CN113264774A - SiC crystal synthesized by seed induced microwave and preparation method thereof - Google Patents
SiC crystal synthesized by seed induced microwave and preparation method thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 5
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/667—Sintering using wave energy, e.g. microwave sintering
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Abstract
The invention discloses a seed-induced microwave synthesized SiC crystal and a preparation method thereof, and relates to the technical field of inorganic non-metallic materials. The method comprises the following steps: uniformly mixing silicon powder, nano carbon black and SiC seed crystal to obtain mixed powder, pressing the mixed powder into a blank, heating by microwave, and carrying out heat preservation at 800-1100 ℃ for 15-30 min to synthesize SiC crystal, thus obtaining the seed crystal induced microwave synthesized SiC crystal. Compared with the seed crystal induction technology which is currently used in industry, the process provided by the invention greatly reduces the difficulty and process conditions of SiC crystal synthesis. The synthesis of SiC by microwave and seed crystal composite induction has good application prospect.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to a seed-induced microwave synthesized SiC crystal and a preparation method thereof.
Background
SiC has the advantages of high strength, high hardness, high elastic modulus, excellent chemical stability, etc., and is widely used in the fields of abrasive tools, refractory materials, metallurgy, machining, etc. The SiC band gap is wide, the electron mobility is high, the high-temperature electric conduction and heat conduction performance is excellent, and the SiC band gap plays an important role in the application fields of electronic device semiconductors and heat exchangers.
The traditional Acheson method is still mainly adopted in the current industrial production method of SiC crystals. The SiC crystal prepared by the Acheson method has the characteristics of cheap raw materials, simple process, easy realization of industrial production and the like. However, the method has the advantages of low thermal efficiency, high synthesis temperature, large energy consumption, long period and serious pollution, and brings serious influence on the atmospheric environment; and the crystal form is complex, the particle size is large, and the application requirement of high-end fields cannot be met. In recent years, new processes for producing SiC crystals have been increasing, such as sol-gel methods, chemical vapor synthesis methods, and solvothermal methods. However, these methods have the disadvantages of complicated synthesis steps, high energy consumption, high production cost, and the like.
Disclosure of Invention
The invention aims to solve the defects in the background technology, and provides a preparation method of a seed crystal induced microwave synthesized SiC crystal, in the process of synthesizing SiC by seed crystal induced microwave, SiC is used as a good microwave absorber material, the SiC seed crystal is coupled with microwave to generate heat, the reaction of raw materials is promoted at low temperature, the SiC seed crystal can be used as a crystallization platform at high temperature to promote the nucleation and growth of the crystal, and the SiC seed crystal can be used as a local hot spot to promote the reaction of the raw materials and can also be used as a crystal growth hot platform to induce the nucleation and in-situ growth of the synthesized SiC. Compared with the seed crystal induction technology which is currently used in industry, the process greatly reduces the difficulty and the process conditions of SiC crystal synthesis. The synthesis of SiC by microwave and seed crystal composite induction has good application prospect.
The invention aims to provide a preparation method of seed crystal induced microwave synthesis SiC crystal, which comprises the following steps:
uniformly mixing silicon powder, nano carbon black and SiC seed crystal to obtain mixed powder, pressing the mixed powder into a blank, heating by microwave, and carrying out heat preservation at 800-1100 ℃ for 15-30 min to synthesize SiC crystal, thus obtaining the seed crystal induced microwave synthesized SiC crystal.
Preferably, in the microwave heating process, the input speed of power is 200-600W/min.
Preferably, the grain size of the SiC seed crystal is 0.5-5 μm, and the addition amount of the SiC seed crystal is 1-20 wt% of the total mass of the raw materials.
Preferably, the molar ratio of the silicon powder to the nano carbon black is 1: 1 to 3.
Preferably, the mixed powder is prepared by mixing silicon powder, nano carbon black and SiC seed crystal by a ball milling method with absolute ethyl alcohol as a dispersion medium, setting the rotating speed at 100r/min, performing ball milling for 12 hours, and then performing vacuum drying at the temperature of 80 ℃ for 12 hours.
More preferably, the particle size of the mixed powder is not less than 60 meshes.
Preferably, when the blank is heated, the blank is placed into an alumina crucible, and quartz sand powder is covered around the blank; then the crucible is put into a heat preservation structure consisting of an alumina heat preservation box and mullite heat preservation cellucotton for microwave heating.
The second purpose of the invention is to provide a seed crystal induced microwave synthesized SiC crystal.
The third purpose of the invention is to provide application of the SiC crystal in electronic device semiconductors and heat exchangers.
Compared with the prior art, the invention has the beneficial effects that:
in the process of synthesizing SiC by seed crystal induction microwave, SiC is used as a good microwave absorber material, and the SiC seed crystal is coupled with the microwave to generate heat and promote the reaction of raw materials at low temperature; the SiC seed crystal can be used as a crystallization platform at high temperature to promote crystal nucleation and growth; therefore, in the microwave heating process, the SiC seed crystal can be used as a local hot spot to promote the reaction of the raw materials and can also be used as a crystal growth hot table to induce and synthesize SiC nucleation and in-situ growth. Compared with the seed crystal induction technology which is currently used in industry, the process greatly reduces the difficulty and the process conditions of SiC crystal synthesis; the synthesis of SiC by microwave and seed crystal composite induction has good application prospect.
Drawings
FIG. 1 shows XRD patterns of SiC crystals synthesized by seed crystal induced microwave as raw materials and provided in examples 1 to 4.
FIG. 2 is an SEM photograph of a seed crystal induced microwave synthesized SiC crystal of the raw material and provided in examples 1 to 4.
FIG. 3 shows XRD patterns of SiC crystals synthesized by seed crystal induced microwave as the raw material and provided in examples 4 to 6.
FIG. 4 is an SEM photograph of the seed crystal induced microwave synthesized SiC crystal provided in examples 4-6.
Figure 5 is the XRD patterns of the seed crystal induced microwave synthesized SiC crystals provided in examples 4, 7 and 8.
Fig. 6 is SEM photographs of the seed crystal induced microwave synthesized SiC crystal provided in examples 4, 7, and 8.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
It should be noted that the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials used are commercially available, unless otherwise specified.
The SiC seed type used in each of the following examples was alpha-SiC granules having a purity of 99.9% and purchased from New materials, Inc., Henry, Baofeng.
The silicon powder is purchased from Shanghai Chaowei nanotechnology GmbH; the nano carbon black is purchased from Hebeixin iron metal materials Co., Ltd;
the technical solution of the present invention is further described with reference to the following specific examples.
Example 1
A preparation method of crystal seed induced microwave synthesis SiC crystal comprises the following steps:
mixing nano carbon black and silicon powder according to a molar ratio of 2: 1mol, 5 μm SiC seed crystal was added in an amount of 20 (wt)%, based on the total mass. And (3) respectively putting the nano carbon black, the silicon powder and the SiC crystal seeds with the particle size of 5 mu m into a ball milling tank by using absolute ethyl alcohol as a dispersion medium, and carrying out ball milling on the mixed materials for 12 hours at the rotating speed of 100 r/min. After the ball milling is finished, the mixture is put into an air-blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then is sieved for standby. And uniaxially pressing 8g of mixed powder into a green body with the mass of 25 multiplied by 35 multiplied by 10 mm by adopting the green body forming pressure of 2 MPa. In order to prevent the oxidation of the green body in the microwave synthesis process, the green body is placed in an alumina crucible, and the periphery of the green body is covered with quartz sand powder. The crucible was placed in a holding structure having an alumina holding box and mullite holding fiber cotton, and heated in a microwave oven of TE666 resonance mode (WXD20S-07, tokyo trile microwave equipment ltd). The microwave frequency is 2.45GHz, and the maximum input power is 10 KW; the temperature is measured by an infrared pyrometer, the initial display is that the heating temperature is controlled by adjusting the incident power to the maximum value of 6400W at the speed of 400W/min in the experiment from 600 ℃, the heating temperature is 800 ℃, the heat preservation time is 20min, and the seed crystal induced microwave synthesized SiC crystal is obtained.
Example 2
The same as in example 1, except that the heating temperature was 900 ℃.
Example 3
The same as in example 1, except that the heating temperature was 1000 ℃.
Example 4
The same as in example 1, except that the heating temperature was 1100 ℃.
Example 5
A preparation method of crystal seed induced microwave synthesis SiC crystal comprises the following steps:
mixing nano carbon black and silicon powder according to a molar ratio of 2: 1mol, 5 μm SiC seed crystal was added in an amount of 20 (wt)%, based on the total mass. And (3) respectively putting the nano carbon black, the silicon powder and the SiC crystal seeds with the particle size of 5 mu m into a ball milling tank by using absolute ethyl alcohol as a dispersion medium, and carrying out ball milling on the mixed materials for 12 hours at the rotating speed of 100 r/min. After the ball milling is finished, the mixture is put into an air-blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then is sieved for standby. And uniaxially pressing 8g of mixed powder into a green body with the mass of 25 multiplied by 35 multiplied by 10 mm by adopting the green body forming pressure of 2 MPa. In order to prevent the oxidation of the green body in the microwave synthesis process, the green body is placed in an alumina crucible, and the periphery of the green body is covered with quartz sand powder. The crucible was placed in a holding structure having an alumina holding box and mullite holding fiber cotton, and heated in a microwave oven of TE666 resonance mode (WXD20S-07, tokyo trile microwave equipment ltd). The microwave frequency is 2.45GHz and the maximum input power is 10 KW. The temperature is measured by an infrared pyrometer, the initial display is that the heating rate is controlled by adjusting the incident power to the maximum value of 6400W at the rate of 200W/min in the experiment from 600 ℃, the heating temperature is 1100 ℃, and the heat preservation time is 20min, thus obtaining the seed crystal induced microwave synthesized SiC crystal.
Example 6
The same as in example 5, except that the heating rate was controlled by adjusting the incident power to a maximum value of 6400W at a rate of 600W/min.
Example 7
A preparation method of crystal seed induced microwave synthesis SiC crystal comprises the following steps:
mixing nano carbon black and silicon powder according to a molar ratio of 2: 1mol, and the amounts of 0.5 μm SiC seed crystals added were each 20 (wt)%, based on the total mass. And (3) respectively putting the nano carbon black, the silicon powder and the SiC crystal seeds with the particle size of 0.5 mu m into a ball milling tank by using absolute ethyl alcohol as a dispersion medium, and ball milling the mixed materials for 12 hours at the rotating speed of 100 r/min. After the ball milling is finished, the mixture is put into an air-blast drying oven to be dried for 12 hours at the temperature of 80 ℃, and then is sieved for standby. And uniaxially pressing 8g of mixed powder into a green body with the mass of 25 multiplied by 35 multiplied by 10 mm by adopting the green body forming pressure of 2 MPa. In order to prevent the oxidation of the green body in the microwave synthesis process, the green body is placed in an alumina crucible, and the periphery of the green body is covered with quartz sand powder. The crucible was placed in a holding structure having an alumina holding box and mullite holding fiber cotton, and heated in a microwave oven of TE666 resonance mode (WXD20S-07, tokyo trile microwave equipment ltd). The microwave frequency is 2.45GHz and the maximum input power is 10 KW. The temperature was measured by an infrared pyrometer and was initially displayed starting at 600 ℃. The heating rate was controlled by adjusting the incident power to a maximum of 6400W at a rate of 400W/min, respectively. Heating temperature is 1100 ℃, and heat preservation time is 20min, thus obtaining the seed crystal induced microwave synthesis SiC crystal.
Example 8
The same as in example 7 except that the SiC seed crystal had a particle size of about 1 μm.
In order to illustrate the correlation performance of the SiC crystal prepared by the preparation method provided by the present invention, the correlation performance of the SiC crystal provided in examples 1 to 10 was tested, and specifically, see fig. 1 to 6.
The phase composition and the microstructure of the product are characterized by an X-ray diffractometer (XRD, SmartLab Japan society of Japan) and a scanning electron microscope (SEM, JSM 7001F Japan society of Japan electronic society).
The invention results are as follows:
1. influence of temperature on seed crystal induced microwave synthesis of SiC crystals
FIG. 1 shows XRD patterns of SiC crystals synthesized by seed crystal induced microwave as raw materials and provided in examples 1 to 4. The raw material in figure 1 is XRD spectrum of the ball-milled and mixed nano carbon black, silicon powder and SiC seed crystal, and as can be seen from figure 1, the power input rate is 400W/min, and the granularity of the SiC seed crystal is 5 μm. As can be seen from figure 1, the full reaction of the raw materials can be realized by keeping the temperature at 800 ℃ for 20min, and the SiC crystal is synthesized. And the crystallinity becomes better and better as the temperature increases.
FIG. 2 is an SEM photograph of a seed crystal induced microwave synthesized SiC crystal of the raw material and provided in examples 1 to 4.
The raw materials in fig. 2 are scanning electron microscope pictures obtained by ball milling and mixing nano carbon black, silicon powder and SiC seed crystals, and it can be seen from fig. 2 that small particles of nano SiC are attached to the silicon carbide seed crystals at 800 ℃, newly synthesized silicon carbide crystals gradually nucleate and grow on the silicon carbide seed crystals along with the temperature rise, and growth steps appear as shown in fig. 2. The silicon carbide crystal seed promotes the reaction of raw materials at a low temperature to induce nucleation and becomes a hot platform for the growth of the silicon carbide crystal at a high temperature.
2. The influence of the temperature rise rate on the synthesis of SiC crystal by seed crystal induced microwave.
FIG. 3 is an XRD (X-ray diffraction) pattern of a raw material and a SiC crystal synthesized by seed crystal induction microwave provided in examples 4 to 6, and FIG. 3 is an XRD pattern of a mixture obtained by ball-milling and mixing nano carbon black, silicon powder and SiC seed crystal as the raw material, and changes of phases of the SiC crystal synthesized by seed crystal induction microwave at power input rates of 200W/min, 400W/min and 600W/min. Wherein, fig. 3a is an XRD spectrum of a mixture obtained by ball-milling and mixing nano carbon black, silicon powder and SiC crystal seeds as raw materials; FIG. 3b is the XRD pattern of the crystal of SiC synthesized by seed crystal induced microwave provided in example 5; FIG. 3c is the XRD pattern of the crystal of SiC synthesized by microwave induced seeding provided in example 4; FIG. 3d is the XRD pattern of the crystal of SiC synthesized by seed crystal induced microwave provided in example 6;
as can be seen from FIG. 3, the full reaction of the raw materials can be realized when the temperature is raised to 1100 ℃ and kept for 20min at power input rates of 200W/min, 400W/min and 600W/min, and the SiC crystal is synthesized. And the crystallinity becomes better and better as the temperature rising rate increases.
FIG. 4 is an SEM photograph of the seed crystal induced microwave synthesized SiC crystal provided in examples 4-6, and FIG. 4 shows the change of the microscopic morphology of the seed crystal induced microwave synthesized SiC crystal at power input rates of 200W/min, 400W/min, and 600W/min, respectively. Wherein, fig. 4a is an SEM photograph of the seed crystal induced microwave synthesized SiC crystal provided in example 5; FIG. 4b is an SEM photograph of a seed crystal induced microwave synthesized SiC crystal provided in example 4; FIG. 4c is an SEM photograph of a seed crystal induced microwave synthesized SiC crystal provided in example 6;
as can be seen from FIG. 4, the temperature is raised to 1100 ℃ at a heating rate of 200W/min and is kept for 20min, the heating rate is relatively slow, and the particle size of the synthesized silicon carbide crystal is relatively small. With the increase of input power, the synthesized silicon carbide crystal has larger grain diameter, clear outline and better crystal morphology and structure at the temperature rise rate of 400W/min and 600W/min.
3. The influence of the grain size of the SiC seed crystal on the synthesis of SiC crystal by seed crystal induced microwave.
FIG. 5 is an XRD pattern of the seed crystal induced microwave synthesis SiC crystals provided in examples 4, 7 and 8, and FIG. 5 is a diagram showing the phase change of the seed crystal induced microwave synthesis SiC crystals under the condition of adding SiC seed crystals having particle diameters of 0.5 μm, 1 μm and 5 μm, respectively. Wherein fig. 6a is a SiC crystal XRD pattern provided in example 7, fig. 6b is a SiC crystal XRD pattern provided in example 8, and fig. 6c is a SiC crystal XRD pattern provided in example 4;
as can be seen from FIG. 5, the SiC crystal can be synthesized by heating to 1100 deg.C at a heating rate of 400W/min and maintaining the temperature for 20min under the condition of adding SiC seed crystals with particle sizes of 0.5 μm, 1 μm and 5 μm, respectively. And the crystallinity degree is better and better along with the increase of the grain size of the SiC seed crystal.
FIG. 6 is SEM photographs of the seed crystal induced microwave synthesized SiC crystals provided in examples 4, 7 and 8, and FIG. 6 shows the change of the microstructure of the seed crystal induced microwave synthesized SiC crystal under the condition of adding SiC seed crystals with particle sizes of 0.5 μm, 1 μm and 5 μm, respectively. Wherein, fig. 6a is the SEM photograph of the SiC crystal provided in example 7, fig. 6b is the SEM photograph of the SiC crystal provided in example 8, and fig. 6c is the SEM photograph of the SiC crystal provided in example 4;
as can be seen from FIG. 6, under the condition of raising the temperature to 1100 ℃ at the temperature raising rate of 400W/min and preserving the temperature for 20min, the silicon carbide crystal synthesized by the sample added with the SiC seed crystal with the small particle size of 0.5 μm has a smaller particle size, and the particle size of the synthesized silicon carbide powder is increased along with the increase of the particle size of the seed crystal, and the silicon carbide powder has a clear outline and better crystal morphology and structure.
In conclusion, in the process of synthesizing SiC by inducing microwaves through SiC seed crystals, SiC is used as a good microwave absorber material, and the SiC seed crystals are coupled with the microwaves to generate heat so as to promote the reaction of raw materials at low temperature; the SiC seed crystal can be used as a crystallization platform at high temperature to promote crystal nucleation and growth; therefore, in the microwave heating process, the SiC seed crystal can be used as a local hot spot to promote the reaction of the raw materials and can also be used as a crystal growth hot table to induce and synthesize SiC nucleation and in-situ growth. Compared with the seed crystal induction technology which is currently used in industry, the process greatly reduces the difficulty and the process conditions of SiC crystal synthesis; the synthesis of SiC by microwave and seed crystal composite induction has good application prospect.
The present invention describes preferred embodiments and effects thereof. Additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method for synthesizing SiC crystal by seed crystal induction microwave is characterized by comprising the following steps:
uniformly mixing silicon powder, nano carbon black and SiC seed crystal to obtain mixed powder, pressing the mixed powder into a blank, heating by microwave, and carrying out heat preservation at 800-1100 ℃ for 15-30 min to synthesize SiC crystal, thus obtaining the seed crystal induced microwave synthesized SiC crystal.
2. The preparation method of the SiC crystal by using the seed crystal to induce the microwave synthesis, according to claim 1, wherein the input rate of power is 200-600W/min in the microwave heating process.
3. The preparation method of the SiC crystal by seed crystal induction microwave synthesis according to claim 1, wherein the grain size of the SiC seed crystal is 0.5-5 μm, and the addition amount of the SiC seed crystal is 1-20 wt% of the total mass of the raw materials.
4. The preparation method of the SiC crystal by seed crystal induction microwave synthesis according to claim 1, wherein the molar ratio of the silicon powder to the nano carbon black is 1: 1 to 3.
5. The preparation method of the SiC crystal by seed crystal induction microwave synthesis according to claim 1, wherein the mixed powder is obtained by mixing silicon powder, nano carbon black and SiC seed crystal by a ball milling method with absolute ethyl alcohol as a dispersion medium, setting the rotating speed at 100r/min, performing ball milling for 12 hours, and then performing vacuum drying at 80 ℃ for 12 hours.
6. The preparation method of the SiC crystal by seed crystal induction microwave synthesis according to claim 5, wherein the particle size of the mixed powder is not less than 60 meshes.
7. The method for preparing the SiC crystal by the seed crystal induced microwave synthesis according to claim 1, wherein when the blank is heated, the blank is placed in an alumina crucible, and quartz sand powder is covered around the blank; and then placing the crucible into a heat insulation structure consisting of an alumina heat insulation box and mullite heat insulation cellucotton for microwave heating.
8. A seed crystal induced microwave synthesized SiC crystal prepared by the preparation method of any one of claims 1 to 7.
9. Use of the SiC crystal of claim 8 in electronic device semiconductors and heat exchangers.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110702201.6A CN113264774A (en) | 2021-06-24 | 2021-06-24 | SiC crystal synthesized by seed induced microwave and preparation method thereof |
PCT/CN2021/105386 WO2022267103A1 (en) | 2021-06-24 | 2021-07-09 | Seed crystal-induced microwave synthesized sic crystal and preparation method therefor |
DE112021007872.0T DE112021007872T5 (en) | 2021-06-24 | 2021-07-09 | THE SEED-INDUCED MICROWAVE SYNTHETIZED SiC CRYSTAL AND THE PRODUCTION METHOD |
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CN114685170A (en) * | 2022-04-29 | 2022-07-01 | 洛阳理工学院 | Method for synthesizing silicon carbide by microwave flash firing |
CN115582547A (en) * | 2022-10-18 | 2023-01-10 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
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Cited By (3)
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CN114685170A (en) * | 2022-04-29 | 2022-07-01 | 洛阳理工学院 | Method for synthesizing silicon carbide by microwave flash firing |
CN115582547A (en) * | 2022-10-18 | 2023-01-10 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
CN115582547B (en) * | 2022-10-18 | 2024-02-23 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
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