CN110981521A - ZrO2Al synergistically toughened with TiC2O3Base ceramic material and preparation method thereof - Google Patents
ZrO2Al synergistically toughened with TiC2O3Base ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention aims to strengthen Al by combining three means of phase change toughening, fiber toughening and particle toughening in the prior art2O3The way of the base ceramic has not been researched, and provides a ZrO2Al synergistically toughened with TiC2O3A base ceramic material and a preparation method thereof, belonging to the field of ceramic materials. The ceramic material comprises the following components in percentage by volume: ZrO (ZrO)25-20% of whiskers, 5-10% of TiC nano particles and MnO20.5～3％，Y2O30 to 1% and the balance of Al2O3. The ceramic material is Al2O3Adding ZrO into matrix2Whisker and TiC nano-particles, and provides a high-hardness, high-strength and high-strength alloy by reasonable material formula and processWear-resistant and toughness-advantageous Al2O3A base ceramic material.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to ZrO2Al toughened by whisker and TiC nano-particle in cooperation2O3A base ceramic material and a preparation method.
Background
With the gradual improvement of the mechanical property of new materials, the mechanical cutting efficiency is difficult to ensure, so that a new challenge is provided for the wear resistance of the cutter material. The advanced ceramic cutter material has the advantages of high hardness, high wear resistance, high heat resistance, high corrosion resistance and the like, but has large brittleness, and the toughness and the bending strength are inferior to those of the traditional hard alloy cutter material. However, the price of cemented carbide cutting tools is increasing today when metal resources such as tungsten and cobalt, which are main components of the materials, are scarce. Therefore, it is a work focus of researchers to improve the toughness and bending strength of ceramic cutting tool materials and to enable the ceramic cutting tool materials to replace hard alloy cutting tool materials.
The common toughening method for the alumina ceramic mainly comprises the modes of particle toughening, phase change toughening, fiber toughening, in-situ growth toughening, composite synergistic toughening and the like. At present, the method for improving the toughness of the Al2O 3-based ceramic material by adopting a composite mode of multiple toughening mechanisms is widely concerned, and the main methods are as follows: multiphase particle composite toughening, fiber-particle composite toughening and the like. The multiphase particle composite toughening is to utilize reinforcing phase particles with different sizes to achieve the aim of multiphase composite toughening; the whisker-particle composite toughening is that Al is provided by utilizing the plastic deformation and bridging of metal particles, the energy consumed by debonding and pulling out of the whisker under stress and the deflection of cracks of the whisker-particle composite toughening2O3Mechanical property of base ceramic material. Patent CN1148580A proposes a method for using SiCwWhiskers and SiCpParticle synergistically enhanced Al2O3Ceramic materials and processing techniques thereof, but the performance improvement is limited; patent CN107673772A proposes Al added with zirconium oxide whisker2O3the/Ti (C, N) nano composite ceramic cutting tool material and its preparation method have obtained good effect, but its base body is Al2O3A Ti (C, N) nanocomposite; patent CN102557702A proposes a titanium boride whisker and particle synergetic toughening titanium nitride-based ceramic cutter material and a preparation method thereof, and achieves good performance in the aspect of synergetic toughening of ceramic cutters.
However, Al is enhanced by combining three means of phase change toughening, fiber toughening and particle toughening2O3The manner of the base ceramic has not been studied.
Disclosure of Invention
The invention aims to strengthen Al by combining three means of phase change toughening, fiber toughening and particle toughening in the prior art2O3The way of the base ceramic has not been researched, and provides a ZrO2Al synergistically toughened with TiC2O3A base ceramic material and a preparation method. The ceramic material is Al2O3Adding ZrO into matrix2Whisker and TiC nano-particles, and provides Al with high hardness, high strength, high wear resistance and toughness advantage through reasonable material formula and process2O3A base ceramic material.
ZrO (ZrO)2Al synergistically toughened with TiC2O3The ceramic material comprises the following components in percentage by volume: ZrO (ZrO)25-20% of whiskers, 5-10% of TiC nano particles and MnO20.5～3％，Y2O30 to 1% and the balance of Al2O3；
The ZrO2The average diameter of the crystal whisker is 0.1-5 μm, and the average length is 10-100 μm;
the average grain size of the TiC nano particles is 30-100 nm;
the Al is2O3The average particle size is 100-800 nm;
the MnO2The average particle size is 100-800 nm;
said Y2O3The average particle diameter is 1 to 3 μm.
Al mentioned above2O3The preparation method of the base ceramic material comprises the following steps:
(1) taking ethanol and polyethylene glycol mixed solution as a dispersion medium, and measuring ZrO in proportion2Whisker and TiC nano-particle, and respectively carrying out first ultrasonic oscillation treatment on the whisker and the TiC nano-particle in a dispersion medium, and then carrying out ZrO treatment on the whisker and the TiC nano-particle2Mixing the whisker dispersion liquid and the TiC nano-particle dispersion liquid, and then carrying out secondary ultrasonic oscillation treatment;
(2) mixing Al2O3、MnO2And Y2O3Or Al2O3And MnO2The mixed powder is ball milled for the first time in deionized water, and then the treated ZrO is added2Mixing the crystal whisker and the TiC nano-particle dispersion liquid, carrying out secondary ball milling, and drying;
(3) sieving the dried powder to obtain uniformly mixed composite powder;
(4) putting the sieved composite powder into a graphite die for hot-pressing sintering molding to obtain Al2O3A base ceramic material.
In the preparation method, the volume ratio of the ethanol to the polyethylene glycol dispersion medium in the step (1) is 25-35: 1.
In the preparation method, the first ultrasonic oscillation treatment time in the step (1) is 20-30 min, and the second ultrasonic oscillation treatment time is 10-20 min.
In the preparation method, when the ball milling is carried out for the first time in the step (2), the volume ratio of the mixed powder, the milling balls and the deionized water is 1: 6-9: 1.5-3.
In the preparation method, the ball milling treatment time of the two times in the step (2) is 15-30 h.
In the preparation method, the sieving in the step (3) is a 100-mesh sieve.
In the preparation method, the hot-pressing sintering temperature in the step (4) is 1600-1900 ℃, the pressure is 30-50 MPa, and the heat preservation time is 1-2 h.
Al prepared by the preparation method2O3The hardness of the base ceramic material is 1431 to 1771HV, the bending strength is 810 to 950MPa, and the fracture toughness is 7.1 to 8.7 MPa.m1/2。
Compared with the prior art, the invention has the advantages that:
the invention combines three means of phase change toughening, fiber toughening and particle toughening, and Al2O3ZrO added to base ceramic material2The crystal whisker has the effects of phase change toughening and fiber toughening, the TiC nano particles have the effect of particle toughening, and nano MnO is added2And Y2O3Is a sintering aid, has synergistic effect of multiple toughening mechanisms, obviously improves the mechanical property and can greatly improve the Al2O3The fracture toughness and the bending strength of the ceramic cutter are improved, so that the service life of the material can be effectively prolonged, and the cost performance of the material is greatly improved.
Drawings
FIG. 1 ZrO in inventive example 12Al toughened by whisker and TiC nano-particle in cooperation2O3SEM pictures of fracture toughness fractures of the base ceramic materials;
FIG. 2 ZrO in example 2 of the present invention2Al toughened by whisker and TiC nano-particle in cooperation2O3SEM pictures of fracture toughness fracture of base ceramic materials.
Detailed Description
ZrO in the examples2Whiskers, TiC nanoparticles, MnO2，Y2O3，Al2O3Are all commercially available. ZrO (ZrO)2The average diameter of the crystal whisker is 0.1-5 μm, and the average length is 10-100 μm; the average grain size of the TiC nano particles is 30-100 nm; al (Al)2O3The average particle size is 100-800 nm; MnO2The average particle size is 100-800 nm; y is2O3The average particle diameter is 1 to 3 μm.
Example 1
Al2O3Measuring ZrO based on the ceramic material25mL of whisker, 5mL of TiC nano-particle and MnO22mL，Y2O30.5mL，Al2O387.5mL。
The preparation method comprises the following steps:
(1) ethanol and polyethylene glycol 300 are used as dispersion media, the volume ratio of the ethanol to the polyethylene glycol is 30: 1, and the total volume is 62 mL;
(2) ZrO 2 is mixed with2Respectively carrying out ultrasonic oscillation treatment on the whiskers and the TiC nano particles in a dispersion medium for 20min, mixing the two dispersions, and carrying out ultrasonic oscillation treatment for 15 min;
(3) mixing Al2O3、MnO2And Y2O3Ball-milling the powder in deionized water for 20h, mixing the powder, the milling ball and the deionized water according to the volume ratio of 1: 7: 2, and adding the treated ZrO2Mixing the whiskers and the TiC nano particles, ball-milling for 20 hours, and drying;
(4) drying, and sieving with 100 mesh stainless steel sieve to obtain uniformly mixed composite powder;
(5) placing the sieved composite powder into a graphite die for hot-pressing sintering molding at 1700 ℃, 40MPa and 1.5h to obtain Al2O3As shown in FIG. 1, the dispersion strengthening and toughening effect of the nanoparticles in this embodiment is dominant, so that the ceramic grains are refined, thereby improving Al content2O3Mechanical properties of the base ceramic material.
Example 2
Al2O3Measuring ZrO based on the ceramic material210mL of whisker, 10mL of TiC nano-particle and MnO22mL，Y2O30.5mL，Al2O377.5mL to obtain Al2O3The pulling-out mechanism of the whisker from the base ceramic material is a key mechanism for improving the toughness of the base ceramic material, and as seen from fig. 2, the whisker and the nano-particle in the content of the whisker and the nano-particle in the embodiment well exert the synergistic strengthening and toughening effects, so that the embodiment obtains excellent mechanical properties.
The preparation method is the same as that of example 1.
Example 3
Al2O3Measuring ZrO based on the ceramic material215mL of whisker, 5mL of TiC nano-particle and MnO22mL，Y2O30.5mL，Al2O377.5mL。
The preparation method is the same as that of example 1.
Example 4
Al2O3Measuring ZrO based on the ceramic material220mL of whisker, 5mL of TiC nano-particle and MnO22mL，Y2O30.5mL，Al2O372.5mL。
The preparation method is the same as that of example 1.
Example 5
Al2O3Measuring ZrO based on the ceramic material220mL of whisker, 7.5mL of TiC nano-particle and MnO22mL，Y2O30.5mL，Al2O370mL。
The preparation method is the same as that of example 1.
Example 6
Al2O3Measuring ZrO based on the ceramic material215mL of whisker, 7.5mL of TiC nano-particle and MnO20.5mL，Al2O377mL。
The preparation method is the same as example 1, except that in the step (1) of the preparation method: mixing ethanol and polyethylene glycol 300 at a volume ratio of 25: 1, wherein the total volume is 52 mL; in the step (2): ZrO 2 is mixed with2Respectively carrying out ultrasonic oscillation treatment on the whiskers and the TiC nano particles in a dispersion medium for 25min, and then carrying out ultrasonic oscillation treatment for 10 min; in the step (3): performing ball milling for 30 hours for the first time, wherein the volume ratio of the mixed powder, the grinding balls and the deionized water is 1: 6: 3, and performing ball milling for 30 hours for the second time; in the step (5): the hot-pressing sintering molding temperature is 1600 ℃, the pressure is 50MPa, and the heat preservation time is 1 h.
Example 7
Al2O3Measuring ZrO based on the ceramic material215mL of whisker, 7.5mL of TiC nano-particle and MnO23mL，Y2O31mL，Al2O373.5mL。
The preparation method is the same asExample 1, with the difference that in step (1) of the preparation process: mixing ethanol and polyethylene glycol 300 at a volume ratio of 35: 1, wherein the total volume is 72 mL; in the step (2): ZrO 2 is mixed with2Respectively carrying out ultrasonic oscillation treatment on the whiskers and the TiC nano particles in a dispersion medium for 30min, and then carrying out ultrasonic oscillation treatment for 20 min; in the step (3): carrying out ball milling for 15h for the first time, wherein the volume ratio of the mixed powder, the grinding balls and the deionized water is 1: 9: 1.5, and carrying out ball milling for 15h for the second time; in the step (5): the hot-pressing sintering molding temperature is 1900 ℃, the pressure is 30MPa, and the heat preservation time is 2 h.
Comparative example 1
Al2O3Measuring MnO content of the base ceramic material22mL，Y2O30.5mL，Al2O397.5mL。
The preparation method is the same as that of example 1.
Comparative example 2
Al2O3Measuring ZrO based on the ceramic material2Whisker 5mL, MnO22mL，Y2O30.5mL，Al2O387.5mL。
The preparation method is the same as that of example 1.
Comparative example 3
Al2O3Taking TiC nano particles of 5mL and MnO as base ceramic material22mL，Y2O30.5mL，Al2O387.5mL。
The preparation method is the same as that of example 1.
The mechanical properties of the three control groups and examples 1 to 5 are shown in Table 1.
TABLE 1 mechanical Properties of the materials
Claims (9)
1. ZrO (ZrO)2Al synergistically toughened with TiC2O3The ceramic material is characterized by comprising the following components in percentage by volume: ZrO (ZrO)25-20% of whiskers, 5-10% of TiC nano particles and MnO20.5～3％，Y2O30 to 1% and the balance of Al2O3。
2. Al according to claim 12O3Based ceramic material, characterized in that the ZrO2The average diameter of the crystal whisker is 0.1-5 μm, and the average length is 10-100 μm; the average grain size of the TiC nano particles is 30-100 nm; the Al is2O3The average particle size is 100-800 nm; the MnO2The average particle size is 100-800 nm; said Y2O3The average particle diameter is 1 to 3 μm.
3. Al according to claim 1 or 22O3The preparation method of the base ceramic material is characterized by comprising the following steps:
(1) taking ethanol and polyethylene glycol mixed solution as a dispersion medium, and measuring ZrO in proportion2Whisker and TiC nano-particle, and respectively carrying out first ultrasonic oscillation treatment on the whisker and the TiC nano-particle in a dispersion medium, and then carrying out ZrO treatment on the whisker and the TiC nano-particle2Mixing the whisker dispersion liquid and the TiC nano-particle dispersion liquid, and then carrying out secondary ultrasonic oscillation treatment;
(2) mixing Al2O3、MnO2、Y2O3The mixed powder is ball milled for the first time in deionized water, and then the treated ZrO is added2Mixing the crystal whisker and the TiC nano-particle dispersion liquid, carrying out secondary ball milling, and drying;
(3) sieving the dried powder to obtain uniformly mixed composite powder;
(4) putting the sieved composite powder into a graphite die for hot-pressing sintering molding to obtain Al2O3A base ceramic material.
4. Al according to claim 32O3The preparation method of the base ceramic material is characterized in thatIn the step (1), the volume ratio of the ethanol to the polyethylene glycol dispersion medium is 25-35: 1.
5. Al according to claim 32O3The preparation method of the base ceramic material is characterized in that the first ultrasonic oscillation treatment time in the step (1) is 20-30 min, and the second ultrasonic oscillation treatment time is 10-20 min.
6. Al according to claim 32O3The preparation method of the base ceramic material is characterized in that when the ball milling is carried out for the first time in the step (2), the volume ratio of the mixed powder, the grinding balls and the deionized water is 1: 6-9: 1.5-3.
7. Al according to claim 32O3The preparation method of the base ceramic material is characterized in that the ball milling treatment time in the step (2) is 15-30 hours.
8. Al according to claim 32O3The preparation method of the base ceramic material is characterized in that the sieving in the step (3) is a 100-mesh sieve.
9. Al according to claim 32O3The preparation method of the base ceramic material is characterized in that the hot-pressing sintering temperature in the step (4) is 1600-1900 ℃, the pressure is 30-50 MPa, and the heat preservation time is 1-2 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042858A (en) * | 1988-11-03 | 1990-06-13 | 钴碳化钨硬质合金公司 | Aluminium oxide-zirconium oxide-carbide whisker strengthens cutting tool |
| CN106542839A (en) * | 2016-10-28 | 2017-03-29 | 宁波鑫汇力精密工具有限公司 | A kind of preparation method of whisker type toughening ceramic |
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- 2019-11-15 CN CN201911117041.8A patent/CN110981521A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042858A (en) * | 1988-11-03 | 1990-06-13 | 钴碳化钨硬质合金公司 | Aluminium oxide-zirconium oxide-carbide whisker strengthens cutting tool |
| CN106542839A (en) * | 2016-10-28 | 2017-03-29 | 宁波鑫汇力精密工具有限公司 | A kind of preparation method of whisker type toughening ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 尹龙卫等: "Al2O3/TiC陶瓷复合材料补强增韧机理研究", 《山东冶金》 * |
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Application publication date: 20200410 |