the metal mesh and the acid. In the reverse design process of the negative dielectric material, the network is gradually weakened or even completely destroyed. In addition, the epoxy resin has good insulating property, and is selected as a matrix of the metal mesh/epoxy resin composite material, so that the composite material can be endowed with certain mechanical strength. The "/" indicates that the composite material is formed by polymerizing a metal mesh and an epoxy resin.
Materials, reagents and the like used in the following examples are commercially available. Wherein the mass fraction of the used hydrochloric acid solution is 18.5-28.5%. In the invention, the mass fraction of the hydrochloric acid solution is not limited to 18.5-28.5%, and if the concentration of the hydrochloric acid solution is lower, the metal corrosion time is prolonged; if the concentration of the hydrochloric acid solution is higher, the metal corrosion time is reduced.
Example 1
A method for reversely designing a negative dielectric material in a nickel mesh/epoxy resin composite material comprises the following steps:
(1) the nickel screen was ultrasonically cleaned with alcohol. While preparing a hydrochloric acid solution. Then the nickel screen is put into hydrochloric acid solution and respectively corroded for 2, 4, 10 and 11 hours. The longer the time for corroding the nickel mesh, the stronger the destructive power to the nickel mesh structure. Fig. 1 (a) is a scanning electron microscope image of the nickel mesh without corrosion, and fig. 1 (b) is a scanning electron microscope image of the nickel mesh when it is corroded for 10 hours, from which it can be seen that the nickel wire becomes thin and even breaks.
(2) 5g of liquid epoxy resin was mixed with 2g of alcohol to reduce the viscosity of the epoxy resin, and 0.2g of curing agent was added to the epoxy resin solution and stirred at 60 ℃ until the solution was clear.
(3) And (3) immersing the nickel screen corroded in the step (1) into the epoxy resin solution in the step (2), and vacuumizing for 1-3 hours to enable the epoxy resin to completely permeate into the nickel screen to obtain the nickel screen/epoxy resin composite material.
(4) And (4) drying the nickel mesh/epoxy resin composite material obtained in the step (3) for 5 hours at the temperature of 120 ℃ in a vacuum drying oven. FIG. 2 is a graph showing the frequency-dependent change of the real part ε' of the dielectric constant of a nickel mesh/epoxy resin composite material. It can be seen from the figure that the longer the nickel mesh etching time, the smaller the value of the negative dielectric constant until the negative dielectric becomes the positive dielectric.
(5) And finally, machining the nickel mesh/epoxy resin composite material into a certain shape and size by using a machining method according to the requirements of parts or applications.
Example 2
A method for reversely designing a negative dielectric material in a copper mesh/epoxy resin composite material comprises the following steps:
(1) the copper mesh was ultrasonically cleaned with alcohol. While preparing a hydrochloric acid solution. Then the copper net is put into hydrochloric acid solution and corroded for 2, 4, 6 and 8 hours respectively.
(2) 5g of liquid epoxy resin was mixed with 2g of alcohol to reduce the viscosity of the epoxy resin, and 0.2g of curing agent was added to the epoxy resin solution and stirred at 60 ℃ until the solution was clear.
(3) And (3) immersing the copper mesh corroded in the step (1) into the epoxy resin solution in the step (2), and vacuumizing for 1-3 hours to enable epoxy resin to permeate into the copper mesh to obtain the copper mesh/epoxy resin composite material.
(4) And (4) drying the copper mesh/epoxy resin composite material obtained in the step (3) for 5 hours at the temperature of 120 ℃ in a vacuum drying oven.
(5) And finally, machining the copper mesh/epoxy resin composite material into a certain shape and size by using a machining method according to the requirements of parts or applications.
Example 3
A method for reversely designing a negative dielectric material in an iron net/epoxy resin composite material comprises the following steps:
(1) the iron net was ultrasonically cleaned with alcohol. While preparing a hydrochloric acid solution. Then the iron net is put into hydrochloric acid solution and corroded for 1, 2, 3 and 4 hours respectively.
(2) 5g of liquid epoxy resin was mixed with 2g of alcohol to reduce the viscosity of the epoxy resin, and 0.2g of curing agent was added to the epoxy resin solution and stirred at 60 ℃ until the solution was clear.
(3) And (3) immersing the iron net corroded in the step (1) into the epoxy resin solution in the step (2), and vacuumizing for 1-3 hours to enable epoxy resin to permeate into the iron net, so that the iron net/epoxy resin composite material is obtained.
(4) And (4) drying the iron net/epoxy resin composite material obtained in the step (3) for 5 hours at the temperature of 120 ℃ in a vacuum drying oven.
(5) And finally, machining the iron net/epoxy resin composite material into a certain shape and size by using a machining method according to the requirements of parts or applications.
In the above embodiment, the composite material with a negative dielectric constant meeting the requirement can be obtained by controlling the reaction time of the metal mesh and the acid solution. The metal mesh also provides mechanical strength to the composite material, allowing it to be easily formed into the desired shape.
In conclusion, the method of the invention adopts the epoxy resin as the matrix, the metal net with good chemical activity as the electromagnetic functional body, and adopts the chemical corrosion and in-situ polymerization process to prepare the metal net/epoxy resin composite material with the negative dielectric constant, the process is simple and convenient, the manufacturing cost is low, and the method has important research value and wide market prospect in the application fields of microwave absorption, metamaterial, wireless power transmission and the like.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (9)
1. A method for reverse engineering negative dielectric material in metal mesh/epoxy resin composite material, which is characterized by comprising the following steps,
step 1: putting a plurality of metal nets into an acid solution with known concentration, and enabling the acid solution to respectively corrode the metal nets for different times, wherein the time is limited by the fact that the metal nets are completely corroded by the acid solution; the metal net is a nickel net;
step 2: uniformly mixing liquid epoxy resin and an organic solvent, adding a curing agent, and uniformly mixing to obtain a mixed solution;
and step 3: respectively immersing the metal mesh corroded by the acid solution into the mixed solution to enable epoxy resin to permeate into the metal mesh, so as to obtain a metal mesh/epoxy resin composite material;
and 4, step 4: drying the metal mesh/epoxy resin composite material under a vacuum condition;
and 5: and (4) detecting the negative dielectric constant of the metal mesh/epoxy resin composite material dried in the step (4), if the negative dielectric constant does not meet the requirement, repeating the steps (1) to (4), and redesigning the time for the metal mesh to be corroded by the acid solution until the metal mesh/epoxy resin composite material with the negative dielectric constant meeting the requirement is prepared.
2. The method of claim 1, wherein in step 1, the acid solution is hydrochloric acid solution.
3. The method for reverse engineering of negative dielectric material in metal mesh/epoxy composite material according to claim 2, wherein the hydrochloric acid solution in step 1 has a mass fraction of 18.5% -28.5%.
4. The method of reverse engineering a negative dielectric material in a metal mesh/epoxy composite according to claim 1, wherein in step 2, the organic solvent is ethanol.
5. The method for reverse engineering a negative dielectric material in a metal mesh/epoxy composite material according to claim 1, wherein the temperature of the mixture of the liquid epoxy resin and the organic solvent in step 2 is 40-60 ℃.
6. The method of claim 1, wherein in step 3, after the metal mesh is immersed in the mixed solution, the metal mesh is placed in a vacuum environment, so that the epoxy resin permeates into the metal mesh.
7. The method for reverse engineering a negative dielectric material in a metal mesh/epoxy composite material according to claim 6, wherein the time for placing the metal mesh in the vacuum environment in step 3 is 1-3 hours.
8. The method for reverse engineering a negative dielectric material in a metal mesh/epoxy composite material according to claim 1, wherein the drying temperature in step 4 is 120 ℃ and the drying time is 5 h.
9. The method of reverse engineering a negative dielectric material in a metal mesh/epoxy composite according to claim 1, further comprising the step of 6: and (3) corroding the metal mesh by using an acid solution according to the corrosion time of the metal mesh with the negative dielectric constant meeting the requirement, and repeatedly preparing the metal mesh/epoxy resin composite material with the negative dielectric constant meeting the requirement according to the steps 2 to 4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108641358A (en) * | 2018-05-17 | 2018-10-12 | 合肥工业大学 | A kind of preparation method of the carbon nano-tube/poly diphenyl sulfide with negative permittivity |
| CN108929542A (en) * | 2018-08-09 | 2018-12-04 | 上海海事大学 | A kind of dimethyl silicone polymer with negative permittivity/graphene flexible composite film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108641358A (en) * | 2018-05-17 | 2018-10-12 | 合肥工业大学 | A kind of preparation method of the carbon nano-tube/poly diphenyl sulfide with negative permittivity |
| CN108929542A (en) * | 2018-08-09 | 2018-12-04 | 上海海事大学 | A kind of dimethyl silicone polymer with negative permittivity/graphene flexible composite film and preparation method thereof |
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| "Tunable radio-frequency negative permittivity in nickel-alumina "natural" meta-composites";Zhi-cheng Shi，et al;《APPLIED PHYSICS LETTERS》;20141231;第104卷;252908 * |
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