CN113248259A - Large-particle porous ceramic and preparation method thereof - Google Patents
Large-particle porous ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a large-particle porous ceramic and a preparation method thereof, wherein the large-particle porous ceramic comprises a main material and an adhesive; particle diameter D of the main material50The range is 50-1500 μm; the adhesive is composed of a low temperature adhesive and a high temperature adhesive. Ceramic productMixing ceramic main materials, adhesive and other additives to form solid mixture or slurry, filling the mold cavity, pressing or pouring to form a blank, and firing to form the large-particle porous ceramic. The obtained large-particle porous ceramic does not need to refine ceramic particles, so that the limitation of the prior art on the particle size, purity and the like of raw materials is reduced, and the application range is wide; the porous ceramic is matched with a low-temperature adhesive and a high-temperature adhesive for use, and is subjected to low-temperature degreasing, glue removal and medium-high temperature bonding and sintering, so that the porous ceramic is quickly and uniformly bonded at the temperature of below 1000 ℃, the open porosity can reach more than 95%, and the bending strength is not less than 2 MPa.
Description
Technical Field
The invention belongs to the technical field of porous ceramics, and particularly relates to large-particle porous ceramics and a preparation method thereof.
Background
The porous ceramic material is prepared by taking corundum sand, silicon carbide and other raw materials as main materials through molding and a special high-temperature sintering process. The porous ceramic material has the advantages of high temperature and high pressure resistance, acid-base and organic medium corrosion resistance, good biological inertia, controllable pore structure and porosity, long service life, renewable products and the like. The composite material is prepared by methods such as an extrusion forming method, a foaming method, a dipping method, a sol-gel method, 3D additive printing and the like, and is widely applied to the fields of metal smelting filter residue nets, environment-friendly treatment filter carriers, composite materials, refractory materials and the like.
The existing products and processes (such as CN111574203A) usually require that the particle size of the main material particle of the porous ceramic is less than 5 μm, and a large amount of pore-forming agent is added to meet the requirement of porosity. The large-particle-size porous ceramic main material with the particle size of more than 50 mu m is adopted, the contact area between powder bodies is smaller, high-temperature sintering at the temperature of more than 1200 ℃ is required, the requirement of the open porosity of more than 90 percent cannot be met, the situation that the bending strength is less than 2MPa is easy to occur, and the ceramic yield is extremely low. The invention simultaneously meets the requirements of open porosity and bending strength by using the main material of the large-particle porous ceramic in combination with the low-temperature adhesive and the high-temperature adhesive, and reduces the sintering process conditions.
Disclosure of Invention
The invention aims to provide large-particle porous ceramic and a preparation method thereof, which simultaneously meet the requirements of open porosity and bending strength and reduce the sintering process conditions in a mode of matching the main material of the large-particle porous ceramic with a low-temperature adhesive and a high-temperature adhesive.
The purpose of the invention is realized by the following technical scheme: a large-particle porous ceramic comprises a main material and a bonding agent; particle diameter D of the main material50The range is 50-1500 μm; the adhesive consists of a low-temperature adhesive and a high-temperature adhesive.
Preferably, the main material is one or more of silicon carbide, corundum, zirconia, boron carbide, alumina, silicon nitride and diamond.
Preferably, the low-temperature adhesive is one or more of paraffin, polyvinyl alcohol, propolis, silica gel, emulsified paraffin and sodium lignosulfonate; the high-temperature adhesive is one or more of silicone resin 249, silica glass powder, aluminum dihydrogen phosphate, cryolite and low-temperature molten salt.
Preferably, the dosage of the adhesive is 0.2-14% of the mass of the main material.
Preferably, the large-particle porous ceramic further comprises a dispersing agent, and the using amount of the dispersing agent is 0.1-5% of the mass of the main material.
Preferably, the dispersant is one or more of sodium citrate, polyethylene glycol, acrylamide and polyacrylic acid.
Preferably, the large-particle porous ceramic further comprises a lubricant; the lubricant is one or more of molybdenum disulfide, polyethylene wax and graphite powder.
A preparation method of large-particle porous ceramic comprises the following steps:
the method comprises the following steps: weighing ceramic main materials, adhesives and other additives, and uniformly mixing to form a mixture;
step two: processing the mixture obtained in the step one to prepare a solid mixture or slurry;
step three: filling the solid mixture or slurry obtained in the step two into a mold cavity, and forming a blank body by dry powder pressing or casting molding;
step four: and (3) firing the blank obtained in the step three, degreasing at 220-350 ℃, removing glue at 440-650 ℃, and sintering and forming at 880-980 ℃ to obtain the large-particle porous ceramic.
Preferably, the solid mixture in the second step is obtained by heating paraffin to form a liquid state, uniformly mixing and then cooling, or is obtained by adding water to form slurry, uniformly mixing and then drying.
Preferably, the preparation method of the large-particle porous ceramic further comprises a third step of subjecting the solid mixture obtained in the second step to sample separation and screening granulation or spray granulation, and controlling the moisture range to be less than or equal to 1.2%.
Compared with the prior art, the invention has the beneficial effects that:
1) by the invention of50The large-particle-size ceramic particles with the range of 50-1500 mu m are used as the main material of the raw material, the technical effect of high open porosity can be achieved without refining the ceramic particles, and the limitation of the prior art on the particle size of the raw material is reduced; meanwhile, the method has no obvious requirements on the purity and impurity components of the ceramic raw material and has wide application range.
2) According to the invention, through the matching use of the large-particle-size ceramic particles, the low-temperature adhesive and the high-temperature adhesive, the bridging connection among the main materials of the large-particle-size porous ceramic is realized through low-temperature degreasing and glue removal and medium-high-temperature bonding and sintering, so that the bending strength of the obtained porous ceramic is more than or equal to 2MPa, and the open porosity is more than or equal to 95%.
3) According to the invention, by using the large-particle-size ceramic particles in combination with the low-temperature adhesive and the high-temperature adhesive, the sintering process conditions are reduced, the sintering temperature is reduced to below 1000 ℃, and the firing period is shortened.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples.
Example 1
The method comprises the following steps: weighing 1000g of particle diameter D50Has a particle diameter D of 251 μm and 500g5060 mu m of silicon carbide powder, and 100g of fully refined paraffin and 60g of silicone resin 249 are added to form a mixture;
step two: heating the mixture obtained in the step one to paraffin to form a liquid state, fully and uniformly mixing the mixture with silicon carbide particles and silicon resin 249, and cooling the mixture until the paraffin forms a solid state to form a blocky solid mixture; granulating the massive solid mixture through a 20-mesh sample sieve to obtain granulated powder;
step three: filling the granulation powder obtained in the second step into a die cavity, and pressing the dry powder with the pressure of 55kgf/cm2The size of the blank is 100mm multiplied by 20 mm;
step four: and (3) firing the green body obtained in the step three, wherein the temperature curve of the firing process is as follows: heating from room temperature at a heating rate of 2 deg.C/min to 220 deg.C for 100min, maintaining at constant temperature for 120min, and degreasing; heating at a heating rate of 3 ℃/min for 75min to 440 ℃, keeping the constant temperature for 60min, and discharging the glue; heating at a speed of 5 deg.C/min for 108-980 deg.C for 60min, and sintering; finally, cooling to room temperature along with the furnace to prepare the large-particle silicon carbide porous ceramic.
The performance detection result of the obtained large-particle silicon carbide porous ceramic is as follows:
| name (R) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 1 | 67.6 | 12.0 | 96.3 |
| Sample 2 | 68.1 | 12.1 | 96.0 |
| Sample 3 | 67.9 | 12.0 | 96.6 |
Comparative example 1
The method comprises the following steps: weighing 1000g particle diameter D50Has a particle diameter D of 251 μm and 500g5060 μm silicon carbide powder, and 100g polyvinyl alcohol (with an effective solid content of 10%), 30g sodium citrate, 10g lubricant (with an effective solid content of 40%) to form a mixture;
step two: adding a proper amount of deionized water into the mixture obtained in the step one, stirring the mixture by a stirrer to be fully and uniformly, preparing silicon carbide micro powder by adopting a spray granulation mode, sieving the silicon carbide micro powder by a 20-mesh sample sieve, and controlling the water content to be between 0.3 and 1.0 percent to prepare granulated powder;
step three: filling the granulation powder obtained in the second step into a die cavity of a dry pressing machine, pressing the dry powder, wherein the pressure is 55kgf/cm2The size of the blank is 100mm multiplied by 20 mm;
step four: and (3) firing the green body obtained in the step three, wherein the temperature curve of the firing process is as follows: heating from room temperature at a heating rate of 2 deg.C/min to 165-350 deg.C for 100min, and defatting; heating at a heating rate of 3 deg.C/min for 100min to 650 deg.C, maintaining at constant temperature for 30min, and removing gel; heating at a heating rate of 4 deg.C/min for 150-1250 deg.C, and maintaining at constant temperature for 120 min; and then heating at the speed of 2 ℃/min to 1780 ℃ for 180min, keeping the constant temperature for 180min, cooling at the speed of 6 ℃/min to 1200 ℃ for 20min, cooling with the furnace for about 720min to 100 ℃, and sintering and forming to obtain the silicon carbide fine-particle recrystallized porous ceramic.
The performance detection results of the fine-particle silicon carbide porous ceramic are as follows:
| name (R) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 1' | 61.2 | 1.1 | 78.2 |
| Sample 2' | 61.4 | 1.0 | 78.8 |
| Sample 3' | 61.0 | 1.3 | 78.6 |
Example 2
The method comprises the following steps: weighing 1000g of particle diameter D501500 μm corundum ceramics raw material, and 200g polyvinyl alcohol (PVA)1788 aqueous solution (its effective solid content is 10%), 50g boron glass powder (particle size is 60 μm), 50g polyethylene glycol (its effective solid content is 20%), 10g lubricant (Luoyangyeku YF-125, its effective solid content is 40%) to form a mixture;
step two: adding a proper amount of deionized water into the mixture obtained in the step one, and stirring the mixture by using a stirrer until the mixture is fully and uniformly formed into slurry; then placing the mixture in a resistance wire drying box with the set temperature of 70 ℃ and drying for 4 hours to form a solid mixture; granulating the solid mixture by using a 6-mesh sample sieve, placing the solid mixture in a closed container for moisture homogenization treatment, and controlling the moisture range to be 0.3-1.2% to prepare granulated powder;
step three: filling the granulation powder obtained in the step two into a die cavity, and pressing the dry powder with the pressure of 55kgf/cm2The size of the blank is 100mm multiplied by 20 mm;
step four: and C, firing the green body obtained in the step four, wherein the temperature curve of the firing process is as follows: heating from room temperature at a heating rate of 2 deg.C/min to 240 deg.C for 110min, maintaining at constant temperature for 80min, and degreasing; heating at 4 deg.C/min for 55-460 deg.C, maintaining at constant temperature for 40min, and removing gel; heating at a heating rate of 3 deg.C/min for 140min to 880 deg.C, maintaining at constant temperature for 60min, and sintering to form; and finally, cooling to room temperature along with the furnace to obtain the large-particle corundum sand porous ceramic.
The performance detection result of the large-particle corundum sand porous ceramic is as follows:
| name (R) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 4 | 42.8 | 2.4 | 95.7 |
| Sample 5 | 42.6 | 2.3 | 96.0 |
| Sample 6 | 43.0 | 2.4 | 95.8 |
Example 3
The method comprises the following steps: weighing 1000g of particle diameter D50Is 50 μmZirconia, and 157.9g of propolis (38% effective solids), 200g of aluminum dihydrogen phosphate (40% strength), 30g of sodium citrate were added to form a mixture;
step two: adding a proper amount of deionized water into the mixture obtained in the step one, stirring the mixture by using a stirrer until the mixture is fully and uniformly stirred, and then carrying out vacuum pumping treatment for 60min at room temperature under the vacuum degree of 10Pa to form slurry;
step three: guiding the slurry obtained in the step two into a gypsum mold cavity for casting molding, demolding and taking a blank, and drying the blank for 360min at 70 ℃, wherein the size of the blank is 60mm multiplied by 30 mm;
step four: and (3) firing the green body obtained in the step three, wherein the temperature curve of the firing process is as follows: heating from room temperature at a heating rate of 2 deg.C/min to 165-350 deg.C for 100min, and defatting; heating at a heating rate of 3 deg.C/min for 100min to 650 deg.C, maintaining at constant temperature for 30min, and removing gel; heating at a heating rate of 4 ℃/min for 60min to 890 ℃, keeping the constant temperature for 60min, and sintering and molding; and finally, cooling to room temperature along with the furnace to obtain the large-particle zirconia porous ceramic.
The performance detection result of the obtained large-particle zirconia porous ceramic is as follows:
| name (R) | Volume fraction (%) | Bending strength (MPa) | Open porosity (%) |
| Sample 7 | 53.0 | 3.5 | 96.8 |
| Sample 8 | 52.8 | 3.8 | 97.1 |
| Sample 9 | 53.2 | 3.9 | 97.3 |
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The large-particle porous ceramic is characterized by comprising a main material and a binder; particle diameter D of the main material50The range is 50-1500 μm; the adhesive is composed of a low temperature adhesive and a high temperature adhesive.
2. The large particle porous ceramic of claim 1, wherein the primary material is one or more of silicon carbide, corundum, zirconia, boron carbide, alumina, silicon nitride, and diamond.
3. The large particle porous ceramic of claim 1, wherein the low temperature binder is one or more of paraffin wax, polyvinyl alcohol, propolis, silica gel, emulsified paraffin wax, sodium lignosulfonate; the high-temperature adhesive is one or more of silicone resin 249, silica glass powder, aluminum dihydrogen phosphate, cryolite and low-temperature molten salt.
4. The large-particle porous ceramic of claim 3, wherein the binder is used in an amount of 0.2-14% by mass of the main material.
5. The large-particle porous ceramic of any one of claims 1 to 4, further comprising a dispersant in an amount of 0.1 to 5% by mass of the main material.
6. The large particle porous ceramic of claim 5, wherein the dispersant is one or more of sodium citrate, polyethylene glycol, acrylamide, polyacrylic acid.
7. The large particle porous ceramic of any one of claims 1 to 4, further comprising a lubricant; the lubricant is one or more of molybdenum disulfide, polyethylene wax and graphite powder.
8. The method for preparing a large-particle porous ceramic according to any one of claims 1 to 7, comprising the steps of:
the method comprises the following steps: weighing ceramic main materials, adhesives and other additives, and uniformly mixing to form a mixture;
step two: processing the mixture obtained in the step one to prepare a solid mixture or slurry;
step three: filling the solid mixture or slurry obtained in the step two into a mold cavity, and forming a blank body by dry powder pressing or casting molding;
step four: and (3) firing the blank obtained in the step three, degreasing at 220-350 ℃, removing glue at 440-650 ℃, and sintering and forming at 880-980 ℃ to obtain the large-particle porous ceramic.
9. The method for preparing large-particle porous ceramic according to claim 8, wherein the solid mixture in the second step is obtained by heating paraffin to form liquid, uniformly mixing and then cooling, or adding water to form slurry, uniformly mixing and then drying.
10. The method for preparing large-particle porous ceramics of claim 9, further comprising the step three of subjecting the solid mixture obtained in the step two to sample screening granulation or spray granulation, and controlling the moisture content to be less than or equal to 1.2%.
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| CN101671172A (en) * | 2009-10-23 | 2010-03-17 | 中南大学 | Composite binder for preparing sintered porous body of silicon carbide powder and using method thereof |
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