CN117735997A - Production method of sizing nozzle for zirconia composite steel-making tundish - Google Patents
Production method of sizing nozzle for zirconia composite steel-making tundish Download PDFInfo
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- CN117735997A CN117735997A CN202311603175.7A CN202311603175A CN117735997A CN 117735997 A CN117735997 A CN 117735997A CN 202311603175 A CN202311603175 A CN 202311603175A CN 117735997 A CN117735997 A CN 117735997A
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- titanium nitride
- zirconia
- fine powder
- zirconia composite
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000004513 sizing Methods 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000009628 steelmaking Methods 0.000 title claims abstract description 22
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 46
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 5
- 239000007767 bonding agent Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 16
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 238000007580 dry-mixing Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 229920001187 thermosetting polymer Polymers 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000003381 stabilizer Substances 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 229920001169 thermoplastic Polymers 0.000 claims description 2
- 239000004416 thermosoftening plastic Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 abstract description 15
- 239000010959 steel Substances 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000003628 erosive effect Effects 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000002893 slag Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 31
- 238000005303 weighing Methods 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000009749 continuous casting Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000035939 shock Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000011819 refractory material Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
The invention provides a production method of a sizing nozzle for a zirconia composite steel-making tundish, which comprises the following steps: granulating the titanium nitride fine powder to obtain titanium nitride particles; mixing the titanium nitride fine powder, the zirconium oxide fine powder, the titanium nitride particles, the mixed powder and the bonding agent; molding in a mold; drying the shaped article; and heating the dried product under an inert atmosphere to obtain the required product. The production method of the sizing water gap for the zirconia composite steel-making tundish solves the problem that the sizing water gap of the zirconia composite material has low high-temperature sintering yield due to the crystal form conversion of the zirconia; the problem of nozzle burst frequently occurs during use, the sintering property of the product is improved and the zirconia crystal form is stabilized by introducing the titanium nitride fine powder and utilizing the activity of the titanium nitride fine powder, so that the sizing nozzle with high strength, high melting point, high thermal stability and high erosion resistance to metal and steel slag is obtained.
Description
Technical Field
The invention belongs to the field of refractory materials, and particularly relates to a production method of a sizing nozzle for a zirconia composite steel-making tundish.
Background
With the continuous development and progress of steelmaking and continuous casting technologies, in order to meet and adapt to the requirements of new high-efficiency continuous casting technologies and new technologies, the aspects of materials, preparation technologies, use technologies and the like of the functional refractory materials for the tundish are greatly advanced and updated. In the continuous casting production process, the sizing water gap is an important tundish functional refractory material, and the service life of the sizing water gap plays a critical role in the continuous casting efficiency and stability, so that the material selection, the preparation process and the like of the water gap are key factors for prolonging the service life of the sizing water gap in the preparation process of the sizing water gap.
If small square billets are generally cast by adopting a sizing nozzle, the sizing nozzle has the main function of controlling the flow of molten steel. Whether molten steel can flow into the crystallizer through the sizing water gap uniformly and stably is a key for ensuring the normal running of continuous casting. Therefore, the metering nozzle must have good erosion resistance and thermal stability, and should not be allowed to clog, fall off, crack and expand in diameter when in use. With the development of high-efficiency continuous casting technology, requirements such as higher service performance and service life, such as long-life hit package, are put forward for the refractory material for continuous casting. The long-life hit package only reduces the labor intensity of workers by reducing the replacement of the middle package, and meanwhile, the occurrence of production accidents can be reduced. However, there are many factors restricting the tundish Bao Ling in the actual production process, and the most common is the phenomenon of steel clamping in the tundish fixed diameter nozzle. The sizing nozzle clamped with steel can not be replaced, so that the tundish Bao Ling is reduced, the production cost is increased, and the sizing nozzle clamped with steel can cause steel drilling accidents when the sizing nozzle clamped with steel is severe. Meanwhile, in the continuous casting using process of the sizing water gap for the tundish, the tundish is corroded and corroded due to chemical components in molten steel, and the pouring ladle is also subjected to the action of temperature shock and mechanical stress, so that the damage mechanism and form of the water gap are complex. Therefore, in the preparation process of the sizing nozzle, the material selection, the preparation process, the microstructure and the like of the nozzle are key factors for prolonging the service life of the nozzle.
The sizing nozzle for the steelmaking tundish at present adopts a high-temperature sintered product made of zirconia, and the zirconia content is between 90 and 95 percent. The sizing nozzle made of the zirconia material has low high-temperature sintering yield due to the crystal form conversion of the zirconia; when in use, the water gap is frequently burst, production safety accidents occur, and steelmaking operation is influenced. In practical application, zrO is added to the material of the water gap 2 Besides, a small amount of stabilizer is also added, so that impurity elements (manganese, silicon, magnesium, aluminum and the like) in molten steel react to generate multi-element low-melting-point oxides in the using process, and erosion and diffusion of a sizing nozzle are caused along with the loss of molten steel. Titanium nitride is a high-melting-point compound, and has a melting point of 2950 ℃, good wear resistance and Mohs hardness of 8-9; the stability is good, the catalyst does not react with metals such as iron, chromium, calcium, magnesium and the like at high temperature, and the catalyst does not react with acid slag and alkaline slag under the atmosphere of carbon monoxide and nitrogen; the heat conducting property is good, and the heat stability is high; at the same time, the titanium nitride can stabilize the zirconia crystal form at high temperature. Although by adding Al 2 O 3 -ZrO 2 The modified sizing nozzle of the composite powder has the advantages of reduced apparent porosity, increased volume density and improved compressive strength, but in the practical application process, the main reason of nozzle damage is the explosion caused by poor thermal shock stability. Therefore, in order to solve the defects of the prior art, the invention prepares the sizing nozzle of the titanium nitride-zirconia composite material by utilizing the characteristics of high melting point, high strength, higher stability and the like of the titanium nitride. The method uses TiN to stabilize ZrO 2 Maintains the function of normal-temperature tetragonal phase and reduces the phase transformation rate. Simultaneous TiN and ZrO 2 The sizing nozzle has the characteristics of good chemical compatibility and no reaction in the sintering process, and is high in melting point, high in thermal stability and high in corrosion resistance to metal and steel slag. By adding TiN, cubic phase TiN can appear in the sintering process, and TiN particles are dispersed in ZrO 2 In the crystal, and is mostly located at grain boundaries. TiN particles at grain boundaries produce a "pinning" effect that retards Zr 4+ Diffusion and movement of grain boundaries, thereby suppressing ZrO 2 The growth of the particles improves the toughening effect and the fracture toughness. The titanium nitride-zirconia sizing nozzle can meet the requirements of high melting point, high thermal stability and high erosion resistance to metal and steel slag on the performance of the nozzle in steelmaking, and can improve the yield of products. Compared with the conventional ZrO 2 The compactness of the sizing nozzle made of titanium nitride-zirconia composite material is improved, the compressive strength is increased, and the thermal shock stability and molten steel flushing resistance of the nozzle are greatly improvedThe brush erosion performance solves the problems that the high-temperature firing yield is low and the nozzle is cracked frequently during use due to the crystal form conversion of zirconia in the sizing nozzle made of zirconia, and has obvious economic benefit.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for producing a metering nozzle for a zirconia composite steelmaking tundish, which solves the above-mentioned problems in the prior art.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a production method of a sizing nozzle for a zirconia composite steel-making tundish comprises the following steps:
(1) Granulating the titanium nitride fine powder: fully mixing the titanium nitride fine powder with phenolic resin powder, adding absolute ethyl alcohol for mixing, performing compression molding, drying, nitriding and sintering, and then crushing into titanium nitride particles;
(2) Mixing titanium nitride fine powder and zirconium oxide fine powder in proportion to obtain mixed powder, adding titanium nitride particles and the mixed powder into a mixing mill for dry mixing, adding a binding agent for secondary mixing, and discharging;
(3) Adding the material obtained in the step (2) into a mould for forming, and demolding;
(4) Drying the product formed in step (3);
(5) And (3) putting the product dried in the step (4) into a furnace body, heating in an inert atmosphere, and cooling to obtain the required product.
Further, in the step (1), the titanium nitride particles include particles having a particle diameter of 0 to 1 mm and particles having a particle diameter of 1 to 2 mm.
Further, in the step (2), the mass ratio of the titanium nitride to the zirconium oxide to the binder is (40-90): (10-60): (3-6).
Further, in the step (1), the titanium content of the titanium nitride fine powder is not less than 75%, the nitrogen content is not less than 18%, the carbon content is not more than 3%, and the oxygen content is not more than 2%.
Further, in the step (2), the purity of the zirconia is not less than 94%; the granularity is smaller than 320 meshes.
Further, the zirconia is unfixed monoclinic zirconia or stabilized zirconia; preferably, the stabilized zirconia stabilizer is calcium oxide or yttrium oxide.
Further, in the step (1), the bonding agent is one or two of thermosetting phenolic resin and thermoplastic phenolic resin.
Further, in the step (2), the titanium nitride fine powder and the zirconia fine powder are premixed in proportion for 30 minutes, the dry mixing time of the titanium nitride particles and the mixed powder is 5 minutes, and the secondary mixing time is 15 minutes.
Further, in the step (4), the drying temperature is 110-200 ℃ and the drying time is 24 hours.
Further, in the step (5), the inert atmosphere is nitrogen atmosphere or argon atmosphere, the heating temperature is 1400-1500 ℃, and the heating time is 3-10h.
Compared with the prior art, the production method of the sizing nozzle for the zirconia composite steelmaking tundish has the following advantages:
the production method of the sizing nozzle made of the titanium nitride-zirconia composite material solves the problem that the sizing nozzle made of the zirconia material has low rate of finished products caused by high-temperature sintering due to the crystal form conversion of the zirconia; the problem of nozzle burst frequently occurs during use, the sintering property of the product is improved and the zirconia crystal form is stabilized by introducing the titanium nitride fine powder and utilizing the activity of the titanium nitride fine powder, so that the sizing nozzle with high strength, high melting point, high thermal stability and high erosion resistance to metal and steel slag is obtained.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The present invention will be described in detail with reference to examples.
Preparation example of titanium nitride particles
1) Weighing the following raw materials in percentage by mass: 80-90 parts of titanium nitride fine powder with the grain diameter of 100-600 meshes and 3-15 parts of phenolic resin powder. Wherein the titanium nitride has a titanium content of not less than 75%, a nitrogen content of not less than 18%, a carbon content of not more than 3%, and an oxygen content of not more than 2%;
2) Mixing the raw materials in the step 1) with absolute ethyl alcohol according to a mass ratio of 10: accurately weighing 0.1-0.5, and then mixing for 5-30 min;
3) The material obtained in the step 2) is subjected to powder tabletting sample preparation to obtain a titanium nitride wafer sample, and the forming pressure is 10-100 MPa;
4) The titanium nitride wafer sample obtained in the step 3) is blown at the temperature of 10-300 ℃ to dry a drying box, so as to obtain a stable granulating material;
5) Heating the granulated material obtained in the step 4) to 800-1700 ℃ in a high-temperature atmosphere sintering furnace at a heating rate of 2-30 ℃/min under nitrogen atmosphere, and preserving heat for 0.5-12 h to obtain a sintered granulated material;
6) Crushing the sintered granulating material in the step 5), and sieving by using a 20-300 mesh screen to obtain titanium nitride particles with the granularity of 0.01-1.5 mm.
Implement one
(1) Weighing titanium nitride: 30 parts of 0-1 mm particles, 30 parts of 1-2 mm particles, 10 parts of 5-micrometer fine powder, and 30 parts of 320-mesh zirconia fine powder are weighed. Firstly, putting 5-micrometer titanium nitride fine powder and 320-mesh zirconia fine powder into a ball mill according to a proportion, and premixing for 30 minutes to obtain mixed powder. Adding the weighed titanium nitride particles and the mixed powder into a mixing mill, dry-mixing for 5 minutes, adding 5 parts of thermosetting liquid phenolic resin, secondary mixing for 15 minutes, and discharging;
(2) Weighing the mixed materials, adding the mixed materials into a mold of a molding machine, and performing compression molding;
(3) Placing the molded product into a drying kiln, and drying for 24 hours at 200 ℃;
(4) And (3) putting the dried product into a furnace body, sealing, and introducing nitrogen or argon. Heating to 1500 ℃ under the protection of nitrogen atmosphere or argon atmosphere, heating for 8 hours, naturally cooling to below 100 ℃, opening a kiln door, and discharging;
(5) And (5) detecting and packaging.
Implement two
(1) Weighing titanium nitride: 30 parts of 0-1 mm particles, 40 parts of 1-2 mm particles, 20 parts of 5-micrometer fine powder, and 10 parts of 0-1 mm zirconia fine powder are weighed. Firstly, putting 5-micrometer titanium nitride fine powder and 320-mesh zirconia fine powder into a ball mill according to a proportion, and premixing for 30 minutes to obtain mixed powder. Adding the weighed titanium nitride particles and the mixed powder into a mixing mill, dry mixing for 5 minutes, adding 5 parts of zirconium sol, secondary mixing for 15 minutes, and discharging;
(2) Weighing the mixed materials, adding the mixed materials into a mold of a molding machine, and performing compression molding;
(3) Placing the molded product into a drying kiln, and drying for 24 hours at 110 ℃;
(4) And (3) putting the dried product into a furnace body, sealing, and introducing nitrogen or argon. Heating to 1600 ℃ under the protection of nitrogen atmosphere or argon atmosphere, heating for 10 hours, naturally cooling to below 100 ℃, opening a kiln door, and discharging;
(5) And (5) detecting and packaging.
Implementation three
(1) Weighing titanium nitride: 15 parts of 0-1 mm particles, 20 parts of 1-2 mm particles, 5 parts of 5-micrometer fine powder and 30 parts of 320-mesh zirconia fine powder are weighed. Firstly, putting 5-micrometer titanium nitride fine powder and 320-mesh zirconia fine powder into a ball mill according to a proportion, and premixing for 30 minutes to obtain mixed powder. Adding the weighed titanium nitride particles and the mixed powder into a mixing mill, dry-mixing for 5 minutes, adding 5 parts of thermosetting liquid phenolic resin, secondary mixing for 15 minutes, and discharging;
(2) Weighing the mixed materials, adding the mixed materials into a mold of a molding machine, and performing compression molding;
(3) Placing the molded product into a drying kiln, and drying for 24 hours at 200 ℃;
(4) And (3) putting the dried product into a furnace body, sealing, and introducing nitrogen or argon. Heating to 1500 ℃ under the protection of nitrogen atmosphere or argon atmosphere, heating for 8 hours, naturally cooling to below 100 ℃, opening a kiln door, and discharging;
(5) And (5) detecting and packaging.
Implement four
(1) Weighing titanium nitride: 30 parts of 0-1 mm particles, 30 parts of 1-2 mm particles, 10 parts of 5-micrometer fine powder, and 60 parts of 320-mesh zirconia fine powder are weighed. Firstly, putting 5-micrometer titanium nitride fine powder and 320-mesh zirconia fine powder into a ball mill according to a proportion, and premixing for 30 minutes to obtain mixed powder. Adding the weighed titanium nitride particles and the mixed powder into a mixing mill, dry-mixing for 5 minutes, adding 5 parts of thermosetting liquid phenolic resin, secondary mixing for 15 minutes, and discharging;
(2) Weighing the mixed materials, adding the mixed materials into a mold of a molding machine, and performing compression molding;
(3) Placing the molded product into a drying kiln, and drying for 24 hours at 200 ℃;
(4) And (3) putting the dried product into a furnace body, sealing, and introducing nitrogen or argon. Heating to 1500 ℃ under the protection of nitrogen atmosphere or argon atmosphere, heating for 8 hours, naturally cooling to below 100 ℃, opening a kiln door, and discharging;
(5) And (5) detecting and packaging.
Comparative example one
Unlike example one, comparative example one was not added with titanium nitride.
Comparative example two
Unlike example one, the titanium nitride particles in comparative example two were each 0-1 mm particles.
Comparative example three
Unlike example one, the titanium nitride particles in comparative example three were all 1-2 mm particles.
Comparative example four
Unlike example one, the titanium nitride particles in comparative example four were all 5 micron fine powders.
Comparative example five
Unlike example one, the titanium nitride of comparative example five contained only 30 parts of particles of 0 to 1 mm, and no titanium nitride fine powder.
Comparative example six
Unlike example one, the titanium nitride of comparative example six contained only 100 parts of particles of 0 to 1 mm, and no titanium nitride fine powder.
Comparative example seven
Unlike in example one, the titanium nitride of comparative example seven comprised only 30 parts of particles of 1 to 2 mm, and was free of titanium nitride fine powder.
Comparative example eight
Unlike example one, the titanium nitride of comparative example eight included only 100 parts of 1-2 mm particles, and was free of titanium nitride fine powder.
Comparative example nine
Unlike example one, comparative example nine comprised only 30 parts of 5 micron fine powder, without titanium nitride particles.
Comparative example ten
Unlike example one, the titanium nitride of comparative example ten contained only 100 parts of 5 μm fine powder, and no titanium nitride particles.
Product performance detection
The products prepared in the examples and the comparative examples are subjected to normal temperature compressive strength test and thermal shock resistance test, and the test results are as follows:
| normal temperature compressive strength/MPa | Thermal shock resistance (1100 ℃ to water cooling)/times | |
| Example 1 | 350 | 38 |
| Example two | 343 | 34 |
| Example III | 310 | 28 |
| Example IV | 338 | 32 |
| Comparative example one | 230 | 7 |
| Comparative example two | 296 | 20 |
| Comparative example three | 308 | 22 |
| Comparative example four | 276 | 18 |
| Comparative example five | 266 | 16 |
| Comparative example six | 243 | 14 |
| Comparative example seven | 290 | 21 |
| Comparative example eight | 281 | 20 |
| Comparative example nine | 303 | 26 |
| Comparative example ten | 322 | 27 |
Claims (10)
1. A production method of a sizing nozzle for a zirconia composite steel-making tundish is characterized by comprising the following steps: the method comprises the following steps:
(1) Granulating the titanium nitride fine powder: fully mixing the titanium nitride fine powder with phenolic resin powder, adding absolute ethyl alcohol for mixing, performing compression molding, drying, nitriding and sintering, and then crushing into titanium nitride particles;
(2) Mixing titanium nitride fine powder and zirconium oxide fine powder in proportion to obtain mixed powder, adding titanium nitride particles and the mixed powder into a mixing mill for dry mixing, adding a binding agent for secondary mixing, and discharging;
(3) Adding the material obtained in the step (2) into a mould for forming, and demolding;
(4) Drying the product formed in step (3);
(5) And (3) putting the product dried in the step (4) into a furnace body, heating in an inert atmosphere, and cooling to obtain the required product.
2. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the titanium nitride particles comprise particles with the particle size of 0-1 mm and particles with the particle size of 1-2 mm.
3. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the mass ratio of the titanium nitride to the zirconium oxide to the binding agent is (40-90): (10-60): (3-6).
4. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the titanium content of the titanium nitride fine powder is not less than 75%, the nitrogen content is not less than 18%, the carbon content is not more than 3% and the oxygen content is not more than 2%.
5. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the purity of the zirconia is not less than 94%; the granularity is smaller than 320 meshes.
6. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 5, wherein the method comprises the following steps: the zirconia is unfixed monoclinic zirconia or stabilized zirconia; preferably, the stabilized zirconia stabilizer is calcium oxide or yttrium oxide.
7. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the bonding agent is one or two of thermosetting phenolic resin and thermoplastic phenolic resin.
8. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the titanium nitride fine powder and the zirconia fine powder are premixed for 30 minutes according to the proportion, the dry mixing time of the titanium nitride particles and the mixed powder is 5 minutes, and the secondary mixing time is 15 minutes.
9. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (4), the drying temperature is 110-200 ℃ and the drying time is 24 hours.
10. The method for producing the sizing nozzle for the zirconia composite steelmaking tundish as claimed in claim 1, wherein the method comprises the following steps: in the step (5), the inert atmosphere is nitrogen atmosphere or argon atmosphere, the heating temperature is 1400-1500 ℃, and the heating time is 3-10h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311603175.7A CN117735997A (en) | 2023-11-28 | 2023-11-28 | Production method of sizing nozzle for zirconia composite steel-making tundish |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311603175.7A CN117735997A (en) | 2023-11-28 | 2023-11-28 | Production method of sizing nozzle for zirconia composite steel-making tundish |
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