CN116621569A - High-purity amorphous quartz ceramic and preparation method thereof - Google Patents
High-purity amorphous quartz ceramic and preparation method thereof Download PDFInfo
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- CN116621569A CN116621569A CN202310600673.XA CN202310600673A CN116621569A CN 116621569 A CN116621569 A CN 116621569A CN 202310600673 A CN202310600673 A CN 202310600673A CN 116621569 A CN116621569 A CN 116621569A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 20
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 239000005350 fused silica glass Substances 0.000 claims abstract description 11
- 229920001353 Dextrin Polymers 0.000 claims abstract description 6
- 239000004375 Dextrin Substances 0.000 claims abstract description 6
- 235000019425 dextrin Nutrition 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 8
- 239000007767 bonding agent Substances 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 6
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000012257 stirred material Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 230000035939 shock Effects 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000002035 prolonged effect Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 229910021487 silica fume Inorganic materials 0.000 abstract description 3
- 239000011230 binding agent Substances 0.000 abstract description 2
- 239000011449 brick Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000000451 tissue damage Effects 0.000 description 1
- 231100000827 tissue damage Toxicity 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
The application discloses a high-purity amorphous quartz ceramic and a preparation method thereof, wherein the high-purity amorphous quartz ceramic comprises the following raw materials, by weight, 80-90 parts of high-purity amorphous fused quartz, 0.5-1 part of fused zirconia, 4-5 parts of zirconium-containing silica fume, 2.5-3.5 parts of white dextrin and 4-8 parts of binding agent; the high-purity amorphous quartz ceramic has the purity silicon dioxide content of more than 99 percent, has high purity, and can not introduce impurities into high-temperature solution in some special use occasions such as the top part of a glass melting pool and the like, thereby reducing the quality of products; the normal-temperature compressive strength of the high-purity amorphous quartz ceramic can reach more than 100MPa, the strength is greatly improved, the wear resistance is greatly improved, and the service life can be greatly prolonged; the high-purity amorphous quartz ceramic has the thermal shock resistance (1100 ℃ and water cooling) of more than 100 times, greatly improves the rapid cooling and rapid heating resistance, and has wider application prospect.
Description
Technical Field
The application relates to the technical field of refractory material processing, in particular to high-purity amorphous quartz ceramic and a preparation method thereof.
Background
At present, the traditional quartz ceramic has the compressive strength of about 50Mpa, the thermal expansion rate (1000 ℃) of about 0.7 percent, the abrasion resistance and the thermal shock stability in daily use are common, and particularly, the service life of the quartz ceramic at the position directly contacted with raw materials and the like is short, so that the application range is limited. And in some parts in direct contact with the high temperature solution, it is more desirable that the material have excellent stability in order to prevent contamination of the high temperature solution. The Chinese patent publication No. CN 113292346B, for example, discloses the field of silica brick preparation, and in particular relates to a sintering promoting agent for preparing silica bricks, a composite silica brick and a preparation method thereof, and an amorphous-crystalline composite silica brick prepared by using the sintering promoting agent and a preparation method thereof. The sintering promoting agent comprises silica sol, aluminum hydroxide and titanium dioxide. The silica brick prepared by the method has high SiO2 content, weak toxicity and high bonding strength, can realize low-temperature volume stability and kiln high-temperature masonry integrity at the same time, and has long high-temperature service life.
Therefore, the high-purity amorphous quartz ceramic with good thermal shock property, long service life and wear resistance and the preparation method thereof are provided, and the high-purity amorphous quartz ceramic is a problem worthy of research.
Disclosure of Invention
The application aims to provide high-purity amorphous quartz ceramic with good thermal shock resistance, long service life and wear resistance and a preparation method thereof.
The purpose of the application is realized in the following way:
the high-purity amorphous quartz ceramic comprises, by weight, 80-90 parts of high-purity amorphous fused quartz, 0.5-1 part of fused zirconia, 4-5 parts of zirconium-containing micro silicon powder, 2.5-3.5 parts of white dextrin and 4-8 parts of bonding agent;
the grain size of the high-purity amorphous fused quartz is 0-2.2mm, the grain size of the fused zirconia is 325 meshes, and the grain size of the zirconium-containing micro silicon powder is 50 mu m.
The bonding agent comprises the following components in parts by weight: 2-8 parts of ethyl silicate and 2-10 parts of zirconium phosphate with the zirconium oxide content of more than or equal to 40 percent.
The high-purity amorphous fused quartz has the particle size of 1-2.2mm, the content of 15-20 parts, the content of 0.5-1mm, the content of 15-20 parts, the content of 1-0mm, the content of 10-15 parts, the content of 180 meshes, the content of 10-15 parts, the content of 220 parts, and the raw materials with different particle sizes are adopted to reduce the porosity of the finished product and improve the compactness and strength of the product.
A preparation method of high-purity amorphous quartz ceramic is characterized in that: the method comprises the following steps:
step 1, premixing raw materials: premixing raw materials according to the raw material proportion of the high-purity amorphous quartz ceramic in the table 1;
step 2, wet mixing: adding the premixed high-purity amorphous quartz ceramic raw material premix into a double-wheel wet mill, adding 2-8% of hydrolyzed ethyl silicate and 2-10% of zirconium phosphate with the zirconium oxide content of more than or equal to 40%, mixing and grinding for 3-5 minutes, and discharging after the materials are uniformly mixed, and performing mechanical press molding;
step 3, molding: filling the stirred material into a servo electric screw press die for compression molding;
step 4, demolding: and when the thickness direction is pressed to the required thickness, demolding can be performed. After demolding, curing the product in a curing room at 30-85 ℃ for 48-72 hours;
step 5, drying: after demolding, drying the product in a dryer at the temperature of 30-85 ℃ for 48-72 hours;
step 6, kiln filling and sintering: loading the dried product into a shuttle kiln, and sintering according to a lower sintering curve;
step 7, kiln discharging and sorting: and sorting the products discharged from the kiln block by block according to the standard, and removing unqualified products.
The beneficial effects of the application are as follows: 1. the high-purity amorphous quartz ceramic has the purity silicon dioxide content of more than 99 percent, has high purity, and can not introduce impurities into high-temperature solution in some special use occasions such as the top part of a glass melting pool and the like, thereby reducing the quality of products;
2. the normal-temperature compressive strength of the high-purity amorphous quartz ceramic can reach more than 100MPa, the strength is greatly improved, the wear resistance is greatly improved, and the service life can be greatly prolonged;
3. the high-purity amorphous quartz ceramic has the thermal shock resistance (1100 ℃ and water cooling) of more than 100 times, greatly improves the rapid cooling and rapid heating resistance, and has wider application prospect;
4. the thermal expansion performance of the high-purity amorphous quartz ceramic can be greatly reduced to about 0.05%, and the volume stability is greatly improved, so that the high-purity amorphous quartz ceramic is very important in a maintenance scene, can be perfectly matched with the original material without gaps, and cannot damage the original material due to volume expansion or shrinkage after the maintenance is finished and after heating;
5. the high-purity amorphous quartz ceramic does not contain alumina components, does not generate mullite with the high-purity amorphous quartz, and can avoid the damage to the material performance in the mullite process.
Detailed Description
The application is illustrated below with reference to the examples:
the high-purity amorphous quartz ceramic comprises, by weight, 80-90 parts of high-purity amorphous fused quartz, 0.5-1 part of fused zirconia, 4-5 parts of zirconium-containing micro silicon powder, 2.5-3.5 parts of white dextrin and 4-8 parts of bonding agent; zirconia is introduced into the fused zirconia and the zirconia-containing silica fume, the introduction of the zirconia can play a role in phase change toughening of the high-purity amorphous quartz ceramic, and the strength and the thermal shock performance of the product are greatly improved from the actual test result; the zirconium-containing micro silicon powder is used for replacing the traditional silicon micro powder, and because of the special spherical structure and fineness of the zirconium-containing micro silicon powder, the zirconium-containing micro silicon powder can be more uniformly dispersed into the high-purity amorphous quartz ceramic, has great significance for improving the strength, and meanwhile, the zirconium oxide component is introduced. The introduction of the white dextrin solves the problem that water is continuously evaporated into the air in the preparation process of the pug, can effectively lock the water in the pug, and improves the molding property of the pug.
The grain size of the high-purity amorphous fused quartz is 0-2.2mm, the grain size of the fused zirconia is 325 meshes, and the grain size of the zirconium-containing micro silicon powder is 50 mu m.
The bonding agent comprises the following components in parts by weight: 2-8 parts of ethyl silicate and 2-10 parts of zirconium phosphate with the zirconium oxide content of more than or equal to 40 percent can be used as a bonding agent to bond aggregate and powder together, so that the molding property of pug is improved, the sintering promotion effect can be achieved, the sintering temperature and time of a product are reduced, energy sources can be saved, and meanwhile, a certain amount of zirconium oxide with gain effect on the product property is introduced.
The high-purity amorphous fused quartz has the particle size of 1-2.2mm, the content of 15-20 parts, the content of 0.5-1mm, the content of 15-20 parts, the content of 1-0mm, the content of 10-15 parts, the content of 180 meshes, the content of 10-15 parts, the content of 220 parts, and the adoption of raw materials with different particle sizes can reduce the porosity of a finished product and improve the compactness and strength of the product.
The preparation method of the high-purity amorphous quartz ceramic comprises the following steps:
and step 1, premixing raw materials. The premixing of the raw materials was performed according to the raw material ratios of the high purity amorphous quartz ceramics of table 1.
And 2, wet mixing. Adding the premixed high-purity amorphous quartz ceramic raw material premix into a double-wheel wet mill, adding 2-8% of hydrolyzed ethyl silicate and 2-10% of zirconium phosphate with the zirconium oxide content of more than or equal to 40%, mixing and grinding for 3-5 minutes, and discharging after the materials are uniformly mixed, and performing mechanical press molding.
And 3, molding. Filling the stirred material into a servo electric screw press die for compression molding.
And 4, demolding. And when the thickness direction is pressed to the required thickness, demolding can be performed. After demolding, curing the product in a curing room at 30-85 ℃ for 48-72 hours.
And 5, drying. After demolding, the product needs to be dried in a dryer at 30-85 ℃ for 48-72 hours.
And 6, kiln loading and sintering. And loading the dried product into a shuttle kiln, and sintering according to a lower sintering curve.
And 7, discharging from the kiln and picking. And sorting the products discharged from the kiln block by block according to the standard, and removing unqualified products.
The raw material ratios of example 1 and example 2 are shown in table 1;
the firing profile of step 6 is shown in Table 2;
experimental results of example 1 and example 2
From the analysis of the detection results of the embodiment 1 and the embodiment 2, it is known that the high-purity amorphous quartz ceramic does not contain harmful impurities such as alumina, calcium oxide, potassium oxide, sodium oxide and the like, and the existence of the impurities can lead to the crystal form transformation of the high-purity amorphous quartz ceramic under the high-temperature use environment, so that cracks and tissue damage are generated, and the high-purity amorphous quartz ceramic has more destructive power on high-silicon products. The zirconium-containing micro silicon powder is filled in gaps among the aggregates, so that the porosity of the high-purity amorphous quartz ceramic is greatly reduced, and the compactness is improved. The high-purity amorphous quartz ceramic has the compressive strength of more than 100MPa, can cope with various impacts and grinding and stripping, improves the supporting capacity and the wear resistance of the high-purity amorphous quartz ceramic, and prolongs the service life. The thermal shock stability reaches more than 100 times, the qualitative leap is realized, and the service life of the high-purity amorphous quartz ceramic in a rapid cooling and rapid heating environment can be greatly prolonged. The ultra-low thermal expansion rate can realize seamless bonding between high-purity amorphous quartz ceramics, reduce the phenomenon of gap enlargement or material extrusion damage caused by volume change, improve the processing precision of industries with higher precision requirements, and avoid precision errors caused by the volume change of supporting materials between a cold state and a hot state.
The application discloses a high-purity amorphous quartz ceramic and a preparation method thereof, wherein the high-purity amorphous quartz ceramic comprises the following raw materials, by weight, 80-90 parts of high-purity amorphous fused quartz, 0.5-1 part of fused zirconia, 4-5 parts of zirconium-containing silica fume, 2.5-3.5 parts of white dextrin and 4-8 parts of binding agent; the high-purity amorphous quartz ceramic has the purity silicon dioxide content of more than 99 percent, has high purity, and can not introduce impurities into high-temperature solution in some special use occasions such as the top part of a glass melting pool and the like, thereby reducing the quality of products; the normal-temperature compressive strength of the high-purity amorphous quartz ceramic can reach more than 100MPa, the strength is greatly improved, the wear resistance is greatly improved, and the service life can be greatly prolonged; the high-purity amorphous quartz ceramic has the thermal shock resistance (1100 ℃ and water cooling) of more than 100 times, greatly improves the rapid cooling and rapid heating resistance, and has wider application prospect.
Claims (4)
1. A high purity amorphous quartz ceramic, characterized by: comprises the following raw materials, by weight, 80-90 parts of high-purity amorphous fused quartz, 0.5-1 part of fused zirconia, 4-5 parts of zirconium-containing micro silicon powder, 2.5-3.5 parts of white dextrin and 4-8 parts of bonding agent;
the grain size of the high-purity amorphous fused quartz is 0-2.2mm, the grain size of the fused zirconia is 325 meshes, and the grain size of the zirconium-containing micro silicon powder is 50 mu m.
2. The high purity amorphous quartz ceramic of claim 1, wherein: the bonding agent comprises the following components in parts by weight: 2-8 parts of ethyl silicate and 2-10 parts of zirconium phosphate with the zirconium oxide content of more than or equal to 40 percent.
3. The high purity amorphous quartz ceramic of claim 1, wherein: the high-purity amorphous fused quartz has the particle size of 1-2.2mm, the content of 15-20 parts, the content of 0.5-1mm, the content of 15-20 parts, the content of 1-0mm, the content of 10-15 parts, the content of 180 meshes, the content of 10-15 parts, the content of 220 parts, and the raw materials with different particle sizes are adopted to reduce the porosity of the finished product and improve the compactness and strength of the product.
4. A preparation method of high-purity amorphous quartz ceramic is characterized in that: the method comprises the following steps:
step 1, premixing raw materials: premixing raw materials according to the raw material proportion of the high-purity amorphous quartz ceramic in the table 1;
step 2, wet mixing: adding the premixed high-purity amorphous quartz ceramic raw material premix into a double-wheel wet mill, adding 2-8% of hydrolyzed ethyl silicate and 2-10% of zirconium phosphate with the zirconium oxide content of more than or equal to 40%, mixing and grinding for 3-5 minutes, and discharging after the materials are uniformly mixed, and performing mechanical press molding;
step 3, molding: filling the stirred material into a servo electric screw press die for compression molding;
step 4, demolding: when the thickness direction is pressed to the required thickness, the mold can be removed,
after demolding, curing the product in a curing room at 30-85 ℃ for 48-72 hours;
step 5, drying: after demolding, drying the product in a dryer at the temperature of 30-85 ℃ for 48-72 hours;
step 6, kiln filling and sintering: loading the dried product into a shuttle kiln, and sintering according to a lower sintering curve;
step 7, kiln discharging and sorting: and sorting the products discharged from the kiln block by block according to the standard, and removing unqualified products.
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