CN109485442B - Preparation method of layered corundum-spinel refractory material - Google Patents

Preparation method of layered corundum-spinel refractory material Download PDF

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CN109485442B
CN109485442B CN201910029605.6A CN201910029605A CN109485442B CN 109485442 B CN109485442 B CN 109485442B CN 201910029605 A CN201910029605 A CN 201910029605A CN 109485442 B CN109485442 B CN 109485442B
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corundum
spinel
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layered
refractory material
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CN109485442A (en
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刘国齐
李红霞
杨文刚
陈勇强
于建宾
钱凡
马天飞
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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    • C04B35/803—
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/101—Refractories from grain sized mixtures
    • C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C04B35/443—Magnesium aluminate spinel
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon

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  • Ceramic Engineering (AREA)
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Abstract

The invention belongs to the technical field of refractory materials, and provides a preparation method of a layered corundum-spinel refractory material. The preparation method of the layered corundum-spinel refractory material comprises the following steps: selecting liquid ceramic precursor polysilazane as a framework material, aluminum sec-butoxide as a doped Al source, adding carbon-carbon double bonds by using divinyltoluene, and preparing a SiAlCN ceramic precursor by using cyclohexane as a solvent; mixing SiAlCN ceramic precursor, composite binder, Ni (NO3)2.6H2O and Al2O3 powder to obtain a mixture, and performing cold press molding on the mixture to obtain an alumina green body; preparing a spinel thin blank by tape casting; then, adopting hot-pressing lamination to alternately laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank; the spinel thin blank and the alumina blank are alternately laminated to prepare the multilayer synergistically enhanced ultra-low carbon corundum-spinel refractory material. The invention has good thermal shock resistance.

Description

Preparation method of layered corundum-spinel refractory material
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a preparation method of a layered corundum-spinel refractory material.
Background
Although the carbon component of the traditional carbon-containing refractory material improves the thermal shock resistance of the refractory material, under the action of high-temperature smelting, carbon is oxidized to form a porous structure in the refractory material, so that the strength of the material is reduced, the material is easy to be corroded and permeated by molten slag, and the content of carbon element in steel is also influenced. The long service life of the refractory material is always a problem in the high-temperature industry, and particularly the long service life of the refractory material for smelting advanced steel materials is a great challenge. The novel structural-function integrated refractory material with good matching of thermal shock resistance, erosion resistance, no pollution and the like is becoming a key point of concern at home and abroad. The existing research widely adopts ways of improving the components of the refractory materials, adding or generating in situ to protect and the like to optimize the erosion resistance, the thermodynamics and the mechanical properties of the refractory materials, but the optimization effect is still single and the good unification of the structural functions can not be achieved all the time. The layered composite material is used as a bionic design, and the fine structure of the layered composite material ensures the excellent comprehensive performance of the material. Therefore, the design and preparation of layered refractory materials are also receiving increasing attention.
Disclosure of Invention
The invention aims to provide a preparation method of a layered corundum-spinel refractory material, which can solve the problems of high carbon content, easy oxidation and easy erosion of the existing carbon-containing refractory material.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a layered corundum-spinel refractory material comprises the following steps:
1) selecting liquid ceramic precursor polysilazane as a framework material, aluminum sec-butoxide as a doped Al source, adding carbon-carbon double bonds by using divinyltoluene, and preparing a SiAlCN ceramic precursor by using cyclohexane as a solvent; selecting liquid phenolic resin and asphalt as a composite binder; adding Ni (NO3)2.6H2O which is decomposed to form Ni as a catalyst as an additive; mixing SiAlCN ceramic precursor, composite binder, Ni (NO3)2.6H2O and Al2O3 powder to obtain a mixture, and performing cold press molding on the mixture to obtain an alumina green body;
2) preparing a spinel thin blank with the thickness of 1-5mm by adopting tape casting; adopting hot-pressing lamination to alternately laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and heating to 1450-1600 ℃ at the speed of 2-5 ℃/min in an N2 atmosphere furnaceoC, preserving heat for 60-120min, turning off a power supply, and naturally cooling to room temperature; the method comprises the following steps of (1) pyrolyzing a Sicilian ceramic precursor to generate continuous ceramic fibers, wherein the continuous ceramic fibers form a three-dimensional space network structure in a refractory material; meanwhile, during the pyrolysis process of the Sicilian ceramic precursor, the generated carbon-containing gas is added with Ni (NO)3)2.6H2N formed after pyrolysis of Oi, generating carbon fibers for further improving the mechanical strength and the thermal shock resistance of the material under the action of a catalyst; the spinel thin blank and the alumina blank are alternately laminated to prepare the multilayer synergistically enhanced ultra-low carbon corundum-spinel refractory material.
The corundum-spinel refractory material is of a multilayer structure.
The carbon content of the corundum-spinel refractory material is less than 1 wt%.
The mixture in the step 1) comprises the following components in percentage by mass: al (Al)2O3The mass fraction of the powder is 80-90wt%, the particle size range is 2-3000 mu m, the composite binder is 5-10wt%, the SiAlCN ceramic precursor is 5-10wt%, and the additive is added, wherein the adding amount is 1-2wt% of the total mass of the mixed material.
The Al2O3 powder comprises the following raw materials in percentage by weight: 15wt% of 1-3mm plate corundum, 25wt% of 0-1mm plate corundum, 30wt% of 45 mu m plate corundum and 30wt% of 2 mu mAl2O3 fine powder.
The composite binder consists of resin and asphalt.
The additive Ni (NO3)2.6H2And O, which decomposes to form Ni as a catalyst to catalytically promote the formation of carbon fibers.
The thickness of the spinel thin blank in the step 2) is 1-5mm, and the raw material is 2 mu m of electric melting spinel.
Heating to 1450-oAnd C, preserving the temperature for 60-120min, turning off the power supply, and naturally cooling to room temperature.
According to the preparation method of the layered corundum-spinel refractory material, the Sicilian ceramic precursor is pyrolyzed to generate continuous ceramic fibers, the continuous ceramic fibers form a three-dimensional space network structure in the refractory material, and simultaneously, carbon-containing gas generated in the pyrolysis process generates carbon fibers under the action of a Ni catalyst, so that the mechanical strength and thermal shock resistance of the material can be further improved; the formation of three-dimensional space network structure and C fiber is inseparable from precursor content, catalyst and heat treatment condition; the catalytic efficiency of the catalyst is closely related to temperature, gas concentration and catalyst content; the content and distribution of the ceramic fibers are not negligible to the performance of the matrix material. The ultralow-carbon high-thermal-shock-resistance Al2O 3-based refractory material is prepared by regulating the concentration and content of a ceramic precursor, the heat treatment temperature and the atmosphere.
In the preparation method of the layered corundum-spinel refractory material, the thermal shock resistance, the erosion resistance and the mechanical property of the layered refractory material are determined by the component structure, the spatial configuration and the interface condition of the layered refractory material; respectively selecting Al2O3 single-layer refractory materials with different structures and dense high-corrosion-resistance single-layer MgAl2O4The material, carry on the alternate lamination of two or three with different thickness ratio; designing novel layered refractory materials with different spatial configurations and interface combination according to the intrinsic characteristics of different single-layer refractory materials; controlling a blank preparation process and a layered refractory material lamination technology, and optimizing a firing process system of the layered refractory material; preparing the layered corundum-spinel refractory material.
In the preparation method of the layered corundum-spinel refractory material, the corundum-spinel refractory material is of a multilayer structure, is enhanced by the three-dimensional ceramic network and the carbon fiber, and has good thermal shock resistance; in addition, the carbon content is lower than 1wt%, and the alloy belongs to an ultra-low carbon refractory material, is vital to clean steel smelting, and has a wide application prospect.
Drawings
FIG. 1 is a schematic view of a layered corundum-spinel structure;
fig. 2 is a SEM image of catalytically produced carbon fibers.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1:
the preparation method of the layered corundum-spinel refractory material of the embodiment comprises the following steps:
1) taking 15wt% of corundum with a plate of 1-3mm, 25wt% of corundum with a plate of 0-1mm, 30wt% of corundum with a plate of 45 mu m and 2 mu mAl2O330wt% of the fine powder, and high-speed mulling for 15min to obtain a mixture; taking 80wt% of the mixture, adding 10wt% of composite additive, adding 10wt% of SiAlCN precursor, and adding 6wt% of Ni (NO)3)2.6H2O, high speed kneadingAnd then, carrying out cold press molding to obtain an aluminum oxide blank with the thickness of 10 mm.
2) Preparing a spinel thin blank with the thickness of 2mm by adopting tape casting, wherein the raw material is 2 mu m of electric melting spinel; adopting hot-pressing lamination to alternatively laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and adding a solvent into the multilayer corundum-spinel blank2Heating to 1450-1600 deg.C/min in an atmosphere furnace at a rate of 2-5 deg.C/minoAnd C, preserving the heat for 60-120 min. And then, turning off a power supply, and naturally cooling to room temperature to obtain the layered corundum-spinel refractory material.
The porosity of the layered corundum-spinel refractory material obtained in the embodiment is 15% and 1100%oAfter water cooling, the strength retention rate was 80%.
Example 2
The layered corundum-spinel refractory of this example includes the following steps:
1) taking 15wt% of corundum with a plate of 1-3mm, 25wt% of corundum with a plate of 0-1mm, 30wt% of corundum with a plate of 45 mu m and 2 mu mAl2O3And (3) high-speed mulling the fine powder for 15min by 30wt% to obtain a mixture. Taking 80wt% of the mixture, adding 10wt% of composite additive, adding 10wt% of SiAlCN precursor, and adding 6wt% of Ni (NO)3)2.6H2And O, performing high-speed mixing, and performing cold press molding to obtain an aluminum oxide green body with the thickness of 10 mm.
2) Preparing a spinel thin blank with the thickness of 5mm by adopting tape casting, wherein the raw material is 2 mu m of electric melting spinel; adopting hot-pressing lamination to alternatively laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and adding a solvent into the multilayer corundum-spinel blank2Heating to 1450-1600 deg.C/min in an atmosphere furnace at a rate of 2-5 deg.C/minoAnd C, preserving the heat for 60-120 min. And then, turning off a power supply, and naturally cooling to room temperature to obtain the layered corundum-spinel refractory material.
The porosity of the layered corundum-spinel refractory material obtained in the embodiment is 12% and 1100%oAfter water cooling, the strength retention rate was 75%.
Example 3
The layered corundum-spinel refractory of this example includes the following steps:
1) taking 15wt% of corundum with a plate of 1-3mm, 25wt% of corundum with a plate of 0-1mm, 30wt% of corundum with a plate of 45 mu m and 2 mu mAl2O330wt% of the fine powder, and high-speed mulling for 15min to obtain a mixture; taking 90wt% of mixed material, adding 5wt% of composite additive, adding 5wt% of SiAlCN precursor and adding 6wt% of Ni (NO)3)2.6H2And O, performing high-speed mixing, and performing cold press molding to obtain an aluminum oxide green body with the thickness of 10 mm.
2) Preparing a spinel thin blank with the thickness of 5mm by adopting tape casting, wherein the raw material is 2 mu m of electric melting spinel; adopting hot-pressing lamination to alternatively laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and adding a solvent into the multilayer corundum-spinel blank2Heating to 1450-1600 deg.C/min in an atmosphere furnace at a rate of 2-5 deg.C/minoAnd C, preserving the heat for 60-120 min. And then, turning off a power supply, and naturally cooling to room temperature to obtain the layered corundum-spinel refractory material.
The porosity of the layered corundum-spinel refractory material obtained in the example is 10%, 1100%oAfter water cooling, the strength retention rate was 70%.
Example 4
The microwave sintering method of the alumina ceramic ball of the embodiment comprises the following steps:
1) taking 15wt% of corundum with a plate of 1-3mm, 25wt% of corundum with a plate of 0-1mm, 30wt% of corundum with a plate of 45 mu m and 2 mu mAl2O3And (3) high-speed mulling the fine powder for 15min by 30wt% to obtain a mixture. Taking 80wt% of the mixture, adding 10wt% of composite additive, adding 10wt% of SiAlCN precursor, and adding 6wt% of Ni (NO)3)2.6H2And O, performing high-speed mixing, and performing cold press molding to obtain an aluminum oxide green body with the thickness of 10 mm.
2) Preparing a spinel thin blank with the thickness of 2mm by adopting tape casting, wherein the raw material is 2 mu m of electric melting spinel; adopting hot-pressing lamination to alternatively laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and adding a solvent into the multilayer corundum-spinel blank2Heating to 1450-1600 deg.C/min in an atmosphere furnace at a rate of 2-5 deg.C/minoAnd C, preserving the heat for 60-120 min. And then, turning off a power supply, and naturally cooling to room temperature to obtain the layered corundum-spinel refractory material.
The porosity of the layered corundum-spinel refractory material obtained in the embodiment is 11% and 1100%oAfter water cooling, the strength retention rate was 75%.

Claims (8)

1. A preparation method of a layered corundum-spinel refractory material is characterized by comprising the following steps: comprises the following steps:
1) selecting liquid ceramic precursor polysilazane as a framework material, aluminum sec-butoxide as a doped Al source, adding carbon-carbon double bonds by using divinyltoluene, and preparing a SiAlCN ceramic precursor by using cyclohexane as a solvent; selecting liquid phenolic resin and asphalt as a composite binder; adding Ni (NO) which decomposes to form Ni as catalyst3)2·6H2O as an additive; the SiAlCN ceramic precursor, the composite binder and Ni (NO)3)2·6H2O and Al2O3Mixing the powder to obtain a mixture, and performing cold press molding on the mixture to obtain an aluminum oxide green body;
2) preparing a spinel thin blank with the thickness of 1-5mm by adopting tape casting, wherein the blank raw material is 2 mu m of electric melting spinel; adopting hot-pressing lamination to alternatively laminate the spinel thin blank and the alumina blank to prepare a multilayer corundum-spinel blank, and adding a solvent into the multilayer corundum-spinel blank2Heating to 1450-1600 ℃ at the speed of 2-5 ℃/min in the atmosphere furnace, preserving the temperature for 60-120min, turning off the power supply, and naturally cooling to room temperature; the method comprises the following steps that continuous ceramic fibers are generated after pyrolysis of a SiAlCN ceramic precursor, and the continuous ceramic fibers form a three-dimensional space network structure in a refractory material; meanwhile, during the pyrolysis process of the SiAlCN ceramic precursor, the generated carbon-containing gas is added into Ni (NO)3)2·6H2Generating carbon fibers for further improving the mechanical strength and the thermal shock resistance of the material under the action of a Ni catalyst formed after O pyrolysis; the spinel thin blank and the alumina blank are alternately laminated to prepare the multilayer synergistically enhanced ultra-low carbon corundum-spinel refractory material.
2. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the corundum-spinel refractory material is of a multilayer structure.
3. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the carbon content of the corundum-spinel refractory material is less than 1 wt%.
4. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the mixture in the step 1) comprises the following components in percentage by mass: al (Al)2O3The mass fraction of the powder is 80-90wt%, the particle size range is 2-3000 mu m, the composite bonding agent is 5-10wt%, the SiAlCN ceramic precursor is 5-10wt%, and the additive is added, wherein the adding amount is 1-2wt% of the total mass of the mixture.
5. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the Al is2O3The powder comprises the following raw materials in percentage by weight: 15wt% of corundum with 1-3mm plate, 25wt% of corundum with 0-1mm plate, 30wt% of corundum with 45 mu m plate and 2 mu mAl2O330wt% of fine powder.
6. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the additive Ni (NO)3)2·6H2And O, which decomposes to form Ni as a catalyst to catalytically promote the formation of carbon fibers.
7. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: the thickness of the spinel thin blank in the step 2) is 1-5mm, and the raw material is 2 mu m of electric melting spinel.
8. The method of claim 1, wherein the layered corundum-spinel refractory is prepared by: heating to 1450-oAnd C, preserving the temperature for 60-120min, turning off the power supply, and naturally cooling to room temperature.
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