阅读说明：本技术 一种高强度Ti-ZrO2-B4C体系复合材料的制备方法 (High-strength Ti-ZrO2-B4Preparation method of C-system composite material ) 是由 贾磊 宋伟 吕振林 于 2020-11-03 设计创作，主要内容包括：本发明提供一种高强度Ti-ZrO-2-B-4C体系复合材料的制备方法：先将纯Ti粉末与B-4C粉末和ZrO-2粉末用三维震动混粉机进行混粉,再在钢模中压制成型,最后用真空热压烧结炉进行烧结；将压制成型得到的坯体放入烧结炉,采用1200℃的烧结温度,烧结时间3h,随炉冷却至室温取出烧结得到的Ti-ZrO-2-B-4C体系复合材料。本发明在传统的纯Ti-B-4C体系复合材料中加入ZrO-2,制备得到的Ti-ZrO-2-B-4C体系复合材料的硬度和强度都有了一定的提升,性能变的更加优异,可以更好的应用到工程领域、汽车工业和航空航天等领域,适用于更高性能要求的行业。(The invention provides high-strength Ti-ZrO 2 ‑B 4 The preparation method of the C system composite material comprises the following steps: firstly pure Ti powder and B 4 C powder and ZrO 2 Mixing the powder by using a three-dimensional vibration powder mixer, then performing compression molding in a steel die, and finally sintering by using a vacuum hot-pressing sintering furnace; putting the blank obtained by press forming into a sintering furnace, adopting the sintering temperature of 1200 ℃ and the sintering time of 3h, cooling to room temperature along with the furnace, taking out and sintering to obtain Ti-ZrO 2 ‑B 4 And C system composite material. The invention is based on the conventional pure Ti-B 4 ZrO is added into C system composite material 2 Preparation of the resulting Ti-ZrO 2 ‑B 4 C systemThe hardness and the strength of the composite material are improved to a certain extent, the performance is more excellent, the composite material can be better applied to the fields of engineering, automobile industry, aerospace and the like, and the composite material is suitable for industries with higher performance requirements.)

1. High-strength Ti-ZrO₂-B₄The preparation method of the C-system composite material is characterized by comprising the following steps:

step 1, mixing the powder

In pure Ti powder and B₄Adding 0.04-0.12 mass percent of vacuum pump oil into the mixed powder of the C powder, mixing the powder for 1 hour, and then adding ZrO₂Continuously mixing the powder and the zirconia balls for 3 hours in a three-dimensional vibration powder mixer, wherein the frequency of the three-dimensional vibration powder mixer is 30-60Hz to obtain mixed powder A, the ball-material ratio is 1-3:1, and the large-ball ratio and the small-ball ratio are 3-4: 1;

step 2, ball milling the mixed powder

Putting the mixed powder A and the zirconia balls obtained in the step 1 into a ball milling tank, and carrying out ball milling by using a planetary ball mill to obtain mixed powder B, wherein the ball-material ratio is 4-5:1, and the mass ratio of big balls to small balls is 3-4: 1;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, wherein the pressing pressure is 5-15 MPa;

step 4, sintering the green body

And (3) putting the blank C obtained in the step (3) into a graphite die, sintering by adopting a vacuum hot-pressing sintering furnace to obtain the composite material D, wherein the heating speed is 8-10 ℃/min, the sintering pressure is 20-60MPa, the sintering temperature is 1000-1300 ℃, and the sintering time is 2-4 h.

2. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: the pure Ti powder in the step 1 has a particle size of 20-30 mu m, B₄C powder with grain diameter of 0.5-1.0 μm, ZrO₂The particle size of the powder is 1-3 μm.

3. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: step 1 said B₄The mass of the C powder accounts for 1.1-2.8% of the total mass of the powder, and ZrO₂The mass of the powder accounts for 0.1-1.1% of the total mass of the powder, and the balance is pure Ti powder.

4. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: and (3) mixing the powder in the step (1) and zirconia balls used in the ball milling in the step (2), wherein the diameter of a large ball is 9-11mm, and the diameter of a small ball is 5-6 mm.

5. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: step 2, adding absolute ethyl alcohol with the mass fraction of 1-3% into a ball milling tank during ball milling, and filling protective gas argon; the rotation speed of the ball mill is 150-.

6. A high strength Ti-ZrO according to claim 1₂-B₄C system compositeThe preparation method of the material is characterized by comprising the following steps: in the step 3, the mould used for pressing is a steel mould with the diameter of 40mm, and the pressure maintaining time is 1-6 min.

7. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: and 4, placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, checking to ensure that the graphite mold is vacuumized, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering procedure, immediately closing the diffusion pump when sintering is finished, cooling the graphite mold to room temperature along with the furnace, and taking out the sintered composite material D.

8. A high strength Ti-ZrO according to claim 1₂-B₄The preparation method of the C system composite material is characterized by comprising the following steps: the diameter of the composite material D is 38-40mm, and the height of the composite material D is 7-8 mm.

Technical Field

The invention belongs to the technical field of titanium-based composite materials, and particularly relates to high-strength Ti-ZrO₂-B₄A preparation method of a C system composite material.

Background

Titanium is an important structural metal developed in the 50 s of the 20 th century, and is particularly widely distributed in nature, and the content of the earth crust reaches about 0.6%. Titanium and titanium alloy are researched and developed in a great deal of countries such as the united states, japan, russia and china, so that the titanium and titanium alloy are applied in many ways, but the titanium alloy has the defects of high production cost, low hardness, low rigidity and the like, and the application range of the titanium alloy is limited to a certain extent. Therefore, in order to overcome these limitations, the compounding of materials has become a necessary trend.

Titanium-based composites refer to composites with superior properties made by adding one or more reinforcing phases to a pure titanium or titanium alloy matrix; the titanium alloy matrix powder is generally prepared by adopting a gas atomization method, the price is relatively expensive, and the pure titanium matrix powder is relatively cheap. With pure Ti-B₄The C system is popular in preparing composite materials, pure titanium matrix powder is used in the system, the performance is good, but the use requirement is more rigorous, and the strength cannot be met, so that the composite materials are continuously reinforced; while better strength is expected to be obtained by using the titanium alloy powder, the cost for preparing the titanium alloy powder is obviously higher, so that the composite material needs to be reinforced by other methods in consideration of economy.

Among the many strengthening methods, the materials workers often adopt a solid solution strengthening approach to improve the strength of the materials. Researches prove that Fe, Zr, O, Si and the like can be dissolved in a pure titanium matrix in a solid mode, so that the crystal lattice of the pure titanium matrix is distorted, and the purpose of solid solution strengthening is achieved. Zirconium oxide (ZrO)₂) The ceramic material has high use temperature, stable high-temperature chemical property, corrosion resistance, oxidation resistance, thermal shock resistance, non-volatility and no pollution; therefore, the pure Ti-B can be prepared by a reasonable preparation method₄Adding a third component ZrO in the C system₂So as to produce solid solution strengthening to obtain high-strength Ti-ZrO₂-B₄And C system composite material. The composite material has better properties such as strength, hardness and the like, and can be better applied to the engineering field, the automobile industry and the aviationThe method is suitable for industries with higher performance requirements in the fields of heaven and the like.

Disclosure of Invention

The invention aims to provide high-strength Ti-ZrO₂-B₄The preparation method of the C-system composite material solves the problem of the existing Ti-B₄The C system composite material has lower strength in practical application and cannot meet the problem of higher use requirement.

The technical scheme adopted by the invention is that high-strength Ti-ZrO₂-B₄The preparation method of the C system composite material comprises the following steps:

step 1, mixing the powder

In pure Ti powder and B₄Adding 0.04-0.12 mass percent of vacuum pump oil into the mixed powder of the C powder, mixing the powder for 1 hour, and then adding ZrO₂Continuously mixing the powder and the zirconia balls for 3 hours in a three-dimensional vibration powder mixer, wherein the frequency of the three-dimensional vibration powder mixer is 30-60Hz to obtain mixed powder A, the ball-material ratio is 1-3:1, and the large-ball ratio and the small-ball ratio are 3-4: 1;

step 2, ball milling the mixed powder

Putting the mixed powder A and the zirconia balls obtained in the step 1 into a ball milling tank, and carrying out ball milling by using a planetary ball mill to obtain mixed powder B, wherein the ball-material ratio is 4-5:1, and the mass ratio of big balls to small balls is 3-4: 1;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, wherein the pressing pressure is 5-15 MPa;

step 4, sintering the green body

And (3) putting the blank C obtained in the step (3) into a graphite die, sintering by adopting a vacuum hot-pressing sintering furnace to obtain the composite material D, wherein the heating speed is 8-10 ℃/min, the sintering pressure is 20-60MPa, the sintering temperature is 1000-1300 ℃, and the sintering time is 2-4 h.

The present invention is also characterized in that,

in step 1, the grain diameter of the pure Ti powder is 20-30 mu m, B₄C powder with grain diameter of 0.5-1.0 μm, ZrO₂The particle size of the powder is 1-3 μm.

B in step 1₄The mass of the C powder accounts for 1.1-2.8% of the total mass of the powder, and ZrO₂The mass of the powder accounts for 0.1-1.1% of the total mass of the powder, and the balance is pure Ti powder.

And (3) mixing the powder in the step (1) and zirconia balls used in the ball milling in the step (2), wherein the diameter of a large ball is 9-11mm, and the diameter of a small ball is 5-6 mm.

Step 2, adding absolute ethyl alcohol with the mass fraction of 1-3% into a ball milling tank during ball milling, and filling protective gas argon; the rotation speed of the ball mill is 150-.

In the step 3, the mould used for pressing is a steel mould with the diameter of 40mm, and the pressure maintaining time is 1-6 min.

And 4, placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, checking to ensure that the graphite mold is vacuumized, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering procedure, immediately closing the diffusion pump when sintering is finished, cooling the graphite mold to room temperature along with the furnace, and taking out the sintered composite material D.

In the step 4, the diameter of the composite material D is 38-40mm, and the height is 7-8 mm.

The preparation method has the beneficial effects that the third component ZrO is prepared by the preparation method₂Is added to Ti-B₄In the C system composite material, the aim of solid solution strengthening is achieved, and the obtained Ti-ZrO₂-B₄The hardness of the C-system composite material reaches 580-620HV, and the highest compressive strength can reach 2680-3100 MPa; Ti-B without addition of a third component₄The hardness of the C-system composite material can only reach 350-400HV and the compressive strength is 2100-2380 MPa. It is obvious that the third component ZrO is added₂Of Ti-ZrO₂-B₄The C system composite material has better hardness and compressive strength and more excellent performance, can be better applied to the fields of engineering, automobile industry, aerospace and the like, and is suitable for industries with higher performance requirements.

Drawings

FIG. 1 shows a 2000-fold microstructure of a composite obtained in example 1 of the present invention;

FIG. 2 is a 2000-fold microstructure of a composite material obtained in example 2 of the present invention;

FIG. 3 shows a 2000-fold microstructure of a composite material obtained in example 3 of the present invention.

Detailed Description

The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

The invention provides high-strength Ti-ZrO₂-B₄The preparation method of the C system composite material specifically comprises the following steps:

step 1, mixing the powder

According to the mass fraction of 0.1 to 1.1 percent, the titanium-boron alloy is in the range of Ti-B₄C powder is added with a third component ZrO₂Powder of which B₄The mass of the C powder accounts for 1.1-2.8% of the total mass of the powder, the grain diameter of the pure Ti powder is 20-30 mu m, and the B powder₄C powder with grain diameter of 0.5-1.0 μm, ZrO₂The particle size of the powder is 1-3 μm. Weighing the required powder and zirconia balls required in powder mixing, wherein the ball-to-material ratio is 1-3:1, the large ball ratio is 3-4:1, the diameter of the large ball is 9-11mm, and the diameter of the small ball is 5-6 mm; mixing powder with three-dimensional vibration powder mixer with frequency of 30-60Hz, firstly mixing pure Ti powder and B powder₄Adding vacuum pump oil with mass fraction of 0.04-0.12% into the C powder, mixing for 1h, and adding prepared ZrO₂Mixing the powder and zirconia balls for 3 hours to obtain mixed powder A;

step 2, ball milling the mixed powder

Putting the mixed powder A obtained in the step 1 and the required zirconia balls into a ball milling tank, adding 1-3% of anhydrous ethanol by mass fraction, filling protective gas argon, and then performing ball milling by using a planetary ball mill to obtain mixed powder B; the ratio of balls to materials is 4-5:1, the ratio of big balls to small balls is 3-4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; the rotation speed of the ball mill is 150-;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, uniformly pressurizing in the pressing process, wherein the die is a steel die with the diameter of 40mm, the pressing pressure is 5-15MPa, and the pressure maintaining time is 1-6 min;

step 4, sintering the green body

Putting the blank C obtained in the step 3 into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for sintering; a graphite die with the diameter of 40mm is adopted, the temperature rise speed of a vacuum hot-pressing sintering furnace is 8-10 ℃/min, the sintering pressure is 20-60MPa, the sintering time is 2-4h, and the sintering temperature is 1000-1300 ℃; placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, starting vacuumizing after checking, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering program, immediately closing the program when sintering is finished, and cooling to room temperature along with the furnace to take out the sintered composite material D; the diameter of the composite material D is 38-40mm, the height is 7-8mm, and the Ti-ZrO thus obtained₂-B₄And finishing the preparation of the C system composite material.

Example 1

The invention provides high-strength Ti-ZrO₂-B₄The preparation method of the C system composite material specifically comprises the following steps:

step 1, mixing the powder

Preparing the required original powder, pure Ti powder with the particle size of 20 μm and B with the particle size of 0.5 μm₄C powder of ZrO having a particle size of 1 μm₂Powder; respectively weighing 49.52g of pure Ti powder and B powder₄C powder 0.81g, ZrO₂0.11g of powder and zirconia balls to be used, and putting the weighed powder and zirconia balls for later use; the ratio of balls to materials is 2:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; mixing powder by using a three-dimensional vibration powder mixer, wherein the frequency of the three-dimensional vibration powder mixer is 50Hz, and pure Ti powder and B powder are firstly mixed₄Adding vacuum pump oil with mass fraction of 0.08% into the C powder, mixing for 1h, and adding prepared ZrO₂Mixing the powder and zirconia balls for 3 hours to obtain mixed powder A;

step 2, ball milling the mixed powder

Putting the mixed powder A obtained in the step 1 and the required zirconia balls into a ball milling tank, adding 1% of anhydrous ethanol by mass, filling protective gas argon, and then performing ball milling by using a planetary ball mill to obtain mixed powder B; the ratio of balls to materials is 5:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; the rotation speed of the ball mill is 200r/min, the ball milling time is 12h, the positive rotation is carried out for 30min, the stopping is carried out for 12min, and the reverse rotation is carried out for 30 min;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, uniformly pressurizing in the pressing process, selecting a steel die with the diameter of 40mm as the die, and keeping the pressing pressure at 5-15MPa for 2 min;

step 4, sintering the green body

Putting the blank C obtained in the step 3 into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for sintering; a graphite die with the diameter of 40mm is adopted, the temperature rising speed of a vacuum hot-pressing sintering furnace is 10 ℃/min, the sintering pressure is 40MPa, the sintering time is 3h, and the sintering temperature is 1200 ℃; placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, starting vacuumizing after checking, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering program, immediately closing the program when sintering is finished, and cooling to room temperature along with the furnace to take out the sintered composite material D; the diameter of the composite material D was 40mm and the height was 8mm, up to this point, Ti-ZrO₂-B₄And finishing the preparation of the C system composite material.

Ti-ZrO produced in example 1 of the invention₂-B₄The microstructure of the C-system composite material is shown in FIG. 1, and the composition of the C-system composite material comprises a pure Ti matrix structure, a blocky TiC structure and a fibrous TiB structure, the interface combination is good, and the third component is ZrO₂The addition amount of (2) is 0.2%, and the Ti is basically and completely dissolved in a Ti matrix; Ti-ZrO by Archimedes drainage method₂-B₄C, calculating the density of the composite material of the system; using an electric Brookfield hardness tester of the model HBRV-187.5 to measure the Vickers hardness, wherein the pressure head of the Vickers hardness is a diamond pressure head of a regular quadrangular pyramid shape, the test force is 30 kg.N, and the pressure maintaining time is 30 s; measuring the compressive strength by using a microcomputer controlled electronic universal testing machine with the model of WDW-20; practice of the invention by the methods described aboveExample 1 preparation of Ti-ZrO₂-B₄The density, hardness and compressive strength of the C system composite material are tested and calculated, and the density is 99.9%, the hardness is 450.8HV and the compressive strength is 2523.8 MPa.

Example 2

The invention provides high-strength Ti-ZrO₂-B₄The preparation method of the C system composite material specifically comprises the following steps:

step 1, mixing the powder

Preparing the required original powder, pure Ti powder with the particle size of 20 μm and B with the particle size of 0.5 μm₄C powder of ZrO having a particle size of 1 μm₂Powder; separately weighing 49.33g of pure Ti powder and B powder₄C powder 0.81g, ZrO₂0.30g of powder and zirconia balls to be used, and putting the weighed powder and zirconia balls for later use; the ratio of balls to materials is 2:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; mixing powder by using a three-dimensional vibration powder mixer, wherein the frequency of the three-dimensional vibration powder mixer is 50Hz, and pure Ti powder and B powder are firstly mixed₄Adding vacuum pump oil with mass fraction of 0.08% into the C powder, mixing for 1h, and adding prepared ZrO₂Mixing the powder and zirconia balls for 3 hours to obtain mixed powder A;

step 2, ball milling the mixed powder

Putting the mixed powder A obtained in the step 1 and the required zirconia balls into a ball milling tank, adding 1% of anhydrous ethanol by mass, filling protective gas argon, and then performing ball milling by using a planetary ball mill to obtain mixed powder B; the ratio of balls to materials is 5:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; the rotation speed of the ball mill is 200r/min, the ball milling time is 12h, the positive rotation is carried out for 30min, the stopping is carried out for 12min, and the reverse rotation is carried out for 30 min;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, uniformly pressurizing in the pressing process, selecting a steel die with the diameter of 40mm as the die, and keeping the pressing pressure at 5-15MPa for 2 min;

step 4, sintering the green body

Putting the blank C obtained in the step 3 into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for sintering; a graphite die with the diameter of 40mm is adopted, the temperature rising speed of a vacuum hot-pressing sintering furnace is 10 ℃/min, the sintering pressure is 40MPa, the sintering time is 3h, and the sintering temperature is 1200 ℃; placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, starting vacuumizing after checking, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering program, immediately closing the program when sintering is finished, and cooling to room temperature along with the furnace to take out the sintered composite material D; the diameter of the composite material D was 40mm and the height was 7.9mm, up to this point, Ti-ZrO₂-B₄And finishing the preparation of the C system composite material.

Ti-ZrO produced in example 2 of the invention₂-B₄The microstructure of the C-system composite material is shown in FIG. 2, and the composition of the C-system composite material comprises a pure Ti matrix structure, a blocky TiC structure and a fibrous TiB structure, the interface combination is good, and the third component is ZrO₂The addition amount of (2) is 0.6%, and the Ti is basically and completely dissolved in a Ti matrix; Ti-ZrO by Archimedes drainage method₂-B₄C, calculating the density of the composite material of the system; using an electric Brookfield hardness tester of the model HBRV-187.5 to measure the Vickers hardness, wherein the pressure head of the Vickers hardness is a diamond pressure head of a regular quadrangular pyramid shape, the test force is 30 kg.N, and the pressure maintaining time is 30 s; measuring the compressive strength by using a microcomputer controlled electronic universal testing machine with the model of WDW-20; Ti-ZrO prepared by the method of example 2 of the present invention₂-B₄The density, hardness and compressive strength of the C system composite material are tested and calculated, and the density is 99.9%, the hardness is 551.3HV and the compressive strength is 2722.8 MPa.

Example 3

The invention provides high-strength Ti-ZrO₂-B₄The preparation method of the C system composite material specifically comprises the following steps:

step 1, mixing the powder

Preparing the required original powder, pure Ti powder with the particle size of 20 μm and B with the particle size of 0.5 μm₄C powder of Z having a particle size of 1 μmrO₂Powder; respectively weighing 49.12g of pure Ti powder and B powder₄C powder 0.81g, ZrO₂0.51g of powder and zirconia balls to be used, and putting the weighed powder and zirconia balls for later use; the ratio of balls to materials is 2:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; mixing powder by using a three-dimensional vibration powder mixer, wherein the frequency of the three-dimensional vibration powder mixer is 50Hz, and pure Ti powder and B powder are firstly mixed₄Adding vacuum pump oil with mass fraction of 0.08% into the C powder, mixing for 1h, and adding prepared ZrO₂Mixing the powder and zirconia balls for 3 hours to obtain mixed powder A;

step 2, ball milling the mixed powder

Putting the mixed powder A obtained in the step 1 and the required zirconia balls into a ball milling tank, adding 1% of anhydrous ethanol by mass, filling protective gas argon, and then performing ball milling by using a planetary ball mill to obtain mixed powder B; the ratio of balls to materials is 5:1, the ratio of big balls to small balls is 4:1, the diameter of the big balls is 9-11mm, and the diameter of the small balls is 5-6 mm; the rotation speed of the ball mill is 200r/min, the ball milling time is 12h, the positive rotation is carried out for 30min, the stopping is carried out for 12min, and the reverse rotation is carried out for 30 min;

step 3, press forming

Putting the mixed powder B obtained in the step 2 into a die for pressing to obtain a blank body C, uniformly pressurizing in the pressing process, selecting a steel die with the diameter of 40mm as the die, and keeping the pressing pressure at 5-15MPa for 2 min;

step 4, sintering the green body

Putting the blank C obtained in the step 3 into a graphite mold, and putting the graphite mold into a vacuum hot-pressing sintering furnace for sintering; a graphite die with the diameter of 40mm is adopted, the temperature rising speed of a vacuum hot-pressing sintering furnace is 10 ℃/min, the sintering pressure is 40MPa, the sintering time is 3h, and the sintering temperature is 1200 ℃; placing the loaded graphite mold into a furnace chamber of a vacuum hot-pressing sintering furnace, starting vacuumizing after checking, starting a diffusion pump when the vacuum degree is less than 20Pa, then starting a heating sintering program, immediately closing the program when sintering is finished, and cooling to room temperature along with the furnace to take out the sintered composite material D; the diameter of the composite material D was 40mm and the height was 8mm, up to this point, Ti-ZrO₂-B₄C system compositeAnd (5) finishing the preparation of the material.

Ti-ZrO produced in example 3 of the invention₂-B₄The microstructure of the C-system composite material is shown in FIG. 3, and it can be seen that the composition comprises a pure Ti matrix structure, a blocky TiC structure and a fibrous TiB structure, the interface bonding is good, and the third component is ZrO₂The addition amount of (1.0%) is basically completely dissolved in the Ti matrix; Ti-ZrO by Archimedes drainage method₂-B₄C, calculating the density of the composite material of the system; using an electric Brookfield hardness tester of the model HBRV-187.5 to measure the Vickers hardness, wherein the pressure head of the Vickers hardness is a diamond pressure head of a regular quadrangular pyramid shape, the test force is 30 kg.N, and the pressure maintaining time is 30 s; measuring the compressive strength by using a microcomputer controlled electronic universal testing machine with the model of WDW-20; Ti-ZrO prepared by the method of example 3 of the present invention₂-B₄The density, hardness and compressive strength of the C system composite material are tested and calculated, and the density is 99.9%, the hardness is 586.7HV and the compressive strength is 2630.4 MPa.