CN113213960A - High-toughness and high-hardness wear-resistant ceramic and preparation method thereof - Google Patents
High-toughness and high-hardness wear-resistant ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of ceramic preparation, and particularly relates to high-toughness high-hardness wear-resistant ceramic and a preparation method thereof. Mixing TiC powder, Mo powder, Sm powder, Ti powder and Si powder according to a certain proportion, and then carrying out ball milling treatment; after ball milling, adding carbon fiber and SiC whisker, continuing ball milling, and vacuumizing the ball-milled slurry and then heating and drying the ball-milled slurry; and then adding polyvinyl alcohol for granulation, preforming the granulated powder through a tablet machine, then pressing under 30-40 MPa to prepare a blank, removing glue for 2-4 h at 600-800 ℃ in a muffle furnace, then sintering for 1-5 h at 1500-1700 ℃, and cooling to room temperature along with the furnace to obtain the ceramic. The invention has the advantages of rich raw material resources, simple preparation process and lower production cost, and the obtained high-toughness high-hardness wear-resistant ceramic has excellent wear resistance and higher hardness and toughness.
Description
Technical Field
The invention belongs to the technical field of ceramic preparation. More particularly, it relates to a high-toughness, high-hardness wear-resistant ceramic and a preparation method thereof.
Background
The ceramic material has the advantages of high temperature resistance, corrosion resistance, wear resistance, light weight and the like, and has wide application prospects in the fields of energy, metallurgy, aerospace, petrochemical industry and the like. However, ceramic materials are inherently brittle and sensitive to defects, which results in poor reliability and repeatability of use, limiting their applications.
Ti3SiC2Is a typical MAX phase ceramic material, first synthesized by jeitschko et al in 1967. Ti3SiC2Has a hexagonal layered structure (space group: P6) in which Ti and C are bonded by a covalent bond and an ionic bond having a high bonding degree6C octahedron, Ti6Layer C andthe Si atomic layers are connected by metal bonds with weak bonding degree and are alternately stacked in the c direction. The special chemical bond composition ensures that the ceramic material has the characteristics of metal and ceramic, and has excellent heat conductivity, mechanical processing property, thermal stability, corrosion resistance and oxidation resistance. The above characteristics make Ti3SiC2Has wide application prospect under the severe working conditions of high temperature, high radiation, strong acid and strong alkali, etc. Thus, Ti3SiC2Has received a great deal of attention from the materials personnel.
However, in practical application, since Ti3SiC2Has a high wear rate due to breakage and extraction of crystal grains, and has a hardness and bending strength that do not meet practical requirements. Generally, the addition of a lubricating phase or a hard phase to the material matrix improves the frictional wear properties and mechanical properties of the material. Preparation of Ti by Islak B T3SiC2The microstructure, the mechanics and the tribology performance of the/SiC composite material are researched. The results show that SiC is uniformly distributed in Ti3SiC2In the matrix, the hardness and fracture toughness of the composite material are better than those of single-phase Ti due to the reinforcing effect of SiC3SiC2All are improved by about 30 percent. Meanwhile, the SiC and the matrix have higher bonding strength, and Ti is inhibited3SiC2The wear resistance of the composite material is higher than that of single-phase Ti by pulling out crystal grains3SiC2The improvement is about 88 percent. Wenhexing and the like prepare Ti with different Mo doping amounts by utilizing a hot-pressing sintering process3SiC2The composite material is based, and the phase composition, the mechanical property and the tribological property of the material are researched. The results show that Mo doping affects Ti in the raw material system3SiC2The Mo-doped sample is mainly formed by TiC, (Ti)0.8Mo0.2)Si2And Mo4.8Si3C0.6The components are equal; with the increase of the doping amount, the density, the Vickers hardness and the bending strength of the material all show the trend of increasing firstly and then reducing, and a sample doped with 16.67 at% of Mo has the optimal comprehensive mechanical property; the samples with Mo doping amounts of 8.33 at% and 16.77 at% were due to the outgrowth of the hard phase, as compared with the sample without Mo dopingThe samples doped at 25 at% and 33.33 at% had lower coefficients of friction but exhibited higher rates of wear due to the less dense samples.
However, the above studies have been on Ti3SiC2The improvement of the ceramic performance is not ideal, and how to better improve Ti3SiC2The hardness of the ceramic is improved, the bending strength is improved, the wear rate is reduced, and the problem which needs to be solved at present is still solved urgently.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the existing Ti3SiC2The defects and defects of low toughness, hardness and abrasion loss of the ceramic are overcome, and the high-toughness high-hardness abrasion-resistant ceramic and the preparation method thereof are provided. It has high hardness, high bending strength and low wear rate.
The invention aims to provide a preparation method of high-toughness high-hardness wear-resistant ceramic. TiC powder, Mo powder, Sm powder, Ti powder and Si powder are proportioned according to a certain proportion and then ball-milled; after ball milling, adding carbon fiber and SiC whisker, continuing ball milling, and vacuumizing the ball-milled slurry and then heating and drying the ball-milled slurry; and then adding polyvinyl alcohol for granulation, preforming the granulated powder through a tablet machine, then pressing under 30-40 MPa to prepare a blank, removing glue for 2-4 h at 600-800 ℃ in a muffle furnace, then sintering for 1-5 h at 1500-1700 ℃, and cooling to room temperature along with the furnace to obtain the ceramic.
The invention also aims to provide the high-toughness high-hardness wear-resistant ceramic.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: x: y: 1-x-y: 1.2, weighing, wherein x is 0.05-0.15; y is 0.05-0.15, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls, taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling inert gas, and then opening the ball milling machine for ball milling treatment;
(2) adding 2-4 wt% of carbon fiber and 2-4 wt% of SiC whisker into the ball milling tank, and continuing ball milling treatment;
(3) vacuumizing the ball-milled slurry, and then heating and drying the slurry;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under the pressure of 30 MPa-40 MPa to prepare a blank, discharging the glue of the obtained blank in a muffle furnace at the temperature of 600-800 ℃ for 2-4 h, then sintering the blank at the temperature of 1500-1700 ℃ for 1-5 h, and cooling the blank to room temperature along with the furnace to obtain the ceramic.
Preferably, in the step (1), Φ of the silicon nitride grinding ball is 4-6 mm, and the ball-to-material ratio is controlled to be (5-9): 1, the addition amount of the absolute ethyl alcohol is 15-25% of the mass of the raw material powder; the ball milling rotating speed is 300-400 r/min, and the ball milling processing time is 6-14 h; the inert gas is helium or argon.
Preferably, in the step (2), the length-diameter ratio of the carbon fiber is 20-40: 1; the length-diameter ratio of the SiC whiskers is 10-30: 1; the ball milling rotating speed is 200-400 r/min, and the ball milling processing time is 6-14 h.
Preferably, in the step (3), after vacuumizing, the air pressure is reduced to less than 0.1MPa, and then drying treatment is carried out at 60-80 ℃.
Preferably, in the step (4), the heating rate in the glue discharging process is 4-6 ℃/min, and the heating rate in the sintering process at 1500-1700 ℃ for 1-5 h is 7-9 ℃/min.
The high-toughness and high-hardness wear-resistant ceramic is prepared by the preparation method of the high-toughness and high-hardness wear-resistant ceramic.
Preferably, the high-toughness and high-hardness wear-resistant ceramic has the hardness Hv of 15.3-16.4 GPa, the bending strength of 450-460 MPa and the wear rate of 3.1 multiplied by 10-5～3.5×10-5。
The invention has the following beneficial effects:
1) a method for preparing high-toughness high-hardness wear-resistant ceramic.TiC powder, Mo powder, Sm powder, Ti powder and Si powder are proportioned according to a certain proportion and then ball-milled; after ball milling, adding carbon fibers and SiC whiskers, continuing ball milling, granulating, pressing into a blank, discharging the glue of the obtained blank in a muffle furnace, and sintering to obtain the ceramic, wherein the ceramic prepared by the method has the hardness Hv of 15.3-16.4 GPa, the bending strength of 450-460 MPa, and the wear rate of 3.1 multiplied by 10-5～3.5×10-5。
2) Doping Mo and Sm into Ti3SiC2In crystal lattice, and the synergistic effect between two elements promotes Ti3SiC2The hardness and the bending strength of the ceramic material are obviously improved, and the ceramic material has lower wear rate.
3) The strength and toughness of the ceramic material can be obviously improved by adding the carbon fibers and the SiC whiskers, so that the comprehensive performance of the ceramic material is improved, and the carbon fibers and the SiC whiskers are unexpectedly found to have a synergistic effect in the aspect of enhancing the strength and toughness.
4) The polyvinyl alcohol is added for compression molding, and the glue is arranged for treatment, so that the ceramic material has good sintering characteristics, the porosity of the ceramic material is obviously reduced, the compactness is improved, and the hardness and the bending strength are further improved.
In conclusion, the high-toughness high-hardness wear-resistant ceramic prepared by the invention is an ideal material for practical production due to higher hardness, bending strength and lower wear rate.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.1: 0.1: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Example 2
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.05: 0.15: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 6mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling argon, and then opening the ball mill for ball milling treatment; controlling the ball-material ratio at 9: 1, the addition amount of the absolute ethyl alcohol is 25 percent of the mass of the raw material powder; the ball milling rotation speed is 400r/min, and the ball milling processing time is 6 h;
(2) adding 4 wt% of carbon fiber (the length of which is 80 μm and the diameter of which is 2 μm) and 2 wt% of SiC whisker (the length of which is 30 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 400r/min, and the ball milling processing time is 6 h;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 80 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 40MPa to prepare a blank, heating the obtained blank from room temperature to 800 ℃ at the heating rate of 6 ℃/min in a muffle furnace, discharging glue for 2h, heating to 1700 ℃ at the heating rate of 7 ℃/min, sintering for 1h, and furnace-cooling to room temperature to obtain the ceramic.
Example 3
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.15: 0.05: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 4mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, charging helium, and then opening the ball mill for ball milling treatment; controlling the ball-material ratio at 5: 1, the addition amount of the absolute ethyl alcohol is 15 percent of the mass of the raw material powder; the ball milling rotation speed is 300r/min, and the ball milling processing time is 14 h;
(2) 2 wt% of carbon fiber (the length of which is 40 μm and the diameter of which is 2 μm) and 4 wt% of SiC whisker (the length of which is 90 μm and the diameter of which is 3 μm) are added into the ball milling tank, and the ball milling treatment is continued; the ball milling rotation speed is 200r/min, and the ball milling processing time is 14 h;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 60 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 30MPa to prepare a blank, heating the obtained blank from room temperature to 600 ℃ at the heating rate of 4 ℃/min in a muffle furnace, discharging glue for 4h, heating to 1500 ℃ at the heating rate of 9 ℃/min, sintering for 5h, and cooling to room temperature along with the furnace to obtain the ceramic.
Comparative example 1
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.2: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 2
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.2: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 3
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 1: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 4
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.1: 0.1: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 6 wt% of carbon fiber (the length of the carbon fiber is 60 mu m, the diameter of the carbon fiber is 2 mu m) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 5
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.1: 0.1: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 6 wt% of SiC whiskers (the length of the SiC whiskers is 60 mu m, and the diameter of the SiC whiskers is 3 mu m) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 6
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.1: 0.1: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) drying the slurry subjected to ball milling at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 5 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 8 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Comparative example 7
A preparation method of high-toughness high-hardness wear-resistant ceramic comprises the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: 0.1: 0.1: 0.8: 1.2, weighing, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls (phi is 5mm), taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling helium gas, and then opening the ball milling machine for ball milling treatment; wherein, the ball-to-feed ratio is controlled to be 7: 1, the addition of absolute ethyl alcohol is 20 percent of the mass of the raw material powder; the ball milling rotation speed is 350r/min, and the ball milling processing time is 10 h;
(2) adding 3 wt% of carbon fiber (the length of which is 60 μm and the diameter of which is 2 μm) and 3 wt% of SiC whisker (the length of which is 60 μm and the diameter of which is 3 μm) into the ball milling tank, and continuing ball milling treatment; the ball milling rotation speed is 300r/min, and the ball milling processing time is 10 hours;
(3) vacuumizing the ball-milled slurry, reducing the air pressure to be less than 0.1MPa, and then drying at 70 ℃;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under 35MPa to prepare a blank, heating the obtained blank from room temperature to 700 ℃ at the heating rate of 8 ℃/min in a muffle furnace, discharging glue for 3h, heating to 1600 ℃ at the heating rate of 5 ℃/min, sintering for 3h, and furnace-cooling to room temperature to obtain the ceramic.
Examples 1 to 3 and comparative examples 1 to 7 were subjected to mechanical property and tribological property tests.
Measuring the Vickers hardness of the material by using a microscopic Vickers hardness tester, wherein the load is 10N, the loading time is 5S, and the hardness value is the average value of five times of measurement; the bending strength of the sample is tested by a PT-1036PC type universal material testing machine, the size of the sample is 3mm multiplied by 4mm multiplied by 20mm, the span is 16mm, the loading speed of a pressure head is 0.5mm/min, the bending strength is the average value of three measurement results, and the tribology performance of the sample is tested by a ball disc type friction machine (HT-1000, Kaiki Huakou technology development Co., Ltd., Lanzhou). Specific test results are shown in table 1:
TABLE 1 mechanical and tribological Properties of examples 1-5 and comparative examples 1-3
In conclusion, the high-toughness high-hardness wear-resistant ceramic prepared by the invention is simple in preparation method, and the synergistic effects between Mo and Sm and between carbon fibers and SiC whiskers can be found out through the comparative examples of example 1 and comparative examples 1-7, so that Ti can be remarkably improved3SiC2The hardness and the bending strength are reduced, the wear rate is reduced, the hardness Hv and the bending strength can respectively reach 16.4GPa and 460MPa, and the wear rate is 3.1 multiplied by 10-5。
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of high-toughness high-hardness wear-resistant ceramic is characterized by comprising the following steps:
(1) TiC powder, Mo powder, Sm powder, Ti powder and Si powder with the purity of more than 99.5 percent are mixed according to the mol ratio of 2: x: y: 1-x-y: 1.2, weighing, wherein x is 0.05-0.15; y is 0.05-0.15, then putting the weighed raw materials into a ball milling tank, adding silicon nitride grinding balls, taking absolute ethyl alcohol as a ball milling medium, vacuumizing, filling inert gas, and then opening the ball milling machine for ball milling treatment;
(2) adding 2-4 wt% of carbon fiber and 2-4 wt% of SiC whisker into the ball milling tank, and continuing ball milling treatment;
(3) vacuumizing the ball-milled slurry, and then heating and drying the slurry;
(4) and then adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5% for granulation, preforming the granulated powder by a tablet machine, pressing the preformed powder under the pressure of 30 MPa-40 MPa to prepare a blank, discharging the glue of the obtained blank in a muffle furnace at the temperature of 600-800 ℃ for 2-4 h, then sintering the blank at the temperature of 1500-1700 ℃ for 1-5 h, and cooling the blank to room temperature along with the furnace to obtain the ceramic.
2. The method for preparing a high toughness, high hardness, wear resistant ceramic according to claim 1, wherein: in the step (1), phi of the silicon nitride grinding ball is 4-6 mm, and the ball-to-material ratio is controlled to be (5-9): 1, the addition amount of the absolute ethyl alcohol is 15-25% of the mass of the raw material powder; the ball milling rotating speed is 300-400 r/min, and the ball milling processing time is 6-14 h; the inert gas is helium or argon.
3. The method for preparing a high toughness, high hardness, wear resistant ceramic according to claim 1, wherein: in the step (2), the length-diameter ratio of the carbon fiber is 20-40: 1; the length-diameter ratio of the SiC whiskers is 10-30: 1; the ball milling rotating speed is 200-400 r/min, and the ball milling processing time is 6-14 h.
4. The method for preparing a high toughness, high hardness, wear resistant ceramic according to claim 1, wherein: in the step (3), after vacuumizing, the air pressure is reduced to be less than 0.1MPa, and then drying treatment is carried out at the temperature of 60-80 ℃.
5. The method for preparing a high toughness, high hardness, wear resistant ceramic according to claim 1, wherein: in the step (4), the heating rate in the glue discharging process is 4-6 ℃/min, and the heating rate in the sintering process at 1500-1700 ℃ for 1-5 h is 7-9 ℃/min.
6. A high toughness, high hardness wear resistant ceramic prepared by the method of preparing a high toughness, high hardness wear resistant ceramic according to any one of claims 1 to 5.
7. A high toughness, high hardness, wear resistant ceramic according to claim 6 wherein: the high-toughness high-hardness wear-resistant ceramic has the hardness Hv of 15.3-16.4 GPa, the bending strength of 450-460 MPa and the wear rate of 3.1 multiplied by 10-5～3.5×10-5。
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