CN114914710B - Electromagnetic wave absorbing material and preparation method and application thereof - Google Patents
Electromagnetic wave absorbing material and preparation method and application thereof Download PDFInfo
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- CN114914710B CN114914710B CN202210541994.2A CN202210541994A CN114914710B CN 114914710 B CN114914710 B CN 114914710B CN 202210541994 A CN202210541994 A CN 202210541994A CN 114914710 B CN114914710 B CN 114914710B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
- H01Q17/008—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems with a particular shape
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- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention belongs to the technical field of microwave absorbing materials, and relates to an electromagnetic wave absorbing material, a preparation method and application thereof. The electromagnetic wave absorbing material is copper-tin bimetallic selenide crystal, has a nano sheet shape and has a size of 200 nm-5 mu m. The preparation method comprises the following steps: and carrying out solvothermal reaction on copper salt, tin salt and selenite in a mixed solution of ethylene glycol and ethylenediamine to obtain the nano-sheet copper-tin bimetallic selenide. The electromagnetic wave absorbing material provided by the invention has excellent microwave absorbing effect in the frequency range of 0.1-40 GHz, and when the thickness is 1.0mm, the maximum reflection loss reaches-20.7 dB, and the effective absorption bandwidth reaches 6.5GHz; when the thickness is 1.5mm, the maximum reflection loss reaches-55.2 dB, and the effective bandwidth is 4.3GHz. The invention has simple synthesis process, excellent wave absorbing performance and good application prospect.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and relates to an electromagnetic wave absorbing material, a preparation method and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Dielectric loss materials mainly rely on electronic polarization or interface polarization attenuation to absorb electromagnetic waves, and the materials have the advantages of light weight, good stability, rich resources, good wave absorbing effect and the like, and are increasingly favored. The dielectric loss materials which are widely studied mainly include carbon materials (such as carbon fibers, carbon nanotubes, graphene, etc.), non-magnetic metallic carbon/oxygen/sulfide, polymers, etc. According to research of the inventor, the two-dimensional nano materials such as molybdenum disulfide, transition metal carbide (MXenes) and the like at present show high-performance microwave absorption effect. However, the existing dielectric loss materials require thicker coatings and the material preparation process is complex. Thus, there is a need to provide new materials with high performance microwave absorption.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an electromagnetic wave absorbing material, a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
in one aspect, the electromagnetic wave absorbing material is copper-tin bimetallic selenide crystals, has a nano sheet shape and has a size of 200 nm-5 mu m.
Experiments show that the copper-tin bimetallic selenide crystal with the unique two-dimensional structure is beneficial to enhancing reflection and scattering of incident electromagnetic waves in a wave-absorbing material matrix, so that the microwave absorption effect is enhanced.
On the other hand, the preparation method of the electromagnetic wave absorbing material comprises the step of carrying out solvothermal reaction on copper salt, tin salt and selenite in a mixed solution of ethylene glycol and ethylenediamine to obtain the nano-sheet copper-tin bimetallic selenide.
The nano flaky copper-tin bimetallic selenide crystal prepared by the method provided by the invention has an irregular shape, and the irregular shape copper-tin bimetallic selenide nano tablet is more beneficial to enhancing the microwave absorption effect.
In a third aspect, an electromagnetic wave absorbing material as described above is used in a wave absorbing device.
Specifically, the surface of the wave absorbing device is coated with a wave absorbing layer, and the wave absorbing material in the wave absorbing layer is the electromagnetic wave absorbing material.
Compared with the prior art, the invention has the following beneficial effects:
1. the electromagnetic wave absorbing material provided by the invention is copper-tin bimetallic selenide and has a two-dimensional nano sheet structure with the size of 200 nm-5 mu m, the material of the structure has the advantages of good wave absorbing effect, wide absorption frequency band and thin thickness (less than 2 mm), and experiments show that the electromagnetic wave absorbing material provided by the invention has excellent microwave absorbing effect in the frequency range of 0.1-40 GHz, and the maximum reflection loss can reach-20.7 dB when the thickness is 1.0mm, and the effective absorption bandwidth is as high as 6.5GHz; when the thickness is 1.5mm, the maximum reflection loss can reach-55.2 dB, and the effective bandwidth is 4.3GHz, so that the method has good application prospect in the wave-absorbing field.
2. The invention adopts a simple one-step solvothermal method, does not need subsequent high-temperature calcination treatment, and has the advantages of simple material preparation process, easy operation and low energy consumption.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is an XRD pattern of the copper tin bi-metal selenide prepared in example 1 and example 2;
FIG. 2 is a TEM image of the copper-tin bimetallic selenide prepared in example 3;
FIG. 3 is a plot of (a) the real part of the dielectric constant and (b) the imaginary part of the dielectric constant as a function of frequency for the copper-tin bi-metal selenide nanoplatelets prepared in example 5;
FIG. 4 is a plot of the change in (a) real and (b) imaginary permeability parts with frequency for the copper-tin bimetallic selenide nanoplatelets prepared in example 5;
fig. 5 is a graph showing the reflection loss of the copper-tin bi-metal selenide nano-sheet wave absorbing material prepared in example 6 at different thicknesses.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In view of the thicker coating required by the existing dielectric loss material and the complex preparation process of the material, the invention provides an electromagnetic wave absorption material and a preparation method and application thereof.
In an exemplary embodiment of the invention, an electromagnetic wave absorbing material is provided, wherein the electromagnetic wave absorbing material is copper-tin bimetallic selenide crystals, and has a nano sheet shape and a size of 200 nm-5 mu m.
Experiments show that the copper-tin bimetallic selenide crystal with the unique two-dimensional structure is beneficial to enhancing reflection and scattering of incident electromagnetic waves in a wave-absorbing material matrix, so that the microwave absorption effect is enhanced.
In some examples of this embodiment, the copper-tin bi-metal selenide is Cu 2 SnSe 4 。
In some examples of this embodiment, the material is a non-magnetic material.
In another embodiment of the invention, a preparation method of an electromagnetic wave absorbing material is provided, and copper salt, tin salt and selenite are subjected to solvothermal reaction in a mixed solution of ethylene glycol and ethylenediamine to obtain nano-sheet copper-tin bimetallic selenide.
The nano flaky copper-tin bimetallic selenide crystal prepared by the method provided by the invention has an irregular shape, and the irregular shape copper-tin bimetallic selenide nano tablet is more beneficial to enhancing the microwave absorption effect.
The solvothermal reaction refers to a reaction carried out on an original mixture in a closed system by taking an organic matter as a solvent at a certain temperature and under the autogenous pressure of a solution.
The copper salt refers to a compound of which the cation is cupric ion, such as cupric chloride, cupric sulfate, cupric nitrate, cupric acetate and the like.
The tin salt refers to a compound of which the cation is tetravalent tin ion, such as tin chloride, tin sulfate, tin nitrate, tin acetate and the like.
The selenite comprises sodium selenite, potassium selenite, ammonium selenite and the like.
In some examples of this embodiment, glucose is added to the solvothermal reaction system. Research shows that the addition of glucose can ensure that the phase of the copper-tin bimetallic selenide in the prepared product is purer, thereby improving the wave absorbing performance of the electromagnetic wave absorbing material.
In one or more embodiments, the glucose is added in an amount of 0.2 to 2.4 times the product mass. When the adding amount of glucose is 0.8-1.6 times of the product quality, the purity of the copper-tin bimetallic selenide phase in the product is further improved.
In some examples of this embodiment, the molar ratio of copper salt, tin salt to selenite is 1.8-2.2:1:3.8-4.2. The copper-tin bimetallic selenide crystal can be better formed.
In some examples of this embodiment, the volume ratio of ethylene glycol to ethylene diamine is 2.5 to 5:1. Under such conditions, the formation of pure Cu can be further ensured 2 SnSe 4 A phase.
In some examples of this embodiment, copper salt, tin salt, selenite, and glucose are added to ethylene glycol and stirred well, then ethylenediamine is added and stirred well again, and then solvothermal reaction is performed. When the raw materials are mixed, because the ethylenediamine has reducibility and alkalinity, if selenite/copper salt/tin salt is added after the ethylenediamine is mixed with ethylene glycol, the uniformity of the solution is affected, and the morphology of the final product is possibly affected.
In some examples of this embodiment, the solvothermal reaction is performed at a temperature of 160 to 200 ℃ for a period of 6 to 20 hours. The time is preferably 12 to 16 hours.
In order to avoid the attachment of soluble substances in the material, which affects the wave-absorbing properties, the product after solvothermal reaction needs to be purified. In some examples of this embodiment, after solvothermal reaction, the product is washed with ethanol and water and dried. The drying mode is vacuum drying, and the temperature is 60-80 ℃.
In a third embodiment of the present invention, there is provided an application of the above electromagnetic wave absorbing material in a wave absorbing device.
Specifically, the surface of the wave absorbing device is coated with a wave absorbing layer, and the wave absorbing material in the wave absorbing layer is the electromagnetic wave absorbing material.
More specifically, the electromagnetic wave absorbing material is mixed with the binder and then applied and cured. The adhesive is preferably paraffin, and the paraffin has little influence on the wave absorbing performance of the electromagnetic wave absorbing material, so that the wave absorbing layer can exert stable wave absorbing performance. The mass ratio of the electromagnetic wave absorbing material to the binder is preferably 1:0.8-1.2.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail with reference to specific embodiments.
Example 1：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.4g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 16 hours at 160 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
The XRD structure of the copper tin duplex metal selenide prepared in this example is shown in FIG. 1 a. It can be seen that the obtained bimetallic selenide has good crystallinity, diffraction peak and Cu 2 SnSe 4 Corresponding to standard cards (PDF # 16-0670), no other phase generation was found. By the technical scheme, the pure copper-tin bimetallic selenide with high crystallinity can be simply and effectively prepared.
Example 2：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0g of glucose are weighed and added into 45mL of ethylene glycol, and are magnetically stirred uniformly, and then 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 16 hours at 160 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
The XRD structure of the copper tin duplex metal selenide prepared in this example is shown in FIG. 1 b. It can be seen that without glucose, the resulting product phase is impure, except for Cu 2 SnSe 4 A portion of the CuSe impurity is also generated.
Example 3：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.4g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 16 hours at 180 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
TEM pictures of the Cu-Sn bimetallic selenide prepared in this example are shown in FIGS. 2a and b. It can be seen that the prepared copper-tin bimetallic selenide is in an irregular nano sheet shape, the size of the copper-tin bimetallic selenide is about 200 nanometers to several micrometers, and the unique two-dimensional structure is beneficial to enhancing the reflection and scattering of incident electromagnetic waves in the wave-absorbing material matrix, so that the microwave absorption effect is enhanced.
Example 4：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.4g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 12 hours at 180 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
Example 5：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.6g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 12 hours at 180 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
The graphs of the real and imaginary parts of the dielectric constants of the copper-tin bi-metal selenide nano-sheets prepared in this example as a function of frequency are shown in fig. 3a and b. It can be seen that in the frequency range of 0.1-40 GHz, the real part and the imaginary part of the dielectric constant of the prepared copper-tin bimetallic selenide nano-sheet have higher values (> 5), which indicates that the material has high dielectric loss capacity. Furthermore, it can be seen that the real and imaginary parts of the dielectric constants have a plurality of distinct formants in the high frequency part, which are related to the polarization relaxation loss caused by various polarization phenomena of the sample. Fig. 4a and b are graphs of the real part and the imaginary part of the magnetic permeability with the change of frequency, and since the copper-tin bimetal selenide nano sheet of the invention is a non-magnetic material, the real part of the magnetic permeability is close to 1, and the imaginary part of the magnetic permeability is close to 0, and the copper-tin bimetal selenide nano sheet of the invention is proved to be a dielectric loss material.
Example 6：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.6g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 16 hours at 180 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
The reflection loss curve diagrams of the copper-tin double-metal selenide nano-sheet wave-absorbing material prepared in the embodiment under different thicknesses are shown in fig. 5. It can be seen that when the thickness of the test sample is 1.0mm, the maximum reflection loss value can reach-20.7 dB at 23.2GHz, and the effective absorption bandwidth (the frequency width corresponding to the reflection loss < 10dB (absorption rate > 90%)) is as high as 6.5GHz (20.3-26.8 GHz); when the thickness is 1.5mm, the sample shows maximum reflection loss at 14.8GHz, reaches-55.2 dB, and has an effective bandwidth of 4.3GHz (13-17.3 GHz); when the thickness is more than or equal to 2mm, the sample also shows good wave absorbing performance in the range of 3-13 GHz. The results show that the copper-tin bimetallic selenide nano-sheet prepared by a simple solvothermal method has the advantages of thin coating thickness, excellent wave absorbing performance and wide absorption frequency band, and is suitable for the field of microwave absorption.
Example 7：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.8g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 12 hours at 180 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder.
Example 8：
0.341g of copper chloride dihydrate, 0.351g of tin tetrachloride pentahydrate, 0.692g of sodium selenite and 0.8g of glucose are weighed and added into 45mL of ethylene glycol, and the mixture is stirred magnetically uniformly, 15mL of ethylenediamine is added, and the magnetic stirring is continued for 1h; then transferring the mixture into a hydrothermal reaction kettle, and preserving heat for 16 hours at 160 ℃; and (3) repeatedly washing the product with ethanol and deionized water after the reaction kettle is cooled, and drying to obtain product powder. The electromagnetic parameters and microwave absorption performance were measured as follows:
the nano-sheet of the copper-tin bimetallic selenide prepared in the embodiment is used as an absorbent and paraffin in a mass ratio of 1:1, uniformly mixing, and pressing into a circular ring sample by using a custom mold; the electromagnetic parameters of the coaxial cable in the frequency range of 0.1-40 GHz are tested by adopting a vector network analyzer and combining a coaxial cable method; according to the transmission line theory, the reflection loss of the material under different thicknesses is calculated in a simulation mode.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. An electromagnetic wave absorbing material is characterized in that the material is a copper-tin bimetallic selenide crystal in a nano sheet shape, and the copper-tin bimetallic selenide is Cu 2 SnSe 4 The method comprises the steps of carrying out a first treatment on the surface of the The size is 200 nm-5 mu m;
the crystal is prepared by carrying out solvothermal reaction on copper salt, tin salt and selenite in a mixed solution of ethylene glycol and ethylenediamine; the molar ratio of the copper salt to the tin salt to the selenite is 1.8-2.2:1:3.8-4.2.
2. The preparation process of electromagnetic wave absorbing material features that copper salt, tin salt and selenite are reacted in solvent in mixed solution of glycol and ethylenediamine to obtain nanometer flaky Cu-Sn bimetallic selenide;
the mol ratio of copper salt, tin salt and selenite is 1.8-2.2:1:3.8-4.2;
the volume ratio of the ethylene glycol to the ethylenediamine is 2.5-5:1;
in the solvothermal reaction, the temperature is 160-200 ℃ and the time is 6-20 hours;
after solvothermal reaction, the copper-tin bimetallic selenide crystal is washed by ethanol and water and then dried.
3. The method for producing an electromagnetic wave absorbing material according to claim 2, wherein glucose is added to the solvothermal reaction system.
4. The method for producing an electromagnetic wave absorbing material according to claim 2, wherein the amount of glucose added is 0.2 to 2.4 times the mass of the copper-tin double metal selenide crystal.
5. The method for preparing an electromagnetic wave absorbing material according to claim 2, wherein copper salt, tin salt, selenite and glucose are added into ethylene glycol and stirred uniformly, then ethylenediamine is added and stirred uniformly continuously, and then solvothermal reaction is carried out.
6. An electromagnetic wave absorbing material according to claim 1 or an electromagnetic wave absorbing material obtained by the preparation method according to any one of claims 2 to 5, for use in a wave absorbing device.
7. The use according to claim 6, wherein the wave absorbing device is coated with a wave absorbing layer, and the wave absorbing material in the wave absorbing layer is the electromagnetic wave absorbing material.
8. The use according to claim 7, wherein the electromagnetic wave absorbing material is mixed with a binder and then cured by coating.
9. The use according to claim 8, wherein the binder is paraffin wax.
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