CN118185571A - One-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and preparation method thereof - Google Patents
One-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and a preparation method thereof. A preparation method of one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material comprises the following steps; s1, accurately dissolving boric acid and urea in 100mL of deionized water, and magnetically stirring to obtain a mixed solution. S2, adding polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a mixed solution. S3, adding nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a mixed solution. S4, placing the obtained uniform mixed solution in a constant temperature box, and drying. S5, placing the obtained solid mixture in a tube furnace, and calcining for 4 hours under the protection of nitrogen atmosphere. S6, cooling to room temperature along with the furnace after heat preservation is finished. The invention has simple process, good repeatability, low cost, continuous production and environmental protection.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and a preparation method thereof.
Background
Stealth technology is a necessary means for improving the survivability, the outburst prevention capability and the comprehensive tactical efficacy of weapon equipment in modern informatization war. The core for improving stealth performance is to develop a novel wave-absorbing material with strong absorption, wide frequency band, low density, high temperature resistance and good stability. The high Mach number aircraft has higher requirements on the light weight, high efficiency, high temperature resistance and stability of the wave absorbing material, so that the traditional single-component wave absorbing material is difficult to meet the wave absorbing requirements. The carbon material (nano carbon fiber, carbon nano tube, graphene and the like) or modified carbon material (BCN, C/SiC, siBCN and the like) with low density, high porosity and excellent electrical property and magnetic material (Fe 3O4, fe, co, ni and other metal oxides or simple substances) are doped, compositely optimized, and the preparation of the composite wave-absorbing material with the multiple loss mechanism is one of effective ways for exploring novel wave-absorbing materials.
The low-dimensional carbon material (carbon nanofibers, carbon nanotubes, graphene, etc.) has unique advantages as an electrically-lossy wave-absorbing material, such as: the light-weight and excellent electrical, mechanical and magnetic properties are the wave-absorbing carrier materials which are relatively concentrated in the current research. The synthesis of representative low-dimensional carbon material wave absorbers reported at home and abroad has developed various viable strategies such as controlling material composition (addition of magnetic components including metals, alloys and carbides), and design of material structure (e.g., rods, core shells, cladding structures, nanotubes and hollow structures). In particular, a magnetic material having excellent magnetic permeability is expected to realize excellent electromagnetic dissipation in a low frequency band due to its excellent magnetic loss attenuation capability. The Ni-based nanocomposite material exhibits a remarkable electromagnetic attenuation capability in the magnetic absorber due to its high saturation magnetization and strong anisotropy field. However, the individual use of magnetic nanoparticles in absorbers has a number of disadvantages, such as the difficulty in practical applications in meeting the light weight, strong absorption and broad frequency characteristics required for good electromagnetic wave absorbing materials.
Therefore, in order to solve the above technical problems, it is necessary to provide a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and a preparation method thereof.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and a preparation method thereof, wherein magnetic nano particles in the one-dimensional C (B/N) nanotube, graphite carbon and doping agents of atoms B and N can generate dipole and interface polarization by the synergistic effect, so that dielectric loss is improved.
In order to achieve the above objective, a specific embodiment of the present invention provides a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and a preparation method thereof, wherein the one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material includes boric acid, urea, nickel nitrate hexahydrate and polyethylene glycol.
In one or more embodiments of the invention, the nickel nitrate hexahydrate is 0.11 to 0.26g, the boric acid is 0.2 to 0.5g, the urea is 6 to 20g, and the polyethylene glycol is 0.7 to 1.6g.
In one or more embodiments of the invention, the nickel nitrate hexahydrate is 0.195g, the boric acid is 0.3g, the urea is 10g, and the polyethylene glycol is 1g.
A preparation method of a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material comprises the following steps of;
S1, accurately weighing corresponding amounts of boric acid and urea, dissolving the boric acid and the urea in 100mL of deionized water at room temperature, and magnetically stirring the solution for 1 hour to obtain a uniform mixed solution.
S2, adding a corresponding amount of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S3, adding a corresponding amount of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S4, placing the obtained uniform mixed solution into a constant temperature box, and drying for 24 hours to obtain a dried C (B/N) precursor.
S5, placing the solid mixture obtained after drying in the step S4 in a tube furnace, placing the solid mixture in the protection of nitrogen atmosphere, setting the temperature to 900 ℃, and calcining for 4 hours.
S6, cooling to room temperature along with the furnace after heat preservation is finished, and finally obtaining the one-dimensional C (B/N) nanotube.
In one or more embodiments of the present invention, boric acid is added in the step S1 in an amount of 0.3g and urea in an amount of 10g.
In one or more embodiments of the present invention, the polyethylene glycol added in the step S2 is 1.0g, and the nickel nitrate hexahydrate added in the step S3 is 0.13g.
In one or more embodiments of the present invention, when the drying process is performed using the oven in the step S3, the oven is set to a temperature of 80 ℃.
In one or more embodiments of the present invention, the heating rate in the step S5 is 5 ℃/min.
In one or more embodiments of the present invention, the morphology diameter of the one-dimensional C (B/N) nanotube composite wave-absorbing material modified by the magnetic nanoparticles is 100nm.
In one or more embodiments of the present invention, the one-dimensional C (B/N) nanotube has magnetic nanoparticles supported thereon, the magnetic nanoparticles having a diameter of 40nm.
In one or more embodiments of the present invention, the magnetic Ni nanoparticles in the composite material are uniformly dispersed in one-dimensional C (B/N) nanotubes.
Compared with the prior art, the one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof have the following benefits;
1) The synergy between the magnetic nanoparticles in the one-dimensional C (B/N) nanotubes, graphitic carbon, and the atomic B and N dopants can create dipoles and interfacial polarization, improving dielectric losses.
2) Meanwhile, the co-doped B and N atoms in the one-dimensional C (B/N) nanotube not only promote the dispersion of the magnetic nano particles, but also regulate and control the impedance matching, thereby enhancing the electromagnetic wave absorption performance.
3) The preparation process has good repeatability, light weight, low cost, environmental friendliness, cleanness and no toxicity, is easy for mass production, and the synthesized one-dimensional nanotube structure is favorable for electromagnetic wave absorption, so that the preparation process is an ideal electromagnetic wave absorbing material which can be practically applied.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a SEM photograph of a one-dimensional C (B/N) nanotube sample;
FIG. 2 is a SEM photograph of a one-dimensional C (B/N) nanotube sample II;
FIG. 3 is a TEM image I of a one-dimensional C (B/N) nanotube sample modified with magnetic Ni nanoparticles;
FIG. 4 is a TEM image II of a one-dimensional C (B/N) nanotube sample modified with magnetic Ni nanoparticles;
FIG. 5 is a graph of the reflection loss of a one-dimensional C (B/N) nanotube sample;
FIG. 6 is a graph of minimum reflection loss for different thicknesses of a sample of modified one-dimensional C (B/N) nanotubes with a magnetic Ni nanoparticle content of 0.13 g;
FIG. 7 is a graph of minimum reflection loss for different thicknesses of a modified one-dimensional C (B/N) nanotube sample with a magnetic Ni nanoparticle content of 0.195 g;
FIG. 8 is a graph of minimum reflection loss for different thicknesses of a sample of modified one-dimensional C (B/N) nanotubes with a magnetic Ni nanoparticle content of 0.26 g;
FIG. 9 is a graph of Effective Absorption Bandwidth (EAB) for different thicknesses of modified one-dimensional C (B/N) nanotube samples with a magnetic Ni nanoparticle content of 0.195 g.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
As shown in FIGS. 1 to 4, a one-dimensional C (B/N) nanotube composite electromagnetic wave absorbing material in an embodiment of the invention comprises boric acid, urea, nickel nitrate hexahydrate and polyethylene glycol.
Further, nickel nitrate hexahydrate 0.11-0.26g, boric acid 0.2-0.5g, urea 6-20g, and polyethylene glycol 0.7-1.6g.
Preferably, the nickel nitrate hexahydrate is 0.195g, the boric acid is 0.3g, the urea is 10g, and the polyethylene glycol is 1g.
A preparation method of a one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material comprises the following steps of;
S1, accurately weighing corresponding amounts of boric acid and urea, dissolving the boric acid and the urea in 100mL of deionized water at room temperature, and magnetically stirring the solution for 1 hour to obtain a uniform mixed solution.
Preferably, boric acid is added in an amount of 0.3g and urea in an amount of 10g.
S2, adding a corresponding amount of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
Preferably, the polyethylene glycol is added at 1.0g.
S3, adding a corresponding amount of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
Preferably, the nickel nitrate hexahydrate is added at 0.13g.
S4, placing the obtained uniform mixed solution in an incubator, setting the temperature of the incubator to 80 ℃ for drying treatment for 24 hours, and obtaining the dried C (B/N) precursor.
S5, placing the solid mixture obtained after drying in the step S4 in a tube furnace, placing the solid mixture under the protection of nitrogen atmosphere, setting the temperature to 900 ℃, and calcining for 4 hours, wherein the heating rate is 5 ℃/min.
S6, cooling to room temperature along with the furnace after heat preservation is finished, and finally obtaining the one-dimensional C (B/N) nanotube.
The magnetic nano particle modified one-dimensional C (B/N) nanotube composite wave-absorbing material has a morphology diameter of 100nm. The one-dimensional C (B/N) nanotube is loaded with magnetic nano particles, and the diameter of the magnetic nano particles is 40nm. The magnetic Ni nano particles in the composite material are uniformly dispersed in the one-dimensional C (B/N) nano tube.
The invention uses light electromagnetic wave-absorbing stealth material as application background, adopts thermal cracking and nano magnetic particle modification technology to prepare one-dimensional C (B/N) nanotube composite wave-absorbing material, and the wave-absorbing material has multiple loss mechanism. The electronegativity of nitrogen (N) and boron (B) in one-dimensional C (B/N) nanotubes is opposite to that of carbon (C), thereby forming dipole polarization. In addition, the synergistic interaction between the magnetic nanoparticles, graphitic carbon, and the dopants for atoms B and N can create dipoles and interfacial polarizations, improve dielectric losses, and can effectively convert electromagnetic energy into thermal energy. Meanwhile, the co-doped B and N atoms in the one-dimensional C (B/N) nanotube not only promote the dispersion of the magnetic nano particles, but also regulate and control the impedance matching, thereby enhancing the electromagnetic wave absorption performance.
The chemicals used in the invention, such as boric acid, urea, nickel (II) nitrate hexahydrate (nickel nitrate hexahydrate) and polyethylene glycol, are all analytically pure; the instruments and equipment used are those commonly used in the laboratory.
Example 1
S1, dissolving 0.3g of boric acid and 10g of urea in 100mL of deionized water at room temperature, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S2, adding 1.0g of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S3, placing the obtained uniform mixed solution in an incubator, adjusting the temperature to 80 ℃, and drying for 24 hours. Calcining the obtained solid mixture for 4 hours at 900 ℃ under the protection of nitrogen, wherein the heating rate is 5 ℃ per minute, and finally obtaining the one-dimensional C (B/N) nanotube sample.
S4, mixing and pressing the prepared one-dimensional C (B/N) nanotube sample and paraffin according to the mass ratio of 1:9 to obtain round samples with different thicknesses and with the outer diameter of 7.0mm and the inner diameter of 3.04 mm.
S5, electromagnetic parameters (dielectric constant, dielectric loss, magnetic conductivity and magnetic loss) are measured by using AgilentN5245A vector network analyzer of Angilen electronic instruments limited company in the frequency range of 2-18 GHz. Finally, the reflection loss is calculated.
As shown in FIG. 5, it was finally found through experiments that the reflection loss value at 7.36GHz was-3.9 dB when the thickness of the current one-dimensional C (B/N) nanotube was 6 mm.
Example 2
S1, dissolving 0.3g of boric acid and 10g of urea in 100mL of deionized water at room temperature, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S2, adding 1.0g of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S3, adding 0.13g of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S4, placing the obtained uniform mixed solution in an incubator, adjusting the temperature to 80 ℃, and drying for 24 hours. Calcining the obtained solid mixture for 4 hours at 900 ℃ under the protection of nitrogen, wherein the heating rate is 5 ℃/min, and finally obtaining the one-dimensional C (B/N) nanotube sample.
S5, mixing the prepared one-dimensional C (B/N) nanotube sample with paraffin according to the mass ratio of 1:9 to prepare annular samples with different thicknesses.
S6, electromagnetic parameters (dielectric constant, dielectric loss, magnetic permeability and magnetic loss) are measured in the frequency range of 2-18GHz by using a AgilentN5245A vector network analyzer of An Jilun electronic instruments, inc., and then reflection loss is calculated.
As shown in FIG. 6, it is finally found through experiments that the reflection loss value of the one-dimensional C (B/N) nanotube at 8.0GHz is-40.1 dB when the thickness of the one-dimensional C (B/N) nanotube is 6mm, and the effective absorption bandwidth of the one-dimensional C (B/N) nanotube is 5.6GHz when the thickness of the one-dimensional C (B/N) nanotube is 6.0 mm.
Example 3
S1, dissolving 0.3g of boric acid and 10g of urea in 100mL of deionized water at room temperature, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S2, adding 1.0g of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S3, adding 0.195g of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S4, placing the obtained uniform mixed solution in a constant temperature box, adjusting the temperature to 80 ℃, and drying for 24 hours. Calcining the obtained solid mixture for 4 hours at 900 ℃ under the protection of nitrogen, wherein the heating rate is 5 ℃/min, and finally obtaining the one-dimensional C (B/N) nanotube sample.
S5, mixing the prepared one-dimensional C (B/N) nanotube sample with paraffin according to the mass ratio of 1:9, and pressing the mixture into annular samples with different thicknesses.
S6, electromagnetic parameters (dielectric constant, dielectric loss, magnetic permeability and magnetic loss) are measured in the frequency range of 2-18GHz by using a AgilentN5245A vector network analyzer of An Jilun electronic instruments, inc., and then reflection loss is calculated.
As shown in FIG. 7, it was finally found from the test that the reflection loss value at 8.24GHz was-56.9 dB when the thickness of the one-dimensional C (B/N) nanotube was 5.69 mm. When the thickness of the one-dimensional C (B/N) nanotube is 5.69mm, the effective absorption bandwidth covering the entire C band is 7.12GHz. The effective absorption bandwidth coverage was 3.1GHz and 3.74GHz when the thickness of the one-dimensional C (B/N) nanotubes was 2.78mm and 2.93 mm.
Example 4
S1, dissolving 0.3g of boric acid and 10g of urea in 100mL of deionized water at room temperature, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S2, adding 1.0g of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S3, adding 0.26g of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution.
S4, placing the obtained uniform mixed solution in a constant temperature box, adjusting the temperature to 80 ℃, and drying for 24 hours. Calcining the obtained solid mixture for 4 hours at 900 ℃ under the protection of nitrogen, wherein the heating rate is 5 ℃/min, and finally obtaining the one-dimensional C (B/N) nanotube sample.
S5, mixing the prepared one-dimensional C (B/N) nanotube sample with paraffin according to the mass ratio of 1:9, and pressing the mixture into annular samples with different thicknesses.
S6, electromagnetic parameters (dielectric constant, dielectric loss, magnetic permeability and magnetic loss) are measured in the frequency range of 2-18GHz by using a AgilentN5245A vector network analyzer of An Jilun electronic instruments, inc., and then reflection loss is calculated.
As shown in FIGS. 6 to 7, it was finally found through experiments that the reflection loss value at 7.44GHz was-34.9 dB when the thickness of the one-dimensional C (B/N) nanotube was 5.1mm, and the effective absorption bandwidth was 6.4GHz when the thickness of the one-dimensional C (B/N) nanotube was 6.0 mm.
Therefore, the application adopts a novel process for synthesizing the light element doped C (B/N) nanotube under normal pressure by adopting a molecular design method. The method breaks through the conventional thought of preparing the low-dimensional carbon-based wave-absorbing material (carbon nano tube, nano carbon fiber, graphene and the like), and establishes a new thought of B, N-doped novel light-weight high-temperature-resistant wave-absorbing material. The synergy between the magnetic nanoparticles in the one-dimensional C (B/N) nanotubes, graphitic carbon, and the atomic B and N dopants can create dipoles and interfacial polarization, improve dielectric losses, and. Meanwhile, the co-doped B and N atoms in the one-dimensional C (B/N) nanotube not only promote the dispersion of the magnetic nano particles, but also regulate and control the impedance matching, thereby enhancing the electromagnetic wave absorption performance. The preparation process has good repeatability, low cost, environmental protection, cleanness, no toxicity and easy mass production, and the synthesized one-dimensional nanotube structure is favorable for electromagnetic wave absorption, thus being an ideal electromagnetic wave absorbing material which can be practically applied.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. A one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material is characterized by comprising boric acid, urea, nickel nitrate hexahydrate and polyethylene glycol.
2. The one-dimensional C (B/N) nanotube composite electromagnetic wave absorbing material according to claim 1, wherein the nickel nitrate hexahydrate is 0.11-0.26g, the boric acid is 0.2-0.5g, the urea is 6-20g, and the polyethylene glycol is 0.7-1.6g.
3. The one-dimensional C (B/N) nanotube composite electromagnetic wave absorbing material of claim 1, wherein the nickel nitrate hexahydrate is 0.195g, the boric acid is 0.3g, the urea is 10g, and the polyethylene glycol is 1g.
4. The preparation method of the one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material is characterized by comprising the following steps of;
s1, accurately weighing corresponding amounts of boric acid and urea, dissolving the boric acid and the urea in 100mL of deionized water at room temperature, and magnetically stirring the solution for 1 hour to obtain a uniform mixed solution;
S2, adding a corresponding amount of polyethylene glycol into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution;
S3, adding a corresponding amount of nickel nitrate hexahydrate into the uniformly mixed solution, and magnetically stirring for 1 hour to obtain a uniform mixed solution;
s4, placing the obtained uniform mixed solution in a constant temperature box, and drying for 24 hours to obtain a dried C (B/N) precursor;
S5, placing the solid mixture obtained after drying in the step S4 in a tube furnace, placing the solid mixture in the protection of nitrogen atmosphere, setting the temperature to 900 ℃, and calcining for 4 hours;
s6, cooling to room temperature along with the furnace after heat preservation is finished, and finally obtaining the one-dimensional C (B/N) nanotube.
5. The one-dimensional C (B/N) nanotube composite electromagnetic wave absorbing material and the preparation method thereof according to claim 3, wherein boric acid added in the step S1 is 0.3g, urea is 10g, polyethylene glycol added in the step S2 is 1.0g, and nickel nitrate hexahydrate added in the step S3 is 0.13g.
6. The one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof according to claim 3, wherein the temperature of the incubator is set to 80 ℃ when the incubator is used for drying treatment in the step S3.
7. The one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof according to claim 3, wherein the heating rate in the step S5 is 5 ℃/min.
8. The one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof according to claim 1 or 3, wherein the morphology diameter of the one-dimensional C (B/N) nanotube composite wave-absorbing material modified by the magnetic nano particles is 100nm.
9. The one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof according to claim 1 or 3, wherein the one-dimensional C (B/N) nanotube is loaded with magnetic nanoparticles with the diameter of 40nm.
10. The one-dimensional C (B/N) nanotube composite electromagnetic wave-absorbing material and the preparation method thereof according to claim 1 or 3, wherein the magnetic Ni nano particles in the composite material are uniformly dispersed in the one-dimensional C (B/N) nanotubes.
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