CN112679224B - Micro-crystallized porous ceramic plate and preparation method thereof - Google Patents
Micro-crystallized porous ceramic plate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a microcrystalline porous ceramic plate and a preparation method thereof, belonging to the technical field of porous ceramic production. The invention uses high calcium water slag and diatomite of iron works as main raw materials, and obtains the product with low production cost, high open porosity, high strength and wide application range through twice foaming and high-temperature sintering. A preparation method of a microcrystallized porous ceramic plate comprises the following steps: 1) mixing the raw materials, and performing wet ball milling to prepare slurry; 2) drying the slurry into powder; 3) adding the powder into a refractory mold, and then placing the mold into a tunnel kiln for sintering to prepare a microcrystalline porous ceramic blank; 4) and grinding and cutting the micro-crystallized porous ceramic blank by a dry method to obtain the plate with holes on the surface.
Description
Technical Field
The invention relates to a microcrystallized porous ceramic plate and a preparation method thereof, belonging to the technical field of porous ceramic production.
Background
The microcrystalline glass ceramic is a polycrystalline solid material containing a large number of microcrystalline phases and glass phases, which is prepared by controlling crystallization in the process of heating raw materials to generate a glass liquid phase. The specific structure of the glass-ceramic is closely related to its formulation composition, except that it contains a certain amount of glass former (SiO) 2 、B 2 O 3 、P 2 O 5 Etc.) and inducing ions (Li) + 、Mg 2+ 、Zn 2+ Etc.) in addition, often by introducing nucleating agents (ZrO) 2 、TiO 2 、CaF 2 Etc.) promote the crystallization of the glass as a whole.
The porous ceramic material with high open porosity and high strength is prepared by using high-quality raw materials such as alumina, silicon carbide and the like as main materials through molding and high-temperature sintering process of over 1300 ℃, and has high production cost.
Disclosure of Invention
The invention provides a microcrystallized porous ceramic plate and a preparation method thereof, aiming at solving the problem of high production cost of the existing porous ceramic, the method takes high-calcium granulated slag and diatomite of iron works as main raw materials, and wollastonite crystal phase is generated through twice foaming and high-temperature sintering, so that the microcrystallized porous ceramic plate with high open porosity, high strength and wide application range is obtained.
In order to achieve the purpose, the invention adopts the technical scheme that:
a microcrystallized porous ceramic plate comprises the following raw materials in percentage by mass: 20-30% of high-calcium granulated slag in iron works, 50-60% of diatomite, 5-15% of kaolin, 5-15% of calcite/limestone, 1-1.5% of zinc oxide, 1-1.5% of barium carbonate and 1-1.5% of silicon carbide.
A microcrystallized porous ceramic plate having the chemical composition: SiO 2 2 ：50-65%，Al 2 O 3 ：6-8%，Fe 2 O 3 ：0.5-1.5%，CaO：18-28%，MgO：1-3%，K 2 O：0.1-2%，Na 2 O：0.1-2% ，ZnO：0.5-1.5% ，BaO：0.5-1.5%，TiO 2 ：0.1-1.5%。
A microcrystalline porous ceramic plate is prepared by carrying out bulk weight 180-.
A microcrystalline porous ceramic plate, wherein pores are distributed on the cell walls, and the pore diameter of meso-pores is as follows: 2 nm < d < 50 nm, pore size of macropores: d > 50 nm.
A preparation method of a microcrystallized porous ceramic plate comprises the following steps:
1) mixing the raw materials, and performing wet ball milling to prepare slurry;
2) drying the slurry into powder;
3) adding the powder into a refractory mold, and then placing the mold into a tunnel kiln for sintering to prepare a microcrystalline porous ceramic blank;
4) and grinding and cutting the micro-crystallized porous ceramic blank by a dry method to obtain the plate with holes on the surface.
The mud drying is spray drying at 600 ℃.
The sintering process comprises the following steps: heating to 900-1000 ℃ at a heating rate of 10-20 ℃/min, preserving heat for 20-30 minutes to foam calcium carbonate in calcite or limestone, heating to a sintering final temperature of 1120-1150 ℃ at a heating rate of 1-5 ℃/min, foaming silicon carbide, and preserving heat for 0And 5-1 h, crystallizing beta-CaSiO by using bubble wall glass phase 3 Cooling the wollastonite crystal phase to room temperature at a cooling rate of 20-30 ℃/min.
The thickness of the microcrystalline porous ceramic blank is 150-200 mm.
The refractory mold is made of mullite-cordierite plate.
Advantageous effects of the invention
Based on the conventional foamed ceramic process, the invention adopts high-calcium water slag of iron works, calcite (or limestone), diatomite, kaolin and the like as raw materials to generate CaO-AI (calcium oxide) through high-temperature sintering reaction 2 O 3 -SiO 2 In the liquid phase, calcium carbonate provided by calcite or limestone is decomposed into calcium oxide and carbon dioxide at 900-1000 ℃, so that a high-temperature liquid phase with certain viscosity forms a foaming state, the silicon carbide raw material is continuously foamed at 1100-1120 ℃ in the bubble wall liquid phase process, the bubble wall is broken into through large and small holes, and the bubble wall glass is crystallized to obtain beta-CaSiO in the process of heat preservation at 1120-1150 ℃ for 30-60 minutes 3 And finally cooling the wollastonite to room temperature at the cooling rate of 20-30 ℃/min to prepare the microcrystallized porous ceramic with the volume weight of 180-200kg/m, the water absorption rate of 200-400% and the porosity of 60-80%, wherein the compressive strength of the microcrystallized porous ceramic is greater than 3 MPa. Because the raw materials adopted by the invention have low cost, the production cost of the product is obviously lower than that of the existing high-strength porous ceramic material with high open porosity; the product has wide application range and can be used as an acoustic board, a plant seedling cultivation lightweight board, a biological bacteria carrier board for sewage treatment, an artificial island and the like; because the high-calcium granulated slag of the iron works is adopted, the treatment and the comprehensive utilization of the slag of the industrial waste of the iron works are facilitated.
Drawings
FIG. 1 is an electron micrograph of a microcrystallized porous ceramic;
fig. 2 is a photograph of fig. 1 magnified 100 times.
Detailed Description
Example 1
A preparation method of a microcrystallized porous ceramic plate comprises the following steps:
1. 30% of iron works high-calcium water granulated slag, 50% of diatomite, 10% of kaolin, 7% of calcite, 1% of silicon carbide, 1% of zinc oxide and 1% of barium carbonate are taken, and the raw materials are mixed and then are prepared into slurry through wet ball milling;
2. spray-drying the slurry at 600 ℃ to obtain powder;
3. adding the powder into a refractory mold made of mullite-cordierite plate, placing the mold into a tunnel kiln for high-temperature sintering, wherein in the sintering process, the temperature is increased to 950 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 30min, calcium carbonate in calcite is foamed, the temperature is increased to 1140 ℃ at the heating rate of 3 ℃/min, silicon carbide is foamed, the temperature is kept for 1 h, the wall glass phase is crystallized to obtain a beta-CaSiO 3 wollastonite crystalline phase, then the temperature is reduced to room temperature at the cooling rate of 20 ℃/min, and a microcrystallized porous ceramic blank with the thickness of 150mm, the volume weight of 200 kg/cube, the water absorption rate of 200 percent, the porosity of 60 percent and the compressive strength of 4.2Mpa is prepared, and the aperture of a middle mesopore: 2 nm < d < 50 nm, pore size of macropores: d is greater than 50 nm;
the composition of the microcrystalline porous ceramic is shown in Table 1:
4. the blank is ground and cut by a dry method according to the requirement to obtain a micro-crystallized porous ceramic plate with holes distributed on each surface and the wall of the hole crystallized into wollastonite, and the micro-crystallized porous ceramic plate can be used as a sound-absorbing plate for rail transit or a movie theater.
Example 2
A preparation method of a microcrystallized porous ceramic plate comprises the following steps:
1. taking 25% of iron works high-calcium water granulated slag, 55% of diatomite, 10% of kaolin, 6.3% of limestone, 1.2% of silicon carbide, 1.3% of zinc oxide and 1.2% of barium carbonate according to mass percentage, mixing the raw materials, and carrying out wet ball milling to prepare slurry;
2. then the slurry is sprayed and dried into powder at 600 ℃;
3. adding the powder into a refractory mold made of mullite-cordierite plate, placing the mold into a tunnel kiln for high-temperature sintering, wherein in the sintering process, the temperature is raised to 980 ℃ at the temperature rise rate of 15 ℃/min, the temperature is kept for 25min, then the temperature is raised to 1130 ℃ at the temperature rise rate of 5 ℃/min, the temperature is kept for 40 min, and then the temperature is lowered to room temperature at the temperature drop rate of 30 ℃/min to prepare a microcrystalline porous ceramic blank with the thickness of 180mm, the volume weight of 190 kg/cube, the water absorption rate of 300 percent, the porosity of 70 percent and the compressive strength of 3.8 Mpa;
the composition of the microcrystalline porous ceramic is shown in Table 2:
4. and (3) grinding and cutting the blank by a six-surface dry method according to requirements to obtain a micro-crystallized porous ceramic plate with holes distributed on each surface and the wall of the hole crystallized into wollastonite, and the micro-crystallized porous ceramic plate can be used as a biological bacteria carrier plate for sewage treatment.
Example 3
A preparation method of a microcrystallized porous ceramic plate comprises the following steps:
1. taking 20% of iron works high-calcium water granulated slag, 60% of diatomite, 5.5% of kaolin, 10% of limestone, 1.5% of silicon carbide, 1.5% of zinc oxide and 1.5% of barium carbonate according to mass percentage, mixing the raw materials, and performing wet ball milling to prepare slurry;
2. spray-drying the slurry at 600 ℃ to obtain powder;
3. adding the powder into a refractory mold made of mullite-cordierite plate, placing the mold into a tunnel kiln for high-temperature sintering, wherein the temperature is increased to 1000 ℃ at the heating rate of 20 ℃/min in the sintering process, the temperature is kept for 20min, the temperature is increased to 1150 ℃ at the heating rate of 1 ℃/min, the temperature is kept for 30min, and then the temperature is reduced to room temperature at the cooling rate of 30 ℃/min to prepare a microcrystallized porous ceramic blank with the thickness of 200mm, the volume weight of 180 kg/cube, the water absorption rate of 400%, the porosity of 80% and the compressive strength of 3.1 Mpa;
the composition of the microcrystalline porous ceramics is shown in Table 3:
4. and (3) grinding and cutting the blank by a six-sided dry method according to requirements to obtain a micro-crystallized porous ceramic plate with holes distributed on each surface and the wall of the hole crystallized into wollastonite, and the micro-crystallized porous ceramic plate can be used as a plant seedling cultivation light plate and an artificial floating island.
Claims (4)
1. A microcrystallized porous ceramic plate is characterized by comprising the following raw materials in percentage by mass: 20-30% of iron works high-calcium water granulated slag, 50-60% of diatomite, 5-15% of kaolin, 5-15% of calcite/limestone, 1-1.5% of zinc oxide, 1-1.5% of barium carbonate and 1-1.5% of silicon carbide, wherein the ceramic plate comprises the following chemical components: SiO 2 2 ：50-65%，Al 2 O 3 ：6-8%，Fe 2 O 3 ：0.5-1.5%，CaO：18-28%，MgO：1-3%，K 2 O：0.1-2%，Na 2 O：0.1-2% ，ZnO：0.5-1.5% ，BaO：0.5-1.5%，TiO 2 : 0.1-1.5%, wherein the volume weight of the ceramic plate is 180-: 2 nm< d <50 nm, pore size of macropores: d>50 nm, the preparation method of the microcrystallized porous ceramic plate comprises the following steps:
1) mixing the raw materials, and performing wet ball milling to prepare slurry;
2) drying the slurry into powder;
3) adding the powder into a refractory mold, and then placing the mold into a tunnel kiln for sintering to prepare a microcrystalline porous ceramic blank;
4) grinding and cutting the microcrystal porous ceramic blank by a dry method to obtain a plate with holes on the surface,
wherein the slurry drying is 600 ℃ spray drying, wherein the sintering process is as follows: heating to 900-class temperature 1000 ℃ at a heating rate of 10-20 ℃/min, preserving heat for 20-30 minutes to foam calcium carbonate in calcite or limestone, heating to a sintering final temperature 1120-class temperature 1150 ℃ at a heating rate of 1-5 ℃/min, foaming silicon carbide, preserving heat for 0.5-1 hour, and crystallizing beta-CaSiO by phase separation of cell wall glass 3 Cooling the wollastonite crystal phase to room temperature at a cooling rate of 20-30 ℃/min.
2. A method for preparing a microcrystallized porous ceramic plate according to claim 1, comprising the steps of:
1) mixing the raw materials, and performing wet ball milling to prepare slurry;
2) drying the slurry into powder;
3) adding the powder into a refractory mold, and then placing the mold into a tunnel kiln for sintering to prepare a microcrystalline porous ceramic blank;
4) grinding and cutting the microcrystal porous ceramic blank by a dry method to obtain a plate with holes on the surface,
wherein, the mud drying is 600 ℃ spray drying, wherein, the sintering process is: heating to 900-class temperature 1000 ℃ at a heating rate of 10-20 ℃/min, preserving heat for 20-30 minutes to foam calcium carbonate in calcite or limestone, heating to a sintering final temperature 1120-class temperature 1150 ℃ at a heating rate of 1-5 ℃/min, foaming silicon carbide, preserving heat for 0.5-1 hour, and crystallizing beta-CaSiO by phase separation of cell wall glass 3 Cooling the wollastonite crystal phase to room temperature at a cooling rate of 20-30 ℃/min.
3. The method as claimed in claim 2, wherein the microcrystalline porous ceramic slab has a thickness of 150-200 mm.
4. A method of making a microcrystallized porous ceramic plate according to claim 2, wherein the refractory mold is made of mullite-cordierite plate.
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