CN114835123B - Preparation method of cubic phase silicon carbide micron particles - Google Patents
Preparation method of cubic phase silicon carbide micron particles Download PDFInfo
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- CN114835123B CN114835123B CN202210570208.1A CN202210570208A CN114835123B CN 114835123 B CN114835123 B CN 114835123B CN 202210570208 A CN202210570208 A CN 202210570208A CN 114835123 B CN114835123 B CN 114835123B
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- 239000002245 particle Substances 0.000 title claims abstract description 45
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000004005 microsphere Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- YOBOXHGSEJBUPB-MTOQALJVSA-N (z)-4-hydroxypent-3-en-2-one;zirconium Chemical compound [Zr].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O YOBOXHGSEJBUPB-MTOQALJVSA-N 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000011859 microparticle Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000012798 spherical particle Substances 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004886 process control Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 150000003376 silicon Chemical class 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method of cubic phase silicon carbide micron particles belongs to the technical field of silicon carbide preparation and semiconductor material preparation, and aims to solve the problems of high cost, high reaction temperature, difficult process control, complex process, low yield, lower purity and uneven particle size distribution in the existing preparation method of cubic phase silicon carbide powder. The method comprises the following steps: treating the silicon dioxide microspheres in a hydrogen peroxide solution to obtain activated silicon source particles; preparing silicon dioxide microspheres loaded with zirconium acetylacetonate, introducing a gas carbon source under inert gas for high-temperature treatment, and removing impurities. In the invention, cobalt acetylacetonate is used as a shape regulator, silica microspheres are used as a shape template and the interaction between gaseous carbon sources, so that supersaturated linear growth of silicon carbide is effectively inhibited, and the morphology and the particle size of spherical particles are controlled. The method has the advantages of simplicity, moderate temperature, easy control, high production efficiency, high product purity and uniform particle size distribution. The method is suitable for preparing micron-sized cubic phase silicon carbide particles.
Description
Technical Field
The invention belongs to the technical field of preparation of silicon carbide and preparation of semiconductor materials, and particularly relates to a preparation method of cubic phase silicon carbide microparticles.
Background
The silicon carbide ceramic has the advantages of good mechanical property, oxidation resistance, wear resistance, thermal stability, thermal shock resistance, chemical corrosion resistance, small thermal expansion coefficient, large thermal conductivity and the like. Some silicon carbide of specific structure requires that the particles have a good spherical micro-morphology, with dimensions concentrated on the micrometer scale. However, the preparation process of micron-sized SiC particles aiming at spherical microcosmic morphology has the defects of low controllability, complex process, linear and granular mixed morphology, low purity of synthesized powder, uneven particle size distribution of powder particles, easy agglomeration of powder particles and the like. The cubic phase has outstanding advantages in all silicon carbide crystal forms, has excellent thermal conductivity and low expansion coefficient, and has ultrahigh strength even at the temperature of above 1600 ℃ and is several times higher than the conductivity of hexagonal or rhombohedral SiC.
Disclosure of Invention
The invention aims to solve the problems of high cost, high reaction temperature, difficult process control, complex process, low yield, lower purity and uneven particle size distribution in the existing preparation method of cubic phase silicon carbide powder, and provides a preparation method of cubic phase silicon carbide microparticles.
The preparation method of the cubic phase silicon carbide micron particles comprises the following steps:
1. dispersing silicon dioxide microspheres in hydrogen peroxide solution, taking out after 1-24 hours, and drying at 60-90 ℃ to obtain activated silicon source particles;
2. placing the activated silicon source particles in a cobalt acetylacetonate solution for treatment for 5-20 hours to obtain silicon dioxide microspheres loaded with zirconium acetylacetonate, then introducing a gas carbon source under inert gas for high-temperature treatment, and removing impurities from the obtained product to obtain cubic phase silicon carbide microparticles to complete the preparation method;
the mass volume ratio of the silicon dioxide microspheres to the hydrogen peroxide solution is 1g (10-50 ml);
the size of the silicon dioxide microsphere is 0.1-5 mu m;
the mass fraction of the hydrogen oxide solution is 10% -30%;
the concentration of the cobalt acetylacetonate solution is 0.05-0.6 mol/L, and the solvent is absolute ethanol or methanol;
the inert gas is argon, and the purity is 99.99%;
the gas carbon source is one or a combination of methanol gas and ethanol gas;
the high temperature treatment: heating to 1000-1200 ℃ at a speed of 1-3 ℃/min, and preserving heat for 3-6 h;
the impurity removal treatment comprises the following steps: the obtained product is treated by absolute ethyl alcohol, hydrofluoric acid and distilled water in sequence; the mass fraction of the hydrofluoric acid is 35%.
The reaction principle of the invention is as follows: spherical silicon dioxide microspheres are selected as a shape template, activated and loaded with cobalt acetylacetonate as a shape regulator, then a carbon source is introduced in a gas introducing mode under the protection of inert gas in a high-temperature environment, and the gaseous carbon source uniformly enters the silicon source to react under the existence of the cobalt acetylacetonate so as to realize the growth of silicon carbide particles. Under the surface modification effect of cobalt acetylacetonate, the hierarchical reaction of the gaseous carbon source and the silicon source can be ensured. The cobalt acetylacetonate can change the molten state, can assist the growth of silicon carbide particles in the molten state, modify crystal faces, and control particle morphology and particle size by controlling the supersaturation degree of gaseous intermediate products generated in the molten state, so that the prepared silicon carbide particles are uniform and stable in size, and the size magnitude of the adopted silicon dioxide microspheres is maintained.
The beneficial effects of the invention are as follows: by adopting cobalt acetylacetonate as a shape regulator and adopting the interaction between the silicon dioxide microspheres as a shape template and a gaseous carbon source, supersaturated linear growth of silicon carbide is effectively inhibited, and the morphology and the particle size of spherical particles are controlled. The preparation method is simple, the reaction temperature is moderate, and the process is easy to control, so that the production efficiency is improved, the product purity is high, the particle size distribution is uniform, and the method is suitable for large-scale industrial production.
The method is suitable for preparing micron-sized cubic phase silicon carbide particles.
Drawings
FIG. 1 is an XRD spectrum of cubic phase silicon carbide microparticles prepared in the examples;
fig. 2 is a graph of the microscopic morphology of the cubic phase silicon carbide microparticles prepared in the examples.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the cubic phase silicon carbide micron particles in the embodiment is realized by the following steps:
1. dispersing silicon dioxide microspheres in hydrogen peroxide solution, taking out after 1-24 hours, and drying at 60-90 ℃ to obtain activated silicon source particles;
2. and (3) placing the activated silicon source particles in a cobalt acetylacetonate solution for treatment for 5-20 hours to obtain silicon dioxide microspheres loaded with zirconium acetylacetonate, then introducing a gas carbon source under inert gas for high-temperature treatment, and removing impurities from the obtained product to obtain cubic phase silicon carbide microparticles to complete the preparation method.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is that the mass-volume ratio of the silica microsphere to the hydrogen peroxide solution in the first step is 1g (10-50 ml). Other steps and parameters are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiments in that the silica microspheres in the first step have a size of 0.1 to 5 μm. Other steps and parameters are the same as in the first or second embodiment.
The specific embodiment IV is as follows: the difference between the present embodiment and the first to third embodiments is that the mass fraction of the hydrogen oxide solution in the first step is 10% -30%. Other steps and parameters are the same as in one to three embodiments.
Fifth embodiment: the difference between the embodiment and the first to fourth embodiments is that the concentration of the cobalt acetylacetonate solution in the second step is 0.05-0.6 mol/L, and the solvent is absolute ethanol or methanol. Other steps and parameters are the same as in one to four embodiments.
Specific embodiment six: the difference between the present embodiment and one of the first to fifth embodiments is that the inert gas in the second step is argon, and the purity is 99.99%. Other steps and parameters are the same as in one of the first to fifth embodiments.
Seventh embodiment: the difference between the present embodiment and one of the first to sixth embodiments is that the gaseous carbon source in the second step is one or a combination of methanol gas and ethanol gas. Other steps and parameters are the same as in one of the first to sixth embodiments.
In the present embodiment, when the gaseous carbon source is a composition, the components are mixed in any ratio.
Eighth embodiment: this embodiment differs from one of the first to seventh embodiments in that the high temperature treatment in the second step: raising the temperature to 1000-1200 ℃ at the speed of 1-3 ℃/min, and preserving the heat for 3-6 h. Other steps and parameters are the same as those of one of the first to seventh embodiments.
Detailed description nine: the present embodiment is different from one of the first to eighth embodiments in that the impurity removal process in the second step: the obtained product is treated by absolute ethyl alcohol, hydrofluoric acid and distilled water in sequence. Other steps and parameters are the same as in one to eight of the embodiments.
Detailed description ten: this embodiment differs from the specific embodiment nine in that the mass fraction of hydrofluoric acid is 35%. Other steps and parameters are the same as in embodiment nine.
The beneficial effects of the invention are verified by the following examples:
examples:
the preparation method of the cubic phase silicon carbide micron particles comprises the following steps:
1. dispersing the silicon dioxide microspheres in a hydrogen peroxide solution, taking out after 6 hours, and drying at 80 ℃ to obtain activated silicon source particles;
2. and (3) placing the activated silicon source particles in a cobalt acetylacetonate solution for treatment for 6 hours to obtain silicon dioxide microspheres loaded with zirconium acetylacetonate, then introducing a gas carbon source under inert gas for high-temperature treatment, and removing impurities from the obtained product to obtain cubic phase silicon carbide microparticles to complete the preparation method.
The mass-volume ratio of the silica microspheres to the hydrogen peroxide solution in the step one of the embodiment is 1g to 50ml.
The silica microspheres in step one of this example were 1 μm in size.
The mass fraction of the hydrogen oxide solution in the first step of this example was 30%.
In the second step of this example, the concentration of the cobalt acetylacetonate solution was 0.2mol/L, and the solvent used was absolute ethanol.
In the second embodiment, the inert gas is argon, and the purity is 99.99%.
In the second embodiment, the gaseous carbon source is methanol gas.
The high temperature treatment in the second step of this embodiment: heating to 1000 ℃ at a speed of 1 ℃/min, and preserving heat for 4 hours.
In the second embodiment, the impurity removing process is as follows: the obtained product is treated by absolute ethyl alcohol, hydrofluoric acid and distilled water in sequence; the mass fraction of the hydrofluoric acid is 35%.
In the growth process of silicon carbide in the embodiment, silicon dioxide microspheres are used as a shape template, the surface of the silicon dioxide microspheres reacts with a gaseous carbon source after the introduction of cobalt acetylacetonate, the cobalt acetylacetonate can assist the growth of silicon carbide particles in a molten state, a crystal face is modified, the supersaturation degree of a gaseous intermediate product is generated in the molten state is controlled, and therefore the morphology and the particle size of the particles are controlled, so that the prepared silicon carbide particles are uniform and stable in size, and the size magnitude of the adopted silicon dioxide microspheres is maintained.
The cubic phase silicon carbide micron particles prepared based on the method of the invention in the embodiment are micron-grade silicon carbide spherical particles, and the X-ray diffraction (XRD) spectrogram of the cubic phase silicon carbide micron particles is shown in figure 1, and diffraction peaks at 35.7 degrees, 41.4 degrees, 60.0 degrees, 71.8 degrees and 75.4 degrees in the figure correspond to (111), (200), (220), (311) and (222) crystal faces of beta-SiC respectively; no impurity peaks were found, indicating that the cubic phase SiC material can be successfully prepared by the method of this example, and the purity of the product is high.
The microscopic morphology of the cubic phase silicon carbide micron particles prepared based on the method of the invention in the embodiment is shown in figure 2, and the average size of the cubic phase silicon carbide micron particles is similar to that of spherical silicon carbide particles with micron-sized average size.
Claims (3)
1. The preparation method of the cubic phase silicon carbide micron particles is characterized by comprising the following steps:
1. dispersing silicon dioxide microspheres in hydrogen peroxide solution, taking out after 1-24 hours, and drying at 60-90 ℃ to obtain activated silicon source particles;
2. placing the activated silicon source particles in a cobalt acetylacetonate solution for treatment for 5-20 hours to obtain silicon dioxide microspheres loaded with zirconium acetylacetonate, then introducing a gas carbon source under inert gas for high-temperature treatment, and removing impurities from the obtained product to obtain cubic phase silicon carbide microparticles to complete the preparation method;
wherein the mass volume ratio of the silicon dioxide microspheres to the hydrogen peroxide solution in the first step is 1g (10-50 ml);
the size of the silicon dioxide microsphere in the first step is 0.1-5 mu m;
the mass fraction of the hydrogen peroxide solution in the first step is 10% -30%;
the concentration of the cobalt acetylacetonate solution in the second step is 0.05-0.6 mol/L, and the solvent is absolute ethyl alcohol or methanol;
in the second step, the gas carbon source is one or a combination of methanol gas and ethanol gas;
the high temperature treatment in the second step: heating to 1000-1200 ℃ at a speed of 1-3 ℃/min, and preserving heat for 3-6 h;
the impurity removal treatment in the second step: the obtained product is treated by absolute ethyl alcohol, hydrofluoric acid and distilled water in sequence.
2. The method for preparing cubic phase silicon carbide micron particles according to claim 1, wherein the inert gas in the second step is argon gas, and the purity is 99.99%.
3. The preparation method of cubic phase silicon carbide micron particles according to claim 1, wherein the mass fraction of hydrofluoric acid is 35%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10020626A1 (en) * | 2000-04-27 | 2001-11-08 | Entwicklungsgesellschaft Elekt | Silicon carbide production from plant matter containing silica involves drying, pulverization and heating at a reaction temperature in reducing process gas atmosphere |
| JP2004161507A (en) * | 2002-11-11 | 2004-06-10 | National Institute For Materials Science | Silicon carbide nanorod and its production process |
| CN1636870A (en) * | 2004-12-30 | 2005-07-13 | 清华大学 | Nanometer SiC powder preparing process |
| JP2009269797A (en) * | 2008-05-08 | 2009-11-19 | Sumitomo Osaka Cement Co Ltd | Method for producing silicon carbide powder |
| CN106430212A (en) * | 2016-11-15 | 2017-02-22 | 扬州中天利新材料股份有限公司 | Method for industrialized mass production of silicon carbide powder |
| CN111446440A (en) * | 2020-05-22 | 2020-07-24 | 扬州大学 | Nitrogen-doped carbon-coated hollow mesoporous silica/cobalt nano composite material and lithium ion battery cathode material thereof |
| CN111646471A (en) * | 2020-06-22 | 2020-09-11 | 黑龙江冠瓷科技有限公司 | Preparation method of nano silicon carbide particles based on KCl shape regulator |
| CN113956049A (en) * | 2021-11-09 | 2022-01-21 | 北方民族大学 | Method for preparing high-density ceramic by pressureless sintering of beta-SiC powder synthesized by self-propagating combustion |
-
2022
- 2022-05-24 CN CN202210570208.1A patent/CN114835123B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10020626A1 (en) * | 2000-04-27 | 2001-11-08 | Entwicklungsgesellschaft Elekt | Silicon carbide production from plant matter containing silica involves drying, pulverization and heating at a reaction temperature in reducing process gas atmosphere |
| JP2004161507A (en) * | 2002-11-11 | 2004-06-10 | National Institute For Materials Science | Silicon carbide nanorod and its production process |
| CN1636870A (en) * | 2004-12-30 | 2005-07-13 | 清华大学 | Nanometer SiC powder preparing process |
| JP2009269797A (en) * | 2008-05-08 | 2009-11-19 | Sumitomo Osaka Cement Co Ltd | Method for producing silicon carbide powder |
| CN106430212A (en) * | 2016-11-15 | 2017-02-22 | 扬州中天利新材料股份有限公司 | Method for industrialized mass production of silicon carbide powder |
| CN111446440A (en) * | 2020-05-22 | 2020-07-24 | 扬州大学 | Nitrogen-doped carbon-coated hollow mesoporous silica/cobalt nano composite material and lithium ion battery cathode material thereof |
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| CN113956049A (en) * | 2021-11-09 | 2022-01-21 | 北方民族大学 | Method for preparing high-density ceramic by pressureless sintering of beta-SiC powder synthesized by self-propagating combustion |
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