CN110894624A - Magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and preparation method thereof - Google Patents
Magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and a preparation method thereof, wherein vanadyl acetylacetonate and polyvinylpyrrolidone are added into an N, N-dimethylformamide solvent, a mixed solution is obtained after stirring and dissolving, then a magnetic metal precursor is added into the mixed solution, and the mixed solution is stirred at room temperature to obtain an electrostatic spinning solution; preparing the obtained electrostatic spinning solution into one-dimensional nano fibers by adopting electrostatic spinning; and carrying out pre-oxidation treatment on the prepared nano-fiber, and then carrying out nitridation treatment to obtain the Fe/(Co, Ni) VN/C nano-fiber electromagnetic wave absorbing agent. The magnetic metal doped vanadium nitride nano composite fiber prepared by the invention has the advantages of complete molding, large length-diameter ratio, stable structure, simple preparation method, excellent repeatability and good wave-absorbing performance, and effectively improves the microwave absorption performance of vanadium nitride.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and particularly relates to a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and a preparation method thereof.
Background
In recent years, with the rapid development of the electronics and electrical industry, the problem of electromagnetic radiation is becoming more severe. In the military field, radar stealth of military targets can realize quick and accurate attack on enemy targets on the premise of ensuring the safety of own weapon equipment. The electromagnetic wave absorbing material can realize the attenuation and absorption of electromagnetic waves by converting electromagnetic energy into heat energy and energy in other forms, and can solve the problems of electromagnetic pollution and radar stealth to a great extent. Therefore, based on the needs of national defense and electromagnetic pollution protection, the development of a high-performance absorbing material with wider absorption band, greater absorption degree and thinner thickness is urgent.
At present, a plurality of materials with certain wave absorption performance are developed, the development and application of the traditional microwave absorption material are often restricted by the defects of high density, poor stability, narrow absorption band, large matching thickness and the like, the requirements of the novel wave absorption material of width, thinness, lightness and width are difficult to realize, based on the defects, the dielectric material becomes a hot point of research in recent years, and the research finds that the vanadium nitride and graphene composite material with excellent physical and chemical properties in the dielectric material has the minimum reflection loss of-41.5 dB and the effective absorption bandwidth (EAB, RL < -10dB) of 3.9GHz under the thickness of 1.5mm, and shows good wave absorption performance. At present, there is no relevant report about the improvement of the wave absorbing performance of vanadium nitride by compounding with other materials.
Meanwhile, the magnetic metals of iron (Fe), cobalt (Co), nickel (Ni) and alloys thereof have higher saturation magnetization intensity, so that the magnetic materials have higher magnetic conductivity, higher magnetic loss and dielectric loss, stronger consumption capacity on electromagnetic waves and hopeful high-absorption-capacity wave-absorbing materials. But because the larger specific surface area is easy to agglomerate, the magnetic conductivity and the magnetic loss are reduced, and the wave-absorbing performance is deteriorated.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a magnetic metal doped vanadium nitride nanocomposite fiber microwave absorbent and a preparation method thereof, aiming at the defects in the prior art, so as to realize the magnetic metal doping of vanadium nitride and enhance the bandwidth and strength of microwave absorption.
The invention adopts the following technical scheme:
a preparation method of a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent comprises the following steps:
s1, adding vanadyl acetylacetonate and polyvinylpyrrolidone into an N, N-dimethylformamide solvent, stirring and dissolving to obtain a mixed solution, adding a magnetic metal precursor into the mixed solution, and stirring at room temperature to obtain an electrostatic spinning solution;
s2, preparing the electrostatic spinning solution obtained in the step S1 into one-dimensional nano fibers by adopting electrostatic spinning;
s3, carrying out pre-oxidation treatment on the nanofiber prepared in the step S2, and then carrying out nitridation treatment to obtain the Fe/(Co, Ni) VN/C nanofiber electromagnetic wave absorbing agent.
Specifically, in step S1, vanadyl acetylacetonate: polyvinylpyrrolidone: magnetic metal precursor: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3) mmol: (0.5-3) mmol: 10 ml.
Furthermore, the concentration of the polyvinylpyrrolidone in the mixed solution is 0.5-0.3 mol/L.
Further, in step S1, the magnetic metal precursor is iron acetate, nickel acetate or cobalt acetate, and the stirring time is 6-12 hours.
Specifically, in step S2, the electrospinning conditions are: a stainless steel needle head with the specification of 20-23 is adopted, and the distance from the needle head to the collector is 15-25 cm; the electrostatic field voltage is 15-30 kV, and the boosting speed is 0.45-1.5 mL/h.
Specifically, in step S3, the process parameters of the pre-oxidation treatment are as follows: the temperature is 100-300 ℃, the heating rate is 1-4 ℃/min, the time is 2-5 h, and then the product is naturally cooled.
Specifically, in step S3, the nitridation process parameters are: the temperature is 500-900 ℃, the heating rate is 1-5 ℃/min, the time is 2-5 h, and then the product is naturally cooled.
The invention also provides a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent, the length-diameter ratio of the absorbent is more than 60, paraffin is taken as a wave-transmitting agent, and the minimum reflection loss of iron, cobalt and nickel doped vanadium nitride nano fibers is respectively as follows: 46.5, -53.2, -40 dB.
Specifically, the effective absorption bandwidth of the nickel-doped vanadium nitride nanofiber is 5.8GHz, and the frequency range is 7.8-13.6 GHz.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention relates to a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and a preparation method thereof, wherein nontoxic vanadyl acetylacetonate is used as a vanadium source, ferric acetate is used as an iron source, an electrostatic spinning method which is suitable for mass production and has simple operation and excellent repeatability is selected, an excellent pre-oxidation process is explored, iron doped vanadium nitride/carbon nano fiber with the length-diameter ratio of more than 60 is obtained by combining with later-stage nitriding treatment, an excellent magnetic metal doped structure is constructed, the magnetic metal (Fe, Co and Ni) doped vanadium nitride with large length-diameter ratio is prepared, the way of compounding vanadium nitride and metal elements is expanded, the magnetic metal doped vanadium nitride/carbon nano composite fiber absorbent is used as a microwave absorbing absorbent, the wave absorbing performance of vanadium nitride is improved, and more possibilities are provided for the application of vanadium nitride in other aspects.
Furthermore, the doping amount of the magnetic metal can be more easily regulated and controlled by adjusting the proportion of the raw materials.
Furthermore, the diameter of the fiber can be conveniently adjusted by adjusting the technological parameters of electrostatic spinning.
Furthermore, in the pre-oxidation process, the polyvinylpyrrolidone is decomposed and uniformly distributed in the fiber, so that favorable conditions are provided for the subsequent formation of a magnetic metal doped structure; and a suitable pre-oxidation process facilitates the nitridation process to mitigate volume shrinkage.
Furthermore, the phase of the metal element can be conveniently changed by adjusting the nitridation process at the later stage, and the metal element can be a simple substance or exist in a nitride form.
The invention relates to a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent, wherein the minimum reflection loss of iron, cobalt and nickel doped vanadium nitride nano fibers is respectively as follows: 46.5, 53.2 and 40dB show good wave absorbing performance, prove that the doping of the magnetic metal improves the absorbing performance of the vanadium nitride to a great extent, and better provide another method and thought for modifying other materials.
In conclusion, the magnetic metal doped vanadium nitride nano composite fiber prepared by the invention has the advantages of complete molding, larger length-diameter ratio, stable structure, simple preparation method, excellent repeatability and good wave absorbing performance, and effectively improves the microwave absorbing performance of vanadium nitride.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an SEM photograph of a pre-oxidized product of example 1;
FIG. 2 is a diagram of the Fe-doped vanadium nitride nanofiber according to example 1, wherein (a) is an XRD (X-ray diffraction) pattern and (b) is an SEM (scanning Electron microscope) picture;
FIG. 3 is a diagram of cobalt-doped vanadium nitride nanofibers of example 2, wherein (a) is an XRD spectrum and (b) is an SEM photograph;
FIG. 4 is a diagram of nickel-doped vanadium nitride nanofibers of example 3, wherein (a) is an XRD spectrum and (b) is an SEM photograph;
FIG. 5 is a reflection loss curve of the magnetic metal-doped vanadium nitride nanocomposite fiber microwave and paraffin complex prepared according to the embodiment of the present invention;
fig. 6 is a reflection loss curve and an effective absorption width curve of the nickel-doped vanadium nitride nanofiber and paraffin wax composite prepared according to the embodiment of the invention under different thicknesses.
Detailed Description
The invention provides a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent, the length-diameter ratio is more than 60, paraffin is used as a wave transmitting agent, the doping of three metals shows stronger absorption strength and wider absorption bandwidth when being doped by 20 wt%, the minimum reflection loss of nickel doped vanadium nitride nano fibers is-40 dB, the effective absorption bandwidth is 5.8GHz, the frequency range is 7.8-13.6 GHz, the micro appearance of the complete nano fibers is realized, the construction of a one-dimensional conductive network is facilitated, a three-dimensional conductive network structure can be generated integrally, and the magnetic loss mechanism and more interface losses provided by the magnetic metal also utilize the strong and wide absorption of the microwave to a great extent.
The invention relates to a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and a preparation method thereof, wherein the magnetic metal doped vanadium nitride nano composite fiber microwave absorbent comprises the following steps:
s1, adding 1-2 g of vanadyl acetylacetonate and 0.5-2 g of polyvinylpyrrolidone into 10mL of N, N-dimethylformamide solvent, stirring and dissolving, adding a magnetic metal precursor into the mixed solution, placing the mixture at room temperature (25 ℃) and stirring for 6-12 hours to obtain electrostatic spinning solution with certain viscosity, wherein the mass ratio of vanadyl acetylacetonate: polyvinylpyrrolidone: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3 mmol): (0.5-3 mmol): 10 ml;
the magnetic metal precursor is ferric acetate, nickel acetate or cobalt acetate.
S2, selecting a stainless steel needle with the specification of No. 20-23, setting the distance from the needle to the collector to be 15-25 cm, the electrostatic field voltage to be 15-30 kV, and the boosting speed to be 0.45-1.5 mL/h, so as to obtain one-dimensional nanofibers, wherein the nanofibers are stacked to form a conductive network;
s3, pre-oxidizing the nanofibers obtained in the second step by a process of controlling the temperature to be 100-300 ℃, the heating rate to be 1-4 ℃/min and the time to be 2-5 h; and after pre-oxidation, performing nitridation treatment by using a process with the temperature of 500-900 ℃, the heating rate of 1-5 ℃/min and the time of 2-5 h, and naturally cooling to obtain the iron-doped vanadium nitride nano composite fiber electromagnetic wave absorber.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 1g of vanadyl acetylacetonate and 1g of polyvinylpyrrolidone into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 0.7g of ferric acetate into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 12 hours to obtain an electrostatic spinning solution with certain viscosity and uniform dispersion;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 23 stainless steel needle, injecting at a speed of 0.45mL/h, at a distance of 25cm between a spinning nozzle and a collector, at a spinning voltage of 15kV, at an indoor temperature of 24 ℃, at a relative humidity of 25-30%, and obtaining precursor nanofibers on the collector along with volatilization of the solvent;
putting the precursor nano-fiber into a box-type furnace, heating to 100 ℃ at a speed of 3 ℃/min, preserving heat for 4h, and naturally cooling to room temperature to obtain pre-oxidized nano-fiber;
placing the pre-oxidized nanofibers in a crucible, using flowing NH in a vacuum tube furnace3And nitriding the gas, heating the gas to 700 ℃ at a speed of 3 ℃/min, preserving the heat for 2 hours, then cooling the gas to 100 ℃ at a speed of 3 ℃/min, and naturally cooling the gas to room temperature to obtain the iron-doped vanadium nitride nano composite fiber electromagnetic wave absorbing agent.
The good pre-oxidation process has great influence on the fiber formation, for example, as shown in fig. 1, the scanning picture of the pre-oxidation sample of the iron-doped vanadium nitride nanofiber shows that the fiber structure is complete and the diameter distribution is uniform; the sample obtained by the final nitriding treatment has good crystallinity, the diffraction peak of the sample is basically consistent with VN PDF standard card (73-1806) and Fe standard card (89-4186), and the effectiveness of iron doping is proved, as shown in figure 2 (a); the volume shrinkage of the fiber can be generated due to the change of the phase during the nitriding treatment, which may cause the structural damage of the fiber, but the final product prepared by the invention has quite complete shape and large long diameter, as shown in fig. 2 (b).
Example 2
Adding 1.5g of vanadyl acetylacetonate and 2g of polyvinylpyrrolidone into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 0.5g of cobalt acetate into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 8 hours to obtain an electrostatic spinning solution with certain viscosity and uniform dispersion;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 20 stainless steel needle with the injection speed of 0.7mL/h, the distance between a spinning nozzle and a collector is 15cm, the spinning voltage is 20kV, the indoor temperature is 24 ℃, the relative humidity is 25-30%, and precursor nanofibers can be obtained on the collector along with the volatilization of a solvent;
putting the precursor nano-fiber into a box-type furnace, heating to 200 ℃ at a speed of 5 ℃/min, preserving heat for 2h, and naturally cooling to room temperature to obtain pre-oxidized nano-fiber;
placing the pre-oxidized nanofibers in a crucible, using flowing NH in a vacuum tube furnace3And nitriding the gas, heating the gas to 900 ℃ at a speed of 3 ℃/min, preserving the heat for 3 hours, then cooling the gas to 100 ℃ at a speed of 3 ℃/min, and naturally cooling the gas to room temperature to obtain the cobalt-doped vanadium nitride nano composite fiber electromagnetic wave absorbing agent.
The cobalt-doped vanadium nitride nano composite fiber obtained by final nitridation treatment has good crystallinity, and the diffraction peak of the cobalt-doped vanadium nitride nano composite fiber is basically consistent with VN PDF standard cards (73-1806) and Co standard cards (89-7093), so that the effectiveness of cobalt doping is proved, and the figure is shown in fig. 3 (a); the volume shrinkage of the fiber can be generated due to the change of the phase during the nitriding treatment, which may cause the structural damage of the fiber, but the final product prepared by the invention has quite complete shape and large long diameter, as shown in fig. 3 (b).
Example 3
Adding 1g of vanadyl acetylacetonate and 0.5g of polyvinylpyrrolidone into 10mL of N, N-dimethylformamide solvent, stirring for dissolving, adding 0.5g of nickel acetate into the mixed solution, and stirring the mixture at room temperature (25 ℃) for 6 hours to obtain an electrostatic spinning solution with certain viscosity and uniform dispersion;
injecting the spinning solution into a 10mL injector with a plastic spray gun head, selecting a No. 22 stainless steel needle, injecting at a speed of 1.0mL/h, at a distance of 20cm between a spinning nozzle and a collector, at a spinning voltage of 30kV, at an indoor temperature of 24 ℃, at a relative humidity of 25-30%, and obtaining precursor nanofibers on the collector along with volatilization of the solvent;
putting the precursor nano-fiber into a box-type furnace, heating to 300 ℃ at a speed of 5 ℃/min, preserving heat for 5h, and naturally cooling to room temperature to obtain pre-oxidized nano-fiber;
placing the pre-oxidized nanofibers in a crucible, using flowing NH in a vacuum tube furnace3And nitriding the gas, heating the gas to 500 ℃ at the speed of 5 ℃/min, preserving the heat for 5 hours, then cooling the gas to 100 ℃ at the speed of 5 ℃/min, and naturally cooling the gas to room temperature to obtain the nickel-doped vanadium nitride nano composite fiber electromagnetic wave absorbing agent.
The cobalt-doped vanadium nitride nano composite fiber obtained by final nitridation treatment has good crystallinity, and the diffraction peak of the cobalt-doped vanadium nitride nano composite fiber is basically consistent with VN PDF standard cards (73-1806) and Ni standard cards (89-7093), so that the effectiveness of nickel doping is proved, and the figure is shown in fig. 4 (a); the volume shrinkage of the fiber can be generated due to the change of the phase during the nitriding treatment, which may cause the structural damage of the fiber, but the final product prepared by the invention has quite complete shape and large long diameter, as shown in fig. 4 (b).
Referring to fig. 5 and 6, when the absorbing agent content is 20 wt%, the minimum reflection loss of the iron, cobalt, and nickel doped vanadium nitride nanofibers is respectively as follows: the nickel-doped vanadium nitride nano-fiber has the advantages of-46.5, -53.2 and-40 dB, and shows good wave absorbing performance, wherein the minimum reflection loss of the nickel-doped vanadium nitride nano-fiber is-40 dB, the effective absorption bandwidth is 5.8GHz, and the frequency range is 7.8-13.6 GHz. The doping of the magnetic metal proves that the absorption performance of the vanadium nitride is improved to a great extent, and another method and thought for modifying other materials are provided better.
In conclusion, the magnetic metal is simply doped into the vanadium nitride nanowire, so that the problem of structural breakage caused by volume change is effectively solved, and vanadium nitride nanoparticles are prevented from agglomerating; on the other hand, the doping of the magnetic metal provides certain magnetic loss, and meanwhile, rich interfaces are formed, so that the interface loss of the material can be improved; the prepared magnetic metal (Fe, Co and Ni) doped vanadium nitride nano composite fiber has the advantages of complete molding, large length-diameter ratio, stable structure, simple preparation method, excellent repeatability and good wave-absorbing performance, effectively improves the microwave absorption performance of vanadium nitride, expands the way of compounding vanadium nitride and metal elements, and provides more possibility for the application of vanadium nitride in other aspects.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a magnetic metal doped vanadium nitride nano composite fiber microwave absorbent is characterized by comprising the following steps:
s1, adding vanadyl acetylacetonate and polyvinylpyrrolidone into an N, N-dimethylformamide solvent, stirring and dissolving to obtain a mixed solution, adding a magnetic metal precursor into the mixed solution, and stirring at room temperature to obtain an electrostatic spinning solution;
s2, preparing the electrostatic spinning solution obtained in the step S1 into one-dimensional nano fibers by adopting electrostatic spinning;
s3, carrying out pre-oxidation treatment on the nanofiber prepared in the step S2, and then carrying out nitridation treatment to obtain the Fe/(Co, Ni) VN/C nanofiber electromagnetic wave absorbing agent.
2. The method of claim 1, wherein in step S1, the ratio of vanadyl acetylacetonate: polyvinylpyrrolidone: magnetic metal precursor: n, N-dimethylformamide solvent ═ 1 mmol: (0.5-3) mmol: (0.5-3) mmol: 10 ml.
3. The method according to claim 2, wherein the concentration of the polyvinylpyrrolidone in the mixed solution is 0.5 to 0.3 mol/L.
4. The method according to claim 1 or 2, wherein in step S1, the magnetic metal precursor is ferric acetate, nickel acetate or cobalt acetate, and the stirring time is 6-12 h.
5. The method of claim 1, wherein in step S2, the electrospinning conditions are: a stainless steel needle head with the specification of 20-23 is adopted, and the distance from the needle head to the collector is 15-25 cm; the electrostatic field voltage is 15-30 kV, and the boosting speed is 0.45-1.5 mL/h.
6. The method as claimed in claim 1, wherein in step S3, the process parameters of the pre-oxidation treatment are: the temperature is 100-300 ℃, the heating rate is 1-4 ℃/min, the time is 2-5 h, and then the product is naturally cooled.
7. The method of claim 1, wherein in step S3, the nitridation process parameters are: the temperature is 500-900 ℃, the heating rate is 1-5 ℃/min, the time is 2-5 h, and then the product is naturally cooled.
8. The magnetic metal-doped vanadium nitride nano composite fiber microwave absorbent prepared by the method of claim 1, wherein the length-diameter ratio of the absorbent is more than 60, paraffin is used as a wave-transmitting agent, and the minimum reflection losses of the iron, cobalt and nickel-doped vanadium nitride nano fibers are respectively as follows: 46.5, -53.2, -40 dB.
9. The magnetic metal-doped vanadium nitride nanocomposite fiber microwave absorber according to claim 8, wherein the effective absorption bandwidth of the nickel-doped vanadium nitride nanofiber is 5.8GHz, and the frequency range is 7.8-13.6 GHz.
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| CN111235695A (en) * | 2020-03-17 | 2020-06-05 | 南京航空航天大学 | Preparation method of porous carbon fiber electromagnetic wave absorbing agent |
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| CN113215614A (en) * | 2021-04-26 | 2021-08-06 | 陕西科技大学 | Carbon-layer-loaded tungsten-doped vanadium nitride nanoparticle composite electrocatalyst and preparation method and application thereof |
| CN113215614B (en) * | 2021-04-26 | 2022-02-11 | 陕西科技大学 | Carbon-layer-loaded tungsten-doped vanadium nitride nanoparticle composite electrocatalyst and preparation method and application thereof |
| CN113718372A (en) * | 2021-08-26 | 2021-11-30 | 山东大学 | Low-pollution high-magnetism cobalt ferrite fiber and preparation method thereof |
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| CN113652769B (en) * | 2021-08-30 | 2023-08-22 | 中国工程物理研究院激光聚变研究中心 | Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption |
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| CN115010502A (en) * | 2022-05-25 | 2022-09-06 | 松山湖材料实验室 | Method for rapidly preparing nano vanadium nitride coated carbon fiber composite ceramic powder, product and application thereof |
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Application publication date: 20200320 |