CN113683075A - Sulfur-doped porous nano carbon electromagnetic wave absorption material and preparation method thereof - Google Patents
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The sulfur-doped porous nano-carbon electromagnetic wave absorption material is black powder and is formed by agglomerating a plurality of nano-carbon particles through electrostatic action, the nano-carbon particles are spherical particles with the diameter of 210-230 nm, the surfaces of the nano-carbon particles are provided with a plurality of micropores formed by hydrogen peroxide etching, functional groups at the defect positions of the edges of the micropores are combined with sulfur elements in a covalent bond mode, the surfaces of the nano-carbon particles are adsorbed with the sulfur elements through electronegativity, and the content of the sulfur elements is 0.5% -5% of the total mass of the material. The preparation method comprises the steps of firstly preparing nano carbon, then carrying out co-heat treatment on the nano carbon and hydrogen peroxide to obtain porous nano carbon, and then mixing and calcining the porous nano carbon and thioacetamide. The sulfur element in the material is doped with the nano carbon particles in two forms of covalent bond combination and electronegativity adsorption, so that the material has the advantages of wider effective absorption frequency bandwidth, higher electromagnetic absorption strength, strong chemical stability, excellent microwave absorption performance, low preparation process cost and simple process.
Description
Technical Field
The invention relates to the field of electromagnetic wave absorbing materials, in particular to a sulfur-doped porous nanocarbon electromagnetic wave absorbing material and a preparation method thereof.
Background
With the development of electromagnetic technology, electromagnetic stealth is more and more widely applied in the industrial and military fields, the demand for electromagnetic wave absorbing materials is increasing, graphitized carbon-based materials have attracted extensive attention of researchers due to the lower density, excellent dielectric properties, and environment-friendly characteristics, and a great amount of reports have been made on various types of nano-sized microwave absorbing materials. The development of various existing carbon-based materials mainly focuses on the nanostructure design and specific element introduction function, and is mainly characterized in that on one hand, the hollow carbon material is adopted to obtain lower density and more excellent electromagnetic absorption performance than the solid material of the same type, for example, the Xuhailong subject group of the university of northwest industry, the electromagnetic absorption performance of the hollow red cell carbon sphere prepared by the template method is about 80% higher than that of the solid carbon sphere, and the maximum effective absorption bandwidth of a sample in a measured frequency band (2-18 GHz) can reach 3.0 GHz; on the other hand, the introduction of the pore structure into the carbon material can effectively improve the electromagnetic wave absorption performance of the material, for example, the group of subjects of the university of aerospace of Nanjing was developed, the honeycomb-shaped nanoporous biomass carbon was synthesized from flour, and the introduction of the pore structure can improve the effective absorption bandwidth of the material to 4.8 GHz.
However, the prior art still has a plurality of problems: 1. the existing nano-sized carbon-based material is difficult to ensure the regular appearance of the product, so that the improvement of the material performance is limited to a certain extent; 2. the carbon material having pores on the surface has a lower conductivity than the carbon material having no pores, and the dielectric loss capacity is impaired. The introduction of sulfur element can balance electromagnetic parameters of the material and improve the electromagnetic absorption performance, so that the preparation and development of the sulfur-doped porous nanocarbon electromagnetic wave absorption material with a simple process and a regular product appearance and uniform size are very necessary.
Disclosure of Invention
The invention aims to provide a sulfur-doped porous nanocarbon electromagnetic wave absorbing material and a preparation method thereof, which overcome the defects that the conventional nanocarbon electromagnetic wave absorbing material is difficult to ensure the product appearance and has weak dielectric loss capacity.
The technical scheme adopted by the invention for solving the technical problems is as follows: a sulfur-doped porous nano-carbon electromagnetic wave absorption material is black powder and is formed by agglomeration of a plurality of nano-carbon particles through electrostatic interaction, the nano-carbon particles are spherical particles with the diameter of 210-230 nm, the surfaces of the nano-carbon particles are provided with a plurality of micropores formed by hydrogen peroxide etching, functional groups at defect positions on the edges of the micropores are combined with sulfur elements in a covalent bond mode, the surfaces of the nano-carbon particles are adsorbed with the sulfur elements through electronegativity, and the content of the sulfur elements is 0.5% -5% of the total mass of the material.
The preparation method of the sulfur-doped porous nanocarbon electromagnetic wave absorption material comprises the following steps:
and 3, mixing the porous nano carbon material obtained in the step 2 and thioacetamide according to the mass ratio of 1: 0.5-1: 2, heating to 200-300 ℃ at the heating rate of 2-5 ℃/min for pre-sintering, wherein the pre-sintering time is 10-20 min, heating to 500-700 ℃ at the heating rate of 2-5 ℃/min for calcining for 1-2 h, and cooling to obtain the sulfur-doped porous nano carbon electromagnetic wave absorbing material.
Preferably, in step 1, the temperature of the high-temperature carbonization treatment is 700 ℃.
According to the technical scheme, the invention has the beneficial effects that:
the sulfur-doped porous nanocarbon electromagnetic wave absorbing material provided by the invention has the advantages that the size of nanoparticles is uniform, the morphology is regular, sulfur elements are doped with the nanocarbon particles in two forms of covalent bond combination and electronegativity adsorption, the chemical stability is strong, the sulfur-doped porous nanocarbon electromagnetic wave absorbing material has wider effective absorption frequency bandwidth and higher electromagnetic absorption strength under ultralow filling degree and low thickness as an electromagnetic wave absorbent, the sulfur-doped porous nanocarbon electromagnetic wave absorbing material has excellent microwave absorption performance, no virulent organic solvent is adopted in the preparation process of the sulfur-doped porous nanocarbon electromagnetic wave absorbing material, the cost is low, the process is simple, the sulfur-doped porous nanocarbon electromagnetic wave absorbing material can be used for large-scale industrial production, the carbon-based material has excellent weather resistance, the sulfur-doped porous nanocarbon electromagnetic wave absorbing material can be applied to electromagnetic protection of various civil devices under the normal temperature condition, the application market is wide, and the economic prospect is wide.
Drawings
Fig. 1 is an X-ray diffraction pattern of sulfur-doped porous nanocarbon;
FIG. 2 is an element characteristic diagram of sulfur-doped porous nanocarbon C;
FIG. 3 is a diagram of elemental species for sulfur-doped porous nanocarbon;
FIG. 4 is a scanning electron microscope image of sulfur-doped porous nanocarbon C
FIG. 5 is a photograph of an infrared absorption spectrum of sulfur-doped porous nanocarbon;
FIG. 6 is a photograph of electromagnetic parameters of sulfur-doped porous nanocarbon;
fig. 7 is a reflection loss picture of sulfur-doped porous nanocarbon a;
fig. 8 is a reflection loss picture of sulfur-doped porous nanocarbon B;
fig. 9 is a reflection loss picture of sulfur-doped porous nanocarbon C;
fig. 10 is a selected thickness reflection loss picture of sulfur-doped porous nanocarbon C.
Detailed Description
A sulfur-doped porous nano-carbon electromagnetic wave absorption material is black powder and is formed by agglomeration of a plurality of nano-carbon particles through electrostatic interaction, the nano-carbon particles are spherical particles with the diameter of 210-230 nm, the surfaces of the nano-carbon particles are provided with a plurality of micropores formed by hydrogen peroxide etching, functional groups at defect positions on the edges of the micropores are combined with sulfur elements in a covalent bond mode, the surfaces of the nano-carbon particles are adsorbed with the sulfur elements through electronegativity, and the content of the sulfur elements is 0.5% -5% of the total mass of the material.
The preparation method of the sulfur-doped porous nanocarbon electromagnetic wave absorption material comprises the following steps:
And 2, uniformly mixing the nano carbon material obtained in the step 1 with 100-500 ml of hydrogen peroxide, and then carrying out co-heat treatment to obtain the porous nano carbon material.
And 3, mixing the porous nano carbon material obtained in the step 2 and thioacetamide according to the mass ratio of 1: 0.5-1: 2, heating to 200-300 ℃ at the heating rate of 2-5 ℃/min for pre-sintering, wherein the pre-sintering time is 10-20 min, heating to 500-700 ℃ at the heating rate of 2-5 ℃/min for calcining for 1-2 h, and cooling to obtain the sulfur-doped porous nano carbon electromagnetic wave absorbing material.
Example 1
The sulfur-doped porous nano carbon electromagnetic wave absorption material and the preparation method thereof comprise the following steps:
And 2, carrying out co-heat treatment on the nano-carbon obtained in the step 1 and hydrogen peroxide to obtain porous nano-carbon.
And 3, weighing 100mg of the porous nano carbon material obtained in the step 2, weighing 50mg of thioacetamide according to the mass ratio of 1:0.5, mixing the porous carbon material and the thioacetamide, grinding the mixture for 20 minutes until the mixture is uniform, transferring the mixture into a crucible, covering the crucible, sealing the whole crucible by using tinfoil, placing a container in a tubular furnace, introducing nitrogen for protection, setting the program, firstly heating to 200 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for ten minutes, then heating to 600 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for 2 hours, and naturally cooling to obtain black powdery sulfur-doped porous nano carbon A.
Example 2
And 3, weighing 100mg of the porous nano carbon material obtained in the step 1, weighing 100mg of thioacetamide according to the mass ratio of 1: 1, mixing and grinding the porous nano carbon material and the thioacetamide uniformly, transferring the mixture into a crucible, covering and sealing the crucible integrally by using tinfoil, placing a container into a tubular furnace, introducing nitrogen for protection, setting a program, heating to 200 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for ten minutes, heating to 600 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for 2 hours, and naturally cooling to obtain black powdery sulfur-doped porous nano carbon B.
Example 3
And 3, weighing 100mg of the porous nano carbon material obtained in the step 1, weighing 200mg of thioacetamide according to the mass ratio of 1: 1, mixing and grinding the porous nano carbon material and the thioacetamide uniformly, transferring the mixture into a crucible, covering and sealing the crucible integrally by using tinfoil, placing a container into a tubular furnace, introducing nitrogen for protection, setting a program, heating to 200 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for ten minutes, heating to 600 ℃ at the heating rate of 2-5 ℃/min, keeping the temperature for 2 hours, and naturally cooling to obtain black powdery sulfur-doped porous nano carbon C.
The powder samples synthesized in examples 1-3 were mixed with paraffin wax in a ratio of 5: 95 and pressed into a ring with an inner diameter of 3.04mm and an outer diameter of 7.00mm, and subjected to electromagnetic parameter testing using a vector network analyzer, and reflection loss performance parameters were obtained by calculation, wherein the sulfur-doped porous nanocarbon of example 3 had the best electromagnetic absorption performance, exhibited excellent electromagnetic absorption performance at a filling ratio as low as 5wt%, and had a minimum reflection loss value of-57 dB, while the effective absorption bandwidth exceeded 6 GHz at a sample thickness of less than 2 mm.
In examples 1 to 3, sulfur element doping is realized by a carbon sphere prepared by a template method and thioacetamide in a high-temperature treatment manner, and the results of X-ray diffraction characterization show that the synthesized sulfur-doped porous nanocarbon with different doping amounts has similar diffraction peaks, and two obvious diffraction peaks are present in the measured range, wherein the two diffraction peaks are respectively (002) and (101) crystal faces corresponding to a carbon material, as shown in fig. 1.
According to the preparation principle of the sulfur-doped porous nanocarbon electromagnetic wave absorption material, a large number of unsaturated bonds exist on the surface of a porous nanocarbon material prepared by a template etching method, thioacetamide is used as a sulfur source, the thioacetamide is decomposed at high temperature, sulfur elements are captured and fixed by the carbon material in a covalent bond mode in a closed environment, the amount of doped sulfur can be regulated and controlled by changing the using amount of the thioacetamide, the introduction of the sulfur elements can improve impedance matching of the material, and dielectric loss performance is greatly improved. The results of the element characteristic test of the sulfur-doped porous nanocarbon C shown in fig. 2 can be seen from the curves that the elements contained in the material comprise C, O, S, and the results of the element content analysis of the sulfur-doped porous nanocarbon shown in fig. 3 show that the sulfur element content in the sulfur-doped porous nanocarbons prepared in examples 1 to 3 is 0.52wt%, 1.2wt%, and 2.16wt%, respectively, while the contents of carbon element and oxygen element in the material are also shown in the curves shown in fig. 3, thus proving the successful introduction of sulfur element.
The sulfur-doped porous nanocarbon electromagnetic wave absorption material is used for synthesizing porous nanocarbon by a template etching method, and sulfur elements are doped by utilizing high-temperature co-heating. In the sulfur-doped porous nanocarbon electromagnetic wave absorption material, the influence of a pore structure in the material on electromagnetic parameters can be regulated and controlled by the doping and content control of sulfur, the dielectric loss is enhanced while impedance matching is balanced, so that the material can show excellent electromagnetic absorption performance when the filling ratio is as low as 5wt%, the minimum reflection loss value can reach-57 dB, and meanwhile, the effective absorption bandwidth can exceed 6 GHz when the thickness of a sample is lower than 2 mm.
The electromagnetic wave absorption performance of the sulfur-doped porous nanocarbon electromagnetic wave absorption material mainly derives from dielectric loss of a carbon material and dipole polarization caused by sulfur element doping, and impedance matching and attenuation performance of the material are balanced through sulfur doping regulation and control, so that the electromagnetic wave attenuation capability of the material is improved. The ultralow density and low filling ratio of the porous material can reduce the production cost of the material in practical application, and can be produced in a large scale to meet the application requirements.
The sulfur-doped porous nanocarbon electromagnetic wave absorbing material of the invention is used as a nano absorbent, has relatively uniform appearance, for example, fig. 4 is a scanning electron microscope picture of sulfur-doped porous nanocarbon C, as can be seen from fig. 4, the size of a single particle of the sulfur-doped porous nanocarbon C is 210nm-230nm, micropores are randomly distributed on the surface of a spherical shell, and the larger broken pores on the surface of a sphere can still basically maintain the spherical structure due to the effect of template etching on the structure.
In the sulfur-doped porous nanocarbon electromagnetic wave absorption material, part of sulfur elements are combined with nanocarbon in the form of chemical bonds, such as the infrared absorption spectrum of the sulfur-doped porous nanocarbon shown in fig. 5, wherein the S-C, S-O bond stretching vibration absorption peak appears at 700cm-1On the left and right, the S = O bond stretching vibration absorption peak appears at 1050cm-1On the left and right sides, the sulfur element is fixed in a chemical bond form instead of being physically mixed, so that the sulfur-doped porous nanocarbon electromagnetic wave absorption material synthesized by the method has certain chemical stability.
According to the sulfur-doped porous nanocarbon electromagnetic wave absorption material, by regulating the doping amount of sulfur element, along with the increase of the doping amount of sulfur, the real part and the imaginary part of the electromagnetic parameter of a corresponding sample are increased, as shown in fig. 6, and the change of the parameters causes the change of the electromagnetic absorption performance, as shown in reflection loss maps of fig. 7, 8 and 9, the minimum reflection loss of the sample does not exceed-10 dB under the condition of low thickness of the sulfur-doped porous nanocarbon A. Under the condition that the filling proportion is 5wt%, the matching thickness of the sulfur-doped porous nano carbon B is 1.95 mm, the effective absorption frequency bandwidth is 2.6 GHz when the frequency is 16 GHz, and the absorption frequency band range corresponds to 15.4-18 GHz. Under the condition that the filling proportion is 5wt%, the matching thickness of the sulfur-doped porous nano carbon C is 1.95 mm, the effective absorption frequency bandwidth is 6.3 GHz, and the absorption frequency band range corresponds to 11.7-18.0 GHz.
The sulfur-doped porous nanocarbon electromagnetic wave absorbing material of the invention finally obtains a sample with the best relative performance under the system through the adjustment and control of the doping amount, as shown in a reflection loss map under the selected thickness of the sulfur-doped porous nanocarbon C shown in fig. 10, under the condition that the filling proportion is 5wt%, the matching thickness is 2.2 mm, and the frequency is 12.5 GHz, the minimum reflection loss can reach-57 dB. The sample with the doping amount has the widest corresponding effective absorption bandwidth, so that the sample has the best electromagnetic absorption performance.
Claims (3)
1. A sulfur-doped porous nanocarbon electromagnetic wave absorbing material is characterized in that: the material is black powder and is formed by agglomeration of a plurality of nano-carbon particles through electrostatic action, the nano-carbon particles are spherical particles with the diameter of 210-230 nm, the surfaces of the nano-carbon particles are provided with a plurality of micropores formed by hydrogen peroxide etching, functional groups at the defect positions of the edges of the micropores are combined with sulfur elements in a covalent bond mode, the surfaces of the nano-carbon particles are adsorbed with the sulfur elements through electronegativity, and the content of the sulfur elements is 0.5-5% of the total mass of the material.
2. The method for preparing the sulfur-doped porous nanocarbon electromagnetic wave absorption material as claimed in claim 1, characterized by comprising the following steps:
step 1, placing nano SiO2Adding 500-1000 ml of ethanol, 20-50 ml of formaldehyde and 2-4 g of resorcinol into the container, adding a proper amount of ammonia water to adjust the mixed solution to be alkaline, stirring at a constant speed for reacting for 18-24 h, then carrying out centrifugal separation, carrying out high-temperature carbonization treatment on the powder obtained by centrifugal separation under the protection of nitrogen, and then using sodium hydroxide solution to etch and remove nano SiO2Obtaining the nano carbon material with the particle diameter of 210-230 nm;
step 2, uniformly mixing the nano carbon material obtained in the step 1 with 100-500 ml of hydrogen peroxide, and then carrying out co-heat treatment to obtain a porous nano carbon material;
and 3, mixing the porous nano carbon material obtained in the step 2 and thioacetamide according to the mass ratio of 1: 0.5-1: 2, heating to 200-300 ℃ at the heating rate of 2-5 ℃/min for pre-sintering, wherein the pre-sintering time is 10-20 min, heating to 500-700 ℃ at the heating rate of 2-5 ℃/min for calcining for 1-2 h, and cooling to obtain the sulfur-doped porous nano carbon electromagnetic wave absorbing material.
3. The method for preparing the sulfur-doped porous nanocarbon electromagnetic wave absorption material according to claim 2, wherein the method comprises the following steps: in step 1, the temperature of the high-temperature carbonization treatment is 700 ℃.
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