CN116178023A - Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material - Google Patents

Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material Download PDF

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CN116178023A
CN116178023A CN202310142307.4A CN202310142307A CN116178023A CN 116178023 A CN116178023 A CN 116178023A CN 202310142307 A CN202310142307 A CN 202310142307A CN 116178023 A CN116178023 A CN 116178023A
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resistant
refractory material
silicon carbide
fine powder
combined
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王刚
刘鹏程
王来稳
杜鹏辉
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention relates to a heat shock resistant and oxidation resistant Si 3 N 4 A method for preparing a combined SiC refractory material. The technical proposal is as follows: silicon carbide and molybdenum disilicide particles with the particle diameters of 1-3mm and 0-1mm are used as aggregate, silicon carbide fine powder, molybdenum disilicide fine powder and metal silicon powder with the particle diameters of less than 0.064 mu m are used as matrixes, and water-soluble resin is used as a bonding agent. Taking proper contents of the raw materials, mixing the aggregate and the binding agent uniformly in an edge mill, then adding the uniformly mixed fine powder of the raw materials, stirring uniformly, and binding properly. Then press-forming on a friction brick press, firstly drying the green body at 110 ℃ for 24 hours, and preserving heat for 3-6 hours at 1400-1450 ℃ to obtain the heat shock resistant and oxidation resistant Si 3 N 4 And SiC refractory material is combined. The invention is thatMainly introduces molybdenum disilicide as a second phase, and effectively improves the thermal shock resistance and oxidation resistance of the material.

Description

Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material
Technical Field
The invention belongs to the technical field of inorganic nonmetallic materials. In particular to a heat shock resistant and oxidation resistant Si 3 N 4 A method for preparing a combined SiC refractory material.
Background
The use environment of the refractory brick lining of the supercharged boiler is very severe, the refractory brick bears severe temperature fluctuation of quenching and quenching, and the boiler frequently works under variable load in use, so that great thermal stress is generated, the material is damaged, the failure of the boiler can be directly caused, and the whole ship loses power. Therefore, the performance of the lining material directly affects the safety and reliability of the marine power plant. The silicon nitride combined silicon carbide refractory material product has excellent high-temperature use performances such as acid and alkali corrosion resistance, thermal shock resistance, scouring resistance and the like, and is widely applied to use environments such as heat resistance, wear resistance and the like in metallurgy, chemical industry and the like. However, si is seen from the practical effect of long-term application 3 N 4 The combined SiC material has the key application problems of poor impact resistance, serious oxidation and the like in service, and seriously influences the service life of refractory products and the normal operation of equipment. Enhancement of Si 3 N 4 The thermal shock resistance and oxidation resistance of the bonded SiC product are important optimization directions of the refractory materials.
MoSi 2 Has the advantages of high melting point (2030 ℃), good electric heat conductivity, excellent high-temperature oxidation resistance and the like, and MoSi 2 Has good physical and chemical compatibility with SiC, in particular MoSi 2 The material has metal-like soft plasticity at the temperature of more than 1000 ℃ and can greatly buffer the thermal stress of the material at high temperature. Therefore, the invention mainly comprises Si 3 N 4 Incorporation of MoSi in different ways and proportions in bonded SiC materials 2 Improves the high-temperature thermal shock resistance and high-temperature oxidation resistance of the material.
Disclosure of Invention
The invention aims at Si 3 N 4 The combined SiC material has the problems of poor shock resistance, serious oxidation and the like in service, the proportion of the material is optimized by adopting a mode of introducing third-phase molybdenum disilicide, the structure of the material is regulated by adopting three different modes of introducing molybdenum disilicide particles or fine powder, the particles and the fine powder together, and the prepared material has better oxidation resistance and thermal shock resistance.
The invention aims at realizing the following technical scheme:
thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material, thermal shock resistant and oxidation resistant Si 3 N 4 The main raw materials of the SiC-combined refractory material are silicon carbide particles, fine powder, molybdenum disilicide particles, fine powder and metal silicon powder; and water-soluble resin is adopted as a bonding agent; the method is characterized in that: the mass percentages of the raw materials are as follows: 15-30% of silicon carbide particles with the particle size of 1-3mm, 15-25% of silicon carbide particles with the particle size of 0-1mm, 10-20% of silicon carbide fine powder with the particle size of less than 0.062mm, 10-20% of molybdenum disilicide particles with the particle size of 1-3mm, 5-15% of molybdenum disilicide fine powder with the particle size of less than 0.062mm, 5-15% of metal silicon powder with the particle size of less than 280 meshes and 2-6% of water-soluble resin; silicon carbide particles and molybdenum disilicide particles are aggregate; according to the components and the proper content, the aggregate and the water-soluble resin are uniformly mixed in an edge runner mill, then the fine powder which is mixed in advance in the raw materials is added, the mixture is fully stirred in the edge runner mill, and the mixture is bundled; then pressing and forming on a friction brick press; firstly, drying the blank at 110 ℃ for 24 hours, and then, preserving heat for 3-6 hours under the nitrogen atmosphere at 1400-1450 ℃ for heat treatment, thus obtaining Si with good thermal shock resistance and oxidation resistance 3 N 4 And SiC refractory material is combined.
The SiC content of the silicon carbide particles is greater than 98.0%.
The SiC content in the silicon carbide fine powder is more than 98.0 percent
MoSi in the molybdenum disilicide particles 2 The content is more than 98.0 percent.
MoSi in the molybdenum disilicide fine powder 2 The content is more than 98.0 percent.
The Si content in the metal silicon powder is more than 98.0%.
The binder is water-soluble resin.
By using the technical scheme, unlike the in-situ synthesis of molybdenum disilicide by an infiltration method reported in the literature, the method directly adds pre-synthesized molybdenum disilicide particles or powder, can directly add the treated used silicon molybdenum rod as a raw material, realizes the recovery of waste materials, and responds to the concept of sustainable development; the invention has the following advantages:
introduction of presynthesis firstTwo-phase molybdenum disilicide can effectively improve Si 3 N 4 The oxidation resistance of the SiC refractory material is combined, so that the structural damage caused by rapid oxidation of the material in the use process is effectively relieved.
2. Molybdenum disilicide is metallic in soft plasticity at 1000 ℃ or higher, and Si can be improved by utilizing the property 3 N 4 Combines the high-temperature plasticity of the SiC refractory material, thereby improving the thermal shock resistance of the material.
Description of the embodiments
The invention is further described below in connection with the following detailed description.
Example 1: thermal shock resistant and oxidation resistant Si 3 N 4 The preparation method of the combined SiC refractory material comprises the following raw materials in parts by weight: 30% of silicon carbide particles with the particle size of 1-3mm, 15% of silicon carbide particles with the particle size of 0-1mm, 20% of silicon carbide fine powder with the particle size of less than or equal to 0.062mm, 15% of molybdenum disilicide particles with the particle size of 1-3mm, 10% of molybdenum disilicide fine powder with the particle size of less than or equal to 0.062mm, 10% of metal silicon powder and 4% of water-soluble resin.
Example 2: thermal shock resistant and oxidation resistant Si 3 N 4 The preparation method of the combined SiC refractory material comprises the following raw materials in parts by weight: 25% of silicon carbide particles with the particle size of 1-3mm, 20% of silicon carbide particles with the particle size of 0-1mm, 25% of silicon carbide fine powder with the particle size of less than or equal to 0.062mm, 10% of molybdenum disilicide particles with the particle size of 1-3mm, 10% of molybdenum disilicide fine powder with the particle size of less than or equal to 0.062mm, 10% of metal silicon powder and 4% of water-soluble resin.
Example 3: thermal shock resistant and oxidation resistant Si 3 N 4 The preparation method of the combined SiC refractory material comprises the following raw materials in parts by weight: 25% of silicon carbide particles with the particle size of 1-3mm, 20% of silicon carbide particles with the particle size of 0-1mm, 25% of silicon carbide fine powder with the particle size of less than or equal to 0.062mm, 20% of molybdenum disilicide particles with the particle size of 1-3mm, 10% of metal silicon powder and 4% of water-soluble resin.
Example 4: thermal shock resistant and oxidation resistant Si 3 N 4 The preparation method of the combined SiC refractory material comprises the following raw materials in parts by weight: 25% of silicon carbide particles with the particle size of 1-3mm, 20% of silicon carbide particles with the particle size of 0-1mm, and 25% of silicon carbide particles with the particle size of less than or equal to 0.062mm20% of fine silicon carbide powder, molybdenum disilicide powder with the particle size less than or equal to 0.062mm, 10% of metal silicon powder and 5% of water-soluble resin.
Example 5: thermal shock resistant and oxidation resistant Si 3 N 4 The preparation method of the combined SiC refractory material comprises the following raw materials in parts by weight: 20% of silicon carbide particles with the particle size of 1-3mm, 15% of silicon carbide particles with the particle size of 0-1mm, 20% of silicon carbide fine powder with the particle size of less than or equal to 0.062mm, 20% of molybdenum disilicide particles with the particle size of 1-3mm, 15% of molybdenum disilicide fine powder with the particle size of less than or equal to 0.062mm, 10% of metal silicon powder and 4% of water-soluble resin.
According to the components and the proper content, the aggregate and the binding agent are firstly mixed uniformly in an edge runner mill, then the fine powder of the raw materials which are mixed uniformly in advance is added, and the mixture is fully and uniformly stirred in the edge runner mill, so that the raw materials are properly bundled. And then is pressed and molded on a friction brick press. Firstly, drying the green body at 110 ℃ for 24 hours, and carrying out heat treatment for 3-6 hours in a nitrogen atmosphere at 1400-1450 ℃ to obtain Si with good thermal shock resistance and oxidation resistance 3 N 4 And SiC refractory material is combined. Through relevant performance tests, the refractory material has high thermal shock stability, water-cooling thermal shock is more than 20 times, and the high-temperature oxidation weight loss rate is greatly reduced.

Claims (6)

1. Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material, thermal shock resistant and oxidation resistant Si 3 N 4 The main raw materials of the SiC-combined refractory material are silicon carbide particles, fine powder, molybdenum disilicide particles, fine powder and metal silicon powder; and water-soluble resin is adopted as a bonding agent; the method is characterized in that: the mass percentages of the raw materials are as follows: 15-30% of silicon carbide particles with the particle size of 1-3mm, 15-25% of silicon carbide particles with the particle size of 0-1mm, 10-20% of silicon carbide fine powder with the particle size of less than 0.062mm, 10-20% of molybdenum disilicide particles with the particle size of 1-3mm, 5-15% of molybdenum disilicide fine powder with the particle size of less than 0.062mm, 5-15% of metal silicon powder with the particle size of less than 280 meshes and 2-6% of water-soluble resin; silicon carbide particles and molybdenum disilicide particles are aggregate; according to the above components and proper content, the aggregate and the water-soluble resin are firstly mixed uniformly in an edge mill, and then the raw materials are addedFully stirring the fine powder which is mixed in advance in an edge mill, and bundling the mixture; then pressing and forming on a friction brick press; firstly, drying the blank at 110 ℃ for 24 hours, and then, preserving heat for 3-6 hours under the nitrogen atmosphere at 1400-1450 ℃ for heat treatment, thus obtaining Si with good thermal shock resistance and oxidation resistance 3 N 4 And SiC refractory material is combined.
2. A heat shock resistant and oxidation resistant Si according to claim 1 3 N 4 The preparation method of the combined SiC refractory material is characterized by comprising the following steps: the SiC content of the silicon carbide particles is greater than 98.0%.
3. A heat shock resistant and oxidation resistant Si according to claim 1 3 N 4 The preparation method of the combined SiC refractory material is characterized by comprising the following steps: the SiC content of the silicon carbide fine powder is more than 98.0%.
4. A heat shock resistant and oxidation resistant Si according to claim 1 3 N 4 The preparation method of the combined SiC refractory material is characterized by comprising the following steps: moSi in the molybdenum disilicide particles 2 The content is more than 98.0 percent.
5. A heat shock resistant and oxidation resistant Si according to claim 1 3 N 4 Preparation method of combined SiC refractory material, wherein MoSi in molybdenum disilicide fine powder 2 The content is more than 98.0 percent.
6. A heat shock resistant and oxidation resistant Si according to claim 1 3 N 4 The preparation method of the combined SiC refractory material is characterized by comprising the following steps: the Si content in the metal silicon powder is more than 98.0%.
CN202310142307.4A 2023-02-21 2023-02-21 Thermal shock resistant and oxidation resistant Si 3 N 4 Preparation method of combined SiC refractory material Pending CN116178023A (en)

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US5130055A (en) * 1987-04-10 1992-07-14 Yoshiyuki Yasutomi Ceramic composite and process for the production thereof
JPH04114968A (en) * 1990-08-31 1992-04-15 Ngk Insulators Ltd Silicon nitride-based sic refractory material and production thereof
US5292691A (en) * 1992-01-13 1994-03-08 United Technologies Corporation Molybdenum disilicide matrix composites reinforced with continuous ceramic fibers
JP2004131318A (en) * 2002-10-09 2004-04-30 National Institute Of Advanced Industrial & Technology Joined body of silicon carbide-based member and method of manufacturing the same
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