CN113620704A - Preparation process of high-zirconium ceramic for special glass molten pool - Google Patents
Preparation process of high-zirconium ceramic for special glass molten pool Download PDFInfo
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Abstract
The invention discloses a preparation process of high-zirconium ceramic for a special glass molten pool, which belongs to the production of ceramic products with high zirconium content by an oversized sintering method in the technical field of application of special glass molten pools, in particular to the production in the fields of electronic glass, automobile glass, medical glass and the like, and at least comprises the following preparation process steps: the invention provides a high-zirconium ceramic product obtained by three preparation processes, which can realize repeated cyclic heating and kiln opening, has excellent anti-corrosion performance, increases and prolongs the service life of a special glass molten pool, obviously reduces the overall energy consumption, and has a series of advantages of reducing the manufacturing cost, improving the yield, reducing the comprehensive carbon emission and the like compared with the prior art.
Description
Technical Field
The invention relates to a sintering preparation process of a high-zirconium ceramic product with a super-large size sintering method in the technical field of application of special glass melting baths, in particular to a sintering preparation process of a high-zirconium ceramic used for special glass melting baths in the fields of electronic glass, automobile glass, medical glass and the like.
Background
The fused zirconia corundum brick is a white solid formed by melting pure alumina powder and zircon sand containing about 65 percent of zirconia and 34 percent of silicon dioxide in an electric melting furnace and injecting the melted zirconia corundum brick into a model for cooling, the rock phase structure of the fused zirconia corundum brick consists of eutectoid bodies of corundum and clinoptilolite and glass phases, and the eutectoid bodies of corundum phase and clinoptilolite are in terms of phase morphology, and the glass phases are filled between crystals of the corundum phase and the clinoptilolite. Because of the existence of the glass phase, under the working condition of long-term constant high temperature, the glass phase reacts with certain substances in the glass liquid and is washed away, so that the liquid phase washing and adhesion loss of the glass phase is caused, further, the porosity is opened, the corundum and the baddeleyite are eroded and washed away by the solution and low-soluble substances, so that the brick body is damaged rapidly, the corundum and the baddeleyite are eroded and washed away continuously and are lost in the glass solution, when the corundum and the baddeleyite are washed away and eroded to a certain extent (or eroded by high-temperature active chemical reaction), the production is stopped and the new kiln pool electric melting brick is replaced, so that the cost is high, the production stopping and maintenance loss is huge, the great cost difficulty is caused to glass product manufacturing enterprises, and the high zirconium bricks produced by the electric melting casting process of domestic and international similar manufacturers have the problems of extremely low yield, internal pore defects and the like.
Currently, casting 33#, 41#, 92#, 95# and the like are commonly available and applied in the market and are respectively used for combination at different parts, wherein the relative price of 33# and 41# is lower by 1.3-3 ten thousand per ton, and the relative price of 92# and 95# brands manufactured by a casting method is 26-32 ten thousand per ton because the yield is extremely low; there are product off-shelf blank areas and price off-shelf blank areas.
Disclosure of Invention
In view of the defects described in the prior art, the invention provides a sintering preparation process of high-zirconium ceramic for a special glass melting bath.
The technology adopted by the invention is as follows:
a sintering preparation process of high-zirconium ceramic for a special glass molten pool comprises the following steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; wherein the proportion of the zirconium dioxide in all the components is more than or equal to 10 percent.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components. As long as the zirconium dioxide content is 10% or more of the whole.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
As a preferable scheme of the invention, the paint specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material comprises the following components in parts by weight: 15 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 75 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
As a preferred scheme of the invention, the invention also provides another sintering preparation process, which comprises the following steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; wherein the proportion of the zirconium dioxide in all the components is more than or equal to 10 percent.
a, adding the composite material into a closed material mixer, and fully and uniformly mixing at a rotating speed of not less than 50 rpm;
and b, smelting the mixed material, wherein the equipment adopted for smelting can be high-frequency induction heating equipment or electric arc furnace heating equipment, the smelting temperature is 1800-plus-3000 ℃, the constant-temperature smelting time at constant temperature of 1800-plus-3000 ℃ is not less than 2 hours, and pouring the molten solution into a material cooling pool built by refractory materials to form a cooled crystal block or naturally cooling the smelting furnace and then taking out the cooled crystal block.
And c, crushing the crystal blocks to 100 meshes, and adding pure water with the same weight as the material.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components. As long as the zirconium dioxide content is 10% or more of the whole.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
As a preferable scheme of the invention, the paint specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material comprises the following components in parts by weight: 15 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 75 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
As a preferred scheme of the invention, the invention also provides another sintering preparation process, which comprises the following specific steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; wherein the proportion of the zirconium dioxide in all the components is more than or equal to 10 percent.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
d, crushing the high-zirconium ceramic obtained in the step S4 again and performing compression molding;
crushing the high-zirconium ceramic obtained in the step S4 into powder with different particle sizes of 100 meshes to 0.5 micron; then uniformly mixing powder with the grain diameter of D50 being 100 meshes-0.5 micron, filling the powder into a die for pressing, increasing the internal pressure of the die to enable the pressure of the die to be 20-300 MPa to obtain a formed blank, and carrying out pre-sintering step processing and fine finishing on the formed blank according to the size requirement;
e, heating and sintering the trimmed blank again and sintering at constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components. As long as the zirconium dioxide content is 10% or more of the whole.
As a preferred scheme of the invention, the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
As a preferable scheme of the invention, the paint specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron.
As a preferable scheme of the invention, the composite raw material comprises the following components in parts by weight: 15 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 75 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
The invention uses zirconium dioxide, bonding agent, pure water and other rare earth oxides to prepare high-zirconium ceramic, and carries out at least one-time crushing on the composite raw material, thereby saving the process time and reducing the process equipment, and the invention has the following advantages:
the method comprises the following steps of firstly, customized production and mould forming manufacturing, is suitable for small batch production, can be manufactured together, and has a yield higher than 99.50%;
and secondly, the zirconium content can be randomly adjusted within the range of 10-95% according to the service life of a customer designed molten pool, and the manufacturing cost is different due to different changes of the zirconium content, so that the method is suitable for the design service life of the customer molten pool, avoids wasting overlong service life resources, reduces emission and reduces consumption.
The preparation method disclosed by the invention completely eradicates the defects of air holes in the product and scouring holes caused by the defects, achieves the effects of consistency of density, consistency of microstructure and smoothness of scouring, simultaneously, has no low-melting substances and impurities because all the components are oxides with the melting point of more than 2000 ℃, is chemically unreactive when being contacted with glass solutions under the same conditions, has high scouring friction density and has the service characteristic of ultra-long service life.
And fourthly, the high-zirconium ceramic product realized by the preparation method has no defect in the interior and no thermal stress concentration phenomenon, and the other components play a role in wrapping and pinning monoclinic zirconia in the heating and cooling process, so that the high-zirconium ceramic product has excellent low thermal expansion coefficient and low volume expansion rate in the heating circulation process, has the characteristic of recycling use of repeatedly starting heating, and is an important advantage which is not possessed by other high-zirconium ceramics, fused and cast AZS and fused and cast high-zirconium processes.
Detailed Description
Example 1:
a sintering preparation process of high-zirconium ceramic for a special glass molten pool comprises the following steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; as long as the proportion of zirconium dioxide in the whole components is more than 10 percent, the zirconium dioxide can be prepared from the following components in parts by weight: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components, and further 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
In the embodiment, the composite raw material specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron. Specifically, 80 parts of zirconium dioxide, 4 parts of yttrium oxide, 1 part of cerium oxide, 15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water can be adopted. The grain diameter of the D50 of the zirconium dioxide is controlled to be 0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 micron; or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 3 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water; or 90 parts of zirconium dioxide, 2 parts of yttrium oxide, 2 parts of cerium oxide, 6 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 70 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. Or 20 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 60 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water; or 50 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 40 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Of course, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron. Specifically, 80 parts of zirconium dioxide, 19 parts of yttrium oxide, 1 part of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water can be adopted. Or 95 parts of zirconium dioxide, 2 parts of yttrium oxide, 3 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 90 parts of zirconium dioxide, 2 parts of yttrium oxide, 8 parts of aluminum oxide, 1 part of binding agent and 2 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 80 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 20 parts of zirconium dioxide, 10 parts of yttrium oxide, 70 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Similarly, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron. Specifically, 80 parts of zirconium dioxide, 1 part of yttrium oxide, 2 parts of cerium oxide, 17 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water can be adopted. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 3 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 90 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 8 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 70 parts of aluminum oxide, 1 part of binding agent and 2 parts of pure water. Or 20 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 70 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Compared with the products produced by the casting AZS33#41#92#95 process and the matching ratio, the comprehensive trace element impurities of the products produced by the invention, including but not limited to silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride calcium oxide and the like, do not exceed 0.6%, the highest bearing temperature of the products is 2400 ℃, compared with the highest bearing temperature of the products of 5-8% of the impurity contents of silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride, calcium oxide and the like of the casting process products, the products have the purity of 1800 ℃, and simultaneously the high-temperature performance change of the low-melting substances to the products is avoided, so the products of the invention have the high-temperature resistance and the long-life performance.
Example 2:
a sintering preparation process of high-zirconium ceramic for a special glass molten pool comprises the following steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; the zirconium dioxide is only required to account for more than 10% of the whole components by mass, and each component can be prepared according to the following weight portions: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components, such as 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
a, adding the composite material into a closed material mixer, and fully and uniformly mixing at a rotating speed of not less than 50 rpm;
and b, smelting the mixed material, wherein the equipment adopted for smelting can be high-frequency induction heating equipment or electric arc furnace heating equipment, the smelting temperature is 1800-plus-3000 ℃, the constant-temperature smelting time at constant temperature of 1800-plus-3000 ℃ is not less than 2 hours, and pouring the molten solution into a material cooling pool built by refractory materials to form a cooled crystal block or naturally cooling the smelting furnace and then taking out the cooled crystal block.
And c, crushing the crystal blocks to 100 meshes, and adding pure water with the same weight as the material.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
In the embodiment, the composite raw material specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron. Specifically, the components with the grain diameter of D50 controlled to be 1 micron, 80 parts of zirconium dioxide, 4 parts of yttrium oxide, 1 part of cerium oxide, 10 parts of aluminum oxide, 5 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water can be adopted. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 2 parts of aluminum oxide, 1 part of titanium dioxide, 2 parts of a binding agent and 5 parts of pure water; or 90 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 6 parts of aluminum oxide, 2 parts of titanium dioxide, 2 parts of a binding agent and 5 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 60 parts of aluminum oxide, 10 parts of titanium dioxide, 2 parts of a binding agent and 5 parts of pure water. Or 20 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 55 parts of aluminum oxide, 5 parts of titanium dioxide, 2 parts of a binding agent and 5 parts of pure water.
Of course, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron. Specifically, 80 parts of zirconium dioxide, 5 parts of yttrium oxide, 15 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water can be adopted. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 4 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 90 parts of zirconium dioxide, 1 part of yttrium oxide, 9 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 80 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 20 parts of zirconium dioxide, 10 parts of yttrium oxide, 70 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Similarly, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of aluminum oxide is controlled to be 0.5 mm-0.5 micron, and specifically 90 parts of zirconium dioxide, 1 part of yttrium oxide, 3 parts of cerium oxide, 6 parts of aluminum oxide, 1-2 parts of a bonding agent and 2-5 parts of pure water can be adopted. The grain diameter of the D50 of the zirconium dioxide is controlled to be 1 micron; the grain size of D50 of the yttrium oxide is controlled to be 1 micron, the grain size of D50 of the cerium oxide is controlled to be 1 micron, and the grain size of D50 of the aluminum oxide is controlled to be 1 micron. Or 80 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 10 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 3 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 80 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 20 parts of zirconium dioxide, 5 parts of yttrium oxide, 75 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Compared with the products produced by the casting AZS33#41#92#95 process and the matching process, the comprehensive trace element impurities of the products produced by the process, including but not limited to silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride calcium oxide and the like, do not exceed 0.6%, the highest bearing temperature of the products is 2400 ℃, and compared with the products produced by the casting process, which contain 5-8% of impurities, such as silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride, calcium oxide and the like, the products have the highest bearing temperature of 1800 ℃, and are more pure, and meanwhile, the high-temperature performance change of the products caused by low-melting substances is avoided, so the products produced by the process have higher high-temperature resistance and longer service life.
Example 3:
a sintering preparation process of high-zirconium ceramic for a special glass molten pool comprises the following steps: s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; the zirconium dioxide is only required to account for more than 10% of the whole components by mass, and each component can be prepared according to the following weight portions: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components, such as 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
S2, performing wet ball milling for 200min by adopting a ball mill at a rotating speed of not less than 100rpm to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
putting the uniformly mixed slurry into a drying oven for heating and drying, and crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, wherein the slurry blocks can be crushed by adopting airflow crushing equipment, screening equipment or any vibration and knocking equipment; then, putting the powder into a mold for pressing, and increasing the pressure inside the mold to enable the pressure of the mold to be 20-300 MPa, so as to obtain a formed blank; the concrete can be formed by a cold isostatic pressing process, a hot die-casting process, a dry isostatic pressing process, an extrusion forming process, a casting process and the like; and the formed blank is processed and finely finished in the steps before sintering according to the size requirement; the irregular part is trimmed mechanically or manually to reach the size required by the presintering of the drawing.
S4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
d, crushing the high-zirconium ceramic obtained in the step S4 again and performing compression molding;
crushing the high-zirconium ceramic obtained in the step S4 into powder with different particle sizes of 100 meshes to 0.5 micron; then uniformly mixing powder with the grain diameter of D50 being 100 meshes-0.5 micron, filling the powder into a die for pressing, increasing the internal pressure of the die to enable the pressure of the die to be 20-300 MPa to obtain a formed blank, and carrying out pre-sintering step processing and fine finishing on the formed blank according to the size requirement;
e, heating and sintering the trimmed blank again and sintering at constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
In the embodiment, the composite raw material specifically comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of aluminum oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of titanium dioxide is controlled to be 0.5 mm-0.5 micron, and concretely, each component with the grain size of D50 controlled to be 0.5 micron, 92 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 4 parts of aluminum oxide, 2 parts of titanium dioxide, 1-2 parts of binding agent and 2-5 parts of pure water can be adopted. Or 80 parts of zirconium dioxide, 4 parts of yttrium oxide, 1 part of cerium oxide, 15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 2 parts of aluminum oxide, 1 part of titanium dioxide, 2 parts of a binding agent and 5 parts of pure water; or 90 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 7 parts of aluminum oxide, 1 part of titanium dioxide, 2 parts of a binding agent and 2 parts of pure water.
Of course, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain diameter of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, and the grain diameter of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron. Specifically, 80 parts of zirconium dioxide, 5 parts of yttrium oxide, 15 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water can be adopted. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 4 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 90 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Similarly, the composite raw material can also comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. The zirconia content in the zirconia is more than 10 percent; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron. Specifically, 90 parts of zirconium dioxide, 1 part of yttrium oxide, 3 parts of cerium oxide, 6 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water can be adopted. Or 80 parts of zirconium dioxide, 2 parts of yttrium oxide, 2 parts of cerium oxide, 16 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water. Or 95 parts of zirconium dioxide, 1 part of yttrium oxide, 1 part of cerium oxide, 3 parts of aluminum oxide, 2 parts of a binding agent and 5 parts of pure water.
Similarly, the composite raw material can also comprise the following components in parts by weight: 15 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 75 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water. And the particle size of D50 of each component is controlled to be 0.5 micron. Or 10 parts of zirconium dioxide, 10 parts of yttrium oxide, 10 parts of cerium oxide, 70 parts of aluminum oxide, 3 parts of a binding agent and 5 parts of pure water. Or 20 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 70 parts of aluminum oxide, 3 parts of a binding agent and 5 parts of pure water.
Compared with the products produced by the casting AZS33#41#92#95 process and the matching process, the comprehensive trace element impurities of the products produced by the process, including but not limited to silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride calcium oxide and the like, do not exceed 0.6%, the highest bearing temperature of the products is 2400 ℃, and compared with the products produced by the casting process, which contain 5-8% of impurities, such as silicon dioxide, ferric oxide, sodium oxide, zinc oxide, boride, calcium oxide and the like, the products have the highest bearing temperature of 1800 ℃, and are more pure, and meanwhile, the high-temperature performance change of the products caused by low-melting substances is avoided, so the products produced by the process have higher high-temperature resistance and longer service life.
Claims (10)
1. A preparation process of high-zirconium ceramic for a special glass molten pool is characterized by comprising the following steps:
s1, preparing a composite raw material;
the composite raw material comprises the following components: zirconium dioxide, a binding agent, pure water and other components, wherein the other components are one or more of yttrium oxide, aluminum oxide, titanium dioxide and cerium oxide; wherein the proportion of the zirconium dioxide in all the components is more than or equal to 10 percent;
s2, performing wet ball milling at a rotating speed of not less than 100rpm for 200min to obtain aqueous slurry with D50 of not more than 0.5 mu m;
s3, drying the slurry, crushing and forming in a mould to obtain a blank, and trimming the blank;
heating and drying the uniformly mixed slurry, crushing the dried slurry blocks when the moisture of the slurry is 0.1-3%, then loading the powder into a mold for pressing, increasing the internal pressure of the mold to enable the mold pressure to be in the range of 20-300 MPa, obtaining a molded blank, and performing pre-sintering step processing and fine finishing on the molded blank according to the size requirement;
s4, heating and sintering the trimmed blank body at a constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
2. The sintering preparation process of high zirconium ceramic for special glass melting bath according to claim 1, characterized in that between step S1 and step S2 there are the following pretreatment steps:
a, adding the composite material into a closed material mixer, and fully and uniformly mixing at a rotating speed of not less than 50 rpm;
b, smelting the mixed materials, wherein the smelting temperature is 1800-3000 ℃, the constant-temperature smelting time at the constant temperature of 1800-3000 ℃ is not less than 2 hours, and cooling the molten solution into a crystal block;
and c, crushing the crystal blocks to 100 meshes, and adding pure water with the same weight as the material.
3. The sintering preparation process of high zirconium ceramic for special glass melting bath according to claim 1, characterized in that after step S4, the following post-treatment steps are provided: d, crushing the high-zirconium ceramic obtained in the step S4 again and performing compression molding;
crushing the high-zirconium ceramic obtained in the step S4 into powder with different particle sizes of 100 meshes to 0.5 micron; then uniformly mixing powder with the grain diameter of D50 being 100 meshes-0.5 micron, filling the powder into a die for pressing, increasing the internal pressure of the die to enable the pressure of the die to be 20-300 MPa to obtain a formed blank, and carrying out pre-sintering step processing and fine finishing on the formed blank according to the size requirement;
e, heating and sintering the trimmed blank again and sintering at constant temperature to obtain high-zirconium ceramic;
and placing the trimmed blank into a sintering furnace, and carrying out heating sintering and constant-temperature sintering, wherein the constant-temperature sintering is sintering at 1400-1850 ℃ for 2-25 h, and after the constant-temperature sintering is finished, naturally cooling to below 100 ℃ within 5-100 h to obtain the large-size high-zirconium ceramic with the monoclinic crystal form and the monoclinic crystal form ratio of not less than 5%.
4. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 1, 2 or 3, wherein the composite raw materials comprise the following components in parts by weight: 10-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-90 parts of other components.
5. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 4, wherein the composite raw materials comprise the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-2 parts of a bonding agent, 2-5 parts of pure water and 5-20 parts of other components.
6. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 5, wherein the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-3 parts of titanium dioxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
7. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 5, wherein the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
8. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 5, wherein the composite raw material comprises the following components in parts by weight: 80-95 parts of zirconium dioxide, 1-8 parts of yttrium oxide, 1-5 parts of cerium oxide, 5-15 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
9. The sintering preparation process of the high-zirconium ceramic for the special glass melting tank as claimed in claim 5, wherein the composite raw material comprises the following components in parts by weight: 15 parts of zirconium dioxide, 5 parts of yttrium oxide, 5 parts of cerium oxide, 75 parts of aluminum oxide, 1-2 parts of a binding agent and 2-5 parts of pure water.
10. The process of claim 1, wherein the zirconia content in the zirconia is 10% or more; the grain diameter of the zirconium dioxide D50 is controlled to be 0.5 mm-0.5 micron; the grain size of D50 of the yttrium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the cerium oxide is controlled to be 0.5 mm-0.5 micron, the grain size of D50 of the aluminum oxide is controlled to be 0.5 mm-0.5 micron, and the grain size of D50 of the titanium dioxide is controlled to be 0.5 mm-0.5 micron.
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| CN202111078490.3A CN113620704A (en) | 2021-09-15 | 2021-09-15 | Preparation process of high-zirconium ceramic for special glass molten pool |
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| CN202111078490.3A CN113620704A (en) | 2021-09-15 | 2021-09-15 | Preparation process of high-zirconium ceramic for special glass molten pool |
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