CN114685170B - Method for synthesizing silicon carbide by microwave flash firing - Google Patents
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 42
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 21
- 238000010304 firing Methods 0.000 title claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000009768 microwave sintering Methods 0.000 claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 22
- 239000010703 silicon Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 16
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011863 silicon-based powder Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
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Abstract
The invention relates to a method for synthesizing silicon carbide by microwave flash sintering, which comprises the steps of firstly, uniformly mixing a silicon source and a carbon source, and then, directly placing the obtained mixed powder in a microwave sintering furnace for microwave sintering, or, preforming the mixed powder, and then placing the mixed powder in the microwave sintering furnace for microwave sintering; the microwave sintering process comprises the following steps: the input power of the microwave sintering furnace is increased to more than 3KW, after the temperature is rapidly increased to the set temperature, the baking is stopped immediately without heat preservation, and the microwave baking is completed to synthesize silicon carbide; the set temperature is not less than 600 ℃. The method has the advantages of rapid microwave heating, energy conservation and environmental protection, and can directly realize the synthesis of silicon carbide within one minute under high microwave input power after mixing the silicon source and the carbon source, so that the efficiency is extremely high, and the alpha-SiC with high purity can be prepared by the method.
Description
Technical Field
The invention relates to the technical field of inorganic nonmetallic material preparation, in particular to a method for synthesizing silicon carbide by microwave flash.
Background
Silicon carbide (SiC) ceramics have excellent high-temperature mechanical properties, strong oxidation resistance, good wear resistance, good thermal stability, small thermal expansion coefficient, large thermal conductivity, high elastic modulus, excellent high Wen Dianxing performance, high hardness, excellent thermal shock resistance, chemical corrosion resistance and other excellent properties, are increasingly widely applied to the fields of automobiles, mechanical engineering, environmental protection, space technology, information electronics, energy sources and the like, become an irreplaceable structural ceramic of other materials with excellent properties in a plurality of industrial fields, and are increasingly valued by people.
The synthesis method of SiC powder is mainly divided into three types:
(1) Solid phase methods including powder calcination, carbothermic reduction, self-propagating high temperature synthesis, and mechanical pulverization;
(2) Liquid phase processes, including sol-gel processes and polymer thermal decomposition processes;
(3) Vapor phase methods including chemical vapor deposition, plasma, and laser-induced methods.
Among them, the solid phase method has been widely used for industrial production due to advantages of low cost, easily available raw materials, etc. However, silicon carbide has extremely strong covalent bonds, so that at present, the synthesis of silicon carbide needs to be realized at high temperature (generally 1400-2700 ℃), the synthesis period is long and generally 5-100 hours, and a large amount of energy waste is caused.
It is apparent that the above-mentioned existing silicon carbide preparation method still has inconvenience and defects, and further improvement is needed, but no applicable method has been reported for a long time. Based on the abundant practical experience and expertise of the design and manufacture of the product for many years, the inventor actively researches and innovates to create a method for synthesizing silicon carbide by microwave flash, which can improve the defects that the general existing synthesis of silicon carbide needs to be completed at high temperature and the synthesis period is long, and finally creates the invention with practical value after continuous research and design and repeated sample and improvement.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a method for synthesizing silicon carbide by microwave flash combustion, which is used for realizing the synthesis of silicon carbide directly within one minute under high microwave input power after mixing a silicon source and a carbon source by virtue of the advantages of rapidness, energy conservation and environmental protection of microwave heating.
The invention aims at realizing the following technical scheme, and provides a method for synthesizing silicon carbide by microwave flash combustion, which specifically comprises the following steps:
(1) Uniformly mixing a silicon source and a carbon source;
(2) Directly placing the mixed powder into a microwave sintering furnace for microwave sintering, or performing the mixed powder in advance and then placing the powder into the microwave sintering furnace for microwave sintering; the microwave sintering process comprises the following steps: the input power of the microwave sintering furnace is increased to more than 3KW, after the temperature is rapidly increased to the set temperature, the baking is stopped immediately without heat preservation, and the microwave baking is completed to synthesize silicon carbide; the set temperature is not less than 600 ℃.
The method for synthesizing silicon carbide by microwave flash sintering, wherein the silicon source in the step (1) comprises one or more of silicon powder, tetraethoxysilane, quartz sand, white carbon black, silica sol and the like.
The method for synthesizing silicon carbide by microwave flash firing, wherein the carbon source in the step (1) comprises one or more of industrial coal, graphite, activated carbon, petroleum coke and the like.
The method for synthesizing silicon carbide by microwave flash combustion, wherein the molar ratio of carbon to silicon in the carbon source and the silicon source in the step (1) is 0.5-10: 1, a step of; the mixing mode includes but is not limited to ball milling, grinding, mechanical stirring and the like.
The method for synthesizing the silicon carbide by microwave flash sintering comprises the molding mode in the step (2) including, but not limited to, dry press molding, isostatic pressing molding, sol-gel molding and the like.
The method for synthesizing the silicon carbide by microwave flash firing, wherein the input power in the step (2) is 3 KW-10 KW during microwave firing, and the heating frequency is 915MHz or 2450MHz.
The method for synthesizing the silicon carbide by microwave flash firing finally prepares the alpha-SiC according to the method.
The method for synthesizing the silicon carbide by microwave flash firing, wherein the prepared alpha-SiC crystal has good development and is of a typical hexagonal structure.
The method for synthesizing the silicon carbide by microwave flash firing has potential great application value in the fields of preparing semiconductor materials, functional ceramics, advanced refractory materials and the like.
Compared with the prior art, the invention has obvious advantages and beneficial effects. By means of the technical scheme, the method for synthesizing the silicon carbide by microwave flash combustion can achieve quite technical progress and practicality, has wide utilization value, and has at least the following advantages:
according to the invention, by means of the advantages of rapidness in microwave heating, energy conservation and environmental protection, the silicon source and the carbon source are directly subjected to microwave sintering after being mixed, or the silicon carbide is synthesized within one minute after being preformed after being mixed, the efficiency is extremely high, the speed of preparing the alpha-SiC is greatly accelerated, the preparation period is shortened, compared with the sintering temperature (generally in the range of 1400-2700 ℃), the sintering temperature of the invention is remarkably reduced, the preparation of the alpha-SiC can be completed within one minute in the range of 600-1100 ℃, and the prepared alpha-SiC has extremely high purity, the purity is more than 99%, and can be applied to the preparation of semiconductor materials, functional ceramics, advanced refractory materials and the like.
The foregoing description is only an overview of the present invention, and is intended to be implemented in accordance with the teachings of the present invention, as well as the preferred embodiments thereof, together with the following detailed description of the invention, given by way of illustration only, together with the accompanying drawings.
Drawings
FIG. 1 is a scanning electron microscope image of silicon carbide prepared in example 1;
fig. 2 is an XRD pattern of silicon carbide prepared in example 1.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments and the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The invention provides a method for synthesizing silicon carbide by microwave flash combustion, which comprises the following steps:
(1) The silicon source and the carbon source are uniformly mixed by a ball milling method, a grinding method, a mechanical stirring method and the like.
The silicon source can be one or more of silicon powder, tetraethoxysilane, quartz sand, white carbon black, silica sol and the like.
The carbon source can be one or more of industrial coal, graphite, activated carbon, petroleum coke and the like; the molar ratio of carbon to silicon is 0.5-10: 1.
(2) The mixed powder is directly placed in a microwave sintering furnace for microwave sintering, or the mixed powder is preformed by dry press forming, isostatic pressing forming, sol-gel forming and other forming methods, and then placed in the microwave sintering furnace for microwave sintering.
The microwave sintering process comprises the following steps: the input power of the microwave sintering furnace is increased to more than 3KW, after the temperature is rapidly increased to the set temperature, the baking is stopped immediately without heat preservation, and the microwave baking is completed to synthesize alpha-SiC; the set temperature is not less than 600 ℃.
Preferably, the input power is 3 KW-10 KW during microwave sintering, and the heating frequency is 915MHz or 2450MHz.
Example 1:
selecting carbon powder with the particle size of 2000 meshes as a carbon source, silicon powder with the particle size of 1000 meshes as a silicon source, wherein the molar ratio of carbon to silicon is 1:1, taking alcohol as a grinding medium, and performing ball milling for 12 hours at 300r/min to mix the powder; and then placing the mixed powder in a microwave sintering furnace, adjusting the input power to 5KW, heating the mixed powder to 2450MHz, rapidly heating the sample to 800 ℃, and immediately ending firing without heat preservation to obtain the silicon carbide.
Fig. 1 is a scanning electron microscope image of silicon carbide prepared in this example, and as can be seen from fig. 1, the prepared silicon carbide crystal has a good development and is a typical hexagonal structure.
Fig. 2 is an XRD pattern of the silicon carbide prepared in this example, as can be seen from fig. 2: the prepared sample is pure alpha-SiC phase.
Example 2:
selecting active carbon with the grain size of 1000 meshes as a carbon source, silicon powder with the grain size of 325 meshes as a silicon source, wherein the carbon-silicon molar ratio is 2:1, alcohol as a grinding medium, and performing ball milling for 24 hours at 300r/min to perform powder mixing; and then placing the mixed powder in a microwave sintering furnace, adjusting the input power to 6KW, heating the mixed powder to 2450MHz, and immediately ending firing after the sample is rapidly heated to 700 ℃ without heat preservation to obtain the silicon carbide.
Example 3:
selecting petroleum coke with the particle size of 325 meshes as a carbon source, quartz sand with the particle size of 2000 meshes as a silicon source, wherein the molar ratio of carbon to silicon is 3:1, taking alcohol as a grinding medium, and performing ball milling for 24 hours at 300r/min to perform powder mixing; and then, the mixed powder is subjected to pressure maintaining for 2 minutes by using an isostatic press under the pressure of 20MPa to obtain a blank body. Placing the blank in a microwave sintering furnace, adjusting the input power to 4KW, heating the blank to 2450MHz, rapidly heating the sample to 900 ℃, and immediately ending firing without heat preservation to obtain the silicon carbide.
Example 4:
selecting graphite with the grain size of 1000 meshes as a carbon source, silicon powder with the grain size of 1000 meshes as a silicon source, wherein the molar ratio of carbon to silicon is 2:1, taking alcohol as a grinding medium, and performing ball milling for 24 hours at 300r/min to mix the powder; and then, the mixed powder is kept for 1min under the pressure of 50MPa by using a dry press to obtain a green body. Placing the blank in a microwave sintering furnace, adjusting the input power to 7KW, heating the blank to 915MHz, rapidly heating the sample to 1000 ℃, and immediately ending firing without heat preservation to obtain the silicon carbide.
Example 5:
selecting graphite with the grain size of 1000 meshes as a carbon source, silicon powder with the grain size of 1000 meshes as a silicon source, wherein the molar ratio of carbon to silicon is 1:1, taking alcohol as a grinding medium, and performing ball milling for 24 hours at 300r/min to mix the powder; and then, maintaining the pressure of the mixed powder for 5min by using an isostatic press under the pressure of 10MPa to obtain a blank. Placing the blank in a microwave sintering furnace, adjusting the input power to 3KW, heating the blank to 2450MHz, rapidly heating the sample to 650 ℃, and immediately ending firing without heat preservation to obtain the silicon carbide.
The foregoing description is only a specific embodiment of the present invention, and is not intended to limit the present invention in any way, and the present invention may have other embodiments according to the above structures and functions, which are not listed. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention without departing from the scope of the technical solution of the present invention will still fall within the scope of the technical solution of the present invention.
Claims (4)
1. The method for synthesizing the silicon carbide by microwave flash burning is characterized by comprising the following steps of:
(1) Uniformly mixing a silicon source and a carbon source, wherein the carbon-silicon molar ratio is (1-3): 1, a silicon source comprises one or more of silicon powder, tetraethoxysilane, quartz sand, white carbon black and silica sol, and a carbon source comprises one or more of industrial coal, graphite, activated carbon and petroleum coke;
(2) Directly placing the mixed powder into a microwave sintering furnace for microwave sintering, or performing the mixed powder in advance and then placing the powder into the microwave sintering furnace for microwave sintering;
the microwave sintering process comprises the following steps: the input power of the microwave sintering furnace is 5-6 kW, the heating frequency is 2450MHz, after the temperature is rapidly increased to 800-900 ℃, the sintering is immediately finished without heat preservation, and the microwave sintering is completed, so that the alpha-SiC with a hexagonal structure is obtained; or the input power of the microwave sintering furnace is 7kW, the heating frequency is 915MHz, the firing is immediately finished without heat preservation after the temperature is rapidly increased to 1000 ℃, and the microwave firing is finished, so that the alpha-SiC with a hexagonal structure is obtained.
2. The method of synthesizing silicon carbide by microwave flash sintering according to claim 1, wherein the mixing mode of the step (1) comprises ball milling or grinding or mechanical stirring.
3. The method of synthesizing silicon carbide by microwave flash sintering according to claim 1, wherein the molding in the step (2) comprises dry press molding, isostatic press molding or sol gel molding.
4. A method for synthesizing silicon carbide by microwave flash sintering as claimed in claim 1, wherein the prepared α -SiC is used for preparing semiconductor materials, functional ceramics or advanced refractory materials.
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| CN202210463925.4A CN114685170B (en) | 2022-04-29 | 2022-04-29 | Method for synthesizing silicon carbide by microwave flash firing |
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| CN202210463925.4A CN114685170B (en) | 2022-04-29 | 2022-04-29 | Method for synthesizing silicon carbide by microwave flash firing |
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