CN111233486A - Preparation method of ceramic microspheres - Google Patents
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Abstract
The invention belongs to the technical field of superfine grinding medium preparation, and particularly relates to a preparation method of ceramic microspheres. The method comprises the following steps: (1) performing a pre-forming process on the ceramic powder to obtain a ceramic microbead spherical blank; (2) immersing the preformed ceramic microbead spherical blank into a high-temperature mixed solution of paraffin and an organic binder for coating; (3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball blank in a warm isostatic pressing device for isostatic pressing; (4) after isostatic pressing, carrying out binder removal and high-temperature sintering; (5) and placing the ceramic microspheres sintered at high temperature and deionized water into a ball milling tank for self-pairing grinding and polishing to obtain the ceramic microsphere 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 microspheres is improved by 30 percent, and the abrasion loss of the microspheres is reduced by 50 percent.
Description
Technical Field
The invention belongs to the technical field of superfine grinding medium preparation, and particularly relates to a preparation method of ceramic microspheres.
Background
The ceramic microspheres refer to ceramic spheres with the diameter of less than 5mm, and are generally prepared by taking nano ceramic powder as a main raw material through various forming processes. In recent years, with the development of nano materials, ceramic grinding media with particle size larger than 5mm cannot meet the requirement of superfine grinding, and the requirement of ceramic microspheres, which are indispensable grinding materials 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 microspheres, such as paint, printing ink, dye, polishing material, battery material, cosmetics, ceramic material and the like, and particularly in the superfine grinding of materials such as ceramic ink, lithium battery material, nano powder and the like, the ceramic microspheres are inevitable options.
At present, the preparation process of the ceramic microspheres mainly comprises three types, namely titration forming, rolling forming and spray forming. The zirconia micro-beads produced by the titration forming 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 forming process generally takes acrylamide as a monomer, and the monomer has high toxicity and does not meet the requirement of environmental protection; in addition, the titration forming adopts a mode of dripping liquid drops into a high-viscosity oily medium for forming, the cleaning of the microbead green compact is difficult, and the production efficiency is not high.
The spray forming and rolling forming process has simple production process, can produce ceramic micro bead products in large scale, but is difficult to prepare high-quality ceramic micro beads. The ball blank produced by spray forming and roll forming has many pores, low density of the green blank and many defects of the green blank, so that the sintered ceramic micro-bead has low compressive strength and no wear loss.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the preparation method of the ceramic microspheres, which has the characteristics of simple and convenient production process, high production efficiency and good product performance, the compressive strength of the prepared ceramic microspheres is improved by 30 percent, and the abrasion loss of the microspheres is reduced by 50 percent.
The preparation method of the ceramic microspheres comprises the following steps:
(1) performing a pre-forming process on the ceramic powder to obtain a ceramic microbead spherical blank;
(2) immersing the preformed ceramic microbead spherical blank into a high-temperature mixed solution of paraffin and an organic binder for coating; in the paraffin and organic binder high-temperature mixed solution, the paraffin accounts for 60-92 wt%, and the organic binder accounts for 8-40 wt%;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball blank in a warm isostatic pressing device for isostatic pressing;
(4) after isostatic pressing, carrying out binder removal and high-temperature sintering;
(5) and placing the ceramic microspheres sintered at high temperature and deionized water into a ball milling tank for self-pairing grinding and polishing to obtain the ceramic microsphere product.
Wherein:
the ceramic powder is any one or a mixture of more than one of zirconia, alumina, zirconium silicate or silicon nitride.
The preforming process is any one of spray forming or rolling forming.
The temperature of the paraffin and organic binder high-temperature mixed solution is 70-80 ℃.
The paraffin is any one or mixture of more than one of fully refined paraffin, semi-refined paraffin or crude paraffin.
The organic binder is selected from any one or a mixture of more than one of high-density polyethylene, low-density polyethylene, ethylene-vinyl acetate copolymer, random polypropylene or polypropylene.
The temperature of the warm isostatic pressing equipment is set to be 40-60 ℃, and the pressure is 100-300 MPa.
The glue discharging is carried out by heat preservation for 1-4 hours at 500-600 ℃, and 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 microspheres sintered at high temperature to the deionized water is 1: 1.2.
the ceramic micro-bead product is a ceramic sphere with the diameter of less than 5 mm.
The invention has the following beneficial effects:
1. according to the invention, the ceramic microbead green compact is coated by the paraffin and organic binder high-temperature mixed solution, and isostatic pressing of the ceramic microbead green compact can be realized without using a flexible sheathing die, so that the problem of pain of difficult preparation of high-quality ceramic microbeads by spray forming and roll forming processes is solved.
2. The paraffin and organic binder high-temperature mixed solution adopted by the invention is fluid at high temperature, and is solidified and coated at low temperature, the ceramic microbead spherical blank can be quickly taken out after being immersed in the paraffin and organic binder high-temperature mixed solution, and can be coated with a layer of paraffin and organic binder film after being cooled in air, the film is easy to burn out, and the degreasing and sintering of the ceramic microbead spherical blank at the later stage can not be influenced.
3. According to the invention, a warm isostatic pressing device is adopted to press the ceramic microbead blank, the paraffin and the organic binder film are hard and brittle at the temperature below 40 ℃ and are not pressure-resistant, the paraffin and the organic binder film can melt at the temperature above 60 ℃, but the paraffin and the organic binder film have good flexibility in a warm aqueous solution at the temperature of 40-60 ℃, can isolate moisture and bear high pressure, and are very suitable for being used as a pressure-bearing film for ceramic microbead isostatic pressing.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples.
Example 1
(1) Rolling and molding 3mol of yttrium-stabilized zirconia powder to obtain a ceramic microbead ball blank, wherein the content of yttrium oxide in the 3mol of yttrium-stabilized zirconia powder accounts for 3 mol%, and the content of zirconium oxide accounts for 97 mol%;
(2) immersing a roll-formed ceramic microbead ball blank into a No. 80 microcrystalline paraffin and ethylene-vinyl acetate copolymer high-temperature mixed solution for coating, wherein in the No. 80 microcrystalline paraffin and ethylene-vinyl acetate copolymer high-temperature mixed solution, the microcrystalline paraffin accounts for 92 wt%, the ethylene-vinyl acetate copolymer accounts for 8 wt%, and the temperature of the mixed solution is 70 ℃;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball 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 150 MPa;
(4) and (3) 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 2 h.
(5) Placing the ceramic microspheres sintered at high temperature and deionized water (mass ratio is 1:1.2) in a ball milling tank for self-pairing grinding and polishing to obtain ceramic microsphere products with the diameter of less than 5mm and excellent performance, wherein the specific performance is shown in table 1.
The compression strength of the zirconia ceramic microspheres is tested by adopting a compression strength tester, the density of the zirconia ceramic microspheres is tested by adopting an Archimedes drainage method, the hardness of the zirconia ceramic microspheres is tested by adopting an indentation method, and the wear resistance of the zirconia ceramic microspheres is tested by adopting a grinding method.
Weighing 5kg of zirconia micro-beads, putting the zirconia micro-beads into a 2.5L sand mill, rotating the sand mill at 1200 revolutions, performing ball milling for 24 hours, cleaning, drying, weighing the weight of the micro-beads after ball milling, subtracting the weight of the micro-beads after ball milling from the weight of the micro-beads before ball milling to obtain the weight loss of the micro-beads, and dividing the weight loss of the micro-beads by the number of kilograms of micro-beads before ball milling and the ball milling time to obtain the average wear loss of each kilogram of micro-beads per hour.
Example 2
(1) Carrying out spray forming on 5mol of cerium-stabilized zirconia powder to obtain a ceramic microbead ball blank, wherein the cerium oxide content in the 5mol of cerium-stabilized zirconia powder accounts for 5 mol%, and the zirconium oxide content accounts for 95 mol%;
(2) immersing a ceramic microbead ball blank subjected to spray forming into a high-temperature mixed solution of No. 80 microcrystalline paraffin and low-density polyethylene for coating, wherein the microcrystalline paraffin accounts for 85 wt% of the high-temperature mixed solution of the No. 80 microcrystalline paraffin and the low-density polyethylene, the low-density polyethylene accounts for 15 wt%, and the temperature of the mixed solution is 80 ℃;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball 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 300 MPa;
(4) and (3) 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 4 h.
(5) Placing the ceramic microspheres sintered at high temperature and deionized water (mass ratio is 1:1.2) in a ball milling tank for self-pairing grinding and polishing to obtain ceramic microsphere products with the diameter of less than 5mm and excellent performance, wherein the specific performance is shown in Table 1.
Example 3
(1) Rolling and molding the 92 porcelain alumina powder to obtain a ceramic microbead ball blank, wherein the content of alumina in the 92 porcelain alumina accounts for 92 wt%;
(2) immersing a ceramic microbead ball blank which is formed by rolling into a high-temperature mixed solution of No. 80 microcrystalline paraffin and low-density polyethylene for coating, wherein the microcrystalline paraffin accounts for 85 wt% of the high-temperature mixed solution of the No. 80 microcrystalline paraffin and the low-density polyethylene accounts for 15 wt%, and the temperature of the mixed solution is 80 ℃;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball 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 100 MPa;
(4) and (3) after isostatic pressing, carrying out glue discharging and high-temperature sintering, wherein the glue discharging is carried out 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 2 h.
(5) Ceramic microspheres sintered at high temperature and deionized water (1:1.2) are placed in a ball milling tank for self-pairing grinding and polishing, and ceramic microsphere products with the diameter of less than 5mm and excellent performance can be prepared, wherein the specific performance is shown in table 1.
Example 4
(1) Rolling and molding the silicon nitride powder to obtain a ceramic microbead spherical blank;
(2) immersing the roll-formed ceramic microbead ball blank into a high-temperature mixed solution of No. 80 microcrystalline paraffin, low-density polyethylene and polypropylene for coating, wherein the microcrystalline paraffin accounts for 85 wt%, the low-density polyethylene accounts for 5 wt% and the polypropylene accounts for 10 wt% of the high-temperature mixed solution of No. 80 microcrystalline paraffin, low-density polyethylene and polypropylene, and the temperature of the mixed solution is 80 ℃;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball 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 220 MPa;
(4) after isostatic pressing, carrying out glue discharging and high-temperature sintering, wherein the glue discharging is carried out by keeping the temperature at 600 ℃ for 2 hours at the heating rate of 30 ℃/h, then continuously heating to 800 ℃, and naturally cooling to room temperature;
(5) and after the glue discharging is finished, carrying out hot-pressing sintering in a 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) Ceramic microspheres sintered at high temperature and deionized water (1:1.2) are placed in a ball milling tank for self-pairing grinding and polishing, and ceramic microsphere products with the diameter of less than 5mm and excellent performance can be prepared, wherein the specific performance is shown in table 1.
TABLE 1 physical Properties of ceramic Microbeads
Claims (10)
1. A preparation method of ceramic microspheres is characterized by comprising the following steps: the method comprises the following steps:
(1) performing a pre-forming process on the ceramic powder to obtain a ceramic microbead spherical blank;
(2) immersing the preformed ceramic microbead spherical blank into a high-temperature mixed solution of paraffin and an organic binder for coating; in the paraffin and organic binder high-temperature mixed solution, the paraffin accounts for 60-92 wt%, and the organic binder accounts for 8-40 wt%;
(3) taking out the coated ceramic microsphere ball blank, and placing the ceramic microsphere ball blank in a warm isostatic pressing device for isostatic pressing;
(4) after isostatic pressing, carrying out binder removal and high-temperature sintering;
(5) and placing the ceramic microspheres sintered at high temperature and deionized water into a ball milling tank for self-pairing grinding and polishing to obtain the ceramic microsphere product.
2. The method for producing ceramic microbeads according to claim 1, characterized in that: the ceramic powder is any one or a mixture of more than one of zirconia, alumina, zirconium silicate or silicon nitride.
3. The method for producing ceramic microbeads according to claim 1, characterized in that: the preforming process is any one of spray forming or rolling forming.
4. The method for producing ceramic microbeads according to claim 1, characterized in that: the temperature of the paraffin and organic binder high-temperature mixed solution is 70-80 ℃.
5. The method for producing ceramic microbeads according to claim 1, characterized in that: the paraffin is any one or mixture of more than one of fully refined paraffin, semi-refined paraffin or crude paraffin.
6. The method for producing ceramic microbeads according to claim 1, characterized in that: the organic binder is selected from any one or a mixture of more than one of high-density polyethylene, low-density polyethylene, ethylene-vinyl acetate copolymer, random polypropylene or polypropylene.
7. The method for producing ceramic microbeads according to claim 1, characterized in that: the temperature of the warm isostatic pressing equipment is set to be 40-60 ℃, and the pressure is 100-300 MPa.
8. The method for producing ceramic microbeads according to claim 1, characterized in that: the glue discharging is carried out by heat preservation for 1-4 hours at 500-600 ℃, and the heating rate is 10-40 ℃/h.
9. The method for producing ceramic microbeads according to claim 1, characterized in that: the high-temperature sintering temperature is 1400-1600 ℃, the heating rate is 120-180 ℃/h, and the heat preservation time is 1-4 h.
10. The method for producing ceramic microbeads according to claim 1, characterized in that: the ceramic micro-bead product is a ceramic sphere with the diameter of less than 5 mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112694321A (en) * | 2020-12-19 | 2021-04-23 | 安徽致磨新材料科技有限公司 | High-strength superfine grinding medium and preparation method thereof |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application thereof |
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| 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 |
| CN112694321A (en) * | 2020-12-19 | 2021-04-23 | 安徽致磨新材料科技有限公司 | High-strength superfine grinding medium and preparation method thereof |
| CN115849919A (en) * | 2022-12-12 | 2023-03-28 | 广东技术师范大学 | High-performance silicon nitride conductive ceramic and preparation method and application 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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