CN106904985B - Titanium-silicon-carbon enhanced alumina-based multiphase composite material and preparation method thereof - Google Patents
Titanium-silicon-carbon enhanced alumina-based multiphase composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium-silicon-carbon enhanced alumina-based multiphase composite material and a preparation method thereof. Weighing titanium powder, alumina powder and silicon carbide powder according to a certain volume ratio, taking alcohol as a dispersion medium and alumina balls as a ball milling medium, fully mixing, and drying to obtain mixed powder; and placing the mixed powder in a vacuum hot-pressing furnace to perform hot-pressing sintering at a certain pressure, a certain heating rate, a certain sintering temperature and a certain heat preservation time. Considering Al in alumina-based multiphase composite material under hot pressing condition2O3And Ti under high temperature to generate a strong interface reaction to generate a titanium-aluminum intermetallic compound, particularly TiAl and Ti3Al, which degrades the performance of the material. The invention generates new compounds TiC and Ti by doping SiC particles to react with Ti3SiC2And the semi-molten Si is filled in partial pores of the material, so that the alumina-based multiphase composite material with high relative density, hardness, toughness and strength is obtained.
Description
Technical Field
The invention belongs to the technical field of preparation of carbide doped ceramic matrix metal composite materials, and relates to a titanium-silicon-carbon enhanced alumina-based multiphase composite material and a preparation method thereof.
Background
In recent years, the research of cermet composite materials, in which Al is attracting attention2O3Ceramics are one of the most widely used ceramic materials. The alumina-based ceramic composite material has the characteristics of wear resistance, corrosion resistance, high temperature resistance, high hardness and the like, and has excellent oxidation resistance and chemical stability,low cost and rich resources. The composite material is widely applied to the fields of aerospace, medical treatment, automobile engines, electronic components, mechanical materials and the like. However, the low toughness of alumina ceramics limits the production application thereof.
At present, ternary carbide and nitride ceramics have excellent performance due to the special layered structure, not only have ceramic characteristics, but also have metal characteristics, improve the brittleness and the toughness of the ceramics, and Ti3SiC2Is one of the most attractive ceramic materials in ternary carbide, ternary Ti3SiC2The material has excellent mechanical property and good oxidation resistance at high temperature. But Ti3SiC2The multiphase composite material of the reinforced alumina has the problems of low hardness and relative density.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a titanium-carbon enhanced alumina-based multiphase composite material which has the advantages of high relative density, high hardness, toughness, high strength and the like.
Meanwhile, the invention also provides a preparation method of the titanium-silicon-carbon enhanced alumina-based multiphase composite material.
The technical scheme of the invention is as follows:
a preparation method of a titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following steps:
1) preparing mixed powder: mixing the following components in a volume ratio of 40: 40-50: 10-20 parts of titanium powder, alumina powder and silicon carbide powder, taking alcohol as a dispersion medium, wherein the volume ratio of the powder to the alcohol is 1:6, ball-milling for 4 hours by using alumina balls as ball-milling media, drying the ball-milled slurry at 70 ℃ for 24 hours, fully drying the ball-milled slurry into powder, and sieving the powder by using a 50-mesh sieve to obtain mixed powder;
2) vacuum hot-pressing sintering: and (3) placing the mixed powder into a vacuum hot-pressing furnace, and hot-pressing and sintering at 1400-1800 ℃ for 1-5 h under the pressure of 20-60 MPa to obtain the titanium-silicon-carbon enhanced alumina-based multiphase composite material.
In the step 1), the silicon carbide powder accounts for 10-20% of the total volume of the used powder;
in the step 1), the volume ratio of the titanium powder to the alumina powder to the silicon carbide powder is preferably 40:40: 20;
in the step 1), the particle size of the titanium powder is 0.5-2 μm, the particle size of the alumina powder is 0.5-3 μm, and the particle size of the silicon carbide powder is 0.5-2 μm.
In the step 2), the sintering is carried out, wherein the heating rate is 5-20 ℃/min.
In the step 2), hot pressing sintering is carried out for 2h at 1600 ℃ in a vacuum hot pressing furnace under the preferable pressure of 30 MPa.
The titanium-silicon-carbon enhanced alumina-based multiphase composite material prepared by the method.
The titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following components in percentage by mass: 45-47% of titanium, 5-12% of silicon, 3-5% of carbon, 17-36% of oxygen and the balance of aluminum;
the elements of the titanium, the carbon and the partial silicon are TiC and Ti5Si3、Ti3SiC2The compound particles are embedded in an alumina matrix, the rest silicon element is solid-dissolved in pores of the composite material in an atomic form, and the proportion of the two parts of silicon element is 70-75: 25 to 30.
The titanium-silicon-carbon enhanced aluminum oxide-based multiphase composite material is plate-shaped or columnar and has a layered structure, and the size of the composite material is 3-5 mu m.
The relative density of the titanium-silicon-carbon enhanced alumina-based multiphase composite material is 90-99%; microhardness of 10-25 GPa, bending strength of 200-600 MPa, and fracture toughness of 3-15 MPa.m1/2。
The multiphase composite material of the invention generates a new compound by adding silicon carbide powder and titanium, wherein TiC and Ti3SiC2The reinforcing and toughening effects are achieved, and the semi-molten Si is filled in partial pores of the material, so that the alumina-based multiphase composite material with high relative density, hardness, toughness and strength is obtained under the hot-pressing condition. SiC as second only to diamond and B4The third hardness material of C has excellent mechanical property and chemical stability, and SiC particles are added into the alumina-based multiphase composite material to be beneficial toReduction of TiAl and Ti metal compounds3And (3) Al is generated. The material before adding the silicon carbide is flaky particles, a certain amount of air holes exist, the crystal grains of the material are gradually increased along with the addition of the silicon carbide, the air holes are gradually reduced, and the disappearance of partial air holes is accompanied. Most importantly, SiC reacts with Ti to form TiC and Ti5Si3、Ti3SiC2Etc. wherein TiC, Ti3SiC2The strengthening and toughening effects are achieved, meanwhile, the TiC is generated, the strength of the material is greatly improved, and the semi-molten phase Si is filled in partial pores to promote the densification of the material, so that the alumina-based multiphase composite material with excellent comprehensive performance is obtained under the hot pressing condition.
Compared with the prior art, the preparation method has the advantages that:
(1) compared with the undoped titanium/alumina composite material, the ceramic matrix composite material prepared by the invention has the advantages that the semi-molten phase Si is filled in the pores, the relative density is further improved, and a relatively excellent sintering aid is provided for hot-pressing sintering of the alumina matrix ceramic composite material;
(2) the added silicon carbide can lead titanium to react with the silicon carbide to generate new substances, inhibit the generation of titanium-aluminum intermetallic compounds and form new compounds, wherein the new phases TiC and Ti3SiC2The reinforcing and toughening effects are achieved, so that the strength and the fracture toughness are greatly improved;
(3) the method has the advantages of simple operation flow, relatively low raw material cost and excellent product performance, and has important significance for practical application and production.
Drawings
FIG. 1 is an XRD pattern of a silicon carbide doped alumina-based heterogeneous composite material of example 1;
FIG. 2 is a SEM image of a cross-section of the silicon carbide doped alumina-based multiphase composite of example 1;
FIG. 3 is an XRD pattern of the alumina-based heterogeneous composite material of comparative example 1;
fig. 4 is a sectional SEM image of the alumina-based heterogeneous composite material in comparative example 1.
Detailed Description
The present invention has been described in conjunction with specific embodiments thereof, and various alterations and modifications made on the basis of ordinary skill in the art and conventional practices without departing from the technical spirit of the present invention are included in the scope of the present invention.
Example 1
A preparation method of a titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following steps:
1) titanium powder, alumina powder and silicon carbide powder are mixed according to the volume ratio of 40:40:20, mixing, namely performing ball milling for 4 hours in a polytetrafluoroethylene tank by using alcohol as a dispersion medium, wherein the volume ratio of the powder to the alcohol is 1:6, and alumina balls as a ball milling medium; placing the ground slurry in a drying box, and drying for 24 hours at 70 ℃; after fully drying the mixture into powder, sieving the powder by a 50-mesh sieve to obtain mixed powder;
2) and (3) putting 30g of the mixed powder into a vacuum hot-pressing furnace, placing the furnace in a graphite mold with the diameter of 45mm, sintering for 2h under the conditions of 1500 ℃ and 30MPa, and heating up at a speed of 10 ℃/min to obtain the titanium-silicon-carbon enhanced alumina-based multiphase composite material.
Through determination, the titanium-silicon-carbon enhanced alumina-based multiphase composite material in the embodiment 1 is in a long column shape or a plate shape with the thickness of 3-5 μm, has a layered structure and consists of the following components in percentage by mass: 46.1% of titanium, 11.4% of silicon, 4.9% of carbon, 17.7% of oxygen and the balance of aluminum; the elements of the titanium, the carbon and the partial silicon are TiC and Ti5Si3、Ti3SiC2The compound particles are embedded in an alumina matrix, and the rest silicon element is solid-dissolved in pores of the composite material in an atomic mode, wherein the ratio of the two parts of silicon is 3: 1. The relative density is 97.76%, the bending strength is 437.26MPa, the microhardness is 19.61 GPa, and the fracture toughness is 9.95 MPa.m1/2. X-ray diffraction analysis shows that after silicon carbide is added, new compounds are formed between Ti and SiC, and the products comprise TiC and Ti5Si3、Ti3SiC2The product of this time Ti3SiC2The content is increased, and the performance of the material is further improved. Meanwhile, by analysis of a scanning electron microscope (images are shown in FIG. 2), it can be seen thatThe contact layer is more tightly combined, and the strength of the composite material is further improved.
Example 2
A preparation method of a titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following steps:
1) titanium powder (1 mu m), alumina powder (1 mu m) and silicon carbide powder (800 nm) are mixed according to the volume ratio of 40: 45: 15 mixing, taking alcohol as a dispersion medium, taking alumina balls as a ball milling medium, and performing ball milling for 4 hours in a polytetrafluoroethylene tank, wherein the dispersion volume ratio is 1: 6; placing the ground slurry in a drying box, and drying for 24 hours at 70 ℃; after fully drying the mixture into powder, sieving the powder by a 50-mesh sieve to obtain mixed powder;
2) and (3) putting 30g of the mixed powder into a vacuum hot-pressing furnace, placing the furnace in a graphite mold with the diameter of 45mm, sintering for 2h under the conditions of 1500 ℃ and 30MPa, and heating up at a speed of 10 ℃/min to obtain the titanium-silicon-carbon enhanced alumina-based multiphase composite material.
Through determination, the titanium-silicon-carbon enhanced alumina-based multiphase composite material in the embodiment 2 is in a long column shape or a plate shape with the thickness of 3-5 μm, has a layered structure and consists of the following components in percentage by mass: 45.8% of titanium, 8.5% of silicon, 3.6% of carbon, 19.8% of oxygen and the balance of aluminum; the elements of the titanium, the carbon and the partial silicon are TiC and Ti5Si3、Ti3SiC2The compound particles are embedded in the alumina matrix, and the rest silicon element is solid-dissolved in the pores of the composite material in the form of atoms, and the ratio of the two parts of silicon is 37: 14. The relative density is 98.47 percent, the bending strength is 431.23MPa, the microhardness is 19.52GPa, and the fracture toughness is 7.83 MPa.m1 /2The performance of the material is remarkably improved. The X-ray diffraction analysis shows that after the silicon carbide is added, Ti and SiC form a new compound, Ti is consumed, and products comprise TiC and Ti5Si3、Ti3SiC2Wherein TiC, Ti3SiC2The composite material has the advantages that the reinforcing and toughening effects are achieved, the strength and the toughness of the material are improved, the semi-molten Si is filled in partial pores, the important significance is achieved on the improvement of the density of the material, the combination of a contact layer is found to be tight through the analysis of a scanning electron microscope, and the strength of the composite material is further improved.
Example 3
A preparation method of a titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following steps:
1) titanium powder (1 mu m), alumina powder (1 mu m) and silicon carbide powder (800 nm) are mixed according to the volume ratio of 40: 50: 10, mixing, taking alcohol as a dispersion medium, taking alumina balls as a ball milling medium in a dispersion volume ratio of 1:6, and performing ball milling for 4 hours in a polytetrafluoroethylene tank; placing the ground slurry in a drying box, and drying for 24 hours at 70 ℃; after fully drying the mixture into powder, sieving the powder by a 50-mesh sieve to obtain mixed powder;
2) and (3) putting 30g of the mixed powder into a vacuum hot-pressing furnace, placing the furnace in a graphite mold with the diameter of 45mm, sintering for 2h under the conditions of 1500 ℃ and 30MPa, and heating up at a speed of 10 ℃/min to obtain the titanium-silicon-carbon enhanced alumina-based multiphase composite material.
Through determination, the titanium-silicon-carbon enhanced alumina-based multiphase composite material in the embodiment 2 is in a long column shape or a plate shape with the thickness of 3-5 μm, has a layered structure and consists of the following components in percentage by mass: 45.6% of titanium, 5.6% of silicon, 2.4% of carbon, 21.8% of oxygen and the balance of aluminum; the elements of the titanium, the carbon and the partial silicon are TiC and Ti5Si3、Ti3SiC2The compound particles are embedded in an alumina matrix, and the rest silicon element is solid-dissolved in pores of the composite material in an atomic mode, wherein the ratio of the two parts of silicon is 7: 3. The relative density is 96.48 percent, the bending strength is 392.39MPa, the microhardness is 17.61GPa, and the fracture toughness is 6.87 MPa.m1/2The performance of the material is remarkably improved. The X-ray diffraction analysis shows that after the silicon carbide is added, Ti and SiC form a new compound, Ti is consumed, and products comprise TiC and Ti5Si3、Ti3SiC2Wherein TiC, Ti3SiC2The composite material has the advantages that the reinforcing and toughening effects are achieved, the strength and the toughness of the material are improved, the semi-molten Si is filled in partial pores, the important significance is achieved on the improvement of the density of the material, the scanning electron microscope analysis shows that the contact layer is more tightly combined, and the strength of the composite material can be improved.
Comparative example 1
Titanium powder (1 μm) and alumina powder (1 μm) were mixed in a ratio of 40: preparing by a volume ratio of 60, taking alcohol as a dispersion medium, taking the dispersion volume ratio as 1:6, taking alumina balls as a ball milling medium, and carrying out ball milling for 4 hours in a polytetrafluoroethylene tank; drying the ground paste in a drying oven at 70 ℃ for 24 h; sieving the dried powder with a 50-mesh sieve to obtain mixed powder; placing 30g of the mixed powder in a graphite die with the diameter of 45mm, sintering for 2h under the conditions of 1500 ℃ and 30MPa, and heating at the rate of 10 ℃/min; and preparing a sample.
The relative density of the sample was found to be 94.52%, the bending strength was found to be 324.46MPa, the microhardness was found to be 15.48GPa, and the fracture toughness was found to be 4.63 MPa.m1/2. X-ray diffraction analysis showed that (image shown in FIG. 3) there was a large amount of TiAl and Ti in the sample3And Al intermetallic compounds are generated, and the substances have strong room temperature brittleness, so that the overall strength and toughness of the composite material are greatly reduced. Meanwhile, the grain boundary of titanium and aluminum is relatively obvious through the analysis of a scanning electron microscope (the image is shown in fig. 4), and the bonding force between the two is weak.
Claims (6)
1. The preparation method of the titanium-silicon-carbon enhanced alumina-based multiphase composite material is characterized by comprising the following steps of:
1) preparing mixed powder: mixing the following components in a volume ratio of 40: 40-45: 15-20 parts of titanium powder, alumina powder and silicon carbide powder, taking alcohol as a dispersion medium, wherein the volume ratio of the powder to the alcohol is 1:6, ball-milling for 4 hours by using alumina balls as ball-milling media, drying the ball-milled slurry at 70 ℃ for 24 hours, fully drying the ball-milled slurry into powder, and sieving the powder by using a 50-mesh sieve to obtain mixed powder;
2) vacuum hot-pressing sintering: placing the mixed powder in a vacuum hot-pressing furnace, and hot-pressing and sintering at 1400-1800 ℃ for 1-5 h under the pressure of 20-60 MPa to obtain the titanium-silicon-carbon enhanced alumina-based multiphase composite material;
the particle size of the titanium powder is 0.5-2 mu m, the particle size of the alumina powder is 0.5-3 mu m, and the particle size of the silicon carbide powder is 0.5-2 mu m;
titanium, carbon and part of silicon element as TiC, Ti5Si3、Ti3SiC2The compound particles are embedded in oxygenIn the aluminum matrix, the rest silicon element is in atomic form and is dissolved in the pores of the composite material, and the proportion of the two parts of silicon element is 70-75: 25 to 30.
2. The method of claim 1, wherein: in the step 1), the volume ratio of the titanium powder, the alumina powder and the silicon carbide powder is 40:40: 20.
3. The method of claim 1, wherein: in the step 2), the sintering is carried out, wherein the heating rate is 5-20 ℃/min.
4. The method of claim 1, wherein: in the step 2), hot pressing and sintering are carried out for 2h at 1600 ℃ in a vacuum hot pressing furnace under the pressure of 30 MPa.
5. A titanium-silicon-carbon reinforced alumina-based multiphase composite prepared by the method of any one of claims 1 to 4;
the titanium-silicon-carbon enhanced alumina-based multiphase composite material comprises the following components in percentage by mass: 45-47% of titanium, 5-12% of silicon, 3-5% of carbon, 17-36% of oxygen and the balance of aluminum;
the elements of the titanium, the carbon and the partial silicon are TiC and Ti5Si3、Ti3SiC2The compound particles are embedded in an alumina matrix, the rest silicon element is solid-dissolved in pores of the composite material in an atomic form, and the proportion of the two parts of silicon element is 70-75: 25-30;
the titanium-silicon-carbon enhanced aluminum oxide based multiphase composite material has the relative density of 97.76-99%, the microhardness of 19.52-25 GPa, the bending strength of 431.23-600 MPa and the fracture toughness of 7.83-15 MPa.m1/2。
6. The titanium-silicon-carbon enhanced alumina-based multiphase composite according to claim 5, wherein: is plate-shaped or column-shaped, has a layered structure, and has a size of 3-5 μm.
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