CN114196845A - Method for preparing titanium-based composite material by recycling TC4 residual powder - Google Patents

Method for preparing titanium-based composite material by recycling TC4 residual powder Download PDF

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CN114196845A
CN114196845A CN202111535231.9A CN202111535231A CN114196845A CN 114196845 A CN114196845 A CN 114196845A CN 202111535231 A CN202111535231 A CN 202111535231A CN 114196845 A CN114196845 A CN 114196845A
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powder
titanium
treatment
composite material
based composite
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黄陆军
刘文齐
任泽祺
卫国梁
陈晓东
张芮
陈润
安琦
耿林
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Harbin Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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Abstract

The invention provides a method for preparing a titanium-based composite material by recycling TC4 residual powder, which comprises the following steps: (1) performing ball milling treatment on the TC4 residual powder and the titanium diboride powder to obtain mixed powder; (2) and carrying out vacuum hot-pressing sintering treatment on the mixed powder to obtain the titanium-based composite material. The method provided by the invention can reuse the residual titanium alloy powder which cannot be utilized by the 3D printing technology and the powder metallurgy technology to prepare the titanium-based composite material with excellent comprehensive performance, and simultaneously realizes the low-cost preparation of the titanium-based composite material.

Description

Method for preparing titanium-based composite material by recycling TC4 residual powder
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a method for preparing a titanium matrix composite material by recycling TC4 residual powder.
Background
The TC4 titanium alloy (nominal component Ti-6Al-4V) is a universal titanium alloy with the most complete variety and specification, the largest industrial dosage and the most mature application in all titanium alloy brands, but with the technological progress and the expansion of application scenes, the requirements on the preparation method and the performance level of the titanium alloy are gradually improved, and the 3D printing technology and the powder metallurgy technology become the main preparation method of the current titanium alloy.
However, the requirements of the 3D printing technology and the powder metallurgy technology on the size and the flowability of the titanium alloy powder are high, so that a large amount of residual titanium alloy powder with large size and containing satellite balls cannot be utilized, and the residual titanium alloy powder becomes waste and is accumulated in a warehouse, which reaches hundreds of tons every year, and causes great resource waste; and with the continuous expansion of the application amount of titanium alloy components prepared by the 3D printing technology and the powder metallurgy technology, the amount of residual titanium alloy powder is rapidly increased. Although the titanium alloy residual powder can be recycled by adopting the traditional powder metallurgy technology, hot pressing sintering or hot isostatic pressing, the titanium alloy residual powder with large size and containing satellite balls can cause the alloy tissue to grow up rapidly and be uneven, and then the prepared titanium alloy has poor performance and cannot meet the use requirement. Therefore, a method capable of reusing the titanium alloy residual powder by the 3D printing technology and the powder metallurgy technology is urgently needed.
Disclosure of Invention
The embodiment of the invention provides a method for preparing a titanium-based composite material by recycling TC4 residual powder, which solves the problem that the titanium residual powder cannot be recycled in a 3D printing technology and a powder metallurgy technology, and realizes the preparation of the titanium-based composite material at low cost.
In a first aspect, the invention provides a method for preparing a titanium-based composite material by recycling TC4 residual powder, which comprises the following steps:
(1) performing ball milling treatment on the TC4 residual powder and the titanium diboride powder to obtain mixed powder;
(2) and carrying out vacuum hot-pressing sintering treatment on the mixed powder to obtain the titanium-based composite material.
Preferably, in the step (1), the particle size of the TC4 residual powder is 150-250 μm;
the residual TC4 powder also comprises satellite balls; wherein the particle size of the satellite ball is 20-70 μm.
Preferably, in the step (1), the mass ratio of the TC4 residual powder to the titanium diboride powder is 100 (0.2-1).
Preferably, in the step (1), the ball-to-material ratio adopted by the ball milling treatment is (2-4): 1;
the rotation speed of the ball milling treatment is 200-300 rpm, and the ball milling time is 210-330 min.
Preferably, after the ball milling treatment, before the obtaining of the mixed powder, the method further comprises: screening treatment;
and the screening treatment is to screen the powder obtained by ball milling the TC4 residual powder and the titanium diboride powder to obtain the mixed powder.
Preferably, the particle size of the mixed powder is 150-250 μm.
Preferably, in the step (2), the vacuum degree in the vacuum hot pressing sintering process is 1 × 10-5～1×10-3Pa, the sintering temperature is 1200-1300 ℃, the heat preservation time is 40-80 min, and the heat preservation pressure is 20-35 MPa.
Preferably, the method further comprises: and carrying out heat treatment on the titanium-based composite material.
Preferably, the heat treatment comprises solution treatment and aging treatment;
more preferably, the solid solution temperature of the solid solution treatment is 930 ℃, and the heat preservation time is 60 min;
the aging temperature of the aging treatment is 550 ℃, and the heat preservation time is 4 h.
In a second aspect, the present invention provides a titanium matrix composite obtained by recycling the residual TC4 powder of the first aspect.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the invention, a vacuum hot-pressing sintering technology is adopted, titanium alloy residual powder (TC4 residual powder) which is large in size and contains satellite balls and cannot be used by a 3D printing technology and a powder metallurgy technology is mixed with a ceramic reinforcing phase raw material (titanium diboride), so that the titanium-based composite material with low cost and high performance is successfully prepared, and the room-temperature tensile strength of the titanium-based composite material is 902-1204 MPa.
(2) Compared with pure TC4 titanium alloy, the invention adopts TC4 residual powder which has lower cost and can not be used for 3D printing technology and powder metallurgy technology, solves the problem of resource waste and has more application prospect; the elongation and tensile strength of the prepared titanium-based composite material are obviously improved, the titanium-based composite material has excellent mechanical property, and the titanium-based composite material has uniform tissue; meanwhile, the titanium-based composite material greatly widens the heat treatment window, and is more beneficial to uniform organization and improvement of mechanical property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing a titanium-based composite material by recycling TC4 residual powder according to an embodiment of the present invention;
FIG. 2 is an electron micrograph of excess TC4 powder of example 2 of the present invention;
FIG. 3 is an electron micrograph of a mixed powder in example 2 of the present invention;
FIG. 4 is an electron micrograph of a titanium-based composite material prepared in example 2 of the present invention;
FIG. 5 is a tensile stress-strain curve of titanium-based composites prepared in examples 2 and 3 and pure TC4 titanium alloy prepared in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention, and based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the scope of the present invention.
Compared with the existing pure titanium alloy, the titanium-based composite material has higher strength, rigidity, wear resistance and higher use temperature, and particularly, the ceramic reinforcing phase in the titanium-based composite material can inhibit the growth of matrix tissues. Therefore, based on the titanium-based composite material regulation and control idea, the ceramic reinforcing phase is added into the large-size TC4 residual powder to further prepare the titanium-based composite material with excellent performance through hot-pressing sintering and in-situ reaction self-generation technology, so that the problem that the titanium alloy residual powder in the 3D printing technology and the powder metallurgy technology cannot be reused is solved.
Specific implementations of the above concepts are described below.
As shown in FIG. 1, the embodiment of the present invention provides a method for preparing a titanium-based composite material by recycling TC4 residual powder, which comprises the following steps:
(1) performing ball milling treatment on the TC4 residual powder and the titanium diboride powder to obtain mixed powder;
(2) and carrying out vacuum hot-pressing sintering treatment on the mixed powder to obtain the titanium-based composite material.
In the present invention, the large size and satellite sphere containing TC4 residual powder is mixed with a ceramic reinforcing phase (titanium diboride TiB)2) Ball milling is carried out to pass through the ballsThe method comprises the steps of grinding, coating TC4 residual powder and dispersing satellite balls with a ceramic reinforcing phase, and then further performing vacuum hot-pressing sintering to enable titanium diboride and titanium (TC4 residual powder) to perform in-situ self-generated reaction to generate a titanium boride whisker (TiBw) reinforcing phase, so that the reinforcing effect can be achieved, the strength of the titanium-based composite material is improved, further coarsening of the titanium-based composite material tissue can be effectively inhibited through coating distribution, the low-cost titanium-based composite material with excellent comprehensive performance is ensured to be obtained, and the problem that the titanium alloy residual powder cannot be reused in the 3D printing technology and the powder metallurgy technology is solved.
On the basis of preparing the titanium-based composite material by powder metallurgy at present, TC4 residual powder is mixed with ceramic reinforcement to replace TC4 powder with higher price, small size and high sphericity, so that TC4 residual powder which cannot be effectively utilized at present is utilized, resource waste is avoided, and cost is reduced from the source, therefore, the method for preparing the titanium-based composite material by reusing the TC4 residual powder has economic and social benefits.
It should be noted that, the method for preparing the titanium-based composite material by reusing the residual powder of TC4 provided by the present invention includes, but is not limited to, the residual powder of TC4, and for other titanium alloy residual powders, the method provided by the present invention can be also used to prepare the titanium-based composite material, and the present invention is preferably the residual powder of TC4 which is widely used and has a large dosage.
According to some preferred embodiments, in step (1), the particle size of the TC4 residual powder is 150 to 250 μm (e.g., may be 150 μm, 160 μm, 170 μm, 180 μm, 190 μm, 200 μm, 210 μm, 220 μm, 230 μm, 240 μm, or 250 μm);
the residual TC4 powder also comprises satellite balls; wherein the particle size of the satellite is 20-70 μm (for example, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm or 70 μm).
It should be noted that the titanium diboride powder may be commercially available titanium diboride powder.
In the invention, it should be noted that, because the requirements of the 3D printing and powder metallurgy technology on the size and the fluidity of the titanium alloy powder are high, the large-size TC4 residual powder with the particle size range of 150-250 μm and containing satellite balls cannot meet the requirements, and cannot be used in the 3D printing and powder metallurgy technology, which causes great waste of the TC4 residual powder.
According to some preferred embodiments, in the step (1), the mass ratio of the TC4 residual powder to the titanium diboride powder is 100 (0.2-1) (for example, 100:0.2, 100:0.3, 100:0.4, 100:0.5, 100:0.6, 100:0.7, 100:0.8, 100:0.9 or 100:1 may be used).
In the invention, the inventor finds that when the mass ratio of the TC4 residual powder to the titanium diboride powder is higher than 100:0.2, the titanium diboride powder accounts for too little and is difficult to achieve the effects of strengthening and inhibiting the growth of matrix tissues, so that the prepared titanium-based composite material has poor performance and cannot meet the use requirement; when the mass ratio of the TC4 residual powder to the titanium diboride powder is lower than 100:1, the prepared titanium-based composite material has high brittleness and even loses use value.
According to some preferred embodiments, in the step (1), the ball milling treatment adopts a ball-to-material ratio of (2-4): 1 (for example, 2:1, 2.5:1, 3:1, 3.5:1 or 4: 1);
the rotation speed of the ball milling treatment is 200-300 rpm (for example, 200rpm, 220rpm, 240rpm, 250rpm, 260rpm, 280rpm or 300rpm can be selected), and the ball milling time is 210-330 min (for example, 210min, 220min, 240min, 250min, 270min, 300min, 320min or 330min can be selected).
In addition, GCr15 bearing steel balls were used for the ball milling treatment.
In the invention, the purpose of ball milling treatment is to uniformly coat fine ceramic powder (namely titanium diboride powder) on the surface of the residual TC4 powder so as to prevent the growth of TC4 matrix tissues in the vacuum hot-pressing sintering process and disperse satellite balls by utilizing the ball milling process.
According to some preferred embodiments, after the ball milling treatment, before the obtaining of the mixed powder, the method further comprises: screening treatment;
and the screening treatment is to screen the powder obtained by ball milling the TC4 residual powder and the titanium diboride powder to obtain the mixed powder.
According to some preferred embodiments, the particle size of the mixed powder is 150 to 250 μm (for example, 150 μm, 160 μm, 170 μm, 180 μm, 190 μm, 200 μm, 210 μm, 220 μm, 230 μm, 240 μm, or 250 μm may be used).
According to the invention, the large-size mixed powder can be further separated from the satellite balls through screening, so that the content of the satellite balls in the mixed powder is greatly reduced, and the satellite balls are basically not contained in the mixed powder, so that the satellite balls are prevented from influencing the comprehensive performance of the prepared titanium-based composite material.
According to some preferred embodiments, in the step (2), the degree of vacuum in the vacuum hot press sintering process is 1 × 10-5～1×10-3Pa (for example, may be 1X 10-5Pa、2×10-5Pa、5×10-5Pa、8×10-5Pa、1×10-4Pa、2×10-4Pa、5×10-4Pa or 1X 10-3Pa, etc.), the sintering temperature is 1200-1300 deg.C (for example, 1200 deg.C, 1220 deg.C, 1240 deg.C, 1250 deg.C, 1260 deg.C, 1280 deg.C, or 1300 deg.C), the holding time is 40-80 min (for example, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, or 80min), and the holding pressure is 20-35 MPa (for example, 20MPa, 22MPa, 25MPa, 28MPa, 30MPa, 32MPa, 34MPa, or 35 MPa).
In the invention, in the vacuum hot-pressing sintering process, titanium diboride and titanium (TC4 residual powder) can generate an in-situ reaction to generate a titanium boride whisker (TiBw) reinforced phase, and meanwhile, the titanium-based composite material can be compacted on the basis of heat preservation pressure to obtain the compact titanium-based composite material.
According to some preferred embodiments, the method further comprises: and carrying out heat treatment on the titanium-based composite material.
According to some preferred embodiments, the heat treatment comprises solution treatment and aging treatment.
According to some more preferred embodiments, the solution temperature of the solution treatment is 930 ℃ and the holding time is 60 min;
the aging temperature of the aging treatment is 550 ℃, and the heat preservation time is 4 h.
More specifically, the temperature and treatment time of the solution treatment and the aging treatment need to be determined with reference to a titanium alloy heat treatment schedule manual. Wherein the heat treating the titanium-based composite material comprises: the titanium-based composite material is subjected to solution treatment and aging treatment in sequence, the titanium-based composite material is firstly placed at 930 ℃ and is subjected to heat preservation for 60min, then is put into water to be quenched to room temperature, the solution treatment is completed, and then the heat preservation is carried out at 550 ℃ for 4h, the aging treatment is completed, so that the matrix structure of the titanium-based composite material is regulated and controlled, and the mechanical property of the titanium-based composite material is optimized.
In the invention, the reinforcing phase is introduced into the titanium-based composite material, so that the heat treatment window is greatly widened, namely, compared with a pure titanium alloy without introducing the reinforcing phase, the temperature ranges of the solid solution treatment and the aging treatment can be controlled without strict control, and the corresponding solid solution treatment and the aging treatment can be realized. By performing the high-temperature solution treatment for a long time in this manner, the matrix structure can be made uniform, and the mechanical properties can be greatly improved.
The invention also provides a titanium-based composite material, which is obtained by the method for preparing the titanium-based composite material by recycling the TC4 residual powder.
The titanium-based composite material prepared by the invention has excellent mechanical properties, and the room-temperature tensile strength is 902-1204 MPa.
In order to more clearly illustrate the technical solution and advantages of the present invention, a method for preparing a titanium-based composite material by recycling the residual TC4 powder is described in detail below through several examples.
Example 1
Preparation of TC4 titanium-based composite with 0.5 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:0.3, carrying out ball milling treatment for 240min at the rotating speed of 220rpm, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 4: 1;
(2) filling the mixed powder obtained in the step (1) into a graphite dieIn 1 × 10-4And (3) keeping the temperature of the titanium matrix composite material at 1200 ℃ for 40min under the conditions of Pa vacuum degree and 25MPa pressure to prepare the TC4 titanium matrix composite material containing 0.5 vol.% TiBw reinforcement.
Example 2
Preparation of TC4 titanium-based composite with 1.0 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:0.59, carrying out ball milling treatment for 240min at the rotating speed of 220rpm, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 4: 1;
(2) putting the mixed powder obtained in the step (1) into a graphite die at a temperature of 1 x 10-4And (3) keeping the temperature of the titanium matrix composite material at 1200 ℃ for 40min under the conditions of Pa vacuum degree and 25MPa pressure to prepare the TC4 titanium matrix composite material containing 1.0 vol.% TiBw reinforcement.
Example 3
Preparation of TC4 titanium-based composite with 1.0 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:0.59, carrying out ball milling treatment for 240min at the rotating speed of 220rpm, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 4: 1;
(2) putting the mixed powder obtained in the step (1) into a graphite die at a temperature of 1 x 10-4Keeping the temperature of the vacuum degree of Pa and the pressure of 25MPa at 1200 ℃ for 40min to prepare the TC4 titanium-based composite material containing 1.0 vol.% TiBw reinforcement;
(3) heat treating the TC4 titanium-based composite material containing 1.0 vol.% TiBw reinforcement obtained in step (2): firstly preserving heat at the solid solution temperature of 930 ℃ for 60min, then putting the titanium-based composite material into water for quenching to room temperature (25 ℃), preserving heat at 550 ℃ for 4h to finish aging treatment, and obtaining the TC4 titanium-based composite material containing 1.0 vol.% TiBw reinforcement after heat treatment.
Example 4
Preparation of TC4 titanium-based composite with 1.7 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:1.0, carrying out ball milling treatment for 240min at the rotating speed of 220rpm, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 4: 1;
(2) putting the mixed powder obtained in the step (1) into a graphite die at a temperature of 1 x 10-4And keeping the temperature of the titanium-based composite material at 1200 ℃ for 40min under the conditions of the vacuum degree of Pa and the pressure of 25MPa to prepare the TC4 titanium-based composite material containing 1.7 vol.% TiBw reinforcement.
Example 5
Example 5 is essentially the same as example 2, except that:
preparation of TC4 titanium-based composite with 0.35 vol.% TiBw reinforcement:
the mass ratio of the TC4 residual powder to the titanium diboride powder in the step (1) is 100: 0.2.
Example 6
Preparation of TC4 titanium-based composite with 1.0 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:0.59, carrying out ball milling treatment for 210min at the rotating speed of 200rpm, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 3: 1;
(2) putting the mixed powder obtained in the step (1) into a graphite die at a temperature of 1 x 10-5And (3) keeping the temperature of the titanium matrix composite material at 1250 ℃ for 60min under the conditions of the vacuum degree of Pa and the pressure of 20MPa to prepare the TC4 titanium matrix composite material containing 1.0 vol.% TiBw reinforcement.
Example 7
Preparation of TC4 titanium-based composite with 1.0 vol.% TiBw reinforcement:
(1) mixing TC4 residual powder (the particle size is 150-250 mu m and contains satellite balls, the particle size of the satellite balls is 20-70 mu m) and titanium diboride powder according to the mass ratio of 100:0.59, carrying out ball milling treatment at the rotating speed of 300rpm for 330min, and carrying out screening treatment after the ball milling is finished to obtain mixed powder (the particle size is 150-250 mu m); GCr15 bearing steel balls are used for ball milling treatment, and the ball-material ratio is 2: 1;
(2) putting the mixed powder obtained in the step (1) into a graphite die at a temperature of 1 x 10-3And (3) keeping the temperature of the titanium matrix composite material at 1300 ℃ for 80min under the conditions of the vacuum degree of Pa and the pressure of 35MPa to prepare the TC4 titanium matrix composite material containing 1.0 vol.% TiBw reinforcement.
Comparative example 1
Preparing pure TC4 titanium alloy:
putting TC4 residual powder (with particle size of 150-250 μm and containing satellite balls with particle size of 20-70 μm) into a graphite mold, and adding into the graphite mold at a temperature of 1 × 10-4And (3) keeping the temperature of the mixture for 40min at 1200 ℃ under the vacuum degree of Pa and the pressure of 25MPa to prepare the pure TC4 titanium alloy.
Comparative example 2
Preparing pure TC4 titanium alloy:
charging pure TC4 powder (particle size less than or equal to 150 μm, no satellite balls) into graphite mold at 1 × 10-4And (3) keeping the temperature of the mixture for 40min at 1200 ℃ under the vacuum degree of Pa and the pressure of 25MPa to prepare the pure TC4 titanium alloy.
Comparative example 3
Comparative example 3 is substantially the same as example 2 except that:
the method is characterized in that the TC4 residual powder (with the particle size of 150-250 mu m and containing satellite balls with the particle size of 20-70 mu m) is not adopted, but pure TC4 powder (with the particle size of less than or equal to 150 mu m and containing no satellite balls) is adopted.
The titanium-based composites prepared in examples 1 to 7 and the materials prepared in comparative examples 1 to 3 were subjected to tensile property tests at room temperature (25 ℃ C.), respectively, and the test results are shown in Table 1.
Specifically, fig. 2 to 4 respectively correspond to electron microscope images of the TC4 residual powder, the mixed powder, and the titanium-based composite material in example 2. As can be seen from fig. 2, the TC4 residual powder before ball milling has more satellite balls and has larger particle size; ball milling of the satellite balls in FIG. 3The amount is greatly reduced, and basically no satellite ball exists; in FIG. 4, fine α/β sheets and TiB are uniformly distributed2And Ti to obtain TiBw crystal whisker through in-situ self-generation reaction. In addition, the tensile strength of the titanium-based composite material prepared in the example 2 at 500 ℃ reaches 647MPa, which shows that the titanium-based composite material prepared in the example of the invention still has good performance at high temperature.
FIG. 5 shows the strain of the titanium-based composites prepared in examples 2 and 3 and the pure TC4 titanium alloy prepared in comparative example 1 under different tensile stresses. Wherein the curve in FIG. 5 corresponding to 1.0 vol.% is the tensile stress-strain curve for the titanium-based composite prepared in example 2; the curve corresponding to 1.0 vol.% heat treatment is the tensile stress-strain curve for the titanium-based composite material prepared in example 3; the curve corresponding to the pure TC4 alloy is the tensile stress-strain curve for the titanium-based composite material prepared in comparative example 1. Obviously, the titanium-based composite material prepared by the method has better tensile strength than pure TC4 alloy, and the tensile strength of the titanium-based composite material after heat treatment is further improved.
TABLE 1
Figure BDA0003412966900000101
As can be seen from Table 1, the tensile strength at room temperature of the pure TC4 titanium alloy prepared by only using the residual TC4 powder in the comparative example 1 is only 766MPa, and the elongation is only 8.2%, which is lower than the tensile strength at room temperature of 889MPa and the elongation of 14% of the pure TC4 titanium alloy prepared by using the high-cost and small-size pure TC4 powder in the comparative example 2. However, in examples 1 to 7, the low-cost titanium diboride powder is added into the residual TC4 powder, so that the room-temperature tensile strength and elongation of the prepared titanium-based composite material are improved, and the advantage of low cost is still achieved; even in comparison with comparative example 3, example 2 has better elongation of the prepared titanium-based composite material while ensuring the advantage of low cost.
In conclusion, the performance effect of directly preparing the pure titanium alloy from the large-size TC4 residual powder is poor, but the strength and the elongation of the material are greatly improved after the titanium diboride is added to prepare the titanium-based composite material, so that the combination of the titanium diboride and the TC4 residual powder is remarkably improved, and the preparation cost of the titanium-based composite material is greatly reduced.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for preparing a titanium-based composite material by recycling TC4 residual powder is characterized by comprising the following steps:
(1) performing ball milling treatment on the TC4 residual powder and the titanium diboride powder to obtain mixed powder;
(2) and carrying out vacuum hot-pressing sintering treatment on the mixed powder to obtain the titanium-based composite material.
2. The method according to claim 1, wherein in step (1):
the particle size of the TC4 residual powder is 150-250 mu m;
the residual TC4 powder also comprises satellite balls; wherein the particle size of the satellite ball is 20-70 μm.
3. The method according to claim 1, wherein in step (1):
the mass ratio of the TC4 residual powder to the titanium diboride powder is 100 (0.2-1).
4. The method according to claim 1, wherein in step (1):
the ball-material ratio adopted in the ball milling treatment is (2-4) to 1;
the rotation speed of the ball milling treatment is 200-300 rpm, and the ball milling time is 210-330 min.
5. The method according to claim 1, wherein in step (1):
after the ball milling treatment, before the mixed powder is obtained, the method further comprises the following steps: screening treatment;
and the screening treatment is to screen the powder obtained by ball milling the TC4 residual powder and the titanium diboride powder to obtain the mixed powder.
6. The method of claim 1, wherein:
the particle size of the mixed powder is 150-250 mu m.
7. The method according to any one of claims 1 to 6, wherein in step (2):
the vacuum degree in the vacuum hot pressing sintering treatment is 1 multiplied by 10-5～1×10-3Pa, the sintering temperature is 1200-1300 ℃, the heat preservation time is 40-80 min, and the heat preservation pressure is 20-35 MPa.
8. The method of any of claims 1 to 7, further comprising: and carrying out heat treatment on the titanium-based composite material.
9. The method of claim 8, wherein:
the heat treatment comprises solution treatment and aging treatment;
preferably, the solid solution temperature of the solid solution treatment is 930 ℃, and the heat preservation time is 60 min;
the aging temperature of the aging treatment is 550 ℃, and the heat preservation time is 4 h.
10. A titanium matrix composite obtained by recycling the residual TC4 powder of any one of claims 1 to 9.
CN202111535231.9A 2021-12-15 2021-12-15 Method for preparing titanium-based composite material by recycling TC4 residual powder Pending CN114196845A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101333607A (en) * 2008-07-31 2008-12-31 哈尔滨工业大学 Process for preparing TiBw/Ti alloy-based composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101333607A (en) * 2008-07-31 2008-12-31 哈尔滨工业大学 Process for preparing TiBw/Ti alloy-based composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈学文: "钛合金粉末冶金制备工艺及力学性能研究", 《冶金与材料》 *

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