CN116425533A - Preparation method of anti-aging yellow zirconium ceramic - Google Patents
Preparation method of anti-aging yellow zirconium ceramic Download PDFInfo
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- CN116425533A CN116425533A CN202310474180.6A CN202310474180A CN116425533A CN 116425533 A CN116425533 A CN 116425533A CN 202310474180 A CN202310474180 A CN 202310474180A CN 116425533 A CN116425533 A CN 116425533A
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- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 77
- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 46
- 239000003381 stabilizer Substances 0.000 claims abstract description 32
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 11
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 19
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000005452 bending Methods 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 25
- 230000032683 aging Effects 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The invention relates to the technical field of ceramic materials, in particular to a preparation method of anti-aging yellow zirconium ceramic, which comprises the following steps: A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder; B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape; C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic. The produced anti-aging yellow zirconium ceramic has excellent bending strength, higher density and excellent anti-aging performance.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a preparation method of anti-aging yellow zirconium ceramic.
Background
Zirconia ceramics have high strength, high toughness, corrosion resistance, wear resistance and good biocompatibility, and are widely applied to the fields of materials, chemical industry, metallurgy, medical treatment and the like. Zirconia has three crystal forms of monoclinic phase, tetragonal phase and cubic phase, wherein the tetragonal phase changes into martensitic phase, and the process can generate 8% of shear strain and 3% -5% of volume increment, so that the application of the zirconia is limited. In order to avoid the volume effect caused by the phase change, a stabilization treatment is generally performed by doping a stabilizer. Currently common oxide stabilizers are alkaline earth metal oxides (e.g., caO, mgO, etc.) and rare earth metal oxides (e.g., Y2O3, la2O3, etc.). The addition of the stabilizer can cause low-temperature aging problem to the zirconia ceramics, and the zirconia ceramics can fail due to surface cracks in a humid environment at 100-400 ℃. This is because the stabilizer forms a solid solution with ZrO2 and generates a proportion of valence-compensated oxygen vacancies due to the different cation valence states. Taking Y-TZP as an example, in a humid environment, moisture is adsorbed on the surface of the Y-TZP and ionized to form OH < - >, permeates into oxygen vacancies of the surface layer of the Y-TZP and compensates electricity price, so that Y < 3+ > is deviated to a place with high concentration of the oxygen vacancies, the surface of the OH < - > -permeated layer cannot stabilize t-ZrO2 because of the reduced concentration of Y < 3+ >, so that t- > m phase transformation occurs, the volume is increased to generate microcracks, and zirconia ceramics are destroyed to fail after the microcracks develop into macroscopic cracks. The problem of low temperature aging of zirconia ceramics has been of great concern because of its direct impact on its useful life.
The main ways of improving the ageing resistance of the zirconia ceramics are adding a stabilizer, refining grains, increasing compactness and the like, and the latter two ways are influenced by the sintering process, the type of the stabilizer and the content of the stabilizer, so that the ageing resistance of the zirconia ceramics is improved mainly by changing the type of the stabilizer and the content of the stabilizer under the same sintering process. Among them, zirconia ceramics added with various stabilizers are more excellent in aging resistance. At present, the common anti-aging zirconia ceramics are prepared by adding two to three stabilizers, and the ageing resistance is optimized, but the service life is still insufficient and still needs to be improved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a preparation method of anti-aging yellow zirconium ceramic, and the produced anti-aging yellow zirconium ceramic has excellent bending strength, higher density and excellent aging resistance.
The aim of the invention is achieved by the following technical scheme: a preparation method of anti-aging yellow zirconium ceramic comprises the following steps:
A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder;
B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape;
C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic.
The stabilizer comprises Y 2 O 3 And CaO, Y 2 O 3 And CaO in a weight ratio of 100:1-2.
ZrO in the step A 2 The weight ratio of the stabilizer to the stabilizer is 100:4-6.
The anti-aging composition in the step A comprises HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (3) to (4) is 13-15:1.5-4:0.4-0.9:0.1-0.6:0.5-3.
The invention adds the anti-aging composition HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 And by controlling the addition amount of each oxide of the anti-aging composition, with ZrO 2 Forming complex multielement stable crystal phase and increasing oxygen vacancies, introducing trivalent cations and replacing Zr4+ to generate oxygen vacancies due to electricity price compensation, enriching around Zr4+ and generating local distortion; the introduction of cations with the same valence or different valence can lead the crystal lattice to generate distortion with different degrees because of different radii with Zr4+, thereby obviously improving the ageing resistance of the zirconia ceramics and obviously prolonging the service life of the ageing resistance yellow zirconium ceramics.
ZrO in the step A 2 The weight ratio of the anti-aging composition is 100:1.2-2.6.
In the step A: ball milling is carried out by adopting deionized water as a medium, wherein the balls adopted in ball milling are alumina balls, the mass ratio of powder to deionized water is 45-55:55, and the ball milling time is 24-72h.
In the step A: drying in an oven at 90-110deg.C, crushing, and sieving to obtain mixed powder.
The molding pressure of the cold isostatic pressing is 190-210MPa, and the pressure maintaining time is 170-190s.
In the step C: argon is adopted as the protective atmosphere, the sintering temperature is 1450-1500 ℃, and the heat preservation time is 2-3h.
The invention has the beneficial effects that: the anti-aging yellow zirconium ceramic produced by the preparation method of the anti-aging yellow zirconium ceramic has excellent bending strength, higher density and excellent anti-aging performance.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art.
Example 1
A preparation method of anti-aging yellow zirconium ceramic comprises the following steps:
A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder;
B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape;
C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic.
The stabilizer comprises Y 2 O 3 And CaO, Y 2 O 3 And CaO in a weight ratio of 100:1.
ZrO in the step A 2 The weight ratio of the stabilizer to the stabilizer is 100:4.
The anti-aging composition in the step A comprises HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (2) is 13:1.5:0.4:0.1:0.5.
ZrO in the step A 2 The weight ratio of the anti-aging composition is 100:1.2.
in the step A: ball milling is carried out by adopting deionized water as a medium, wherein balls adopted in ball milling are alumina balls, the mass ratio of powder to deionized water is 45:55, and the ball milling time is 24 hours.
In the step A: drying in an oven at 90 deg.c, crushing, and sieving to obtain mixed powder.
The molding pressure of the cold isostatic molding is 190MPa, and the pressure maintaining time is 170s.
In the step C: argon is adopted as the protective atmosphere, the sintering temperature is 1450 ℃, and the heat preservation time is 2 hours.
Example 2
A preparation method of anti-aging yellow zirconium ceramic comprises the following steps:
A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder;
B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape;
C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic.
The stabilizer comprises Y 2 O 3 And CaO, Y 2 O 3 And CaO in a weight ratio of 100:1.5.
ZrO in the step A 2 The weight ratio of the stabilizer to the stabilizer is 100:5.
The anti-aging composition in the step A comprises HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And (3) the methodTiO 2 The weight ratio of (2) to (2.5) to (0.7) to (0.35) to (1.5).
ZrO in the step A 2 The weight ratio of the anti-aging composition is 100:1.9.
in the step A: ball milling is carried out by adopting deionized water as a medium, wherein balls adopted in ball milling are alumina balls, the mass ratio of powder to deionized water is 50:55, and the ball milling time is 48 hours.
In the step A: drying in an oven at 100deg.C, crushing, and sieving to obtain mixed powder.
The molding pressure of the cold isostatic pressing is 200MPa, and the pressure maintaining time is 180s.
In the step C: argon is adopted as the protective atmosphere, the sintering temperature is 1480 ℃, and the heat preservation time is 2.5h.
Example 3
A preparation method of anti-aging yellow zirconium ceramic comprises the following steps:
A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder;
B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape;
C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic.
The stabilizer comprises Y 2 O 3 And CaO, Y 2 O 3 And CaO in a weight ratio of 100:2.
ZrO in the step A 2 The weight ratio of the stabilizer to the stabilizer is 100:6.
The anti-aging composition in the step A comprises HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 Weight of (2)The ratio was 15:4:0.9:0.6:3.
ZrO in the step A 2 The weight ratio of the anti-aging composition is 100:2.6.
in the step A: ball milling is carried out by adopting deionized water as a medium, wherein balls adopted in ball milling are alumina balls, the mass ratio of powder to deionized water is 55:55, and the ball milling time is 72 hours.
In the step A: drying in an oven at 110 deg.c, crushing, and sieving to obtain mixed powder.
The molding pressure of the cold isostatic molding is 210MPa, and the dwell time is 190s.
In the step C: argon is adopted as the protective atmosphere, the sintering temperature is 1500 ℃, and the heat preservation time is 3 hours.
Comparative example 1
The difference between this comparative example and example 1 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contains Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
Al in the anti-aging composition 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (2) is 1.5:0.4:0.1:0.5.
Comparative example 2
The difference between this comparative example and example 2 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contained HfO 2 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (2) is 14:0.7:0.35:1.5.
Comparative example 3
The difference between this comparative example and example 3 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contained HfO 2 、Al 2 O 3 、Cr 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (2) is 15:4:0.6:3.
Comparative example 4
The difference between this comparative example and example 1 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contained HfO 2 、Al 2 O 3 、Fe 2 O 3 And TiO 2 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 And TiO 2 The weight ratio of (2) is 13:1.5:0.4:0.5.
Comparative example 5
The difference between this comparative example and example 2 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contained HfO 2 、Al 2 O 3 、Fe 2 O 3 And Cr 2 O 3 。
HfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 And Cr 2 O 3 The weight ratio of (2) to (2.5) to (0.7) to (0.35).
Comparative example 6
The difference between this comparative example and example 3 is that: the anti-aging compositions employed are different.
The anti-aging composition used in this comparative example contains Al 2 O 3 。
Anti-aging Huang Gao ceramics having the same size and shape were produced by using the technical schemes of examples 1 to 3 and comparative examples 1 to 6 of the present invention, and the flexural strength, density and aging resistance of each anti-aging yellow zirconium ceramic were examined and recorded in the following table. And (3) ageing resistance detection: and placing the anti-aging yellow zirconium ceramic in a reaction kettle at 180 ℃ for hydrothermal aging treatment, and recording the nondestructive time of the anti-aging yellow zirconium ceramic, wherein the performance of the anti-aging yellow zirconium ceramic is about to be damaged.
Flexural Strength MPa | Density g/cm3 | Lossless time h | |
Example 1 | 1035 | 6.04 | 235.4 |
Example 2 | 1008 | 5.98 | 227.3 |
Example 3 | 1075 | 6.07 | 224.5 |
Comparative example 1 | 936 | 5.63 | 184.5 |
Comparative example 2 | 918 | 5.91 | 195.4 |
Comparative example 3 | 945 | 5.87 | 191.8 |
Comparative example 4 | 967 | 5.94 | 197.6 |
Comparative example 5 | 984 | 5.91 | 189.7 |
Comparative example 6 | 786 | 5.36 | 143.5 |
The above embodiments are preferred embodiments of the present invention, and besides, the present invention may be implemented in other ways, and any obvious substitution is within the scope of the present invention without departing from the concept of the present invention.
Claims (10)
1. A preparation method of anti-aging yellow zirconium ceramic is characterized by comprising the following steps: the method comprises the following steps:
A. ZrO (ZrO) 2 Adding the stabilizer and the anti-aging composition into ball milling equipment, ball milling until the mixture is uniform, and drying to obtain mixed powder;
B. and (3) forming: cold isostatic pressing the mixed powder to obtain a ceramic blank with a regular shape;
C. sintering: and placing the ceramic blank into sintering equipment, sintering under a protective atmosphere, and cooling to obtain the anti-aging yellow zirconium ceramic.
2. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: the stabilizer comprises Y 2 O 3 And CaO, Y 2 O 3 And CaO in a weight ratio of 100:1-2.
3. The method for preparing the anti-aging yellow zirconium ceramic according to claim 2, which is characterized in that: zrO in the step A 2 The weight ratio of the stabilizer to the stabilizer is 100:4-6.
4. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: the anti-aging composition in the step A comprises HfO 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 。
5. The method for preparing the anti-aging yellow zirconium ceramic according to claim 4, which is characterized in that: hfO in the anti-aging composition 2 、Al 2 O 3 、Fe 2 O 3 、Cr 2 O 3 And TiO 2 The weight ratio of (3) to (4) is 13-15:1.5-4:0.4-0.9:0.1-0.6:0.5-3.
6. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: zrO in the step A 2 The weight ratio of the anti-aging composition is 100:1.2-2.6.
7. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: in the step A: ball milling is carried out by adopting deionized water as a medium, wherein the balls adopted in ball milling are alumina balls, the mass ratio of powder to deionized water is 45-55:55, and the ball milling time is 24-72h.
8. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: in the step A: drying in an oven at 90-110deg.C, crushing, and sieving to obtain mixed powder.
9. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: the molding pressure of the cold isostatic pressing is 190-210MPa, and the pressure maintaining time is 170-190s.
10. The method for preparing the anti-aging yellow zirconium ceramic according to claim 1, which is characterized in that: in the step C: argon is adopted as the protective atmosphere, the sintering temperature is 1450-1500 ℃, and the heat preservation time is 2-3h.
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