CN115536397B - Self-repairing silicon carbide refractory material for carbon-embedded atmosphere - Google Patents

Self-repairing silicon carbide refractory material for carbon-embedded atmosphere Download PDF

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CN115536397B
CN115536397B CN202211340865.3A CN202211340865A CN115536397B CN 115536397 B CN115536397 B CN 115536397B CN 202211340865 A CN202211340865 A CN 202211340865A CN 115536397 B CN115536397 B CN 115536397B
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silicon carbide
carbon
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powder
sialon
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CN115536397A (en
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曹会彦
吴吉光
郑翰
相宇博
黄志刚
张新华
李�杰
程竹
万龙刚
王建栋
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention relates to a self-repairing silicon carbide refractory material for a carbon-embedded atmosphere, and belongs to the technical field of refractory materials. In particular to a self-repairing silicon carbide refractory material for carbon-embedded atmosphere, which comprises beta-SiAlON and 9Al 2 O 3 ·2B 2 O 3 Silicon carbide is the main crystalline phase as the binding phase; the self-repairing silicon carbide refractory materials beta-SiAlON and 9Al used for carbon-embedded atmosphere 2 O 3 ·2B 2 O 3 The content of the silicon carbide main crystal phase is 10-30%, and the content of the silicon carbide main crystal phase is 70-90%. The self-repairing silicon carbide refractory material for the carbon-embedded atmosphere has high-temperature flexural strength under the carbon-embedded atmosphere condition, can generate proper amount of internal defects of the liquid phase repairing material under the high-temperature thermal stress condition, prevents the material from being cracked prematurely, and improves the service life by at least more than 2 times.

Description

Self-repairing silicon carbide refractory material for carbon-embedded atmosphere
Technical Field
The invention relates to a silicon carbide refractory material, in particular to a self-repairing silicon carbide refractory material for a carbon-embedded atmosphere.
Background
Compared with a carbon-embedded atmosphere, the nitride-combined silicon carbide refractory material shows more excellent high-temperature flexural strength and cracking resistance when applied in an air atmosphere or an atmosphere with higher oxygen partial pressure, so that the refractory material has longer service life; it is widely accepted by those skilled in the art that silicon carbide or nitride undergoes protective oxidation at high temperature, a compact siliceous protective film is formed on the surface of the material, and the protective film can prevent further permeation of oxidizing gas inside the material, thereby protecting the internal bonding phase from oxidation and maintaining the integrity of the original structure; meanwhile, a proper amount of liquid phase can repair internal defects of the material and prevent crack growth, namely, the self-repair of the nitride-combined silicon carbide material in an air atmosphere or an atmosphere with higher oxygen partial pressure is realized.
In the carbon-embedded atmosphere, the nitride-combined silicon carbide refractory material is forced to be taken off line in advance due to the lack of necessary oxidization and insufficient liquid phase generation mechanism, so that the refractory material cracks in the early stage of service; in particular to a high-temperature flexural strength detection experiment furnace pushing plate for a carbon-containing refractory material, because carbon in the carbon-containing material is prevented from being oxidized, the high-temperature flexural strength detection is carried out under the condition of carbon burying, the service life of a silicon carbide pushing plate is only 1 time and is cracked, and the silicon carbide pushing plate can be recycled for multiple times in the air atmosphere detection.
Disclosure of Invention
The invention aims to provide a self-repairing silicon carbide refractory material for a carbon-embedding atmosphere, which can improve the service life of various high-temperature kiln linings or supporting materials in or corresponding to the carbon-embedding condition service; wherein the high-temperature kiln which is in service under the carbon burying condition or is equivalent to the carbon burying condition comprises but is not limited to a high-temperature flexural strength detection experiment furnace pushing plate of the carbon burying atmosphere; the coke industry dry quenching furnace chute area is especially provided with a bracket, a ring beam and other parts of working linings; rotating the inclined cone section of the coke tank, the inner lining of the bottom gate and the like; the small coke oven furnace lining is used for a coal blending coking test in a coking plant; kiln deck plates such as aluminum carbon water gap, aluminum carbon sliding plate and the like for carbon burying heat treatment; push plate of a heat treatment furnace (carburization or carbonitriding), muffle, etc.; an asphalt tank for burning the anode material of the silicon-carbon battery, etc.
The invention adopts the following technical scheme for accomplishing the purposes:
self-repairing silicon carbide refractory for carbon-embedded atmosphereThe self-repairing silicon carbide refractory material for the carbon-embedded atmosphere is prepared from silicon powder, aluminum oxide micro powder and B 4 C powder and silicon carbide are used as raw materials; silicon powder nitriding reaction to generate silicon nitride; aluminum powder is nitrided to generate aluminum nitride, and then aluminum nitride and aluminum oxide micro powder are dissolved in silicon nitride generated by nitriding silicon powder to generate beta-SiAlON; b (B) 4 The oxygen element in the alumina micropowder in the raw material is extracted by the C powder and is sequentially converted into B with low melting point 2 O 3 Providing sufficient liquid phase for the generation of beta-SiAlON, and reducing the sintering temperature; in the latter stage of the reaction, B having a low melting point 2 O 3 Absorbing residual Al not participating in solid solution reaction 2 O 3 Conversion to high melting 9Al 2 O 3 ·2B 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The self-repairing silicon carbide refractory material takes silicon carbide as a main crystal phase and takes beta-SiAlON and 9Al 2 O 3 ·2B 2 O 3 Is a binding phase; well-developed columnar beta-SiAlON and whisker-like 9Al 2 O 3 ·2B 2 O 3 And organically combining to prepare the silicon carbide refractory material with the self-repairing function under the carbon embedding condition.
The reaction of beta-SiAlON generation is carried out in two steps: the first step of nitriding reaction of Si powder to generate Si 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Second step AlN and Al 2 O 3 In Si 3 N 4 The solid solution reaction in (2) produces beta-SiAlON.
The reaction and formation of the binding phase in the self-repairing silicon carbide refractory is achieved at 1350-1450 ℃ under nitrogen atmosphere.
beta-SiAlON and 9Al in self-repairing silicon carbide refractory materials 2 O 3 ·2B 2 O 3 The content of the bonding phase is 10% -30%, and the content of the main crystal phase of silicon carbide is 70% -90%; wherein the content of beta-SiAlON in the binding phase is 10-20%, 9Al 2 O 3 ·2B 2 O 3 The content is 5-10%.
The raw materials comprise the following components in percentage by mass: 8-15% of silicon powder, 1-5% of aluminum powder, 2-10% of aluminum oxide micropowder and B 4 The mass content of the C powder is 1-3%, and the mass content of the silicon carbide is 65-80%.
The preparation method of the self-repairing silicon carbide refractory material for the carbon-embedded atmosphere comprises the following steps: firstly uniformly mixing silicon carbide particles, then uniformly mixing a binding agent accounting for 1-3% of the total amount of the added raw materials and a solvent accounting for 0.5-3.5% of the total amount of the added raw materials, so that the binding agent forms a uniform film on the surfaces of the silicon carbide particles, and then adding pre-mixed silicon powder, aluminum oxide micro powder and B 4 Mixing the powder C and the silicon carbide fine powder uniformly, pressing a sample, loading the dried sample into a sintering furnace, heating to 1350-1450 ℃ in sections under the nitrogen atmosphere of 0.1Mpa, and preserving heat for 6-10 h at the temperature to obtain the self-repairing silicon carbide refractory material for carbon embedding atmosphere; the self-repairing silicon carbide refractory material for the carbon-embedding atmosphere prepared by the method has the service life which is more than 2 times that of the common nitride-combined silicon carbide refractory material under the carbon-embedding atmosphere condition or is equivalent to the high-temperature kiln lining or supporting material applied under the carbon-embedding atmosphere condition.
The self-repairing silicon carbide refractory material for the carbon-embedded atmosphere provided by the invention has high-temperature flexural strength under the carbon-embedded condition, and can generate proper amount of internal defects of the liquid phase repairing material under the high-temperature thermal stress condition, so that the material is prevented from being cracked prematurely, and the service life is prolonged;
B 4 conversion of C powder to Low melting Point B 2 O 3 Production of Si for nitriding Si powder 3 N 4 And aluminum nitride and added Al produced by nitriding aluminum powder 2 O 3 In Si 3 N 4 The beta-SiAlON generated by the solid solution reaction provides sufficient liquid phase, so that the beta-SiAlON can develop into a good columnar structure with higher length-diameter ratio, and a pulling-out toughening mechanism is generated in the material breaking process;
low melting point B in the late stage of reaction 2 O 3 By absorbing residual Al not participating in the solution reaction 2 O 3 Conversion of micropowder to higher melting 9Al 2 O 3 ·2B 2 O 3 A bonding phase, which is generally a whisker structure, which does not cause a hazard to high temperature flexural strength; at Al 2 O 3 And B 2 O 3 In the binary phase diagram, 2Al is formed below 1035 DEG C 2 O 3 ·B 2 O 3 Conversion to 9Al at 1035-1950deg.C 2 O 3 ·2B 2 O 3 And B is connected with 2 O 3 The liquid phases coexist. It can be seen that Al 2 O 3 And B 2 O 3 The material has the capability of generating a proper amount of liquid phase in a very wide temperature range, and simultaneously has the capability of being converted into a higher melting point substance along with the temperature rise, and can utilize the 9Al of the material under the condition that the service environment is buried carbon or the partial pressure of oxygen is equivalent to buried carbon 2 O 3 ·2B 2 O 3 And oxygen element reserved by beta-SiAlON to realize proper supply of liquid phase, thereby realizing self-repairing function under the condition of carbon burying.
The self-repairing silicon carbide refractory material for the carbon-embedded atmosphere has high-temperature flexural strength under the carbon-embedded condition, can generate proper amount of internal defects of the liquid phase repairing material under the high-temperature thermal stress condition, prevents the material from being cracked prematurely, and can improve the service life of various high-temperature kiln linings or supporting materials serving under the carbon-embedded condition or equivalent to the carbon-embedded condition. Wherein the high temperature kiln which is in service under or equivalent to the carbon burying condition comprises but is not limited to the following application fields: pushing plate of experimental furnace for detecting high-temperature flexural strength of carbon-embedded atmosphere; the coke industry dry quenching furnace chute area is especially provided with a bracket, a ring beam and other parts of working linings; rotating the inclined cone section of the coke tank, the inner lining of the bottom gate and the like; the small coke oven furnace lining is used for a coal blending coking test in a coking plant; kiln deck plates such as aluminum carbon water gap, aluminum carbon sliding plate and the like for carbon burying heat treatment; push plate of a heat treatment furnace (carburization or carbonitriding), muffle, etc.; an asphalt tank for burning the anode material of the silicon-carbon battery, etc.
Detailed Description
The invention will be described in detail with reference to specific examples:
example 1:
the self-repairing silicon carbide refractory material for the carbon-embedded atmosphere comprises the following final phase components: silicon carbide ratio of 70%, beta-SiAlON+9Al 2 O 3 ·2B 2 O 3 The proportion is 30%. The amount of Si powder introduced as a raw material was 15%, the amount of Al powder introduced was 1%, al 2 O 3 Micro powder (D) 50 =1 μm), B 4 The introduction amount of the C powder was 3%, the introduction amount of the 240 mesh SiC fine powder was 12%, and the introduction amount of the 0.1-1.43mm SiC particles was 59%. The binder is water-soluble amino resin, the apparent porosity of the product is 8.0%, and the volume density is 2.75g/cm 3 The high-temperature flexural strength of the carbon-embedded type steel is 65.0Mpa under the condition of carbon embedding at 1400 ℃.
Example 2:
the self-repairing silicon carbide refractory material for the carbon-embedded atmosphere comprises the following final phase components: silicon carbide ratio of 80%, beta-SiAlON+9Al 2 O 3 ·2B 2 O 3 The proportion is 20%. The amount of Si powder introduced as a raw material was 12%, the amount of Al powder was 5%, and Al 2 O 3 Micro powder (D) 50 =1 μm), B 4 The introduction amount of the C powder is 1%, the introduction amount of the 240 mesh SiC fine powder is 10%, the introduction amount of the 0.1-1.43mm SiC particles is 70%, the bonding agent is phenolic resin, the apparent porosity of the product is 9.0%, and the volume density is 2.60g/cm 3 The high-temperature flexural strength under the condition of carbon embedding at 1400 ℃ is 60.0Mpa,
example 3:
the self-repairing silicon carbide refractory material for the carbon-embedded atmosphere comprises the following final phase components: silicon carbide ratio of 90%, beta-SiAlON+9Al 2 O 3 ·2B 2 O 3 The proportion is 10%. The amount of Si powder introduced as a raw material was 8%, the amount of Al powder was 2%, al 2 O 3 Micro powder (D) 50 =1 μm), B 4 The introduction amount of the C powder is 2%, the introduction amount of the 240 mesh SiC fine powder is 8%, the introduction amount of the 0.1-1.43mm SiC particles is 76%, the binding agent is dextrin and calcium lignosulfonate, the apparent porosity of the product is 9.5%, and the volume density is 2.7g/cm 3 High-temperature flexural strength of 1400 ℃ is 50.0Mpa.

Claims (4)

1. A self-healing silicon carbide refractory material for use in a carbon-embedded atmosphere, characterized by: the self-repairing silicon carbide refractory material for the carbon-embedded atmosphere is prepared from silicon powder, aluminum oxide micro powder and B 4 C powder and silicon carbide are used as raw materials; silicon powder nitriding reaction to generate silicon nitride; aluminum powder is nitrided to form aluminum nitride, and then nitrogenDissolving aluminum oxide and aluminum oxide micropowder into silicon nitride generated by nitriding silicon powder to generate beta-SiAlON; b (B) 4 The oxygen element in the alumina micropowder in the raw material is extracted by the C powder and is sequentially converted into B with low melting point 2 O 3 Providing sufficient liquid phase for the generation of beta-SiAlON, and reducing the sintering temperature; in the latter stage of the reaction, B having a low melting point 2 O 3 Absorbing residual Al not participating in solid solution reaction 2 O 3 Conversion to high melting 9Al 2 O 3 ·2B 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the The self-repairing silicon carbide refractory material takes silicon carbide as a main crystal phase and takes beta-SiAlON and 9Al 2 O 3 ·2B 2 O 3 Is a binding phase; beta-SiAlON and 9Al in self-repairing silicon carbide refractory materials 2 O 3 ·2B 2 O 3 The content of the bonding phase is 10% -30%, and the content of the main crystal phase of silicon carbide is 70% -90%; wherein the content of beta-SiAlON in the binding phase is 10-20%, 9Al 2 O 3 ·2B 2 O 3 The content is 5-10%; well-developed columnar beta-SiAlON and whisker-like 9Al 2 O 3 ·2B 2 O 3 And organically combining to prepare the silicon carbide refractory material with the self-repairing function under the carbon embedding condition.
2. A self-healing silicon carbide refractory for use in a carbon-embedded atmosphere as claimed in claim 1, wherein: the reaction of beta-SiAlON generation is carried out in two steps: the first step of nitriding reaction of Si powder to generate Si 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Second step AlN and Al 2 O 3 In Si 3 N 4 The solid solution reaction in (2) produces beta-SiAlON.
3. A self-healing silicon carbide refractory for use in a carbon-embedded atmosphere as claimed in claim 1, wherein: the reaction and formation of the binding phase in the self-repairing silicon carbide refractory is achieved at 1350-1450 ℃ under nitrogen atmosphere.
4. A self-healing silicon carbide refractory for use in a carbon-embedded atmosphere as claimed in claim 1, wherein: the mass of each component in the raw materialsThe content is as follows: 8-15% of silicon powder, 1-5% of aluminum powder, 2-10% of aluminum oxide micropowder and B 4 The mass content of the C powder is 1-3%, and the mass content of the silicon carbide is 65-80%.
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