CN111170761A - Silicon carbide @ metal oxide wave-absorbing foam and preparation method thereof - Google Patents
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Abstract
The invention discloses silicon carbide @ metal oxide wave-absorbing foam and a preparation method thereof, and belongs to the field of preparation of wave-absorbing materials. The silicon carbide nano-wire aerogel is used as a matrix, and metal oxide nano-particles are loaded on nano-wires of the silicon carbide nano-wire aerogel, so that the silicon carbide @ metal oxide wave-absorbing foam with the ultrahigh specific surface area and the three-dimensional network structure is obtained. The preparation method comprises the steps of immersing the silicon carbide nanowire aerogel into a precursor solution of the metal oxide, carrying out hydrothermal/solvothermal reaction, washing a product after hydrothermal/solvothermal reaction, and drying to obtain the silicon carbide @ metal oxide wave-absorbing foam. The maximum reflection loss of the material can reach-16 dB, the effective wave-absorbing frequency band can reach 5.76GHz, and the material has excellent wave-absorbing performance and can be applied to the field of wave-absorbing materials.
Description
Technical Field
The invention belongs to the field of preparation of wave-absorbing materials, and particularly relates to silicon carbide @ metal oxide wave-absorbing foam and a preparation method thereof.
Background
The development of electromagnetic technology and the common use of various electronic devices bring convenience to the production and life of people, and simultaneously threaten the safety of human bodies, such as damage to the nervous system, the immune system and the like of the human bodies, and the wave-absorbing material plays an increasingly important role in the field of electromagnetic protection. In addition, in the military aspect, the radar stealth technology is an important means for improving the success rate of operations and the survival rate of equipment, and the wave-absorbing material is already applied to high-precision military equipment such as stealth airplanes and the like, so that the research and development of the high-performance wave-absorbing material has profound significance in civil use and military use.
Wave-absorbing materials have been widely studied, and common wave-absorbing materials such as carbon materials, metal oxides, silicon carbide and the like have been widely studied. However, the existing wave-absorbing materials are difficult to meet the requirements of people on an ideal wave-absorbing body: namely, the novel wave-absorbing material has four characteristics of thin thickness, wide absorption frequency band, light weight and strong wave-absorbing capability. To achieve the above objectives simultaneously, not only the composition of the wave-absorbing material needs to be optimized, but also the optimization needs to be made from the viewpoint of material structure. However, no wave-absorbing material capable of meeting the requirement exists at present, so that the development of a structure-function integrated wave-absorbing material is urgently needed.
Silicon carbide is a traditional dielectric wave-absorbing material, and has attracted much attention in recent years due to its low density, high mechanical properties, good chemical stability and thermal stability. The silicon carbide nanowires can generate rich interface polarization due to high long-diameter ratio, carriers can be transmitted along the nanowires, and when the nanowires are mutually lapped, a conductive network structure is formed, so that electromagnetic wave consumption can be further performed. However, how to uniformly disperse SiC nanowires and obtain longer conductive paths still remains an urgent problem to be solved.
By mixing magnetic metal oxides (e.g. Fe)3O4、Co3O4Etc.) is loaded on the surface of the SiC nanowire, so that the impedance matching characteristic of the SiC nanowire can be improved, more electromagnetic waves can enter the wave-absorbing material, and meanwhile, the magnetic loss can be introduced, so that the electromagnetic waves are further lost. However, the problems of large addition amount, large density and narrow wave-absorbing frequency band in the matrix limit further application.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the silicon carbide @ metal oxide wave-absorbing foam and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses silicon carbide @ metal oxide wave-absorbing foam which is a three-dimensional network structure consisting of silicon carbide nanowire aerogel and metal oxide loaded on the surfaces of the nanowires;
wherein the silicon carbide nanowire aerogel is prepared by adopting the technology disclosed by the invention patent with the publication number of CN109627006A, and the density is 5mg/cm3～100mg/cm3The length of the nano wire of the silicon carbide nano wire aerogel is 100-1000 mu m, and the diameter is 20 nm-0.5 mu m; the particle size of the metal oxide is 4nm to 500 nm.
Preferably, the metal oxide is ferroferric oxide, ferric oxide or cobaltosic oxide.
Preferably, the silicon carbide @ metal oxide wave-absorbing foam has wave-absorbing performance at 4-18 GHz, and the reflection loss is lower than-10 dB.
The invention discloses a preparation method of the silicon carbide @ metal oxide wave-absorbing foam, which is characterized by comprising the following steps of:
1) preparing a metal oxide precursor solution: ultrasonically dispersing a metal oxide precursor in a solvent to prepare a metal oxide precursor solution with the concentration of (0.3-120) g/L;
2) hydrothermal/solvothermal treatment: carrying out heat preservation treatment on the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) at the temperature of 150-220 ℃ for 4-24 h by using a hydrothermal/solvothermal method, and generating metal oxide nanoparticles on the surfaces of the nanowires of the silicon carbide nanowire aerogel;
3) washing: washing the product prepared in the step 2) to remove the metal oxide nanoparticles which are not loaded on the surface of the silicon carbide nanowire;
4) and (3) drying: and (3) drying the product obtained by the treatment in the step 3) to prepare the silicon carbide @ metal oxide wave-absorbing foam.
Preferably, in step 1), the metal oxide precursor is ferric acetylacetonate, ferrous acetylacetonate, ferrocene, FeCl3·6H2O、FeCl2·4H2O、FeSO4·7H2O, cobalt acetylacetonate, Co (NO)3)2·6H2O and Co (AC)2·4H2Any one or more of O.
Preferably, in the step 1), the solvent is one or more of deionized water, absolute ethyl alcohol, ethyl acetate, chloroform, acetone and benzene.
Preferably, the dosage ratio of the silicon carbide nanowire aerogel to the metal oxide precursor solution prepared in the step 1) is (0.5-10) g/L.
Preferably, in the step 4), the drying is carried out for 1 to 12 hours at a temperature of between 30 and 100 ℃.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the silicon carbide nanowire aerogel with a three-dimensional continuous network structure is used as a matrix, metal oxide nanoparticles are generated on the surface of the nanowire of the silicon carbide nanowire aerogel by virtue of the continuous network structure and the ultrahigh specific surface area of the silicon carbide nanowire aerogel and adopting a hydrothermal/solvothermal method, so that the silicon carbide @ metal oxide wave-absorbing foam with the ultrahigh specific surface area and a three-dimensional network structure is finally obtained, and the prepared silicon carbide @ metal oxide wave-absorbing foam belongs to a dielectric loss and magnetic loss composite wave-absorbing material due to the coupling effect between the silicon carbide three-dimensional porous continuous network structure and the metal oxide, on one hand, the loaded metal oxide can adjust the dielectric constant and the magnetic conductivity of the silicon carbide aerogel, and the impedance matching performance of a wave-absorbing agent can be improved; on the other hand, magnetic loss is introduced after the metal oxide is loaded, and an interface polarization phenomenon is generated on an interface combined with the silicon carbide, so that the wave absorbing performance is enhanced. Meanwhile, the silicon carbide nanowire aerogel is adopted to load the metal oxide, so that the using amount of the metal oxide can be reduced, the density of the material is reduced, the metal oxide can be well dispersed, and in addition, the porous structure in the obtained silicon carbide @ metal oxide wave-absorbing foam can perform multi-stage reflection on incident electromagnetic waves, so that the electromagnetic waves are further consumed, and the wave-absorbing performance of the material is enhanced.
The wave-absorbing foam prepared by the invention has good wave-absorbing performance at 4-18 GHz, the reflection loss is lower than-10 dB, the maximum reflection loss reaches-16 dB, the effective wave-absorbing frequency band can reach 5.76GHz, the wave-absorbing foam has excellent wave-absorbing performance, has the advantages of thin thickness, low density, controllable wave-absorbing frequency band and the like, and can be applied to the field of wave-absorbing materials.
The preparation method of the silicon carbide @ metal oxide wave-absorbing foam disclosed by the invention does not need special equipment, is simple in process, is suitable for large-scale production, and can be used as a wave-absorbing material in the fields of electromagnetic shielding and absorption.
Drawings
FIG. 1 is a microscopic scanning photograph of a silicon carbide nanowire aerogel prepared using the technology disclosed in the patent publication CN 109627006A;
FIG. 2 is a macro morphology photograph of the silicon carbide @ metal oxide microwave absorbing foam prepared in example 1;
FIG. 3 is a wave-absorbing property curve of the silicon carbide @ metal oxide wave-absorbing foam prepared in example 1;
FIG. 4 is an XRD pattern of the silicon carbide @ metal oxide microwave absorbing foam prepared in example 2;
FIG. 5 is a microscopic scanning photograph of the silicon carbide @ metal oxide microwave absorbing foam prepared in example 3;
Detailed Description
In order to make the technical solutions of the present invention better understood, 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 only a part of the embodiments of the present invention, and not all of the embodiments. 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.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the invention discloses silicon carbide @ metal oxide wave-absorbing foam which is three-dimensional network structure foam consisting of silicon carbide nanowire aerogel and metal oxide nanoparticles loaded on the surfaces of the nanowires of the silicon carbide nanowire aerogel;
the silicon carbide nanowire aerogel disclosed by the invention is prepared by adopting the technology disclosed by the invention patent with the publication number of CN109627006A, and FIG. 1 is an SEM image of the silicon carbide nanowire aerogel. The diameter distribution of the silicon carbide nano-wires is 20 nm-0.5 μm, and the length is 100 μm-1000 μm. The metal oxide refers to ferroferric oxide, ferric oxide and cobaltosic oxide, and the particle size distribution is 4-500 nm.
The preparation method of the silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
s1, preparing a metal oxide precursor solution: weighing a certain amount of metal oxide precursor, adding a solvent, and performing ultrasonic dispersion;
s2, hydrothermal/solvent heat treatment: placing the silicon carbide nanowire aerogel and the metal oxide precursor solution into a reaction kettle, and preserving heat for 4-24 hours at the temperature of 150-220 ℃, wherein a large amount of metal oxide nanoparticles are generated on the surface of the silicon carbide nanowire in the process;
s3, washing: washing the product prepared in the step S2 with deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nanoparticles which are not loaded on the surface of the silicon carbide nanowire;
s4, drying: and (4) putting the product obtained in the step (S3) into an oven, and drying for 1-12 h at the temperature of 30-100 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
Preferably, in step S1, the selected metal oxide precursor is ferric acetylacetonate, ferrous acetylacetonate, ferrocene, FeCl3·6H2O、FeCl2·4H2O、FeSO4·7H2O, cobalt acetylacetonate, Co (NO)3)2·6H2O、Co(AC)2·4H2Any one or more of O.
Preferably, in step S1, the solvent of the precursor solution is any one or more of deionized water, absolute ethyl alcohol, ethyl acetate, chloroform, acetone, and benzene, and further preferably, deionized water or absolute ethyl alcohol is used as the solvent.
Preferably, in step S1, the concentration of the precursor solution is: (0.3-120) g/L.
Preferably, in step S2, the ratio of the silicon carbide nanowire aerogel to the metal oxide precursor solution prepared in step S1 is (0.5-10) g/L.
Example 1
A preparation method of silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
1) preparing a metal oxide precursor solution: weighing 0.02g of ferric acetylacetonate, dissolving in 60mL of absolute ethanol, and performing ultrasonic dispersion for 5 min;
2) solvent heat treatment: 30mg of the powder with the density of 5mg/cm3Transferring the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) into a reaction kettle, heating to 150 ℃, and preserving heat for 24 hours to carry out solvothermal reaction;
3) washing: washing the product obtained in the step 2) with deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nanoparticles which are not loaded on the surface of the silicon carbide nanowire;
4) and (3) drying: and (3) putting the product obtained in the step 3) into an oven to be dried for 8 hours at the temperature of 30 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
Referring to fig. 2, a macroscopic photograph of the silicon carbide @ metal oxide wave-absorbing foam prepared in this example is shown, and it can be seen from fig. 2 that the silicon carbide @ metal oxide wave-absorbing foam prepared by the method of the present invention is grayish gray in macroscopic view, and is a porous foam material.
Referring to fig. 3, a wave absorbing performance curve of the silicon carbide @ metal oxide wave absorbing foam prepared in this embodiment is shown. As can be seen from FIG. 3, when the thickness of the absorber is 2mm, the maximum reflection loss reaches-16 dB, and the effective wave-absorbing frequency bandwidth less than-10 dB is 5.76 GHz.
Example 2
A preparation method of silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
1) preparing a metal oxide precursor solution: 4.053g of FeCl were weighed3·6H2O and 1.988g FeCl2·4H2Dissolving O in 50mL of deionized water, performing ultrasonic dispersion for 10min, and adjusting the pH to 9 by using a NaOH solution;
2) hydrothermal treatment: 60mg of the extract with the density of 10mg/cm3Transferring the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) into a reaction kettle, heating to 160 ℃, and preserving heat for 8 hours to perform solvothermal reaction;
3) washing: washing the product obtained in the step 2) by using deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nano particles which are not loaded on the surface of the silicon carbide nano wire.
4) And (3) drying: and (3) putting the product obtained in the step 3) into an oven to be dried for 8 hours at the temperature of 50 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
Results referring to fig. 4, the XRD spectrum of the silicon carbide @ metal oxide microwave absorbing foam prepared in this example is shown. As can be seen from FIG. 4, XRD peaks correspond to silicon carbide and ferroferric oxide, respectively, which shows that the wave-absorbing material is composed of silicon carbide and ferroferric oxide.
Example 3
A preparation method of silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
1) preparing a metal oxide precursor solution: weighing 1g of ferric acetylacetonate, dissolving in 60mL of ethyl acetate, and performing ultrasonic dispersion for 20 min;
2) solvent heat treatment: 300mg and a density of 50mg/cm3Transferring the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) into a reaction kettle, heating to 200 ℃, and keeping the temperature for 12 hours to perform a solvothermal reaction;
3) washing: washing the product obtained in the step 2) by using deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nano particles which are not loaded on the surface of the silicon carbide nano wire.
4) And (3) drying: and (3) putting the product obtained in the step 3) into an oven to be dried for 8 hours at the temperature of 40 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
The results are shown in figure 5, which is a microscopic scanning photograph of the prepared silicon carbide @ metal oxide wave absorbing foam. As can be seen from FIG. 5, the silicon carbide @ metal oxide wave-absorbing foam is a network-like structure formed by a plurality of silicon carbide nanowires which are intertwined with one another in a microscopic manner, and ferroferric oxide nanoparticles are loaded on the silicon carbide nanowires.
Example 4
A preparation method of silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
1) preparing a metal oxide precursor solution: weighing 2g of ferrous acetylacetonate, dissolving in 60mL of acetone, and performing ultrasonic dispersion for 30 min;
2) solvent heat treatment: 300mg and a density of 50mg/cm3Transferring the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) into a reaction kettle, heating to 220 ℃, and preserving heat for 4 hours to perform solvothermal reaction;
3) washing: washing the product obtained in the step 2) by using deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nano particles which are not loaded on the surface of the silicon carbide nano wire.
4) And (3) drying: and (3) putting the product obtained in the step 3) into an oven to be dried for 12 hours at the temperature of 30 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
Example 5
A preparation method of silicon carbide @ metal oxide wave-absorbing foam comprises the following steps:
1) preparing a metal oxide precursor solution: weighing 4g of cobalt acetylacetonate, dissolving in 60mL of benzene, and performing ultrasonic dispersion for 30 min;
2) solvent heat treatment: 600mg, density 100mg/cm3Transferring the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) into a reaction kettle, heating to 200 ℃, and keeping the temperature for 6 hours to perform solvothermal reaction;
3) washing: washing the product obtained in the step 2) by using deionized water and absolute ethyl alcohol for 3 times respectively to remove the metal oxide nano particles which are not loaded on the surface of the silicon carbide nano wire.
4) And (3) drying: and (3) putting the product obtained in the step 3) into an oven to be dried for 10 hours at the temperature of 50 ℃ to obtain the silicon carbide @ metal oxide wave-absorbing foam.
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. The silicon carbide @ metal oxide wave-absorbing foam is characterized by being of a three-dimensional network structure consisting of silicon carbide nanowire aerogel and metal oxide loaded on the surfaces of the nanowires of the silicon carbide @ metal oxide wave-absorbing foam.
2. The silicon carbide @ metal oxide wave-absorbing foam of claim 1, wherein the metal oxide is ferroferric oxide, ferric oxide, or cobaltosic oxide, and the particle size of the metal oxide is 4nm to 500 nm.
3. According to the claimsThe silicon carbide @ metal oxide wave-absorbing foam of claim 1 is characterized in that the silicon carbide nanowire aerogel is a three-dimensional network structure constructed by SiC nanowires, and the density of the silicon carbide nanowire aerogel is 5mg/cm3～100mg/cm3(ii) a The SiC nanowire has the length of 100-1000 μm and the diameter of 20-0.5 μm.
4. The silicon carbide @ metal oxide wave-absorbing foam of claim 1, wherein the silicon carbide @ metal oxide wave-absorbing foam has wave-absorbing properties at 4-18 GHz, and has a reflection loss of less than-10 dB.
5. A preparation method of silicon carbide @ metal oxide wave-absorbing foam is characterized by comprising the following steps:
1) preparing a metal oxide precursor solution: ultrasonically dispersing a metal oxide precursor in a solvent to prepare a metal oxide precursor solution with the concentration of (0.3-120) g/L;
2) hydrothermal/solvothermal treatment: carrying out heat preservation treatment on the silicon carbide nanowire aerogel and the metal oxide precursor solution prepared in the step 1) at the temperature of 150-220 ℃ for 4-24 h by using a hydrothermal/solvothermal method, and generating metal oxide nanoparticles on the surfaces of the nanowires of the silicon carbide nanowire aerogel;
3) washing: washing the product prepared in the step 2) to remove the metal oxide nanoparticles which are not loaded on the surface of the silicon carbide nanowire;
4) and (3) drying: and (3) drying the product obtained by the treatment in the step 3) to prepare the silicon carbide @ metal oxide wave-absorbing foam.
6. The method for preparing silicon carbide @ metal oxide wave-absorbing foam according to claim 5, wherein in the step 1), the metal oxide precursor is ferric acetylacetonate, ferrous acetylacetonate, ferrocene, FeCl3·6H2O、FeCl2·4H2O、FeSO4·7H2O, cobalt acetylacetonate, Co (NO)3)2·6H2O and Co (AC)2·4H2Any one or more of O.
7. The method for preparing silicon carbide @ metal oxide wave-absorbing foam according to claim 5, wherein in the step 1), the solvent is one or more of deionized water, absolute ethyl alcohol, ethyl acetate, chloroform, acetone and benzene.
8. The preparation method of silicon carbide @ metal oxide wave-absorbing foam according to claim 5, wherein the dosage ratio of the silicon carbide nanowire aerogel to the metal oxide precursor solution prepared in step 1) is (0.5-10) g/L.
9. The method for preparing silicon carbide @ metal oxide wave-absorbing foam according to claim 5, wherein in the step 4), the drying is performed for 1 to 12 hours at a temperature of 30 to 100 ℃.
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| CN111935968A (en) * | 2020-08-21 | 2020-11-13 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
| CN111935968B (en) * | 2020-08-21 | 2021-08-27 | 山东大学 | Preparation method of iron/nitrogen/carbon composite material |
| CN114773092A (en) * | 2022-04-29 | 2022-07-22 | 西安交通大学 | Method for improving mechanical property and heat-insulating property of silicon carbide nanowire aerogel through oxidation treatment |
| CN115849948A (en) * | 2022-11-30 | 2023-03-28 | 中国科学院上海硅酸盐研究所 | Fe 3 O 4 /SiC nw /Si 3 N 4 Composite wave-absorbing ceramic and preparation method thereof |
| CN115849948B (en) * | 2022-11-30 | 2023-12-08 | 中国科学院上海硅酸盐研究所 | Fe (Fe) 3 O 4 /SiC nw /Si 3 N 4 Composite wave-absorbing ceramic and preparation method thereof |
| CN115991607A (en) * | 2022-12-27 | 2023-04-21 | 中国科学院上海硅酸盐研究所 | Porous ceramic wave-absorbing material loaded with magnetic particles and preparation method thereof |
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