CN111730924B - Terahertz wave-absorbing material with gradient aperture structure and preparation method thereof - Google Patents
Terahertz wave-absorbing material with gradient aperture structure and preparation method thereof Download PDFInfo
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Abstract
A terahertz wave-absorbing material with a gradient aperture structure belongs to the technical field of terahertz wave-absorbing. The wave-absorbing material comprises three layers of three-dimensional graphene/PDMS composite materials, wherein the aperture range of the three-dimensional graphene on the uppermost layer is 100-120 mu m, the aperture range of the three-dimensional graphene in the middle layer is 50-70 mu m, and the aperture range of the three-dimensional graphene on the lowermost layer is 20-40 mu m. The terahertz wave-absorbing material has extremely strong broadband terahertz wave absorption characteristics, and the average absorption rate in the ultra-wideband frequency spectrum range of 0.2-1.2THz is up to more than 93%; the terahertz wave-absorbing material is extremely thin, the thickness of each layer is controlled within 1mm, the total thickness of the terahertz wave-absorbing material is within 3mm, and the terahertz wave-absorbing material is far superior to the existing terahertz wave-absorbing foam material; excellent flexibility characteristics such as bending, stretching and mechanical elasticity; the raw materials are low in price, the preparation method is simple, and large-area preparation can be realized.
Description
Technical Field
The invention belongs to the technical field of terahertz wave absorption, and particularly relates to a three-dimensional graphene/PDMS terahertz wave absorption material with a gradient aperture structure and a preparation method thereof.
Background
Terahertz (THz,1THz ═ 10)12Hz) wave refers to electromagnetic waves with a frequency of 0.1THz-10THz and a wavelength of 0.03mm-0.3 mm. In frequency, terahertz waves are between infrared and millimeter waves. In the electromagnetic spectrum, research on infrared technology and microwave technology has been very mature, but research on terahertz waves is still in progress and has not been sufficiently developed and applied. In recent years, with the rapid development of terahertz radiation sources and terahertz detectors, the development of terahertz technology is gradually accelerated, and the terahertz radiation source and the terahertz detector show significant scientific values in the fields of physics, biology, astronomy, national defense, mobile communication and the like. The absorption and energy capture of terahertz waves are the basis for realizing terahertz detection. With the increasingly complex electromagnetic radiation environment, new problems such as how to avoid radiation of terahertz waves to a human body, how to realize a stealth technology of the terahertz radar in military application, how to avoid interference of terahertz clutter to a system in complex electronic circuits and certain electronic components and the like gradually emerge. The terahertz wave-absorbing material just solves the problems provided above. The resonance type high-efficiency terahertz wave absorption can be realized by utilizing the electromagnetic metamaterial, but the terahertz wave absorption can only work in a narrow band at one or more frequency points, and has no good flexibility characteristic, and the preparation process is complex and is difficult to prepare in a large area. Therefore, a terahertz absorption material with high absorption, ultra-wideband, ultra-thin and flexibility is urgently needed at present.
Another possible method for realizing a terahertz absorber with high broadband and high absorption strength is to use a porous structure, and use the surface of the porous structure to have electromagnetic parameters similar to air, so that a large amount of terahertz waves can enter a sample and are lost and absorbed inside the sample. In 2018, the professor cheng yong of the university of southern development (z.huang, h.chen, y.huang, et al.ultra-Broadband Wide-Angle Terahertz Absorption Properties of 3D graphics Foam [ J ] Advanced Functional Materials,2018,28,1704363) reported that the Terahertz Absorption material based on the three-dimensional (3D) Graphene Foam realizes the Terahertz super-Absorption within the range of 0.2THz to 1.2THz, and the maximum reflection loss is as high as 19 dB. However, such porous 3D graphene foam has two problems: 1) the influence of the aperture on the absorption characteristic must be effectively balanced, and the incident of terahertz waves is blocked due to the excessively small aperture, so that the reflection on the surface of the material is enhanced, and the absorption capacity is reduced; the too large aperture leads to a reduction in the attenuation effect of the terahertz wave inside the material, so the thickness of the absorbing material has to be increased to improve the absorption rate. The existing 3D foam terahertz wave absorbing material has the advantages that due to the fact that the size of a single pore is adopted, the absorption efficiency and the thickness must be compromised, and the optimal material performance cannot be achieved; 2) the high-conductivity 3D graphene foam needs to be subjected to high-temperature annealing treatment at 1500 ℃, so that the foam is very fragile and has no flexible functions such as stretching, bending and pressure resistance, and the actual using effect of the foam is greatly limited. Therefore, a broadband terahertz absorbing material meeting the practical requirement is still an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a three-dimensional graphene/PDMS terahertz wave-absorbing material with a gradient aperture structure and a preparation method thereof, aiming at the defects in the background art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the terahertz wave-absorbing material with the gradient aperture structure is characterized by comprising three layers of three-dimensional graphene/PDMS composite materials; in the first layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 100-120 mu m; in the second layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 50-70 μm; in the third layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 20-40 μm.
Further, the first layer of three-dimensional graphene/PDMS composite material is obtained by soaking three-dimensional graphene in PDMS solution, curing and drying; the second layer of three-dimensional graphene/PDMS composite material is obtained by stretching the first layer of three-dimensional graphene/PDMS composite material and then removing the external force, wherein the stretching length is 2 times of the length of the first layer of three-dimensional graphene/PDMS composite material; the third layer of three-dimensional graphene/PDMS composite material is obtained by stretching the first layer of three-dimensional graphene/PDMS composite material and then removing the external force, wherein the stretching length is 3 times of the length of the first layer of three-dimensional graphene/PDMS composite material.
Further, the thicknesses of the first layer of three-dimensional graphene/PDMS composite material, the second layer of three-dimensional graphene/PDMS composite material and the third layer of three-dimensional graphene/PDMS composite material are all below 1 mm.
Further, the preparation process of the first layer of three-dimensional graphene/PDMS composite material specifically comprises: firstly, the volume ratio of (8-10): 1, taking a polydimethylsiloxane prepolymer and a curing agent according to the proportion, and uniformly stirring to obtain a PDMS solution; then, immersing the three-dimensional graphene into a PDMS solution, treating in a vacuum box at 19-25 ℃ until the pressure of the vacuum box is less than 0.08Pa, and taking out; finally, curing for 1 hour at the temperature of 90-100 ℃.
Further, ethyl acetate can be added into the PDMS solution, and the volume ratio of the ethyl acetate to the curing agent is (100-120): 1.
the invention provides a terahertz wave-absorbing material with a gradient aperture structure, which is composed of three layers of composite materials: the first layer is a composite material formed by combining three-dimensional graphene with the aperture of 100-120 mu m and PDMS; the second layer structure is the same as the first layer structure and is obtained by stretching the first layer structure and then removing the external force, the stretching length is 2 times of the length of the first layer structure, and the aperture of the three-dimensional graphene in the second layer structure is 50-70 mu m after the external force is removed; the third layer structure is the same as the first layer structure and is obtained by stretching the first layer structure and then removing the external force, the stretching length is 3 times of the length of the first layer structure, and the aperture of the three-dimensional graphene in the third layer structure is 20-40 mu m after the external force is removed. Due to the mechanical elasticity and inertia of the PDMS, after the PDMS recovers to the original state, the three-dimensional graphene pore diameters in the second layer and the third layer structure become small, the transmission of the terahertz wave is reduced, the multiple reflections of the terahertz wave in the terahertz wave are increased, and therefore the energy of the incident terahertz wave is further consumed, and the absorption rate of the terahertz wave becomes very high.
The invention provides a terahertz wave-absorbing material with a gradient aperture structure, which has the working principle that:
firstly, the aperture of three-dimensional graphene on the first layer of the terahertz wave absorbing material is 100-120 microns, the electromagnetic parameter of the three-dimensional graphene is close to that of air, the reflectivity of the surface of the three-dimensional graphene is very low, meanwhile, Polydimethylsiloxane (PDMS) in the terahertz wave absorbing material is almost transparent to terahertz waves, namely the transmissivity of the polydimethylsiloxane is close to 100%, and the reflection of the polydimethylsiloxane is very weak, so that the terahertz waves can enter the material almost without reflection; secondly, the aperture of the three-dimensional graphene in the terahertz wave absorbing material is sequentially reduced, so that terahertz waves are subjected to strong multiple reflection and loss in the material to form strong internal absorption; finally, the aperture of the lowest layer is very small, which can generate strong blocking effect on terahertz waves, and the transmission of the material is extremely low. Therefore, the terahertz wave-absorbing material has extremely low surface reflection, extremely low transmission and extremely high internal electromagnetic loss, and has an absorption rate of more than 93%. Wherein, all wave-absorbing materials satisfy the formula: the absorption rate is 1-transmittance-reflectance.
Compared with the prior art, the invention has the beneficial effects that:
the terahertz wave-absorbing material with the gradient aperture structure has extremely strong broadband terahertz wave absorption characteristic, and the average absorption rate in the ultra-wideband frequency spectrum range of 0.2-1.2THz is as high as more than 93%; the terahertz wave-absorbing material is extremely thin, the thickness of each layer is controlled within 1mm, the total thickness of the terahertz wave-absorbing material is within 3mm, and the terahertz wave-absorbing material is far superior to the existing terahertz wave-absorbing foam material; excellent flexibility characteristics such as bending, stretching and mechanical elasticity; the raw materials are low in price, the preparation method is simple, and large-area preparation can be realized.
Drawings
FIG. 1 is a schematic structural diagram of a terahertz wave-absorbing material with a gradient aperture structure provided by the invention; wherein, the black hexagon represents three-dimensional graphene, and the transparent square box represents Polydimethylsiloxane (PDMS);
FIG. 2 is a Scanning Electron Microscope (SEM) of the three-dimensional graphene obtained in step 2 of the example;
FIG. 3 is the transmittance of the terahertz wave absorbing material of the three-dimensional graphene/PDMS with the gradient aperture structure obtained in the embodiment to terahertz waves;
fig. 4 shows the reflectivity of the terahertz wave absorbing material of the three-dimensional graphene/PDMS with the gradient aperture structure obtained in the embodiment to the terahertz wave.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
As shown in fig. 1, the invention provides a schematic structural diagram of a terahertz wave-absorbing material with a gradient aperture structure; the terahertz wave-absorbing material comprises three layers of three-dimensional graphene/PDMS composite materials from top to bottom, and a first layer of three-dimensional graphene/PDMS composite material, a second layer of three-dimensional graphene/PDMS composite material and a third layer of three-dimensional graphene/PDMS composite material in sequence. In the three-layer three-dimensional graphene/PDMS composite material, the three-dimensional graphene has different apertures, and a gradient aperture structure from large to small is formed from top to bottom. The pore diameter range of the three-dimensional graphene on the uppermost layer is 100-120 mu m, the pore diameter range of the three-dimensional graphene on the middle layer is 50-70 mu m, and the pore diameter range of the three-dimensional graphene on the lowermost layer is 20-40 mu m. The three-dimensional graphene adopted in the terahertz wave-absorbing material is the same raw material, and the gradient aperture structures of different layers are formed in the preparation process by utilizing the strong elasticity of PDMS (polydimethylsiloxane), and the raw materials with different apertures are not required to be adopted.
Examples
Step 1, preparing three-dimensional graphene with a nickel substrate and an average pore size of 110 microns. The chemical deposition method adopting template guide comprises the following steps: taking foamed nickel as a deposition substrate, methane as a growth carbon source and a quartz tube furnace with the caliber of 100mm as growth equipment; putting the foamed nickel with the average pore diameter of 110 mu m into a tubular furnace, and introducing 10sccm methane as a growth gas for 30 min; after the completion, the methane gas is closed, and the temperature is naturally reduced to the room temperature.
And 2, preparing the three-dimensional graphene. Taking 10ml of Hydrogen Chloride (HCL) solution with the concentration of 2mol/L and ferric trichloride (FeCl) with the concentration of 2mol/L3) 10ml of solution, dissolving hydrogen chloride solution and ferric trichlorideMixing the solutions to obtain a mixed solution; putting the three-dimensional graphene with the nickel substrate obtained in the step 1 into the mixed solution, standing for 12 hours overnight, and removing metallic nickel; washing the obtained three-dimensional graphene in deionized water, and drying;
and 3, preparing the three-dimensional graphene/Polydimethylsiloxane (PDMS) terahertz wave-absorbing material with the gradient pore diameter structure. The Polydimethylsiloxane (PDMS) of this example was a silicone rubber type SYLAGARD 184 produced by Dow Corning Crop, USA, which included a PDMS prepolymer and a curing agent.
3.1 in order to make the prepared PDMS have good elasticity and flexibility, in the embodiment, 10ml of polydimethylsiloxane prepolymer and 1ml of curing agent are respectively taken, the prepolymer and the curing agent are fully stirred by a glass rod to be uniformly mixed, and then 100ml of ethyl acetate is added to obtain a PDMS solution;
3.2 soaking the three-dimensional graphene prepared in the step 2 in the PDMS solution obtained in the step 3.1, and then placing the three-dimensional graphene in a vacuum box to extract air in the PDMS solution, wherein the temperature of the vacuum box is kept at 19 ℃, and when the pressure of the vacuum box is less than 0.08Pa, a few bubbles are found on the surface of the sample, which indicates that the extraction of the air in the sample is completed;
3.3, placing the sample treated in the step 3.2 on a heating table, heating and curing for 1 hour in an environment of 90 ℃, then placing the sample in a dry environment for one day (24 hours), and completely eliminating bubbles on the surface of the sample to obtain a first layer of three-dimensional graphene/PDMS composite material;
3.4 preparing a structure which is the same as the first layer of three-dimensional graphene/PDMS composite material by adopting the processes from the step 3.1 to the step 3.3, then stretching the structure to be twice as long as the first layer of three-dimensional graphene/PDMS composite material, removing the external force, and restoring the original state to obtain a second layer of three-dimensional graphene/PDMS composite material, wherein the average pore diameter of the three-dimensional graphene in the second layer of structure is changed from 110 mu m to 60 mu m;
3.5 preparing a structure which is the same as the first layer of three-dimensional graphene/PDMS composite material by adopting the processes from the step 3.1 to the step 3.3, then stretching the structure to be three times as long as the first layer of three-dimensional graphene/PDMS composite material, removing the external force, and restoring the original state to obtain a third layer of three-dimensional graphene/PDMS composite material, wherein the average pore diameter of the three-dimensional graphene in the third layer of structure is changed from 110 mu m to 30 mu m;
3.6 sequentially adhering the first layer of three-dimensional graphene/PDMS composite material obtained in the step 3.3, the second layer of three-dimensional graphene/PDMS composite material obtained in the step 3.4 and the third layer of three-dimensional graphene/PDMS composite material obtained in the step 3.5 from top to bottom (the viscosity of PDMS is strong), curing for 1 hour in a heating box at 60 ℃, and then placing for one hour in a dry environment to obtain the terahertz wave-absorbing material of the three-dimensional graphene/Polydimethylsiloxane (PDMS) with the gradient pore size structure.
In the terahertz wave-absorbing material obtained in the embodiment, each layer structure is composed of a three-dimensional graphene/PDMS composite material in appearance, the three-dimensional graphene seems to grow in transparent Polydimethylsiloxane (PDMS), and the PDMS tightly wraps the three-dimensional graphene. The three-dimensional graphene is light in weight and weak in structure, but after the three-dimensional graphene is combined with PDMS, the three-dimensional graphene and the PDMS are mutually crosslinked, and the structure becomes relatively flexible; and the PDMS has hydrophobic property and stable chemical and physical properties, and can protect the structure of the three-dimensional graphene from being damaged by the outside.
FIG. 3 is the transmittance of the terahertz wave absorbing material of the three-dimensional graphene/PDMS with the gradient aperture structure obtained in the embodiment to terahertz waves; fig. 4 shows the reflectivity of the terahertz wave absorbing material of the three-dimensional graphene/PDMS with the gradient aperture structure obtained in the embodiment to the terahertz wave. As can be seen from fig. 3 and 4, the transmittance of the terahertz wave absorbing material obtained in the embodiment to terahertz waves is up to 8% in 0.2-1.2THz, and is as low as 2% at some terahertz frequency points, so that the average transmittance of the terahertz wave absorbing material with the aperture gradient structure to terahertz waves is 5%; the highest reflectivity of the terahertz wave absorbing material to terahertz waves is close to 4% within 0.2THz-1.2THz, and the reflectivity on certain terahertz frequency points is zero, so that the average reflectivity is 2%. Therefore, the average absorption rate of the terahertz wave absorbing material to terahertz waves is up to 93%, and the absorption rate of the terahertz wave absorbing material to terahertz waves on some terahertz frequency points is close to 98%. The effect is far better than the effect that the existing three-dimensional graphene absorbs terahertz independently.
According to the three-dimensional graphene/PDMS terahertz wave-absorbing material with the gradient aperture structure, due to the strong viscosity of PDMS, the terahertz wave-absorbing material can be adhered to the surface of an electronic component or clothes, so that the influence of terahertz clutter on an electronic system in a complex electromagnetic environment can be avoided, the human body can be hidden for terahertz waves, and terahertz radiation is avoided.
Claims (4)
1. The terahertz wave-absorbing material with the gradient aperture structure is characterized by comprising three layers of three-dimensional graphene/PDMS composite materials; in the first layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 100-120 mu m; in the second layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 50-70 μm; in the third layer of three-dimensional graphene/PDMS composite material, the aperture of the three-dimensional graphene is 20-40 μm; the first layer of three-dimensional graphene/PDMS composite material is obtained by soaking three-dimensional graphene in PDMS solution, curing and drying; the second layer of three-dimensional graphene/PDMS composite material is obtained by stretching the first layer of three-dimensional graphene/PDMS composite material and then removing the external force, wherein the stretching length is 2 times of the length of the first layer of three-dimensional graphene/PDMS composite material; the third layer of three-dimensional graphene/PDMS composite material is obtained by stretching the first layer of three-dimensional graphene/PDMS composite material and then removing the external force, wherein the stretching length is 3 times of the length of the first layer of three-dimensional graphene/PDMS composite material.
2. The terahertz wave-absorbing material with the gradient aperture structure of claim 1, wherein the thicknesses of the first layer of three-dimensional graphene/PDMS composite material, the second layer of three-dimensional graphene/PDMS composite material and the third layer of three-dimensional graphene/PDMS composite material are all below 1 mm.
3. The terahertz wave-absorbing material with the gradient aperture structure according to claim 1, wherein the preparation process of the first layer of the three-dimensional graphene/PDMS composite material is as follows: firstly, the volume ratio of (8-10): 1, taking a polydimethylsiloxane prepolymer and a curing agent according to the proportion, and uniformly stirring to obtain a PDMS solution; then, immersing the three-dimensional graphene into a PDMS solution, treating in a vacuum box at 19-25 ℃ until the pressure of the vacuum box is less than 0.08Pa, and taking out; finally, curing for 1 hour at the temperature of 90-100 ℃.
4. The terahertz wave-absorbing material with the gradient aperture structure of claim 3, wherein ethyl acetate is added into the PDMS solution, and the volume ratio of the ethyl acetate to the curing agent is (100-120): 1.
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