CN114890770A - Preparation method of porous silicon carbide/carbon composite aerogel - Google Patents
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Abstract
A preparation method of porous silicon carbide/carbon composite aerogel relates to a preparation method of silicon carbide/carbon composite aerogel. The invention aims to solve the problems of high requirement on the preparation equipment and complex process of the existing silicon carbide/carbon composite material, and simultaneously solves the problems of narrow absorption band and limited absorption performance of a single silicon carbide material. The preparation method comprises the following steps: firstly, preparing a hydrogel precursor; secondly, preparing an aerogel precursor; and thirdly, sintering. The preparation method is used for preparing the porous silicon carbide/carbon composite aerogel.
Description
Technical Field
The invention relates to a preparation method of silicon carbide/carbon composite aerogel.
Background
The ceramic aerogel is known for its low density, high porosity, large surface area, excellent thermal stability and chemical stability, and shows wide application prospects in the aspects of electromagnetic wave absorption, high-temperature heat insulation materials, catalyst carriers, filters, light structural materials, various application functional material matrixes and the like. Among them, silicon carbide aerogel has excellent high temperature chemical stability and better heat resistance than oxide ceramic aerogel, and at the same time it has typical semiconductor characteristics, and is an electromagnetic wave absorbing material with wide application prospect. However, a single silicon carbide material has limited electromagnetic wave absorption capacity, and the defect of a single component can be overcome by preparing a composite material. Carbon materials are often used for preparing composite materials due to the advantages of low density, high conductivity and the like, and the silicon carbide/carbon composite materials can realize excellent electromagnetic wave absorption capacity and can be widely applied to the fields of aerospace, communication, protection and the like.
Because the physical and chemical properties of silicon carbide are extremely stable, the preparation of the silicon carbide and carbon composite material is difficult, the existing synthesis methods mostly adopt methods such as chemical vapor infiltration, electrostatic spinning and the like, and the methods have high requirements on equipment, are complex in process and are difficult to meet application requirements.
Disclosure of Invention
The invention aims to solve the problems of high requirement on the existing preparation equipment of the silicon carbide/carbon composite material and complex process, and simultaneously solves the problems of narrow absorption band and limited absorption performance of a single silicon carbide material, thereby providing a preparation method of the porous silicon carbide/carbon composite aerogel.
A preparation method of porous silicon carbide/carbon composite aerogel is carried out according to the following steps:
firstly, preparing a hydrogel precursor:
dissolving acrylamide and N, N-methylene bisacrylamide in ultrapure water, adding carbon fiber for ultrasonic dispersion, then dropping ammonium persulfate solution, and finally curing to obtain a hydrogel precursor;
the mass ratio of the acrylamide to the N, N-methylene-bisacrylamide is (10-50) to 1; the mass ratio of the acrylamide to the ultrapure water is (0.1-1) to 1; the volume ratio of the mass of the carbon fiber to the ultrapure water is (0-5) g:1 mL; the volume ratio of the mass of the acrylamide to the volume of the ammonium persulfate solution is 1g (1-5) mL; the concentration of the ammonium persulfate solution is 0.05 g/mL-2 g/mL;
secondly, preparing an aerogel precursor:
pre-freezing the hydrogel precursor for 12-48 h at the temperature of-20 to-60 ℃ to obtain frozen hydrogel, and freeze-drying the frozen hydrogel to obtain an aerogel precursor;
thirdly, sintering:
laying silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering an aerogel precursor on the surface of the reaction silicon source layer, then sintering at high temperature under inert gas, and cooling to room temperature to obtain the porous silicon carbide/carbon composite aerogel.
The invention has the beneficial effects that:
the invention develops a simple and easily-amplified method for preparing the porous silicon carbide/carbon fiber/carbon composite aerogel, and the method has low requirements on instruments and is easy to repeat;
secondly, by changing the sintering temperature, the reaction degree can be controlled, and composite materials with different contents of silicon carbide and carbon are obtained;
and the prepared porous material has excellent electromagnetic wave absorption performance, the problems of narrow absorption band and limited wave absorption performance of single silicon carbide are solved, the reflection loss of-52.6 dB can be achieved when the thickness of a sample is 3.2mm, about 99.999% of electromagnetic waves can be absorbed, and the effective absorption band (the band corresponding to the reflection loss < -10 dB) under the thickness is 8.6 GHz.
The invention relates to a preparation method of porous silicon carbide/carbon composite aerogel.
Drawings
Fig. 1 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared in example one;
FIG. 2 is an XRD pattern of the porous silicon carbide/carbon composite aerogel prepared in the first example, wherein ● is carbon and diamond-like carbon is silicon carbide;
fig. 3 is a graph of wave-absorbing properties of the porous silicon carbide/carbon composite aerogel prepared in the first embodiment at different thicknesses, which is calculated through simulation of test results of a coaxial method, wherein 1 is 1mm, 2 is 2mm, 3 is 3mm, 4 is 3.2mm, 5 is 3.5mm, 6 is 4mm, 7 is 4.5mm, and 8 is 5 mm;
FIG. 4 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared according to example II;
FIG. 5 is an XRD pattern of the porous silicon carbide/carbon composite aerogel prepared in example two, wherein ● is carbon and diamond-solid is silicon carbide;
fig. 6 is a graph of wave-absorbing properties of the porous silicon carbide/carbon composite aerogel prepared in example two at different thicknesses, which is simulated and calculated through a coaxial method test result, wherein 1 is 1mm, 2 is 2mm, 3 is 3mm, 4 is 4.03mm, 5 is 4.5mm, and 6 is 5 mm;
FIG. 7 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared by a comparative experiment;
FIG. 8 is an XRD diagram of a porous silicon carbide/carbon composite aerogel prepared by comparative experiments, wherein ● is carbon and diamond-solid is silicon carbide;
fig. 9 is a wave-absorbing property diagram of the porous silicon carbide/carbon composite aerogel prepared by a comparative experiment of simulation calculation of a test result of a coaxial method under different thicknesses, wherein 1 is 1mm, 2 is 1.5mm, 3 is 1.67mm, 4 is 2mm, 5 is 2.5mm, 6 is 3mm, 7 is 4mm, and 8 is 5 mm.
Detailed Description
The first embodiment is as follows: the preparation method of the porous silicon carbide/carbon composite aerogel comprises the following steps:
firstly, preparing a hydrogel precursor:
dissolving acrylamide and N, N-methylene bisacrylamide in ultrapure water, adding carbon fiber for ultrasonic dispersion, then dropping ammonium persulfate solution, and finally curing to obtain a hydrogel precursor;
the mass ratio of the acrylamide to the N, N-methylene bisacrylamide is (10-50) to 1; the mass ratio of the acrylamide to the ultrapure water is (0.1-1) to 1; the volume ratio of the mass of the carbon fiber to the ultrapure water is (0-5) g:1 mL; the volume ratio of the mass of the acrylamide to the volume of the ammonium persulfate solution is 1g (1-5) mL; the concentration of the ammonium persulfate solution is 0.05 g/mL-2 g/mL;
secondly, preparing an aerogel precursor:
pre-freezing the hydrogel precursor for 12-48 h at the temperature of-20 to-60 ℃ to obtain frozen hydrogel, and freeze-drying the frozen hydrogel to obtain an aerogel precursor;
thirdly, sintering:
laying silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering an aerogel precursor on the surface of the reaction silicon source layer, then sintering at high temperature under inert gas, and cooling to room temperature to obtain the porous silicon carbide/carbon composite aerogel.
The principle is as follows: the good electromagnetic wave absorption performance of the porous silicon carbide/carbon composite aerogel is obtained due to the synergistic effect of carbon and the silicon carbide components. It is known that carbon materials have high electrical conductivity, which is beneficial to improve the electrical conduction loss of materials, so that electromagnetic waves are converted into other energy to be dissipated, but the high electrical conductivity of carbon also causes strong mismatch with the impedance of free space, so that the electromagnetic waves are reflected at the material interface and cannot enter the materials. The introduction of silicon carbide with a lower dielectric constant can significantly improve the impedance matching of the material. Therefore, the silicon carbide/carbon composite aerogel obtains the optimal impedance matching and strong attenuation capability, thereby obtaining excellent electromagnetic wave absorption performance.
The beneficial effects of the embodiment are as follows:
the method for preparing the porous silicon carbide/carbon fiber/carbon composite aerogel is simple and easy to amplify, and has low requirements on instruments and is easy to repeat;
secondly, by changing the sintering temperature, the reaction degree can be controlled, and composite materials with different contents of silicon carbide and carbon are obtained;
and the prepared porous material has excellent electromagnetic wave absorption performance, the problems of narrow absorption band and limited wave absorption performance of single silicon carbide are solved, the reflection loss of-52.6 dB can be achieved when the thickness of a sample is 3.2mm, about 99.999% of electromagnetic waves can be absorbed, and the effective absorption band (the band corresponding to the reflection loss < -10 dB) under the thickness is 8.6 GHz.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the length of the carbon fiber in the step one is 0.05 mm-1 mm. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the ultrasonic dispersion in the first step is specifically ultrasonic dispersion for 1 to 24 hours under the condition that the magnetic stirring rotating speed is 100 to 600 rpm; the curing in the step one is specifically curing for 10min to 80min at the temperature of 30 ℃ to 70 ℃. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the freeze drying in the step two is to freeze dry for 12 to 48 hours under the temperature of minus 40 to minus 60 ℃. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the silicon source powder in the third step is a mixture of silicon dioxide powder and silicon powder; the molar ratio of the silicon dioxide powder to the silicon powder is (0.1-1): 1. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the mixture of the silicon dioxide powder and the silicon powder is prepared by the following steps: under the condition that the rotating speed is 60 r/min-100 r/min, mixing the silicon dioxide powder and the silicon powder for 1 h-10 h by using a ball mill. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the particle size of the silicon dioxide powder is 50-1000 meshes; the particle size of the silicon powder is 50-1000 meshes. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the inert gas in the third step is nitrogen or argon. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and the mass ratio of the aerogel precursor to the silicon source powder in the third step is 1 (1-10). The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: the high-temperature sintering in the third step is to raise the temperature from room temperature to 800-1600 ℃, and then to preserve heat for 0.5-24 h under the condition that the temperature is 800-1600 ℃. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of porous silicon carbide/carbon composite aerogel is carried out according to the following steps:
firstly, preparing a hydrogel precursor:
dissolving 4g of acrylamide and 0.2g N, N-methylene bisacrylamide in 20mL of ultrapure water, adding 1.4g of carbon fiber for ultrasonic dispersion, then dripping 10mL of ammonium persulfate solution, and finally curing to obtain a hydrogel precursor;
the concentration of the ammonium persulfate solution is 0.3 g/mL;
secondly, preparing an aerogel precursor:
pre-freezing the hydrogel precursor for 12h at the temperature of-20 ℃ to obtain frozen hydrogel, and freeze-drying the frozen hydrogel to obtain an aerogel precursor;
thirdly, sintering:
laying 17.6g of silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering 4g of aerogel precursor on the surface of the reaction silicon source layer, then sintering at high temperature under inert gas, and cooling to room temperature to obtain the porous silicon carbide/carbon composite aerogel.
The average length of the carbon fiber in the step one is 0.5 mm;
the ultrasonic dispersion in the step one is specifically ultrasonic dispersion for 10 hours under the condition that the magnetic stirring rotating speed is 400 rpm.
The curing in the step one is specifically curing for 10min at the temperature of 50 ℃.
The freeze drying in the second step is to freeze dry for 48 hours under the temperature of minus 50 ℃.
The silicon source powder in the third step is a mixture of 12g of silicon dioxide powder and 5.6g of silicon powder.
The mixture of the silicon dioxide powder and the silicon powder is prepared by the following steps: mixing silicon dioxide powder and silicon powder by a ball mill for 10 hours at the rotating speed of 60r/min,
the particle size of the silicon dioxide powder is 600 meshes; the particle size of the silicon powder is 600 meshes.
The inert gas in the third step is argon.
In the third step, the temperature is raised from room temperature to 1500 ℃, and then the temperature is kept for 2 hours under the condition of 1500 ℃.
Fig. 1 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared in example one; as can be seen from the figure, the microstructure of the prepared composite aerogel is represented by a highly porous three-dimensional network-like structure comprising a porous framework, nanowires and fibers.
FIG. 2 is an XRD pattern of the porous silicon carbide/carbon composite aerogel prepared in the first example, wherein ● is carbon and diamond-like carbon is silicon carbide; as can be seen from the figure, no other impurity phase or impurity is mixed in the composite aerogel, the carbon content is 16.0%, and the silicon carbide content is 84.0%.
Fig. 3 is a graph of wave-absorbing properties of the porous silicon carbide/carbon composite aerogel prepared in the first embodiment at different thicknesses, which is calculated through simulation of test results of a coaxial method, wherein 1 is 1mm, 2 is 2mm, 3 is 3mm, 4 is 3.2mm, 5 is 3.5mm, 6 is 4mm, 7 is 4.5mm, and 8 is 5 mm; as can be seen from the figure, the optimal absorption performance is that the reflection loss can reach-52.6 dB when the thickness of a sample is 3.2mm, the sample can absorb about 99.999 percent of electromagnetic waves, and the effective absorption frequency band (the frequency band corresponding to the reflection loss < -10 dB) at the thickness is 8.6 GHz.
Example two: the difference between the present embodiment and the present embodiment is: and in the first step, no carbon fiber is added. The rest is the same as the first embodiment.
FIG. 4 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared according to example II; as can be seen from the figure, the microstructure of the prepared composite aerogel is represented by a highly porous three-dimensional network-like structure comprising a porous framework and nanowires.
FIG. 5 is an XRD pattern of the porous silicon carbide/carbon composite aerogel prepared in example two, wherein ● is carbon and diamond-solid is silicon carbide; as can be seen from the figure, no other impurity phase or impurity is mixed in the composite aerogel, the carbon content is 13.3%, and the silicon carbide content is 86.7%.
Fig. 6 is a graph of wave-absorbing properties of the porous silicon carbide/carbon composite aerogel prepared in example two at different thicknesses, which is simulated and calculated through a coaxial method test result, wherein 1 is 1mm, 2 is 2mm, 3 is 3mm, 4 is 4.03mm, 5 is 4.5mm, and 6 is 5 mm; as can be seen from the figure, the best absorption performance is that the reflection loss of-16.5 dB can be achieved when the thickness of the sample is 4.03mm, about 98% of electromagnetic waves can be absorbed, and the effective absorption band at the thickness is 6.5 GHz.
Comparative experiment: the difference between the comparative experiment and the embodiment is as follows: the high-temperature sintering in the third step is to increase the temperature from room temperature to 1400 ℃, and then keep the temperature at 1400 ℃ for 2 h. The rest is the same as the first embodiment.
FIG. 7 is an SEM photograph of a porous silicon carbide/carbon composite aerogel prepared by a comparative experiment; as can be seen from the figure, the microstructure of the prepared composite aerogel is represented by a highly porous three-dimensional network-like structure comprising a porous skeleton, nanowires and fibers.
FIG. 8 is an XRD diagram of a porous silicon carbide/carbon composite aerogel prepared by comparative experiments, wherein ● is carbon and diamond-solid is silicon carbide; as can be seen from the figure, no other impurity phase or impurity is mixed in the composite aerogel, the carbon content is 44.4%, and the silicon carbide content is 55.6%.
Fig. 9 is a graph of wave-absorbing properties of the porous silicon carbide/carbon composite aerogel prepared by a comparative experiment through simulation calculation of test results of a coaxial method under different thicknesses, wherein 1 is 1mm, 2 is 1.5mm, 3 is 1.67mm, 4 is 2mm, 5 is 2.5mm, 6 is 3mm, 7 is 4mm, and 8 is 5 mm; as can be seen from the figure, the best absorption performance is that the reflection loss of-14.0 dB can be achieved when the thickness of the sample is 1.67mm, the electromagnetic wave can be absorbed by about 96%, and the effective absorption band at the thickness is 1.9 GHz.
Claims (10)
1. The preparation method of the porous silicon carbide/carbon composite aerogel is characterized by comprising the following steps of:
firstly, preparing a hydrogel precursor:
dissolving acrylamide and N, N-methylene bisacrylamide in ultrapure water, adding carbon fiber for ultrasonic dispersion, then dropping ammonium persulfate solution, and finally curing to obtain a hydrogel precursor;
the mass ratio of the acrylamide to the N, N-methylene bisacrylamide is (10-50) to 1; the mass ratio of the acrylamide to the ultrapure water is (0.1-1) to 1; the volume ratio of the mass of the carbon fiber to the ultrapure water is (0-5) g:1 mL; the volume ratio of the mass of the acrylamide to the volume of the ammonium persulfate solution is 1g (1-5) mL; the concentration of the ammonium persulfate solution is 0.05 g/mL-2 g/mL;
secondly, preparing an aerogel precursor:
pre-freezing the hydrogel precursor for 12-48 h at the temperature of-20 to-60 ℃ to obtain frozen hydrogel, and freeze-drying the frozen hydrogel to obtain an aerogel precursor;
thirdly, sintering:
laying silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering an aerogel precursor on the surface of the reaction silicon source layer, then sintering at high temperature under inert gas, and cooling to room temperature to obtain the porous silicon carbide/carbon composite aerogel.
2. The method for preparing a porous silicon carbide/carbon composite aerogel according to claim 1, wherein the length of the carbon fiber in the step one is 0.05mm to 1 mm.
3. The preparation method of the porous silicon carbide/carbon composite aerogel according to claim 1, wherein the ultrasonic dispersion in the step one is specifically ultrasonic dispersion for 1 to 24 hours under the condition that the magnetic stirring rotation speed is 100 to 600 rpm; the curing in the step one is specifically curing for 10min to 80min at the temperature of 30 ℃ to 70 ℃.
4. The method for preparing the porous silicon carbide/carbon composite aerogel according to claim 1, wherein the freeze-drying in the step two is performed for 12 to 48 hours at a temperature of-40 to-60 ℃.
5. The method for preparing the porous silicon carbide/carbon composite aerogel according to claim 1, wherein the silicon source powder in the step three is a mixture of silicon dioxide powder and silicon powder; the molar ratio of the silicon dioxide powder to the silicon powder is (0.1-1): 1.
6. The preparation method of the porous silicon carbide/carbon composite aerogel according to claim 5, characterized in that the mixture of the silicon dioxide powder and the silicon powder is prepared by the following steps: under the condition that the rotating speed is 60 r/min-100 r/min, mixing the silicon dioxide powder and the silicon powder for 1 h-10 h by using a ball mill.
7. The method for preparing the porous silicon carbide/carbon composite aerogel according to claim 5, wherein the particle size of the silicon dioxide powder is 50-1000 meshes; the particle size of the silicon powder is 50-1000 meshes.
8. The method for preparing a porous silicon carbide/carbon composite aerogel according to claim 1, wherein the inert gas in step three is nitrogen or argon.
9. The preparation method of the porous silicon carbide/carbon composite aerogel according to claim 1, wherein the mass ratio of the aerogel precursor to the silicon source powder in the step three is 1 (1-10).
10. The method for preparing the porous silicon carbide/carbon composite aerogel according to claim 1, wherein the high-temperature sintering in the step three is to raise the temperature from room temperature to 800-1600 ℃, and then to keep the temperature at 800-1600 ℃ for 0.5-24 h.
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| CN115748257A (en) * | 2022-12-11 | 2023-03-07 | 浙江理工大学 | Rapid preparation method of porous composite hydrogel and application of porous composite hydrogel in photo-thermal seawater desalination |
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