CN116199509A - Toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets and production process thereof - Google Patents

Toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets and production process thereof Download PDF

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CN116199509A
CN116199509A CN202310081537.4A CN202310081537A CN116199509A CN 116199509 A CN116199509 A CN 116199509A CN 202310081537 A CN202310081537 A CN 202310081537A CN 116199509 A CN116199509 A CN 116199509A
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parts
weight
zirconia
die
drying
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王传学
吴佩霞
吴建湘
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Jiangsu Tairui Refractory Co ltd
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Jiangsu Tairui Refractory Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D41/00—Casting melt-holding vessels, e.g. ladles, tundishes, cups or the like
    • B22D41/50—Pouring-nozzles
    • B22D41/52—Manufacturing or repairing thereof
    • B22D41/54—Manufacturing or repairing thereof characterised by the materials used therefor
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    • 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
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract

The invention relates to the technical field of continuous steel casting, in particular to a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets, which comprises a zirconia ceramic inner liner and a refractory material outer liner; the zirconia ceramic lining comprises the following raw materials in parts by weight: 10 to 60 parts of stabilized zirconia, 35 to 90 parts of monoclinic phase zirconia, 2 to 17 parts of alpha-Al 2O3 micro powder, 1 to 11 parts of silicon carbide micro powder, 1 to 3 parts of boron nitride micro powder, 1 to 6 parts of magnesia micro powder and 1 to 2 parts of yttrium oxide micro powder; the refractory material jacket comprises brown corundum, white corundum, high-alumina homogenized material or high-alumina bauxite, crystalline flake graphite, fused quartz granule, calcined alumina micropowder, metal silicon powder and phenolic resin. The tundish nozzle has long service life, can improve the service life of a tundish, the yield/operation rate of a continuous casting machine, the molten steel yield and the quality of continuous casting billets, and can obviously reduce the refractory material consumption of the tundish per ton of steel and save the cost.

Description

Toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets and production process thereof
Technical Field
The invention relates to the technical field of steel continuous casting, in particular to a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, bloom and rectangular billets and a production process thereof.
Background
In modern steel production, molten steel after smelting is cast into continuous casting blanks which can be directly used for rolling steel by a continuous casting machine, so as to roll various commodity steels, wherein the long-flow process is started from iron ore sintering or the short-flow process is started from scrap steel smelting.
The continuous casting of steel is completed by a continuous casting machine, and the continuous casting machine consists of a ladle turntable, a tundish, a crystallizer, a secondary cooling zone, a withdrawal and straightening machine, a casting blank fixed-length cutting device, a deburring number spraying device and the like; molten steel smelted in a metallurgical furnace is poured into a steel containing barrel (ladle) and then is lifted to a ladle rotary table of a continuous casting machine, the ladle rotary table rotates the ladle molten steel above a tundish, the ladle is poured into the tundish through a sliding gate and a long gate, after the molten steel in the tundish floats upwards through inclusions and is homogenized in temperature, the molten steel is matched with a tundish gate through a stopper rod to control flow through a switch, the molten steel is poured into a crystallizer through a submerged gate hung at the bottom of the tundish, the molten steel in the crystallizer is condensed into a billet shell with a certain thickness and a billet with a liquid core under the forced cooling action of high-pressure cooling water, a withdrawal and straightening machine straightens the continuous casting billet through a dummy bar in a gas spray cooling secondary cooling zone, the fully condensed and solidified continuous casting billet reaching a specified length is cut off by a casting billet cutting device, and is sent to a warehouse or directly hot-rolled to a steel mill after being cooled by a cooling bed through a deburring and finishing number spraying procedure and the like.
The tundish is a core component of the continuous casting machine and mainly has the functions of purifying molten steel, homogenizing components/temperatures, shunting the molten steel to each crystallizer, controlling the flow of the molten steel injected into the crystallizer, temporarily storing the molten steel to keep continuous casting and the like.
Because the design parameters of the cooling intensity of the crystallizer and the cooling intensity of the secondary cooling zone are different, the billet drawing speed of each casting flow of different sections of each continuous casting machine is limited in a specified range (exceeding the specified range can lead to the casting billet to be drawn still, cracked or leaked), so the flow of molten steel injected into the crystallizer from a tundish must be continuously stabilized in the limited range, and can be regulated at any time according to the solidification state of the casting billet.
The continuous casting operation of the square (round) billet/rectangular billet and slab continuous casting machine generally adopts a bowl mouth of a tundish nozzle buried at the bottom of a tundish, and is matched with a stopper rod head hoisted at the upper part of the bowl mouth of the nozzle, so as to play roles of switching and controlling the flow of molten steel. After the bowl mouth/inner core and the stopper rod head of the tundish nozzle are washed and corroded seriously, the molten steel quantity injected into the crystallizer exceeds the upper limit of the billet drawing speed of the continuous casting machine, and the continuous casting operation is stopped to replace the tundish. The maximum service life of the zirconium nozzle for continuous casting of the square (round) billet/rectangular billet continuous casting machine is generally 18-35 hours. Most of slab continuous casting machines use tundish water feeding ports made of aluminum-carbon materials, and the highest service life is generally 15-20 hours.
The existing tundish is short in service life and needs to be replaced frequently, consumable cost is high, production is required to be suspended in the replacement process, and the continuous casting billet is cut back to the furnace, so that the productivity and the operation rate of the continuous casting machine and the molten steel yield are difficult to be improved.
The service life of the tundish nozzle is prolonged, the problem of neck clamping of the service life of the tundish nozzle is solved, the service life of the tundish can be prolonged synchronously, the productivity and the operation rate of a continuous casting machine are improved, the molten steel yield is improved, the quality of continuous casting billets is improved, and the refractory material consumption of the tundish per ton of steel can be obviously reduced.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets and a production process thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, bloom and rectangular bloom and the production process thereof comprise a zirconia ceramic inner liner and a refractory material outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
10 to 60 parts of stabilized zirconia, 35 to 90 parts of monoclinic phase zirconia, 2 to 17 parts of alpha-Al 2O3 micro powder, 1 to 11 parts of silicon carbide micro powder, 1 to 3 parts of boron nitride micro powder, 1 to 6 parts of magnesia micro powder and 1 to 2 parts of yttrium oxide micro powder;
The fireproof material jacket comprises the following raw materials in parts by weight:
45-80 parts of brown alumina, white corundum, high-alumina homogenized material or high-alumina bauxite, 8-25 parts of crystalline flake graphite, 5-25 parts of fused Dan Yingke granules, 3-15 parts of calcined alumina micropowder, 0.5-4 parts of metal silicon powder and 8-12 parts of phenolic resin.
Preferably, the stabilized zirconia in the zirconia ceramic lining material has a stability of 60 to 80%.
Preferably, the alumina grade of brown alumina, white corundum, high-alumina homogenized material or high-alumina bauxite in the refractory material jacket raw material is 85% or more.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
s1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: adding stabilized zirconia, monoclinic phase zirconia, alpha-Al 2O3 micro powder, silicon carbide micro powder, boron nitride micro powder, magnesium oxide micro powder and yttrium oxide micro powder into a homomixer according to parts by weight for premixing to obtain a premixed batch;
s1-2, grinding and pulping: filling the premixed batch into a high-speed ball mill with a zirconia lining, adding deionized water, and grinding to obtain slurry;
s1-3, molding: the molding mode is one of injection molding, grouting molding, pressurizing vibration molding, mechanical pressing molding and isostatic pressing molding;
S1-4, drying the green body: forced drying by using a forced air drying kiln, wherein the water content of the dried blank is less than 0.1%;
s1-5, sintering: sintering by using a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating body, wherein the highest sintering temperature is 1520-1760 ℃, the heating speed is 4-8 ℃/h, and the heat preservation time at the highest temperature is not less than 6 hours;
s1-6, processing and grinding and coating surface paint;
s2, preparing a fireproof material jacket:
s2-1, proportioning: placing brown corundum, white corundum, high-alumina homogenized material or high-alumina bauxite, crystalline flake graphite, fused quartz granule material, calcined alumina micropowder and metal silicon powder into a batching machine according to weight parts, and uniformly mixing;
s2-2, mixing and granulating: putting all the matched powder materials into a mixing granulator with a high-speed rotor, carrying out dry mixing for 3-7 minutes, putting phenolic resin into the mixing granulator, carrying out high-speed mixing granulation for 8-30 minutes, and discharging;
s2-3, mud drying: mixing the materials, trapping the materials for 24 hours, drying, and discharging redundant solvent;
s2-4, product molding: adopting a 20Gr or 45# quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: assembling the inner die and the outer die, filling and sealing the die, loading the die into a high-pressure cylinder of an isostatic press for pressurization treatment, and taking out for demolding;
S2-5, drying: forced drying is carried out by using a forced air drying kiln, and the water content of the dried blank is less than 0.1 percent;
s2-6, sintering: firing at a temperature of up to 1040 ℃ in a reducing atmosphere to form a carbon network bond;
s2-7, processing.
Preferably, when the zirconia ceramic lining is formed by adopting a grouting method, in the step S1-2, the premixed batch is filled into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and the mixture is ground and stirred for 30 minutes at a grinding speed of 200-400 revolutions per minute to prepare slurry;
the casting method is used for forming, a gypsum mold is used for manufacturing a forming mold, slurry is processed in vacuum, the slurry is injected into the mold, the mold after injection molding is put into a curing room with the temperature of 20-35 ℃ and the relative humidity of 65-85% for curing for 24-36 hours, and the molded blank is obtained after demolding.
Preferably, when the zirconia ceramic lining is formed by adopting a compression vibration forming method, in the step S1-2, the premixed batch is filled into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and the mixture is ground and stirred for 30 minutes at a grinding speed of 200-400 revolutions per minute to prepare slurry;
Spray granulation and drying steps are added between the step S1-2 and the step S1-3: loading the slurry into a storage tank of a spray granulator, carrying out spray drying granulation at the air temperature of 150-300 ℃ to obtain a granulation material with the granularity of 0.01-1.5 mm, keeping the granulation material in a sealed state with the water content of 0.3-1.1%, and trapping the granulation material for 24-36 hours at the temperature of 30+/-2 ℃;
and (3) forming by a pressurizing vibration forming method, namely adding the pelleting material into a quenching steel die to smooth the material surface, pressurizing for multiple times according to the principle of light before heavy middle exhaust, and discharging the die after pressurizing when the upper pressure head reaches the limit.
Preferably, when the zirconia ceramic lining is formed by adopting an isostatic pressing method, in the step S1-2, the premixed batch is filled into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and the mixture is ground and stirred for 30 minutes at a grinding speed of 200-400 revolutions per minute to prepare slurry;
spray granulation and drying steps are added between the step S1-2 and the step S1-3: loading the slurry into a storage tank of a spray granulator, carrying out spray drying granulation at the air temperature of 150-300 ℃ to obtain a granulation material with the granularity of 0.01-1.5 mm, keeping the granulation material in a sealed state with the water content of 0.3-1.1%, and trapping the granulation material for 24-36 hours at the temperature of 30+/-2 ℃;
The isostatic compaction method is to use a combined die with an inner core of a quenching steel die and an outer die of hard rubber or high-elasticity polyurethane, to inject pelleting materials into the die, to vibrate for 5-20 seconds by using a high-frequency vertical vibration type vibrating table, to supplement pelleting materials in the die, to seal the die, to put the die into a high-pressure cylinder of an isostatic press to be pressurized to 90-250 Mpa for 3-12 minutes, to release pressure, and to take out and to demould.
Preferably, when the zirconia ceramic lining is formed by adopting a coagulation injection method, loading the premixed batch into a high-speed ball mill of the zirconia lining, respectively adding 50-80 parts by weight of acrylamide monomer, 10-20 parts by weight of methylene bisacrylamide cross-linking agent, 5-10 parts by weight of JA281 dispersing agent and 40-200 parts by weight of deionized water, grinding and stirring for 20-40 minutes at a grinding speed of 200-400 rpm, and then adding ammonium persulfate initiator, and stirring to obtain slurry;
the casting method is to manufacture a forming die by using aluminum alloy, vacuum treat slurry, inject the slurry into the die, put the die after injection molding into a drying oven with the temperature of 80-100 ℃ for curing for 2 hours, and remove and demould the die to obtain a formed blank.
Preferably, in the step S2-4, the pressure of the isostatic press is 90-250 Mpa, and the holding time is 3-12 minutes.
The beneficial effects of the invention are as follows:
1. the zirconium lining uses micro powder such as alumina, silicon carbide, boron nitride, magnesium oxide and the like as a toughening agent, so that the strength and toughness of the product are greatly improved, and the flushing resistance and fracture resistance of the lining are improved; the product has uniform and compact structure, is difficult to infiltrate and corrode, and greatly improves the flushing resistance and corrosion resistance of the product; the micro-scale and nano-scale micropores formed by the tissue reduce the thermal expansion coefficient and the uniformity of thermal expansion of the product, and improve the thermal shock stability of the product to the maximum extent.
2. The components with good dispersibility and large specific gravity difference of each ingredient component are not easy to segregate, and the dry powder material is prepared by adopting a slurry spray granulation method, so that the components and the tissues of each part of the product can be ensured to be uniform no matter the slurry is directly used for molding or the dry powder material is used for molding.
3. The composite outer sleeve and the inner liner are secondarily molded by using a press, so that the product has good integrity and standard external dimension, the use accidents of bowl removal, zirconium core fracture, mud joint drilling steel and the like of the traditional fireclay assembly process product are avoided, and the density strength uniformity of the outer sleeve secondarily molded by an isostatic pressing method is good, thereby being beneficial to prolonging the service life and the quality stability of a tundish nozzle.
4. The zirconium lining is shaped and thickness-selected according to the use requirement of the product, and different shaping methods are selected, so that not only is the thermal shock stability of the zirconium lining improved, but also the consumption of high-cost zirconia raw materials is greatly reduced, and the product profit is greatly increased for production enterprises.
Drawings
Fig. 1 is a schematic diagram of a tundish nozzle of toughened zirconia ceramic for continuous casting of slabs, billets and rectangular billets.
In the figure: 1-zirconia ceramic lining, 2-refractory material jacket, 3-graphite argon blowing nozzle and 4-zirconium slide sheet.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Embodiment one:
referring to fig. 1, a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets comprises a zirconia ceramic inner liner and a refractory outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
20 parts of stabilized zirconia with 60-80% stability, 70 parts of monoclinic phase zirconia and alpha-Al 2 O 3 5 parts of micropowder, 3 parts of silicon carbide micropowder, 2 parts of boron nitride micropowder, 1 part of magnesium oxide micropowder and 2 parts of yttrium oxide micropowder.
The fireproof material jacket comprises the following raw materials in parts by weight:
60 parts of bauxite, 10 parts of crystalline flake graphite, 15 parts of fused quartz particles, 10 parts of calcined alumina micropowder, 2 parts of metal silicon powder and 8 parts of phenolic resin.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
s1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micropowder, the silicon carbide micropowder, the boron nitride micropowder, the magnesium oxide micropowder and the yttrium oxide micropowder into a homomixer according to parts by weight, and premixing for 20 minutes to obtain a premixed batch;
s1-2, grinding and pulping:
preparing grouting slurry, loading the premixed batch into a high-speed ball mill with a zirconia lining, adding 2 parts by weight of polyvinyl alcohol, 0.5 part by weight of dextrin or hydroxymethyl cellulose, 150 parts by weight of deionized water and 100 parts by weight of zirconia grinding balls with the diameter of 5mm, and grinding and stirring at a grinding speed of 300 revolutions per minute for 30 minutes to obtain the slurry;
s1-3, molding: the grouting method is pressureless casting molding, and the volume density of the produced product is about 0.16-0.21 g/cm lower than that of the pressurizing vibration molding method, the mechanical pressing method and the isostatic pressing method 3 And air holes are easily formed in the molding process.
The casting method is adopted for molding, a gypsum mold is used for manufacturing a molding mold, and the setting of a mold firing shrinkage scale is 15%. Placing the mould into a vacuum box, carrying out vacuum stirring treatment on the prepared slurry for at least 30 minutes under the vacuum degree of-90 Kpa, and injecting the slurry after the vacuum treatment into the mould through a discharge pipe at the bottom of a slurry barrel. And (3) placing the die subjected to injection molding into a curing room with the temperature of 30 ℃ and the relative humidity of 80 percent for curing for 30 hours, and demolding to obtain the molded blank. The molded blank is maintained for 30 hours under the condition of maintaining 55% relative humidity, and is naturally dried. After naturally drying for 24 hours, forced drying was performed.
S1-4, drying the green body: forced drying is performed using a forced air drying kiln. The heating rates of the two temperature sections of 80-110 ℃ and 150-180 ℃ are not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S1-5, sintering: sintering in a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating element.
S1-5-1, uniformly paving 8mm thick zirconia sand with granularity of 0.5mm on a kiln table, and then stably placing the ceramic blank on the zirconia sand in a field. When a plurality of kilns are installed, the interval distance between two adjacent kilns is required to be more than 30mm. The distance between the blank and the heating element is more than 30mm;
S1-5-2, setting the highest firing temperature at 1600 ℃, controlling the heating speed at 6 ℃/h, and keeping the temperature at the highest temperature for at least 6 hours;
s1-5-3, after the sintering is finished, naturally cooling, controlling the cooling speed to be not more than 15 ℃/h in the range of 1200-900 ℃, and discharging the kiln after the kiln temperature is reduced to be below 200 ℃.
S1-6, processing and grinding: cutting the end of the sintered blank by using a diamond cutter for the part exceeding the standard size, wherein the end face is kept perpendicular to the axis during cutting; the sintered blank meeting the requirement of the appearance size does not need to be processed.
The ceramic lining can be integrally formed into an integral lining, and can also be assembled into a combined lining after being molded and sintered in a segmented mode according to equipment conditions and individuation requirements based on lining performance.
S1-7, coating: to reduce the heat transfer of the ceramic liner to the refractory jacket, the outer surface of the ceramic liner is coated with a low expansion, low thermal conductivity coating to prevent cracking of the jacket by thermal shock from the ceramic liner.
S2, preparing a fireproof material jacket:
s2-1, proportioning: placing high bauxite, crystalline flake graphite, fused quartz particles, calcined alumina micropowder and metal silicon powder with the grade of 85% or more into a proportioning machine, and uniformly mixing;
S2-2, mixing and granulating: all the powder is put into a mixing granulator with a high-speed rotor to be mixed for 5 minutes, and the mixture is put into phenolic resin to be mixed and granulated for 15 minutes at high speed and then discharged.
S2-3, mud drying: after the mixture is trapped for 24 hours, the mixture is dried by a dryer, excess solvent is discharged, and the residual volatile is kept within the range of 0.8-1.4%.
S2-4, product molding: adopting a 20Gr quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: and (3) assembling a steel mould and a rubber soft mould, mounting a zirconium inner bushing on a steel core for fixing, weighing aluminum-carbon outer sleeve pug with proper weight, adding the aluminum-carbon outer sleeve pug into the mould, uniformly vibrating the soft mould for filling the pug, and sealing the mould. The mould is put into a high-pressure cylinder of an isostatic press to be pressurized to 150Mpa for 10 minutes, and then is decompressed and taken out for demoulding. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S2-5, drying: forced drying is carried out by using a forced air drying kiln, the heating speed of two temperature sections of 80-110 ℃ and 150-180 ℃ is not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S2-6, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S2-7, processing: and (3) machining the outer surface of the product and grinding the surface of the sliding plate to ensure that the appearance size of the product meets the drawing requirement of a user.
S2-8, auxiliary processing: and carrying out auxiliary processing operations such as anti-oxidation coating, anti-sticking coating, graphite nozzle installation, graphite emulsion coating and the like on the processed product, and packaging.
Embodiment two:
referring to fig. 1, a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets comprises a zirconia ceramic inner liner and a refractory outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
30 parts of stabilized zirconia with 60-80% of stability, 60 parts of monoclinic phase zirconia and alpha-Al 2 O 3 10 parts of micropowder, 1 part of silicon carbide micropowder, 1 part of boron nitride micropowder, 3 parts of magnesium oxide micropowder and 1 part of yttrium oxide micropowder.
The fireproof material jacket comprises the following raw materials in parts by weight:
50 parts of brown corundum, 15 parts of crystalline flake graphite, 15 parts of fused quartz particles, 10 parts of calcined alumina micropowder, 4 parts of metal silicon powder and 10 parts of phenolic resin.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
S1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micropowder, the silicon carbide micropowder, the boron nitride micropowder, the magnesium oxide micropowder and the yttrium oxide micropowder into a homomixer according to parts by weight, and premixing for 20 minutes to obtain a premixed batch;
s1-2, grinding and pulping:
preparing slurry for a compression vibration molding method, loading the premixed batch into a high-speed ball mill with a zirconia lining, adding 3 parts by weight of polyvinyl alcohol, 0.5 part by weight of dextrin or hydroxymethyl cellulose, 180 parts by weight of deionized water and 100 parts by weight of zirconia grinding balls with the diameter of 5mm, and grinding and stirring at a grinding speed of 300 revolutions per minute for 30 minutes to obtain the slurry;
s1-3, spray granulation and drying: the slurry is put into a storage tank of a spray granulator, the air temperature is set to 200 ℃, spray drying granulation is carried out, and the granulation material with the main granularity of 0.01-1.5 mm is prepared, and the water content of qualified granulation material is controlled to be 0.3-1.1%. And (3) hermetically preserving the qualified pelleting material, and using the pelleting material after trapping the pelleting material for 30 hours at the temperature of 30+/-2 ℃.
S1-4, molding: the method adopts a pressurizing vibration molding method, adopts a 45# quenching steel mold, and adopts a pressurizing vibration molding machine, a double-sided pressurizing oil press or a friction press for pressurizing molding. Weighing a pelleting material with a set weight, adding the pelleting material into a die to smooth the material surface, pressurizing for multiple times according to the principle of light before heavy middle exhaust, and discharging the die after pressurizing is finished when an upper pressure head reaches limit.
When the molding is performed by the mechanical press method, the molding step is the same as that of the molding by the pressing vibration molding method.
S1-5, drying the green body: forced drying is performed using a forced air drying kiln. The heating rates of the two temperature sections of 80-110 ℃ and 150-180 ℃ are not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S1-6, sintering: sintering in a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating element.
S1-6-1, uniformly paving 8mm thick zirconia sand with granularity of 0.5mm on a kiln table, and then stably placing the ceramic blank on the zirconia sand in a field. When a plurality of kilns are installed, the interval distance between two adjacent kilns is required to be more than 30mm. The distance between the blank and the heating element is more than 30mm;
s1-6-2, setting the highest firing temperature at 1600 ℃, controlling the heating speed at 6 ℃/h, and keeping the temperature at the highest temperature for at least 6 hours;
s1-6-3, after the sintering is finished, naturally cooling, controlling the cooling speed to be not more than 15 ℃/h in the range of 1200-900 ℃, and discharging the kiln after the kiln temperature is reduced to be below 200 ℃.
S1-7, processing and grinding: cutting the end of the sintered blank by using a diamond cutter for the part exceeding the standard size, wherein the end face is kept perpendicular to the axis during cutting; the sintered blank meeting the requirement of the appearance size does not need to be processed.
The ceramic lining can be integrally formed into an integral lining, and can also be assembled into a combined lining by using fireclay after being molded and sintered in a segmented mode according to equipment conditions and individuation requirements based on lining performance.
S1-8, coating: to reduce the heat transfer of the ceramic liner to the refractory jacket, the outer surface of the ceramic liner is coated with a low expansion, low thermal conductivity coating to prevent cracking of the jacket by thermal shock from the ceramic liner.
S2, preparing a fireproof material jacket:
s2-1, proportioning: placing brown corundum, crystalline flake graphite, fused quartz particles, calcined alumina micropowder and metal silicon powder into a batching machine, and uniformly mixing;
s2-2, mixing and granulating: all the powder is put into a mixing granulator with a high-speed rotor to be mixed for 5 minutes, and the mixture is put into phenolic resin to be mixed and granulated for 20 minutes at high speed and then discharged.
S2-3, mud drying: after the mixture is trapped for 24 hours, the mixture is dried by a dryer, excess solvent is discharged, and the residual volatile is kept within the range of 0.8-1.4%.
S2-4, product molding: adopting a 45# quenched steel inner die and a high-elasticity polyurethane outer die, and forming by using an isostatic press: and (3) assembling a steel mould and a rubber soft mould, mounting a zirconium inner bushing on a steel core for fixing, weighing aluminum-carbon outer sleeve pug with proper weight, adding the aluminum-carbon outer sleeve pug into the mould, uniformly vibrating the soft mould for filling the pug, and sealing the mould. The mould is put into a high-pressure cylinder of an isostatic press to be pressurized to 150Mpa for 10 minutes, and then is decompressed and taken out for demoulding. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S2-5, drying: forced drying is carried out by using a forced air drying kiln, the heating speed of two temperature sections of 80-110 ℃ and 150-180 ℃ is not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S2-6, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S2-7, processing: and (3) machining the outer surface of the product and grinding the surface of the sliding plate to ensure that the appearance size of the product meets the drawing requirement of a user.
S2-8, auxiliary processing: and carrying out auxiliary processing operations such as anti-oxidation coating, anti-sticking coating, graphite nozzle installation, graphite emulsion coating and the like on the processed product, and packaging.
Embodiment III:
referring to fig. 1, a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets comprises a zirconia ceramic inner liner and a refractory outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
50 parts of stabilized zirconia with 60-80% of stability, 40 parts of monoclinic phase zirconia and alpha-Al 2 O 3 8 parts of micropowder, 5 parts of silicon carbide micropowder, 1 part of boron nitride micropowder, 1 part of magnesium oxide micropowder and 2 parts of yttrium oxide micropowder.
The fireproof material jacket comprises the following raw materials in parts by weight:
50 parts of high-alumina homogenized material, 15 parts of crystalline flake graphite, 5 parts of fused quartz particles, 12 parts of calcined alumina micropowder, 2 parts of metal silicon powder and 10 parts of phenolic resin.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
s1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micropowder, the silicon carbide micropowder, the boron nitride micropowder, the magnesium oxide micropowder and the yttrium oxide micropowder into a homomixer according to parts by weight, and premixing for 20 minutes to obtain a premixed batch;
s1-2, grinding and pulping: preparing slurry for an isostatic compaction method, loading the premixed batch into a high-speed ball mill with a zirconia lining, adding 2 parts by weight of polyvinyl alcohol, 1 part by weight of dextrin or hydroxymethyl cellulose, 160 parts by weight of deionized water and 100 parts by weight of zirconia grinding balls with the diameter of 5mm, and grinding and stirring at a grinding speed of 300 revolutions per minute for 30 minutes to obtain the slurry;
s1-3, spray granulation and drying: the slurry is put into a storage tank of a spray granulator, the air temperature is set to 200 ℃, spray drying granulation is carried out, and the granulation material with the main granularity of 0.01-1.5 mm is prepared, and the water content of qualified granulation material is controlled to be 0.3-1.1%. And (3) hermetically preserving the qualified pelleting material, and using the pelleting material after trapping the pelleting material for 30 hours at the temperature of 30+/-2 ℃.
S1-4, molding: and (3) isostatic compaction is adopted, and a combined die with an inner core of 20Gr quenching steel die and an outer die of high-elasticity polyurethane is used. Weighing the granulating material with proper weight, injecting into a mould, vibrating for 15 seconds by using a high-frequency vertical vibration type vibrating table, supplementing the granulating material in the mould to a proper height, and sealing the mould. The die is put into a high-pressure cylinder of an isostatic press to be pressurized to 150Mpa for 10 minutes, and then is decompressed, taken out and demoulded. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S1-5, drying the green body: forced drying is performed using a forced air drying kiln. The heating rates of the two temperature sections of 80-110 ℃ and 150-180 ℃ are not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S1-6, sintering: sintering in a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating element.
S1-6-1, uniformly spreading zirconia sand with the granularity of 0.3mm and the thickness of 6mm on a kiln table, and then stably placing the ceramic blank on the zirconia sand in a field. When a plurality of kilns are installed, the interval distance between two adjacent kilns is required to be more than 30mm. The distance between the blank and the heating element is more than 30mm;
S1-6-2, setting the highest firing temperature at 1580 ℃, controlling the heating speed at 6 ℃/h, and keeping the temperature at the highest temperature for at least 6 hours;
s1-6-3, after the sintering is finished, naturally cooling, controlling the cooling speed to be not more than 15 ℃/h in the range of 1200-900 ℃, and discharging the kiln after the kiln temperature is reduced to be below 200 ℃.
S1-7, processing and grinding: cutting the end of the sintered blank by using a diamond cutter for the part exceeding the standard size, wherein the end face is kept perpendicular to the axis during cutting; the sintered blank meeting the requirement of the appearance size does not need to be processed.
The ceramic lining can be integrally formed into an integral lining, and can also be assembled into a combined lining by using fireclay after being molded and sintered in a segmented mode according to equipment conditions and individuation requirements based on lining performance.
S1-8, coating: to reduce the heat transfer of the ceramic liner to the refractory jacket, the outer surface of the ceramic liner is coated with a low expansion, low thermal conductivity coating to prevent cracking of the jacket by thermal shock from the ceramic liner.
S2, preparing a fireproof material jacket:
s2-1, proportioning: placing 85% or more grade high-alumina homogenized material, crystalline flake graphite, fused quartz granule material, calcined alumina micropowder and metal silicon powder into a proportioning machine, and uniformly mixing;
S2-2, mixing and granulating: all the powder is put into a mixing granulator with a high-speed rotor to be mixed for 5 minutes, and the mixture is put into phenolic resin to be mixed and granulated for 15 minutes at high speed and then discharged.
S2-3, mud drying: after the mixture is trapped for 24 hours, the mixture is dried by a dryer, excess solvent is discharged, and the residual volatile is kept within the range of 0.8-1.4%.
S2-4, product molding: adopting a 45# quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: and (3) assembling a steel mould and a rubber soft mould, mounting a zirconium inner bushing on a steel core for fixing, weighing aluminum-carbon outer sleeve pug with proper weight, adding the aluminum-carbon outer sleeve pug into the mould, uniformly vibrating the soft mould for filling the pug, and sealing the mould. The mould is put into a high-pressure cylinder of an isostatic press to be pressurized to 150Mpa for 10 minutes, and then is decompressed and taken out for demoulding. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S2-5, drying: forced drying is carried out by using a forced air drying kiln, the heating speed of two temperature sections of 80-110 ℃ and 150-180 ℃ is not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S2-6, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S2-7, processing: and (3) machining the outer surface of the product and grinding the surface of the sliding plate to ensure that the appearance size of the product meets the drawing requirement of a user.
S2-8, auxiliary processing: and carrying out auxiliary processing operations such as anti-oxidation coating, anti-sticking coating, graphite nozzle installation, graphite emulsion coating and the like on the processed product, and packaging.
Embodiment four:
referring to fig. 1, a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets comprises a zirconia ceramic inner liner and a refractory outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
40 parts of stabilized zirconia with 60-80% of stability, 50 parts of monoclinic phase zirconia and alpha-Al 2 O 3 5 parts of micropowder, 5 parts of silicon carbide micropowder, 2 parts of boron nitride micropowder, 2 parts of magnesium oxide micropowder and 1 part of yttrium oxide micropowder.
The fireproof material jacket comprises the following raw materials in parts by weight:
45 parts of white corundum, 25 parts of crystalline flake graphite, 25 parts of fused Dan Yingke granules, 3 parts of calcined alumina micropowder, 2 parts of metal silicon powder and 8 parts of phenolic resin.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
S1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micropowder, the silicon carbide micropowder, the boron nitride micropowder, the magnesium oxide micropowder and the yttrium oxide micropowder into a homomixer according to parts by weight, and premixing for 20 minutes to obtain a premixed batch;
s1-2, grinding and pulping: preparing slurry formed by a coagulation injection method, filling the premixed batch into a high-speed ball mill lined with zirconia, respectively adding 60 parts by weight of acrylamide monomer, 10 parts by weight of methylene bisacrylamide crosslinking agent, 8 parts by weight of JA281 dispersing agent and 180 parts by weight of deionized water, grinding and stirring for 30 minutes at a grinding speed of 300 revolutions per minute, then adding ammonium persulfate initiator, and stirring for 3 minutes to obtain slurry;
s1-3, molding: the molding is carried out by adopting an injection method, an aluminum alloy is used for manufacturing a molding die, and the die firing shrinkage scale is set to 15%. Placing the mould into a vacuum box, carrying out vacuum stirring treatment on the prepared slurry for at least 30 minutes under the vacuum degree of-90 Kpa, and injecting the slurry after the vacuum treatment into the mould through a discharge pipe at the bottom of a slurry barrel. And (3) placing the die subjected to injection molding into a drying oven at the temperature of 90 ℃ for curing for 2 hours, and removing and demolding to obtain the molded blank. The molded blank needs to be maintained for more than 8 hours under the condition of maintaining 65% relative humidity and can be naturally dried. After 24 hours of natural drying, forced drying may be performed.
S1-4, drying the green body: forced drying is performed using a forced air drying kiln. The heating rates of the two temperature sections of 80-110 ℃ and 150-180 ℃ are not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S1-5, sintering: sintering in a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating element.
S1-5-1, uniformly paving 8mm thick zirconia sand with granularity of 0.3mm on a kiln table, and then stably placing the ceramic blank on the zirconia sand in a field. When a plurality of kilns are installed, the interval distance between two adjacent kilns is required to be more than 30mm. The distance between the blank and the heating element is more than 30mm;
s1-5-2, setting the highest firing temperature at 1600 ℃, controlling the heating speed at 6 ℃/h, and keeping the temperature at the highest temperature for at least 6 hours;
s1-5-3, after the sintering is finished, naturally cooling, controlling the cooling speed to be not more than 15 ℃/h in the range of 1200-900 ℃, and discharging the kiln after the kiln temperature is reduced to be below 200 ℃.
S1-6, processing and grinding: cutting the end of the sintered blank by using a diamond cutter for the part exceeding the standard size, wherein the end face is kept perpendicular to the axis during cutting; the sintered blank meeting the requirement of the appearance size does not need to be processed.
The ceramic lining can be integrally formed into an integral lining, and can also be assembled into a combined lining after being molded and sintered in a segmented mode according to equipment conditions and individuation requirements based on lining performance.
S1-7, coating: to reduce the heat transfer of the ceramic liner to the refractory jacket, the outer surface of the ceramic liner is coated with a low expansion, low thermal conductivity coating to prevent cracking of the jacket by thermal shock from the ceramic liner.
S2, preparing a fireproof material jacket:
s2-1, proportioning: white corundum, crystalline flake graphite, fused quartz particles, calcined alumina micropowder and metal silicon powder are put into a batching machine and uniformly mixed;
s2-2, mixing and granulating: all the powder is put into a mixing granulator with a high-speed rotor to be mixed for 5 minutes, and the mixture is put into phenolic resin to be mixed and granulated for 15 minutes at high speed and then discharged.
S2-3, mud drying: after the mixture is trapped for 24 hours, the mixture is dried by a dryer, excess solvent is discharged, and the residual volatile is kept within the range of 0.8-1.4%.
S2-4, product molding: adopting a 20Gr quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: and (3) assembling a steel mould and a rubber soft mould, mounting a zirconium inner bushing on a steel core for fixing, weighing aluminum-carbon outer sleeve pug with proper weight, adding the aluminum-carbon outer sleeve pug into the mould, uniformly vibrating the soft mould for filling the pug, and sealing the mould. Putting the die into a high-pressure cylinder of an isostatic press, pressurizing to 200Mpa, maintaining for 8 minutes, releasing pressure, taking out and demolding. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S2-5, drying: forced drying is carried out by using a forced air drying kiln, the heating speed of two temperature sections of 80-110 ℃ and 150-180 ℃ is not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S2-6, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S2-7, processing: and (3) machining the outer surface of the product and grinding the surface of the sliding plate to ensure that the appearance size of the product meets the drawing requirement of a user.
S2-8, auxiliary processing: and carrying out auxiliary processing operations such as anti-oxidation coating, anti-sticking coating, graphite nozzle installation, graphite emulsion coating and the like on the processed product, and packaging.
Fifth embodiment:
referring to fig. 1, a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets comprises a zirconia ceramic inner liner and a refractory outer liner;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
35 parts of stabilized zirconia with 60-80% of stability, 55 parts of monoclinic phase zirconia and alpha-Al 2 O 3 8 parts of micropowder, 4 parts of silicon carbide micropowder, 3 parts of boron nitride micropowder, 1 part of magnesium oxide micropowder and 1 part of yttrium oxide micropowder.
The fireproof material jacket comprises the following raw materials in parts by weight:
60 parts of high-alumina homogenized material, 10 parts of crystalline flake graphite, 10 parts of fused quartz particles, 5 parts of calcined alumina micropowder, 1 part of metal silicon powder and 10 parts of phenolic resin.
The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets comprises the following steps:
s1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micropowder, the silicon carbide micropowder, the boron nitride micropowder, the magnesium oxide micropowder and the yttrium oxide micropowder into a homomixer according to parts by weight, and premixing for 20 minutes to obtain a premixed batch;
s1-2, grinding and pulping:
preparing grouting slurry, loading the premixed batch into a high-speed ball mill with a zirconia lining, adding 2.5 parts by weight of polyvinyl alcohol, 0.8 part by weight of dextrin or hydroxymethyl cellulose, 160 parts by weight of deionized water and 100 parts by weight of zirconia grinding balls with the diameter of 5mm, and grinding and stirring at a grinding speed of 300 revolutions per minute for 30 minutes to obtain slurry;
s1-3, molding: the grouting method is pressureless casting molding, and the volume density of the produced product is about 0.16-0.21 g/cm lower than that of the pressurizing vibration molding method, the mechanical pressing method and the isostatic pressing method 3 And air holes are easily formed in the molding process.
The casting method is adopted for molding, a gypsum mold is used for manufacturing a molding mold, and the setting of a mold firing shrinkage scale is 15%. Placing the mould into a vacuum box, carrying out vacuum stirring treatment on the prepared slurry for at least 30 minutes under the vacuum degree of-90 Kpa, and injecting the slurry after the vacuum treatment into the mould through a discharge pipe at the bottom of a slurry barrel. And (3) placing the die subjected to injection molding into a curing room with the temperature of 30 ℃ and the relative humidity of 70 percent for curing for 30 hours, and demolding to obtain the molded blank. The molded blank is maintained for 30 hours under the condition of maintaining 55% relative humidity, and is naturally dried. After naturally drying for 24 hours, forced drying was performed.
S1-4, drying the green body: forced drying is performed using a forced air drying kiln. The heating rates of the two temperature sections of 80-110 ℃ and 150-180 ℃ are not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S1-5, sintering: sintering in a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating element.
S1-5-1, uniformly paving 8mm thick zirconia sand with granularity of 0.3mm on a kiln table, and then stably placing the ceramic blank on the zirconia sand in a field. When a plurality of kilns are installed, the interval distance between two adjacent kilns is required to be more than 30mm. The distance between the blank and the heating element is more than 30mm;
S1-5-2, setting the highest firing temperature at 1600 ℃, controlling the heating speed at 6 ℃/h, and keeping the temperature at the highest temperature for at least 6 hours;
s1-5-3, after the sintering is finished, naturally cooling, controlling the cooling speed to be not more than 15 ℃/h in the range of 1200-900 ℃, and discharging the kiln after the kiln temperature is reduced to be below 200 ℃.
S1-6, processing and grinding: cutting the end of the sintered blank by using a diamond cutter for the part exceeding the standard size, wherein the end face is kept perpendicular to the axis during cutting; the sintered blank meeting the requirement of the appearance size does not need to be processed.
The ceramic lining can be integrally formed into an integral lining, and can also be assembled into a combined lining after being molded and sintered in a segmented mode according to equipment conditions and individuation requirements based on lining performance.
S1-7, coating: to reduce the heat transfer of the ceramic liner to the refractory jacket, the outer surface of the ceramic liner is coated with a low expansion, low thermal conductivity coating to prevent cracking of the jacket by thermal shock from the ceramic liner.
S2, preparing a fireproof material jacket:
s2-1, proportioning: placing 85% or more grade high-alumina homogenized material, crystalline flake graphite, fused quartz granule material, calcined alumina micropowder and metal silicon powder into a proportioning machine, and uniformly mixing;
S2-2, mixing and granulating: all the powder is put into a mixing granulator with a high-speed rotor to be mixed for 5 minutes, and the mixture is put into phenolic resin to be mixed and granulated for 20 minutes at high speed and then discharged.
S2-3, mud drying: after the mixture is trapped for 24 hours, the mixture is dried by a dryer, excess solvent is discharged, and the residual volatile is kept within the range of 0.8-1.4%.
S2-4, product molding: adopting a 20Gr quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: and (3) assembling a steel mould and a rubber soft mould, mounting a zirconium inner bushing on a steel core for fixing, weighing aluminum-carbon outer sleeve pug with proper weight, adding the aluminum-carbon outer sleeve pug into the mould, uniformly vibrating the soft mould for filling the pug, and sealing the mould. Putting the die into a high-pressure cylinder of an isostatic press, pressurizing to 200Mpa, maintaining for 8 minutes, releasing pressure, taking out and demolding. The demolded blank is naturally dried for 24 hours and then can be forced dried.
S2-5, drying: forced drying is carried out by using a forced air drying kiln, the heating speed of two temperature sections of 80-110 ℃ and 150-180 ℃ is not higher than 3 ℃/h, the highest drying temperature is set to 260 ℃, the high-temperature heat preservation time is not less than 4 hours, and the total drying time is controlled to 45 hours. The water content of the dried blank is less than 0.1%.
S2-6, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S2-7, processing: and (3) machining the outer surface of the product and grinding the surface of the sliding plate to ensure that the appearance size of the product meets the drawing requirement of a user.
S2-8, auxiliary processing: and carrying out auxiliary processing operations such as anti-oxidation coating, anti-sticking coating, graphite nozzle installation, graphite emulsion coating and the like on the processed product, and packaging.
Comparative example one:
s1, production of a zirconium bowl and a zirconium core:
s1-1, proportioning: 20 parts by weight of industrial zirconia, 40 parts by weight of stabilized zirconia and 10 parts by weight of zircon sand, adopting 4-grade ingredients, wherein the granularity size of the main raw materials is generally 100#; the monoclinic zirconium stabilizer/sintering aid was yttrium oxide and magnesium oxide in total 2 parts by weight and the binder was polyvinyl alcohol in 5 parts by weight.
S1-2, pug mixing: mixing materials by using a wheel mill type mixer with a stirring function.
S1-3, molding: and (3) using a quenching steel die, and performing double-sided compression molding by using a 150-ton oil press.
S1-4, sintering: the high temperature firing was performed at 1680 c using a trolley (or pusher kiln) tunnel kiln heated with silicon molybdenum rods (or heated with natural gas).
S2, production of the jacket:
s2-1, proportioning: 60 parts by weight of 80-88% grade high bauxite of 200# is used as a main raw material, 10 parts by weight of Suzhou soil is used as a high-temperature bonding agent, and 3 parts by weight of aluminum phosphate is used as a medium-low-temperature bonding agent;
s2-2, mixing: using a large grinding wheel mixer with a stirring function to mix pugs;
s2-3, molding: carrying out double-sided compression molding by using a quenching steel die and a friction press of 300 tons;
s2-4, sintering: the material is sintered or not sintered at 1300 ℃.
S3, product assembly: and (3) cementing the zirconium bowl and the multisection zirconium core together in series by using a special tool, and then cementing the corundum fireclay for the zirconium lining and the high-aluminum jacket together. And (3) loading the assembled zirconium composite nozzle into a drying kiln, and drying at 180 ℃. And checking and packaging the products after the products are discharged from the kiln.
Comparative example two:
s1, proportioning: the method comprises the following steps of uniformly mixing 30 parts by weight of fused corundum, 10 parts by weight of crystalline flake graphite, 20 parts by weight of magnesia alumina spinel, 5 parts by weight of sintered alumina micropowder, 10 parts by weight of metallic silicon, 2 parts by weight of silicon carbide, 5 parts by weight of fused quartz, 3 parts by weight of boron carbide and 10 parts by weight of phenolic resin through a premixing machine.
S2, mixing and granulating: the mixing granulation is carried out by using a roller-free high-speed mixing granulator with a high-speed stirring function, so that the batch materials with various granularities and different specific gravities can be uniformly mixed. The mixed and granulated pug can be used for forming after the indexes of residual volatile matters, granularity composition, green compact density and the like meet the standard requirements after being dried and trapped.
S3, forming: the quenching steel mould and the rubber soft mould are adopted as forming moulds, and an isostatic press is used for forming. The physical indexes of the molded blank, such as the volume density, the porosity and the like of any part of the same material are uniform.
S4, drying green bricks: and (3) according to a set heating curve, solidifying and drying the molded blank at the temperature of 250 ℃ at the maximum.
S5, sintering: and (3) sintering at the highest 1040 ℃ according to a set temperature rising curve under the reducing atmosphere to form the carbon network combination.
S6, processing: and (3) machining the outer surface of the product to ensure that the appearance size of the product meets the requirement of a user drawing.
The performance indexes of the zirconia ceramic lining in the first to fifth examples, the zirconia lining in the first comparative example and the aluminum-carbon composite tundish nozzle in the second comparative example were tested, and the service lives of the products in the first to fifth examples and the first to second comparative examples were tested, and the test results are as follows:
Examples Flexural Strength at Normal temperature/MPa Flexural Strength at 1450 ℃ per MPa Coefficient of thermal expansion/×10 -6 *1/℃ Fracture toughness/Mpa M 1/2 Thermal shock stability (700 ℃ air-cooled non-crack)/secondary Service life/h
Example 1 205 57 7.2 4.2 47 69
Example two 218 62 7.1 4.2 49 70
Example III 220 60 6.8 4.3 53 68
Example IV 209 61 6.9 4.1 51 72
Example five 214 54 7.0 4.4 47 71
Comparative example one 80 / 7.3 3.2 32 32
Comparative example two 15 / 18.2 1.2 12 19
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (9)

1. The toughened zirconia ceramic tundish nozzle for continuous casting of slabs, bloom and rectangular billets is characterized by comprising a zirconia ceramic inner liner and a refractory material outer sleeve;
the zirconia ceramic lining comprises the following raw materials in parts by weight:
10 to 60 parts of stabilized zirconia, 35 to 90 parts of monoclinic phase zirconia and alpha-Al 2 O 3 2 to 17 parts of micro powder, 1 to 11 parts of silicon carbide micro powder, 1 to 3 parts of boron nitride micro powder, 1 to 6 parts of magnesium oxide micro powder and 1 to 2 parts of yttrium oxide micro powder;
the fireproof material jacket comprises the following raw materials in parts by weight:
45-80 parts of brown alumina, white corundum, high-alumina homogenized material or high-alumina bauxite, 8-25 parts of crystalline flake graphite, 5-25 parts of fused Dan Yingke granules, 3-15 parts of calcined alumina micropowder, 0.5-4 parts of metal silicon powder and 8-12 parts of phenolic resin.
2. The toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets as claimed in claim 1, wherein the stabilized zirconia in the zirconia ceramic lining raw material has a stability of 60 to 80%.
3. The toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets as claimed in claim 1, wherein the grade of brown alumina, white alumina, high alumina homogenized material or high alumina bauxite in the refractory material outer jacket raw material is 85% or more.
4. The production process of the toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets is characterized by comprising the following steps of:
s1, preparation of a zirconia ceramic lining:
s1-1, mixing and premixing: stabilized zirconia, monoclinic phase zirconia, alpha-Al 2 O 3 Adding the micro powder, the silicon carbide micro powder, the boron nitride micro powder, the magnesium oxide micro powder and the yttrium oxide micro powder into a homomixer for premixing according to parts by weight to obtain a premixed batch;
s1-2, grinding and pulping: filling the premixed batch into a high-speed ball mill with a zirconia lining, adding deionized water, and grinding to obtain slurry;
s1-3, molding: the molding mode is one of injection molding, grouting molding, pressurizing vibration molding, mechanical pressing molding and isostatic pressing molding;
S1-4, drying the green body: forced drying by using a forced air drying kiln, wherein the water content of the dried blank is less than 0.1%;
s1-5, sintering: sintering by using a high-temperature box furnace or a tunnel type high-temperature kiln with a high-temperature silicon molybdenum rod as a heating body, wherein the highest sintering temperature is 1520-1760 ℃, the heating speed is 4-8 ℃/h, and the heat preservation time at the highest temperature is not less than 6 hours;
s1-6, processing and grinding and coating surface paint;
s2, preparing a fireproof material jacket:
s2-1, proportioning: placing brown corundum, white corundum, high-alumina homogenized material or high-alumina bauxite, crystalline flake graphite, fused quartz granule material, calcined alumina micropowder and metal silicon powder into a batching machine according to weight parts, and uniformly mixing;
s2-2, mixing and granulating: putting all the matched powder materials into a mixing granulator with a high-speed rotor, carrying out dry mixing for 3-7 minutes, putting phenolic resin into the mixing granulator, carrying out high-speed mixing granulation for 8-30 minutes, and discharging;
s2-3, mud drying: mixing the materials, trapping the materials for 24 hours, drying, and discharging redundant solvent;
s2-4, product molding: adopting a 20Gr or 45# quenched steel inner die, a hard rubber or high-elasticity polyurethane outer die, and forming by using an isostatic press: assembling the inner die and the outer die, filling and sealing the die, loading the die into a high-pressure cylinder of an isostatic press for pressurization treatment, and taking out for demolding;
S2-5, drying: forced drying is carried out by using a forced air drying kiln, and the water content of the dried blank is less than 0.1 percent;
s2-6, sintering: firing at a temperature of up to 1040 ℃ in a reducing atmosphere to form a carbon network bond;
s2-7, processing.
5. The process for producing a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets according to claim 4, wherein when the zirconia ceramic lining is formed by a grouting method, in the step S1-2, the premixed batch is put into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and grinding and stirring are carried out for 30 minutes at a grinding speed of 200-400 rpm, so as to obtain slurry;
the casting method is used for forming, a gypsum mold is used for manufacturing a forming mold, slurry is processed in vacuum, the slurry is injected into the mold, the mold after injection molding is put into a curing room with the temperature of 20-35 ℃ and the relative humidity of 65-85% for curing for 24-36 hours, and the molded blank is obtained after demolding.
6. The process for producing a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets according to claim 4, wherein when the zirconia ceramic lining is molded by a pressurized vibration molding method, in the step S1-2, the premixed batch is put into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and grinding and stirring are carried out for 30 minutes at a grinding speed of 200-400 rpm, so as to obtain slurry;
Spray granulation and drying steps are added between the step S1-2 and the step S1-3: loading the slurry into a storage tank of a spray granulator, carrying out spray drying granulation at the air temperature of 150-300 ℃ to obtain a granulation material with the granularity of 0.01-1.5 mm, keeping the granulation material in a sealed state with the water content of 0.3-1.1%, and trapping the granulation material for 24-36 hours at the temperature of 30+/-2 ℃;
and (3) forming by a pressurizing vibration forming method, namely adding the pelleting material into a quenching steel die to smooth the material surface, pressurizing for multiple times according to the principle of light before heavy middle exhaust, and discharging the die after pressurizing when the upper pressure head reaches the limit.
7. The process for producing a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets according to claim 4, wherein when the zirconia ceramic lining is formed by an isostatic compaction method, in the step S1-2, the premixed batch is put into a high-speed ball mill of the zirconia lining, 0.4-6 parts by weight of polyvinyl alcohol, 0.2-3 parts by weight of dextrin or hydroxymethyl cellulose, 40-200 parts by weight of deionized water and 30-200 parts by weight of zirconia grinding balls with the diameter of 1-10 mm are added, and grinding and stirring are carried out for 30 minutes at a grinding speed of 200-400 rpm, so as to obtain slurry;
Spray granulation and drying steps are added between the step S1-2 and the step S1-3: loading the slurry into a storage tank of a spray granulator, carrying out spray drying granulation at the air temperature of 150-300 ℃ to obtain a granulation material with the granularity of 0.01-1.5 mm, keeping the granulation material in a sealed state with the water content of 0.3-1.1%, and trapping the granulation material for 24-36 hours at the temperature of 30+/-2 ℃;
the isostatic compaction method is to use a combined die with an inner core of a quenching steel die and an outer die of hard rubber or high-elasticity polyurethane, to inject pelleting materials into the die, to vibrate for 5-20 seconds by using a high-frequency vertical vibration type vibrating table, to supplement pelleting materials in the die, to seal the die, to put the die into a high-pressure cylinder of an isostatic press to be pressurized to 90-250 Mpa for 3-12 minutes, to release pressure, and to take out and to demould.
8. The process for producing a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, billets and rectangular billets according to claim 4, wherein when the zirconia ceramic lining is formed by adopting a casting method, the premixed batch is put into a high-speed ball mill of the zirconia lining, 50 to 80 parts by weight of acrylamide monomer, 10 to 20 parts by weight of methylene bisacrylamide cross-linking agent, 5 to 10 parts by weight of JA281 dispersing agent and 40 to 200 parts by weight of deionized water are respectively added, and the mixture is ground and stirred for 20 to 40 minutes at a grinding speed of 200 to 400 revolutions per minute, and then ammonium persulfate initiator is added and stirred to prepare slurry;
The casting method is to manufacture a forming die by using aluminum alloy, vacuum treat slurry, inject the slurry into the die, put the die after injection molding into a drying oven with the temperature of 80-100 ℃ for curing for 2 hours, and remove and demould the die to obtain a formed blank.
9. The process for producing a toughened zirconia ceramic tundish nozzle for continuous casting of slabs, blooms and rectangular billets according to claim 4, wherein in step S2-4, the pressure of the isostatic press is 90-250 Mpa and the holding time is 3-12 minutes.
CN202310081537.4A 2023-02-08 2023-02-08 Toughened zirconia ceramic tundish nozzle for continuous casting of slabs, large square billets and rectangular billets and production process thereof Pending CN116199509A (en)

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