CN111039694A - Preparation method of zirconia-based foamed ceramic filter - Google Patents
Preparation method of zirconia-based foamed ceramic filter Download PDFInfo
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Abstract
The invention relates to the field of refractory materials and molten metal purification, in particular to a preparation method of a zirconia-based foamed ceramic filter for high-temperature molten liquid filtration and purification, which comprises the following steps: uniformly mixing zirconium oxide, magnesium oxide and cerium oxide, and putting into an electric arc furnace for melting to obtain fused zirconium oxide; mixing the ground fused zirconia with tungsten carbide to obtain zirconia-based composite ceramic powder; mixing zirconia-based composite ceramic powder and a binder to obtain zirconia-based composite slurry; soaking and absorbing the zirconium oxide-based composite slurry by using plastic foam according to a foamed ceramic forming process to prepare a blank; and roasting the formed blank, and cooling the sintered blank along with the furnace to obtain the zirconia-based composite ceramic filter. Different from the prior art, the preparation method of the zirconia-based foamed ceramic filter provided by the invention has the advantages that the mechanical strength, the high-temperature scouring erosion resistance and the thermal shock resistance of a filter product are better improved by controlling the formula and the manufacturing process.
Description
Technical Field
The invention relates to the field of refractory materials and molten metal purification, in particular to a preparation method of a zirconia-based foamed ceramic filter for high-temperature molten liquid filtration and purification.
Background
With the vigorous development of smelting and casting industries, the metal melt filtering process is adopted to rectify and remove impurities from molten metal, so that the metal melt filtering process is popularized in the casting industries of smelting at home and abroad. The core component for filtering the high-temperature metal melt is the filter, and in recent years, the foamed ceramic filter becomes the mainstream of metal melt filtration and is widely popularized and applied in the smelting and casting industry. Because of the high melting temperature of cast steel, the filters currently used for cast steel are essentially all ceramic foam filters, at which temperatures the filters need to maintain adequate mechanical strength, thermal shock resistance, and low specific heat capacity. Generally, the smaller the thermal expansion coefficient of the material itself, the larger the thermal conductivity, and the higher the strength, the smaller the change in stress of the material due to a change in temperature, and the more excellent the corresponding thermal shock resistance, erosion resistance, and ability to withstand thermal stress without breaking.
In recent years, a plurality of foam filters made of different ceramic materials have been developed at home and abroad according to different alloy characteristics, but due to the difference between production formulas and processes of different manufacturers, the existing ceramic filters in the market have different quality, and most of the existing ceramic filters have the defects of insufficient mechanical strength, poor high-temperature scouring resistance and thermal shock resistance, short life cycle of the filter and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a zirconium oxide-based foamed ceramic filter with good high-temperature strength, good thermal shock resistance and scouring resistance.
In order to solve the technical problems, the invention adopts the technical scheme that: the preparation method of the zirconia-based ceramic foam filter comprises the following steps:
uniformly mixing zirconium oxide, magnesium oxide and cerium oxide according to a certain ratio, putting the mixture into an electric arc furnace for melting, and naturally cooling the melted solution to obtain the fused zirconium oxide, wherein the weight ratio of the zirconium oxide to the magnesium oxide to the cerium oxide is 100: 2.55-2.95: 0.55-0.95;
grinding the fused zirconia, and mixing the ground fused zirconia with tungsten carbide to obtain zirconia-based composite ceramic powder, wherein the weight ratio of the fused zirconia to the tungsten carbide is 100: 0.08-0.35;
uniformly mixing zirconia-based composite ceramic powder and a binder, adding 1-2 drops of a defoaming agent, and mechanically and forcibly stirring and modulating to obtain zirconia-based composite slurry, wherein the weight ratio of the zirconia-based composite ceramic powder to the binder is 100: (3-8);
soaking and absorbing the zirconium oxide-based composite slurry by using plastic foam according to a foamed ceramic forming process, and extruding to prepare a blank;
and (3) drying the formed blank body in a constant temperature environment, then placing the dried blank body in an argon furnace for roasting, and cooling the roasted blank body along with the furnace to obtain the zirconia-based composite ceramic filter.
Preferably, in the above method for preparing a zirconia-based ceramic foam filter, the binder is an aqueous solution prepared from dextrin and an additive, the additive is one or a mixture of polyvinyl alcohol and/or polypropylene alcohol, and the water: additive: the weight ratio of dextrin is: 100:(5-11): (0.5-1.2).
Preferably, in the above method for manufacturing a zirconia-based ceramic foam filter, the steps of: the step of naturally cooling the melted solution to obtain the fused zirconia specifically comprises the following steps: pouring the molten liquid into a heat preservation furnace for natural cooling, wherein the cooling time is more than or equal to 36 hours.
Preferably, in the above method for preparing a zirconia-based ceramic foam filter, in the step of "grinding the fused zirconia", the fused zirconia is ground until the mass ratio of the powder with the particle size of 12000 meshes is 10-20%, the mass ratio of the powder with the particle size of 8000 meshes-12000 meshes is 25-35%, the mass ratio of the powder with the particle size of 4500 meshes-8000 meshes is 25-35%, the mass ratio of the powder with the particle size of 1500 meshes-4500 meshes is 20-30%, and the mass ratio of the powder with the particle size of 1500 meshes is less than or equal to 3%.
Preferably, in the above method for preparing a zirconia-based ceramic foam filter, the tungsten carbide has a particle size of 4500 mesh or less.
Preferably, in the above method for preparing a zirconia-based ceramic foam filter, the mechanically-forced stirring time is not less than 45min in the step of mechanically-forced stirring and preparing to obtain the zirconia-based composite slurry.
Preferentially, in the above method for preparing a zirconia-based ceramic foam filter, the step of "drying the formed blank in a constant temperature environment" is specifically: and (3) placing the molded blank body in a constant temperature environment with the heat preservation temperature of 70-110 ℃, and drying for more than or equal to 8 hours.
Preferably, in the above method for preparing a zirconia-based ceramic foam filter, the step "then placing in an argon furnace for calcination" includes: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, furnace cooling to 25-30 ℃.
Preferentially, in the preparation method of the zirconia-based foamed ceramic filter, the purity of the zirconia is more than or equal to 99%, the purity of the magnesia is more than or equal to 99.8%, the purity of the cerium oxide is more than or equal to 99.8%, and the purity of the tungsten carbide is more than or equal to 99.8%.
The invention has the beneficial effects that: different from the prior art, the preparation method of the zirconia-based foamed ceramic filter provided by the invention has the advantages that the mechanical strength, the high-temperature scouring erosion resistance and the thermal shock resistance of a filter product are better improved by controlling the formula and the manufacturing process. Compared with the existing filter products in the market, the high-temperature heat shock resistance and corrosion resistance of the high-temperature heat shock resistance and corrosion resistance filter has excellent high-temperature heat shock resistance and corrosion resistance, and when the high-temperature heat shock resistance filter is applied to cast steel filtration, the service cycle of the high-temperature heat shock resistance filter is 1.03-1.2 times that of the existing products. The zirconia-based foamed ceramic filter prepared by the preparation method solves the problems of poor high-temperature scouring resistance, short service cycle and the like of the existing ceramic filter, and brings new progress to the field of refractory materials for high-temperature filtration.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is that the preparation of the electric melting zirconia composite powder is realized through a smelting process, the physical strength, high temperature scouring resistance and thermal shock resistance of zirconia are enhanced and stabilized through a component proportion and a cooling process, the control of the particle size of the powder, the reasonable grading of the particle size and the introduction of trace tungsten carbide powder are realized through a grinding process, the effective strengthening and the improvement of the comprehensive performance of the zirconia-based foamed ceramic filter are realized again, and the excellent performance and the quality stability of the product in the sintering and molding process are ensured through reasonable drying and roasting temperature rise and fall curves.
The invention provides a preparation method of a zirconia-based foamed ceramic filter, which comprises the following steps:
uniformly mixing zirconium oxide, magnesium oxide and cerium oxide according to a certain ratio, putting the mixture into an electric arc furnace for melting, and naturally cooling the melted solution to obtain the fused zirconium oxide, wherein the weight ratio of the zirconium oxide to the magnesium oxide to the cerium oxide is 100: 2.55-2.95: 0.55-0.95;
grinding the fused zirconia, and mixing the ground fused zirconia with tungsten carbide to obtain zirconia-based composite ceramic powder, wherein the weight ratio of the fused zirconia to the tungsten carbide is 100: 0.08-0.35;
uniformly mixing zirconia-based composite ceramic powder and a binder, adding 1-2 drops of a defoaming agent, and mechanically and forcibly stirring and modulating to obtain zirconia-based composite slurry, wherein the weight ratio of the zirconia-based composite ceramic powder to the binder is 100: (3-8);
soaking and absorbing the zirconium oxide-based composite slurry by using plastic foam according to a foamed ceramic forming process, and extruding to prepare a blank;
and (3) drying the formed blank body in a constant temperature environment, then placing the dried blank body in an argon furnace for roasting, and cooling the roasted blank body along with the furnace to obtain the zirconia-based composite ceramic filter.
Specifically, the preparation method of the zirconia ceramic filter specifically comprises the following steps:
1. mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: uniformly mixing 100 parts of cerium oxide to 2.55-2.95 parts of cerium oxide to 0.55-0.95 parts of cerium oxide, and putting the mixture into an electric arc furnace for melting;
2. quickly pouring the molten zirconium oxide into a heat preservation furnace for natural cooling for more than or equal to 36 hours, and naturally growing zirconium oxide crystals to eliminate metastable crystal forms;
3. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 10-20%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 25-35%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 25-35%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 20-30%, and the mass ratio of the powder under the particle size of 1500 meshes is less than or equal to 3%;
4. uniformly mixing the ground zirconium oxide powder and tungsten carbide according to the weight ratio of 100: 0.08-0.35 to obtain zirconium oxide-based composite ceramic powder, wherein the granularity of the tungsten carbide is less than or equal to 4500 meshes;
5. the binder is aqueous solution prepared from dextrin and polyvinyl alcohol (or polyvinyl alcohol or mixture of the dextrin and the polyvinyl alcohol), and the water is prepared according to the mass ratio: polyvinyl alcohol (polyvinyl alcohol): dextrin is 100 (5-11): (0.5-1.2) preparing;
6. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100: (3-8), adding 1-2 drops of defoaming agent, and mechanically stirring for more than or equal to 45min to prepare slurry;
7. soaking and absorbing the zirconium oxide-based composite slurry by using plastic foam according to a foamed ceramic forming process, and extruding to prepare a blank;
8. and (3) placing the formed blank body in a constant temperature environment of 70-110 ℃ to dry for more than or equal to 8 hours, and then placing the blank body in an argon furnace to roast. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
In the preparation method, the volume effect of the zirconia material is eliminated and the crystal grains grow slowly through the component formula and the cooling process in the steps 1 and 2, so that the mechanical strength and the high-temperature mechanical property are improved and stabilized; step 3, realizing the control of the particle size of the powder and the reasonable grading of the particle size through a grinding process, and increasing the surface area of the powder to excite the surface energy of the powder; step 4, by adding trace tungsten carbide powder, the high-temperature scouring and corrosion resistance of the filter is obviously improved, and the comprehensive performance of the zirconia-based foamed ceramic filter is effectively enhanced and improved again; and 8, sintering the powder into the zirconia-based foamed ceramic filter with good mechanical strength and excellent high-temperature thermal shock resistance and scouring resistance by a reasonable sintering technology.
From the above description, the beneficial effects of the present invention are: compared with the prior art, the zirconia-based foamed ceramic filter prepared by the method disclosed by the invention has the advantages that the mechanical strength, the high-temperature scouring erosion resistance and the thermal shock resistance of a filter product are better improved. Compared with the existing products in the market, the high-temperature heat shock resistant and corrosion resistant filter has excellent high-temperature heat shock resistance and corrosion resistance, and when the high-temperature heat shock resistant and corrosion resistant filter is applied to cast steel filtration, the service cycle of the filter is 1.03-1.15 times that of the existing products. The method can solve the problems of poor high-temperature scouring resistance, short service cycle and the like of the existing ceramic filter, and brings new progress to the field of refractory materials for high-temperature filtration.
Furthermore, the purity of the raw material zirconium oxide is more than or equal to 99%, the purity of the magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Example 1:
1. mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: the cerium oxide is mixed evenly in a ratio of 100: 2.58: 0.85 and is put into an electric arc furnace for melting. Quickly pouring the molten zirconium oxide into a heat preservation furnace to naturally cool for 40 hours;
2. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 16.5%, the mass ratio of the powder between 8000 meshes and 12000 meshes is 27.5%, the mass ratio of the powder between 4500 meshes and 8000 meshes is 31%, the mass ratio of the powder between 1500 meshes and 4500 meshes is 23.7%, and the mass ratio of the powder above 1500 meshes is 1.3%;
3. uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.11 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 6: preparing at a ratio of 0.8;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100:5, adding 1 drop of defoaming agent, mechanically and forcibly stirring for 75min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 10.0h at the constant temperature of 105 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Through the continuous hot scouring detection of high-temperature molten steel, the service life cycle of the prepared zirconia-based foamed ceramic filter is 1.1 times that of the existing zirconia-based foamed ceramic filter in the market. The material shows better high-temperature thermal shock resistance and scouring resistance.
The existing zirconia-based foamed ceramic filter in the market is mainly formed by taking zirconia as a matrix and adding one or more of magnesia, alumina, calcium oxide, silicon carbide and the like in a certain proportion into a formula, pressing and molding the mixture and then sintering the mixture, and the formula and the sintering process of each family are different but have almost the same performance.
Example 2
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: the cerium oxide was mixed uniformly at a ratio of 100: 2.81: 0.62, and charged into an arc furnace to be melted. Quickly pouring the molten zirconium oxide into a holding furnace for natural cooling for 37 hours;
2. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 18%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 30%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 29.5%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 21.5%, and the mass ratio of the powder under the particle size of 1500 meshes is 1.0%;
3. uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.09 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 8: preparing at a ratio of 0.6;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100: 4.5, adding 2 drops of defoaming agent, mechanically and forcibly stirring for 60min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 12.0h in a constant temperature environment of 90 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Through the continuous hot scouring detection of high-temperature molten steel, the service life cycle of the prepared zirconia-based foamed ceramic filter is 1.05 times that of the conventional filter, and the prepared zirconia-based foamed ceramic filter has better high-temperature thermal shock resistance and scouring resistance.
Example 3
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: the cerium oxide is mixed evenly in a ratio of 100: 2.75: 0.91, and is put into an electric arc furnace for melting. Quickly pouring the molten zirconium oxide into a heat preservation furnace for natural cooling for 55 hours;
2. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 15%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 33%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 27%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 23%, and the mass ratio of the powder under the particle size of 1500 meshes is 2.0%;
3. uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.28 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 6.5: 1.07 preparing;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100: 7, adding 2 drops of defoaming agent, mechanically and forcibly stirring for 90min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 10.0h in a constant temperature environment of 100 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Through the continuous hot scouring detection of high-temperature molten steel, the service life cycle of the prepared zirconia-based foamed ceramic filter is 1.13 times that of the conventional filter, and the prepared zirconia-based foamed ceramic filter shows better high-temperature thermal shock resistance and scouring resistance.
Example 4
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: cerium oxide is 100: 2.55: 0.55; mixing uniformly, and melting in an electric arc furnace. And quickly pouring the molten zirconium oxide into a holding furnace for natural cooling for 36 hours.
2. Grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 10%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 25%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 32%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 30%, and the mass ratio of the powder under the particle size of 1500 meshes is 3%.
3. Uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of 4500 meshes according to the weight ratio of 100: 0.08 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 5: preparing at a ratio of 0.5;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100: 3, adding 1 drop of defoaming agent, mechanically and forcibly stirring for 75min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 8 hours at the constant temperature of 70 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-1350 ℃: 300min, 1350-1350 ℃: 70min, 1350-1730 ℃: 150min, 1730-1730 ℃: 200 min; the cooling curve is: 1730-1350 ℃: 200min, 1350-1350 ℃: 30min, 1350-600 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Through the continuous hot scouring detection of high-temperature molten steel, the service life cycle of the prepared zirconia-based foamed ceramic filter is 1.12 times that of the conventional filter, and the prepared zirconia-based foamed ceramic filter shows better high-temperature thermal shock resistance and scouring resistance.
Example 5
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: cerium oxide is 100: 2.95: 0.95; mixing uniformly, and melting in an electric arc furnace. Quickly pouring the molten zirconium oxide into a heat preservation furnace to naturally cool for 40 hours; the cooling time was 36 hours.
2. The fused zirconia is ground until the mass ratio of the powder under the particle size of 12000 meshes is 20%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 33%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 25%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 20%, and the mass ratio of the powder under the particle size of 1500 meshes is 2%.
3. Uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.35 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 11: 1.2, preparing in proportion;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100:8, adding 1 drop of defoaming agent, mechanically and forcibly stirring for 45min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 10.0h in a constant temperature environment of 110 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-1350 ℃: 300min, 1350-1350 ℃: 70min, 1350-1730 ℃: 150min, 1730-1730 ℃: 200 min; the cooling curve is: 1730-1350 ℃: 200min, 1350-1350 ℃: 30min, 1350-600 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
Through the continuous hot scouring detection of high-temperature molten steel, the service life cycle of the prepared zirconia-based foamed ceramic filter is 1.13 times that of the conventional filter, and the prepared zirconia-based foamed ceramic filter shows better high-temperature thermal shock resistance and scouring resistance.
Comparative example 1
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: the cerium oxide is mixed evenly in a ratio of 100: 2.15: 0.45, and is put into an electric arc furnace for melting. Quickly pouring the molten zirconium oxide into a heat preservation furnace to naturally cool for 45 hours;
2. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 15%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 29%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 31%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 23%, and the mass ratio of the powder under the particle size of 1500 meshes is 2.0%;
3. uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.09 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 6: 1.0 proportion;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100:6, adding 1 drop of defoaming agent, mechanically and forcibly stirring for 75min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 10.0h at the constant temperature of 105 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
The life cycle of the prepared zirconia-based foamed ceramic filter is 0.94 times that of the existing filter through high-temperature molten steel hot flushing detection, and the high-temperature thermal shock resistance and flushing resistance performances are general due to the lack of magnesium oxide and cerium oxide serving as stabilizing agents.
Comparative example 2
1. Mixing zirconium oxide, magnesium oxide and cerium oxide according to the weight ratio of zirconium oxide: magnesium oxide: the cerium oxide is mixed evenly in a ratio of 100: 2.75: 0.83, and is put into an electric arc furnace for melting. Quickly pouring the molten zirconium oxide into a heat preservation furnace to naturally cool for 45 hours;
2. grinding the fused zirconia until the mass ratio of the powder under the particle size of 12000 meshes is 17%, the mass ratio of the powder under the particle size of 8000 meshes-12000 meshes is 28%, the mass ratio of the powder under the particle size of 4500 meshes-8000 meshes is 30%, the mass ratio of the powder under the particle size of 1500 meshes-4500 meshes is 24.5%, and the mass ratio of the powder under the particle size of 1500 meshes is 0.5%;
3. uniformly mixing the ground zirconia powder with tungsten carbide with the granularity of less than or equal to 4500 meshes according to the weight ratio of 100: 0.03 to obtain zirconia-based composite ceramic powder;
4. preparing an aqueous solution by using dextrin and polyvinyl alcohol, and mixing the following water in percentage by mass: polyvinyl alcohol: dextrin is 100: 6: 1.0 proportion;
5. mixing zirconia-based composite ceramic powder and a binder according to the mass ratio of 100:6.5, adding 1 drop of defoaming agent, mechanically and forcibly stirring for 75min to prepare slurry, soaking and absorbing the zirconia-based composite slurry by using plastic foam, and extruding to prepare a blank;
6. and (3) drying the formed blank body for 10.0h at the constant temperature of 105 ℃, and then placing the blank body in an argon furnace for roasting. The sintering temperature rise curve is as follows: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, and then cooling to normal temperature along with the furnace.
The purity of the selected raw materials, namely zirconium oxide is more than or equal to 99%, the purity of magnesium oxide is more than or equal to 99.8%, the purity of cerium oxide powder is more than or equal to 99.8%, and the purity of tungsten carbide powder is more than or equal to 99.8%.
The life cycle of the prepared zirconia-based foamed ceramic filter is 0.98 times that of the existing filter through high-temperature molten steel hot flushing detection, and the high-temperature thermal shock resistance and flushing resistance of the filter are general due to the fact that the tungsten carbide is not added.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (9)
1. The preparation method of the zirconia-based ceramic foam filter is characterized by comprising the following steps of:
uniformly mixing zirconium oxide, magnesium oxide and cerium oxide, putting the mixture into an electric arc furnace for melting, and naturally cooling the melted solution to obtain the fused zirconium oxide, wherein the weight ratio of the zirconium oxide to the magnesium oxide to the cerium oxide is 100: 2.55-2.95: 0.55-0.95;
grinding the fused zirconia, and mixing the ground fused zirconia with tungsten carbide to obtain zirconia-based composite ceramic powder, wherein the weight ratio of the fused zirconia to the tungsten carbide is 100: 0.08-0.35;
uniformly mixing zirconia-based composite ceramic powder and a binder, adding 1-2 drops of a defoaming agent, and mechanically and forcibly stirring and modulating to obtain zirconia-based composite slurry, wherein the weight ratio of the zirconia-based composite ceramic powder to the binder is 100: (3-8);
soaking and absorbing the zirconium oxide-based composite slurry by using plastic foam according to a foamed ceramic forming process, and extruding to prepare a blank;
and (3) drying the formed blank body in a constant temperature environment, then placing the dried blank body in an argon furnace for roasting, and cooling the roasted blank body along with the furnace to obtain the zirconia-based composite ceramic filter.
2. The method of claim 1, wherein the binder is an aqueous solution prepared from dextrin and an additive, the additive is one or a mixture of polyvinyl alcohol and/or polyallyl alcohol, and the ratio of water: additive: the weight ratio of dextrin is: 100:(5-11): (0.5-1.2).
3. The method of manufacturing a zirconia-based ceramic foam filter according to claim 1, wherein the steps of: the step of naturally cooling the melted solution to obtain the fused zirconia specifically comprises the following steps: pouring the molten liquid into a heat preservation furnace for natural cooling, wherein the cooling time is more than or equal to 36 hours.
4. The method for preparing a zirconia-based ceramic foam filter according to claim 1, wherein in the step of grinding the fused zirconia, the fused zirconia is ground until the mass ratio of powder with a particle size of 12000 meshes is 10-20%, the mass ratio of powder with a particle size of 8000-12000 meshes is 25-35%, the mass ratio of powder with a particle size of 4500-8000 meshes is 25-35%, the mass ratio of powder with a particle size of 1500-4500 meshes is 20-30%, and the mass ratio of powder with a particle size of 1500 meshes is less than or equal to 3%.
5. The method of claim 1, wherein the tungsten carbide has a particle size of 4500 mesh or less.
6. The method for preparing a zirconia-based ceramic foam filter according to claim 1, wherein the mechanically forced stirring time of the zirconia-based composite slurry obtained by the mechanically forced stirring preparation is not less than 45 min.
7. The method for preparing a zirconia-based ceramic foam filter according to claim 1, wherein the step of "drying the molded blank in a constant temperature environment" is specifically: and (3) placing the molded blank body in a constant temperature environment with the heat preservation temperature of 70-110 ℃, and drying for more than or equal to 8 hours.
8. The method of claim 1, wherein the step "firing the zirconia-based ceramic foam filter in an argon furnace" comprises a temperature rise curve of: 0-600 ℃: 270min, 600-600 ℃: 150min, 600-: 300min, 1350 ℃: 70min, 1350-: 150min, 1730 ℃: 200 min; the cooling curve is: 1730-: 200min, 1350 ℃: 30min, 1350 ℃: 300min, furnace cooling to 25-30 ℃.
9. The method for preparing a zirconia-based ceramic foam filter according to claim 1, wherein the purity of zirconia is not less than 99%, the purity of magnesia is not less than 99.8%, the purity of ceria is not less than 99.8%, and the purity of tungsten carbide is not less than 99.8%.
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