CN110550952A - zirconia ceramic powder and preparation method thereof - Google Patents
zirconia ceramic powder and preparation method thereof Download PDFInfo
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- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
Abstract
the invention discloses zirconia ceramic powder and a preparation method thereof. The method comprises the following steps: mixing a rare earth nitric acid compound, zirconia, alumina, absolute ethyl alcohol and water, and uniformly stirring to obtain a mixture; performing ball milling treatment on the mixture to obtain uniform slurry; drying the uniform slurry to obtain coarse bulk zirconia ceramic powder; grinding the coarse grinding powder of the blocky zirconia ceramics into powder, and then heating the powder for roasting treatment to obtain roasted zirconia ceramic powder; and carrying out fine grinding treatment on the roasted zirconia ceramic powder, and sieving to obtain the zirconia ceramic powder. The zirconium oxide powder is prepared by the coating method, so that the zirconium oxide ceramic powder with small particle size and high purity can be prepared, the defects of complicated process flow, low production efficiency, low fracture toughness and the like of the traditional zirconium oxide ceramic powder preparation process can be overcome, the preparation efficiency of the zirconium oxide powder is improved, and the performance of the prepared zirconium oxide powder is more stable.
Description
Technical Field
The invention belongs to the field of ceramic powder preparation, and particularly relates to zirconia ceramic powder and a preparation method thereof.
Background
Stabilized zirconia, as an important oxide ceramic material, has been widely used in the fields of structural ceramics, functional ceramics, refractory materials, etc. in recent years due to its excellent properties such as high strength, high hardness, high melting point, high temperature resistance, wear resistance, corrosion resistance, biocompatibility, and low heat conduction. The zirconia ceramics are widely applied, the preparation process of the zirconia ceramics generally comprises powder preparation, prepressing forming and sintering, and the granularity and the purity of the zirconia powder are the most main factors influencing the physical and chemical properties of the zirconia ceramics.
At present, most of the traditional preparation methods of the domestic zirconium oxide are as follows: hydrothermal synthesis, coprecipitation, and sol-gel methods. The defects of complex process, expensive equipment, relatively harsh conditions, high raw material cost and the like of the methods ensure that the zirconia powder is not easy to produce on a large scale. The preparation of zirconia powder by a coprecipitation method is most common, but chlorides are difficult to completely remove in the powder preparation process by the coprecipitation method, and impurities are easily introduced into the powder. Meanwhile, the coprecipitation method for producing the zirconia powder has long period and high cost. So far, the preparation of zirconia powder by using a coating method in China has not been reported. Therefore, the development of a preparation method which has low cost and simple process and can prepare zirconia particles with fine and sufficiently pure granularity has important practical significance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide zirconia ceramic powder and a preparation method thereof.
the invention provides a preparation method of zirconia powder, which is a coating method. The method comprises the following steps: according to the stoichiometric ratio of different rare earth oxide stabilizer components in a target material, preparing a metal salt solution with water as a solvent, adding ethanol in a certain proportion to form a mixed solution, then adding monoclinic phase zirconia powder into the mixed solution to form a suspension, and performing ball milling treatment on the suspension in order to enable rare earth metal ions in the suspension to fully coat the zirconia powder. And drying the suspension subjected to ball milling and calcining to achieve a stabilizing effect. At present, the traditional zirconia powder preparation method is most common for preparing zirconia powder by a coprecipitation method, but the nanometer rare earth stable zirconia powder prepared by the traditional coprecipitation method is crystallized from an amorphous precursor. The rare earth ions exist in the precursor uniformly, and are finally and uniformly distributed in the zirconia crystal after the crystal bloom process. Different from the coprecipitation method, the zirconium oxide powder prepared by the coating method is prepared by coating the surface layer of m-phase zirconium oxide powder by a rare earth ion salt film, and then uniformly distributing rare earth ions in the zirconium oxide ceramic through diffusion after subsequent calcination.
the purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of zirconia ceramic powder, which comprises the following steps:
(1) Preparing slurry: mixing a rare earth nitric acid compound, zirconia, alumina, absolute ethyl alcohol and deionized water in a nylon ball milling tank, and fully and uniformly stirring to obtain a mixture;
(2) Ball milling of slurry: placing the nylon ball tank filled with the mixture in the step (1) in a planetary ball mill for ball milling treatment to obtain uniform slurry;
(3) drying the slurry: drying the uniform slurry obtained in the step (2) to obtain blocky zirconia ceramic coarse grinding powder;
(4) coarse grinding and roasting of powder: grinding the coarse bulk zirconia ceramic powder obtained in the step (3) into powder, and then placing the powder in a resistance furnace to heat for roasting treatment to obtain roasted zirconia ceramic powder (zirconia ceramic powder with solid solution of rare earth oxide);
(5) fine grinding of powder: and (4) finely grinding the roasted zirconia ceramic powder in the step (4), and sieving to obtain the zirconia ceramic powder.
furthermore, the molar ratio of the rare earth nitric acid compound to the zirconium oxide (ZrO 2) in the step (1) is 2:99-7:93, and the rare earth nitric acid compound is more than one of yttrium nitrate (Y (NO 3) 3 & 6H 2 O) and cerium nitrate (Ce (NO 3) 3 & 6H 2 O).
Preferably, the zirconia of step (1) is an m-phase zirconia.
Further, the mass of the alumina (Al 2 O 3) in the step (1) is 1wt.% to 3wt.% of the total mass of both the zirconia and the rare earth nitrate compound.
Preferably, the alumina in the step (1) is nano alumina.
Further, the mass ratio of the absolute ethyl alcohol to the water in the step (1) is 3:2-5: 2.
further, the rotation speed of the ball milling treatment in the step (2) is 300-.
Preferably, the time of the ball milling treatment in the step (2) is 10 ~ 16 h.
Further, zirconia ball grinding balls are added in the ball milling treatment in the step (2), and the ball-to-material ratio of the zirconia ball grinding balls to the mixture is 2:1-4: 1.
Preferably, in the ball milling treatment in the step (2), the ball milling ratio is 3: 1.
Further, the drying temperature in the step (3) is 70-80 ℃, and the drying time is 30-40 h.
Further, the temperature rising rate of the step (4) is 3-7 ℃/min.
Preferably, the temperature rising rate of the step (4) is 3-6 ℃/min.
Further, the temperature of the roasting treatment in the step (4) is 600-.
Preferably, the temperature of the roasting treatment in the step (4) is 700 ~ 900 ℃.
preferably, the roasting treatment time of the step (4) is 2 ~ 4 h.
Further, the fine grinding treatment in the step (5) is one of ball milling treatment and grinding; the size of the sieved mesh is 200 meshes.
The invention adopts a preparation method of zirconia powder, namely a coating method. The method has the advantages of simple process, high efficiency and low cost, and is suitable for industrial production.
compared with the prior art, the preparation method of the zirconia powder provided by the invention has the advantages that the prepared multi-element rare earth oxide stabilized zirconia ceramic powder is subjected to primary slurry ball milling and drying, and then the powder ball milling is carried out to refine crystal grains, so that the zirconia ceramic powder with fine and uniform powder granularity, high purity and less agglomeration can be prepared, and the work efficiency of the zirconia ceramic powder preparation can be greatly improved.
the invention discloses zirconia ceramic powder and a preparation method (coating method) thereof. The method comprises the following steps: pouring a rare earth nitric acid compound, aluminum oxide, absolute ethyl alcohol and deionized water into a nylon ball milling tank, and fully stirring to obtain slurry; placing the sealed nylon tank in a planetary ball mill for ball milling to obtain uniformly mixed slurry; placing the uniformly mixed slurry in a drying oven for drying treatment to obtain dried agglomerated zirconia ceramic powder; grinding the dried agglomerated zirconia ceramic powder into coarser powder (coarse ground powder); placing the coarse ground powder in a resistance furnace for roasting treatment to obtain zirconia ceramic powder with solid solution of rare earth oxide (zirconia powder with stable rare earth oxide); and grinding the zirconia powder body with stable rare earth oxide (zirconia ceramic powder body with solid solution of rare earth oxide), and sieving to obtain fine grinding powder body. The zirconium oxide powder is prepared by using a coating method, so that the zirconium oxide ceramic powder with small particle size and high purity can be prepared, the defects of complicated process flow, low production efficiency, low fracture toughness and the like of the traditional zirconium oxide ceramic powder preparation process can be overcome, the preparation efficiency of the zirconium oxide powder is improved, and the performance of the prepared zirconium oxide powder is more stable.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the preparation method of the zirconia ceramic powder has the advantages of simple process, high efficiency, low cost, suitability for industrial production and the like;
(2) The fracture toughness of the zirconia ceramic powder provided by the invention is higher than that of the zirconia ceramic powder prepared by the traditional method (such as a coprecipitation method), the fracture toughness range of the zirconia ceramic powder provided by the invention is 8.10 MPa-m 1/2 -8.54 MPa-m 1/2, and the fracture toughness range of the zirconia ceramic powder prepared by the traditional coprecipitation method is 5.13 MPa-m 1/2 -7.64 MPa-m 1/2.
Drawings
FIG. 1 is a scanning electron micrograph of the zirconia ceramic powder obtained in example 1 magnified 5000 times.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
a preparation method of zirconia ceramic powder comprises the following steps:
(1) The preparation method of the slurry comprises the steps of mixing yttrium nitrate (Y (NO 3) 3.6H 2 O), zirconium oxide (ZrO 2), aluminum oxide (Al 2 O 3, nano aluminum oxide powder), 100g of absolute ethyl alcohol and 50g of deionized water, uniformly stirring to obtain a mixture, and pouring the mixture into a nylon tank, wherein the molar ratio of the yttrium nitrate to the zirconium oxide is 3: 97, and the mass of the aluminum oxide is 1 wt% of the total mass of the yttrium nitrate and the zirconium oxide;
(2) Ball milling of slurry: placing the mixture obtained in the step (1) in a planetary ball mill for ball milling treatment, wherein the rotating speed of the ball milling treatment is 300r/min, and the ball milling treatment time is 8h, so as to obtain uniform slurry; zirconia ball grinding balls are added in the ball milling treatment, and the ball material ratio of the zirconia ball grinding balls to the mixture in the step (1) is 2: 1;
(3) drying the slurry: putting the uniform slurry obtained in the step (2) into a drying oven for drying at the temperature of 70 ℃ for 30h to obtain coarse bulk zirconia ceramic powder (dried agglomerated zirconia powder);
(4) Coarse grinding and roasting of powder: grinding the rough ground blocky zirconia ceramic powder in the step (3) into powder, and then heating for roasting treatment, wherein the heating rate is 3 ℃/min, the roasting temperature is 600 ℃, and the roasting time is 1h, so as to obtain roasted zirconia ceramic powder;
(5) Fine grinding of powder: and (4) grinding and sieving the roasted zirconia ceramic powder in the step (4) to obtain zirconia ceramic powder particles with the sieve mesh size of 200 meshes.
When the zirconia ceramic powder particles prepared in example 1 are observed under SEM, the average particle size of the powder is 4um, and the zirconia ceramic powder has fine and uniform particle size, high purity, and less agglomeration, as shown in fig. 1.
Effect verification
The zirconia ceramic powder prepared in the example 1 is heated to 1600 ℃ for sintering, the sintering time is 2h, the zirconia ceramic is obtained, and the fracture toughness of the zirconia ceramic obtained in the example 1 can reach 8.24 MPa.m 1/2 through the test of an Indentation Method (IM). the fracture toughness of the zirconia ceramic obtained by the traditional coprecipitation method is 5.50 MPa.m 1/2 through the test of the Indentation Method (IM) when the zirconia ceramic powder prepared by the traditional coprecipitation method is heated to 1600 ℃ for sintering for 2 h.
Example 2
A preparation method of zirconia ceramic powder comprises the following steps:
(1) The preparation method of the slurry comprises the steps of mixing yttrium nitrate (Y (NO 3) 3.6H 2 O), zirconium oxide (ZrO 2), aluminum oxide (Al 2 O 3, nano aluminum oxide powder), 100g of absolute ethyl alcohol and 50g of deionized water, uniformly stirring to obtain a mixture, pouring the mixture into a nylon tank, wherein the molar ratio of the yttrium nitrate to the zirconium oxide is 3: 97, and the mass of the aluminum oxide is 2wt% of the total mass of the yttrium nitrate and the zirconium oxide.
(2) Ball milling of slurry: placing the mixture obtained in the step (1) in a planetary ball mill for ball milling treatment, wherein the rotating speed of the ball milling treatment is 330r/min, and the ball milling treatment time is 12 hours, so as to obtain uniform slurry; zirconia ball grinding balls are added in the ball milling treatment, and the ball material ratio of the zirconia ball grinding balls to the mixture in the step (1) is 3: 1;
(3) Drying the slurry: placing the uniform slurry obtained in the step (2) in a drying oven for drying at the temperature of 75 ℃ for 35h to obtain coarse bulk zirconia ceramic powder (dried agglomerated zirconia powder);
(4) Coarse grinding and roasting of powder: grinding the rough ground blocky zirconia ceramic powder in the step (3) into powder, and then heating for roasting treatment, wherein the heating rate is 5 ℃/min, the roasting temperature is 800 ℃, and the roasting time is 2h, so as to obtain roasted zirconia ceramic powder;
(5) Fine grinding of powder: and (4) grinding and sieving the roasted zirconia ceramic powder in the step (4) to obtain zirconia ceramic powder particles with the sieve mesh size of 200 meshes.
The zirconia ceramic powder prepared in example 2 also has the characteristics of fine and uniform particle size, high purity and less agglomeration, and can be seen in fig. 1.
effect verification
The zirconia ceramic powder prepared in the example 2 is heated to 1600 ℃ for sintering, the sintering time is 2h, the zirconia ceramic is obtained, and the fracture toughness of the zirconia ceramic obtained in the example 2 can reach 8.10 MPa.m 1/2 through the test of an Indentation Method (IM). the fracture toughness of the zirconia ceramic obtained by the traditional coprecipitation method is only 5.50 MPa.m 1/2 through the test of the Indentation Method (IM) when the zirconia ceramic powder prepared by the traditional coprecipitation method is heated to 1600 ℃ for sintering for 2 h.
Example 3
a preparation method of zirconia ceramic powder comprises the following steps:
(1) The preparation method of the slurry comprises the steps of mixing yttrium nitrate (Y (NO 3) 3.6H 2 O), cerium nitrate (Ce (NO 3) 3.6H 2 O), zirconium oxide (ZrO 2), aluminum oxide (Al 2 O 3, nano aluminum oxide powder), 100g of absolute ethyl alcohol and 50g of deionized water, uniformly stirring to obtain a mixture, pouring the mixture into a nylon tank, wherein the molar ratio of yttrium nitrate to zirconium oxide is 1.5: 93, the molar ratio of cerium nitrate to zirconium oxide is 5.5: 93, and the mass of aluminum oxide is 3wt% of the total mass of yttrium nitrate, cerium nitrate and zirconium oxide.
(2) Ball milling of slurry: placing the mixture obtained in the step (1) in a planetary ball mill for ball milling treatment, wherein the rotating speed of the ball milling treatment is 360r/min, and the ball milling treatment time is 16h, so as to obtain uniform slurry; zirconia ball grinding balls are added in the ball milling treatment, and the ball material ratio of the zirconia ball grinding balls to the mixture in the step (1) is 4: 1;
(3) drying the slurry: placing the uniform slurry obtained in the step (2) in a drying oven for drying at the temperature of 80 ℃ for 40h to obtain coarse bulk zirconia ceramic powder (dried agglomerated zirconia powder);
(4) Coarse grinding and roasting of powder: grinding the rough ground blocky zirconia ceramic powder obtained in the step (3) into powder, and then heating for roasting treatment, wherein the heating rate is 7 ℃/min, the roasting temperature is 1000 ℃, and the roasting time is 4 hours, so as to obtain roasted zirconia ceramic powder;
(5) Fine grinding of powder: and (3) placing the roasted zirconia ceramic powder in the step (4) into a planetary ball mill for ball milling treatment, wherein the ball milling rotation speed is 300r/min, the ball milling time is 6 hours, drying is carried out, the drying temperature is 75 ℃, the drying time is 35 hours, and sieving is carried out, wherein the sieve mesh size is 200 meshes, so as to obtain the zirconia ceramic powder particles.
the zirconia ceramic powder obtained in example 3 also has the characteristics of fine and uniform particle size, high purity and less agglomeration, as shown in fig. 1.
effect verification
the zirconia ceramic powder prepared in the example 3 is heated to 1600 ℃ for sintering, the sintering time is 2h, the zirconia ceramic is obtained, and the fracture toughness of the zirconia ceramic obtained in the example 3 can reach 8.54 MPa.m 1/2 through the test of an Indentation Method (IM). the fracture toughness of the zirconia ceramic obtained by the traditional coprecipitation method is only 5.50 MPa.m 1/2 through the test of the Indentation Method (IM) when the zirconia ceramic powder prepared by the traditional coprecipitation method is heated to 1600 ℃ for sintering for 2 h.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. the preparation method of the zirconia ceramic powder is characterized by comprising the following steps:
(1) Mixing a rare earth nitric acid compound, zirconia, alumina, absolute ethyl alcohol and water, and uniformly stirring to obtain a mixture;
(2) Performing ball milling treatment on the mixture obtained in the step (1) to obtain uniform slurry;
(3) Drying the uniform slurry obtained in the step (2) to obtain blocky zirconia ceramic coarse grinding powder;
(4) Grinding the rough grinding powder of the blocky zirconia ceramics obtained in the step (3) into powder, and then heating for roasting treatment to obtain roasted zirconia ceramic powder;
(5) And (4) finely grinding the roasted zirconia ceramic powder in the step (4), and sieving to obtain the zirconia ceramic powder.
2. The method for preparing zirconia ceramic powder according to claim 1, wherein the molar ratio of the rare earth nitric acid compound to the zirconia in the step (1) is 2:99 to 7: 93; the rare earth nitric acid compound is more than one of yttrium nitrate and cerium nitrate.
3. The method for preparing zirconia ceramic powder according to claim 1, wherein the mass of the alumina in the step (1) is 1-3 wt.% of the total mass of the zirconia and the rare earth nitrate compound.
4. The method for preparing zirconia ceramic powder according to claim 1, wherein the mass ratio of the absolute ethyl alcohol to the water in the step (1) is 3:2-5: 2.
5. The method for preparing zirconia ceramic powder according to claim 1, wherein the rotation speed of the ball milling treatment in step (2) is 300-.
6. The method for preparing zirconia ceramic powder according to claim 1, wherein zirconia ball grinding balls are added in the ball milling treatment in step (2), and the ball-to-material ratio between the zirconia ball grinding balls and the mixture is 2:1-4: 1.
7. The method for preparing zirconia ceramic powder according to claim 1, wherein the drying temperature in step (3) is 70-80 ℃ and the drying time is 30-40 h.
8. The method for preparing zirconia ceramic powder according to claim 1, wherein the rate of temperature rise in step (4) is 3-7 ℃/min; the temperature of the roasting treatment is 600-1000 ℃, and the time of the roasting treatment is 1-4 h.
9. the method for preparing zirconia ceramic powder according to claim 1, wherein the fine grinding treatment in step (5) is one of ball milling treatment and grinding; the size of the sieved mesh is 200 meshes.
10. the zirconia ceramic powder produced by the production method according to any one of claims 1 to 9, characterized by a fracture toughness of 8.10 MPa-m 1/2 to 8.54 MPa-m 1/2.
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| CN112898018A (en) * | 2021-02-02 | 2021-06-04 | 淄博松阳锆业科技有限公司 | Antibacterial zirconia ceramic knife raw material powder and preparation method thereof |
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