CN112093801B - Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof - Google Patents
Rice hull-based nano silicon carbide/carbon composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing a nano silicon carbide/carbon composite wave-absorbing material by using rice hulls as raw materials, which comprises the following synthetic steps: and putting the rice hulls which are cleaned and dried by distilled water into a crucible, and then putting the crucible into a tubular furnace or a muffle furnace for heat treatment to respectively obtain carbonized rice hulls and nano silicon dioxide. Then, the carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to a certain mass proportion and mixed by a ball mill. And putting the mixed materials into a reaction kettle, and putting the reaction kettle into a tubular furnace for heating and reacting. And (3) putting the product obtained after the reaction into a hydrochloric acid solution, stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying to obtain the nano silicon carbide/carbon composite wave-absorbing material with adjustable carbon content. The method takes the agricultural waste rice hulls as the raw materials, has simple, efficient and pollution-free preparation process, is easy to realize industrial production, and accords with the concept of sustainable development.
Description
Technical Field
The invention belongs to the field of electromagnetic wave absorption, and particularly relates to a nano silicon carbide/carbon composite wave-absorbing material and a preparation method thereof.
Background
With the rapid development of information technology and the widespread use of electrical devices, electromagnetic pollution has become a crucial issue. In order to solve the problem, high-performance wave-absorbing materials attract more and more attention in the fields of civilian use, commercial use, military use, aerospace and the like. An ideal electromagnetic wave absorbing material should have strong absorption capacity, a wide absorption band, light weight, good corrosion resistance and high temperature stability. Absorbing materials are generally composed of an absorbing phase, referred to as the absorber, and a transmitting phase. Conventional electromagnetic absorption materials, such as ferrite and metal materials, have been widely used because they have strong absorption properties due to their good electrical conductivity and magnetic loss. However, they are limited in their widespread use by disadvantages such as excessive density, poor corrosion resistance and poor thermal stability.
Silicon carbide (SiC) has good absorption properties, a wide absorption band, tunable dielectric properties and a low density, and has proven to be a good choice for electromagnetic absorbers. In addition, silicon carbide has high mechanical strength, inert chemistry and good high temperature stability under severe working conditions. However, pure silicon carbide materials have limited their practical applications due to their weak electromagnetic loss capabilities, limited polarization relaxation loss modes, and low electrical conductivity. The polarization loss and the conductance loss of pure silicon carbide nanoparticles are insufficient, and thus are far from the actual requirements. In order to improve the electromagnetic wave absorption performance of high-purity silicon carbide, compounding, surface decoration and doping with other materials are three effective strategies. Carbon-based materials are ideal materials for compounding with silicon carbide due to their low density, good electrical conductivity and large dielectric loss. Different types of carbon materials, such as carbon nanotubes, carbon black and graphene, have been introduced into developed silicon carbide/carbon composites, which exhibit significantly enhanced electromagnetic wave absorption efficiency and have a wider effective absorption bandwidth than pure silicon carbide. In most cases, silicon carbide/carbon composites are made with nanosized silicon carbide externally incorporated into nanocarbon structures, which often results in interfaces that are limited and unstable. Moreover, the above methods involve complicated synthetic processes or require high-cost precursors. These drawbacks greatly hinder the widespread use of silicon carbide-based composites in the field of electromagnetic wave absorption.
Therefore, it remains a great challenge to prepare an ideal silicon carbide/carbon composite electromagnetic wave absorbing material having an abundant and stable carbon/silicon carbide interface by an economically feasible method.
The invention aims to solve the problems that: the prepared nano silicon carbide/carbon composite material is used as an electromagnetic wave absorbent, has rich and stable carbon/silicon carbide interfaces, high electromagnetic wave absorption efficiency and wider effective absorption bandwidth.
Disclosure of Invention
The technical scheme provided by the invention for solving the problems is as follows: provides a rice hull-based nano silicon carbide/carbon composite wave-absorbing material and a preparation method thereof.
The composite wave-absorbing material is prepared by taking carbonized rice hulls converted from the rice hulls and nano silicon dioxide as raw materials and taking metal magnesium powder as a catalyst for reaction.
Further, the carbonized rice hulls are prepared by putting the cleaned rice hulls into a heat treatment furnace with atmosphere protection (nitrogen or argon), heating to 500-1000 ℃ at the heating rate of 1-20 ℃/min for heat treatment for 2h, and cooling along with the furnace.
Further, the nano silicon dioxide is prepared by putting the cleaned rice hulls into a muffle furnace, heating to 500-1000 ℃ at the heating rate of 1-20 ℃/min for heat treatment for 2h, and cooling along with the furnace.
Further, the mass ratio of the reaction raw materials of the carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder is 1:0.1-3:0.1-10, and the nano silicon carbide/carbon composite wave-absorbing material with different carbon contents can be prepared by adjusting the ratio.
A method for preparing a nano silicon carbide/carbon composite wave-absorbing material by taking rice husks as raw materials comprises the following synthetic steps:
firstly, preparing carbonized rice hulls and nano silicon dioxide by taking the rice hulls as raw materials;
secondly, mixing the carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder according to a certain mass ratio, and mixing the materials by using a ball mill;
thirdly, putting the materials mixed by the ball mill in the step two into a reaction kettle, and putting the materials into a heat treatment furnace for reaction;
fourthly, putting the product obtained after the reaction in the third step into a hydrochloric acid solution for stirring, then separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and then putting the residues into an oven for drying to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Further, the reaction kettle in the third step is made of metal and can be sealed.
Further, the reaction mode in the heat treatment furnace in the third step is that nitrogen or argon is firstly introduced for protection, then the temperature is raised to 500-1000 ℃ at the heating rate of 1-20 ℃/min for reaction for 0.5-10h, and the reaction is cooled along with the furnace.
The main advantages of the invention are:
(1) according to the invention, the agricultural waste rice hulls are used as raw materials to prepare the nano silicon carbide/carbon composite material through magnesium thermal reaction, and nano silicon carbide particles are uniformly generated in the carbon matrix, so that the nano silicon carbide/carbon composite material has the characteristics of rich silicon carbide-carbon interface and stability.
(2) The composition of the silicon carbide/carbon nano composite material can be regulated and controlled by adjusting the proportion of the reaction raw materials of the carbonized rice hulls and the nano silicon dioxide to prepare the silicon carbide/carbon nano composite material with different carbon contents, the carbon content plays an important role in the electromagnetic wave absorption performance, the impedance matching is optimized by adjusting the carbon content, the electromagnetic loss capability is enhanced, and the composite material has excellent electromagnetic wave absorption performance.
(3) The silicon carbide/carbon nano composite material takes agricultural waste rice hulls as raw materials, has simple preparation process, high efficiency and no pollution, is easy to realize industrial production, accords with the concept of sustainable development, and provides technical support for popularization of the nano silicon carbide/carbon composite wave-absorbing material.
Drawings
FIG. 1 is a scanning electron microscope image of a nano-SiC/carbon composite prepared in example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of the nano silicon carbide/carbon composite material prepared in example 1 of the present invention;
FIG. 3 is an XRD pattern of the nano-SiC/carbon composite materials prepared in examples 1, 2 and 3 according to the present invention and comparative example 1;
FIG. 4 is a thermogram of the nano-SiC/carbon composite prepared in examples 1, 2 and 3 of the present invention and comparative example 1;
FIG. 5 is an electromagnetic reflection loss chart of the nano-SiC/carbon composite material prepared in examples 1, 2 and 3 and comparative examples 1 and 2 of the present invention at different frequencies (the samples were uniformly mixed with paraffin wax at a mass ratio of 1:1 and then tested);
FIG. 6 is a scanning electron microscope image of the nano-SiC/carbon composite material prepared in example 2 of the present invention;
FIG. 7 is a transmission electron microscope image of the nano-SiC/carbon composite material prepared in example 2 of the present invention;
FIG. 8 is a scanning electron microscope image of the nano-SiC/carbon composite material prepared in example 3 of the present invention;
fig. 9 is a transmission electron microscope image of the nano silicon carbide/carbon composite material prepared in example 3 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the scope of the invention.
Example 1
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:1.5:2, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 650 ℃ at the heating rate of 3 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
As can be seen from the scanning electron microscope image in fig. 6, a small amount of carbon blocks exist in the nano silicon carbide/carbon composite material prepared in this example, and the nano silicon carbide particles are tightly bonded to the carbon.
As can be seen from the transmission electron micrograph of FIG. 7, the nano-SiC particles in the nano-SiC/carbon composite prepared in this example are tightly bonded to carbon, and the grain size of the SiC particles is about 30-100 nm.
The XRD diffraction pattern of fig. 3 proves the existence of amorphous carbon and cubic phase nano-silicon carbide in the nano-silicon carbide/carbon composite material prepared in this example.
As can be seen from the thermogravimetric graph of fig. 4, the carbon content in the nano silicon carbide/carbon composite material prepared in this example is about 3.5%.
Comparative example 1
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls. The method comprises the following steps of proportioning carbonized rice hulls and metal magnesium powder according to the mass ratio of 1:0.5, and then mixing the materials uniformly by using a ball mill. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 650 ℃ at the heating rate of 3 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
The XRD diffraction pattern of fig. 3 proves the existence of amorphous carbon and cubic phase nano-silicon carbide in the nano-silicon carbide/carbon composite material prepared in this example.
As can be seen from the thermogravimetric graph of fig. 4, the carbon content of the nano silicon carbide/carbon composite material prepared in this example is about 49.6%.
Comparative example 2
Putting the nano silicon carbide/carbon composite material prepared in the example 1 into a muffle furnace, heating to 600 ℃ to remove carbon in the nano silicon carbide/carbon composite material to obtain pure nano silicon carbide; the carbonised rice husk prepared in example 1 was taken up in sodium hydroxide solution to remove the silica therefrom to obtain pure carbon. The silicon carbide and the carbon are proportioned according to the mass ratio of 96.5:3.5, and then are uniformly mixed by a ball mill to obtain the nano silicon carbide/carbon composite wave-absorbing material with the carbon content of 3.5 percent.
And (3) comparing the results: as can be seen from the reflection loss graphs of FIG. 5 at different frequencies, the minimum value of-27.78 dB of the reflection loss of the nano-SiC/carbon composite material prepared in example 1 at the frequency of 10.1GHz is significantly better than the minimum value of-2.50 dB of the reflection loss of comparative example 1 at the frequency of 10.1GHz and the minimum value of-14.87 dB of the reflection loss of comparative example 2 at the frequency of 10.1 GHz.
The comparison result of the electromagnetic wave absorption performance of the embodiment 1 and the comparative example 1 shows that the carbon content of the nano silicon carbide/carbon composite wave-absorbing material of the embodiment 1 is more suitable. The carbon content of the example 1 is the same as that of the comparative example 2, but the electromagnetic wave absorption performance of the example 1 is excellent, which shows that the silicon carbide-carbon interface existing in the nano silicon carbide/carbon prepared by the reaction has obvious effect on the electromagnetic wave absorption.
Example 2
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:1:1.5, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 650 ℃ at the heating rate of 3 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
As can be seen from the scanning electron microscope image in fig. 1, the nano silicon carbide/carbon composite material prepared in this example has obvious carbon blocks, and the nano silicon carbide particles are tightly bonded to the carbon.
As can be seen from the transmission electron microscope image in FIG. 2, the nano-silicon carbide particles in the nano-silicon carbide/carbon composite material prepared in this example are tightly bonded to carbon, and the particle size of the silicon carbide is about 30-100 nm.
The XRD diffraction pattern of fig. 3 proves the existence of amorphous carbon and cubic phase nano-silicon carbide in the nano-silicon carbide/carbon composite material prepared in this example.
As can be seen from the thermogravimetric graph of fig. 4, the carbon content in the nano silicon carbide/carbon composite material prepared in this example is about 13.4%.
As can be seen from the reflection loss chart of FIG. 5 at different frequencies, the nano-SiC/carbon composite material prepared in this example has a minimum reflection loss value of-6.69 dB at a frequency of 5.1 GHz.
Example 3
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:2:2.5, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 650 ℃ at the heating rate of 3 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
As can be seen from the scanning electron microscope image in fig. 8, no obvious carbon block exists in the nano silicon carbide/carbon composite material prepared in this embodiment, and the nano silicon carbide particles have a uniform size.
As can be seen from the TEM image of FIG. 9, the SiC particles in the SiC/carbon composite material prepared in this example are about 30-100nm in size.
The XRD diffraction pattern of fig. 3 demonstrates the existence of cubic phase nano-silicon carbide in the nano-silicon carbide/carbon composite prepared in this example.
As can be seen from the thermogravimetric graph of fig. 4, the carbon content in the nano silicon carbide/carbon composite material prepared in this example is about 0.8%.
As can be seen from the reflection loss graph of FIG. 5 at different frequencies, the nano-SiC/carbon composite material prepared in this example has a minimum reflection loss value of-10.28 dB at a frequency of 14.9 GHz.
Example 4
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 700 ℃ at a heating rate of 3 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are washed and dried by distilled water into a muffle furnace, heating to 700 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:2.5:3.5, and then a ball mill is used for mixing the materials to be uniform. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 650 ℃ at the heating rate of 3 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Example 5
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at a heating rate of 10 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 800 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The method comprises the following steps of proportioning carbonized rice hulls, nano silicon dioxide and metal magnesium powder according to the mass ratio of 1:1:2, and then mixing uniformly by using a ball mill. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 750 ℃ at the heating rate of 10 ℃/min, reacting for 2.5h, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Example 6
Putting the rice hulls which are washed and dried by distilled water into a heat treatment type furnace, firstly introducing nitrogen for protection, then heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are washed and dried by distilled water into a muffle furnace, heating to 700 ℃ at the heating rate of 10 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:0.5:1.8, and then a ball mill is used for mixing the materials to be uniform. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 700 ℃ at a heating rate of 15 ℃/min, reacting for 3 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Example 7
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 650 ℃ at the heating rate of 1 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are washed and dried by distilled water into a muffle furnace, heating to 650 ℃ at the heating rate of 1 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:1:1.5, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, placing the stainless steel reaction kettle in a heat treatment furnace, introducing argon for protection, raising the temperature to 650 ℃ at the heating rate of 1 ℃/min, reacting for 5 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Example 8
Putting the rice hulls which are washed and dried by distilled water into a heat treatment furnace, firstly introducing nitrogen for protection, then heating to 800 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 800 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:1:2.5, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, placing the stainless steel reaction kettle in a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 850 ℃ at the heating rate of 3 ℃/min, reacting for 1 hour, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
Example 9
Putting the rice hulls which are washed and dried by distilled water into a tubular furnace, firstly introducing nitrogen for protection, then heating to 500 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain carbonized rice hulls; putting the rice hulls which are cleaned and dried by distilled water into a muffle furnace, heating to 600 ℃ at the heating rate of 5 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide. The carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder are proportioned according to the mass ratio of 1:2:3, and then a ball mill is used for mixing the materials uniformly. Putting the mixed materials into a stainless steel reaction kettle, putting the stainless steel reaction kettle into a heat treatment furnace, introducing nitrogen for protection, raising the temperature to 750 ℃ at the heating rate of 5 ℃/min, reacting for 2 hours, and cooling along with the furnace. And putting the reacted product into a hydrochloric acid solution, fully stirring, separating out residues in the hydrochloric acid solution by using a filtering device, washing the residues to be neutral by using distilled water, and finally drying the residues in an oven to obtain the nano silicon carbide/carbon composite wave-absorbing material.
It should be noted that the above detailed description is only for exemplary purposes, and the present invention is not limited to the above described embodiments. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (7)
1. A nanometer silicon carbide/carbon composite wave-absorbing material prepared by taking rice hulls as raw materials is characterized in that:
the composite wave-absorbing material is prepared by taking carbonized rice hulls converted from the rice hulls and nano silicon dioxide as raw materials and using metal magnesium powder as a catalyst through reaction,
putting the cleaned rice hulls into a muffle furnace, heating to 500-1000 ℃ at the heating rate of 1-20 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the nano silicon dioxide.
2. The nano silicon carbide/carbon composite wave-absorbing material according to claim 1, wherein: putting the cleaned rice hulls into a heat treatment furnace with nitrogen or argon and with an atmosphere protection function, heating to 500-1000 ℃ at the heating rate of 1-20 ℃/min for heat treatment for 2h, and cooling along with the furnace to obtain the carbonized rice hulls.
3. The nano silicon carbide/carbon composite wave-absorbing material according to claim 1, which is characterized in that: the mass ratio of the reaction raw materials of the carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder is 1:0.1-3:0.1-10, and the nano silicon carbide/carbon composite wave-absorbing material with different carbon contents can be prepared by adjusting the ratio.
4. The preparation method of the nano silicon carbide/carbon composite wave-absorbing material according to claim 1, which is characterized by comprising the following specific preparation steps:
step one, preparing carbonized rice hulls and nano silicon dioxide by taking the rice hulls as raw materials;
step two, mixing the carbonized rice hulls, the nano silicon dioxide and the metal magnesium powder according to a certain mass proportion,
mixing materials by using a ball mill;
step three, putting the materials mixed by the ball mill in the step two into a reaction kettle, and putting the reaction kettle into a heat treatment furnace
Carrying out reaction;
step four, putting the product obtained after the reaction in the step three into a hydrochloric acid solution for stirring, and then filtering the solution
Separating out the residue in hydrochloric acid solution, washing with distilled water to neutrality, and oven drying
Obtaining the nano silicon carbide/carbon composite wave-absorbing material; wherein the content of the first and second substances,
in the first step, the cleaned rice hulls are put into a muffle furnace, heated to 500-1000 ℃ at the heating rate of 1-20 ℃/min for heat treatment for 2h, and cooled along with the furnace to obtain the nano silicon dioxide.
5. The preparation method of the nano silicon carbide/carbon composite wave-absorbing material according to claim 4, characterized by comprising the following steps: and the reaction kettle in the third step is made of metal and can be sealed.
6. The preparation method of the nano silicon carbide/carbon composite wave-absorbing material according to claim 4, characterized by comprising the following steps: the reaction mode in the heat treatment furnace in the third step is that nitrogen or argon is firstly introduced for protection, then the temperature is raised to 500-1000 ℃ at the heating rate of 1-20 ℃/min for reaction for 0.5-10h, and the reaction is cooled along with the furnace.
7. Use of the nano silicon carbide/carbon composite material according to claim 1 in the preparation of an electromagnetic wave absorber.
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