CN112851312A - Zirconia toughened alumina composite ceramic material and preparation method thereof - Google Patents
Zirconia toughened alumina composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a zirconia toughened alumina composite ceramic material which comprises the following raw materials in parts by mass: 5-10 parts of zirconium oxide powder, 75-90 parts of aluminum oxide powder and 2-10 parts of sintering aid; the sintering aid comprises lanthanum oxide and magnesium oxide. Also provided is a method for preparing the above complex phase ceramic material, comprising: and preparing a precursor mixed solution of lanthanum oxide and magnesium oxide. Preparing the mixed powder of zirconia powder and alumina. And forming the mixed powder to prepare a blank. And sintering the green body for the first time to obtain a ceramic green body. And (3) soaking the ceramic green body in the precursor mixed solution for a period of time, and then carrying out secondary sintering. The preparation method of the zirconia toughened alumina complex phase ceramic material provided by the invention can fully play the role of the sintering aid, effectively reduce the sintering temperature and save energy, and the zirconia toughened alumina complex phase ceramic material prepared by the method has excellent comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a zirconia toughened alumina complex phase ceramic material and a preparation method thereof.
Background
The alumina ceramic has the advantages of corrosion resistance, high temperature resistance, wear resistance, light weight, low cost and the like, and is an industrial ceramic material with the largest production and the widest application range in the world at present. The material has wide application prospect in the technical field of defense and protection such as aerospace and the like and the general industrial fields such as machinery, metallurgy, chemical industry and the like, but the most fatal mechanical weakness is the brittleness of the material, which is determined by the structural characteristics of the material. Chemical bonds in the ceramic material are mainly covalent bonds and ionic bonds, and both the chemical bonds have strong directionality and high bonding strength, so that remarkable dislocation movement in the structure is difficult to occur. Thus limiting the further spread of its practical application range. Therefore, toughening of ceramics, particularly alumina ceramics, has become a central issue in the recent research of structural ceramic materials.
In the prior art, zirconia is usually adopted to toughen alumina ceramics to prepare zirconia toughened alumina ceramic materials, but in the preparation process of the zirconia toughened alumina complex-phase ceramic materials, solid-phase sintering of the alumina complex-phase ceramic materials is usually assisted by adding a sintering aid to refine grains, so that the strength of products is improved. The process route of the prior art is as follows: the sintering aid is directly mixed with ceramic powder, wet-ground to a predetermined particle size, spray granulation, blank forming and sintering. Because the sintering aid is not suitable to be added in a large amount, the addition amount of the sintering aid is small, the sintering aid is directly mixed with the ceramic powder in the process route, the sintering aid is difficult to be uniformly distributed in the mixing process, the sintering aid is partially lost in the process before sintering, the sintering aid cannot fully exert the functions of reducing the sintering temperature and inhibiting or promoting the crystal phase transformation of the sintering aid due to the reasons, and the method is not beneficial to improving the comprehensive performance of the zirconia toughened alumina composite ceramic material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the zirconia toughened alumina complex phase ceramic material and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the zirconia toughened alumina composite ceramic material comprises the following raw materials in parts by mass: 5-10 parts of zirconium oxide powder, 75-90 parts of aluminum oxide powder and 2-10 parts of sintering aid; wherein the sintering aid comprises lanthanum oxide and magnesium oxide.
The further improvement of the technical scheme is as follows:
the composite material comprises the following raw materials in parts by mass: 5-10 parts of zirconium oxide powder, 75-90 parts of aluminum oxide powder, 1-5 parts of lanthanum oxide and 1-5 parts of magnesium oxide.
The invention also provides a method for preparing the zirconia toughened alumina composite ceramic material, which comprises the following steps:
preparing a precursor mixed solution: preparing a precursor mixed solution of lanthanum oxide and magnesium oxide;
preparing mixed powder: weighing zirconium oxide powder and aluminum oxide powder according to a proportion, mixing and granulating to obtain mixed powder;
preparing a blank body: molding the mixed powder to prepare a blank;
first sintering: sintering the green body for the first time to obtain a ceramic green body;
and (3) second sintering: placing the ceramic green body in a container, vacuumizing, sucking the precursor mixed solution, dipping the ceramic green body in the precursor mixed solution, taking out the ceramic green body, and sintering the ceramic green body for the second time to obtain the zirconia toughened alumina complex-phase ceramic material;
wherein the mass of the zirconia powder, the mass of the alumina powder and the total mass ratio of the lanthanum oxide to the magnesium oxide are (5-10): (75-90): (2-10).
Further, the step of preparing the precursor mixed solution specifically comprises: respectively taking lanthanum oxide and magnesium oxide as precursors La (NO)3)3、Mg(NO3)2.6H2And preparing the precursor mixed solution with O as a solute, citric acid as a complexing agent, absolute ethyl alcohol as a solvent and PVP as a dispersing agent under the condition that the pH value is 5, wherein the concentration of the precursor mixed solution is 0.2 mol/L.
Further, in the step of preparing the mixed powder, the mixing mode adopts wet grinding, and the grain diameter of the ground powder is 0.5-1.5 μm.
Further, the particle size value of the mixed powder in the step of preparing the mixed powder is 20-200 μm.
Further, the sintering temperature in the first sintering step is 1000-1050 ℃, and the heat preservation time is 2-4 h.
Further, the sintering temperature in the second sintering step is 1300-1350 ℃, and the heat preservation time is 2-4 h.
Further, in the second sintering step, the vacuum degree of the vacuumizing treatment is less than or equal to 500Pa, and the impregnation time is 4-8 h.
Further, the mass ratio of the zirconia powder to the alumina powder to the lanthanum oxide to the magnesium oxide is (5-10): (75-90): (1-5):(1-5).
According to the technical scheme of the invention, the sintering aid of the zirconia toughened alumina composite ceramic material is lanthanum oxide and magnesium oxide, and the raw materials are reasonable in proportion, so that the zirconia toughened alumina composite ceramic material with excellent comprehensive performance can be prepared. According to the preparation method of the zirconia toughened alumina complex phase ceramic material, the sintering aid is prepared into the precursor mixed solution, and the ceramic green body is soaked in the precursor mixed solution through the secondary sintering step, so that the ceramic green body is fully contacted with the precursor mixed solution, and the precursor mixed solution is uniformly filled into the holes of the ceramic green body, thereby being beneficial to the sintering aid to better play a role. And before the secondary sintering step, the sintering aid does not participate, so that the sintering aid is not lost, the function of the sintering aid can be exerted to a greater extent, the sintering temperature is effectively reduced, the crystal phase transformation is inhibited or promoted, and the comprehensive performance of the zirconia toughened alumina composite ceramic material is favorably improved.
Drawings
Fig. 1 is a flow chart of a zirconia toughened alumina complex phase ceramic material and a preparation method thereof according to an embodiment of the invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The zirconia toughened alumina composite ceramic material comprises the following raw materials in parts by mass: zirconium oxide (3Y-ZrO)2) 5-10 parts of powder and aluminum oxide (Al)2O3) 75-90 parts of powder and 2-10 parts of sintering aid. Wherein the sintering aid comprises lanthanum oxide (La)2O3) And magnesium oxide (MgO). Wherein, the lanthanum oxide accounts for 1 to 5 parts, and the magnesium oxide accounts for 1 to 5 parts.
As shown in fig. 1, the method for preparing the zirconia toughened alumina composite ceramic material comprises the following steps:
s1, preparing a precursor mixed solution: and preparing a precursor mixed solution of lanthanum oxide and magnesium oxide. Respectively taking lanthanum oxide and magnesium oxide as precursors La (NO)3)3、Mg(NO3)2.6H2And preparing the precursor mixed solution with O as a solute, citric acid as a complexing agent, absolute ethyl alcohol as a solvent and PVP as a dispersing agent under the condition that the pH value is 5, wherein the concentration of the precursor mixed solution is 0.2 mol/L. Wherein, the mass portion of lanthanum oxide is 1-5 portions, and the mass portion of magnesium oxide is 1-5 portions.
S2, preparing mixed powder: weighing 5-10 parts of zirconia powder and aluminum oxide (Al) according to the mass parts2O3) 75-90 parts of powder, and fully and uniformly mixing, and grinding by a wet method to ensure that the particle size of the ground powder reaches 0.5-1.5 mu m. Drying and granulating by a spray drying tower to obtain mixed powder. The particle size value of the mixed powder is 20-200 μm. In the spray drying process, the temperature of the drying air is 200-.
S3, preparing a blank: and carrying out cold isostatic pressing on the mixed powder to prepare a blank. The pressure of the cold isostatic pressing is 150-200MPa, and the time is 3-5 min.
S4, first sintering: and placing the green body in a high-temperature kiln, and sintering for the first time at the sintering temperature of 1000-1050 ℃ for 2-4h to obtain a ceramic green body.
S5, secondary sintering: and placing the ceramic green body in a container, vacuumizing the container, sucking the precursor mixed solution, soaking the ceramic green body in the precursor mixed solution, wherein the vacuum degree of vacuumizing is less than or equal to 500Pa, the soaking time is 4-8h, fully contacting the ceramic green body with the precursor mixed solution, placing the ceramic green body in a high-temperature kiln again, and sintering for the second time, wherein the sintering temperature is 1300-1350 ℃, and the heat preservation time is 2-4h, so that the zirconia toughened alumina composite ceramic material is obtained.
Example 1: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is the same as the preparation method, and is not described herein again, and the specific implementation data is as follows:
s1, preparing a precursor mixed solution: according to the mass parts, the lanthanum oxide accounts for 3 parts, and the magnesium oxide accounts for 3 parts.
S2, preparing mixed powder: weighing 5 parts of zirconia powder and 90 parts of alumina powder according to parts by mass. The particle size of the ground powder was 1.2 μm, and the particle size of the granulated mixed powder was 85 μm.
S4, first sintering: the sintering temperature is 1050 ℃, and the heat preservation time is 3 h.
S5, secondary sintering: the vacuum degree was 500Pa, and the immersion time was 5 hours. The sintering temperature is 1300 ℃, and the heat preservation time is 3 h.
Example 2: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is basically the same as that of the embodiment 1, and the difference is that:
s2, preparing mixed powder: weighing 6 parts of zirconia powder and 90 parts of alumina powder according to parts by mass. The particle size of the ground powder was 0.8. mu.m, and the particle size of the granulated mixed powder was 60 μm.
S4, first sintering: the sintering temperature is 1050 ℃, and the heat preservation time is 2 hours.
S5, secondary sintering: the vacuum degree was 500Pa, and the dipping time was 4 hours. The sintering temperature is 1300 ℃, and the heat preservation time is 2 hours.
Example 3: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is basically the same as that of the embodiment 1, and the difference is that:
s1, preparing a precursor mixed solution: according to the mass parts, the lanthanum oxide accounts for 3 parts, and the magnesium oxide accounts for 1 part.
S2, preparing mixed powder: weighing 7 parts of zirconia powder and 80 parts of alumina powder according to the parts by mass. The particle size of the ground powder was 0.8. mu.m, and the particle size of the granulated mixed powder was 60 μm.
S5, secondary sintering: the vacuum degree is 300Pa, and the immersion time is 6 h.
Example 4: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is basically the same as that of the embodiment 1, and the difference is that:
s1, preparing a precursor mixed solution: according to the mass parts, the lanthanum oxide is 4 parts, and the magnesium oxide is 5 parts.
S2, preparing mixed powder: weighing 8 parts of zirconia powder and 85 parts of alumina powder according to parts by mass. The particle size of the ground powder was 0.5. mu.m, and the particle size of the granulated mixed powder was 120. mu.m.
S4, first sintering: the sintering temperature is 1000 ℃, and the heat preservation time is 4 h.
S5, secondary sintering: the sintering temperature is 1350 ℃, and the heat preservation time is 4 h.
Example 5: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is basically the same as that of the embodiment 1, and the difference is that:
s1, preparing a precursor mixed solution: according to the mass parts, the lanthanum oxide is 4 parts, and the magnesium oxide is 5 parts.
S2, preparing mixed powder: weighing 9 parts of zirconia powder and 85 parts of alumina powder according to parts by mass. The particle size of the ground powder was 0.5. mu.m, and the particle size of the granulated mixed powder was 120. mu.m.
S4, first sintering: the sintering temperature is 1000 ℃, and the heat preservation time is 4 h.
S5, secondary sintering: the vacuum degree was 500Pa and the immersion time was 6 hours. The sintering temperature is 1350 ℃, and the heat preservation time is 4 h.
Example 6: the preparation method of the zirconia toughened alumina composite ceramic material of the embodiment is basically the same as that of the embodiment 1, and the difference is that:
s1, preparing a precursor mixed solution: according to the mass parts, the lanthanum oxide accounts for 5 parts, and the magnesium oxide accounts for 5 parts.
S2, preparing mixed powder: weighing 10 parts of zirconia powder and 75 parts of alumina powder according to parts by mass. The particle size of the ground powder was 1.5 μm, and the particle size of the granulated mixed powder was 200. mu.m.
S4, first sintering: the sintering temperature is 1040 ℃, and the holding time is 3 h.
S5, secondary sintering: the vacuum degree is 400Pa, and the immersion time is 6 h. The sintering temperature is 1350 ℃, and the heat preservation time is 3 h.
Comparative example: in order to prove the beneficial effects of the preparation method of the invention, the preparation method of the prior art is adopted to prepare the zirconia toughened alumina complex phase ceramic material as a contrast, and the preparation method of the comparative example comprises the following steps:
s1, preparing mixed powder: weighing zirconium oxide (3Y-ZrO) according to the mass parts2) 10 parts of powder, aluminum oxide (Al)2O3) 75 parts of powder and lanthanum oxide (La)2O3)5 parts of magnesium oxide (MgO), and fully and uniformly mixing, and adopting wet grinding to ensure that the grain diameter of the ground powder reaches 1.5 mu m. Drying and granulating by a spray drying tower to obtain mixed powder. The particle size value of the mixed powder is 200 mu m. In the spray drying process, the temperature of the drying air is 200-.
S2, preparing a blank: and carrying out cold isostatic pressing on the mixed powder to prepare a blank. The pressure of the cold isostatic pressing is 150-200MPa, and the time is 3-5 min.
S3, first sintering: and placing the green body in a high-temperature kiln, and sintering for the first time at 1040 ℃ for 3 hours to obtain a ceramic green body.
S4, secondary sintering: and placing the ceramic green body in a high-temperature kiln again, and sintering for the second time, wherein the sintering temperature is 1350 ℃ and the heat preservation time is 3 hours, so as to obtain the zirconia toughened alumina composite ceramic material.
The zirconia toughened alumina composite ceramic materials prepared in the six examples and the comparative example are detected, and the detection results are shown in table 1.
TABLE 1
As can be seen from the data in the table above, the zirconia toughened alumina composite ceramic material prepared by the method of the invention has the advantages that the sintering aid fully plays a role, the density, the fracture toughness and the four-point bending resistance are obviously improved, and the comprehensive performance is excellent.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The zirconia toughened alumina composite ceramic material is characterized in that: the composite material comprises the following raw materials in parts by mass: 5-10 parts of zirconium oxide powder, 75-90 parts of aluminum oxide powder and 2-10 parts of sintering aid; wherein the sintering aid comprises lanthanum oxide and magnesium oxide.
2. The zirconia toughened alumina composite ceramic material according to claim 1, wherein: the composite material comprises the following raw materials in parts by mass: 5-10 parts of zirconium oxide powder, 75-90 parts of aluminum oxide powder, 1-5 parts of lanthanum oxide and 1-5 parts of magnesium oxide.
3. A preparation method of zirconia toughened alumina complex phase ceramic material is characterized by comprising the following steps: the method comprises the following steps:
preparing a precursor mixed solution: preparing a precursor mixed solution of lanthanum oxide and magnesium oxide;
preparing mixed powder: weighing zirconium oxide powder and aluminum oxide powder according to a proportion, mixing and granulating to obtain mixed powder;
preparing a blank body: molding the mixed powder to prepare a blank;
first sintering: sintering the green body for the first time to obtain a ceramic green body;
and (3) second sintering: placing the ceramic green body in a container, vacuumizing, sucking the precursor mixed solution, dipping the ceramic green body in the precursor mixed solution, taking out the ceramic green body, and sintering the ceramic green body for the second time to obtain the zirconia toughened alumina complex-phase ceramic material;
wherein the mass of the zirconia powder, the mass of the alumina powder and the total mass ratio of the lanthanum oxide to the magnesium oxide are (5-10): (75-90): (2-10).
4. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: the step of preparing the precursor mixed solution specifically comprises the following steps:
respectively taking lanthanum oxide and magnesium oxide as precursors La (NO)3)3、Mg(NO3)2.6H2And preparing the precursor mixed solution with O as a solute, citric acid as a complexing agent, absolute ethyl alcohol as a solvent and PVP as a dispersing agent under the condition that the pH value is 5, wherein the concentration of the precursor mixed solution is 0.2 mol/L.
5. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: in the step of preparing the mixed powder, the mixing mode adopts wet grinding, and the grain diameter of the ground powder is 0.5-1.5 mu m.
6. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: the particle size value of the mixed powder in the step of preparing the mixed powder is 20-200 mu m.
7. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: the sintering temperature in the first sintering step is 1000-1050 ℃, and the heat preservation time is 2-4 h.
8. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: the sintering temperature in the second sintering step is 1300-1350 ℃, and the heat preservation time is 2-4 h.
9. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: in the second sintering step, the vacuum degree of the vacuumizing treatment is less than or equal to 500Pa, and the impregnation time is 4-8 h.
10. The preparation method of the zirconia toughened alumina composite ceramic material according to claim 3, characterized in that: wherein the mass ratio of the zirconia powder to the alumina powder to the lanthanum oxide to the magnesium oxide is (5-10): (75-90): (1-5):(1-5).
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| CN114105633A (en) * | 2021-11-18 | 2022-03-01 | 长裕控股集团有限公司 | Method for improving aging resistance of zirconia ceramic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134692A (en) * | 1993-11-12 | 1996-10-30 | 美国3M公司 | Abrasive grain and method for making the same |
| CN102264862A (en) * | 2008-10-30 | 2011-11-30 | 3M创新有限公司 | Crystalline ceramic particles |
| CN111072375A (en) * | 2019-12-31 | 2020-04-28 | 青海圣诺光电科技有限公司 | Preparation method of aluminum oxide grinding balls |
-
2021
- 2021-03-26 CN CN202110324160.1A patent/CN112851312A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134692A (en) * | 1993-11-12 | 1996-10-30 | 美国3M公司 | Abrasive grain and method for making the same |
| CN102264862A (en) * | 2008-10-30 | 2011-11-30 | 3M创新有限公司 | Crystalline ceramic particles |
| CN111072375A (en) * | 2019-12-31 | 2020-04-28 | 青海圣诺光电科技有限公司 | Preparation method of aluminum oxide grinding balls |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114105633A (en) * | 2021-11-18 | 2022-03-01 | 长裕控股集团有限公司 | Method for improving aging resistance of zirconia ceramic |
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