CN113105216A - Injection-molded zirconium-aluminum composite ceramic and preparation method thereof - Google Patents
Injection-molded zirconium-aluminum composite ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- DNXNYEBMOSARMM-UHFFFAOYSA-N alumane;zirconium Chemical compound [AlH3].[Zr] DNXNYEBMOSARMM-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000001746 injection moulding Methods 0.000 claims abstract description 34
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 44
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 19
- 235000015895 biscuits Nutrition 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 14
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 12
- 238000000748 compression moulding Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 4
- 239000003292 glue Substances 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 230000009466 transformation Effects 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000013001 point bending Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Abstract
The invention provides an injection-molded zirconium-aluminum composite ceramic and a preparation method thereof, wherein the preparation method comprises the steps of mixing 70-80 parts of 95 porcelain aluminum oxide, 1-30 parts of zirconium oxide, 1-5 parts of yttrium oxide, 1-2 parts of lanthanum oxide and 1-10 parts of polyvinyl butyral (PVB), ball-milling by taking deionized water as a solvent to obtain ceramic slurry, drying by a vacuum drying furnace, grinding to obtain ceramic powder, injection-molding to prepare a ceramic blank, and sintering in a high-pressure sintering furnace with protective atmosphere introduced to remove glue to obtain the zirconium-aluminum composite ceramic. The zirconium-aluminum composite ceramic prepared by the invention has the advantages of simple preparation method, good ceramic wear resistance, high fracture toughness and high bending strength.
Description
Technical Field
The invention relates to the field of ceramic materials, and in particular relates to injection-molded zirconium-aluminum composite ceramic and a preparation method thereof.
Background
ZTA is a novel complex phase ceramic material which takes alumina as a matrix and partially stable zirconia as a reinforcing and toughening phase. Because of its advantages of high strength, high hardness, corrosion resistance and low cost, it is widely used in high-temperature, mechanical and electronic fields. The mechanical property of ZTA ceramic is superior to that of single-component ceramic, and ZrO is utilized2Although the phase transformation toughening can greatly improve the brittleness of the ceramic, the single phase strengthens and toughens the Al2O3The wear resistance of the ceramic is still to be improved, and due to the difference of physical parameters of the additive phase and the matrix material, the toughening and the reinforcement of the material cannot be achieved at the same time. With the development of special ceramics, ZTA ceramics can not meet the requirements of special fields such as aerospace, transportation and the like. However, the mechanical property and the wear resistance of the ZTA ceramic material can be effectively improved by utilizing the coupling of multi-element synergistic strengthening and a plurality of toughening mechanisms, which brings a new hope for the ZTA ceramic.
In ZTA ceramics, Al2O3ZrO is uniformly distributed on the substrate2Particles, ZrO due to some particular stage with increasing or decreasing temperature2The particles can generate phase transformation, the phase transformation belongs to martensite phase transformation, volume expansion and shear strain are correspondingly generated, adverse defects such as tensile stress and microcrack are caused, the internal porosity of the material is increased due to the generation of the defects, the relative density is reduced, and ZrO is greatly influenced2The ceramic phase transformation toughening effect. However, the phenomenon can be effectively improved by adding rare earth oxide into ZTA ceramic, and the mechanical property of the ZTA ceramic is improved. In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide injection-molded zirconium-aluminum composite ceramic and a preparation method thereof, and the zirconium-aluminum composite ceramic with good fracture toughness, large bending strength and good wear resistance can be prepared.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: a preparation method of injection-molded zirconium-aluminum composite ceramic comprises the following steps: step 1, mixing 60-80 parts of alumina, 1-30 parts of zirconia, 1-5 parts of yttria, 1-2 parts of lanthanum oxide and 1-10 parts of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
step 2, dispersing the mixed material obtained in the step 1 in deionized water by taking the deionized water as a solvent, and performing ball milling to obtain ceramic slurry;
step 3, drying and grinding the ceramic slurry obtained in the step 2, sieving to obtain ceramic powder, and pressing and forming the ceramic powder;
and 4, sintering the biscuit to obtain an initial plate sample, and polishing the initial plate sample to obtain a finished product.
Further, in the step 1, the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, the particle size range is 1-2 mu m, and the density is 3.96g/cm3The purity is 99.9-100%.
Further, in step 1, the zirconia is yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
Further, in the step 1, the purity of the lanthanum oxide is 99.9-100%, and the density is 6.41g/cm3The particle size range is 1 to 1.5 μm.
Further, in the step 2, the rotation speed of the ball milling is 250-300 r/min, and the ball milling time is 10-12 h.
Further, in step 3, the drying and screening specifically includes the following operations: and taking out the slurry, drying, carrying out vacuum drying at the temperature of 60-100 ℃, grinding the completely dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder.
Further, in the step 3, the compression molding adopts an injection molding method, the prepared ceramic powder is subjected to injection molding, the injection molding pressure in the injection molding is 0-0.7MPa, the mold temperature is 10-60 ℃, the injection molding temperature is 60-70 ℃, the melt temperature is 200-280 ℃, and the highest melt temperature is 300 ℃, so that the ceramic biscuit is obtained.
Further, in the step 4, rubber is discharged from the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere, the temperature in the rubber discharging process is 400-480 ℃, and the rubber is discharged for 5-9 hours; and (3) heating to 1500 ℃ at the speed of 1-2 ℃/min in a high-temperature sintering furnace, and sintering for 1-3 h to obtain a ceramic blank.
The injection-molded zirconium-aluminum composite ceramic is prepared by the preparation method.
Compared with the prior art, the injection-molded zirconium-aluminum composite ceramic and the preparation method thereof adopting the technical scheme have the following beneficial effects:
the injection-molded zirconium-aluminum composite ceramic and the preparation method thereof are adopted, wherein alpha-phase alumina and zirconia are used as raw materials, yttrium oxide and lanthanum oxide rare earth oxide are added, and a small amount of PVB (polyvinyl butyral) binder is matched for hot-pressing sintering in a protective atmosphere after injection molding, so that the zirconium-aluminum composite ceramic with good fracture toughness, large bending strength and good wear resistance is prepared;
secondly, in the preparation method of the zirconium-aluminum composite ceramic, the raw materials are not required to be treated, the production cost is low, the process is simple and convenient, and the production period is short;
and thirdly, rare earth oxide, namely yttrium oxide/lanthanum oxide, is added to prevent the volume expansion caused by irregular phase change of ZrO2 in the zirconium-aluminum composite ceramic material and promote the formation of metastable t-ZrO2 so as to improve the mechanical property.
Drawings
FIG. 1 is a scanning electron microscope image of an injection-molded zirconium-aluminum composite ceramic according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction chart of the zirconium aluminum composite ceramic injection-molded in this example.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The first embodiment is as follows:
a preparation method of injection-molded zirconium-aluminum composite ceramic comprises the following steps: the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, the particle size range is 1-2 mu m, and the density is 3.96g/cm3The purity is 99.9-100%. The lanthanum oxide has a purity of 99.9-100% and a density of 6.41g/cm3The particle size range is 1 to 1.5 μm. The zirconia is yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
Step 1, mixing 60g of alpha-alumina, 30g of zirconia, 2g of yttria, 3g of lanthanum oxide and 5g of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
and 2, dispersing the mixed material obtained in the step 1 in deionized water by taking deionized water as a solvent, and carrying out ball milling to obtain ceramic slurry, wherein the ball milling rotation speed is 300r/min, and the ball milling time is 12 hours.
And 3, drying and grinding the ceramic slurry obtained in the step 2, taking out the slurry, drying, carrying out vacuum drying at the temperature of 70 ℃, grinding the thoroughly dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder. And then, carrying out compression molding on the ceramic powder, wherein in the embodiment, the compression molding adopts an injection molding method, and the prepared ceramic powder is subjected to injection molding, wherein the injection molding pressure in the injection molding is 0.2MPa, the mold temperature is 30 ℃, the injection molding temperature is 60 ℃, the melt temperature is 200 ℃, and the highest melt temperature is 300 ℃ to obtain the ceramic biscuit.
Step 4, sintering the biscuit to obtain an initial plate sample, and discharging the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere at the temperature of 400 ℃ for 5 hours; heating to 1500 ℃ at the speed of 1 ℃/min in a high-temperature sintering furnace, sintering for 1.5h to obtain a ceramic blank, and polishing and grinding the initial plate sample to obtain a finished product.
An injection-molded zirconium-aluminum composite ceramic is prepared by adopting the preparation method. The density of the prepared zirconium-aluminum composite ceramic is 5.09g/cm3And testing the flexural strength of the zirconium-aluminum composite ceramic by adopting a three-point bending method to be 15.4 Gpa. Analyzing the phase composition of the sintered body by using an X-ray diffractometer; and observing the microstructure of the section of the zirconium-aluminum composite ceramic by adopting a scanning electron microscope.
Example two:
a preparation method of injection-molded zirconium-aluminum composite ceramic comprises the following steps: the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, and the grain size range thereof1 to 2 μm, and a density of 3.96g/cm3The purity is 99.9-100%. The lanthanum oxide has a purity of 99.9-100% and a density of 6.41g/cm3The particle size range is 1 to 1.5 μm. The zirconia is yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
Step 1, mixing 65g of alpha-alumina, 25g of zirconia, 2g of yttria, 3g of lanthanum oxide and 5g of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
and 2, dispersing the mixed material obtained in the step 1 in deionized water by taking deionized water as a solvent, and carrying out ball milling to obtain ceramic slurry, wherein the rotating speed of the ball milling is 280r/min, and the ball milling time is 12 hours.
And 3, drying and grinding the ceramic slurry obtained in the step 2, taking out the slurry, drying, carrying out vacuum drying at the temperature of 70 ℃, grinding the thoroughly dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder. And then, carrying out compression molding on the ceramic powder, wherein in the embodiment, the compression molding adopts an injection molding method, and the prepared ceramic powder is subjected to injection molding, wherein the injection molding pressure in the injection molding is 0.4MPa, the mold temperature is 40 ℃, the injection molding temperature is 60 ℃, the melt temperature is 220 ℃, and the highest melt temperature is 300 ℃ to obtain the ceramic biscuit.
Step 4, sintering the biscuit to obtain an initial plate sample, and discharging the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere at the temperature of 420 ℃ for 6 hours; heating to 1500 ℃ at the speed of 1.5 ℃/min in a high-temperature sintering furnace, sintering for 2h to obtain a ceramic blank, and polishing and grinding the initial plate sample to obtain a finished product.
An injection-molded zirconium-aluminum composite ceramic is prepared by adopting the preparation method. The density of the prepared zirconium-aluminum composite ceramic is 5.05g/cm3And testing the flexural strength of the zirconium-aluminum composite ceramic by a three-point bending method to be 16.8 GPa. Analyzing the phase composition of the sintered body by using an X-ray diffractometer; and observing the microstructure of the section of the zirconium-aluminum composite ceramic by adopting a scanning electron microscope.
Example three:
injection-molded zirconium-aluminum composite potteryThe preparation method of the porcelain comprises the following steps: the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, the particle size range is 1-2 mu m, and the density is 3.96g/cm3The purity is 99.9-100%. The lanthanum oxide has a purity of 99.9-100% and a density of 6.41g/cm3The particle size range is 1 to 1.5 μm. The zirconia is yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
Step 1, mixing 70g of alpha-alumina, 20g of zirconia, 2g of yttria, 3g of lanthanum oxide and 5g of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
and 2, dispersing the mixed material obtained in the step 1 in deionized water by taking deionized water as a solvent, and carrying out ball milling to obtain ceramic slurry, wherein the rotating speed of the ball milling is 280r/min, and the ball milling time is 12 hours.
And 3, drying and grinding the ceramic slurry obtained in the step 2, taking out the slurry, drying, carrying out vacuum drying at the temperature of 70 ℃, grinding the thoroughly dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder. And then, carrying out compression molding on the ceramic powder, wherein in the embodiment, the compression molding adopts an injection molding method, and the prepared ceramic powder is subjected to injection molding, wherein the injection molding pressure in the injection molding is 0.5MPa, the mold temperature is 40 ℃, the injection molding temperature is 65 ℃, the melt temperature is 250 ℃, and the highest melt temperature is 300 ℃ to obtain the ceramic biscuit.
Step 4, sintering the biscuit to obtain an initial plate sample, and discharging the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere at the temperature of 450 ℃ for 7 hours; heating to 1500 ℃ at the speed of 1.5 ℃/min in a high-temperature sintering furnace, sintering for 2h to obtain a ceramic blank, and polishing and grinding the initial plate sample to obtain a finished product.
An injection-molded zirconium-aluminum composite ceramic is prepared by adopting the preparation method. The density of the prepared zirconium-aluminum composite ceramic is 4.91g/cm3And testing the flexural strength of the zirconium-aluminum composite ceramic by a three-point bending method to be 17.1 GPa. Analyzing the phase composition of the sintered body by using an X-ray diffractometer; and observing the microstructure of the section of the zirconium-aluminum composite ceramic by adopting a scanning electron microscope.
Example four:
a preparation method of injection-molded zirconium-aluminum composite ceramic comprises the following steps: the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, the particle size range is 1-2 mu m, and the density is 3.96g/cm3The purity is 99.9-100%. The lanthanum oxide has a purity of 99.9-100% and a density of 6.41g/cm3The particle size range is 1 to 1.5 μm. The zirconia is yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
Step 1, mixing 75g of alpha-alumina, 15g of zirconia, 2g of yttria, 3g of lanthanum oxide and 5g of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
and 2, dispersing the mixed material obtained in the step 1 in deionized water by taking deionized water as a solvent, and carrying out ball milling to obtain ceramic slurry, wherein the ball milling rotation speed is 250r/min, and the ball milling time is 11 hours.
And 3, drying and grinding the ceramic slurry obtained in the step 2, taking out the slurry, drying, carrying out vacuum drying at the temperature of 90 ℃, grinding the thoroughly dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder. And then, carrying out compression molding on the ceramic powder, wherein in the embodiment, the compression molding adopts an injection molding method, and the prepared ceramic powder is subjected to injection molding, wherein the injection molding pressure in the injection molding is 0.7MPa, the mold temperature is 60 ℃, the injection molding temperature is 70 ℃, the melt temperature is 280 ℃, and the highest melt temperature is 300 ℃ to obtain the ceramic biscuit.
Step 4, sintering the biscuit to obtain an initial plate sample, and discharging the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere at 480 ℃ for 8 hours; heating to 1500 ℃ at the speed of 2 ℃/min in a high-temperature sintering furnace, sintering for 2h to obtain a ceramic blank, and polishing and grinding the initial plate sample to obtain a finished product.
An injection-molded zirconium-aluminum composite ceramic is prepared by adopting the preparation method. The density of the prepared zirconium-aluminum composite ceramic is 4.81g/cm3And testing the flexural strength of the zirconium-aluminum composite ceramic by a three-point bending method to be 15.6 GPa. Using X-ray diffractometerSeparating out the phase composition of the sintered body; and observing the microstructure of the section of the zirconium-aluminum composite ceramic by adopting a scanning electron microscope.
As shown in fig. 1, which is a scanning electron microscope image of the injection-molded zirconium-aluminum composite ceramic, after sintering, the addition of rare earth oxide can effectively hinder the unstable crystal transformation of ZrO2 and promote the formation of metastable t-ZrO 2. As shown in fig. 2, the X-ray diffraction pattern of the injection-molded zirconium-aluminum composite ceramic is shown in fig. 2, the zirconium-aluminum composite ceramic is prone to microcrack under the action of frictional stress, and the addition of the rare earth oxide yttrium oxide/lanthanum oxide can effectively promote the formation of a good microstructure of the zirconium-aluminum composite ceramic material.
The alpha-phase alumina and zirconia are used as raw materials, yttrium oxide and lanthanum oxide rare earth oxide are added, and a small amount of PVB (polyvinyl butyral) binder is matched for injection molding and then hot pressing sintering in a protective atmosphere, so that the zirconium-aluminum composite ceramic with good fracture toughness, large bending strength and good wear resistance is prepared.
The preparation method of the invention does not need to process the raw materials, has low production cost, simple and convenient process and short production period. The rare earth oxide is added in the preparation method, so that the volume expansion caused by irregular phase change of ZrO2 in the zirconium-aluminum composite ceramic material can be prevented, and the formation of the metastable t-ZrO2 is promoted to improve the mechanical property.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (9)
1. A preparation method of injection-molded zirconium-aluminum composite ceramic is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing 60-80 parts of alumina, 1-30 parts of zirconia, 1-5 parts of yttria, 1-2 parts of lanthanum oxide and 1-10 parts of polyvinyl butyral (PVB), and uniformly mixing to obtain a mixed material;
step 2, dispersing the mixed material obtained in the step 1 in deionized water by taking the deionized water as a solvent, and performing ball milling to obtain ceramic slurry;
step 3, drying and grinding the ceramic slurry obtained in the step 2, sieving to obtain ceramic powder, and pressing and forming the ceramic powder;
and 4, sintering the biscuit to obtain an initial plate sample, and polishing the initial plate sample to obtain a finished product.
2. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in the step 1, the alumina adopts 95 porcelain alumina, the 95 porcelain alumina is alpha-Al 2O3, the particle size range is 1-2 mu m, and the density is 3.96g/cm3The purity is 99.9-100%.
3. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in step 1, the zirconia was yttria partially stabilized zirconia (3Y-ZrO2) having a particle size in the range of 50nm and a density of 5.89g/cm3The purity of the powder is 99.9-100%.
4. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in step 1, the lanthanum oxide has a purity of 99.9-100% and a density of 6.41g/cm3The particle size range is 1 to 1.5 μm.
5. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in the step 2, the rotation speed of the ball milling is 250-300 r/min, and the ball milling time is 10-12 h.
6. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in step 3, the drying and screening specifically comprises the following operations: and taking out the slurry, drying, carrying out vacuum drying at the temperature of 60-100 ℃, grinding the completely dried powder, and sieving with a 100-mesh sieve to obtain the ceramic powder.
7. The method of claim 6, wherein the injection-molded zirconium-aluminum composite ceramic comprises: in the step 3, the compression molding adopts an injection molding method, the prepared ceramic powder is subjected to injection molding, the injection molding pressure in the injection molding is 0-0.7MPa, the mold temperature is 10-60 ℃, the injection molding temperature is 60-70 ℃, the melt temperature is 200-280 ℃, and the highest melt temperature is 300 ℃, so that the ceramic biscuit is obtained.
8. The method of preparing an injection-molded zirconium aluminum composite ceramic according to claim 1, wherein: in the step 4, rubber is discharged from the ceramic biscuit in a high-pressure sintering furnace in a protective atmosphere, the temperature in the rubber discharging process is 400-480 ℃, and the rubber is discharged for 5-9 hours; and (3) heating to 1500 ℃ at the speed of 1-2 ℃/min in a high-temperature sintering furnace, and sintering for 1-3 h to obtain a ceramic blank.
9. The utility model provides an injection moulding's zirconium aluminium composite ceramic which characterized in that: prepared by the preparation method of any one of claims 1 to 8.
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