CN111233486B - Preparation method of ceramic microbeads - Google Patents
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Abstract
The invention belongs to the technical field of preparation of superfine grinding media, and particularly relates to a preparation method of ceramic microbeads. The method comprises the following steps: (1) Performing a preforming process on the ceramic powder to obtain ceramic microsphere blanks; (2) Immersing preformed ceramic microsphere blanks into a paraffin wax and organic binder high-temperature mixed solution for coating; (3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing; (4) after isostatic pressing is finished, discharging glue and sintering at high temperature; (5) And placing the ceramic microbeads sintered at high temperature and deionized water in a ball milling tank for self-polishing, thus obtaining the ceramic microbead product. The invention has the characteristics of simple and convenient production process, high production efficiency and good product performance, the compressive strength of the prepared ceramic microbeads is improved by 30%, and the abrasion loss of the microbeads is reduced by 50%.
Description
Technical Field
The invention belongs to the technical field of preparation of superfine grinding media, and particularly relates to a preparation method of ceramic microbeads.
Background
Ceramic microbeads are ceramic spheres with diameters below 5mm, and are generally prepared from nano ceramic powder serving as a main raw material through various molding processes. In recent years, with the development of nano materials, ceramic grinding media with particle diameters larger than 5mm cannot meet the requirement of superfine grinding, and the requirement of an indispensable grinding material, namely ceramic microbeads, in the production of superfine powder is increasing. Many superfine materials at home and abroad need to be subjected to superfine grinding by using ceramic microbeads, such as paint, ink, dye, polishing material, battery material, cosmetics, ceramic material and the like, and the ceramic microbeads are a necessary option in the superfine grinding of ceramic ink, lithium battery material, nano powder and other materials.
At present, the preparation process of the ceramic microbeads mainly comprises three steps of titration molding, rolling molding and spray molding. The zirconia microbeads produced by the titration molding process have high sphericity and good wear resistance, but the process is complex, and the yield and the qualification rate are greatly limited. The titration molding process generally uses acrylamide as a monomer, so that the monomer has higher toxicity and does not meet the requirements of environmental protection; in addition, the titration molding adopts a mode of dripping liquid drops into a high-viscosity oily medium for molding, the cleaning of the microsphere green body is difficult, and the production efficiency is low.
The spray forming and rolling forming process is simple and convenient in production process, and ceramic microbead products can be produced in large quantities, but high-quality ceramic microbeads are difficult to prepare. The ball blank produced by spray forming and rolling forming has a plurality of air holes, low green density and a plurality of green defects, so that the ceramic microbeads after firing have low compressive strength and are not abrasion-resistant, and if the isostatic pressing technology is adopted to improve the green defects, a large number of sheathing molds are needed, and the cost is high, the technology is complex and the labor capacity is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of ceramic microbeads, which has the characteristics of simple and convenient production process, high production efficiency and good product performance, the compressive strength of the prepared ceramic microbeads is improved by 30%, and the abrasion loss of the microbeads is reduced by 50%.
The preparation method of the ceramic microbeads comprises the following steps:
(1) Performing a preforming process on the ceramic powder to obtain ceramic microsphere blanks;
(2) Immersing preformed ceramic microsphere blanks into a paraffin wax and organic binder high-temperature mixed solution for coating; wherein, in the high-temperature mixed solution of paraffin and organic binder, the paraffin accounts for 60-92 wt% and the organic binder accounts for 8-40 wt%;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing;
(4) After isostatic pressing is finished, discharging glue and sintering at high temperature;
(5) And placing the ceramic microbeads sintered at high temperature and deionized water in a ball milling tank for self-polishing, thus obtaining the ceramic microbead product.
Wherein:
the ceramic powder is any one or more than one of zirconia, alumina, zirconium silicate or silicon nitride.
The preforming process is any one of spray forming or roll forming.
The temperature of the paraffin wax and the organic binder high-temperature mixed solution is 70-80 ℃.
The paraffin is any one or more than one of refined paraffin, semi-refined paraffin or crude paraffin.
The organic binder is selected from one or more of high-density polyethylene, low-density polyethylene, ethylene-vinyl acetate copolymer, random polypropylene or polypropylene.
The temperature of the temperature isostatic pressing equipment is set to be 40-60 ℃ and the pressure is 100-300 MPa.
The glue discharging is to heat-insulating at 500-600 ℃ for 1-4 hours, the heating rate is 10-40 ℃/h.
The high-temperature sintering temperature is 1400-1600 ℃, the heating rate is 120-180 ℃/h, and the heat preservation time is 1-4 h.
The mass ratio of the ceramic microbeads after high-temperature sintering to deionized water is 1:1.2.
the ceramic microbead product is a ceramic sphere with the diameter below 5 mm.
The beneficial effects of the invention are as follows:
1. according to the invention, the ceramic microsphere green body is coated by the paraffin and organic binder high-temperature mixed solution, and isostatic pressing of the ceramic microsphere green body can be realized without using a flexible sheath die, so that the problem that the spray forming and rolling forming processes are difficult to prepare the high-quality ceramic microsphere is solved.
2. The paraffin and organic binder mixed solution adopted by the invention is fluid at high temperature and is solidified and coated at low temperature, the ceramic microsphere blank is immersed in the paraffin and organic binder mixed solution at high temperature and can be quickly taken out, and after the ceramic microsphere blank is cooled in air, a layer of paraffin and organic binder film can be coated, and the film is easy to burn and lose and does not influence degreasing and sintering of the ceramic microsphere blank at later stage.
3. The invention adopts the warm isostatic pressing equipment to press the ceramic microsphere blank, the paraffin and the organic binder film are hard and brittle at the temperature below 40 ℃ and are not pressure-resistant, and can melt at the temperature above 60 ℃, but the ceramic microsphere blank has better flexibility in warm water solution at the temperature of 40-60 ℃, can isolate moisture and bear higher pressure, and is very suitable for being used as a pressure-bearing film for the isostatic pressing of ceramic microspheres.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples.
Example 1
(1) Rolling and forming 3mol of yttrium-stabilized zirconia powder to obtain ceramic microsphere blanks, wherein the content of yttrium oxide in the 3mol of yttrium-stabilized zirconia powder accounts for 3mol percent, and the content of zirconium oxide accounts for 97mol percent;
(2) Immersing the rolled ceramic microsphere blank into 80 # microcrystalline paraffin and ethylene-vinyl acetate copolymer high-temperature mixed solution for coating, wherein the 80 # microcrystalline paraffin and ethylene-vinyl acetate copolymer high-temperature mixed solution comprises 92wt% of microcrystalline paraffin, 8wt% of ethylene-vinyl acetate copolymer and the temperature of the mixed solution is 70 ℃;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing, wherein the temperature of the warm isostatic pressing device is set to be 50 ℃ and the pressure is set to be 150MPa;
(4) And after isostatic pressing, performing glue discharging and high-temperature sintering, wherein the glue discharging is performed by heat preservation at 500 ℃ for 4 hours, the heating rate is 20 ℃/h, the high-temperature sintering temperature is 1450 ℃, the heating rate is 120 ℃/h, and the heat preservation time is 2h.
(5) And (3) placing the ceramic microbeads sintered at high temperature and deionized water (the mass ratio is 1:1.2) in a ball milling tank for self-counter grinding and polishing to obtain ceramic microbead products with diameters below 5mm and excellent performances, wherein the specific performances are shown in Table 1.
The compressive strength of the zirconia ceramic microbeads is tested by adopting a compressive strength tester, the compactness of the zirconia ceramic microbeads is tested by adopting an Archimedes drainage method, the hardness of the zirconia ceramic microbeads is tested by adopting an indentation method, and the wear resistance of the zirconia ceramic microbeads is tested by adopting a grinding method.
Weighing 5kg of zirconia microbeads, putting the zirconia microbeads into a 2.5L sand mill, rotating the sand mill at 1200 revolutions, ball milling for 24 hours, cleaning, drying, weighing the weight of the microbeads after ball milling, subtracting the weight of the microbeads after ball milling from the weight of the microbeads before ball milling to obtain the loss weight of the microbeads, and dividing the loss weight of the microbeads by the kg number of the microbeads before ball milling and the ball milling time to obtain the average wear amount of the microbeads per hour.
Example 2
(1) Spraying 5mol of cerium stabilized zirconia powder to obtain a ceramic microsphere blank, wherein the content of cerium oxide in the 5mol of cerium stabilized zirconia powder is 5mol percent, and the content of zirconium oxide is 95mol percent;
(2) Immersing the spray-formed ceramic microsphere blank into a high-temperature mixed solution of 80 # microcrystalline paraffin and low-density polyethylene for coating, wherein the microcrystalline paraffin accounts for 85wt% in the high-temperature mixed solution of 80 # microcrystalline paraffin and low-density polyethylene, the low-density polyethylene accounts for 15wt% and the temperature of the mixed solution is 80 ℃;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing, wherein the temperature of the warm isostatic pressing device is set to be 60 ℃ and the pressure is set to be 300MPa;
(4) And after isostatic pressing, performing glue discharging and high-temperature sintering, wherein the glue discharging is performed by heat preservation at 550 ℃ for 3 hours, the heating rate is 40 ℃/h, the high-temperature sintering temperature is 1500 ℃, the heating rate is 120 ℃/h, and the heat preservation time is 4h.
(5) And (3) placing the ceramic microbeads sintered at high temperature and deionized water (the mass ratio is 1:1.2) in a ball milling tank for self-opposite grinding and polishing to obtain ceramic microbead products with diameters below 5mm and excellent performances, wherein the specific performances are shown in Table 1.
Example 3
(1) Rolling and forming 92 ceramic alumina powder to obtain ceramic microsphere blanks, wherein the content of alumina in the 92 ceramic alumina accounts for 92wt%;
(2) Immersing the rolled ceramic microsphere blank into a high-temperature mixed solution of 80 # microcrystalline paraffin and low-density polyethylene for coating, wherein the microcrystalline paraffin in the high-temperature mixed solution of 80 # microcrystalline paraffin and low-density polyethylene accounts for 85wt%, the low-density polyethylene accounts for 15wt%, and the temperature of the mixed solution is 80 ℃;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing, wherein the temperature of the warm isostatic pressing device is set to be 60 ℃ and the pressure is set to be 100MPa;
(4) And after isostatic pressing, performing glue discharging and high-temperature sintering, wherein the glue discharging is performed by heat preservation at 530 ℃ for 1 hour, the heating rate is 10 ℃/h, the high-temperature sintering temperature is 1550 ℃, the heating rate is 180 ℃/h, and the heat preservation time is 2h.
(5) And (3) placing the ceramic microbeads sintered at high temperature and deionized water (1:1.2) in a ball milling tank for self-polishing to obtain ceramic microbead products with diameters below 5mm and excellent performances, wherein the specific performances are shown in Table 1.
Example 4
(1) Rolling and forming the silicon nitride powder to obtain ceramic microsphere blanks;
(2) Immersing the rolled ceramic microsphere blank into a high-temperature mixed solution of 80 # microcrystalline paraffin, low-density polyethylene and polypropylene for coating, wherein the microcrystalline paraffin in the high-temperature mixed solution of 80 # microcrystalline paraffin, low-density polyethylene and polypropylene accounts for 85wt%, the low-density polyethylene accounts for 5wt%, the polypropylene accounts for 10wt%, and the temperature of the mixed solution is 80 ℃;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing, wherein the temperature of the warm isostatic pressing device is set to be 50 ℃ and the pressure is 220MPa;
(4) After isostatic pressing, performing glue discharging and high-temperature sintering, wherein the glue discharging is to perform glue discharging treatment at 600 ℃ for 2 hours, the heating rate is 30 ℃/h, then the temperature is continuously raised to 800 ℃, and the temperature is naturally lowered to the room temperature;
(5) And after the glue is discharged, hot-pressing sintering is carried out under the nitrogen atmosphere, wherein the temperature is 1600 ℃, the heating rate is 180 ℃/h, the heat preservation time is 2h, and the pressure is 100T.
(6) And (3) placing the ceramic microbeads sintered at high temperature and deionized water (1:1.2) in a ball milling tank for self-polishing to obtain ceramic microbead products with diameters below 5mm and excellent performances, wherein the specific performances are shown in Table 1.
TABLE 1 physical Properties of ceramic microbeads
Claims (6)
1. A preparation method of ceramic microbeads is characterized in that: the method comprises the following steps:
(1) Performing a preforming process on the ceramic powder to obtain ceramic microsphere blanks;
(2) Immersing preformed ceramic microsphere blanks into a paraffin wax and organic binder high-temperature mixed solution for coating; wherein, in the high-temperature mixed solution of paraffin and organic binder, the paraffin accounts for 60-92 wt% and the organic binder accounts for 8-40 wt%;
(3) Taking out the coated ceramic microsphere blank, and placing the ceramic microsphere blank in a warm isostatic pressing device for isostatic pressing;
(4) After isostatic pressing is finished, discharging glue and sintering at high temperature;
(5) Placing the ceramic microbeads sintered at high temperature and deionized water in a ball milling tank for self-polishing, thus obtaining ceramic microbead products;
the paraffin is any one or more than one mixture of fully refined paraffin, semi-refined paraffin or crude paraffin;
the organic binder is selected from any one or more than one of high-density polyethylene, low-density polyethylene, ethylene-vinyl acetate copolymer or polypropylene;
the temperature of the temperature isostatic pressing equipment is set to be 40-60 ℃ and the pressure is 100-300 MPa;
the temperature of the paraffin wax and the organic binder high-temperature mixed solution is 70-80 ℃.
2. The method for preparing ceramic microbeads according to claim 1, wherein: the ceramic powder is any one or more than one of zirconia, alumina, zirconium silicate or silicon nitride.
3. The method for preparing ceramic microbeads according to claim 1, wherein: the preforming process is any one of spray forming or roll forming.
4. The method for preparing ceramic microbeads according to claim 1, wherein: the glue discharging is to heat-insulating at 500-600 ℃ for 1-4 hours, the heating rate is 10-40 ℃/h.
5. The method for preparing ceramic microbeads according to claim 1, wherein: the high-temperature sintering temperature is 1400-1600 ℃, the heating rate is 120-180 ℃/h, and the heat preservation time is 1-4 h.
6. The method for preparing ceramic microbeads according to claim 1, wherein: the ceramic microbead product is a ceramic sphere with the diameter below 5 mm.
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| CN111807832A (en) * | 2020-06-24 | 2020-10-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of indium tin oxide grinding ball |
| CN111825435A (en) * | 2020-07-30 | 2020-10-27 | 苏州贝尔德新材料科技有限公司 | Preparation method of wear-resistant high-purity alumina grinding ball |
| CN112694321B (en) * | 2020-12-19 | 2022-08-02 | 安徽致磨新材料科技有限公司 | High-strength superfine grinding medium and preparation method thereof |
| CN115849919B (en) * | 2022-12-12 | 2024-04-05 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
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