CN110550940A - Ti (C, N) solid solution combined corundum-spinel refractory material and preparation method thereof - Google Patents

Ti (C, N) solid solution combined corundum-spinel refractory material and preparation method thereof Download PDF

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Publication number
CN110550940A
CN110550940A CN201910827707.2A CN201910827707A CN110550940A CN 110550940 A CN110550940 A CN 110550940A CN 201910827707 A CN201910827707 A CN 201910827707A CN 110550940 A CN110550940 A CN 110550940A
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corundum
refractory material
solid solution
resistance
percent
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李勇
孙洋
李宏宇
薛文东
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • 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
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to a Ti (C , N) solid solution combined corundum-spinel refractory material and a preparation method thereof, belonging to the field of refractory materials, wherein the material comprises 55-75 wt% of corundum, 5-20 wt% of fused magnesia, 1-15 wt% of titanium oxide, 1-15 wt% of metal aluminum and 2-6 wt% of phenolic resin as a binding agent, in the production process, the raw materials are weighed according to the proportion, uniformly mixed, mixed to obtain a pug, then pressed and molded, dried at 120-600 ℃ for 5-25h, and then sintered at 1200-1600 ℃ in a nitriding atmosphere for 5-25 h.

Description

Ti (C, N) solid solution combined corundum-spinel refractory material and preparation method thereof
Technical Field
the invention belongs to the technical field of refractory materials. In particular to a Ti (C, N) solid solution combined corundum-spinel refractory material and a preparation method thereof.
Background
Since the last 70 s, carbon composite refractory materials have been widely used in key parts of converters, electric furnaces, ladle slag lines, continuous casting systems and the like due to their excellent properties of high temperature resistance, thermal shock resistance, slag corrosion resistance and the like. In order to meet the requirements of special parts on thermal shock resistance and slag corrosion resistance, a large amount of graphite (10-20 wt%, and part of graphite reaches 30 wt%) is introduced into the traditional carbon composite refractory material (mainly magnesium carbon, aluminum carbon and zirconium carbon). For molten steel refining, the introduction of large amounts of graphite into the carbon-containing refractory material increases on the one hand the thermal conductivity of the material, while also running the risk of significant carburetion into the molten steel. In terms of energy conservation and emission reduction and the significance of smelting clean steel, the carbon content in the carbon composite refractory material must be controlled no matter in a molten steel refining or continuous casting system.
The Hongzaghuo, etc. in the research of non-oxide composite refractory material, the theory of metal-plastic phase composite refractory material and the process for realizing said material, i.e. transition-plastic phase process, are proposed. A certain amount of metal is added into the rigid inorganic oxide, and the metal changes the rigid forming of the original material into plastic forming in the material forming process, so that the blank making density is improved, and the porosity is reduced; in the sintering process, the metal phase is liquefied or softened, the pores are filled, and the metal phase reacts with the material and the ambient atmosphere to generate a non-oxide reinforced phase, so that the high-temperature strength and the thermal shock stability of the material are improved. The non-oxide has the same characteristic of being not easy to be wetted by molten steel as carbon, so that the oxide-non-oxide composite refractory material becomes a novel carbon-free refractory material for replacing the carbon composite refractory material.
Ti (C, N) is a non-oxide ceramic material with excellent performance and wide application, has the advantages of TiN and TiC, has the characteristics of high melting point, high hardness, wear resistance, oxidation resistance, corrosion resistance and the like, has good thermal conductivity, electrical conductivity and chemical stability, and has wide application in many fields of machinery, chemical engineering, automobile manufacturing, aerospace and the like. Iron-smelting workers prove that the use of the titanium-containing furnace charge is an effective means for protecting the hearth and the bottom of the furnace and prolonging the service life of the blast furnace through years of practice, and the reason is that titanium oxide is partially reduced in the iron-smelting process, so that a layer of slag crust mainly comprising TiC, TiN and Ti (C, N) is formed on the wall and the bottom of the blast furnace to play a good furnace protection role. It is thus demonstrated that Ti (C, N) can be an excellent non-oxide component in the refractory material.
Disclosure of Invention
The invention aims to prepare a Ti (C, N) solid solution combined corundum-spinel refractory material without oil immersion. The product introduces a novel non-oxide reinforcing phase Ti (C, N) into the corundum-spinel refractory material. The product has the characteristics of high strength, good thermal shock stability, good erosion resistance, long service life and the like.
The technical scheme of the invention is as follows:
The raw materials comprise 55-75% of corundum, 5-20% of fused magnesia, 1-15% of titanium oxide, 1-15% of metal aluminum, and phenolic resin accounting for 2-6% of the total amount of the raw materials as a binding agent.
The corundum particle size range is as follows: the granularity is not less than 1mm and not more than 3mm, the granularity is not less than 0.1mm and not more than 1mm, the granularity is not less than 0.1mm, and the granularity of the magnesia is as follows: the granularity is more than or equal to 0 and less than or equal to 1mm, and the granularity of the titanium oxide is as follows: the granularity is more than or equal to 0 and less than or equal to 0.1mm, and the granularity of the metal aluminum is as follows: the granularity is more than or equal to 0 and less than or equal to 0.1 mm.
the preparation method of the Ti (C, N) solid solution combined corundum-spinel refractory material is characterized by comprising the following steps: weighing the raw materials according to the proportion, uniformly mixing, mixing to obtain pug, then pressing and forming, drying at the temperature of 120-600 ℃ for 5-25h, and then sintering at the temperature of 1200-1600 ℃ for 5-25h to obtain the product.
The method is based on the transition plasticity theory, and the metal aluminum plays a role of a transition plasticity phase in the using process of the sliding plate, namely, part of the metal aluminum reacts with TiO 2 and other raw materials in the temperature rising process of the sliding plate to generate a non-oxide reinforcing phase Ti (C, N), and the rest of the metal aluminum is used as the transition plasticity phase, so that the Ti (C, N) solid solution combined corundum-spinel refractory material which does not contain easy-to-hydrate phases Al 4 C 3 and AlN and does not need an oil immersion process is prepared.
Positive effects of the invention
1. The invention prepares the Ti (C, N) solid solution combined corundum-spinel refractory material by using a transition plastic phase process, and Al 4 C 3 and AlN which are easy to hydrate do not exist in the material, so that the material has better hydration resistance.
2. The product obtained by the invention is a metal and nonmetal combined sliding plate, wherein the free aluminum can reduce the porosity of the material and play a role of a plastic phase, and the toughness and the thermal shock stability of the material are improved.
3. As AlN and Al 4 C 3 are not generated in the skateboard, the skateboard has good hydration resistance and is convenient for long-term storage.
4. The product of the invention introduces novel non-oxide reinforced phase Ti (C, N) into the refractory material, and improves the erosion resistance and high-temperature strength of the material.
5. The invention has excellent physical performance indexes, the apparent porosity is 2-15%, the volume density is 2.80-3.40g/cm 3, and the normal temperature compressive strength is 100-.
Detailed Description
Example 1: a preparation method of a Ti (C, N) solid solution combined corundum-spinel refractory material comprises the following raw materials in percentage by weight: 73 percent of corundum, 10 percent of fused magnesia, 2 percent of titanium oxide, 15 percent of metallic aluminum and 3.5 percent of thermosetting phenolic resin.
During production, weighing various raw materials according to a ratio, uniformly mixing, mixing to obtain pug, then pressing and molding by a friction brick press, and drying for 9 hours at 200 ℃; then sintering for 8h under 1400 ℃ nitriding atmosphere to obtain the product of the invention.
The powder material is metal aluminum powder with the granularity of less than 200 meshes, titanium oxide powder and partial corundum, the aggregate is corundum with the granularity of 3-1mm and 1-0.1mm and magnesia with the granularity of 1-0.1mm, the corundum is plate-shaped corundum and white corundum respectively, and the magnesia is fused magnesia.
The performance indexes of the obtained product are as follows: the apparent porosity is 12.2 percent, the volume density is 2.82g/cm3, the normal-temperature compressive strength is 202MPa, and the thermal shock resistance, the erosion resistance, the oxidation resistance and the hydration resistance are all better.
Example 2: the production process was the same as in example 1, except that:
The raw materials comprise the following components in percentage by weight: 71 percent of corundum, 10 percent of fused magnesia, 15 percent of metallic aluminum, 4 percent of titanium oxide and 3.5 percent of thermosetting phenolic resin. The performance indexes of the obtained product are as follows: the apparent porosity is 8.9 percent, the volume density is 2.89g/cm3, the normal-temperature compressive strength is 196MPa, and the thermal shock resistance, the erosion resistance, the oxidation resistance and the hydration resistance are all better.
Example 3: the production process was the same as in example 1, except that:
The raw materials comprise the following components in percentage by weight: 69 percent of corundum, 10 percent of fused magnesia, 15 percent of metallic aluminum, 6 percent of titanium oxide and 3.5 percent of thermosetting phenolic resin. The performance indexes of the obtained product are as follows: the apparent porosity is 6.7 percent, the volume density is 2.96g/cm3, the normal-temperature compressive strength is 198MPa, and the thermal shock resistance, the erosion resistance, the oxidation resistance and the hydration resistance of the material are good.
Example 4: the production process was the same as in example 1, except that:
The raw materials comprise the following components in percentage by weight: 67% of corundum, 10% of fused magnesia, 15% of metallic aluminum, 8% of titanium oxide and 3.5% of thermosetting phenolic resin. The performance indexes of the obtained product are as follows: 3.9 percent of apparent porosity, 2.99g/cm3 of volume density, 187MPa of normal-temperature compressive strength and better thermal shock resistance, erosion resistance, oxidation resistance and hydration resistance.
Example 5: the production process was the same as in example 1, except that:
The raw materials comprise the following components in percentage by weight: 65% of corundum, 10% of fused magnesia, 15% of metallic aluminum, 10% of titanium oxide and 3.5% of thermosetting phenolic resin. The performance indexes of the obtained product are as follows: the apparent porosity is 1.99 percent, the volume density is 3.02g/cm3, the normal-temperature compressive strength is 182MPa, and the thermal shock resistance, the erosion resistance, the oxidation resistance and the hydration resistance are all better.

Claims (3)

1. a refractory material of corundum-spinel combined with Ti (C , N) solid solution is prepared from corundum (55-75 wt.%), fused magnesite (5-20), titanium oxide (1-15), aluminium metal (1-15) and phenolic resin (2-6) as binder.
2. The Ti (C , N) solid solution bonded corundum-spinel refractory according to claim 1, wherein the corundum has a particle size of 1-3 mm, 0.1-1 mm, 0-0.1 mm, 0-0 mm, 0-1 mm, 0-0 mm, 0-0.1 mm, 0-0 mm, and 0-0.1 mm.
3. A method for preparing a Ti (C , N) solid solution combined corundum-spinel refractory material as claimed in claim 1 or 2, characterized in that the raw materials are weighed according to the proportion, mixed uniformly, mixed to obtain a pug, then pressed to form, dried at 120-600 ℃ for 5-25h, and then sintered at 1200-1600 ℃ in a nitriding atmosphere for 5-25h to obtain the product of the invention.
CN201910827707.2A 2019-09-03 2019-09-03 Ti (C, N) solid solution combined corundum-spinel refractory material and preparation method thereof Pending CN110550940A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647007A (en) * 2020-08-24 2021-04-13 河南熔金高温材料股份有限公司 Titanium-magnesia-alumina spinel-brown fused alumina composite sliding plate and production method thereof
CN114455941A (en) * 2022-01-19 2022-05-10 北京科技大学 Silicon-corundum-high titanium mullite composite refractory material for blast furnace and preparation method thereof
CN114956797A (en) * 2022-05-06 2022-08-30 中国矿业大学 Refractory castable for plasma melting furnace and preparation method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112647007A (en) * 2020-08-24 2021-04-13 河南熔金高温材料股份有限公司 Titanium-magnesia-alumina spinel-brown fused alumina composite sliding plate and production method thereof
CN114455941A (en) * 2022-01-19 2022-05-10 北京科技大学 Silicon-corundum-high titanium mullite composite refractory material for blast furnace and preparation method thereof
CN114455941B (en) * 2022-01-19 2022-12-13 北京科技大学 Silicon-corundum-high titanium mullite composite refractory material for blast furnace and preparation method thereof
CN114956797A (en) * 2022-05-06 2022-08-30 中国矿业大学 Refractory castable for plasma melting furnace and preparation method

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Application publication date: 20191210