CN117088694A - Low-temperature sintering method of high-performance silicon carbide ceramic material - Google Patents
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 28
- 238000009766 low-temperature sintering Methods 0.000 title claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 239000002019 doping agent Substances 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 6
- 239000001095 magnesium carbonate Substances 0.000 claims description 6
- 238000009768 microwave sintering Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
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Abstract
The invention relates to the technical field of ceramic material preparation, in particular to a low-temperature sintering method of a high-performance silicon carbide ceramic material, which comprises the following steps of; preparing materials: selecting proper silicon carbide powder, selecting high-purity silicon carbide powder with the particle size range of 0.1-10 microns, and selecting proper doping agent powder; mixing materials: uniformly mixing silicon carbide powder and dopant powder to ensure that the dopant can be uniformly distributed in the silicon carbide ceramic material in the sintering process; briquetting treatment: briquetting the mixed silicon carbide powder and dopant powder to form a uniform pre-sintered block; sintering the presintered block in vacuum or protective atmosphere after low-temperature sintering. The invention has good mechanical property, heat resistance and oxidation resistance, breaks through the limit of the traditional sintering method, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a low-temperature sintering method of a high-performance silicon carbide ceramic material.
Background
Among the ceramic materials, silicon Carbide (CSi) ceramics have been widely used in the fields of aerospace, power electronics, chemical industry, automobiles, defense, etc., because of their excellent mechanical properties, excellent heat resistance and oxidation resistance.
However, the conventional sintering method of the CSi ceramic material generally requires a high temperature (usually more than 2000 ℃) and needs to maintain the high temperature for a long time, which not only has high energy consumption, but also has high requirements on equipment, and severely limits the application range thereof, so that the development of the method of the CSi ceramic material sintered at a low temperature is particularly important.
Disclosure of Invention
Based on the above purpose, the invention provides a low-temperature sintering method of a high-performance silicon carbide ceramic material.
A low-temperature sintering method of a high-performance silicon carbide ceramic material comprises the following steps of;
preparing materials: selecting proper silicon carbide powder, selecting high-purity silicon carbide powder with the particle size range of 0.1-10 microns, and selecting proper doping agent powder;
mixing materials: uniformly mixing silicon carbide powder and dopant powder to ensure that the dopant can be uniformly distributed in the silicon carbide ceramic material in the sintering process, wherein the mass ratio of the dopant powder to the silicon carbide powder is 1:10%;
briquetting treatment: briquetting the mixed silicon carbide powder and dopant powder to form a uniform pre-sintered block;
and (3) sintering at low temperature: sintering the presintered block in vacuum or protective atmosphere at a temperature lower than 2000 ℃, specifically 1500-1900 ℃ for 2-5 hours;
the product is obtained: the silicon carbide ceramic material obtained after sintering has good mechanical property, heat resistance and oxidation resistance, and has higher strength than the silicon carbide ceramic material obtained by the traditional sintering method.
Further, the dopant powder comprises one or more of aluminum oxide, aluminum nitride, magnesium carbonate, and calcium carbonate.
Further, the low-temperature sintering process is performed in vacuum or protective atmosphere.
Further, the protective atmosphere comprises one or more mixed gases of nitrogen, argon and helium.
Further, in the step 2, the mixing of the materials may be achieved by mechanical mixing, ultrasonic mixing or grinding mixing.
Further, in the step 3, the briquetting treatment may be cold press forming, and the pressure used is in the range of 20-200 MPa.
Further, the sintering process adopts one of microwave sintering, hot press sintering or flash heat sintering.
The invention has the beneficial effects that:
according to the invention, the silicon carbide powder and the dopant powder are uniformly mixed by adopting the dopant and powder metallurgy process, and then sintered at the temperature lower than 2000 ℃, so that the production cost is greatly reduced, the equipment requirement is reduced, and the finally obtained silicon carbide ceramic material has good mechanical property, heat resistance and oxidation resistance.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method according to an embodiment of the invention;
FIG. 2 is a schematic diagram of a sintering method according to an embodiment of the present invention.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1-2, a low temperature sintering method of a high performance silicon carbide ceramic material comprises the following steps;
step one: preparing materials: selecting proper silicon carbide powder, selecting high-purity silicon carbide powder with the particle size range of 0.1-10 microns, and selecting proper doping agent powder;
step two: mixing materials: uniformly mixing silicon carbide powder and dopant powder to ensure that the dopant can be uniformly distributed in the silicon carbide ceramic material in the sintering process, wherein the mass ratio of the dopant powder to the silicon carbide powder is 1:10%;
step three: briquetting treatment: briquetting the mixed silicon carbide powder and dopant powder to form a uniform pre-sintered block;
step four: and (3) sintering at low temperature: sintering the presintered block in vacuum or protective atmosphere at a temperature lower than 2000 ℃, specifically 1500-1900 ℃ for 2-5 hours;
step five: the product is obtained: the silicon carbide ceramic material obtained after sintering has good mechanical property, heat resistance and oxidation resistance, and has higher strength than the silicon carbide ceramic material obtained by the traditional sintering method.
The dopant powder comprises one or more of aluminum oxide, aluminum nitride, magnesium carbonate and calcium carbonate.
The low-temperature sintering process is carried out in vacuum or protective atmosphere.
The protective atmosphere comprises one or more mixed gases of nitrogen, argon and helium.
In the step 2, the mixed materials can be mixed mechanically, ultrasonically or by grinding.
In the step 3, the briquetting treatment can be cold press molding, and the pressure used is in the range of 20-200 MPa.
The sintering process adopts one of microwave sintering, hot pressing sintering or flash heat sintering.
The following are specific examples of the present invention.
Example 1
In this example, the silicon carbide powder has a particle size in the range of 1 micron and the dopant selected is alumina powder, the mass of the dopant being 3% of the mass of the silicon carbide powder. Mechanically mixing silicon carbide powder and aluminum oxide powder, and then adopting 100MPa pressure to perform cold press molding to form a presintered block. And then hot-pressing sintering is carried out in a nitrogen protection atmosphere at 1700 ℃ for 4 hours. The silicon carbide ceramic material obtained after sintering has excellent mechanical properties, heat resistance and oxidation resistance through X-ray diffraction and scanning electron microscope analysis.
Example 2
In this example, the silicon carbide powder has a particle size in the range of 2 microns and the dopant selected is calcium carbonate powder, the mass of dopant being 5% of the mass of the silicon carbide powder. After ultrasonic mixing, silicon carbide powder and calcium carbonate powder are subjected to cold press molding by adopting pressure of 150MPa, so as to form a presintered block. Then, the temperature is 1800 ℃ in an argon protection atmosphere, and the microwave sintering is carried out for 3 hours. The silicon carbide ceramic material obtained after sintering has excellent mechanical properties, heat resistance and oxidation resistance through X-ray diffraction and scanning electron microscope analysis.
Example 3
In this example, the silicon carbide powder had a particle size in the range of 0.5 microns and the dopant selected was aluminum nitride powder, the mass of dopant being 7% of the mass of the silicon carbide powder. Grinding and mixing silicon carbide powder and aluminum nitride powder, and then adopting 200MPa pressure to perform cold press molding to form a presintered block. Then flash sintering was performed in a mixed gas of nitrogen and argon at a temperature of 1900 ℃ for 2 hours. The silicon carbide ceramic material obtained after sintering has excellent mechanical properties, heat resistance and oxidation resistance through X-ray diffraction and scanning electron microscope analysis.
Example 4
In this example, the silicon carbide powder has a particle size in the range of 0.8 microns and the dopant selected is magnesium carbonate powder, the mass of the dopant being 10% of the mass of the silicon carbide powder. After ultrasonic mixing, silicon carbide powder and magnesium carbonate powder are subjected to cold press molding by adopting pressure of 75MPa, so as to form a presintered block. Then, the mixture was subjected to microwave sintering at 1850℃for 5 hours in a mixed gas of argon and helium. The silicon carbide ceramic material obtained after sintering has excellent mechanical properties, heat resistance and oxidation resistance through X-ray diffraction and scanning electron microscope analysis.
The following is a table of data versus experimental data between the various examples.
Comparison of example 1 with example 2:
comparison of example 3 with example 4:
| example 3 | Implementation of the embodimentsExample 4 | |
| Particle size of powder (micron) | 0.5 | 0.8 |
| Dopant(s) | Aluminum nitride | Magnesium carbonate |
| Dopant mass ratio (%) | 7 | 10 |
| Mixing mode | Grinding and mixing | Ultrasonic mixing |
| Pressure (MPa) | 200 | 75 |
| Sintering mode | Flash sintering | Microwave sintering |
| Protective atmosphere | Mixed gas of nitrogen and argon | Mixed gas of argon and helium |
| Sintering temperature (. Degree. C.) | 1900 | 1850 |
| Sintering time (hours) | 2 | 5 |
| Mechanical properties of materials (MPa) | 365 | 315 |
| Evaluation of Heat resistance | Excellent in | Excellent in |
| Evaluation of Oxidation resistance | Excellent in | Excellent in |
The two experimental data tables clearly show the specific operation differences among the examples and the mechanical property differences of the silicon carbide ceramic materials obtained after sintering, and can show that the silicon carbide ceramic materials obtained after sintering of all the examples have excellent mechanical properties, heat resistance and oxidation resistance, and prove the high efficiency and feasibility of the invention.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (7)
1. The low-temperature sintering method of the high-performance silicon carbide ceramic material is characterized by comprising the following steps of;
step one: preparing materials: selecting proper silicon carbide powder, selecting high-purity silicon carbide powder with the particle size range of 0.1-10 microns, and selecting proper doping agent powder;
step two: mixing materials: uniformly mixing silicon carbide powder and dopant powder to ensure that the dopant can be uniformly distributed in the silicon carbide ceramic material in the sintering process, wherein the mass ratio of the dopant powder to the silicon carbide powder is 1:10%;
step three: briquetting treatment: briquetting the mixed silicon carbide powder and dopant powder to form a uniform pre-sintered block;
step four: and (3) sintering at low temperature: sintering the presintered block in vacuum or protective atmosphere at a temperature lower than 2000 ℃, specifically 1500-1900 ℃ for 2-5 hours;
step five: the product is obtained: the silicon carbide ceramic material obtained after sintering has good mechanical property, heat resistance and oxidation resistance, and has higher strength than the silicon carbide ceramic material obtained by the traditional sintering method.
2. The method of claim 1, wherein the dopant powder comprises one or more of aluminum oxide, aluminum nitride, magnesium carbonate, and calcium carbonate.
3. The method for low-temperature sintering of high-performance silicon carbide ceramic material according to claim 1, wherein the low-temperature sintering process is performed in vacuum or a protective atmosphere.
4. A method of low temperature sintering a high performance silicon carbide ceramic material according to claim 3 wherein said protective atmosphere comprises one or more of nitrogen, argon and helium.
5. The method according to claim 1, wherein in the step 2, the mixed material may be obtained by mechanical mixing, ultrasonic mixing or grinding mixing.
6. The method according to claim 1, wherein in the step 3, the briquetting process is cold press forming, and the pressure is 20-200 MPa.
7. The method of claim 1, wherein the sintering process is one of microwave sintering, hot press sintering or flash thermal sintering.
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| US20130000212A1 (en) * | 2011-06-30 | 2013-01-03 | Saint-Gobain Ceramics & Plastics, Inc. | Liquid phase sintered silicon carbide abrasive particles |
| US20130207324A1 (en) * | 2010-07-30 | 2013-08-15 | Lg Innotek Co., Ltd. | Method for manufacturing silicon carbide sintered material using ball |
| WO2016186365A1 (en) * | 2015-05-18 | 2016-11-24 | 주식회사 원익큐엔씨 | Low-resistance silicon carbide ceramic material using atmospheric sintering scheme and method for manufacturing same |
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