CN105330288A - Preparation method of zirconia microspheres - Google Patents
Preparation method of zirconia microspheres Download PDFInfo
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- CN105330288A CN105330288A CN201510629431.9A CN201510629431A CN105330288A CN 105330288 A CN105330288 A CN 105330288A CN 201510629431 A CN201510629431 A CN 201510629431A CN 105330288 A CN105330288 A CN 105330288A
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Abstract
The invention provides a preparation method of zirconia microspheres. The method includes the following main steps: (1) preparation of a Y-TZP precursor powder: with ZrOCl2.8H2O as an initial raw material, adding a Y2O3 powder and an ammonia water solution, to obtain the Y2O3 stabilized zirconia precursor powder (Y-TZP); (2) preparation of a slurry: according to a certain proportion, weighing a monomer, a crosslinking agent, a dispersing agent and deionized water, mixing and stirring, adjusting a pH value, weighing a certain weight of the Y-TZP powder, mixing uniformly, and then adding an initiator, to obtain the slurry; (3) molding: dispersing the slurry to hot methyl silicone oil, and curing the slurry into a spherical shape; and (4) calcination: drying and calcining the molded sphere blanks to obtain the stable ZrO2 ceramic microspheres. The preparation method adopts a gel-casting process, and can prepare ceramic spheres having the diameter of 0.5-2 mm and having good spherical shape and high mechanical properties.
Description
Technical field
The present invention relates to zirconia ball preparation field, be specifically related to a kind of preparation method of zirconium oxide microballoons.
Background technology
Zirconium oxide microballoons has the features such as high strength, high tenacity, high-density, high rigidity, excellent wear resistance and erosion resistance, is used widely in fields such as mechanical chemical industry, biological chemistry, medicine industries.
Gel-casting process is a kind of novel forming method.It utilizes non-punch die, adds a small amount of additive thus make ceramic size generation chemical reaction solidify in place become base substrate in slurry inside, has that setting time is adjustable, intensity is high, solid load is high, technique is simple, the advantage of near-net-shape.With the preparation method of traditional ceramics microballoon, as the technique such as spraying granulation, isostatic pressing is compared, the method cost is low, without the need to following process, be applicable to mass production.
Summary of the invention
The present invention aims to provide a kind of method preparing zirconium oxide microballoons, can prepare the Ceramic Balls of 0.5 ~ 2mm diameter, and spherical good, mechanical property is high.
In order to realize foregoing invention object, the technical scheme of the embodiment of the present invention is as follows:
Prepare a method for zirconium oxide microballoons, comprise the steps:
(1) Y-TZP precursor powder preparation: take ZrOCl28H2O as initial feed, add Y2O3 powder and ammonia soln according to a certain percentage, the zirconium white precursor powder (Y-TZP) that obtained Y2O3 is stable;
(2) Pulp preparation: take monomer, linking agent, dispersion agent and deionized water by a certain percentage, mix and blend, adjust ph, takes the Y-TZP powder of certainweight, adds initiator after mixing, obtained slip;
(3) shaping: by the methyl-silicone oil under mud dispersivity to certain temperature, slip is solidified into spherical;
(4) calcine: by shaping ball base through super-dry, the obtained stable ZrO2 ceramic microsphere of calcining.
As preferably, the ratio of described Y2O3 powder is ZrO2/Y2O3=97/3;
As preferably, described monomer is acrylamide, and linking agent is N, N '-methylene-bisacrylamide, dispersion agent is poly amic acid, and initiator is ammonium persulphate.
As preferably, the content of Y-TZP powder is 28-35%, and the content of monomer is 15-25%, and the content of linking agent is 2-3%, and the content of dispersion agent is 0.5-2%, and the content of initiator is 0.4-0.6%, and all the other are deionized water, and pH is 8-9.
As preferably, shaping temperature is 75-90 DEG C.
As preferably, calcine and carry out in chamber type electric resistance furnace, temperature is 1500-1600 DEG C, insulation 100-180min.
The present invention prepares zirconium oxide microballoons by gel injection molding and forming technology, and technique is simple, and the time is short, and efficiency is high, and cost is low, can realize near-net-shape requirement, can prepare the Ceramic Balls of 0.5 ~ 2mm diameter, and spherical good, mechanical property is high.
Embodiment
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiments are only for illustration of the present invention, its scope do not limited the present invention in any way.
Embodiment 1: a kind of method preparing zirconium oxide microballoons, comprises the steps:
(1) Y-TZP precursor powder preparation: take ZrOCl28H2O as initial feed, add Y2O3 powder and ammonia soln according to the ratio of ZrO2/Y2O3=97/3, the zirconium white precursor powder (Y-TZP) that obtained Y2O3 is stable;
(2) Pulp preparation: take 18% acrylamide monomer, 2%N, N '-methylene-bisacrylamide linking agent, 1.6% poly amic acid dispersion agent and deionized water, mix and blend, adjust ph 8-9, take the Y-TZP powder of 30%, 0.4% initiator is added, obtained slip after mixing;
(3) shaping: by mud dispersivity in the methyl-silicone oil at 85 DEG C of temperature, slip is solidified into spherical;
(4) calcine: by shaping ball base through super-dry, calcine in chamber type electric resistance furnace, calcining temperature is 1550 DEG C, insulation 120min, obtained stable ZrO2 ceramic microsphere.
Embodiment 2: a kind of method preparing zirconium oxide microballoons, comprises the steps:
(1) Y-TZP precursor powder preparation: take ZrOCl28H2O as initial feed, add Y2O3 powder and ammonia soln according to the ratio of ZrO2/Y2O3=97/3, the zirconium white precursor powder (Y-TZP) that obtained Y2O3 is stable;
(2) Pulp preparation: take 22% acrylamide monomer, 2.5%N, N '-methylene-bisacrylamide linking agent, 1.8% poly amic acid dispersion agent and deionized water, mix and blend, adjust ph 8-9, take the Y-TZP powder of 32%, 0.4% initiator is added, obtained slip after mixing;
(3) shaping: by mud dispersivity in the methyl-silicone oil at 85 DEG C of temperature, slip is solidified into spherical;
(4) calcine: by shaping ball base through super-dry, calcine in chamber type electric resistance furnace, calcining temperature is 1550 DEG C, insulation 120min, obtained stable ZrO2 ceramic microsphere.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. prepare a method for zirconium oxide microballoons, it is characterized in that, comprise the steps:
(1) Y-TZP precursor powder preparation: take ZrOCl28H2O as initial feed, proportionally add Y2O3 powder and ammonia soln, the zirconium white precursor powder (Y-TZP) that obtained Y2O3 is stable;
(2) Pulp preparation: take monomer, linking agent, dispersion agent and deionized water in proportion, mix and blend, adjust ph, takes Y-TZP powder, adds initiator after mixing, obtained slip;
(3) shaping: by mud dispersivity in methyl-silicone oil, slip is solidified into spherical;
(4) calcine: by shaping ball base through super-dry, the obtained stable ZrO2 ceramic microsphere of calcining.
2. a kind of method preparing zirconium oxide microballoons according to claim 1, is characterized in that, the ratio of described Y2O3 powder is ZrO2/Y2O3=97/3.
3. a kind of method preparing zirconium oxide microballoons according to claim 1, is characterized in that, described monomer is acrylamide, and linking agent is N, N '-methylene-bisacrylamide, dispersion agent is poly amic acid, and initiator is ammonium persulphate.
4. a kind of method preparing zirconium oxide microballoons according to claim 1, it is characterized in that, the content of Y-TZP powder is 28-35%, the content of monomer is 15-25%, the content of linking agent is 2-3%, the content of dispersion agent is 0.5-2%, and the content of initiator is 0.4-0.6%, and all the other are deionized water.
5. a kind of method preparing zirconium oxide microballoons according to claim 1, is characterized in that, shaping temperature is 75-90 DEG C.
6. a kind of method preparing zirconium oxide microballoons according to claim 1, is characterized in that, the temperature of calcining is 1500-1600 DEG C, insulation 100-180min.
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| CN201510629431.9A CN105330288A (en) | 2015-09-29 | 2015-09-29 | Preparation method of zirconia microspheres |
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| CN201510629431.9A CN105330288A (en) | 2015-09-29 | 2015-09-29 | Preparation method of zirconia microspheres |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN111302791A (en) * | 2020-02-24 | 2020-06-19 | 东莞市永笃纳米科技有限公司 | Zirconia micro-bead and preparation method thereof |
| CN112457005A (en) * | 2020-12-11 | 2021-03-09 | 景德镇陶瓷大学 | Composite preparation method of submillimeter-level zirconia ceramic microspheres |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935478A (en) * | 2006-10-16 | 2007-03-28 | 清华大学 | Method and apparatus for preparing ceramic microball by injection-condensation |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935478A (en) * | 2006-10-16 | 2007-03-28 | 清华大学 | Method and apparatus for preparing ceramic microball by injection-condensation |
Non-Patent Citations (1)
| Title |
|---|
| 李承亮等: "注凝工艺制备二氧化锆陶瓷微球", 《材料工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN107140953B (en) * | 2017-04-18 | 2019-11-22 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN111302791A (en) * | 2020-02-24 | 2020-06-19 | 东莞市永笃纳米科技有限公司 | Zirconia micro-bead and preparation method thereof |
| CN112457005A (en) * | 2020-12-11 | 2021-03-09 | 景德镇陶瓷大学 | Composite preparation method of submillimeter-level zirconia ceramic microspheres |
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