CN113061779B - Additive manufacturing method of nanoparticle reinforced titanium-based composite material based on selective electron beam melting - Google Patents

Additive manufacturing method of nanoparticle reinforced titanium-based composite material based on selective electron beam melting Download PDF

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CN113061779B
CN113061779B CN202110287771.3A CN202110287771A CN113061779B CN 113061779 B CN113061779 B CN 113061779B CN 202110287771 A CN202110287771 A CN 202110287771A CN 113061779 B CN113061779 B CN 113061779B
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牛红志
谭浩
殷宝国
张德良
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Northeastern University China
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    • 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
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    • 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
    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
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    • 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
    • B33Y80/00—Products made by additive manufacturing
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    • 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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Abstract

The invention relates to an additive manufacturing method of a nanoparticle reinforced titanium-based composite material based on selective electron beam melting, which comprises S1, manufacturing spherical powder of the titanium-based composite material; s2, screening powder; s3, constructing a digital model; s4, electron beam additive manufacturing; and S5, post-processing. The method directly uses the spherical pre-alloy powder of the titanium-based composite material to perform additive manufacturing of the nano-particle reinforced titanium-based composite material under the conditions of high vacuum and in-situ annealing, and realizes in-situ self-generation and dense three-dimensional net-shaped uniform distribution of a nano-reinforced phase. The density of the nano-particle reinforced titanium-based composite material prepared by the invention is as high as 99.8%, the oxygen content is lower than 0.12 wt%, the volume fraction of the reinforced phase can reach more than 5.0%, and the mechanical property is close to the level of a conventional forging. Therefore, the method provided by the invention is particularly suitable for low-cost manufacture of high-performance nano-particle reinforced titanium matrix composite complex structural parts.

Description

Additive manufacturing method of nanoparticle reinforced titanium-based composite material based on selective electron beam melting
Technical Field
The invention relates to an additive manufacturing method of a nanoparticle reinforced titanium-based composite material based on selective melting of an electron beam, and belongs to the technical field of additive manufacturing of metal-based composite materials.
Background
The particle reinforced titanium-based composite material is a light high-temperature high-strength structural material with great application prospect, and has important strategic position in the fields of aerospace, marine equipment, weapon equipment light weight and the like. However, the titanium-based composite material is difficult to be plastically deformed at high temperature, and has high-temperature activity, so that precision die forging or precision casting forming is difficult. The breakage and directional arrangement of the reinforcing phase whiskers during plastic working weaken the reinforcing effect and deteriorate the plasticity. The particle reinforced titanium-based composite material manufactured by the conventional ingot metallurgy method and the powder metallurgy method is difficult to realize the superfine/nanometer of reinforcing phase particles, and is not beneficial to the improvement of the room temperature plasticity and the strength of the titanium-based composite material.
Laser and electron beam additive manufacturing (3D printing) is a near-net-shape flexible manufacturing technology based on a three-dimensional discrete digital model of a component, and has the outstanding advantages of short process flow, high material utilization rate, high shape freedom, no need of manufacturing a mold and the like. Additive manufacturing has become a key technology for the manufacture of complex parts such as difficult-to-machine/form titanium alloys, titanium-based composites, superalloys, and intermetallic compounds. The additive manufacturing has the characteristics of powder layer-by-layer solidification and accumulation and rapid solidification, and can realize in-situ self-generation, uniform distribution and particle size nanocrystallization of a reinforcing phase in the metal matrix composite. In other words, the additive manufacturing provides a new path for preparing the nano reinforced titanium-based composite material and forming parts with complex geometric shapes, and simultaneously realizes new breakthrough in mechanical properties.
Currently, mainstream laser selective melting additive manufacturing titanium-based composite materials is to perform mechanical ball milling or chemical mixing on alloy matrix spherical powder and reinforcement raw materials to obtain powder raw materials for additive manufacturing. The mixed powder raw material has the defects of poor liquidity, large difference of energy absorption coefficients of a matrix and a reinforcement material, incapability of accurately controlling the content of the reinforcement, uneven distribution of the reinforcement material and the like. These disadvantages result in insufficient melting of the reinforcing phase particles, high particle clustering, oxygen and impurity content, and easily induced holes and cracks during the laser additive manufacturing process. Therefore, the titanium-based composite material manufactured by the laser additive based on the mixed powder raw material has small forming size, and parts with complex geometric shapes are difficult to manufacture; and because holes and cracks generally exist, the titanium-based composite material manufactured by the laser additive has poor room-temperature tensile plasticity and tensile strength.
The laser selective melting additive manufacturing of the titanium-based composite material is carried out by directly using the spherical pre-alloy powder, so that the defects caused by mixed powder raw materials can be avoided, but the defects of low content of the reinforcing phase and small forming size still exist, and the manufacturing of a sample with a complex geometric shape is difficult to realize. The reason is that the titanium-based composite material has high-temperature strength, and the ultrahigh temperature gradient and the ultrahigh cooling speed in a tiny molten pool in the laser additive manufacturing process can easily induce higher residual stress, so that the cracking and buckling deformation of a sample are caused. Therefore, the development of an additive manufacturing technology for complex parts of the nanoparticle reinforced titanium matrix composite is needed.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems that the titanium-based composite material manufactured by laser additive in the prior art has high oxygen and impurity contents, difficult accurate control of the content of a reinforcing phase, difficult realization of high-content reinforcing phase, impermeable clustering and melting of reinforcing phase particles, easy induction of cracking and holes and the like, the invention provides a manufacturing method of a nanoparticle reinforced titanium-based composite material additive based on selective melting of electron beams, which lays a technical foundation for manufacturing complex parts of the high-performance nanoparticle reinforced titanium-based composite material.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a method of additive manufacturing of a nanoparticle reinforced titanium matrix composite based on selective electron beam melting, comprising the steps of:
s1, manufacturing spherical powder of the titanium-based composite material;
s2, screening powder;
s3, constructing a digital model;
s4, electron beam additive manufacturing;
and S5, post-processing.
In the manufacturing method described above, preferably, in step S1, the spherical powder is manufactured by using a plasma rotary electrode method or a crucible-free electrode gas atomization method to manufacture spherical prealloyed powder of titanium-based composite material.
In the manufacturing method as described above, preferably, in step S1, the raw material of the titanium-based composite spherical powder includes an alloy matrix and a reinforcing phase, the alloy matrix is any one of pure titanium, TC4, TA15, Ti6242 or Ti-Al-Sn-Zr-Mo-Si series high temperature titanium alloy, and the reinforcing phase is TiB, TiC, TiN, Ti5Si3Or one or more rare earth oxides; the volume fraction of the reinforcing phase is selected between 0.5% and 8.0%.
Further, the rare earth oxide is La2O3Or Y2O3. The rare earth oxide is preferably used as a reinforcing phase, so that the oxygen content of the alloy matrix can be reduced, and the particle strengthening effect is achieved.
The reinforcing phase is self-generated in situ and uniformly distributed in each spherical powder particle, and the electrode rod for powder preparation is manufactured by using the methods of vacuum casting, high-temperature forging and machining.
In the above production method, in step S2, the screened spherical powder having a particle size of 40 to 140 μm is preferable.
A large number of experiments prove that the powder granularity range of the invention is preferably 40-140 mu m, the oxygen content of the manufactured alloy sample is generally lower, the sample has high density, and the forming quality is best. If the particle size of the powder deviates from the range of 40 to 140 μm, the manufacturing efficiency is reduced, and the fusion-through or interlayer void defects are generated.
In the manufacturing method as described above, preferably, in step S3, the digital model is a three-dimensional digital model of a titanium-based composite material sample with a target shape, which is constructed by using computer drawing software, and then the three-dimensional digital model is subjected to slice discretization processing and exported as a digital model file for direct additive manufacturing.
Further, preferably, the computer drawing software is Proe, UG, Solidworks or Materialise Magics and the like, a three-dimensional digital model of the titanium-based composite material sample with the target shape is constructed, and a support structure is reasonably designed and added. And then, discretizing the constructed three-dimensional digital model by means of slicing software (such as Magics), and finally exporting the three-dimensional digital model as a three-dimensional digital model file which can be directly used for electron beam selective melting additive manufacturing.
In the manufacturing method described above, preferably, in step S4, the parameters of the selective electron beam melting process used in the electron beam additive manufacturing are: the melting current is 6.0-25 mA, the melting scanning speed is 4.0-20 m/s, the preheating current is 20-50 mA, the preheating scanning speed is 15-50 m/s, the layer thickness is 35-90 μm, the channel interval is 60-120 μm, the reciprocating or checkerboard scanning strategy is adopted, and the substrate preheating temperature is 400-1000 ℃. These optimized electron beam selective melting technological parameters are the key to ensure the normal operation of the forming process, raise the compactness of the sample, reduce cracking and ensure the size precision of the sample. The fusion penetration and interlayer hole defects can be caused by small fusion current or too high fusion scanning speed; and the keyhole defect is easily formed because the melting current is too large or the melting scanning speed is too slow. The electron beam preheats the powder layer quickly, fully ensures the stability and firmness of the powder layer laying, and avoids the powder blowing and the powder layer scattering in the electron beam melting process.
It should be noted that before the selective melting of the electron beam, the spherical powder is loaded into the powder bin, the forming chamber is vacuumized to less than or equal to 0.005Pa, and then the substrate is preheated to 400-1000 ℃ by the electron beam.
The substrate is preferably preheated to 400-1000 ℃ in order to significantly reduce the thermal stress during the forming process and prevent the cracking and deformation of the sample. Without preheating the substrate in advance, cracking and deformation of the titanium-based composite material sample manufactured by the electron beam additive manufacturing can be caused. In the manufacturing method, in step S4, the vacuum degree of the forming chamber is preferably maintained at 0.01Pa or less, or the forming chamber is preferably maintained at 0.10 to 1.0Pa of flowing helium gas during the electron beam additive manufacturing process.
The forming chamber preferably adopts flowing helium with the pressure less than or equal to 1.0Pa, so that the phenomena of gasification of alloy liquid and powder blowing of a powder bed can be effectively inhibited.
In the selective melting process of the electron beams, the powder spreading thickness is equal to the slice thickness of the digital model in the step III, and when one layer of powder is spread, a large-current electron beam is used for quickly preheating a powder layer, and then a small-current electron beam is used for carrying out contour scanning and selective melting, and the process is carried out in a circulating mode until the forming is finished.
In the manufacturing method as described above, preferably, in step S5, the post-treatment is that the titanium-based composite material sample manufactured in step S4 is taken out from the powder bed, separated from the substrate, and subjected to powder cleaning, stent cutting, surface blasting, and heat treatment.
And after the post-treatment is finished, obtaining the nano particle reinforced titanium-based composite material sample or part manufactured by electron beam additive manufacturing.
(III) advantageous effects
The invention has the beneficial effects that:
(1) the nano particle reinforced titanium-based composite material additive manufacturing method based on electron beam selective melting provided by the invention is formed by high-energy electron beam selective melting under a high vacuum condition, and the manufactured nano particle reinforced titanium-based composite material has high purity, the oxygen content is usually less than or equal to 0.10 wt%, and the density is more than or equal to 99.5%.
(2) The method provided by the invention adopts high-temperature preheating of the substrate and rapid scanning of the electron beam to preheat the powder bed, realizes in-situ stress relief annealing and homogenization of the forming tissue, effectively avoids cracking, warping and layering of a sample in the manufacturing process, and is particularly suitable for manufacturing high-volume-fraction particle reinforced titanium-based composite material parts with complex geometric shapes.
(3) In the selective melting process of the high-energy electron beams, the nanometer reinforcing phase is subjected to rapid dissolution and in-situ regeneration, and is uniformly distributed in three dimensions in a titanium-based composite material sample. In particular, the nano-rod/flake TiB and the nano-spherical rare earth oxide (such as Y) which are in situ synthesized in the liquid phase region and the solid-liquid two-phase region2O3、La2O3) The nano TiN, TiC and the like are distributed in a dense three-dimensional net shape, and the unit grid size is less than or equal to 2 mu m; and eutectoid type compounds, e.g. Ti5Si3And may be randomly distributed in the alloy matrix.
(4) The method provided by the invention has outstanding advantages of room-temperature and high-temperature mechanical properties. The room temperature tensile plasticity is higher than that of the precision casting titanium-based composite material, and the tensile strength between room temperature and 700 ℃ reaches the level equivalent to that of the conventional forging titanium-based composite material.
The method of the invention is an ideal means for manufacturing high-quality nano-particle reinforced titanium-based composite materials, in particular to titanium-based composite material parts with complex geometric shapes.
Drawings
FIG. 1 is a titanium matrix composite sample block and a complex impeller sample piece manufactured additively;
FIG. 2 is a 5.5% enhanced phase volume fraction of (TiB + Y) made in accordance with the present invention2O3+Ti5Si3) The microstructure and the reinforcing phase morphology of the/Ti-6 Al-3Sn-4Zr-0.9Mo titanium-based composite material;
FIG. 3 is a graph of room temperature and high temperature tensile properties of a nanoparticle reinforced titanium matrix composite;
FIG. 4 is a graph of tensile properties of a nanoparticle-reinforced titanium-based composite material after a solution & age heat treatment.
Detailed Description
The manufacturing method provided by the invention takes spherical pre-alloy powder of the titanium-based composite material as a raw material, and adopts an electron beam selective melting technology under the conditions of high vacuum and in-situ stress relief annealing to realize the additive manufacturing of the high-quality nano reinforced titanium-based composite material. The reinforcing phase nano particles are self-generated in situ and directly and uniformly distributed in the spherical powder particles, so that the high volume fraction reinforcing phase content and the precise control of the reinforcing phase content are realized. The titanium-based composite material spherical powder is directly used, and is matched with a vacuum environment in an electron beam additive manufacturing process, so that the pollution of oxygen and impurities is obviously reduced, the uniform distribution of reinforcing phase particles in a formed sample is realized, and the defects of reinforcing phase particle clusters and fusion impermeability are avoided; the substrate high-temperature preheating and the electron beam rapid preheating powder layer have the in-situ stress relief annealing effect, and the cracking and deformation of a formed sample are avoided. The invention provides a nano particle reinforced titanium-based composite material additive manufacturing method based on selective electron beam melting, which mainly comprises the following processesThe method comprises the following steps: manufacturing spherical powder; sieving the powder; constructing a digital model; electron beam additive manufacturing; fifthly, post-treatment. The alloy matrix of the titanium-based composite material can be any one of the titanium alloys reported in the present disclosure, and the reinforcement can be selected from in-situ self-generated TiB, TiC, TiN and Ti5Si3Rare earth oxides (e.g. Y)2O3、La2O3) And the like.
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
Example 1
This example provides a volume fraction of reinforcing phase of 5.5% (TiB + Y) for a nano-multiphase particle reinforced high temperature titanium-based composite material2O3+Ti5Si3) Additive manufacturing method of/Ti-6 Al-3Sn-4Zr-0.9 Mo. The in-situ self-generated high-temperature titanium-based composite material comprises the following corresponding chemical elements in percentage by mass: ti-6Al-3Sn-4Zr-0.9Mo-0.3Si-0.4Y-0.6B, namely 6 percent of Al, 3 percent of Sn, 4 percent of Zr, 0.9 percent of Mo, 0.3 percent of Si, 0.4 percent of Y, 0.6 percent of B and the balance of Ti in mass ratio. The nanoreinforcement phase comprises 3.4% TiB and 0.95% Y in situ2O3And about 1.2% Ti5Si3。
First, the spherical powder is produced in the step (1). Firstly, preparing raw materials according to the element mass ratio of Ti-based composite material Ti-6Al-3Sn-4Zr-0.9Mo-0.3Si-0.4Y-0.6B, and manufacturing a standard electrode rod for powder preparation by means of conventional vacuum casting, high-temperature forging and machining process flows. Spherical powder was produced by using the processed titanium-based composite electrode rod by a Plasma Rotary Electrode Process (PREP). The technological parameters of the powder preparation by the PREP method are as follows: voltage 60V, current 1800A, electrode bar
Figure BDA0002981191920000071
The rotating speed of the electrode bar is 19000r/min, the feeding speed is 0.8mm/s, and the pressure of the argon atmosphere is 0.085 MPa.
Then, the process step of sieving the powder is carried out. And (3) screening the spherical powder manufactured in the process step I, and screening the spherical powder with the granularity range of 30-140 mu m for electron beam additive manufacturing of the nano-particle reinforced titanium-based composite material.
And then, finishing the process step and constructing the digital model. And constructing a three-dimensional digital model of the titanium-based composite material sample with the target shape by means of computer three-dimensional drawing software UG, and reasonably designing and adding a support structure. And then, discretizing the constructed three-dimensional digital model by means of slicing software Magics, and exporting the three-dimensional digital model as a three-dimensional digital model file which can be directly used for selective melting additive manufacturing of the electron beam.
And (4) carrying out electron beam selective melting additive manufacturing on the titanium-based composite material by using the spherical powder screened in the step (c) and the three-dimensional digital model constructed in the step (c). Sequentially mounting Ti-6Al-4V titanium alloy substrates, filling spherical powder into a forming bin, and pumping the vacuum degree of the forming bin to 1.0 multiplied by 10-3Pa, electron beam heating the substrate to 730 ℃. Then, electron beam selective melting forming of the titanium-based composite material is carried out. And (3) preheating the powder layer by rapidly scanning the powder layer for 1-3 times by using an electron beam for each layer of powder, then carrying out contour scanning and selective melting by using a slow electron beam, and circulating the steps until the forming is finished. The adopted electron beam selective melting process parameters are as follows: 18mA of melting current, 6m/s of melting scanning speed, 35mA of preheating current, 20m/s of preheating scanning speed, 50 μm of layer thickness, 100 μm of pass interval and a reciprocating scanning strategy. In the selective melting and forming process of the electron beams, helium flow of 0.15Pa in a forming chamber is always kept;
finally, finishing the post-treatment in the process step (v). And (4) taking the titanium-based composite material rectangular block and the turbine sample piece which are manufactured by the electron beam additive manufacturing from the powder bed, removing the base plate, cutting the bracket, and performing surface sand blasting treatment. After the post-treatment works are completed, the electron beam additive manufacturing nano particle reinforced titanium-based composite material rectangular block and the turbine sample piece are obtained, as shown in figure 1. The volume fraction of reinforcing phase produced in this example was 5.5% (TiB + Y)2O3+Ti5Si3) Samples of/Ti-6 Al-3Sn-4Zr-0.9Mo nanoreinforced titanium matrix composites and turbine componentsThe oxygen content is only 0.095 wt%, and the density reaches 99.6%. The reinforced phase presents typical dense three-dimensional network uniform distribution, and the in-situ self-generated reinforced phase comprises nano needle-shaped TiB and nano particle Y2O3And Ti5Si3. FIG. 2 shows the distribution and morphology of the Ti-based composite material particle-reinforced phase observed by scanning electron microscopy, wherein a is the distribution of the particle-reinforced phase on the cross section of the sample, and the particle-reinforced phase under low-power scanning electron microscopy is shown to be densely distributed in a net shape, b is the distribution of the rod-shaped TiB particles and matrix phase on the longitudinal section of the sample observed by high-power scanning electron microscopy, and c is the TiB nanorods and the nanoparticles Y observed by high-power scanning electron microscopy2O3And Ti5Si3The morphology of (2). The average cell size of the reinforcing phase fine network was only 1.5 μm. Tensile samples were horizontally sampled and prepared from the block samples, and room temperature and high temperature tensile properties were measured on a tensile tester, and the results are shown in FIG. 3. As can be seen, the room temperature tensile elongation at break of the printed sample reaches 3.5%, the room temperature tensile strength reaches 1220MPa, the 600 ℃ tensile strength reaches 760MPa, and the 650 ℃ tensile strength is still maintained at 600 MPa. The tensile strength of the nano reinforced titanium-based composite material sample prepared by the embodiment at room temperature, 600 ℃ and 650 ℃ is respectively improved by 250 MPa, 140 MPa and 70MPa relative to the matrix alloy sample in a printing state.
Example 2:
this example provides a 5.5% by volume (TiB + Y) nano-multiphase particle reinforced Ti-based composite2O3) Additive manufacturing method of Ti-6 Al-4V. The in-situ self-generated high-temperature titanium-based composite material comprises the following chemical elements in percentage by mass: ti-6Al-4V-0.9Y-0.6B, namely 6 percent of Al, 4 percent of V, 0.9 percent of Y, 0.6 percent of B and the balance of Ti by mass ratio. The in situ self-generated nanoreinforcement phase comprises 3.4% TiB and 2.1% Y by volume2O3。
First, the spherical powder is produced in the step (1). Firstly, preparing raw materials according to the mass ratio of alloy elements of Ti-6Al-4V-0.9Y-0.6B of the titanium-based composite material, and manufacturing a standard electrode rod for powder preparation by means of conventional vacuum casting, high-temperature forging and machining process flows. Spherical powder was produced by using the processed titanium-based composite electrode rod by a Plasma Rotary Electrode Process (PREP). The technological parameters of the powder preparation by the PREP method are as follows: voltage is 60V, current is 1600A, electrode rod rotating speed is 20000r/min, feeding speed is 1.0mm/s, and argon atmosphere pressure is 0.080 MPa.
Then, the process step of sieving the powder is carried out. And (3) screening the spherical powder manufactured in the process step I, and screening the spherical powder with the particle size range of 40-130 mu m for electron beam additive manufacturing of the nano particle reinforced titanium-based composite material.
And then, finishing the process step and constructing the digital model. And constructing a three-dimensional digital model of the titanium-based composite material sample with the target shape by using computer drawing software Solidworks, and reasonably designing and adding a support structure. And then, discretizing the constructed three-dimensional digital model by means of slicing software Magics, and exporting the three-dimensional digital model as a three-dimensional digital model file which can be directly used for selective melting additive manufacturing of the electron beam.
And (4) carrying out the process step of electron beam selective melting additive manufacturing of the titanium-based composite material by using the spherical powder screened in the step (c) and the discretized three-dimensional digital model constructed in the step (c). Sequentially mounting Ti-6Al-4V titanium alloy substrates, filling spherical powder into a forming bin, and vacuumizing the forming bin to 5.0 x 10-3Pa, heating the substrate to 600 ℃ by electron beams, and the like. Then, electron beam selective melting forming of the titanium-based composite material is carried out. And (3) preheating the powder layer by rapidly scanning the powder layer for 1-3 times by using an electron beam for each layer of powder, then carrying out contour scanning and selective melting by using a slow electron beam, and circulating the steps until the forming is finished. The parameters of the selective melting process of the electron beams are as follows: 15mA of melting current, 6m/s of melting scanning speed, 30mA of preheating current, 20m/s of preheating scanning speed, 60 μm of layer thickness, 95 μm of pass interval and a reciprocating scanning strategy. In the selective melting and forming process of the electron beam, the vacuum degree of a forming chamber is always kept to be less than or equal to 0.01 Pa;
finally, finishing the post-treatment in the process step (v). And (4) taking the titanium-based composite material sample manufactured by the electron beam additive manufacturing from the powder bed, removing the substrate, cutting off the bracket, and performing surface sand blasting treatment. After the post-treatment work is finished, the nano-particle reinforced titanium-based composite material sample piece manufactured by electron beam additive manufacturing is obtained.
The volume ratio of (TiB + Y) produced in this example was 5.5%2O3) The oxygen content of the samples and the complex components of the/Ti-6 Al-4V nano reinforced titanium-based composite material is only 0.090 wt%, and the compactness reaches 99.8%. Nanoneedle-like TiB and nanoparticle Y2O3Typical dense three-dimensional network uniform distribution is exhibited, with the average cell size of the reinforcing phase fine network structure being only 2.0 μm. The room temperature fracture elongation of the printing titanium-based composite material sample reaches 6.0 percent, the room temperature tensile strength reaches 1320MPa, and the 600 ℃ tensile strength reaches 650 MPa.
Example 3
This example provides a 5.5% by volume (TiB + Y) nano-multiphase particle reinforced high temperature titanium-based composite2O3+Ti5Si3) Additive manufacturing method of/Ti-6 Al-3Sn-4Zr-0.9 Mo. The in-situ self-generated high-temperature titanium-based composite material comprises the following corresponding alloy elements in percentage by mass: ti-6Al-3Sn-4Zr-0.9Mo-0.3Si-0.4Y-0.6B, namely 6% of Al, 3% of Sn, 4% of Zr, 0.9% of Mo, 0.3% of Si, 0.4% of Y, 0.6% of B and the balance of Ti by mass ratio. The nano reinforcing phase comprises 3.4 percent of TiB and 0.95 percent of Y which are self-generated in situ in volume ratio2O3And about 1.2% Ti5Si3。
This embodiment differs from embodiment 1 in that: the spherical powder is produced by crucible-free induction atomization (EIGA). The powder preparation process parameters of the EIGA method are as follows: electrode bar size
Figure BDA0002981191920000101
The melting temperature is 1850 ℃ and the argon pressure is 3.0 MPa.
The difference between this example and example 1 is that the post-treatment in process step (v) is to take the titanium-based composite material sample manufactured by electron beam additive manufacturing from the powder bed, remove the substrate, cut off the support, and perform surface blasting. Then, the solution treatment and the aging treatment of 1020 ℃/30 min/water cooling +650 ℃/3 h/air cooling are continuously carried out.
The volume ratio of (TiB + Y) produced in this example was 5.5%2O3+Ti5Si3) The oxygen content of a/Ti-6 Al-3Sn-4Zr-0.9Mo nano reinforced titanium-based composite material sample is only 0.09 wt% by means of an oxygen nitrogen hydrogen analyzer, and the density reaches 99.6%. The nanoreinforcement phase exhibits a typical dense three-dimensional network-like uniform distribution, with the average cell size of the fine network structure of the reinforcement phase being only 1.5 μm. The elongation at break at room temperature of the printed sample reaches 3.8%, the tensile strength at room temperature reaches 1200MPa, the tensile strength at 600 ℃ reaches 770MPa, and the tensile strength at 650 ℃ is still maintained at 620 MPa. Solid solution through 1020 ℃/30 min/water cooling +650 ℃/3 h/air cooling&Aging treatment, coarsening most of reinforcing phase particles, enabling the net structure to be arranged and disappear, wherein the TiB crystal whisker consists of superfine rods and nanorods, the diameter of the superfine rods is 50-250 nm, the length of the superfine rods is less than or equal to 2 mu m, and Y is2O3And Ti5Si3The nano particles evolve into superfine spheres and nano spheres with the size less than or equal to 250 nm. Solid solution&The results of the tensile properties test of the titanium matrix composite after the aging heat treatment are shown in FIG. 4. Visible, solid solution&The tensile strength of the titanium-based composite material after aging heat treatment is increased to 1320MPa at room temperature, and the tensile strength of the titanium-based composite material at 600 ℃ and 650 ℃ is respectively increased to 890MPa and 780 MPa. Compared with an alloy matrix sample, the tensile strength of the titanium-based composite material in a heat treatment state is improved by more than 150MPa within the temperature range of room temperature to 700 ℃.
Comparative example
5.5% volume fraction enhanced phase of (TiB + Y) for electron beam additive manufacturing of the invention2O3+Ti5Si3) Compared with a TiB/Ti-6Al-3Sn-4Zr-0.9Mo titanium-based composite material which is also manufactured by adopting electron beam additive manufacturing and has the volume fraction of 5.5 percent enhanced TiB, the tensile fracture elongation at room temperature is improved by 2.0 percent, the tensile strength at room temperature is improved by 200MPa, and the tensile strength at 650 ℃ is improved by 100 MPa.
The TiB/Ti-6Al-4V titanium-based composite material of the 5.5 volume fraction reinforcing phase prepared by laser deposition additive manufacturing by taking spherical powder prepared by a crucible-free electrode gas atomization method as a raw material has the compactness of only 98.5 percent, the room-temperature plasticity of less than 1.5 percent and the 650 ℃ tensile strength of 460 MPa. Therefore, the electron beam additive manufactured multiphase nano particle reinforced titanium-based composite material has outstanding technical advantages in the geometric complexity, compactness, oxygen content and mechanical property indexes of the component.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (9)

1. A manufacturing method of a nanoparticle reinforced titanium-based composite material additive based on selective electron beam melting is characterized by comprising the following steps:
s1, manufacturing spherical powder of the titanium-based composite material;
s2, screening powder;
s3, constructing a digital model;
s4, electron beam additive manufacturing;
s5, post-processing;
in step S4, the parameters of the selective electron beam melting process used in the electron beam additive manufacturing are: the melting current is 6.0-25 mA, the melting scanning speed is 4.0-20 m/s, the preheating current is 20-50 mA, the preheating scanning speed is 15-50 m/s, the layer thickness is 35-90 μm, the channel interval is 60-120 μm, the reciprocating or checkerboard scanning strategy is adopted, and the substrate preheating temperature is 400-1000 ℃.
2. The method of claim 1, wherein the spherical powder is produced by plasma rotary electrode or crucible-less electrode gas atomization to produce spherical pre-alloyed powder of titanium-based composite material.
3. The manufacturing method of claim 1, wherein in step S1, the raw material of the titanium-based composite spherical powder comprises an alloy matrix and a reinforcing phase, the alloy matrix is any one of pure titanium, TC4, TA15, Ti6242 or Ti-Al-Sn-Zr-Mo-Si series high temperature titanium alloy, and the reinforcing phase is TiB, TiC, TiN, Ti5Si3Or one or more rare earth oxides; the volume fraction of the reinforcing phase is selected between 0.5% and 8.0%.
4. The method of claim 3, wherein the rare earth oxide is La2O3Or Y2O3。
5. The method of claim 1, wherein in step S2, the screened spherical powder has a particle size of 40 to 140 μm.
6. The manufacturing method according to claim 1, wherein in step S3, the digital model is a three-dimensional digital model of a ti-based composite sample with a target shape, which is constructed by using computer drawing software, and then the three-dimensional digital model is discretized into a digital model file for direct additive manufacturing.
7. The method of manufacture of claim 6, wherein the computer graphics software is Proe, UG, Solidworks, or Materialise Magics.
8. The method of claim 1, wherein in step S4, the vacuum degree of the forming chamber is maintained at 0.01Pa or less, or the forming chamber is maintained at 0.10-1.0 Pa flowing helium gas during the electron beam additive manufacturing process.
9. The method of manufacturing of claim 1, wherein in step S5, the post-processing is that the titanium-based composite material sample manufactured in step S4 is taken out of the powder bed, separated from the substrate, and subjected to powder cleaning, stent cutting, surface blasting, and heat treatment.
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