CN115159997A - High-strength corrosion-resistant SiC refractory material and preparation method thereof - Google Patents
High-strength corrosion-resistant SiC refractory material and preparation method thereof Download PDFInfo
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- 230000007797 corrosion Effects 0.000 title claims abstract description 54
- 238000005260 corrosion Methods 0.000 title claims abstract description 54
- 239000011819 refractory material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 94
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 92
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229940075624 ytterbium oxide Drugs 0.000 claims abstract description 16
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000748 compression moulding Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000008878 coupling Effects 0.000 abstract description 13
- 238000010168 coupling process Methods 0.000 abstract description 13
- 238000005859 coupling reaction Methods 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 230000035939 shock Effects 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 4
- 239000011449 brick Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000011363 dried mixture Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- -1 Rare earth silicate Chemical class 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The SiC refractory material comprises the following raw materials: 80-95 parts of silicon carbide, 0.1-8 parts of ytterbium oxide and 3-15 parts of silica sol. The preparation method of the high-strength corrosion-resistant SiC refractory material comprises the steps of uniformly mixing 80-95 parts of silicon carbide, 0.1-8 parts of ytterbium oxide and 3-15 parts of silica sol, then carrying out compression molding under a certain pressure, drying, and then carrying out high-temperature sintering at 1200-1550 ℃ to obtain the high-strength corrosion-resistant SiC refractory material. The high-strength corrosion-resistant SiC refractory material prepared by the invention has small aperture, high strength and high temperature H resistance 2 O‑O 2 And the coupling corrosion performance is strong.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a high-strength corrosion-resistant SiC refractory material and a preparation method thereof.
Background
The SiC refractory material has excellent mechanical property and slag corrosion resistance and is used for a garbage incinerator, however, a large amount of water vapor and high-temperature H are generated in the garbage incineration process 2 O-O 2 The coupling environment seriously erodes the lining SiC refractory material.
The SiC refractory is a porous heterogeneous material, and comprises a binder phase and a large number of pores (the apparent porosity is about 5-20%). Because SiC has strong covalent bond bonding and low self-diffusion coefficient, the SiC is extremely difficult to sinter, densify and bondHas important influence on the service performance of the SiC refractory material. The spline shaft is connected to the SiO 2 The SiC brick has obviously raised strength (the hard disk, wangjianwan, huangzhigang, etc. refractory material 2020,54 (1): 70-73). Liyong SiC-Si composite material is subjected to high-temperature nitridation reaction to generate Si 3 N 4 And (4) combining SiC bricks. (Li Yong, zhu Xiao Yan, wang Jia Ping, et al., silicate academic, 2011,39 (3): 447-451.). However, the above-mentioned binder phase SiO 2 And Si 3 N 4 All can be heated by high temperature H 2 O-O 2 Etching to form Si (OH) 4 Gas (Liutao, he Libang. International thermal spray workshop and national thermal spray annual, 2018, 35-48.), severely corrodes furnace lining SiC refractories.
Disclosure of Invention
The invention aims to provide a high-temperature H resistant material with small aperture, high strength and high temperature resistance aiming at the defects of the prior art 2 O-O 2 A high-strength corrosion-resistant SiC refractory material with strong coupling corrosion performance and a preparation method thereof.
The invention relates to a high-strength corrosion-resistant SiC refractory material, which comprises the following raw materials: 80-95 parts of silicon carbide, 0.1-8 parts of ytterbium oxide and 3-15 parts of silica sol.
Further, the SiC content of the silicon carbide is more than or equal to 98wt%; the grain composition of the silicon carbide is as follows:
the silicon carbide accounts for 9 to 18 weight percent of the silicon carbide with the grain diameter of less than 5mm and more than or equal to 3 mm;
the silicon carbide accounts for 30-35wt% of the silicon carbide, and the grain diameter is less than 3mm and is more than or equal to 1 mm;
the silicon carbide accounts for 20-25wt% of the silicon carbide, and the grain diameter is less than 1mm and not less than 0.088 mm;
the silicon carbide accounts for 30-40wt% of the silicon carbide, and the grain diameter is less than 0.088mm and not less than 0.044 mm.
Further, yb of said ytterbium oxide 2 O 3 The content is more than or equal to 99wt%, and the grain diameter of the ytterbium oxide is less than or equal to 5 mu m.
Further, siO of the silica sol 2 The content is 25-30 wt%.
Further, the pH value of the silica sol is 9-11.
The preparation method of the high-strength corrosion-resistant SiC refractory material comprises the steps of uniformly mixing 80-95 parts of silicon carbide, 0.1-8 parts of ytterbium oxide and 3-15 parts of silica sol, then performing compression molding under a certain pressure, drying, and then performing high-temperature sintering at 1200-1550 ℃ to obtain the high-strength corrosion-resistant SiC refractory material.
Further, the pressure for press molding was 150MPa.
For SiC refractory materials containing a large number of pores, H2O-O2 firstly permeates into the materials through pores on the surfaces of the materials during high-temperature wet air corrosion, then is adsorbed on the surfaces of SiC particles and finally reacts with the SiC particles. The air holes are important for the influence of H2O-O2 coupling corrosion resistance of the SiC material. The smaller the pore diameter of the pore is, the more complex the pore structure is, the more difficult corrosive gas permeates into the material, the average pore diameter is reduced by regulating the microstructure of the SiC refractory material, and the gas permeability can be obviously reduced by improving the tortuosity of the pore channel, so that the gas corrosion resistance of the material is improved.
The invention introduces ytterbium oxide into the silica sol combined SiC refractory material, and a series of chemical reactions occur after high-temperature sintering in the air atmosphere. During sintering, the gaseous intermediate has a decisive influence on the structure and properties of the material, O in air 2 Enters the SiC brick to generate oxidation reaction to generate SiO (g) and CO (g) gases. SiO final oxidation product of SiC 2 Can be further combined with Yb 2 O 3 Reaction combined to form Yb 2 Si 2 O 7 A ceramic phase which retains SiO (g) and CO (g) gases in the green body to finally form microporous Yb 2 Si 2 O 7 Ceramic binder phase (pore size less than 5 μm). Simultaneously, the gas reacts to generate SiC crystal whiskers, and finally, micropores Yb are formed 2 Si 2 O 7 the-SiC whisker complex phase bonding phase greatly improves the mechanical property of the SiC brick after firing. Yb with pore size of less than 5 μm 2 Si 2 O 7 The network structure is tightly combined with the SiC matrix, and the micropores Yb 2 Si 2 O 7 The generation of-SiC whisker complex phase bonding phase reduces apparent porosity, simultaneously reduces aperture, complicates pore structure and can effectively reduce H under high temperature condition 2 The diffusion channel of O (g) obviously improves the high temperature of the materialThermal shock stability after water vapor corrosion.
Rare earth silicate Yb 2 Si 2 O 7 Has excellent H resistance 2 O-O 2 Coupled corrosion performance, thermal expansion coefficient close to that of SiC matrix, difficult thermal mismatch at high temperature, and in-situ generation of Yb in SiC refractory material 2 Si 2 O 7 The binder phase can improve resistance to aqueous oxygen corrosion.
The high-strength corrosion-resistant SiC refractory material prepared by the invention is detected as follows: the apparent porosity is 15-20%, the median diameter is 1-6 μm, and the normal-temperature flexural strength is 20-45MPa; h at 1000 DEG C 2 O-O 2 After 100h of coupling corrosion, the compressive strength is 15-35MPa, and after 5 times of thermal shock water cooling cycle tests, the residual compressive strength of a corroded sample is 10-25MPa.
Therefore, the high-strength corrosion-resistant SiC refractory material prepared by the invention has small aperture, high strength and high temperature H resistance 2 O-O 2 And the coupling corrosion performance is strong.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
Example 1
A high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The preparation method in this example is:
the high-strength corrosion-resistant SiC refractory material is prepared by taking 80-85wt% of silicon carbide, 4.5-8wt% of ytterbium oxide and 9-15wt% of silica sol as raw materials, uniformly mixing, then pressing and forming under the pressure of 150MPa, drying, and then sintering at the high temperature of 1200-1550 ℃.
The high-strength corrosion-resistant SiC refractory material prepared by the embodiment is detected as follows: the apparent porosity is 15-18%, the median diameter is 1-4 μm, and the normal-temperature flexural strength is 37-45MPa; h at 1000 DEG C 2 O-O 2 After 100h of coupling corrosion, the compressive strength is 30-35MPa, and after 5 times of thermal shock water cooling cycle tests, the residual compressive strength of the corroded sample is 21-25MPa.
Example 2
A high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The preparation method in this example is:
82-87wt% of silicon carbide, 4-7wt% of ytterbium oxide and 8-12wt% of silica sol are used as raw materials, the raw materials are uniformly mixed, then the mixture is pressed and formed under the pressure of 150MPa, and the dried mixture is sintered at the high temperature of 1200-1550 ℃ to prepare the high-strength corrosion-resistant SiC refractory material.
The high-strength corrosion-resistant SiC refractory material prepared by the embodiment is detected as follows: the apparent porosity is 16-18.5%, the median diameter is 2-4.5 μm, and the normal-temperature rupture strength is 32-38MPa; h at 1000 DEG C 2 O-O 2 After 100h of coupling corrosion, the compressive strength is 25-31MPa, and after 5 times of thermal shock water cooling cycle tests, the residual compressive strength of a corroded sample is 17-22MPa.
Example 3
A high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The preparation method in this example is:
86-91wt% of silicon carbide, 2-5wt% of ytterbium oxide and 5-10wt% of silica sol are used as raw materials, the raw materials are uniformly mixed, then the mixture is pressed and formed under the pressure of 150MPa, and the dried mixture is sintered at the high temperature of 1200-1550 ℃ to prepare the high-strength corrosion-resistant SiC refractory material.
The high-strength corrosion-resistant SiC refractory material prepared by the embodiment is detected as follows: the apparent porosity is 17-19%, the median diameter is 3-5 μm, and the normal-temperature flexural strength is 27-33MPa; h at 1000 DEG C 2 O-O 2 After 100h of coupling corrosion, the compressive strength is 21-26MPa, and after 5 times of thermal shock water cooling cycle tests, the residual compressive strength of a corroded sample is 15-20MPa.
Example 4
A high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The preparation method in this example is:
89-93wt% of silicon carbide, 1-4wt% of ytterbium oxide and 4-8wt% of silica sol are used as raw materials, the raw materials are uniformly mixed, then the mixture is pressed and formed under the pressure of 150MPa, and the mixture is baked at the high temperature of 1200-1550 ℃ after being dried, so that the high-strength corrosion-resistant SiC refractory material is prepared.
The high-strength corrosion-resistant SiC refractory material prepared by the embodiment is detected as follows: apparent porosity of18-20%, the median diameter is 4-5.5 μm, and the normal temperature flexural strength is 22-28MPa; h at 1000 DEG C 2 O-O 2 After 100h of coupling corrosion, the compressive strength is 18-22MPa, and the residual compressive strength of the corroded sample after 5 times of thermal shock water cooling cycle tests is 12-16MPa.
Example 5
A high-strength corrosion-resistant SiC refractory material and a preparation method thereof. The preparation method in this example is:
taking 90-95wt% of silicon carbide, 0.1-4wt% of ytterbium oxide and 3-8wt% of silica sol as raw materials, uniformly mixing, then pressing and molding under the pressure of 150MPa, drying, and then sintering at the high temperature of 1200-1550 ℃ to prepare the high-strength corrosion-resistant SiC refractory material.
The high-strength corrosion-resistant SiC refractory material prepared by the embodiment is detected as follows: the apparent porosity is 18-20%, the median diameter is 5-6 μm, and the normal-temperature flexural strength is 20-25MPa; h at 1000 DEG C 2 O-O 2 The compressive strength after 100h of coupling corrosion is 15-19MPa, and the residual compressive strength of the corroded sample after 5 times of thermal shock water cooling cycle tests is 10-14MPa.
The detection shows that the high-strength corrosion-resistant SiC refractory material prepared by the specific embodiment has the following characteristics: the apparent porosity is 15-20%, the median diameter is 1-6 μm, and the normal-temperature flexural strength is 20-45MPa; h at 1000 DEG C 2 O-O 2 The compressive strength after 100h of coupling corrosion is 15-30MPa, and the residual compressive strength of the corroded sample after 5 times of thermal shock water cooling cycle tests is 10-25MPa.
Therefore, the high-strength corrosion-resistant SiC refractory material prepared by the embodiment has small pore diameter, high strength and high-temperature H resistance 2 O-O 2 And the coupling corrosion performance is strong.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it should be understood by those skilled in the art that the foregoing description is for purposes of illustration only and not by way of limitation, and that various modifications, additions and substitutions can be made to the specific embodiments described without departing from the scope of the invention as defined in the accompanying claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (7)
1. A high-strength corrosion-resistant SiC refractory material is characterized by comprising the following raw materials: 80-95 parts of silicon carbide, 0.1-8 parts of ytterbium oxide and 3-15 parts of silica sol.
2. The high-strength corrosion-resistant SiC refractory according to claim 1, wherein the SiC content of the silicon carbide is not less than 98wt%; the grain composition of the silicon carbide is as follows:
the silicon carbide accounts for 9 to 18 weight percent of the silicon carbide with the grain diameter of less than 5mm and more than or equal to 3 mm;
the silicon carbide accounts for 30-35wt% of the silicon carbide, and the grain diameter is less than 3mm and is more than or equal to 1 mm;
the silicon carbide accounts for 20-25wt% of the silicon carbide, and the grain diameter is less than 1mm and not less than 0.088 mm;
the silicon carbide accounts for 30-40wt% of the silicon carbide, and the grain diameter is less than 0.088mm and more than or equal to 0.044 mm.
3. The SiC-based refractory material with high strength and corrosion resistance according to claim 1, wherein Yb of ytterbium oxide is 2 O 3 The content is more than or equal to 99wt%, and the grain size of the ytterbium oxide is less than or equal to 5 mu m.
4. The SiC-based refractory material with high strength and corrosion resistance according to claim 1, wherein SiO of the silica sol 2 The content is 25-30 wt%.
5. The SiC refractory according to claim 1, wherein the silica sol has a pH of 9 to 11.
6. The method for preparing a high-strength corrosion-resistant SiC refractory material according to any one of claims 1 to 5, wherein the high-strength corrosion-resistant SiC refractory material is prepared by uniformly mixing 80 to 95 parts of silicon carbide, 0.1 to 8 parts of ytterbium oxide and 3 to 15 parts of silica sol, then performing compression molding under a certain pressure, drying and then performing high-temperature sintering at 1200 to 1550 ℃.
7. The production method according to claim 6, wherein the pressure for press molding is 150MPa.
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