CN113416064A - Zirconia/alumina ceramic composite material and preparation method thereof - Google Patents
Zirconia/alumina ceramic composite material and preparation method thereof Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 122
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 62
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 62
- 238000005245 sintering Methods 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 50
- 238000007731 hot pressing Methods 0.000 claims abstract description 43
- 239000011812 mixed powder Substances 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 33
- 239000000463 material Substances 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005299 abrasion Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 210000003298 dental enamel Anatomy 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 12
- 239000010439 graphite Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 230000035882 stress Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005452 bending Methods 0.000 description 4
- 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 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 230000006355 external stress Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 230000027311 M phase Effects 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000326 densiometry Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- -1 whiskers Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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Abstract
The invention relates to a zirconia/alumina ceramic composite material and a preparation method thereof, belonging to the technical field of alumina ceramics. The preparation method of the zirconia/alumina ceramic composite material comprises the following steps: reacting 3Y-ZrO2And Al2O3Carrying out vacuum hot-pressing sintering on the mixed powder, and cooling to obtain the powder; 3Y-ZrO in the mixed powder2And Al2O3The mass ratio of (A) to (B) is 15-65: 100. According to the preparation method of the zirconia/alumina ceramic composite material, due to the adoption of the hot-pressing sintering technology, the closed air holes are exhausted in the sintering preparation process of the material under the pressure promotion, the higher compactness can be realized in a shorter time or at a lower temperature, the interface performance of the material is optimized, and the performances of the zirconia/alumina ceramic composite material, such as friction, abrasion and the like, are obviously improved.
Description
Technical Field
The invention relates to a zirconia/alumina ceramic composite material and a preparation method thereof, belonging to the technical field of alumina ceramics.
Background
Al2O3The ceramic has the characteristics of high melting point, high hardness, wear resistance, corrosion resistance, low cost and the like, is an industrial ceramic material with the widest application range and the largest output in the world at present, and has wide application prospects in the fields of chemical industry, metallurgy, machinery, aerospace and the like. However, Al2O3The toughness of the ceramic is low, the brittleness is high, and in order to continuously expand the application field of the ceramic, a reinforcing phase is often required to be added to improve the toughness. The main toughening principle at present is Al2O3The microstructure of the ceramic incorporates various energy dissipation factors such as fibers, whiskers, particles, and the like. The principle of improving fracture toughness is that the introduced reinforcement can consume more energy when the material is fractured, and the current main toughening methods include: ZrO (ZrO)2Toughening, nanotechnology toughening, whisker and fiber toughening, particle dispersion toughening and the like.
ZrO2With Al2O3The ZTA ceramic is composed of two phases, is not a single solid solution, and the toughening mechanism can be summarized at present as follows: stress induced phase change toughening and microcrack toughening. Firstly, stress induced phase change toughening is carried out, and when partially stable tetragonal zirconia is dispersed in Al2O3In a ceramic matrix, i.e. tetragonal zirconia (t-ZrO) is present2) With monoclinic phase zirconia (m-ZrO)2) The reversible phase transition characteristic of (2) is that the transformation of the crystal structure is accompanied by 3-5% volume expansion. When the matrix is to ZrO2The particles have sufficient compressive stress while ZrO2Has a particle size sufficiently small that the phase transition temperature thereof can be reduced to below room temperature, so that ZrO becomes at room temperature2The tetragonal phase can still be maintained. When the material is subjected to external stress, the matrix is opposite to ZrO2Is relaxed to obtain ZrO2The particles immediately take t-m phaseAnd changing to form a phase change process area. Therefore, the stress-induced texture transformation consumes the external stress, reduces the stress intensity factor of the crack tip, and enables the crack which can continue to expand to terminate expansion due to the fact that the driving force is weakened due to energy consumption, and therefore the fracture toughness of the material is improved. This is ZrO2The stress induced phase change toughening. Second, microcrack toughening, t-ZrO2Dispersed in Al2O3When in the ceramic matrix, the particle diameter d is larger than dm(critical grain size of m-phase grains) crystal grains undergo t-m phase transformation during cooling, and microcrack is induced due to the significant volume effect. Thus, no matter ZrO2The phase change induced microcrack generated in the cooling process of the ceramic or the microcrack caused by the stress induced phase change formed in the tip region of the crack in the expansion process of the crack play a role in dispersing the energy of the tip of the main crack, thereby reducing the crack expansion driving force and improving the toughness of the material, which is called as microcrack toughening.
In the prior art with ZrO2Toughened Al2O3When the ceramic is used, 3Y-ZrO is usually used2(molar ratio of zirconia to yttria 97:3) to toughen Al2O3Ceramic, since 3% yttria can suppress ZrO2A drastic volume change resulting from the transition from monoclinic to tetragonal phase, resulting in ZrO2Better plays the role of toughening, but 3Y-ZrO is used in the prior art2To toughen Al2O3High sintering temperatures or/and pressures are often required to achieve high densification and high strength, thus limiting the industrial application of ZTA complex phase ceramics.
Disclosure of Invention
The invention aims to provide a preparation method of a zirconia/alumina ceramic composite material, which can obviously improve the strength and the compactness of the zirconia/alumina ceramic composite material while reducing the sintering temperature and the sintering pressure.
The invention also provides a zirconia/alumina ceramic composite material prepared by the preparation method.
In order to realize the purposes, the preparation method of the zirconia/alumina ceramic composite material adopts the technical scheme that:
a preparation method of a zirconia/alumina ceramic composite material comprises the following steps: reacting 3Y-ZrO2And Al2O3Carrying out vacuum hot-pressing sintering on the mixed powder, and cooling to obtain the powder; 3Y-ZrO in the mixed powder2And Al2O3The mass ratio of (A) to (B) is 15-65: 100.
The preparation method of the zirconia/alumina ceramic composite material of the invention controls 3Y-ZrO2And Al2O3The vacuum hot-pressing sintering technology is adopted, so that the sintering temperature and the sintering pressure can be reduced, the discharge of closed air holes in the sintering preparation process of the material can be promoted, the higher density can be realized in a shorter time or at a lower temperature, the interface performance of the material is optimized, and the performances of the zirconia/alumina ceramic composite material such as friction and wear are obviously improved.
The preparation method of the zirconia/alumina ceramic composite material applies external force to the mixed powder in the high-temperature sintering process by a hot-pressing sintering (HP) method, is beneficial to the mass transfer processes of contact, diffusion, flow and the like of powder particles, and reduces the sintering temperature and the pressure applied by sintering, thereby inhibiting the growth of crystal grains. The hot pressing method is easy to obtain a sintered body with the theoretical density and the porosity close to zero, a fine grain structure is easy to obtain, the orientation effect of the crystal is easy to realize, and the structure change of a high vapor compression subsystem is easy to control, so that a product with good mechanical property and electrical property is easy to obtain.
Preferably, the 3Y-ZrO in the mixed powder2And Al2O3The mass ratio of (A) to (B) is 35-65: 100.
Preferably, the temperature of the vacuum hot-pressing sintering is 1400-1750 ℃, and further preferably 1550-1750 ℃. The vacuum degree of the vacuum hot-pressing sintering is 10-2kPa。
Preferably, the rate of heating to the vacuum hot-pressing sintering temperature is 5-16 ℃/min, for example 10 ℃/min. And applying a pressure of 15-40 MPa to the mixed powder in the temperature rising process.
Preferably, the pressure of the vacuum hot-pressing sintering is 15-40 MPa.
Preferably, the time of the vacuum hot-pressing sintering is 0.5-2 hours, and preferably 1-2 hours.
Preferably, the preparation method of the mixed powder comprises the following steps: reacting 3Y-ZrO2Raw material powder and Al2O3And performing wet ball milling and mixing on the raw material powder, and then drying to obtain the powder. The 3Y-ZrO can be prepared by adopting wet ball milling2Raw material powder and Al2O3The raw material powder is mixed more uniformly. The dispersant adopted by the wet ball milling is ethanol. The wet ball milling adopts a planetary ball mill. The grinding balls adopted by the wet ball milling are agate balls.
Preferably, the revolution speed of the wet ball milling is 90-150 r/min, the rotation speed is 180-300 r/min, and the time is 180-300 min. The material ball ratio of the wet ball milling is 1: 1.5-4.
Preferably, the 3Y-ZrO2The average particle diameter of the raw material powder is 0.03 to 5 μm, preferably 0.5 to 2 μm, and more preferably 1 to 2 μm. The Al is2O3The average particle diameter of the raw material powder is 0.1 to 10 μm, and more preferably 0.5 to 1.5 μm.
Preferably, the drying treatment is drying in an air box for 8-12 hours, and then drying in an electric constant-temperature drying box at 80-100 ℃ for 8-16 hours.
The mould adopted by the hot-pressing sintering is a graphite mould. The cavity of the graphite mold can be in various shapes, such as a cylinder shape, and the diameter is preferably 20-50 mm. Preferably, the vacuum hot-pressing sintering is carried out in a hot-pressing sintering furnace, and the cooling is carried out to 150-250 ℃ along with the furnace, and then the air cooling is carried out. The hot pressing sintering furnace may be an oscillating pressure sintering furnace. And air cooling is to cool the mixture to room temperature along with air outside the furnace.
The technical scheme adopted by the zirconia/alumina ceramic composite material is as follows:
the zirconia/alumina ceramic composite material is prepared by the preparation method of the zirconia/alumina ceramic composite material.
The zirconia/alumina ceramic composite material has higher bending strength and frictional wear performance, and can be widely applied to the fields of chemical industry, metallurgy, machinery, aerospace and the like.
Drawings
FIG. 1 is an XRD spectrum of the zirconia/alumina ceramic composite materials prepared in example 1, example 3 and comparative example 1;
FIG. 2 is a SEM image of a fracture of the zirconia/alumina ceramic composite prepared in example 2;
FIG. 3 is a SEM image of a fracture of the zirconia/alumina ceramic composite prepared in example 4;
FIG. 4 is a SEM photograph of a fracture of the zirconia/alumina ceramic composite obtained in comparative example 2.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The preparation method of the zirconia/alumina ceramic composite material comprises the following steps:
1) 20g of 3Y-ZrO were taken2Raw material powder, 133g of Al2O3Raw material powder (3Y-ZrO)2Raw material powder and Al2O3The mass ratio of the raw material powder is 15:100) is put into two ball milling tanks, agate balls are put into each ball milling tank, the material-ball ratio is controlled to be 1:2, 150ml of absolute ethyl alcohol is added into each ball milling tank, the mixture is uniformly stirred and then is sealed and fixed in a planetary ball mill, and the programs are set for ball milling: the revolution speed of the ball mill is 120r/min, the rotation speed is 240r/min, and the time is 256 min; using 3Y-ZrO2The average particle diameter of the raw material powder was 0.5. mu.m, Al2O3The average particle size of the raw material powder was 0.5 μm;
after the ball milling is finished, the wet 3Y-ZrO bonded with the agate balls2And Al2O3Taking out the powder, filtering with 60 mesh sieve, drying in air oven for 12 hr, taking out the rectangular enamel plate, drying in heating enamel plate at 80 deg.C for 12 hr, and dryingThen the powder is taken out and sieved for a plurality of times to obtain dry and fine 3Y-ZrO2And Al2O3The mixed powder of (1);
2) taking 3Y-ZrO2And Al2O3The mixed powder 12g was charged into a graphite mold having an inner diameter of 30mm (the inner cavity of the mold was cylindrical), and the graphite mold charged with the mixed powder was placed in a hot-pressing sintering furnace under vacuum (degree of vacuum of 10)-2kPa), applying a constant pressure of 40MPa, heating to 1450 ℃ at a constant rate of 10 ℃/min, and maintaining the temperature and the pressure for 0.5h (namely, at a temperature of 1450 ℃, an application pressure of 40MPa and a vacuum degree of 10℃)-2And (3) carrying out vacuum hot-pressing sintering for 0.5h under kPa), closing a hot-pressing sintering furnace after the hot-pressing sintering is finished, taking out the mold to cool in the air when the temperature in the furnace is reduced to 150 ℃, and taking out the sample after the mold is slowly cooled to room temperature.
Example 2
The preparation method of the zirconia/alumina ceramic composite material comprises the following steps:
1) 20g of 3Y-ZrO were taken2Raw powder, 57.14g of Al2O3Raw material powder (3Y-ZrO)2Raw material powder and Al2O3The mass ratio of the raw material powder is 35:100) is put into two ball milling tanks, agate balls are put into each ball milling tank, the material-ball ratio is controlled to be 1:2, 150ml of absolute ethyl alcohol is added into each ball milling tank, the mixture is uniformly stirred and then is sealed and fixed in a planetary ball mill, and the programs are set for ball milling: the revolution speed of the ball mill is 120r/min, the rotation speed is 240r/min, and the time is 256 min; using 3Y-ZrO2The average particle diameter of the raw powder was 1 μm, Al2O3The average particle size of the raw material powder was 0.5 μm;
after the ball milling is finished, the wet 3Y-ZrO bonded with the agate balls2And Al2O3Taking out the powder, filtering the agate balls out by using a 60-mesh sieve, putting the powder into a rectangular enamel plate, putting the rectangular enamel plate into an air box for drying for 12 hours, taking out the rectangular enamel plate, putting the powder into a heating enamel plate, putting the heating enamel plate into an electric heating constant-temperature drying box for drying for 12 hours at the temperature of 80 ℃, taking out the powder after drying, and sieving the powder for multiple times to obtain the dry and fine 3Y-ZrO2And Al2O3The mixed powder of (1);
2) taking 3Y-ZrO2And Al2O3The mixed powder (11 g) was charged into a graphite mold having an inner diameter of 30mm (the inner cavity of the mold was cylindrical), and the graphite mold charged with the powder was placed in a hot-pressing sintering furnace under vacuum (degree of vacuum of 10)- 2kPa), applying a constant pressure of 40MPa, heating to 1550 ℃ at a constant rate of 10 ℃/min, and keeping the temperature and the pressure for 2h (namely, at the temperature of 1550 ℃, the applied pressure of 40MPa and the vacuum degree of 10℃)-2And (4) carrying out vacuum hot-pressing sintering for 2h under kPa), closing the hot-pressing sintering furnace after the hot-pressing sintering is finished, taking out the mold to cool in the air when the temperature in the furnace is reduced to 150 ℃, and taking out the sample after the mold is slowly cooled to room temperature.
Example 3
The preparation method of the zirconia/alumina ceramic composite material comprises the following steps:
the 3Y-ZrO prepared in example 2 was taken2And Al2O3The mixed powder (11 g) was charged into a graphite mold having an inner diameter of 30mm (the inner cavity of the mold was cylindrical), and the graphite mold charged with the powder was placed in a hot-pressing sintering furnace under vacuum (degree of vacuum of 10)-2kPa) under a constant pressure of 30MPa, then heating to 1650 ℃ at a constant rate of 10 ℃/min, and maintaining the temperature and pressure for 2h (namely, under the conditions of 1650 ℃, 30MPa of applied pressure and 10 degrees of vacuum)-2And (4) carrying out vacuum hot-pressing sintering for 2h under kPa), closing the hot-pressing sintering furnace after the hot-pressing sintering is finished, taking out the mold to cool in the air when the temperature in the furnace is reduced to 150 ℃, and taking out the sample after the mold is slowly cooled to room temperature.
Example 4
The preparation method of the zirconia/alumina ceramic composite material comprises the following steps:
1) 20g of 3Y-ZrO were taken2Raw powder, 30.77g of Al2O3Raw material powder (3Y-ZrO)2Raw material powder and Al2O3The mass ratio of the raw material powder is 65:100) is put into two ball milling tanks, agate balls are put into each ball milling tank, the material-ball ratio is controlled to be 1:2, and then the agate balls are added into each ball milling tank150ml of absolute ethyl alcohol is stirred uniformly and then is fixed in a planetary ball mill in a sealing way, and the ball milling is carried out by setting the program: the revolution speed of the ball mill is 120r/min, the rotation speed is 240r/min, and the time is 256 min; using 3Y-ZrO2The average particle diameter of the raw powder was 2 μm, Al2O3The average particle size of the raw material powder was 1.5 μm;
after the ball milling is finished, the wet 3Y-ZrO bonded with the agate balls2And Al2O3Taking out the powder, filtering the agate balls out by using a 60-mesh sieve, putting the powder into a rectangular enamel plate, putting the rectangular enamel plate into an air box for drying for 12 hours, taking out the rectangular enamel plate, putting the powder into a heating enamel plate, putting the heating enamel plate into an electric heating constant-temperature drying box for drying for 12 hours at the temperature of 80 ℃, taking out the powder after drying, and sieving the powder for multiple times to obtain the dry and fine 3Y-ZrO2And Al2O3The mixed powder of (1);
2) taking 3Y-ZrO2And Al2O3The mixed powder (10 g) was charged into a graphite mold having an inner diameter of 30mm (the inner cavity of the mold was cylindrical), and the graphite mold charged with the powder was placed in a hot-pressing sintering furnace under vacuum (degree of vacuum of 10)-2kPa), then the temperature is increased to 1750 ℃ at a constant speed of 10 ℃/min, the temperature and the pressure are kept for 1h (namely, the temperature is 1750 ℃, the applied pressure is 15MPa, and the vacuum degree is 10)-2And (4) carrying out vacuum hot-pressing sintering for 1h under kPa), closing the hot-pressing sintering furnace after the hot-pressing sintering is finished, taking out the mold to cool in the air when the temperature in the furnace is reduced to 150 ℃, and taking out the sample after the mold is slowly cooled to room temperature.
Comparative example 1
The preparation method of the zirconia/alumina ceramic composite material of the comparative example comprises the following steps:
the 3Y-ZrO prepared in example 1 was taken2And Al2O312g of the mixed powder (B) was charged into a graphite mold having an inner diameter of 30mm (the inner cavity of the mold was cylindrical), and the graphite mold charged with the powder was placed in a hot-pressing sintering furnace under vacuum conditions (degree of vacuum of 10)-2kPa) under a constant pressure of 30MPa, then the temperature is raised to 1350 ℃ at a constant speed of 10 ℃/min, and the temperature and the pressure are maintained for 1h (namely, the temperature is 1350 ℃; after the temperature is lowered,The applied pressure is 30MPa, the vacuum degree is 10-2And carrying out hot-pressing sintering for 1h under the condition of kPa (kPa), closing a hot-pressing sintering furnace after the hot-pressing sintering under the constant pressure of 30MPa is finished in the heat preservation period, taking out the mold to cool in the air when the temperature in the furnace is reduced to 150 ℃, and taking out a sample after the mold is slowly cooled to the room temperature.
Comparative example 2
The preparation method of the zirconia/alumina ceramic composite material of the comparative example comprises the following steps:
the 3Y-ZrO prepared in example 1 was taken2And Al2O3The mixed powder 12g is subjected to dry pressing forming with the diameter of 30mm under the pressure of 30MPa, then the formed biscuit is placed into a muffle furnace for pressureless sintering, the temperature is raised to 1450 ℃ at the constant speed of 10 ℃/min during temperature rising and is preserved for 1h (namely, the pressureless sintering is carried out for 1h at 1450 ℃), the muffle furnace is closed after the temperature preservation is finished, the mold is taken out when the temperature in the furnace is reduced to 150 ℃, the mold is cooled in the air, and the sample is taken out after the mold is slowly cooled to the room temperature.
Experimental example 1
3Y-ZrO prepared in example 1, example 3 and comparative example 1 was subjected to X-ray diffraction analysis (XRD)2/Al2O3The ceramic composite material is subjected to phase characterization, and then phase change of the raw material and the preparation process thereof and the final phase composition of the ceramic composite material are obtained through analysis, and the result is shown in fig. 1. As can be seen from the figure, the main crystal phase of the sample after hot-pressing sintering is Al2O3And ZrO2No other diffraction peak appeared, and 3Y-ZrO was also shown2And Al2O3In the preparation process of the mixed powder, other impurities are not introduced. Also, since the sintering temperature of comparative example 1 was 1350 deg.C, m-ZrO2There was still a residue, whereas in examples 1 and 3, m-ZrO2Is totally converted into t-ZrO2。
Experimental example 2
The 3Y-ZrO prepared in Experimental example 2, Experimental example 4 and comparative example 2 was examined and analyzed by Scanning Electron Microscope (SEM) model JSM-7001F using Japanese Electron (JEOL)2/Al2O3Microscopic morphology of ceramic composite block, as shown in FIG. 2 to E4. As can be seen from FIGS. 2 to 3, 3Y-ZrO produced in the examples2/Al2O3The ceramic composite material has higher density, 3Y-ZrO2With Al2O3The crystal grains are tightly combined, the crystal grains are uniformly distributed, the internal structure is compact, and no obvious air hole exists. As can be seen from FIG. 4, 3Y-ZrO produced in comparative example2/Al2O3The ceramic composite material has relatively more air holes and lower density than the former two.
Experimental example 3
3Y-ZrO prepared in examples 1 to 4 and comparative examples 1 to 2 were measured by Archimedes densitometry2/Al2O3Bulk density of the ceramic composite. The ratio of actual to theoretical density was then calculated to give the relative density, and the results are shown in table 1.
TABLE 1 3Y-ZrO prepared in examples 1 to 4 and comparative examples 1 to 22/Al2O3Bulk and relative density of ceramic composites
As can be seen from Table 1, 3Y-ZrO2/Al2O3Densification of ceramic composite Material with temperature variation during sintering, 3Y-ZrO obtained in examples 3 and 42/Al2O3The ceramic composite materials (sintering temperature 1650 ℃ and 1750 ℃ respectively) have the largest and not big difference in relative density, and the 3Y-ZrO prepared in the example 1 and the example 22/Al2O3Ceramic composite materials (sintering temperatures 1450 ℃ C. and 1550 ℃ C., respectively) having relative density ratios of 3Y-ZrO prepared in examples 3 and 42/Al2O3The ceramic composite is slightly lower. 3Y-ZrO produced in comparative example 1 (sintering temperature 1350 ℃ C.) and comparative example 2 (pressureless sintering 1450 ℃ C.)2/Al2O3Ceramic composites are the lowest in density because the sintering temperature of 1350 c is too low, and pressureless sintered articles are less dense than hot pressed sintering.
Experimental example 4
The 3Y-ZrO prepared in examples 1 to 4 and comparative examples 1 to 2 were subjected to a universal testing machine2/Al2O3The ceramic composite was subjected to a frictional wear test and then the average coefficient of friction of the material was calculated and the results are shown in table 2. From Table 2, it can be seen that 3Y-ZrO of comparative example2/Al2O3The average friction coefficient of the ceramic composite material is higher than that of the 3Y-ZrO of the embodiment2/Al2O3A ceramic composite material.
TABLE 2 3Y-ZrO prepared in examples 1 to 4 and comparative examples 1 to 22/Al2O3Average coefficient of friction of ceramic composite
| Average coefficient of friction | |
| Example 1 | 0.288 |
| Example 2 | 0.231 |
| Example 3 | 0.123 |
| Example 4 | 0.307 |
| Comparative example 1 | 0.402 |
| Comparative example 2 | 0.299 |
Experimental example 5
Testing the 3Y-ZrO prepared in the examples 1-4 and the comparative examples 1-2 by using the national abrasive tool quality supervision and inspection center according to the GB/T6569-2006 fine ceramic bending strength experimental method2/Al2O3The flexural strength of the ceramic composite material is shown in Table 3. As is clear from Table 3, 3Y-ZrO obtained in example 32/Al2O3The bending strength of the ceramic composite material is the highest and is 1250 MPa.
TABLE 3Y-ZrO prepared in examples 1 to 4 and comparative examples 1 to 22/Al2O3Bending strength of ceramic composite material
Claims (10)
1. A preparation method of a zirconia/alumina ceramic composite material is characterized by comprising the following steps: the method comprises the following steps: reacting 3Y-ZrO2And Al2O3Carrying out vacuum hot-pressing sintering on the mixed powder, and cooling to obtain the powder; 3Y-ZrO in the mixed powder2And Al2O3The mass ratio of (A) to (B) is 15-65: 100.
2. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: the temperature of the vacuum hot-pressing sintering is 1400-1750 ℃.
3. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: the rate of heating to the vacuum hot-pressing sintering temperature is 5-16 ℃/min.
4. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: the pressure of the vacuum hot-pressing sintering is 15-40 MPa.
5. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: the time of the vacuum hot-pressing sintering is 0.5-2 h.
6. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: the preparation method of the mixed powder comprises the following steps: reacting 3Y-ZrO2Raw material powder and Al2O3And performing wet ball milling and mixing on the raw material powder, and then drying to obtain the powder.
7. The method for preparing a zirconia/alumina ceramic composite according to claim 6, characterized in that: the 3Y-ZrO2The average particle diameter of the raw material powder is 0.03-5 mu m, and the Al is2O3The average particle diameter of the raw material powder is 0.1 to 10 μm.
8. The method for producing a zirconia/alumina ceramic composite according to claim 6 or 7, characterized in that: the wet ball milling adopts a planetary ball mill, the revolution speed of the wet ball milling is 90-150 r/min, the rotation speed is 180-300 r/min, and the time is 180-300 min.
9. The method for preparing a zirconia/alumina ceramic composite according to claim 1, characterized in that: and the vacuum hot-pressing sintering is carried out in a hot-pressing sintering furnace, and the cooling is carried out to 150-250 ℃ along with the furnace, and then the air cooling is carried out.
10. A zirconia/alumina ceramic composite material prepared by the method for preparing the zirconia/alumina ceramic composite material according to any one of claims 1 to 9.
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