CN116693276B - TiN-MgAlON-Al2O3Composite refractory material, preparation method and application - Google Patents
TiN-MgAlON-Al2O3Composite refractory material, preparation method and application Download PDFInfo
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- 239000011819 refractory material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 85
- 239000002131 composite material Substances 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 43
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 42
- 239000010431 corundum Substances 0.000 claims abstract description 40
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 25
- 238000005121 nitriding Methods 0.000 claims abstract description 24
- 238000007670 refining Methods 0.000 claims abstract description 22
- 239000011230 binding agent Substances 0.000 claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 229920001187 thermosetting polymer Polymers 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 28
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 239000000463 material Substances 0.000 abstract description 19
- 229910000831 Steel Inorganic materials 0.000 abstract description 17
- 239000010959 steel Substances 0.000 abstract description 17
- 239000000203 mixture Substances 0.000 abstract description 14
- 229910010038 TiAl Inorganic materials 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 9
- 229910045601 alloy Inorganic materials 0.000 abstract description 8
- 239000000956 alloy Substances 0.000 abstract description 8
- 239000007787 solid Substances 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 229910001209 Low-carbon steel Inorganic materials 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 17
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 239000011449 brick Substances 0.000 description 9
- 230000003628 erosive effect Effects 0.000 description 9
- 230000035939 shock Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000003014 reinforcing effect Effects 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000007767 bonding agent Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910021392 nanocarbon Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910018514 Al—O—N Inorganic materials 0.000 description 1
- 241001408630 Chloroclystis Species 0.000 description 1
- 229910004349 Ti-Al Inorganic materials 0.000 description 1
- 229910004692 Ti—Al Inorganic materials 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/10—Handling in a vacuum
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/0003—Linings or walls
- F27D1/0006—Linings or walls formed from bricks or layers with a particular composition or specific characteristics
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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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
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
The invention relates to a TiN-MgAlON-Al 2O3 composite refractory material, a preparation method and application. The method comprises the following steps: mixing and stirring corundum, titanium aluminum alloy powder, magnesia and a binding agent according to a certain proportion to prepare pug; pressing the pug into a composite green body and drying; and nitriding and sintering the composite green body to obtain the TiN-MgAlON-Al 2O3 composite refractory material. The invention takes titanium-aluminum alloy powder, alumina powder, magnesia powder and magnesia particles as raw materials to prepare the chromium-free and carbon-free TiN-MgAlON-Al 2O3 composite material. The invention adopts high-melting-point TiAl alloy as a raw material to be used as a precursor for synthesizing intermediate phases of TiN and AlN, realizes high-efficiency synthesis and uniform distribution of TiN and MgAlON through a high-efficiency gas-solid reaction mechanism, and optimizes the composition and microstructure of the material. The invention improves the service life of the RH refining furnace when the prepared refractory material is used as the inner lining of the RH refining furnace, and simultaneously meets the smelting requirements of high-quality steel such as ultra-low carbon steel, clean steel and the like.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a TiN-MgAlON-Al 2O3 composite refractory material, a preparation method and application.
Background
External refining is a key process in the production of steel, especially high-quality clean steel. Impurities and inclusions in molten steel can be removed by external refining while adjusting and homogenizing the chemical composition of the molten steel. The RH vacuum refining technology has the advantages of high efficiency, suitability for batch processing, low equipment investment, easy operation and the like, is one of the most important methods in external refining, and is widely applied to modern steelworks. The refractory material for the inner lining of the RH refining furnace has harsh service environment and needs to bear the vacuum effect of high temperature (up to 1700 ℃) for a long time, the scouring and erosion effect of molten steel, the cyclic thermal shock effect and the like, so the refractory material is required to have high refractoriness, high strength, wear resistance, erosion resistance, good thermal shock resistance, good vacuum stability and the like.
The service temperature of the refractory material for the RH refining furnace lining may be as high as 1700 ℃. At present, the refractory material for the lining of the RH refining furnace mainly comprises magnesia chrome bricks (more than or equal to 50 percent), and the refractory material of magnesia carbon bricks (5 percent) is partially used. The RH lower groove is a high corrosion area of the whole furnace lining, and mainly adopts electrofusion re-combined magnesia-chrome brick with high slag penetration resistance and Cr 2O3 content reaching 24-26%. However, under the conditions of high-temperature oxidation atmosphere and existence of alkaline oxides, cr 3+ in the Cr 2O3 material can be converted into Cr 6+,Cr6+ which is a toxic carcinogen, and the Cr 6+,Cr6+ has great harm to human bodies and the environment. The carbon material has higher heat conductivity and is not easy to be wetted by slag, and the magnesia carbon brick developed by introducing the carbonaceous raw material into the MgO material has good slag penetration resistance, corrosion resistance and spalling resistance, and the service life is improved by about 15 percent compared with that of the common magnesia chrome brick. However, under high temperature vacuum conditions, C in magnesia carbon bricks can cause MgO to undergo a reduction reaction, mg (g) and CO (g) are formed to escape, and the structure is loose. Meanwhile, carbon causes pollution to molten steel, so that the magnesia carbon brick is not suitable for smelting low-carbon steel and clean steel.
In the prior art, metal aluminum powder, aluminum oxide powder and magnesia particles are used as raw materials, the temperature is kept at 500-700 ℃ for 2-10h, and then the temperature is kept at 1400-1700 ℃ for 2-6h, so that the MgAlON combined corundum composite refractory material is prepared. However, mgO matrix and single metal aluminum are adopted as raw materials, the melting point is low, and the severe nitriding temperature is higher than 800 ℃. That is, the aluminum powder in the billet has melted before the severe nitriding temperature of the metallic aluminum is reached. The formation of molten aluminum in the system causes the reduction of the reactivity of aluminum on one hand, and on the other hand, the inward diffusion of nitrogen is greatly hindered, so that the synthesis difficulty and the uneven distribution of AlN mesophase are caused, the controllable synthesis and the even distribution of MgAlON are further hindered, and free metallic aluminum exists in the obtained material, so that the material performance is not ideal.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a TiN-MgAlON-Al 2O3 composite refractory material, a preparation method and application thereof, which are used for solving the problems in the prior art.
A method for preparing a TiN-MgAlON-Al 2O3 composite refractory material, the method comprising the steps of:
s1, mixing and stirring corundum, titanium aluminum alloy powder, magnesia and a binding agent according to a certain proportion to prepare pug;
S2, pressing the pug into a composite green body, and drying the green body;
S3, nitriding and sintering the composite green body to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
The aspects and any possible implementation manner described above further provide an implementation manner, wherein the mass fraction ratio of corundum, titanium aluminum alloy powder and magnesia in S1 is as follows: 65 to 90 weight percent of corundum and 5 to 20 weight percent of titanium aluminum alloy powder; 5-15 wt% of magnesia; the mass fraction ratio of the binding agent is 2-5 wt%.
In aspects and any one of the possible implementations described above, there is further provided an implementation wherein the corundum includes corundum aggregate having a particle size of 3-1 mm, less than 1mm and activated alumina fines having a particle size of less than 5 μm.
In the aspect and any possible implementation manner, there is further provided an implementation manner, wherein in the mass fraction range of the corundum, the corundum aggregate with the particle size of 3-1 mm and less than 1mm is 75-90% by mass, and the alumina fine powder is 10-25% by mass.
In the aspect and any possible implementation manner as described above, there is further provided an implementation manner, where the drying in S2 includes: and drying the composite green body at the temperature of 120-200 ℃ for 10-50 hours.
In the aspect and any possible implementation manner as described above, there is further provided an implementation manner, where the nitriding sintering in S3 includes: and placing the dried composite green body in a sagger, placing the sagger in a nitriding furnace filled with nitrogen, heating to 1200-1800 ℃ at a speed of 3-20 ℃/min, and preserving heat for 1-8 h for nitriding and firing.
In the aspect and any possible implementation manner, there is further provided an implementation manner, wherein the mass percentage of Ti in the titanium-aluminum alloy is 2% -80%.
In aspects and any one of the possible implementations described above, there is further provided an implementation, the binder is a thermosetting phenolic resin binder.
The invention also provides a TiN-MgAlON-Al 2O3 composite refractory material, which is prepared by adopting the preparation method.
The invention also provides an application of the TiN-MgAlON-Al 2O3 composite refractory material as a lining in an RH refining furnace.
The beneficial effects of the invention are that
Compared with the prior art, the invention has the following beneficial effects:
Aiming at the problems that Cr 3+ in a magnesia-chrome brick (MgO-Cr 2O3) for an RH refining furnace is easy to be converted into Cr 6+, the human health and the environment are endangered, carbon in a magnesia-carbon brick (MgO-C) is easy to be dissolved in molten steel, carburetion pollution is caused and the like in the prior art. The invention takes titanium-aluminum alloy powder, alumina powder, magnesia powder and magnesia particles as raw materials to prepare a chromium-free and carbon-free TiN-MgAlON-Al 2O3 composite material, and prepares the TiN and MgAlON synergistically enhanced Al 2O3 composite refractory material through high-temperature nitridation. The invention adopts high-melting-point TiAl alloy as a raw material to be used as a precursor for synthesizing intermediate phases of TiN and AlN, realizes high-efficiency synthesis and uniform distribution of the TiN and MgAlON through a high-efficiency gas-solid reaction mechanism, and optimizes the composition and microstructure of the prepared material. MgAlON has excellent molten iron and slag erosion resistance and thermal shock resistance, tiN has excellent wear resistance, higher hardness and good high-temperature stability, and the synergistic effect of the two can greatly improve the service life of the RH refining furnace when the prepared refractory material is used as an inner lining of the RH refining furnace, and simultaneously meets the smelting requirements of high-quality steel such as ultra-low carbon steel, clean steel and the like:
(1) Under RH refining service environment, C in MgO-C material in the prior art is easy to dissolve in molten steel, and pollutes the molten steel; cr 3+ in the MgO-Cr 2O3 composite material is easily converted into Cr 6+, which is harmful to human health and pollutes the environment. The TiN-MgAlON-Al 2O3 composite refractory material is a synergistic Al 2O3 composite material of TiN and MgAlON after high-temperature nitridation firing, is a carbon-free and chromium-free refractory material, has excellent chemical stability, does not pollute molten steel, and has no harm to the environment and human body;
(2) In the RH refining service process, the single MgAlON-MgO/Al 2O3 composite refractory material in the prior art has insufficient wear resistance and is easy to cause material defects and damage. The TiN has high melting point, high hardness, excellent wear resistance, excellent erosion resistance, excellent thermal shock resistance and excellent chemical stability, and the key service performance of the refractory material for the RH refining furnace can be cooperatively improved by utilizing the TiAl alloy to synthesize the TiN and the MgAlON in situ, so that the long-life development of the refractory material for the RH refining furnace can be realized.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a schematic diagram of a Ti-Al binary phase according to the present invention.
Detailed Description
For a better understanding of the present invention, the present disclosure includes, but is not limited to, the following detailed description, and similar techniques and methods should be considered as falling within the scope of the present protection. In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
It should be understood that the described embodiments of the invention are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
As shown in fig. 1, the preparation method of the TiN-MgAlON-Al 2O3 composite refractory material of the invention comprises the following steps:
s1, mixing and stirring corundum, titanium aluminum alloy powder, magnesia and a binding agent according to a certain proportion to prepare pug;
S2, pressing the pug into a composite green body, and drying the green body;
S3, nitriding and sintering the composite green body to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
Specifically, the preparation process of the invention is as follows:
(1) Weighing corundum aggregate, corundum fine powder, magnesia fine powder, titanium-aluminum alloy powder and a binding agent according to a proportion, and uniformly stirring to prepare pug;
(2) Pressing the pug obtained in the step (1) into a TiAl-MgO-Al 2O3 composite blank by a press, wherein TiAl is from titanium aluminum alloy powder, mgO is from magnesia fine powder, al 2O3 is from corundum, and drying the composite blank for 10-50 hours at the temperature of 120-200 ℃;
(3) Placing the dried TiAl-MgO-Al 2O3 composite blank in a sagger, placing the sagger in a nitriding furnace, introducing nitrogen into the nitriding furnace, heating to 1200-1800 ℃ at a speed of 3-20 ℃/min, and preserving heat for 1-8 h for nitriding and sintering.
In the nitriding sintering process, tiAl alloy particles in the TiAl-MgO-Al 2O3 composite blank and N 2 in the atmosphere react chemically, specifically as shown in a reaction formula (1), tiN, ti 2 AlN and AlN are generated in situ; as the temperature is further increased to more than 1200 ℃, the newly generated AlN further reacts with active Al 2O3 and MgO in the system, specifically as shown in a reaction formula (2), an MgAlON reinforcing phase is generated in situ, and the newly generated Ti 2 AlN reacts with active Al 2O3 and MgO in the system, specifically as shown in a reaction formula (3), so as to generate TiN and MgAlON reinforcing phases; in addition, at higher temperature, i.e. at the temperature of more than or equal to 1200 ℃, the liquid TiAl alloy can directly react with Al 2O3, mgO and N 2 to generate MgAlON and TiN; the composite corundum refractory material combined by TiN and MgAlON is finally prepared through a series of chemical reactions under the nitrogen atmosphere, and the composite corundum refractory material is prepared by the specific formula (4).
TiAl(s) +N 2(g)→TiN(s)+AlN(s)+Ti2 AlN(s) (1) (gas-solid reaction)
AlN(s) +Al 2O3(s) +MgO(s). Fwdarw.MgAlON(s) (2) (solid phase reaction)
Ti 2AlN(s)+Al2O3(s) +MgO(s) →MgAlON(s) +TiN(s) (3) (solid
Phase reaction
TiAl(l)+N2(g)+Al2O3(s)+MgO(s)→MgAlON(s)+TiN(s)(4)
(Gas-liquid-solid reaction)
Compared with the prior art that an MgO matrix is adopted, corundum is adopted as aggregate, and the high-temperature vacuum stability is better; the MgO added in the invention is fine powder, has higher reaction activity, is completely converted into MgAlON reinforcing phase in the high-temperature nitriding sintering process, and has better high-temperature stability and chemical stability; compared with the prior art, single metal aluminum is adopted as a raw material, the metal aluminum is utilized to react with N 2 at high temperature to generate AlN, and the AlN further reacts with Al 2O3 and MgO to generate MgAlON reinforcing phase. However, metallic aluminum has a lower melting point (660 ℃) and a severe nitriding temperature of more than 800 ℃. That is, the aluminum powder in the billet has melted before the severe nitriding temperature of the metallic aluminum is reached. On one hand, the formation of molten aluminum in the system causes the reduction of the reactivity of aluminum, on the other hand, the inward diffusion of nitrogen is greatly hindered, the synthesis difficulty and the uneven distribution of AlN mesophase are further hindered, the controllable synthesis and the even distribution of MgAlON are further hindered, and the obtained material has free metallic aluminum, so that the material performance is not ideal, therefore, the invention adopts titanium-aluminum alloy as the raw material, the melting point is far higher than that of the metallic aluminum, as shown in figure 2, when the temperature reaches 800 ℃, the reaction (gas-solid reaction) of the solid titanium-aluminum alloy and nitrogen has more dynamic advantages, the reaction speed is relatively high, the efficient mass production and the even distribution of AlN mesophase are facilitated, and the controllable synthesis of MgAlON at a lower temperature is promoted; according to the invention, the titanium aluminum alloy is used as a raw material, so that the TiN reinforcing phase is further synthesized in situ while the AlN intermediate phase is generated by nitriding metal aluminum, the TiN is a material with excellent wear resistance, and the synergistic effect of the TiN and MgAlON can effectively improve the comprehensive performance of the material, thereby prolonging the service life.
Further, the mass fraction of each of the materials is as follows: 65-90 wt% of corundum, 5-20 wt% of titanium aluminum alloy powder and 5-15 wt% of magnesia, wherein 2-5 wt% of binding agent is added into the materials, and the proportion is proportioned according to the performance requirement of the refractory material to be prepared, wherein the aggregate is prepared according to the grain size: fines ≡7:3, preparing, wherein the aggregate adopts corundum, the matrix adopts corundum, aluminum titanium alloy and magnesia mixed powder, the corundum, aluminum titanium alloy and magnesia fine powder of the matrix part have higher activity at high temperature, all participate in the reaction under nitrogen atmosphere, and the aggregate has low activity and hardly participate in the reaction; the binder plays a role in binding and is used for binding raw material particles with different particle sizes together to prepare pugs with certain plasticity so as to facilitate the molding of the composite green body.
Further, the corundum comprises corundum aggregate with granularity of 3-1 mm and less than 1mm, and the granularity ratio is favorable for obtaining a composite blank with a certain porosity after molding; and activated alumina fine powder with the granularity of less than 5 mu m, wherein the activated alumina powder with the granularity of less than 5 mu m is one of raw materials adopted by refractory products, has higher activity, and is added into a matrix to be beneficial to participating in the reaction so as to generate MgAlON. Further, in 65 to 90wt% of corundum, the mass percentage of corundum aggregate with the granularity of 3 to 1mm and less than 1mm is 75 to 90 percent, and the mass percentage of the active alumina fine powder is 10 to 25 percent. The corundum aggregate has large particle size and low activity and hardly participates in the reaction; the mass percentage of the active alumina fine powder is 5-30%, and the amount of Al 2O3 participating in the reaction is controlled by controlling the addition amount of the active alumina fine powder, so that the generation amount of MgAlON is controlled.
Preferably, the Ti content in the titanium-aluminum alloy is 2-80% by mass, the Ti content is different, the TiN/MgAlON ratio generated by the reaction is different, and the comprehensive performance of the generated composite material can be regulated and controlled according to the service environment.
Preferably, the bonding agent is a thermosetting phenolic resin bonding agent, the phenolic resin is one of the refractory bonding agents, and the thermosetting phenolic resin bonding agent is wrapped on the surfaces of raw material particles at normal temperature, so that the bonding agent can play a role in bonding and endow the material with certain strength; the high-temperature pyrolysis can generate a small amount of residual nano carbon, and the residual nano carbon is uniformly dispersed in the material, so that the wettability of TiAl alloy, mgO and Al 2O3 particles can be improved, and the generation of MgAlON is promoted.
According to the invention, corundum aggregate, corundum fine powder, titanium-aluminum alloy powder and a binding agent are weighed according to a proportion and uniformly stirred to prepare pug; pressing the pug into a green body by a press, drying and nitriding and firing at high temperature to enable TiAl alloy, N 2 and MgO and Al 2O3 to fully react, thus obtaining the corundum composite refractory material with the synergistic enhancement of TiN and MgAlON.
Preferably, the green body is dried for 10 to 50 hours at the temperature of between 120 and 200 ℃, and the drying rate of the green body is moderate in the temperature range and the time range, so that the residual moisture is less than 1 percent, and the cracking of the green body is not easy to cause. If the temperature is too high, the drying rate is too high, and the product is easy to crack; if the temperature is too low or the drying time is too short, the residual moisture is hardly reduced to 1% or less, and the product is cracked during firing, resulting in defects.
Preferably, the high-temperature nitriding is performed by heating to 1200-1800 ℃ at a speed of 3-20 ℃/min under the condition of nitrogen atmosphere in a nitriding furnace, and preserving heat for 1-8 hours.
Preferably, the nitriding furnace comprises a tunnel kiln, a shuttle kiln and an electric kiln, and all the device kilns can be used as preparation sites.
In nitrogen atmosphere, when the temperature of the system reaches about 800 ℃, tiAl alloy particles start to be significantly nitrided to generate TiN, ti 2 AlN and AlN, the reaction is a gas-solid reaction mechanism, the reaction has higher dynamic advantage, the reaction speed is higher, and the reaction products are uniformly distributed; as the temperature is further increased to more than 1200 ℃, the newly generated AlN further reacts with active Al 2O3 and MgO in the system to generate MgAlON reinforcing phases, and the newly generated Ti 2 AlN reacts with active Al 2O3 and MgO in the system to generate TiN and MgAlON reinforcing phases.
The invention also provides a TiN-MgAlON-Al 2O3 composite refractory material which is prepared by adopting the preparation method, has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 8-16%, and the normal-temperature compressive strength of 90-400 MPa, is used as a carbon-free and chromium-free refractory material, has excellent chemical stability, does not pollute molten steel and has no harm to the environment and human body. Compared with the traditional oxide refractory material, the non-oxide refractory material prepared by the invention has excellent erosion resistance, thermal shock resistance stability and thermochemical stability, and does not pollute molten steel. MgAlON in the composite material is a spinel structure solid solution in a Mg-Al-O-N system, and is a material with excellent molten iron and slag erosion resistance. The TiN has a melting point of 2950 ℃, has a Mohs hardness of 8-9, has good thermal shock resistance and excellent wear resistance, and has excellent thermal shock resistance and erosion resistance of non-oxide and excellent oxidation resistance. The metal Al or Ti is introduced into the MgO-Al 2O3 composite refractory material as a component, and is sintered in the high-temperature nitrogen atmosphere, so that MgAlON or TiN reinforcing phase is hopefully synthesized in situ, the erosion resistance, thermal shock resistance and wear resistance of the material are synergistically improved, and the service life of the material is prolonged.
The invention also provides an application of the TiN-MgAlON-Al 2O3 composite refractory material as a lining in an RH refining furnace, which can cooperatively improve the erosion resistance, thermal shock resistance, wear resistance and high-temperature vacuum stability of the RH refining furnace, thereby improving the key service performance of the RH refining furnace and realizing the long-life development of the RH refining furnace.
Example 1
Mixing 70wt.% of corundum aggregate, 20wt.% of alumina powder, 5wt.% of titanium-aluminum alloy powder and 5wt.% of magnesia powder, adding 3wt.% of phenolic resin binder of the mixture, uniformly mixing, pressing and forming to obtain a TiAl-MgO-Al 2O3 composite material blank, and drying at 120 ℃ for 24 hours. Heating the dried TiAl-MgO-Al 2O3 blank to 1400 ℃ at the heating rate of 10 ℃/min, and preserving heat for 4 hours to burn the TiAl-MgO-Al 2O3 blank to prepare the TiN-MgAlON-Al 2O3 composite refractory material.
The obtained TiN-MgAlON-Al 2O3 composite refractory material has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 12.2 percent and the normal-temperature compressive strength of 276MPa.
Example 2
Mixing 60wt.% of corundum aggregate, 5wt.% of alumina powder, 20wt.% of titanium-aluminum alloy powder and 15wt.% of magnesia powder, adding 4wt.% of phenolic resin binder of the mixture, uniformly mixing, pressing and forming to obtain a TiAl-MgO-Al 2O3 composite material blank, and drying at 200 ℃ for 12 hours. Heating the dried TiAl-MgO-Al 2O3 blank to 1600 ℃ at a heating rate of 5 ℃/min, and preserving heat for 3 hours to sinter to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
The obtained TiN-MgAlON-Al 2O3 composite refractory material has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 9.8 percent and the normal-temperature compressive strength of 346MPa.
Example 3
Mixing 80wt.% of corundum aggregate, 5wt.% of alumina powder, 8wt.% of titanium-aluminum alloy powder and 7wt.% of magnesia powder, adding 5wt.% of phenolic resin binder into the mixture, uniformly mixing, pressing and forming to obtain a TiAl-MgO-Al 2O3 composite material blank, and drying at 150 ℃ for 48 hours. And heating the dried TiAl-MgO-Al 2O3 blank to 1200 ℃ at a heating rate of 15 ℃/min, and preserving heat for 8 hours to sinter to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
The obtained TiN-MgAlON-Al 2O3 composite refractory material has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 13.1 percent and the normal-temperature compressive strength of 197MPa.
Example 4
Mixing 85wt.% of corundum aggregate, 5wt.% of alumina powder, 5wt.% of titanium-aluminum alloy powder and 5wt.% of magnesia powder, adding 4.5wt.% of phenolic resin binder into the mixture, uniformly mixing, and performing compression molding to obtain a TiAl-MgO-Al 2O3 composite blank, and drying at 120 ℃ for 50 hours. Heating the dried TiAl-MgO-Al 2O3 blank to 1700 ℃ at the heating rate of 20 ℃/min, and preserving heat for 2 hours to sinter to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
The obtained TiN-MgAlON-Al 2O3 composite refractory material has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 11.6 percent and the normal-temperature compressive strength of 159MPa.
Example 5
Mixing 72wt.% of corundum aggregate, 8wt.% of alumina powder, 10wt.% of titanium-aluminum alloy powder and 10wt.% of magnesia powder, adding 3.5wt.% of phenolic resin binder into the mixture, uniformly mixing, and performing compression molding to obtain a TiAl-MgO-Al 2O3 composite blank, and drying at 200 ℃ for 10 hours. Heating the dried TiAl-MgO-Al 2O3 blank to 1800 ℃ at the heating rate of 3 ℃/min, and preserving heat for 1h to burn to obtain the TiN-MgAlON-Al 2O3 composite refractory material.
The obtained TiN-MgAlON-Al 2O3 composite refractory material has the phase composition of Al 2O3, tiN and MgAlON, the apparent porosity of 14.1 percent and the normal-temperature compressive strength of 282MPa.
While the foregoing description illustrates and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as limited to other embodiments, and is capable of numerous other combinations, modifications and environments and is capable of changes or modifications within the scope of the inventive concept as expressed herein, either as a result of the foregoing teachings or as a result of the knowledge or technology of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (9)
1. The preparation method of the TiN-MgAlON-Al 2O3 composite refractory material is characterized by comprising the following steps:
S1, mixing and stirring corundum, titanium aluminum alloy powder, magnesia raw materials and a binding agent according to a certain proportion to prepare pug;
S2, pressing the pug into a composite green body, and drying the green body;
S3, nitriding and sintering the composite green body to obtain the TiN-MgAlON-Al 2O3 composite refractory material; the mass fraction ratio of corundum, titanium aluminum alloy powder and magnesia in the S1 is as follows: 65 to 90 weight percent of corundum and 5 to 20 weight percent of titanium aluminum alloy powder; 5-15 wt% of magnesia; the mass fraction ratio of the binding agent is 2-5 wt%.
2. The method for preparing the composite refractory material of TiN-MgAlON-Al 2O3 according to claim 1, wherein the corundum comprises corundum aggregate with a granularity of 3-1 mm and less than 1mm and activated alumina fine powder with a granularity of less than 5 μm.
3. The method for preparing the TiN-MgAlON-Al 2O3 composite refractory according to claim 2, wherein in the mass fraction range of the corundum, the mass percentage of the corundum aggregate with the particle size of 3-1 mm and less than 1mm is 75% -90%, and the mass percentage of the alumina fine powder is 10-25%.
4. The method for preparing the TiN-MgAlON-Al 2O3 composite refractory according to claim 1, wherein the drying in S2 comprises: and drying the composite green body at the temperature of 120-200 ℃ for 10-50 hours.
5. The method for preparing the TiN-MgAlON-Al 2O3 composite refractory according to claim 1, wherein the nitriding sintering in S3 comprises: and placing the dried composite green body in a sagger, placing the sagger in a nitriding furnace filled with nitrogen, heating to 1200-1800 ℃ at a speed of 3-20 ℃/min, and preserving heat for 1-8 h for nitriding and firing.
6. The preparation method of the TiN-MgAlON-Al 2O3 composite refractory material according to claim 1, wherein the mass percentage of Ti in the titanium-aluminum alloy is 2% -80%.
7. The method of preparing a TiN-MgAlON-Al 2O3 composite refractory according to claim 1, wherein the binder is a thermosetting phenolic resin binder.
8. A TiN-MgAlON-Al 2O3 composite refractory material, characterized in that the TiN-MgAlON-Al 2O3 composite refractory material is prepared by the preparation method according to any one of claims 1 to 7.
9. Use of a TiN-MgAlON-Al 2O3 composite refractory according to claim 8 as a lining in an RH refining furnace.
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