CN114393209A - Titanium-based composite powder with core-shell structure and preparation method and application thereof - Google Patents

Titanium-based composite powder with core-shell structure and preparation method and application thereof Download PDF

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CN114393209A
CN114393209A CN202210237845.7A CN202210237845A CN114393209A CN 114393209 A CN114393209 A CN 114393209A CN 202210237845 A CN202210237845 A CN 202210237845A CN 114393209 A CN114393209 A CN 114393209A
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powder
titanium
based composite
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CN114393209B (en
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安琦
黄陆军
王帅
张芮
王存玉
陈润
孟凡超
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
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
    • 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
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

The invention relates to the technical field of titanium-based composite materials, in particular to titanium-based composite powder with a core-shell structure, and a preparation method and application thereof. The preparation method of the titanium-based composite material comprises the following steps: the method comprises the following steps: uniformly mixing titanium metal powder and ceramic powder to obtain a mixture, wherein the particle size of the ceramic powder is smaller than that of the titanium metal powder; step two: heating the mixture to raise the temperature of the mixture to a preset temperature, wherein the preset temperature is the temperature at which the titanium metal powder and the ceramic undergo in-situ self-generation reaction; step three: and carrying out heat preservation treatment on the mixture at the preset temperature to obtain the titanium-based composite powder with the core-shell structure. The invention provides titanium-based composite powder with a core-shell structure and a preparation method thereof, and the titanium-based composite powder can be applied to the additive manufacturing technology for preparing a titanium-based composite material.

Description

Titanium-based composite powder with core-shell structure and preparation method and application thereof
Technical Field
The invention relates to the technical field of titanium-based composite materials, in particular to titanium-based composite powder with a core-shell structure, and a preparation method and application thereof.
Background
The titanium-based composite material has excellent performances such as high specific strength, high temperature resistance and the like, and is an important material applied to the technical field of aerospace, such as parts of aircrafts prepared from the titanium-based composite material. The additive manufacturing technology is a manufacturing technology for integrally molding powder raw materials, and is a main technical means for preparing titanium-based composite material parts at present.
In the prior art, the method for preparing the titanium-based composite material by using the additive manufacturing technology mainly comprises the following three methods: (1) the titanium metal powder and the fine reinforcement powder are uniformly mixed to enable the ceramic powder to be distributed on the surfaces of titanium metal powder particles, then the titanium-based composite material is manufactured by using an additive manufacturing technology, but the bonding strength of the ceramic distributed on the surfaces of the titanium metal and the titanium metal is weak, the ceramic is easy to fall off in the powder feeding process, and the microstructure and the performance of the manufactured titanium-based composite material are further influenced. In addition, during the additive manufacturing process, the ceramic powder and the titanium metal powder can undergo an in-situ self-generated reaction, which is an exothermic reaction, so that the local thermal stress is increased, and further the cracking risk of the titanium-based composite material is increased. (2) Firstly, processing titanium metal and ceramic into a titanium-based composite material rod by using a hot-pressing sintering or fusion casting method, then processing the titanium-based composite material rod into titanium-based composite powder by using a gas atomization powder preparation technology or a rotary electrode powder preparation technology, and then preparing the titanium-based composite powder into the titanium-based composite material by using an additive manufacturing technology. The titanium-based composite powder prepared by the method has high quality and good performance, and because the in-situ self-generated reaction is generated in the process of preparing the titanium-based composite powder, the in-situ self-generated reaction can not be generated in the process of subsequently manufacturing the titanium-based composite material by the additive, and the problem of thermal stress caused by the reaction is also avoided. However, the method has the disadvantages of complex preparation process, long period and high cost. (3) The titanium metal powder and the ceramic powder are respectively fed into a molten pool by two sets of powder feeding systems, and the titanium-based composite material is prepared by directly utilizing an additive manufacturing technology. However, the method easily causes the uneven mixing of the two powders and insufficient reaction, thereby causing defects in the prepared titanium-based composite material, poor microstructure and poor performance.
Disclosure of Invention
The embodiment of the invention provides titanium-based composite powder with a core-shell structure and a preparation method and application thereof, and can provide titanium-based composite powder with a core-shell structure and a preparation method thereof.
In a first aspect, a method for preparing a titanium-based composite powder with a core-shell structure comprises the following steps:
the method comprises the following steps: uniformly mixing titanium metal powder and ceramic powder to obtain a mixture, wherein the particle size of the ceramic powder is smaller than that of the titanium metal powder;
step two: heating the mixture to raise the temperature of the mixture to a preset temperature, wherein the preset temperature is the temperature at which the titanium metal powder and the ceramic undergo in-situ self-generation reaction;
step three: and carrying out heat preservation treatment on the mixture at the preset temperature to obtain the titanium-based composite powder with the core-shell structure.
Preferably, in the step one, the titanium metal powder is pure titanium powder, TC4 titanium alloy powder or TA15 titanium alloy powder, and the ceramic powder is graphite powder or TiB powder2Powder or B4And C, powder.
Preferably, in the step one, the particle size of the titanium metal powder is 50 to 200 μm, and the particle size of the ceramic powder is 0.5 to 8 μm.
Preferably, in step one, the method comprises the following steps:
performing ball milling treatment on the titanium metal powder and the ceramic powder in an argon atmosphere for 3-6 hours, wherein the rotating speed of the ball milling treatment is 150-250r/min, and the ball-to-material ratio is (2-6): 1.
Preferably, the ball milling tank and the milling balls of the ball milling treatment are both made of hard alloy.
Preferably, in the step one, after the ball milling treatment, the obtained mixture is subjected to a standing treatment in an argon atmosphere, and the standing treatment time is more than 5 hours.
Preferably, in the second step, the heating treatment is performed in a vacuum environment with a vacuum degree of 1 × 10-3～1×10-2Pa, and the preset temperature is 700-1100 ℃.
Preferably, in the third step, the heat preservation treatment is performed in a vacuum environment with a vacuum degree of 1 × 10-3～1×10-2Pa, and the treatment time of the heat preservation treatment is 0.5-2 h.
In a second aspect, the invention provides a titanium-based composite powder with a core-shell structure, which is prepared by the preparation method of any one of the first aspect.
Preferably, the volume fraction of the reinforcing phase in the titanium-based composite material is 1-10 vol.%.
In a third aspect, the invention provides an application of the titanium-based composite powder with the core-shell structure, wherein the titanium-based composite powder is the titanium-based composite powder in the second aspect, and the titanium-based composite powder is applied to the preparation of a titanium-based composite material by adopting an additive manufacturing technology.
Compared with the prior art, the invention at least has the following beneficial effects:
in the invention, the titanium metal powder and the ceramic powder are uniformly mixed, so that the fine ceramic powder is uniformly coated on the particle surface of the titanium metal powder, and the mixture with the ceramic-coated titanium metal structure is obtained. And heating the mixture to a preset temperature, wherein the ceramic and the titanium metal undergo an in-situ self-generation reaction at the preset temperature, and the titanium element on the surface of the titanium metal particle begins to react with the ceramic coated on the surface of the titanium metal particle to generate a reinforcing phase. And (2) carrying out heat preservation treatment on the mixture at the preset temperature to provide sufficient reaction time for in-situ self-generated reaction of the ceramic and the titanium metal, so that the reaction is carried out more fully, the ceramic coated on the surface of the titanium metal particle is completely reacted to form a reinforcing phase, and the reinforcing phase is coated on the surface of the titanium metal particle to form a core-shell structure, thereby obtaining the titanium-based composite powder with the core-shell structure.
In the present invention, since the reinforcing phase is directly formed on the surface of the titanium metal particles by reaction, the interface bonding strength between the reinforcing phase and the titanium metal particles is high and the titanium metal particles are not easily detached. In addition, the titanium-based composite powder with the core-shell structure provided by the invention has in-situ autogenous reaction during preparation, so that the in-situ autogenous reaction cannot occur when the titanium-based composite powder with the core-shell structure is used for preparing the titanium-based composite material by adopting an additive manufacturing technology, thereby avoiding the problem of local thermal stress increase in the process of additive manufacturing of the titanium-based composite material, and further ensuring that the prepared titanium-based composite material has good performance and is not easy to crack.
In the invention, the titanium-based composite powder with the core-shell structure can be obtained only by uniformly mixing the titanium metal powder and the ceramic powder and then carrying out heating and heat preservation treatment. In addition, the prepared titanium-based composite powder with the core-shell structure has high sphericity and good fluidity, the type and size of the powder and the content of the reinforcing phase can be adjusted by adjusting the type, the grain diameter and the mass ratio of the titanium metal powder and the ceramic powder, and the titanium-based composite powder provided by the invention is suitable for additive manufacturing technology.
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 sectional electron microscope of titanium-based composite powder particles with a core-shell structure provided in example 2 of the present invention;
FIG. 2 is a partially enlarged sectional electron microscope of titanium-based composite powder particles having a core-shell structure according to example 2 of the present invention;
FIG. 3 is an electron microscope image of the surface of a titanium-based composite powder particle having a core-shell structure provided in example 2 of the present invention;
FIG. 4 is a partially enlarged surface electron micrograph of titanium-based composite powder particles having a core-shell structure according to example 2 of the present invention.
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.
The embodiment of the invention provides a preparation method of titanium-based composite powder with a core-shell structure, which comprises the following steps:
the method comprises the following steps: uniformly mixing titanium metal powder and ceramic powder to obtain a mixture, wherein the particle size of the ceramic powder is smaller than that of the titanium metal powder;
step two: heating the mixture to raise the temperature of the mixture to a preset temperature, wherein the preset temperature is the temperature at which the titanium metal powder and the ceramic undergo in-situ self-generation reaction;
step three: and carrying out heat preservation treatment on the mixture at the preset temperature to obtain the titanium-based composite powder with the core-shell structure.
In the invention, the titanium metal powder and the ceramic powder are uniformly mixed, so that the fine ceramic powder is uniformly coated on the particle surface of the titanium metal powder, and the mixture with the ceramic-coated titanium metal structure is obtained. And heating the mixture to a preset temperature, wherein the ceramic and the titanium metal undergo an in-situ self-generation reaction at the preset temperature, and the titanium element on the surface of the titanium metal particle begins to react with the ceramic coated on the surface of the titanium metal particle to generate a reinforcing phase. And (2) carrying out heat preservation treatment on the mixture at the preset temperature to provide sufficient reaction time for in-situ self-generated reaction of the ceramic and the titanium metal, so that the reaction is carried out more fully, the ceramic coated on the surface of the titanium metal particle is completely reacted to form a reinforcing phase, and the reinforcing phase is coated on the surface of the titanium metal particle to form a core-shell structure, thereby obtaining the titanium-based composite powder with the core-shell structure.
In the present invention, since the reinforcing phase is directly formed on the surface of the titanium metal particles by reaction, the interface bonding strength between the reinforcing phase and the titanium metal particles is high and the titanium metal particles are not easily detached. In addition, the titanium-based composite powder with the core-shell structure provided by the invention has in-situ autogenous reaction during preparation, so that the in-situ autogenous reaction cannot occur when the titanium-based composite powder with the core-shell structure is used for preparing the titanium-based composite material by adopting an additive manufacturing technology, thereby avoiding the problem of local thermal stress increase in the process of additive manufacturing of the titanium-based composite material, and further ensuring that the prepared titanium-based composite material has good performance and is not easy to crack.
In the invention, the titanium-based composite powder with the core-shell structure can be obtained only by uniformly mixing the titanium metal powder and the ceramic powder and then carrying out heating and heat preservation treatment. In addition, the prepared titanium-based composite powder with the core-shell structure has high sphericity and good fluidity, the type and size of the powder and the content of the reinforcing phase can be adjusted by adjusting the type, the grain diameter and the mass ratio of the titanium metal powder and the ceramic powder, and the titanium-based composite powder provided by the invention is suitable for additive manufacturing technology.
According to some preferred embodiments, in the step one, the titanium metal powder is pure titanium powder, TC4 titanium alloy powder or TA15 titanium alloy powder, and the ceramic powder is graphite powder, TiB2Powder or B4And C, powder.
In the invention, pure titanium powder, TC4 titanium alloy powder or TA15 titanium alloy powder are selected to prepare titanium-based composite powder with a core-shell structure, wherein the TA15 titanium alloy has excellent high-temperature resistance; meanwhile, the type of the titanium alloy powder can be selected according to the use requirement.
In the present invention, TiB2After being mixed, the ceramic powder and the titanium metal powder can perform in-situ self-reaction at a preset temperature to form a stable TiB reinforcing phase. After being mixed, the graphite powder and the titanium metal powder can perform in-situ self-reaction at a preset temperature to form a stable TiC reinforcing phase. B is4After being mixed, the C ceramic powder and the titanium metal powder can perform in-situ self-reaction at a preset temperature to form stable TiC and TiB reinforcing phases.
It should be noted that the titanium metal powder is not limited to the titanium alloy powder described above, and any titanium-containing alloy is suitable for the preparation method provided by the present invention.
According to some preferred embodiments, in the first step, the titanium metal powder has a particle size of 50 to 200 μm (for example, 50 μm, 100 μm, 150 μm or 200 μm), and the ceramic powder has a particle size of 0.5 to 8 μm (for example, 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm or 8 μm).
In the invention, the grain diameter of the ceramic powder is 0.5-8 μm, and the grain diameter of the titanium metal powder is 50-200 μm, so that after the two powders are uniformly mixed, the fine ceramic powder can wrap the surface of the titanium metal powder particles.
According to some preferred embodiments, in the step one, the method comprises the following steps:
performing ball milling treatment on the titanium metal powder and the ceramic powder in an argon atmosphere for 3-6 h (for example, 3h, 4h, 5h or 6h), wherein the rotation speed of the ball milling treatment is 150-250r/min (for example, 150r/min, 200r/min or 250r/min), and the ball-to-material ratio is (2-6): 1 (for example, 2:1, 3:1, 4:1, 5:1 or 6: 1).
In the invention, the titanium metal powder and the ceramic powder can be fully and uniformly mixed by ball milling treatment, and the titanium metal powder and the ceramic powder can be protected from being oxidized in the ball milling process under the argon atmosphere. In the process of ball milling, under the action of the grinding balls, the ceramic powder is adhered and wrapped on the surfaces of the titanium metal powder particles.
It should be noted that, in the solution of the present invention, the low-energy ball milling process at the rotation speed of 150-. According to some preferred embodiments, the ball milling pot and the milling balls of the ball milling process are made of cemented carbide.
In the invention, the hard alloy has a series of excellent performances of high hardness, wear resistance, good strength and toughness, heat resistance, corrosion resistance and the like, particularly high hardness and wear resistance, and is suitable for manufacturing ball milling tanks and grinding balls. The ball milling treatment is carried out by adopting the ball milling tank and the milling balls made of hard alloy, so that the ceramic powder can be more uniformly adhered and wrapped on the surfaces of the titanium metal powder particles.
According to some preferred embodiments, in the step one, after the ball milling treatment, the obtained mixture is subjected to a standing treatment in an argon atmosphere, and the standing treatment time is more than 5 h.
In the invention, because the temperature of the mixture powder after ball milling treatment is high, the mixture is subjected to standing treatment in an argon atmosphere to reduce the heat of the mixture powder to room temperature (15-35 ℃), so that the phenomenon that the high-temperature mixture powder is oxidized by reacting with oxygen to pollute the mixture powder can be avoided.
According to some preferred embodiments, in the second step, the heating treatment is performed in a vacuum environment with a vacuum degree of 1 × 10-3～1×10-2Pa, the preset temperature is 700-1100 ℃ (for example, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ or 1100 ℃).
In the invention, the temperature is raised to the preset temperature in the vacuum environment, so that the ceramic and the titanium metal can react, the titanium metal powder can not be melted, and the generated enhanced phase has small size and uniform distribution. If the temperature of the heating treatment cannot reach 700 ℃, the ceramic and the titanium metal cannot be fully reacted, and the ceramic remains; if the temperature of the heating treatment is higher than 1100 ℃, the titanium metal powder can be seriously softened and adhered to each other to form blocks, and the prepared titanium-based composite material powder has poor quality and low powder rate.
According to some preferred embodiments, in step three, the heat-preserving treatment is performed in a vacuum environment with a vacuum degree of 1 × 10-3～1×10-2Pa, and the treatment time of the heat preservation treatment is 0.5-2 h (for example, 0.5h, 1h, 1.5h or 2 h).
In the invention, the mixture is subjected to heat preservation treatment in a vacuum environment, so that the ceramic can be completely reacted, and the ceramic can completely generate a reinforcing phase.
The embodiment of the invention also provides titanium-based composite powder with a core-shell structure, which is prepared by adopting any one of the preparation methods.
Experiments prove that the titanium-based composite powder provided by the embodiment of the invention has a core-shell structure, and in an electron microscope image, nano TiB reinforcing phase whiskers can be observed to be uniformly coated outside titanium metal particles, wherein the transverse size of the TiB reinforcing phase whiskers is nano, the major diameter is large, and the sphericity of the titanium-based composite powder is high.
According to some preferred embodiments, the volume fraction of reinforcing phase in the titanium-based composite material is 1 to 10 vol.%.
In the present invention, if a graphite powder and a titanium metal powder are used to prepare a titanium matrix composite powder, a TiC reinforced titanium matrix composite powder having a volume fraction of a reinforcing phase of 1 to 5 vol.% (for example, 1 vol.%, 2 vol.%, 3 vol.%, 4 vol.%, or 5 vol.%) can be obtained, wherein the titanium metal powder has a mass fraction of 99 to 99.8 wt.% (for example, 99 wt.%, 99.1 wt.%, 99.2 wt.%, 99.3 wt.%, 99.4 wt.%, 99.5 wt.%, 99.6 wt.%, 99.7 wt.%, or 99.8 wt.%), and the graphite powder has a mass fraction of 0.2 to 1 wt.% (for example, 0.2 wt.%, 0.3 wt.%, 0.4 wt.%, 0.5 wt.%, 0.6 wt.%, 0.7 wt.%, 0.8 wt.%, 0.9 wt.%, or 1 wt.%);
if TiB is adopted2The powder and the titanium metal powder can be used for preparing the TiB reinforced titanium-based composite powder with the volume fraction of the reinforcing phase being 1-10 vol.% (for example, 1 vol.%, 2 vol.%, 3 vol.%, 4 vol.%, 5 vol.%, 6 vol.%, 7 vol.%, 8 vol.%, 9 vol.% or 10 vol.%), wherein the mass fraction of the titanium metal powder is 94-99.5 wt.% (for example, 94 wt.%, 95 wt.%, 96 wt.%, 97 wt.%, 98 wt.%, 99 wt.% or 99.5 wt.%), and TiB is2A mass fraction of the powder of 0.5 to 7 wt.% (e.g., can be 0.5 wt.%, 1 wt.%, 2 wt.%, 3 wt.%, 4 wt.%, 5 wt.%, or 6 wt.%);
if B is adopted4C powder and titanium metal powder, the volume fraction of the reinforcing phase is 1-5 vol% (for example, 1 vol.%, 2 vol.%, 3 vol.%, 4 vol.% or 5 vol.%) of TiB + TiC reinforced titanium-based composite powder can be obtained, wherein the mass fraction of the titanium metal powder is 99-99.8 wt.% (for example, 99 wt.%, 99.1 wt.%, 99.2 wt.%, 99.3 wt.%, 99.4 wt.%, 99.5 wt.%, 99.6 wt.%, 99.7 wt.% or 99.8 wt.%), and B powder is 99-99.8 wt.% (or 99.1 wt.%), and4the mass fraction of the C powder is 0.2 to 1 wt.% (e.g., may be 0.2 wt.%, 0.3 wt.%, 0.4 wt.%, 0.5 wt.%, 0.6 wt.%, 0.7 wt.%, 0.8 wt.%, 0.9 wt.%, or 1 wt.%).
The embodiment of the invention also provides application of the titanium-based composite powder with the core-shell structure, wherein the titanium-based composite powder is the titanium-based composite powder, and the titanium-based composite powder is applied to manufacturing of a titanium-based composite material by adopting an additive manufacturing technology.
It should be noted that additive manufacturing techniques include, but are not limited to, laser additive, electron beam additive, arc additive, cold thermal spray, and the like.
In the invention, the titanium-based composite powder with the core-shell structure can be applied to the additive manufacturing of the titanium-based composite material, so that the prepared titanium-based composite material has a compact microstructure and good mechanical properties.
In order to more clearly illustrate the technical solution and advantages of the present invention, a titanium-based composite powder with a core-shell structure and a method for preparing the same are described in detail below by way of several examples.
Example 1
100 μm of TA15 titanium alloy powder and 4 μm of TiB2Performing ball milling treatment on the powder for 5 hours in an argon atmosphere, wherein the mass fraction of TA15 titanium alloy powder is 95 wt.%, and TiB2The mass fraction of the powder is 4 wt.%, the rotation speed of ball milling treatment is 200r/min, the ball-to-material ratio is 4:1, and the mixture is obtained after standing for 6 hours in argon atmosphere;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 900 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1h under the environment to obtain the TiB reinforced titanium-based composite powder with the core-shell structure and the volume fraction of the reinforced phase of 6.8 vol.%.
Example 2
50 μm of TC4 titanium alloy powder and 0.5 μm of TiB2Performing ball milling treatment on the powder for 3 hours in an argon atmosphere, wherein the mass fraction of TC4 titanium alloy powder is 93 wt.%, and TiB2The mass fraction of the powder is 6 wt.%, the rotation speed of ball milling treatment is 150r/min, the ball-to-material ratio is 2:1, and the mixture is obtained after standing for 5 hours in argon atmosphere;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 1000 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1.5h to obtain the TiB reinforced titanium-based composite powder with a core-shell structure and a reinforced phase volume fraction of 10 vol.%.
Example 3
200 μm of pure titanium powder and 5 μm of TiB2Performing ball milling treatment on the powder for 6 hours in an argon atmosphere, wherein the mass fraction of the pure titanium powder is 99.5 wt.%, and the TiB powder is2The mass fraction of the powder is 0.6 wt.%, the rotation speed of the ball milling treatment is 250r/min, the ball-material ratio is 6:1,standing for 6 hours in an argon atmosphere to obtain a mixture;
the mixture was brought to a vacuum of 1X 10-2Heating the mixture to 800 deg.C;
continuously in a vacuum degree of 1 × 10-2The temperature is kept for 0.5h under the environment of (1), and TiB reinforced titanium-based composite powder with a core-shell structure and a reinforced phase volume fraction of 1 vol.% is obtained.
Example 4
Performing ball milling treatment on 100-micron TA15 titanium alloy powder and 3-micron graphite powder in an argon atmosphere for 5 hours, wherein the mass fraction of the TA15 titanium alloy powder is 99 wt.%, the mass fraction of the graphite powder is 1 wt.%, the rotating speed of the ball milling treatment is 200r/min, the ball-to-material ratio is 4:1, and standing in the argon atmosphere for 6 hours to obtain a mixture;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 900 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1h under the environment to obtain the TiC reinforced titanium-based composite powder with a core-shell structure and the volume fraction of a reinforced phase of 5 vol.%.
Example 5
Performing ball milling treatment on 100-micron TA15 titanium alloy powder and 4-micron graphite powder in an argon atmosphere for 5 hours, wherein the mass fraction of the TA15 titanium alloy powder is 99.8 wt.%, the mass fraction of the graphite powder is 0.2 wt.%, the rotating speed of the ball milling treatment is 200r/min, the ball-to-material ratio is 4:1, and standing in the argon atmosphere for 6 hours to obtain a mixture;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 800 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1h under the environment to obtain the TiC reinforced titanium-based composite powder with a core-shell structure and the volume fraction of a reinforced phase of 1 vol.%.
Example 6
100 μm of TA15 titanium alloy powder and 4 μm of B4C, performing ball milling treatment on the powder for 5 hours in argon atmosphere, wherein TA15 titanium alloy powderIs 99 wt.%, B4The mass fraction of the C powder is 1 wt.%, the rotation speed of ball milling treatment is 200r/min, the ball-to-material ratio is 4:1, and a mixture is obtained after standing for 6 hours in an argon atmosphere;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 1000 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1h under the environment to obtain the TiB + TiC reinforced titanium-based composite powder with the core-shell structure and the volume fraction of the reinforced phase of 5 vol.%.
Example 7
100 μm of TA15 titanium alloy powder and 4 μm of B4Performing ball milling treatment on the powder C for 5 hours in an argon atmosphere, wherein the mass fraction of TA15 titanium alloy powder is 99.8 wt.%, and the mass fraction of B is4The mass fraction of the C powder is 0.2 wt.%, the rotation speed of ball milling treatment is 200r/min, the ball-to-material ratio is 4:1, and a mixture is obtained after standing for 6 hours in an argon atmosphere;
the mixture was brought to a vacuum of 1X 10-3Heating the mixture to 900 deg.C;
continuously in a vacuum degree of 1 × 10-3The temperature is kept for 1h under the environment to obtain TiB + TiC reinforced titanium-based composite powder with a core-shell structure and the volume fraction of a reinforced phase of 1 vol.%.
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 preparation method of titanium-based composite powder with a core-shell structure is characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing spherical titanium metal powder and ceramic powder to obtain a mixture, wherein the particle size of the ceramic powder is smaller than that of the titanium metal powder;
step two: carrying out vacuum heating treatment on the mixture to raise the temperature of the mixture to a preset temperature, wherein the preset temperature is the temperature at which the titanium metal powder and the ceramic undergo in-situ self-generation reaction;
step three: and carrying out heat preservation treatment on the mixture at the preset temperature to obtain the titanium-based composite powder with the core-shell structure.
2. The method of claim 1, wherein in the first step, the titanium metal powder is pure titanium powder, TC4 titanium alloy powder or TA15 titanium alloy powder, and the ceramic powder is graphite powder, TiB2Powder or B4And C, powder.
3. The method according to claim 1, wherein in the first step, the titanium metal powder has a particle size of 50 to 200 μm, and the ceramic powder has a particle size of 0.5 to 8 μm.
4. The method according to claim 1, wherein the step one comprises:
performing ball milling treatment on the titanium metal powder and the ceramic powder in an argon atmosphere for 3-6 hours, wherein the rotating speed of the ball milling treatment is 150-250r/min, and the ball-to-material ratio is (2-6): 1; preferably, the ball milling tank and the milling balls of the ball milling treatment are both made of hard alloy.
5. The preparation method according to claim 4, wherein in the first step, after the ball milling treatment, the obtained mixture is subjected to a standing treatment in an argon atmosphere, and the standing treatment time is more than 5 hours.
6. The production method according to claim 1, wherein, in the second step, the heat treatment is performed in a vacuum atmosphere, and the vacuum atmosphere isVacuum degree of (1X 10)-3～1×10-2Pa, and the preset temperature is 700-1100 ℃.
7. The method according to claim 1, wherein the heat-retaining treatment is performed in step three under a vacuum atmosphere having a degree of vacuum of 1X 10-3～1×10-2Pa, and the treatment time of the heat preservation treatment is 0.5-2 h.
8. Titanium-based composite powder of core-shell structure, characterized in that it is obtained by the process according to any one of claims 1 to 7.
9. The titanium-based composite powder according to claim 8, wherein the volume fraction of the reinforcing phase in the titanium-based composite material is 1 to 10 vol.%.
10. Use of a titanium-based composite powder prepared according to the preparation method of any one of claims 1 to 7 or of claim 8 for the preparation of a titanium-based composite material using additive manufacturing techniques.
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