CN113699426A - Titanium-based composite material and preparation method thereof - Google Patents
Titanium-based composite material and preparation method thereof Download PDFInfo
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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
- C22C32/0047—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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- 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
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- 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
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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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- 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
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- 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
Abstract
The invention relates to a titanium-based composite material and a preparation method thereof, wherein the titanium-based composite material comprises a substrate and a reinforcement body, wherein the substrate is a titanium alloy, and the titanium-based composite material is characterized in that: the reinforcement is Ti5Si3And TiB, wherein the volume fraction of the reinforcing body is 5-12 vol%, and the balance is the matrix. The preparation method comprises the following steps: firstly, carrying out ball milling and mixing on titanium alloy powder, silicon powder and titanium diboride powder; secondly, the mixed powder is filled into a stainless steel sheath, the inside of the sheath is filled and compact, and after degassing, vacuumizing and sealing, cold-hot composite rotary swaging is carried out to compactMelting; thirdly, sintering the rotary-swaged bar; and finally, processing and removing the sheath to obtain the titanium-based composite material. The invention has the advantages that: the titanium-based composite material has the advantages of excellent mechanical property, controllable oxygen content in the preparation process, short flow of the preparation method, low cost and energy consumption and good industrial application prospect.
Description
Technical Field
The invention belongs to the field of metal matrix composite materials, and particularly relates to a titanium matrix composite material and a preparation method thereof.
Background
Titanium-based composites (TMC) are composites of titanium or titanium alloy substrates incorporating high modulus, high strength, high hardness and good high temperature performance reinforcement which combine the high plasticity of the substrate with the high strength, high modulus of the reinforcement to provide superior performance to titanium alloys. The titanium-based composite materials are mainly classified into continuous fiber reinforced titanium-based composite materials and particle/short fiber reinforced titanium-based composite materials according to the form of reinforcement. The particle/short fiber reinforced titanium-based composite material has the characteristics of isotropy, simple preparation process, lower cost and the like, and is widely concerned by researchers.
The powder metallurgy method based on the in-situ autogenous technology becomes an important method for controllable preparation of the high-performance titanium-based composite material due to the advantages of good compatibility of a matrix and a reinforcement, high interface bonding strength, high material design freedom and the like. At present, the preparation process approaches mainly comprise: 1. ball milling → pressing of composite powder into a blank (cold pressing, isostatic pressing or hot pressing) → densification sintering (hot pressing sintering, spark plasma sintering, microwave sintering) → finished product. For example, the Chinese invention patent "a method for preparing a titanium-based composite material containing titanium-silicon intermetallic compound and silicon carbide particles", which has patent number ZL201911399358.5 and publication number (CN111020291B), discloses a preparation method comprising: 1) mixing Ti3SiC2Ball milling the powder to obtain uniform Ti3SiC2Powder; 2) mixing titanium alloy powder with uniform Ti3SiC2Continuously carrying out ball milling on the powder uniformly to obtain mixed powder; 3) drying and screening the mixed powder to obtain dry powder; 4) benefit toSintering and molding the dry powder obtained in the step 3) by using a hot-pressing sintering system to obtain the Ti-containing powder5Si3And TiC particles. In the approach, after the composite powder is sintered by hot pressing, small holes which are not closed still exist in a sintering blank, and the density of the material is difficult to reach more than 98%; the other preparation process is that ball milling → mixed powder cold isostatic pressing → vacuum sintering → vacuum heat treatment → hot forming (forging, rotary forging, extrusion) → annealing → finished product. In addition, the spherical titanium powder has a problem that cold isostatic pressing is not easy to mold. The second approach has the problems of long flow in the preparation process, strict requirements on equipment conditions, easy oxidation in the hot processing process and the like.
For another example, the Chinese invention patent, a method for preparing a TiB nano-reinforced titanium-based composite material, has patent number ZL201810684391.1 and publication number (CN108796265B), discloses a method for preparing a TiB nano-reinforced titanium-based composite material, and the titanium-based composite material is prepared by ball milling, spark plasma sintering and hot rolling. By ball milling of nano TiB2Powder and titanium powder, or nano TiB2Preparing original powder from the powder and titanium alloy powder; controlling TiB at lower sintering temperature and high pressure2Preparing high-density sintered blocks on the premise that the particles and the surrounding titanium or titanium alloy matrix do not react in situ; finally, TiB in the sintered body is hot rolled2The particles and the surrounding titanium or titanium alloy matrix are subjected to in-situ reaction to form whiskers, and meanwhile, matrix grains are deformed, so that the strength and the plasticity of the composite material are improved. However, the sintered block prepared by the method is limited in size, difficult to prepare blanks of large-size components and relatively limited in application range; in addition, the preparation process is longer, the energy consumption is higher, and the requirement on equipment conditions is higher. And the titanium-based composite material prepared by the method can not meet the strong plasticity requirements of tensile strength of more than 1000MPa and elongation of more than 5 percent at the same time.
Therefore, further improvements in the preparation of titanium-based composites are needed.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide a titanium-based composite material having both high tensile strength and elongation against the current situation of the prior art.
The second technical problem to be solved by the invention is to provide a preparation method of the titanium-based composite material with controllable oxygen content, short flow and high generalization degree.
The technical scheme adopted by the invention for solving the first technical problem is as follows: a titanium-based composite material comprises a substrate and a reinforcement, wherein the substrate is a titanium alloy, and the titanium-based composite material is characterized in that: the reinforcement is Ti5Si3And TiB, wherein the volume fraction of the reinforcing body is 5-12 vol%, and the balance is the matrix.
The content of the components of the titanium alloy is preferably: the titanium alloy comprises the following components in percentage by mass: 5.5% -7.3%, molybdenum: 3.0% -4.0%, silicon: 0.15% -0.35%, zirconium: 1.0 to 2.0 percent of titanium element and the balance. The titanium alloy with the components is an alpha + beta type dual-phase titanium alloy, and has excellent strength, good plasticity, good formability and heat resistance.
The technical scheme adopted by the invention for solving the second technical problem is as follows: the preparation method of the titanium-based composite material is characterized by sequentially comprising the following steps of:
1) ball-milling and mixing titanium alloy powder, silicon powder and titanium diboride powder to obtain mixed powder;
2) putting the mixed powder obtained in the step 1) into a sheath, applying a pressure of 30-50 MPa to ensure that the powder is solid and tight in the sheath, degassing, vacuumizing, sealing and welding, and performing cold-hot composite rotary forging densification to obtain a bar stock;
3) sintering the rotary-forged bar stock obtained in the step 2) to obtain in-situ authigenic Ti5Si3Sintering the blank with a TiB reinforced titanium-based composite material;
4) processing the sintered blank obtained in the step 3) to remove the sheath, and obtaining the titanium-based composite material.
Preferably, in the step 1), the average grain diameter of the titanium alloy powder is 100-200 μm, and the grain diameters of the silicon powder and the titanium diboride powder are both 1-3 μm. Wherein, the titanium-based composite material prepared by adopting large-size (100-200 mu m) titanium alloy powder has the advantages that: on one hand, the spherical large-size titanium alloy powder is usually derived from 3D printing residual powder, so that the cost is low; on the other hand, the large-size titanium alloy powder can improve the plasticity of the titanium-based composite material by adopting a proper ball milling process.
In the step 1), ball milling and mixing are carried out under the protection of argon atmosphere, the ball milling rotating speed is 100-200 r/min, and the ball milling time is 3-8 h. Under the low-energy ball milling process, small-size silicon and titanium diboride powder can be uniformly embedded on the surface of a large-size titanium alloy, and the method is a key technical link for regulating and controlling the organization structure of the high-strength plastic titanium-based composite material.
Specifically, in step 2), the cold-hot combined swaging densification is: performing rotary swaging on the sheath filled with the powder at room temperature according to the machining rate of 0.5-5 mm per pass, so that the density of the powder reaches over 95%; and then, performing hot rotary swaging on the sheath filled with the powder at the temperature of 500-800 ℃ according to the machining rate of 0.2-1 mm per pass, so that the density of the powder reaches more than 99%. The cold and hot compound rotary swaging technology has the advantages that: the mixed powder is compacted by cold rotary swaging, and the density reaches over 95 percent; furthermore, metallurgical reaction occurs between the mixed powder through hot rotary swaging, the interface bonding effect is strengthened, and the density is up to more than 99%. The method can save energy consumption and is an important technical link for preparing the high-density titanium-based composite material.
Preferably, in the step 3), the heating temperature for sintering is 1100-1300 ℃, and the heat preservation time is 1-2 h. Thus, Ti and Si, Ti and TiB are added under the temperature and the holding time2In-situ autogenous reaction is carried out to obtain in-situ autogenous Ti5Si3And TiB reinforced titanium-based composite material.
Preferably, the jacket is a stainless steel jacket. In addition, steel jackets may also be employed.
Compared with the prior art, the invention has the advantages that: the matrix titanium alloy in the titanium-based composite material has higher mechanical property and heat resistance, and the reinforcement bodies Ti5Si3 and TiB have the advantages of high strength, high modulus, high temperature resistance, wear resistance and the like, and are reinforcedThe volume fraction of the body is 5 vol.% to 12 vol.%, and the equiaxed and micron-sized TiC particles are distributed around the titanium alloy matrix, so that the material is low in plasticity and high in brittleness. The micron whisker-shaped TiB adopted by the invention is distributed around the titanium alloy matrix and grows into the titanium alloy matrix, so that the effect of strengthening and toughening is achieved, and the plasticity of the material is higher. Based on a titanium alloy matrix with large size, strong plasticity and excellent heat resistance, and high-strength, high-modulus and nano-scale fine needle-like Ti5Si3And a material system of a micron-sized whisker-shaped TiB reinforcing phase, under the preparation method of the invention, a multi-scale heterogeneous reinforced titanium-based composite material microstructure characteristic is constructed, so that the titanium-based composite material has high tensile strength and high elongation. The preparation method adopts a short-flow preparation process of ball milling, cold and hot combined rotary swaging and sintering, and the powder is filled into a stainless steel ladle sleeve for cold and hot combined rotary swaging and sintering, so that the oxygen content in the whole process is controllable, the material oxidation is effectively avoided, the requirements on equipment conditions are low, the cost is low, the generalization degree is high, and the preparation method has a wide industrial application prospect.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a titanium matrix composite material according to an embodiment of the present invention
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1:
the Ti-based composite material of the embodiment comprises a substrate and a reinforcement, wherein the substrate is a Ti alloy, and the reinforcement is Ti5Si3And TiB, and the volume fractions are 2 vol.% and 5 vol.%, respectively. Thus, the reinforcement of this example has a volume fraction of 7 vol.% with the balance being the matrix. The titanium alloy comprises the following components in percentage by mass: 6.5%, molybdenum: 3.5%, silicon: 0.25%, zirconium: 1.43 percent and the balance of titanium element.
As shown in FIG. 1, the preparation method of the titanium-based composite material of the embodiment sequentially comprises the following steps:
1) according to the designed components of the composite material, ball-milling and mixing spherical titanium alloy powder with the average particle size of 150 microns, silicon powder and titanium diboride powder with the particle sizes of 1 micron under the argon protection atmosphere at the ball-milling rotating speed of 200r/min for 4h to obtain mixed powder;
2) filling the mixed powder obtained in the step 1) into a stainless steel sheath, applying 50MPa pressure to ensure that the powder is filled and compacted in the sheath, degassing, vacuumizing, sealing and welding, and performing cold-hot composite rotary swaging densification to obtain a bar. The cold and hot combined swaging densification means: at room temperature, performing rotary swaging on the sheath filled with the powder according to the machining rate of 5mm per pass for 4-10 passes to ensure that the density of the sheath is over 95 percent; then, carrying out hot rotary swaging on the sheath filled with the powder at the temperature of 500 ℃ according to the machining rate of 0.5mm per pass, and carrying out rotary swaging for 3-10 passes to enable the density of the sheath to reach more than 99%;
3) sintering the rotary-forged bar stock obtained in the step 2), wherein the heating temperature during sintering is 1200 ℃, the heat preservation time is 1.5h, and in the process, Ti and Si, Ti and TiB2In-situ autogenous reaction is carried out to obtain in-situ autogenous Ti5Si3Sintering the blank with a TiB reinforced titanium-based composite material;
4) and 3) processing the sintered blank obtained in the step 3) to remove the stainless steel sheath, thus obtaining the titanium-based composite material.
The tensile strength of the titanium-based composite material of the embodiment is 1110MPa and the elongation is 5% by adopting a room-temperature tensile property test. Hardness test the hardness of the titanium matrix composite of this example was 46 HRC. The density of the titanium-based composite material of the embodiment is 99.1%.
Example 2:
this embodiment differs from embodiment 1 described above only in that:
1. the reinforcement content is different, in particular, Ti in the reinforcement5Si3And TiB of 4 vol.% and 3.5 vol.%, respectively, the reinforcement has a volume fraction of 7.5 vol.%.
2. The preparation method of the titanium-based composite material has different process parameters, and specifically comprises the following steps:
in the step 1), the average grain diameter of the spherical titanium alloy powder is 100 microns, the grain diameters of the silicon powder and the titanium diboride powder are both 3 microns, the ball milling speed is 150r/min, and the ball milling time is 6 hours; in the step 2), in the cold-hot composite rotary swaging densification, the sheath filled with the powder is subjected to rotary swaging at room temperature according to the machining rate of 4mm per pass, so that the compactness of the sheath reaches over 95 percent; then, carrying out hot rotary swaging on the sheath filled with the powder at the temperature of 600 ℃ according to the processing rate of 0.3mm per pass, so that the density of the sheath reaches more than 99%;
in the step 3), the heating temperature of sintering is 1300 ℃, and the temperature is kept for 1.0 h.
The tensile strength of the titanium-based composite material of the embodiment is 1200MPa and the elongation rate is 6 percent by adopting a room temperature tensile property test. The hardness of the titanium matrix composite of this example was measured to be 47 HRC. The density of the titanium-based composite material of the embodiment is 99.1%.
Example 3:
this embodiment differs from embodiment 1 described above only in that:
1. the reinforcement content is different, in particular, Ti in the reinforcement5Si3And TiB are 2 vol.% and 3 vol.%, respectively, the reinforcement has a volume fraction of 5 vol.%.
The titanium alloy has different component contents, and specifically, the titanium alloy comprises the following components in percentage by mass: 5.5%, molybdenum: 4.0%, silicon: 0.15%, zirconium: 2.0 percent and the balance of titanium element.
2. The preparation method of the titanium-based composite material has different process parameters, and specifically comprises the following steps:
in the step 1), the average grain diameter of the spherical titanium alloy powder is 180 microns, the grain diameters of the silicon powder and the titanium diboride powder are both 2.5 microns, the ball milling speed is 100r/min, and the ball milling time is 3 hours;
in the step 2), the applied pressure is 40MPa, and in cold-hot composite rotary swaging densification, the sheath filled with the powder is subjected to rotary swaging at room temperature according to the machining rate of 0.5mm per pass, so that the density of the sheath is over 95 percent; then, carrying out hot rotary swaging on the sheath filled with the powder at the temperature of 700 ℃ according to the processing rate of 0.2mm per pass, so that the density of the sheath reaches more than 99%;
in the step 3), the heating temperature of sintering is 1100 ℃, and the temperature is kept for 2.0 h.
The tensile strength of the titanium-based composite material of the embodiment is 1150MPa and the elongation rate is 5 percent by adopting a room temperature tensile property test. Hardness test the hardness of the titanium matrix composite of this example was 46 HRC. The density of the titanium-based composite material of the embodiment is 99.2%.
Example 4:
this embodiment differs from embodiment 1 described above only in that:
1. the reinforcement content is different, in particular, Ti in the reinforcement5Si3And TiB are 5 vol.% and 7 vol.%, respectively, the reinforcement has a volume fraction of 12 vol.%.
The titanium alloy has different component contents, and specifically, the titanium alloy comprises the following components in percentage by mass: 7.3%, molybdenum: 3.0%, silicon: 0.35%, zirconium: 1.0 percent and the balance of titanium element.
2. The preparation method of the titanium-based composite material has different process parameters, and specifically comprises the following steps:
in the step 1), the average grain diameter of the spherical titanium alloy powder is 200 microns, the grain diameters of the silicon powder and the titanium diboride powder are both 2 microns, the ball milling speed is 120r/min, and the ball milling time is 5 hours;
in the step 2), the applied pressure is 45MPa, and in cold-hot composite rotary swaging densification, the sheath filled with the powder is subjected to rotary swaging at room temperature according to the processing rate of 2mm per pass, so that the density of the sheath is over 95 percent; then, carrying out hot rotary swaging on the sheath filled with the powder at the temperature of 800 ℃ according to the processing rate of 1mm per pass, so that the density of the sheath reaches more than 99%;
in the step 3), the heating temperature of sintering is 1150 ℃, and the temperature is kept for 1.5 h.
The tensile strength of the titanium-based composite material of the embodiment is 1250MPa and the elongation rate is 6 percent by adopting a room temperature tensile property test. The hardness of the titanium matrix composite of this example was measured to be 48 HRC. The density of the titanium-based composite material of the embodiment is 99.1%.
Claims (8)
1. A titanium-based composite material comprises a substrate and a reinforcement, wherein the substrate is a titanium alloy, and the titanium-based composite material is characterized in that: the reinforcement is Ti5Si3And TiB, wherein the volume fraction of the reinforcing body is 5-12 vol%, and the balance is the matrix.
2. The titanium-based composite material according to claim 1, wherein: the titanium alloy comprises the following components in percentage by mass: 5.5% -7.3%, molybdenum: 3.0% -4.0%, silicon: 0.15% -0.35%, zirconium: 1.0 to 2.0 percent of titanium element and the balance.
3. A process for the preparation of a titanium-based composite material according to claim 1 or 2, comprising the following steps in sequence:
1) ball-milling and mixing titanium alloy powder, silicon powder and titanium diboride powder to obtain mixed powder;
2) putting the mixed powder obtained in the step 1) into a sheath, applying a pressure of 30-50 MPa to ensure that the powder is solid and tight in the sheath, degassing, vacuumizing, sealing and welding, and performing cold-hot composite rotary forging densification to obtain a bar stock;
3) sintering the rotary-forged bar stock obtained in the step 2) to obtain in-situ authigenic Ti5Si3Sintering the blank with a TiB reinforced titanium-based composite material;
4) processing the sintered blank obtained in the step 3) to remove the sheath, and obtaining the titanium-based composite material.
4. The production method according to claim 3, characterized in that: in the step 1), the average grain diameter of the titanium alloy powder is 100-200 μm, and the grain diameters of the silicon powder and the titanium diboride powder are both 1-3 μm.
5. The method of claim 4, wherein: in the step 1), ball milling and mixing are carried out under the protection of argon atmosphere, the ball milling rotating speed is 100-200 r/min, and the ball milling time is 3-8 h.
6. The production method according to claim 3, characterized in that: in the step 2), the cold-hot composite rotary swaging densification is as follows: performing rotary swaging on the sheath filled with the powder at room temperature according to the machining rate of 0.5-5 mm per pass, so that the density of the powder reaches over 95%; and then, performing hot rotary swaging on the sheath filled with the powder at the temperature of 500-800 ℃ according to the machining rate of 0.2-1 mm per pass, so that the density of the powder reaches more than 99%.
7. The production method according to claim 3, characterized in that: in the step 3), the heating temperature of sintering is 1100-1300 ℃, and the heat preservation time is 1-2 h.
8. The method of claim 1, wherein: the sheath is a stainless steel sheath.
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