CN116854493B - RH vacuum furnace lining refractory material and preparation method thereof - Google Patents
RH vacuum furnace lining refractory material and preparation method thereof Download PDFInfo
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- CN116854493B CN116854493B CN202311126806.0A CN202311126806A CN116854493B CN 116854493 B CN116854493 B CN 116854493B CN 202311126806 A CN202311126806 A CN 202311126806A CN 116854493 B CN116854493 B CN 116854493B
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- vacuum furnace
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- furnace lining
- lining
- silicon nitride
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- 239000011819 refractory material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 61
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000011159 matrix material Substances 0.000 claims abstract description 46
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 38
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 26
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 25
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 25
- 239000011733 molybdenum Substances 0.000 claims abstract description 25
- 239000011591 potassium Substances 0.000 claims abstract description 25
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 25
- 239000000835 fiber Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 12
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021343 molybdenum disilicide Inorganic materials 0.000 claims abstract description 10
- 238000011049 filling Methods 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010426 asphalt Substances 0.000 claims abstract description 4
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 238000005087 graphitization Methods 0.000 claims abstract description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 30
- 239000002121 nanofiber Substances 0.000 claims description 21
- 239000004964 aerogel Substances 0.000 claims description 20
- 239000000919 ceramic Substances 0.000 claims description 20
- 239000004113 Sepiolite Substances 0.000 claims description 17
- 229910052624 sepiolite Inorganic materials 0.000 claims description 17
- 235000019355 sepiolite Nutrition 0.000 claims description 17
- 239000000395 magnesium oxide Substances 0.000 claims description 15
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 14
- 239000001110 calcium chloride Substances 0.000 claims description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920001732 Lignosulfonate Polymers 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004568 cement Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052878 cordierite Inorganic materials 0.000 claims description 6
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 6
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 6
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 6
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 6
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000001680 brushing effect Effects 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000009941 weaving Methods 0.000 abstract description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 32
- 239000000945 filler Substances 0.000 description 9
- 230000002035 prolonged effect Effects 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 210000001161 mammalian embryo Anatomy 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NACUKFIFISCLOQ-UHFFFAOYSA-N [Mg].[Cr] Chemical compound [Mg].[Cr] NACUKFIFISCLOQ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011384 asphalt concrete Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- -1 methyl vinyl Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
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- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The application relates to the technical field of refractory materials, and particularly discloses an RH vacuum furnace lining refractory material and a preparation method thereof. The RH vacuum furnace lining refractory material comprises a lining matrix formed by a three-dimensional weaving preformed body and a filling material filled in the three-dimensional weaving preformed body, and a titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating on the surface of the lining matrix; the carbon-alumina fiber is prepared from polyacrylonitrile fiber, asphalt fiber and aluminum silicate fiber with the mass ratio of 1:1:3 through stabilizing treatment, carbonization treatment and graphitization treatment respectively in sequence; the molybdenum disilicide-silicon nitride coating comprises the following raw materials: molybdenum disilicide powder, silicon nitride powder, titanium dioxide powder, potassium hexatitanate whisker, high hydrogen silicone oil, divinylbenzene and chloroplatinic acid. The RH vacuum furnace lining refractory material can prolong the service life of the RH vacuum furnace lining.
Description
Technical Field
The application relates to the technical field of refractory materials, in particular to an RH vacuum furnace lining refractory material and a preparation method thereof.
Background
The secondary refining technology is an important technical means for improving the quality of steel. Secondary refining techniques, particularly RH vacuum refining techniques, need to be implemented by means of an RH vacuum furnace. Thus, RH vacuum furnaces are one of the important devices in the steel industry. With the development of the steel industry, the quality requirements on steel materials are higher and higher, and correspondingly, the requirements on lining refractory materials of RH vacuum furnaces are higher and higher. In the secondary refining process of steel, the RH vacuum furnace is intermittently subjected to the scouring and splashing actions of molten steel under the vacuum and high temperature conditions, so that the service life of lining materials of the RH vacuum furnace is greatly influenced.
The lining material commonly used in the traditional RH vacuum furnace mainly adopts magnesium-chromium products. However, such lining materials are easily oxidized under high-temperature alkaline conditions, releasing hexavalent chromium ions, and thus causing environmental pollution. Therefore, it is needed to provide an environment-friendly RH vacuum furnace lining refractory material which can further improve the fire resistance of the RH vacuum furnace lining material and prolong the service life of the RH vacuum furnace.
Disclosure of Invention
The application provides an antifreezing asphalt pavement composition and a pavement construction method for improving the antifreezing performance of an asphalt concrete pavement.
In a first aspect, the application provides an RH vacuum furnace lining refractory material, which adopts the following technical scheme:
an RH vacuum furnace lining refractory material comprises a three-dimensional woven preform, a lining matrix formed by filling materials in the three-dimensional woven preform, and a surface of the lining matrixMolybdenum disilicide-silicon nitride coatings doped with titanium dioxide and potassium hexatitanate whiskers; the three-dimensional braided preform comprises carbon-alumina fibers and silica glass fibers in a mass ratio of 3:1, and the three-dimensional braided preform is of a three-dimensional four-way structure; the carbon-alumina fiber is obtained by sequentially carrying out stabilization treatment, carbonization treatment and graphitization treatment on polyacrylonitrile fiber, asphalt fiber and aluminum silicate fiber with the mass ratio of 1:1:3; the filling material comprises the following raw materials in parts by weight: 1.5 to 2.5 parts of ceramic nanofiber aerogel, 15 to 20 parts of fused magnesia, 8 to 15 parts of calcium chloride modified sepiolite powder, 3 to 4 parts of microcrystalline cellulose, 2 to 3 parts of cordierite powder, 0.2 to 0.5 part of organosilicon resin powder, 1 to 2 parts of calcium aluminate cement, 0.2 to 0.5 part of aluminum dihydrogen phosphate and NaHCO 3 0.05-0.08 part, boric acid 0.02-0.05 part, magnesium lignosulfonate 0.05-0.08 part; the ceramic nanofiber aerogel is in a chip shape; the molybdenum disilicide-silicon nitride coating comprises the following raw materials in parts by weight: 20-25 parts of molybdenum disilicide powder, 8-12 parts of silicon nitride powder, 0.8-1.2 parts of titanium dioxide powder, 1.4-1.6 parts of potassium hexatitanate whisker, 0.1-0.2 part of high-hydrogen silicone oil, 1-1.3 parts of divinylbenzene and 0.02-0.05 part of chloroplatinic acid.
By adopting the technical scheme, the trial service life of the lower groove prepared by the lining refractory material of the RH vacuum furnace is in the range of 200-206 furnaces; the life span of the circulation pipe is 103-107 furnaces. The RH vacuum furnace lining refractory material can prolong the service life of the vacuum furnace lining through the mutual synergistic effect of the raw materials, and meets the market demand.
In the application, the three-dimensional woven preform is taken as a framework, and the framework is filled with the filler, so that the prepared lining matrix has excellent impact resistance and compression resistance. In the filler, the ceramic nanofiber aerogel, the fused magnesia and the calcium chloride modified sepiolite powder have excellent high temperature resistance, so that the lining matrix has excellent high temperature resistance. Furthermore, the ceramic nanofiber aerogel does not deform and has super elasticity at high temperature, so that the impact resistance of the lining matrix can be further improved, and the micropores of the ceramic nanofiber aerogel can improve the heat insulation performance of the lining matrix, so that the service life of the RH vacuum furnace lining is prolonged.
In addition, the molybdenum disilicide-silicon nitride coating has excellent oxidation resistance and high temperature resistance, and is a compact coating, and the pattern layer is coated on the surface of the lining matrix, so that the oxidation of the lining matrix can be reduced, and the high temperature resistance of the lining matrix can be improved. In addition, titanium dioxide and potassium hexatitanate whiskers are doped in the molybdenum disilicide-silicon nitride coating, infrared electromagnetic radiation can be effectively scattered, the heat insulation performance of the molybdenum disilicide-silicon nitride coating is further improved, and therefore the service life of the RH vacuum furnace lining is further prolonged.
Optionally, the mass ratio of molybdenum disilicide powder to silicon nitride powder in the titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating is 7:3.
Alternatively, the silicon nitride powder has a particle size of 1-3 μm.
Alternatively, the three-dimensional woven preform is prepared by a four-step process.
Optionally, the grain size of the fused magnesia is 1-3mm.
Optionally, mgO in the fused magnesia is more than 97wt%.
Optionally, caO in the fused magnesia is less than 1wt%.
In a second aspect, the application provides a preparation method of an RH vacuum furnace lining refractory material, which adopts the following technical scheme:
a preparation method of an RH vacuum furnace lining refractory material comprises the following steps: soaking the three-dimensional woven preform in a 2wt% sodium hydroxide solution for 30-40min to obtain a treated three-dimensional woven preform; placing the treated three-dimensional woven preform in a mold; ceramic nanofiber aerogel, fused magnesia, calcium chloride modified sepiolite powder, cordierite powder, organosilicon resin powder, calcium aluminate cement, aluminum dihydrogen phosphate, microcrystalline cellulose and NaHCO 3 Uniformly mixing boric acid and magnesium lignosulfonate to obtain a mixture I; uniformly paving 1/3-1/2 of the total amount of the mixture I in a die, then paving the processed three-dimensional braided preform, and uniformly paving the rest amount of the mixture I on the surface of the processed three-dimensional braided preform to obtain a lining matrix mixture; then lining the matrix mixtureSpraying water at 45 ℃ until the lining matrix mixture is completely soaked, wherein the dosage of the water at 45 ℃ is 20-30% of the total mass of the lining matrix mixture, and obtaining a lining matrix embryo; sintering the lining matrix blank in a vacuum furnace for 4-6 hours at 900-1100 ℃, then cooling to 600-800 ℃, preserving heat for 2 hours, cooling to room temperature, and demoulding to obtain the lining matrix; uniformly mixing molybdenum disilicide powder, silicon nitride powder, titanium dioxide powder and potassium hexatitanate whisker, sequentially adding high-hydrogen silicone oil, divinylbenzene and chloroplatinic acid, and stirring until the materials are uniformly mixed to obtain a coating; coating the coating on the surface of the lining matrix by adopting a brushing method, and then preserving heat for 3 hours at the temperature of 120 ℃ in an oven to obtain a sample; and sintering the sample at 1000 ℃ for 2 hours under the protection of inert gas to obtain the RH vacuum furnace lining refractory material.
In summary, the application has at least the following advantages:
1. according to the RH vacuum furnace lining refractory material, the three-dimensional woven preformed body is taken as a framework, and the filling material is filled in the framework, so that the prepared lining matrix has excellent impact resistance and compression resistance, and the service life of the RH vacuum furnace lining is prolonged;
2. according to the refractory material for the RH vacuum furnace lining, the ceramic nanofiber aerogel is not deformed and super-elastic at high temperature, so that the shock resistance of the lining matrix can be further improved, and the micropores of the ceramic nanofiber aerogel can improve the heat insulation performance of the lining matrix, so that the service life of the RH vacuum furnace lining is prolonged;
3. according to the refractory material for the RH vacuum furnace lining, titanium dioxide and potassium hexatitanate whiskers are doped in the molybdenum disilicide-silicon nitride coating, so that the heat insulation performance of the molybdenum disilicide-silicon nitride coating is further improved, and the service life of the RH vacuum furnace lining is further prolonged.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example
Preparation example 1
A carbon-alumina fiber is obtained by uniformly mixing 10kg of polyacrylonitrile fiber, 10kg of pitch fiber and 30kg of aluminum silicate fiber, and then sequentially carrying out stabilization treatment at 300 ℃, carbonization treatment at 800 ℃ and graphitization treatment under the condition of argon protection at 1800 ℃.
Preparation example 2
The calcium chloride modified sepiolite powder is prepared by the following method: preparing 10wt% calcium chloride solution, mixing 12kg of sepiolite powder and 30kg of calcium chloride solution, stirring to a dry and loose state, and drying in a 110 ℃ oven to obtain the calcium chloride modified sepiolite powder. Wherein, the sepiolite powder product number is 00216556.
Examples
Example 1
An RH vacuum furnace lining refractory material comprises a lining matrix formed by a three-dimensional weaving preformed body and a filling material filled in the three-dimensional weaving preformed body, and a titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating on the surface of the lining matrix; the mass of the three-dimensional braided preform is 12% of the total mass of the refractory material of the inner lining of the RH vacuum furnace, the mass of the molybdenum disilicide-silicon nitride coating doped with titanium dioxide and potassium hexatitanate whiskers is 2% of the total mass of the refractory material of the inner lining of the RH vacuum furnace, and the balance is filler. The three-dimensional braided preform is prepared from carbon-alumina fibers and high silica glass fibers prepared in preparation example 1 in a mass ratio of 3:1 through a four-step method, and the three-dimensional braided preform has a three-dimensional four-way structure.
The filling material comprises the following raw materials by weight: 1.5kg of chip-shaped ceramic nanofiber aerogel, 16kg of fused magnesia, 10kg of calcium chloride modified sepiolite powder prepared in preparation example 2, 3.5kg of microcrystalline cellulose, 2kg of cordierite powder, 0.5kg of organic silicon resin powder, 1.3kg of calcium aluminate cement, 0.3kg of aluminum dihydrogen phosphate and NaHCO 3 0.06kg, 0.03kg boric acid and 0.06kg magnesium lignin sulfonate. Wherein, the grain diameter of the fused magnesia is 1-3mm, mgO is more than 97wt percent, and CaO is less than 1wt percent. The pH of the magnesium lignin sulfonate is 6-7. The model of the organic silicon resin powder is methyl vinyl MQ silicon resin RY-JJ-01. The ceramic nanofiber aerogel is prepared from SiO2 nanofibers and an aluminoborosilicate (AlBSi) matrix, and has a Poisson ratio of 0 at 1100 ℃.The ceramic nanofiber aerogel is in the form of fragments, and the area of each fragment is not more than 0.5cm 2 The thickness is not more than 60 μm.
The titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating comprises the following raw materials by weight: 21kg of molybdenum disilicide powder, 9kg of silicon nitride powder, 0.8kg of titanium dioxide powder, 1.4kg of potassium hexatitanate whisker, 0.1kg of high hydrogen silicone oil, 1kg of divinylbenzene and 0.02kg of chloroplatinic acid. Wherein the particle size of the silicon nitride powder is 1-3 μm. The particle size of the molybdenum disilicide powder was 1 μm. The titanium dioxide powder is anatase titanium dioxide nano-scale powder, and the model is LJ-80. The model of the high hydrogen silicone oil is HQ-17.
A preparation method of an RH vacuum furnace lining refractory material comprises the following steps:
s1: the three-dimensional woven preform was immersed in a 2wt% sodium hydroxide solution for 30 minutes to obtain a treated three-dimensional woven preform.
S2: ceramic nanofiber aerogel, fused magnesia, calcium chloride modified sepiolite powder, cordierite powder, organosilicon resin powder, calcium aluminate cement, aluminum dihydrogen phosphate, microcrystalline cellulose and NaHCO 3 And uniformly mixing boric acid and magnesium lignosulfonate to obtain a mixture I.
S3: uniformly paving 1/3 of the total amount of the mixture I in a die, then paving the processed three-dimensional woven preform, and uniformly paving the rest amount of the mixture I on the surface of the processed three-dimensional woven preform to obtain the lining matrix mixture.
S4: then spraying water at 45 ℃ to the lining matrix mixture until the lining matrix mixture is completely soaked, wherein the water at 45 ℃ is 26% of the total mass of the lining matrix mixture, and obtaining a lining matrix embryo body.
S5: sintering the lining matrix blank in a vacuum furnace for 6 hours at 1000 ℃, then cooling to 700 ℃, preserving heat for 2 hours, cooling to room temperature, and demoulding to obtain the lining matrix.
S6: and uniformly mixing molybdenum disilicide powder, silicon nitride powder, titanium dioxide powder and potassium hexatitanate whisker, sequentially adding high-hydrogen silicone oil, divinylbenzene and chloroplatinic acid, and stirring until the materials are uniformly mixed to obtain the coating.
S7: and (3) coating the coating on the surface of the lining matrix by adopting a brushing method, and then preserving heat for 3 hours at the temperature of 120 ℃ in an oven to obtain a sample.
S8: and sintering the sample at 1000 ℃ for 2 hours under the protection of inert gas to obtain the RH vacuum furnace lining refractory material.
Example 2
An RH vacuum furnace lining refractory is different from example 1 in that in step S3, after uniformly laying the rest amount of the mixture I on the surface of the processed three-dimensional woven preform, ultrasonic treatment is performed at 10kHz for 1min to obtain a lining matrix mixture, and the rest is the same as in example 1.
Example 3
In the step S3, 1/2 of the total amount of the mixture I is uniformly paved in a die, then the three-dimensional braided preform after the tiling treatment is paved, the rest amount of the mixture I is uniformly paved on the surface of the three-dimensional braided preform after the treatment, and ultrasonic treatment is performed for 1min at 10kHz to obtain a lining matrix mixture, and the rest amount is the same as that in the embodiment 2.
Example 4
In the step S3, 2/5 of the total amount of the mixture I is uniformly paved in a die, then the three-dimensional braided preform after the tiling treatment is paved, the rest amount of the mixture I is uniformly paved on the surface of the three-dimensional braided preform after the treatment, and ultrasonic treatment is performed for 1min at 10kHz to obtain a lining matrix mixture, and the rest amount is the same as that in the embodiment 2.
Example 5
An RH vacuum furnace lining refractory is different from example 4 in that the addition amount of ceramic nanofiber aerogel in the raw material of the filler is 1.8kg, and the rest is the same as example 4.
Example 6
An RH vacuum furnace lining refractory is different from example 5 in that the addition amount of ceramic nanofiber aerogel in the raw material of the filler is 2.5kg, and the rest is the same as example 5.
Comparative example
Comparative example 1
An RH vacuum furnace lining refractory is different from example 1 in that the raw material of the filler does not include ceramic nanofiber aerogel, and the rest is the same as example 1.
Comparative example 2
An RH vacuum furnace lining refractory is different from example 1 in that carbon-alumina fibers are replaced with an equal amount of alumina refractory fibers in the raw material of the three-dimensional woven preform, and the rest is the same as in example 1.
Comparative example 3
An RH vacuum furnace lining refractory is different from example 1 in that the molybdenum disilicide-silicon nitride coating is undoped with titanium dioxide, and the rest is the same as in example 1.
Comparative example 4
An RH vacuum furnace lining refractory is different from example 1 in that the molybdenum disilicide-silicon nitride coating is undoped with potassium hexatitanate whiskers, and the rest is the same as in example 1.
Comparative example 5
An RH vacuum furnace lining refractory is different from example 1 in that potassium hexatitanate whiskers and titanium dioxide are not doped in a molybdenum disilicide-silicon nitride coating, and the rest are the same as in example 1.
Comparative example 6
An RH vacuum furnace lining refractory is different from example 1 in that the same amount of sepiolite powder is used for replacing calcium chloride modified sepiolite powder in the raw materials of the filling material, and the rest is the same as example 1.
Comparative example 7
An RH vacuum furnace lining refractory material, which does not include a three-dimensional woven preform, was the same as in example 1.
Comparative example 8
An RH vacuum furnace lining refractory material which does not include a titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating, and the rest is the same as in example 1.
Performance test
The 14 RH vacuum furnace lining refractory materials prepared in examples 1 to 6 and comparative examples 1 to 8 were subjected to the following performance tests:
test life of lower tank and circulation pipe prepared by 14 RH vacuum furnace lining refractory materials is tested, and test results are shown in table 1.
TABLE 1 detection results
As can be seen from Table 1, the RH vacuum furnace lining refractory of the present application can improve the service life of the vacuum furnace. Wherein the trial life range of the lower tank is 200-206 furnaces; the life span of the circulation pipe is 103-107 furnaces. The RH vacuum furnace lining refractory material improves the service life of the lining of the vacuum furnace through the mutual synergistic effect of the raw materials, and meets the market demand.
Comparing comparative example 1 with example 1, wherein the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 1 has a lower tank life of 190 furnaces and a circulating pipe life of 82 furnaces. In the RH vacuum furnace lining refractory of comparative example 1, the raw material of the filler does not include ceramic nanofiber aerogel, compared to example 1, so that the life span of the lower tank and the circulation pipe is reduced. The ceramic nanofiber aerogel can improve the shock resistance and the high temperature resistance of the RH vacuum furnace lining, and is beneficial to prolonging the service life of the RH vacuum furnace lining.
Comparing comparative example 2 with example 1, the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 2 has a trial life of 196 furnaces for the lower tank and 100 furnaces for the circulating pipe. In the RH vacuum furnace lining refractory of comparative example 2, the carbon-alumina fibers were replaced with the same amount of alumina refractory fibers in the raw material of the three-dimensional woven preform, compared to example 1, so that the trial life of the lower tank and the circulation pipe was reduced. The addition of the carbon-alumina fiber can improve the shock resistance and the high temperature resistance of the RH vacuum furnace lining, and is beneficial to prolonging the service life of the RH vacuum furnace lining.
Comparing comparative examples 3-5 with example 1, wherein the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 3 has a trial life of 191 furnaces and a trial life of 84 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 4 has a lower tank life of 189 furnaces and a circulating pipe life of 82 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 5 has a lower tank life of 173 furnaces and a circulating pipe life of 70 furnaces. Compared to example 1, in the RH vacuum furnace lining refractory of comparative example 3, the molybdenum disilicide-silicon nitride coating was undoped with titanium dioxide, resulting in reduced life span of the lower tank and the circulation tube; in the RH vacuum furnace lining refractory material in comparative example 4, the molybdenum disilicide-silicon nitride coating is not doped with potassium hexatitanate whiskers, so that the service lives of the lower tank and the circulation pipe are reduced; in the RH vacuum furnace lining refractory of comparative example 5, the molybdenum disilicide-silicon nitride coating was not doped with potassium hexatitanate whiskers and titanium dioxide, which further reduced the life of the lower tank and the circulating pipe. The doped potassium hexatitanate whisker and titanium dioxide cooperate with each other, so that the heat insulation performance of the molybdenum disilicide-silicon nitride coating is improved, the high temperature resistance of the RH vacuum furnace lining can be improved, and the service life of the RH vacuum furnace lining is prolonged.
Comparing comparative example 6 with example 1, the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 6 has a lower tank life of 195 furnaces and a circulating pipe life of 97 furnaces. Compared with example 1, in the RH vacuum furnace lining refractory in comparative example 6, the equivalent amount of sepiolite powder was used to replace the calcium chloride modified sepiolite powder in the raw materials of the filler, so that the service lives of the lower tank and the circulation pipe were reduced. The sepiolite powder is modified by calcium chloride, so that the moisture absorption performance of the sepiolite powder is improved, the lining matrix mixture can be effectively wetted by water at 45 ℃ in the preparation process of the RH vacuum furnace lining refractory material, the filler is uniformly adhered to the three-dimensional woven preform, the impact resistance and the high temperature resistance of the RH vacuum furnace lining can be improved, and the service life of the RH vacuum furnace lining is prolonged.
Comparing comparative example 7 with example 1, the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 7 has a lower tank life of 183 furnaces and a circulating pipe life of 81 furnaces. The RH vacuum furnace lining refractory of comparative example 7 does not include a three-dimensional braided preform, compared to example 1, so that the trial life of the lower tank and the circulation tube is reduced. The addition of the three-dimensional woven preform can improve the shock resistance and the high temperature resistance of the RH vacuum furnace lining, and is beneficial to prolonging the service life of the RH vacuum furnace lining.
Comparing comparative example 8 with example 1, the RH vacuum furnace lining refractory material prepared in example 1 has a lower tank life of 200 furnaces and a circulating pipe life of 103 furnaces; the RH vacuum furnace lining refractory material prepared in comparative example 8 has a lower tank life of 147 furnaces and a circulating pipe life of 71 furnaces. The RH vacuum furnace lining refractory of comparative example 8 does not include a titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating, compared to example 1, resulting in reduced shelf life of the lower tank and the circulating pipe. The titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating has excellent heat insulation performance, is beneficial to improving the high temperature resistance of the RH vacuum furnace lining, and further improves the service life of the RH vacuum furnace lining.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (8)
1. An RH vacuum furnace lining refractory material is characterized by comprising a three-dimensional braided preform, a lining matrix formed by filling materials in the three-dimensional braided preform, and a titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating on the surface of the lining matrix;
the three-dimensional braided preform comprises carbon-alumina fibers and silica glass fibers in a mass ratio of 3:1, and the three-dimensional braided preform is of a three-dimensional four-way structure;
the carbon-alumina fiber is obtained by sequentially carrying out stabilization treatment, carbonization treatment and graphitization treatment on polyacrylonitrile fiber, asphalt fiber and aluminum silicate fiber in a mass ratio of 1:1:3;
the filling material comprises the following raw materials in parts by weight: 1.5 to 2.5 parts of ceramic nanofiber aerogel, 15 to 20 parts of fused magnesia, 8 to 15 parts of calcium chloride modified sepiolite powder, 3 to 4 parts of microcrystalline cellulose, 2 to 3 parts of cordierite powder, 0.2 to 0.5 part of organosilicon resin powder, 1 to 2 parts of calcium aluminate cement, 0.2 to 0.5 part of aluminum dihydrogen phosphate and NaHCO 3 0.05-0.08 part, boric acid 0.02-0.05 part, magnesium lignosulfonate 0.05-0.08 part;
the ceramic nanofiber aerogel is in a chip shape;
the molybdenum disilicide-silicon nitride coating comprises the following raw materials in parts by weight: 20-25 parts of molybdenum disilicide powder, 8-12 parts of silicon nitride powder, 0.8-1.2 parts of titanium dioxide powder, 1.4-1.6 parts of potassium hexatitanate whisker, 0.1-0.2 part of high-hydrogen silicone oil, 1-1.3 parts of divinylbenzene and 0.02-0.05 part of chloroplatinic acid.
2. An RH vacuum furnace lining refractory according to claim 1, wherein the mass ratio of molybdenum disilicide powder to silicon nitride powder in the titanium dioxide and potassium hexatitanate whisker doped molybdenum disilicide-silicon nitride coating is 7:3.
3. An RH vacuum furnace lining refractory according to claim 2, wherein the silicon nitride powder has a particle size of 1-3 μm.
4. The RH vacuum furnace lining refractory of claim 1, wherein said three-dimensional braided preform is prepared by a four-step process.
5. An RH vacuum furnace lining refractory according to claim 1, wherein the grain size of the fused magnesia is 1-3mm.
6. An RH vacuum furnace lining refractory according to claim 1, wherein MgO in the fused magnesia is > 97wt%.
7. An RH vacuum furnace lining refractory according to claim 1, wherein CaO in the fused magnesia is less than 1wt%.
8. A method of preparing the RH vacuum furnace lining refractory of claim 1, comprising the steps of:
soaking the three-dimensional woven preform in a 2wt% sodium hydroxide solution for 30-40min to obtain a treated three-dimensional woven preform;
ceramic nanofiber aerogel, fused magnesia, calcium chloride modified sepiolite powder, cordierite powder, organosilicon resin powder, calcium aluminate cement, aluminum dihydrogen phosphate, microcrystalline cellulose and NaHCO 3 Uniformly mixing boric acid and magnesium lignosulfonate to obtain a mixture I;
uniformly paving 1/3-1/2 of the total amount of the mixture I in a die, then paving the processed three-dimensional braided preform, and uniformly paving the rest amount of the mixture I on the surface of the processed three-dimensional braided preform to obtain a lining matrix mixture;
then spraying water at 45 ℃ to the lining matrix mixture until the lining matrix mixture is completely soaked, wherein the water at 45 ℃ is 20% -30% of the total mass of the lining matrix mixture, and a lining matrix blank body is obtained;
sintering the lining matrix blank in a vacuum furnace for 4-6 hours at 900-1100 ℃, then cooling to 600-800 ℃, preserving heat for 2 hours, cooling to room temperature, and demoulding to obtain the lining matrix;
uniformly mixing molybdenum disilicide powder, silicon nitride powder, titanium dioxide powder and potassium hexatitanate whisker, sequentially adding high-hydrogen silicone oil, divinylbenzene and chloroplatinic acid, and stirring until the materials are uniformly mixed to obtain a coating;
coating the coating on the surface of the lining matrix by adopting a brushing method, and then preserving heat for 3 hours at the temperature of 120 ℃ in an oven to obtain a sample;
and sintering the sample at 1000 ℃ for 2 hours under the protection of inert gas to obtain the RH vacuum furnace lining refractory material.
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