CN110835263A - Method for preparing zirconia ceramic microspheres - Google Patents
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Abstract
A method for preparing zirconia ceramic microspheres comprises the steps of dripping zirconia slurry prepared by mixing zirconia powder, deionized water and an auxiliary agent into an oily medium through a titration device to form zirconia microspheres, then separating the zirconia microspheres, degreasing and sintering to prepare the zirconia ceramic microspheres, mixing a binder capable of being solidified under the action of a cross-linking agent into the zirconia slurry, dripping the zirconia slurry into the oily medium mixed with the cross-linking agent, and enabling the binder in the zirconia slurry liquid drops to react with the cross-linking agent to be solidified to form the zirconia microspheres. The problems of high operation difficulty and the like caused by the fact that the binder and the cross-linking agent are contacted in advance are solved, the process complexity is greatly reduced, the zirconium oxide microsphere blank is ensured, the subsequent operations of separation, drying, transportation, degreasing and the like are facilitated, and the yield and the quality of a final product are ensured.
Description
Technical Field
The invention relates to a preparation method of a ceramic material, in particular to a method for preparing zirconia ceramic microspheres.
Background
Y2O3Stabilized zirconia ceramicsThe ceramic microspheres have the characteristics of good chemical stability and mechanical strength, so that the ceramic microspheres are widely applied to the fields of grinding dispersion, biochemistry, medical industry and the like of high-added-value ceramics with high requirements on product purity, and have good development prospects. Meanwhile, due to the further improvement of the requirements of various industries on the granularity and the depolymerization degree of the ceramic powder, the requirements on the wear resistance and the strength of the zirconia grinding medium ball with the diameter size of less than 1 μm are increasingly urgent. The existing preparation methods of the zirconia microspheres with the diameter of less than 1 μm mainly comprise a rolling method, a spraying method, an extrusion molding method and the like, but the preparation processes are difficult to simultaneously meet the requirements of high sphericity, high wear resistance, size uniformity and low cost of the zirconia microspheres. At present, the method of titration forming is also proposed to form a microsphere blank, but the preparation process has various defects.
CN1241876C discloses a method and an apparatus for preparing ceramic pellets, which comprises mixing organic monomers, cross-linking agent, water and ceramic powder to make slurry, and then dropping into heated oily medium to make ceramic microspheres. However, this method requires mixing the organic monomer, the crosslinking agent and the initiator in advance in preparing the slurry. Due to the mixing of the cross-linking agent and the initiator, it is difficult to ensure that the organic monomer is completely dropped into the oily medium before cross-linking and curing. The requirements on process conditions and operation are high, the operation difficulty is high, the complexity is high, and the quality of a final product is even affected.
CN102303305A discloses a method and an apparatus for forming ceramic microbead green compact, which abandons the use of organic monomer and cross-linking agent, uses polyacrylic acid as binder, and uses ammonium citrate. This method, although avoiding the problem of the complicated operation of CN1241876C, correspondingly loses the benefits of the organic monomer and the cross-linking agent. Although polyacrylic acid can act as a binder to aggregate and bond ceramic powder, the polyacrylic acid has poor binding property, is not beneficial to subsequent operation of ceramic microsphere green bodies, and cannot ensure the quality of final ceramic microsphere products.
CN106830927A discloses a method for preparing zirconia ceramic microspheres by titration molding, which comprises the steps of mixing ceramic powder with hot-melted mixed glue, and forming ceramic microsphere green bodies by air cooling and shaping in the process of dripping by utilizing titration equipment. Because the cooling and solidification of the microbeads are carried out in the air, the gob is stretched to a certain degree in the vertical direction under the action of gravity traction, and the sphericity is difficult to guarantee.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and provide a method for preparing zirconia ceramic microspheres.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing zirconia ceramic microspheres comprises the steps of dripping zirconia slurry prepared by mixing zirconia powder, deionized water and an auxiliary agent into an oily medium through a titration device to form zirconia microspheres, then separating the zirconia microspheres, degreasing and sintering to prepare the zirconia ceramic microspheres, mixing a binder capable of being solidified under the action of a cross-linking agent into the zirconia slurry, dripping the zirconia slurry into the oily medium mixed with the cross-linking agent, and enabling the binder in the zirconia slurry liquid drops to react with the cross-linking agent to be solidified to form the zirconia microspheres.
The binder is polyvinyl alcohol, and the dosage of the binder is 1.5-3% of the weight of the zirconia powder.
The polymerization degree of the polyvinyl alcohol is 2000-3000.
The cross-linking agent is boric acid, and the dosage of the boric acid is 15-20% of the weight of the oily medium.
The auxiliary agent comprises a dispersing agent, wherein the dispersing agent is one of ammonium polycarboxylate, ammonium acrylate, ammonium citrate and sodium hexametaphosphate, and the addition amount of the dispersing agent is 0.5-1.5% of the weight of the zirconia powder.
The auxiliary agent comprises an organic reinforcing agent.
The organic reinforcing agent is cotton fiber, and the adding amount of the organic reinforcing agent is 0.3-0.6% of the weight of the zirconia powder.
The zirconia powder is Y2O3The preparation method of the stable zirconia powder comprises the following steps: with ZrOCl2·8H2O as a raw material, according to ZrO formed after calcination2/Y2O3Is 97: 3 ratio of Y (NO)3)3·6H2O and ammonia water, and drying the precipitate to obtain Y2O3Calcining the precursor powder at 1000-1100 ℃ to obtain Y2O3Stabilized zirconia powder.
The solid content of the prepared zirconia ceramic slurry is 70-75%.
And (3) carrying out microwave drying on the separated zirconium oxide microspheres for 1-2 h at the temperature of 150-200 ℃, then transferring the zirconium oxide microspheres into a muffle furnace, and carrying out heat preservation for 2-3 h at the temperature of 600-700 ℃ to finish degreasing.
And (3) preserving the heat of the degreased zirconia microspheres for 2-5 hours at 1400-1550 ℃, and sintering to obtain the zirconia ceramic microspheres.
The invention has the beneficial effects that: the binder and the cross-linking agent are respectively mixed in the zirconia slurry and the oily medium, and contact reaction is carried out only after the liquid drops fall into the oily medium, so that the problems of high operation difficulty and the like caused by the early contact of the binder and the cross-linking agent are solved, the process complexity is greatly reduced, the equipment cost is low, the working procedures are few, and the efficiency is high. Meanwhile, the zirconium oxide microspheres are cured by matching the binder and the cross-linking agent, so that the zirconium oxide microsphere blank is ensured, the subsequent operations of separation, drying, transportation, degreasing and the like are facilitated, and the yield and the quality of final products are ensured.
Detailed Description
The following examples are provided to specifically describe embodiments of the present invention.
The preparation method of the zirconia ceramic microspheres comprises the steps of mixing zirconia powder with deionized water and an auxiliary agent to prepare zirconia slurry, mixing and stirring the deionized water, the binder and the dispersing agent in proportion to prepare a premixed solution, and adding an organic reinforcing agent according to needs to increase the strength. And adding the zirconia powder into the premixed solution to prepare zirconia slurry through a nanosphere mill, wherein the zirconia powder can be added in times in the process.
The zirconia powder selects Y2O3The preparation method of the stable zirconia powder comprises the following steps: with ZrOCl2·8H2O is used as raw material and is calcinedZrO formed after2/Y2O3Is 97: 3 ratio of Y (NO)3)3·6H2O and ammonia water, and drying the precipitate to obtain Y2O3Calcining the precursor powder at 1000-1100 ℃ to obtain Y2O3Stabilized zirconia powder.
The auxiliary agent is a dispersant and an organic reinforcing agent. The dispersant is selected from one of ammonium polycarboxylate, ammonium acrylate, ammonium citrate and sodium hexametaphosphate, and the addition amount of the dispersant is 0.5-1.5 percent of the weight of the zirconia powder. The organic reinforcing agent is a reinforcing agent such as cotton fiber, and the adding amount of the organic reinforcing agent is 0.3-0.6% of the weight of the zirconia powder.
The binder can be solidified under the action of a cross-linking agent, and polyvinyl alcohol (PVA) with the polymerization degree of 2000-3000 is selected, and the dosage of the PVA is 1.5-3% of the weight of the zirconia powder. The solid content of the prepared zirconia ceramic slurry is 70-75%.
And filling the zirconia slurry prepared by mixing into a titration apparatus, wherein the titration forming equipment comprises a dispenser, an air compressor and a micro-injector nozzle. The size of the microsphere product is controlled by adjusting the aperture of the spray head. And dropping the zirconia slurry into an oily medium such as silicone oil containing 15-20% of a cross-linking agent through a titration device. The cross-linking agent is boric acid, the slurry liquid drops are solidified through the cross-linking reaction of polyvinyl alcohol and boric acid, and simultaneously, the slurry liquid drops are sunk to the bottom of a collecting device containing silicon oil, and a dry blank of the zirconia microspheres is prepared.
And washing the collected dry zirconium oxide microsphere blank, performing microwave drying for 1-2 h at the temperature of 150-200 ℃, transferring to a muffle furnace, and preserving heat for 2-3 h at the temperature of 600-700 ℃ to finish degreasing. And (3) preserving the heat of the degreased zirconia microspheres for 2-5 hours at 1400-1550 ℃, and sintering to obtain the zirconia ceramic microspheres. The zirconia ceramic microspheres are rough blanks, the rough blanks are subjected to wet self-grinding for 20-40 hours in a roller ball mill, and polishing treatment is carried out to obtain zirconia ceramic microsphere finished products, wherein the density of the ceramic microspheres reaches 6.050-6.055 g/cm3(relative density 99.67-99.75%).
Example 1
A method of preparing zirconia ceramic microspheres comprising the steps of:
with ZrOCl2·8H2O as starting material, according to ZrO2/Y2O3Is 97: 3 ratio of ammonia to Y (NO)3)3·6H2O, calcining the precursor powder at 1000 ℃ to obtain Y2O3Stabilized zirconia powder; according to the proportion of relative powder raw materials, respectively adding 1% of dispersant ammonium acrylate, 3% of binder PVA and 0.5% of cotton fiber reinforcing agent, uniformly mixing with deionized water to obtain a premixed solution, and preparing zirconia slurry with the solid content of 70% by adopting a nanosphere mill by adopting a 3-time feeding technology; transferring the zirconia slurry into a micro-injector nozzle container, boosting compressed air by a motor of a dispenser, and dripping the slurry in the nozzle into silicone oil mixed with 15% boric acid in advance by the generated extrusion force to realize curing molding; washing the zirconium oxide spherical blank collected at the bottom, drying the zirconium oxide spherical blank by microwave for 1h at the temperature of 150 ℃, transferring the zirconium oxide spherical blank to a muffle furnace, preserving the temperature at 600 ℃ for 2h, completely degreasing the zirconium oxide spherical blank, and sintering the degreased spherical blank for 5h at the temperature of 1550 ℃ to obtain a zirconium oxide ceramic microsphere rough blank; finally, carrying out wet self-grinding on the microsphere rough blank in a roller ball mill for 20h for polishing treatment to obtain a finished product of zirconia ceramic microspheres; the density of the prepared ceramic microspheres reaches 6.055g/cm3(relative density 99.75%) and has the characteristics of good sphericity, uniform size and high wear resistance.
Example 2
A method of preparing zirconia ceramic microspheres comprising the steps of:
with ZrOCl2·8H2O as starting material, according to ZrO2/Y2O3Is 97: 3 ratio of ammonia to Y (NO)3)3·6H2O, calcining the precursor powder at 1100 ℃ to prepare Y2O3Stabilized zirconia powder; according to the proportion of relative powder raw materials, respectively adding 1.5% of dispersant ammonium polycarboxylate, 1.5% of binder PVA and 0.3% of cotton fiber reinforcing agent, uniformly mixing with deionized water to obtain a premixed solution, and preparing zirconia slurry with the solid content of 75% by adopting a nanosphere mill by adopting a 3-time feeding technology; transferring the zirconia slurry into a micro-injector nozzle container, and passing the slurry through a dispenserThe motor boosts and compresses air, and the generated extrusion force is used for dripping the slurry in the spray head into silicon oil mixed with 20% boric acid in advance to realize curing molding; washing the zirconium oxide spherical blank collected at the bottom, drying the zirconium oxide spherical blank by microwave for 1.2h at the temperature of 180 ℃, transferring the zirconium oxide spherical blank into a muffle furnace, preserving the temperature at 700 ℃ for 2.5h, completely degreasing the zirconium oxide spherical blank, and sintering the degreased spherical blank for 2h at the temperature of 1500 ℃ to obtain a zirconium oxide ceramic microsphere rough blank; finally, carrying out wet self-grinding on the microsphere rough blank in a roller ball mill for 25h for polishing treatment to obtain a finished product of zirconia ceramic microspheres; the density of the prepared ceramic microspheres reaches 6.051g/cm3(relative density 99.74%) and has the characteristics of good sphericity, uniform size and high wear resistance.
Example 3
A method of preparing zirconia ceramic microspheres comprising the steps of:
with ZrOCl2·8H2O as starting material, according to ZrO2/Y2O3Is 97: 3 ratio of ammonia to Y (NO)3)3·6H2O, calcining the precursor powder at 1000 ℃ to obtain Y2O3Stabilized zirconia powder; according to the proportion of relative powder raw materials, respectively adding 0.5% of dispersing agent sodium hexametaphosphate, 2% of binder PVA and 0.6% of cotton fiber reinforcing agent, uniformly mixing with deionized water to obtain a premixed solution, and preparing zirconia slurry with the solid content of 73% by adopting a nanosphere mill by adopting a 3-time feeding technology; transferring the zirconia slurry into a micro-injector nozzle container, boosting compressed air by a motor of a dispenser, and dripping the slurry in the nozzle into silicone oil mixed with 18% boric acid in advance by the generated extrusion force to realize solidification molding; washing the zirconium oxide ball blank collected at the bottom, drying the zirconium oxide ball blank by microwave for 2h at the temperature of 200 ℃, transferring the zirconium oxide ball blank to a muffle furnace, preserving the temperature at 650 ℃ for 3h, completely degreasing the zirconium oxide ball blank, and sintering the degreased ball blank for 4h at the temperature of 1400 ℃ to obtain a zirconium oxide ceramic microsphere rough blank; finally, carrying out wet self-grinding on the microsphere rough blank in a roller ball mill for 40h for polishing treatment to obtain a finished product of the zirconia ceramic microsphere; the density of the prepared ceramic microspheres reaches 6.054g/cm3(relative density 99.75%) and has the characteristics of good sphericity, uniform size and high wear resistance.
Claims (10)
1. The utility model provides a method for preparing zirconia ceramic microsphere, the zirconia thick liquids that are prepared with zirconia powder and deionized water and auxiliary agent mixture drop into through titration outfit and form the zirconia microsphere in the oily medium, then degrease, sintering make zirconia ceramic microsphere after separating the zirconia microsphere, its characterized in that: when preparing zirconia slurry, mixing a binder capable of being solidified under the action of a cross-linking agent, dripping the zirconia slurry into an oily medium mixed with the cross-linking agent, and reacting the binder in the zirconia slurry drops with the cross-linking agent to solidify and form zirconia microspheres.
2. The method of preparing zirconia ceramic microspheres of claim 1, wherein: the binder is polyvinyl alcohol, and the dosage of the binder is 1.5-3% of the weight of the zirconia powder.
3. The method of preparing zirconia ceramic microspheres of claim 2, wherein: the polymerization degree of the polyvinyl alcohol is 2000-3000.
4. The method of preparing zirconia ceramic microspheres of claim 1, wherein: the cross-linking agent is boric acid, and the dosage of the boric acid is 15-20% of the weight of the oily medium.
5. The method of preparing zirconia ceramic microspheres of claim 1, wherein: the auxiliary agent comprises a dispersing agent, wherein the dispersing agent is one of ammonium polycarboxylate, ammonium acrylate, ammonium citrate and sodium hexametaphosphate, and the addition amount of the dispersing agent is 0.5-1.5% of the weight of the zirconia powder.
6. The method of preparing zirconia ceramic microspheres of claim 1, wherein: the auxiliary agent comprises an organic reinforcing agent, the organic reinforcing agent is cotton fiber, and the adding amount of the organic reinforcing agent is 0.3-0.6% of the weight of the zirconia powder.
7. As claimed in claim1, the method for preparing the zirconia ceramic microspheres is characterized by comprising the following steps: the zirconia powder is Y2O3The preparation method of the stable zirconia powder comprises the following steps: with ZrOCl2·8H2O as a raw material, according to ZrO formed after calcination2/Y2O3Is 97: 3 ratio of Y (NO)3)3·6H2O and ammonia water, and drying the precipitate to obtain Y2O3Calcining the precursor powder at 1000-1100 ℃ to obtain Y2O3Stabilized zirconia powder.
8. The method of preparing zirconia ceramic microspheres of claim 1, wherein: the solid content of the prepared zirconia ceramic slurry is 70-75%.
9. The method of preparing zirconia ceramic microspheres of claim 1, wherein: and (3) carrying out microwave drying on the separated zirconium oxide microspheres for 1-2 h at the temperature of 150-200 ℃, then transferring the zirconium oxide microspheres into a muffle furnace, and carrying out heat preservation for 2-3 h at the temperature of 600-700 ℃ to finish degreasing.
10. The method of preparing zirconia ceramic microspheres of claim 1, wherein: and (3) preserving the heat of the degreased zirconia microspheres for 2-5 hours at 1400-1550 ℃, and sintering to obtain the zirconia ceramic microspheres.
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Cited By (8)
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| CN111673632A (en) * | 2020-06-22 | 2020-09-18 | 河源帝诺新材料有限公司 | Preparation method of nano-grade zirconium oxide grinding medium |
| CN112939611A (en) * | 2021-01-28 | 2021-06-11 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ceramic microspheres by adopting direct titration forming technology |
| CN113307635A (en) * | 2021-05-24 | 2021-08-27 | 中国船舶重工集团公司第七二五研究所 | Method for directly titrating and forming ceramic microspheres through gel casting of track |
| CN112851368B (en) * | 2021-01-27 | 2022-06-07 | 湖南柯盛新材料有限公司 | Method for preparing coated wear-resistant ceramic microspheres by non-impregnation method and wear-resistant ceramic microspheres |
| CN114773041A (en) * | 2022-03-21 | 2022-07-22 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ceramic hollow microspheres at low cost |
| CN116003139A (en) * | 2022-12-26 | 2023-04-25 | 赣州科盈结构陶瓷有限公司 | Preparation device and preparation method of ceramic microbeads and ceramic microbeads |
| CN116375496A (en) * | 2023-03-14 | 2023-07-04 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | Submillimeter-grade porous ceramic microsphere and preparation method thereof |
| CN117383914A (en) * | 2023-09-22 | 2024-01-12 | 广东省科学院新材料研究所 | Preparation method of nano zirconia toughened nano alumina ceramic |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11278847A (en) * | 1998-03-30 | 1999-10-12 | Nuclear Fuel Ind Ltd | Production of zirconia particle |
| CN100999408A (en) * | 2006-12-15 | 2007-07-18 | 清华大学 | Method of preparing UO2 ceramic fuel microsphere |
| CN102674834A (en) * | 2012-05-22 | 2012-09-19 | 江西理工大学 | Preparation method of zirconium oxide structural ceramics |
| CN106082993A (en) * | 2016-06-08 | 2016-11-09 | 中国船舶重工集团公司第七二五研究所 | A kind of method preparing high-performance ITO pelletizing |
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN108203299A (en) * | 2018-01-15 | 2018-06-26 | 中国地质大学（武汉） | A kind of method that presoma comminution granulation prepares spherical zirconia powder |
| CN108298977A (en) * | 2018-01-10 | 2018-07-20 | 中国船舶重工集团公司第七二五研究所 | A method of improving ITO target blank strength |
| CN108840683A (en) * | 2018-07-05 | 2018-11-20 | 清华大学 | It is used to prepare the technique and zirconium nitride ceramic microsphere of zirconium nitride ceramic microsphere |
-
2019
- 2019-10-31 CN CN201911049578.5A patent/CN110835263A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11278847A (en) * | 1998-03-30 | 1999-10-12 | Nuclear Fuel Ind Ltd | Production of zirconia particle |
| CN100999408A (en) * | 2006-12-15 | 2007-07-18 | 清华大学 | Method of preparing UO2 ceramic fuel microsphere |
| CN102674834A (en) * | 2012-05-22 | 2012-09-19 | 江西理工大学 | Preparation method of zirconium oxide structural ceramics |
| CN106082993A (en) * | 2016-06-08 | 2016-11-09 | 中国船舶重工集团公司第七二五研究所 | A kind of method preparing high-performance ITO pelletizing |
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN108298977A (en) * | 2018-01-10 | 2018-07-20 | 中国船舶重工集团公司第七二五研究所 | A method of improving ITO target blank strength |
| CN108203299A (en) * | 2018-01-15 | 2018-06-26 | 中国地质大学（武汉） | A kind of method that presoma comminution granulation prepares spherical zirconia powder |
| CN108840683A (en) * | 2018-07-05 | 2018-11-20 | 清华大学 | It is used to prepare the technique and zirconium nitride ceramic microsphere of zirconium nitride ceramic microsphere |
Non-Patent Citations (3)
| Title |
|---|
| 周长春等: "《大学化学》", 30 March 2018, 中国矿业大学出版社 * |
| 杜双明: "《材料科学与工程概论》", 31 August 2011, 西安电子科技大学出版社 * |
| 陈大明: "《先进陶瓷材料的注凝技术与应用》", 30 November 2011, 国防工业出版社 * |
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|---|---|---|---|---|
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| CN116003139B (en) * | 2022-12-26 | 2024-03-05 | 赣州科盈结构陶瓷有限公司 | Preparation device and preparation method of ceramic microbeads and ceramic microbeads |
| CN116375496A (en) * | 2023-03-14 | 2023-07-04 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | Submillimeter-grade porous ceramic microsphere and preparation method thereof |
| CN116375496B (en) * | 2023-03-14 | 2024-05-10 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | Submillimeter-grade porous ceramic microsphere and preparation method thereof |
| CN117383914A (en) * | 2023-09-22 | 2024-01-12 | 广东省科学院新材料研究所 | Preparation method of nano zirconia toughened nano alumina ceramic |
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