CN116332658A - High-strength high-heat-conductivity composite material for annular heating furnace and preparation method thereof - Google Patents
High-strength high-heat-conductivity composite material for annular heating furnace and preparation method thereof Download PDFInfo
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- CN116332658A CN116332658A CN202310062086.XA CN202310062086A CN116332658A CN 116332658 A CN116332658 A CN 116332658A CN 202310062086 A CN202310062086 A CN 202310062086A CN 116332658 A CN116332658 A CN 116332658A
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- silicon carbide
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000010438 heat treatment Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 98
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 98
- 238000005245 sintering Methods 0.000 claims abstract description 62
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 43
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000011029 spinel Substances 0.000 claims abstract description 36
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 36
- 230000001590 oxidative effect Effects 0.000 claims abstract description 32
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 46
- 229910052710 silicon Inorganic materials 0.000 claims description 46
- 239000010703 silicon Substances 0.000 claims description 46
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 42
- 229910052750 molybdenum Inorganic materials 0.000 claims description 42
- 239000011733 molybdenum Substances 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- 239000007767 bonding agent Substances 0.000 claims description 14
- 229920001353 Dextrin Polymers 0.000 claims description 3
- 239000004375 Dextrin Substances 0.000 claims description 3
- 235000019425 dextrin Nutrition 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 235000019580 granularity Nutrition 0.000 claims 4
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 40
- 229910000831 Steel Inorganic materials 0.000 abstract description 15
- 239000010959 steel Substances 0.000 abstract description 15
- 238000002844 melting Methods 0.000 abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011819 refractory material Substances 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 description 65
- 239000002184 metal Substances 0.000 description 65
- 238000007254 oxidation reaction Methods 0.000 description 19
- 230000003647 oxidation Effects 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 10
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 229910052863 mullite Inorganic materials 0.000 description 9
- 230000032683 aging Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 230000007774 longterm Effects 0.000 description 8
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 5
- 229910039444 MoC Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910000976 Electrical steel Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- 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
- C04B2235/401—Alkaline earth metals
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- 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
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- 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
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- 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
- C04B2235/428—Silicon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention discloses a high-strength high-heat-conductivity composite material for an annular heating furnace and a preparation method thereof, and belongs to the technical field of refractory materials. The composite material consists of a main material, a sintering agent, an antioxidant and a binding agent, wherein the main material is silicon carbide with different granularity, the sintering agent consists of alpha-alumina micropowder and aluminum magnesium spinel micropowder, and the composite material is prepared by three-step complex phase sintering. The composite material has the advantages of high silicon carbide content, low silicon dioxide content, high heat conductivity, high compressive strength, high load softening temperature, good thermal shock resistance, long service life and the like, and can solve the problems that SiO is generated by oxidizing SiC in the existing annular heating furnace lining material 2 Liquid phase material, siO 2 React with high-purity magnesium powder to generate low-melting matters which cause adhesion with steel plates and SiO under pure hydrogen atmosphere 2 Escape causes the problem of loose material structure.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a high-strength high-heat-conductivity composite material for an annular heating furnace and a preparation method thereof.
Background
The annular heating furnace is key equipment in the production of high-purity silicon steel, is responsible for the heating process before tube blank rolling, has complex operation working condition, is in oxidation-strong reduction (hydrogen-rich) -oxidation state for a long time according to different parts and feeding and discharging operations, has very harsh lining refractory material use environment due to the influence of factors such as high environmental temperature, frequent temperature rise and reduction, uneven high-temperature furnace gas convection, heavy load bearing of steel coil and the like in the annealing process, is subjected to alternating stress and scouring corrosion of high-temperature gas, particularly high-temperature hydrogen-rich atmosphere corrosion, and requires the lining material to have the characteristics of good thermal shock stability, high compressive strength, good high-temperature oxidation-reduction atmosphere corrosion resistance, good air flow scouring resistance and the like, and does not contain SiO 2 The component does not contain boron, phosphorus and other impurities, does not pollute the silicon steel and does not adhere to the contact surface of the silicon steel.
The prior art mostly adopts high-strength corundum mullite bricks, and has low heat conductivity coefficient and SiO during the use process 2 And the catalyst reacts with hydrogen in a strong reducing atmosphere, so that the binding capacity is lost, the porosity of the brick is increased, the structure is loose, and the service life is reduced by about half a year. In order to improve the heat conductivity, some attempts have been made to add SiC, silicon nitride-bonded SiC and oxide-bonded SiC, but because the production process of the annular heating furnace is oxidation-strong reduction (pure hydrogen) -oxidation atmosphere, siC reacts with oxygen in the oxidation atmosphere to generate a large amount of SiO 2 The film is adhered to the surface of the material, and reacts with high-purity magnesia to generate a large amount of low-melting substances in the use process, so that the low-melting substances are adhered to the steel plate, and great difficulty is brought to the quality of the steel plate and tapping.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to solve the problem of SiO generated by oxidation of SiC in the existing lining material of the annular heating furnace 2 And high-purity magnesite react to generate low-melting matters which are adhered to the steel plate, thereby providingA high-purity high-strength high-heat-conductivity composite material for an annular heating furnace and a preparation method thereof.
The invention provides a high-strength high-heat-conductivity composite material for an annular heating furnace, which is prepared from main materials, a sintering agent, an antioxidant and a binding agent, wherein the main materials are silicon carbide with different particle sizes, the sintering agent is composed of alpha-alumina micro powder and aluminum magnesium spinel micro powder, and the composite material comprises the following specific raw materials in parts by weight:
65-95 parts of silicon carbide,
3-7 parts of alpha-alumina micropowder,
1-2 parts of aluminum magnesium spinel micropowder,
4-11 parts of an antioxidant,
10-15 parts of a binding agent.
In one embodiment of the present invention, the silicon carbide is composed of 10 to 15 parts of silicon carbide with a particle size of 4 to 1mm, 25 to 35 parts of silicon carbide with a particle size of 1 to 0mm, and 30 to 45 parts of silicon carbide with a particle size of 200 meshes.
In one embodiment of the present invention, the fine α -alumina powder has a particle size of 1 to 5. Mu.m.
In one embodiment of the present invention, the particle size of the fine powder of aluminum magnesium spinel is 2 to 5. Mu.m.
In an embodiment of the invention, the antioxidant is composed of metallic silicon and/or metallic molybdenum.
In one embodiment of the present invention, the metal silicon is composed of 200 mesh, 325 mesh, 500 mesh.
In one embodiment of the present invention, the metal molybdenum is composed of 200 mesh, 325 mesh, 500 mesh.
In an embodiment of the invention, the antioxidant is composed of metallic silicon and metallic molybdenum.
In one embodiment of the present invention, the antioxidant is composed of 3-8 parts by weight of metallic silicon and 1-3 parts by weight of metallic molybdenum.
In an embodiment of the present invention, the binding agent is one or more selected from alumina gel, aluminum magnesium gel, white dextrin, and pulp.
In one embodiment of the present invention, the binder is composed of alumina gel and aluminum magnesium gel.
The second aspect of the invention provides a preparation method of a high-strength high-heat-conductivity composite material for an annular heating furnace, which is prepared by three-step complex phase sintering, and specifically comprises the following steps:
sintering at 1300-1450 deg.c in oxidizing atmosphere for 5-7 hr,
sintering at 1300-1450 deg.c in oxidizing atmosphere for 5-10 hr,
sintering at 1300-1550 deg.c in oxidizing atmosphere for 6-12 hr.
In one embodiment of the present invention, the preparation method specifically includes:
(1) Preparing raw materials according to a preset weight ratio;
(2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder;
(3) Mixing silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm, adding a bonding agent for mixing, and adding the premixed powder for mixing;
(4) Trapping the materials for 1-4 days, and performing high-pressure molding to obtain a blank;
(5) The composite material with high strength and high heat conductivity for the annular heating furnace is prepared by the three-step method complex phase sintering.
Compared with the prior art, the invention has the following technical effects:
(1) SiO caused by silicon carbide oxidation can be prevented by adding alpha-alumina micropowder and aluminum magnesium spinel micropowder as sintering agents 2 And (5) migration. The specific principle is as follows: the aluminum magnesium spinel micropowder can be mixed with SiO 2 Forming a small amount of glass phase to play a role in promoting sintering; alpha-alumina micropowder and aluminum-magnesium spinel micropowder can generate aluminum-magnesium spinel phase, alpha-alumina micropowder and SiO 2 The mullite phase can be formed, a small amount of glass phase, spinel phase and mullite phase are formed in the whole sintering reaction process, various ores are interwoven together to form a viscous liquid phase, and SiO caused by oxidation of SiC products can be blocked 2 And (5) migration.
(2) The particle size gradient connection of the antioxidant particles forms oxidation protection for silicon carbide. The antioxidant consists of particles with different particle size gradients, and the particles with different particle size gradients play a role in oxidation protection in different temperature ranges, and block the oxidation of silicon carbide to form a blocking barrier for preventing the oxidation of the silicon carbide. And a layer of compact and continuous glass thin-layer silicon oxide with self-healing capability is generated on the surface, so that further contact between silicon carbide and oxygen is isolated, and further oxidation of the silicon carbide is prevented. In addition, a secondary SiC phase can be generated, so that the structural stability is enhanced, and the thermal conductivity of the material is improved. The oxidation inhibitor adopts the combination of metallic silicon and metallic molybdenum, the silicon and the molybdenum not only can play the role of oxidation prevention, but also can react to generate molybdenum silicide, and compared with other oxidation inhibitors, the oxidation inhibitor can improve the high-temperature creep property and the impact resistance of the material. The metal silicon and the metal molybdenum are respectively composed of 200-mesh, 325-mesh and 500-mesh particles, and have a specific proportion, and when in sintering, the 500-mesh metal silicon and the metal molybdenum are firstly oxidized with silicon carbide to form gas phase SiO 2 And carbon in the gas phase to form high-melting point silicon carbide and high-melting point molybdenum carbide, and coating the surfaces of the silicon carbide particles, thereby preventing the silicon carbide from being oxidized continuously and forming silicon carbide (melting point 2700 ℃) and high-melting point molybdenum carbide (melting point 2692 ℃). The temperature is raised to 1000-1200 ℃,325 meshes of metallic silicon and metallic molybdenum continue to oxidize with silicon carbide to form gas phase SiO 2 Reacts with the carbon in the gas phase and encapsulates the silicon carbide particles, preventing the silicon carbide from being oxidized and continuing to form silicon carbide and high melting point molybdenum carbide. As the temperature continues to rise, 200 mesh metallic silicon and metallic molybdenum continue to form gas phase SiO with silicon carbide oxidation 2 And carbon in the gas phase, prevents the silicon carbide from being oxidized and continues to form silicon carbide and high melting point molybdenum carbide with the antioxidant. The process not only protects the silicon carbide from being oxidized, but also forms the gradient connection of granularity and generates high-melting-point carbide, so that each temperature point is provided with matched antioxidant which is easy to promote sintering and prevent oxidization, the porosity of the material is reduced, the volume density is improved, the toughness is increased, the capability of the material for bearing thermal stress impact is improved, and the material has higher thermal shock stability.
(3) The binder is preferably alumina gel and aluminum magnesium gel, and can be combined with aluminum magnesium gel at high temperature while utilizing its cementing capabilityFree SiO 2 The mullite phase and the spinel phase are secondarily generated, so that SiO is reduced 2 The content is as follows.
(4) The preparation method adopts three-step method complex phase sintering, so that the crystals of the mullite phase and the spinel phase generated by the secondary process are more stable, the mullite phase, the spinel phase and a large amount of SiC are combined together, the thermal conductivity of the material can be improved, the compressive strength is improved, and the SiO is enabled to be formed 2 The content is reduced to be extremely low, and adhesion with the contact surface of silicon steel is reduced.
(5) Through the use of the technical means, the problem that SiO is generated by oxidation of SiC in the existing annular heating furnace lining material can be solved 2 Liquid phase material, siO 2 React with high-purity magnesium powder to generate low-melting matters to cause adhesion with steel plates and SiO under pure hydrogen atmosphere 2 The composite material for the annular heating furnace has silicon carbide content of more than 87%, silicon dioxide content of less than 1%, high heat conductivity, heat conductivity coefficient of 31.2W/m.k at 300 ℃, heat conductivity coefficient of 20.5W/m.k at 1000 ℃, normal-temperature compressive strength of more than 150MPa and load softening temperature of 0.2MPa T0.6>The water cooling at 1700 ℃ and the thermal shock 1100 ℃ is more than or equal to 35 times, and the service life is more than 2 times that of the existing annular heating furnace lining material.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
Example 1
The raw material composition comprises the following components in parts by weight: 12 parts of silicon carbide with the granularity of 4-1mm, 30 parts of silicon carbide with the granularity of 1-0mm, 36 parts of silicon carbide with the granularity of 200 meshes, 4 parts of alpha-alumina micropowder, 1.5 parts of aluminum magnesium spinel micropowder, 5.5 parts of antioxidant and 11 parts of binding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 0.5 part of metal molybdenum with granularity of 200 meshes, 0.5 part of metal molybdenum with granularity of 325 meshes and 0.5 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a bonding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Example 2
The raw material composition comprises the following components in parts by weight: 15 parts of silicon carbide with the granularity of 4-1mm, 25 parts of silicon carbide with the granularity of 1-0mm, 41 parts of silicon carbide with the granularity of 200 meshes, 3 parts of alpha-alumina micropowder, 2 parts of aluminum magnesium spinel micropowder, 4 parts of antioxidant and 10 parts of binding agent. The antioxidant consists of 1 part of metal silicon with the granularity of 200 meshes, 2 parts of metal silicon with the granularity of 325 meshes and 1 part of metal silicon with the granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 5 minutes, adding a bonding agent, mixing for 5 minutes, and adding the premixed powder, mixing for 8 minutes; (4) ageing the materials for 1 day, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering for 7 hours at 1300 ℃ in an oxidizing atmosphere, sintering for 10 hours at 1300 ℃ in an oxidizing atmosphere, and sintering for 12 hours at 1300 ℃ in an oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Example 3
The raw material composition comprises the following components in parts by weight: 10 parts of silicon carbide with the granularity of 4-1mm, 25 parts of silicon carbide with the granularity of 1-0mm, 30 parts of silicon carbide with the granularity of 200 meshes, 7 parts of alpha-alumina micro powder, 2 parts of aluminum magnesium spinel micro powder, 11 parts of an antioxidant and 15 parts of a bonding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 2 parts of metal silicon with granularity of 500 meshes, 2 parts of metal molybdenum with granularity of 200 meshes, 2 parts of metal molybdenum with granularity of 325 meshes and 2 parts of metal molybdenum with granularity of 500 meshes. The binder consisted of 4 parts alumina gel, 4 parts aluminum magnesium gel, 4 parts white dextrin and 3 parts pulp.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 5 minutes, adding a bonding agent, mixing for 8 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the mixture for 3 days, and performing high-pressure forming to obtain a blank; and (5) three-step method complex phase sintering: sintering for 5 hours at 1300 ℃ in an oxidizing atmosphere, sintering for 6 hours at 1450 ℃ in the oxidizing atmosphere, and sintering for 6 hours at 1550 ℃ in the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Example 4
The raw material composition comprises the following components in parts by weight: 25 parts of silicon carbide with the granularity of 4-1mm, 55 parts of silicon carbide with the granularity of 1-0mm, 0 part of silicon carbide with the granularity of 200 meshes, 3 parts of alpha-alumina micropowder, 1 part of aluminum magnesium spinel micropowder, 6 parts of antioxidant and 10 parts of binding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 1 part of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 1 part of metal molybdenum with granularity of 200 meshes, 1 part of metal molybdenum with granularity of 325 meshes and 1 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 2 parts alumina gel and 8 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a binding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Comparative example 1 (sintering agent consisting of fine alpha-alumina powder alone, otherwise the same as in example 1)
The raw material composition comprises the following components in parts by weight: 12 parts of silicon carbide with the granularity of 4-1mm, 30 parts of silicon carbide with the granularity of 1-0mm, 36 parts of silicon carbide with the granularity of 200 meshes, 5.5 parts of alpha-alumina micropowder, 5.5 parts of antioxidant and 11 parts of bonding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 0.5 part of metal molybdenum with granularity of 200 meshes, 0.5 part of metal molybdenum with granularity of 325 meshes and 0.5 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder and an antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a bonding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Comparative example 2 (sintering agent consisting of fine powder of aluminum magnesium spinel only, otherwise the same as in example 1)
The raw material composition comprises the following components in parts by weight: 12 parts of silicon carbide with the granularity of 4-1mm, 30 parts of silicon carbide with the granularity of 1-0mm, 36 parts of silicon carbide with the granularity of 200 meshes, 5.5 parts of aluminum magnesium spinel micropowder, 5.5 parts of antioxidant and 11 parts of bonding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 0.5 part of metal molybdenum with granularity of 200 meshes, 0.5 part of metal molybdenum with granularity of 325 meshes and 0.5 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, aluminum magnesium spinel micropowder and an antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a bonding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Comparative example 3 (sintering agent consisting of clay, otherwise identical to example 1)
The raw material composition comprises the following components in parts by weight: 12 parts of silicon carbide with the granularity of 4-1mm, 30 parts of silicon carbide with the granularity of 1-0mm, 36 parts of silicon carbide with the granularity of 200 meshes, 5.5 parts of clay, 5.5 parts of antioxidant and 11 parts of bonding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 0.5 part of metal molybdenum with granularity of 200 meshes, 0.5 part of metal molybdenum with granularity of 325 meshes and 0.5 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon carbide with the granularity of 200 meshes, clay and an antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a bonding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
Comparative example 4 (silicon nitride was used as the main component, otherwise the same as in example 1)
The raw material composition comprises the following components in parts by weight: 12 parts of silicon carbide with the granularity of 4-1mm, 30 parts of silicon carbide with the granularity of 1-0mm, 36 parts of silicon nitride with the granularity of 200 meshes, 4 parts of alpha-alumina micropowder, 1.5 parts of aluminum magnesium spinel micropowder, 5.5 parts of antioxidant and 11 parts of bonding agent. The antioxidant consists of metal silicon and metal molybdenum, and comprises the following components in parts by weight: 1 part of metal silicon with granularity of 200 meshes, 2 parts of metal silicon with granularity of 325 meshes, 1 part of metal silicon with granularity of 500 meshes, 0.5 part of metal molybdenum with granularity of 200 meshes, 0.5 part of metal molybdenum with granularity of 325 meshes and 0.5 part of metal molybdenum with granularity of 500 meshes. The binder consisted of 6 parts alumina gel and 5 parts aluminum magnesium gel.
The preparation method comprises the following steps: (1) preparing raw materials according to a preset weight proportion; (2) Premixing silicon nitride with granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder; (3) Adding silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm into a mixing machine, mixing for 4 minutes, adding a bonding agent, mixing for 6 minutes, and adding the premixed powder, mixing for 10 minutes; (4) ageing the materials for 2 days, and forming under high pressure to obtain a blank; and (5) three-step method complex phase sintering: sintering at 1400 ℃ for 6 hours under an oxidizing atmosphere, sintering at 1450 ℃ for 7 hours under the oxidizing atmosphere, and sintering at 1500 ℃ for 9 hours under the oxidizing atmosphere to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
The composites prepared in examples 1-4 and comparative examples 1-4 above were tested to have the performance indices shown in Table 1 below
TABLE 1 Performance index of the composites prepared in examples 1-4 and comparative examples 1-4
The composite materials prepared in examples 1 to 4 and comparative examples 1 to 4 were put into a simulated environment of a ring-shaped heating furnace for testing, adhesion to steel plates was observed and service lives were estimated, and the results were shown in table 2 below:
table 2 adhesion of composite to steel plate and estimated service life
| Sample of | Adhesion to steel plate | Estimated service life |
| Example 1 | Substantially free of sticking and good in strength under long-term operating conditions | 1.5-2 years |
| Example 2 | Substantially free of sticking and good in strength under long-term operating conditions | 1.5-2 years |
| Example 3 | Substantially free of sticking and good in strength under long-term operating conditions | 1.5-2 years |
| Example 4 | Substantially free of sticking and good in strength under long-term operating conditions | 1.5-2 years |
| Comparative example 1 | With adhesion and loss of strength under long-term operating conditions | Half a year |
| Comparative example 2 | Has the advantages of adhesion and good adhesion,loss of strength under long-term operating conditions | Half a year |
| Comparative example 3 | With adhesion and loss of strength under long-term operating conditions | Half a year |
| Comparative example 4 | With adhesion and loss of strength under long-term operating conditions | Half a year |
As can be seen from table 2 above:
examples 1-4, which did not adhere to the steel sheet during use, were seen to prevent SiO 2 Migration to form SiO 2 The film reacts with the high-purity magnesite to generate low-melting matters, which is an effective means for solving the problem that the material is adhered to the steel plate.
The addition of the alpha-alumina micropowder and the aluminum-magnesium spinel micropowder plays a role in promoting sintering and can generate aluminum-magnesium spinel phase at the same time, and the alpha-alumina micropowder and SiO 2 The alpha-alumina micropowder can also form mullite phase, and can inhibit the decomposition of the aluminum-magnesium spinel micropowder, and the whole sintering reaction process has a small amount of glass phase, spinel phase, mullite phase and various ores which are interwoven together to form viscous liquid phase for blocking SiO caused by oxidation of SiC products 2 And (5) migration. The two sintering agents are used in a compounding way to enable the atmosphere to be alkaline, magnesium powder between a steel coil and a material can be replaced, adhesion between the steel coil and an aluminum-silicon material can be prevented, the toughness of the aluminum-magnesium spinel rivet can improve the capability of the material for coping with rapid cooling and rapid heating, and the load softening temperature of the material is improved, so that the service life is prolonged. On the other hand, the particle size gradient connection of the added antioxidant forms antioxidant protection for the silicon carbide and prevents the silicon carbide from oxidizing. In addition, the secondary SiC phase and the molybdenum carbide phase can be generated, the structural stability is enhanced, and the thermal conductivity of the material is improvedThe rate. Alumina gel and aluminum magnesium gel in the binder can be combined with free SiO at high temperature 2 The mullite phase and the spinel phase are secondarily generated, so that SiO is reduced 2 The content of the alloy is used for further preventing adhesion between the material and the steel plate. And after the sintering agents are adjusted in comparative examples 1-4, the technical effects are greatly different, the adhesion between materials and steel plates is serious, and the service life is reduced.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. The high-strength high-heat-conductivity composite material for the annular heating furnace is characterized by being prepared from main materials, sintering agents, anti-oxidation agents and binding agents, wherein the main materials are silicon carbide with different granularities, the sintering agents are composed of alpha-alumina micro powder and aluminum magnesium spinel micro powder, and the composite material comprises the following specific raw materials in parts by weight:
65-95 parts of silicon carbide,
3-7 parts of alpha-alumina micropowder,
1-2 parts of aluminum magnesium spinel micropowder,
4-11 parts of an antioxidant,
10-15 parts of a binding agent.
2. The composite material according to claim 1, wherein the silicon carbide consists of 10-15 parts of silicon carbide with a particle size of 4-1mm, 25-35 parts of silicon carbide with a particle size of 1-0mm, and 30-45 parts of silicon carbide with a particle size of 200 meshes.
3. The composite material according to claim 1, wherein the alpha-alumina micropowder has a particle size of 1-5 μm and/or the aluminium magnesium spinel micropowder has a particle size of 2-5 μm.
4. The composite material according to claim 1, wherein the antioxidant consists of metallic silicon and/or metallic molybdenum.
5. The composite material of claim 4, wherein the metallic silicon consists of 200 mesh, 325 mesh, 500 mesh,
and/or, the metallic molybdenum consists of 200 meshes, 325 meshes and 500 meshes.
6. The composite material according to claim 1, wherein the antioxidant consists of metallic silicon and metallic molybdenum, preferably the antioxidant consists of 3-8 parts by weight of metallic silicon and 1-3 parts by weight of metallic molybdenum.
7. The composite material of claim 1, wherein the binding agent is selected from one or more of alumina gel, aluminum magnesium gel, white dextrin, pulp.
8. The composite material of claim 1, wherein the binder consists of an alumina gel and an aluminum magnesium gel.
9. The method for preparing a composite material according to any one of claims 1 to 8, characterized in that it is prepared by three-step complex phase sintering, in particular:
sintering at 1300-1450 deg.c in oxidizing atmosphere for 5-7 hr,
sintering at 1300-1450 deg.c in oxidizing atmosphere for 5-10 hr,
sintering at 1300-1550 deg.c in oxidizing atmosphere for 6-12 hr.
10. The preparation method according to claim 9, characterized in that it comprises in particular:
(1) Preparing raw materials according to a preset weight ratio;
(2) Premixing silicon carbide with the granularity of 200 meshes, alpha-alumina micropowder, aluminum magnesium spinel micropowder and antioxidant to obtain premixed powder;
(3) Mixing silicon carbide with the granularity of 4-1mm and silicon carbide with the granularity of 1-0mm, adding a bonding agent for mixing, and adding the premixed powder for mixing;
(4) Trapping the materials for 1-4 days, and performing high-pressure molding to obtain a blank;
(5) The three-step method is adopted to perform complex phase sintering to prepare the high-strength high-heat-conductivity composite material for the annular heating furnace.
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| CN107879753A (en) * | 2017-11-24 | 2018-04-06 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of carborundum magnesia-aluminum spinel composite fire-resistant material |
| CN111662090A (en) * | 2020-07-07 | 2020-09-15 | 中钢集团洛阳耐火材料研究院有限公司 | Magnesium aluminate spinel-silicon carbide-aluminum composite refractory material |
| CN111704466A (en) * | 2020-07-07 | 2020-09-25 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide-magnesium aluminate spinel-aluminum composite refractory material |
| CN114988898A (en) * | 2022-07-15 | 2022-09-02 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon carbide-magnesia-alumina spinel non-fired refractory material |
| CN115286395A (en) * | 2022-08-10 | 2022-11-04 | 中南大学 | Modified SiC-based composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117430437A (en) * | 2023-12-20 | 2024-01-23 | 中钢洛耐科技股份有限公司 | Composite refractory material for regenerator cell of melting furnace and preparation method and application thereof |
| CN117430437B (en) * | 2023-12-20 | 2024-03-12 | 中钢洛耐科技股份有限公司 | Composite refractory material for regenerator cell of melting furnace and preparation method and application thereof |
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