CN113319292B - Tantalum-tungsten alloy preparation process based on selective laser melting forming and tantalum-tungsten alloy - Google Patents
Tantalum-tungsten alloy preparation process based on selective laser melting forming and tantalum-tungsten alloy Download PDFInfo
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- CN113319292B CN113319292B CN202110592195.3A CN202110592195A CN113319292B CN 113319292 B CN113319292 B CN 113319292B CN 202110592195 A CN202110592195 A CN 202110592195A CN 113319292 B CN113319292 B CN 113319292B
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/66—Treatment of workpieces or articles after build-up by mechanical means
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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
- B33Y10/00—Processes of additive manufacturing
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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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- 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
- C22C1/045—Alloys based on refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention discloses a tantalum-tungsten alloy preparation process based on selective laser melting and forming and a tantalum-tungsten alloy, and the preparation process comprises a forming process, wherein the forming process adopts selective laser melting and forming to obtain a tantalum-tungsten alloy component, and parameters of selective laser melting and forming are optimized to obtain optimal forming parameters of different structures such as inner filling, a structural body, a grid support, an upper surface test piece and a lower surface test piece. According to the invention, by reasonably designing laser forming parameters, the tantalum-tungsten alloy component without defects such as poor interlayer bonding, air holes and cracks can be formed, and the TaW alloy manufactured based on additive is higher in cost-effectiveness ratio, lower in processing cost and higher in efficiency than the TaW alloy material adopting traditional powder metallurgy.
Description
Technical Field
The invention relates to the technical field of laser additive manufacturing, in particular to a tantalum-tungsten alloy preparation process based on selective laser melting and forming and a tantalum-tungsten alloy.
Background
Because of excellent high temperature resistance and corrosion resistance, tantalum alloy is increasingly applied under severe working condition environments, but because tantalum-tungsten alloy has high hardness and high melting point, the traditional powder metallurgy process and material reduction manufacturing method have the defects of low material utilization rate, high cost, long processing period and low material yield during processing, and the higher price of the tantalum alloy has a great barrier effect on the expansion of application range and dosage.
Disclosure of Invention
The invention aims to provide a tantalum-tungsten alloy preparation process based on selective laser melting forming, which adopts a laser additive manufacturing technology to solve the problems of low material utilization rate, high cost, long processing period and low yield of the existing tantalum-tungsten alloy forming process.
The invention is realized by the following technical scheme:
a tantalum-tungsten alloy preparation process based on selective laser melting forming is characterized by comprising a forming process, wherein the forming process adopts selective laser melting forming to obtain a tantalum-tungsten alloy component, and parameters of selective laser melting forming are shown in table 1:
TABLE 1 Process parameters for selective laser melting formation of tantalum-tungsten alloy
The method comprises the steps of respectively printing test pieces with different structures on the inner filling, the structure body, the grid support, the upper surface and the lower surface under different process parameters, determining process conditions by comparing the quality of the test pieces, setting parameters in table 1 to be the optimal process conditions of the inner filling, the structure body, the grid support, the upper surface and the lower surface, and setting according to the parameters in table 1 during printing according to the specific structural characteristics of the specific test pieces to finish the printing of the test pieces.
The melting, solidification and cooling processes of tantalum-tungsten alloy laser forming are all carried out under the extremely rapid condition, defects such as poor interlayer bonding, air holes, cracks and the like are easily formed due to improper parameter control, and the forming quality of the tantalum-tungsten alloy is comprehensively influenced by parameters such as laser power, scanning speed, scanning path, layer thickness, spot diameter and the like, so that the key point of obtaining the tantalum-tungsten alloy component by adopting selective laser melting forming lies in parameter setting.
The invention adopts different entity forming parameters to form a metallographic specimen and a surface quality test piece, researches the sintering condition of the surface of the specimen during forming, the distribution and quantity of defects such as unfused, air holes and cracks in the formed specimen, researches the influence of parameters such as laser power, scanning speed, channel spacing, scanning path and the like on the defects in the entity and the surface quality, finally optimizes the process parameters of no defects such as unfused, surface crack and air holes in the metallographic specimen through repeated superposition of multiple combination parameters, and simultaneously aims at the high melting point (above 3000 ℃) of tantalum-tungsten alloy and the large internal stress remained in the alloy after rapid solidification, thereby easily causing cracking and deformation of thin-wall pieces, being more easily shrunk and deformed for thin-wall shell type components and being difficult to control the forming precision between thin walls. The applicant measures the size of a typical feature part by using a three-dimensional scanner, performs size precision correction by local structure optimization, model size compensation and scanning spot offset technology according to the size data of a typical tantalum-tungsten member to be formed, and obtains forming basic process parameters shown in table 1 after repeated verification.
Therefore, the invention not only can form and obtain the tantalum-tungsten alloy component without the defects of poor interlayer bonding, air holes, cracks and the like by reasonably designing laser forming parameters, but also can manufacture the TaW alloy based on additive materials, has higher efficiency and cost ratio, lower processing cost and higher efficiency than the TaW alloy material adopting the traditional powder metallurgy, and solves the problems of low material utilization rate, high cost, long processing period and low yield of the existing tantalum-tungsten alloy forming process.
The invention can print out the model machines with different shapes according to different support structure designs and linear cutting modes, and the model machines comprise hollow structures, blocks, outer rings, flat plates and cavities.
Further, the method also comprises a post-treatment process, wherein the post-treatment process comprises the following steps of carrying out heat treatment on the tantalum-tungsten alloy component, and the parameters of the heat treatment are as follows: heat treatment at 1500 deg.C for 2h, and furnace cooling.
The influence of the heat treatment process on the grain structure and the mechanical property optimizes the heat treatment process of the tantalum-tungsten alloy, and can improve the mechanical property of the tantalum-tungsten alloy.
The invention adopts metallographic samples to carry out vacuum annealing test, adjusts annealing temperature and heat preservation time, respectively obtains coarse structures of stress relief annealing, partial recrystallization, complete recrystallization and complete recrystallization grains, selects the above 4 groups of heat treatment processes to carry out annealing on mechanical property samples, carries out room temperature mechanical property test after the annealing, and analyzes the influence of microscopic structures on the mechanical property. The typical workpiece is subjected to heat treatment by adopting a group of heat treatment processes with optimal mechanical properties, whether the workpiece is deformed or not is observed, the size is measured, correction is carried out by reducing the heating rate or processing tools and other methods, and finally the heat treatment process is solidified, wherein the specific process comprises the following steps:
five heat treatment schedules are designed according to the characteristics of the tantalum-tungsten material, and the specific heat treatment schedule is shown in the following table 2:
TABLE 2 Heat treatment Process parameters
| Serial number | Heat treatment System | Content providing method and apparatus |
| 1 | HT1 | 1150 ℃ for 2h, furnace cooling |
| 2 | HT2 | 900 ℃,2h, furnace cooling |
| 3 | HT3 | 1400 ℃,2h, furnace cooling |
| 4 | HT4 | Furnace cooling at 1500 ℃,2h |
| 5 | HT5 | Furnace cooling at 1500 ℃,5h |
Selecting the same equipment and the same parameters, comparing tensile samples under the same heat treatment furnace, performing room-temperature tensile sample according to GB/T228.1-2010 after post-treatment and machining of the standard tensile sample, and performing tensile sample at room temperature (20 ℃), wherein the tensile sample is taken
The mechanical property data of the sample under the specific heat treatment system are shown in Table 3:
TABLE 3 mechanical property test results corresponding to different heat treatment systems
From the data in table 3, it can be seen that:
and selecting the optimal heat treatment method for 1500-2 h.
Further, the post-treatment process also comprises the step of cutting the tantalum-tungsten alloy component after the heat treatment so as to separate the base material from the test piece.
Further, the method comprises the following steps:
s1, pretreating tantalum-tungsten powder and a base material;
s2, adopting selective laser melting forming to obtain a tantalum-tungsten alloy component;
s3, carrying out heat treatment on the formed tantalum-tungsten alloy component;
and S4, cutting the tantalum-tungsten alloy component after heat treatment to separate the base material from the test piece.
Further, in step S1, the particle size of the tantalum tungsten powder is 10 to 60 μm.
The method is characterized in that the particle size of tantalum-tungsten powder is obtained by referring to the requirements of material powder such as titanium alloy, high-temperature alloy and aluminum alloy, and the flowability, particle size distribution, spherical percentage, hollow percentage and chemical composition of raw material powder are detected.
Further, in step S1, the thickness of the base material is 15mm to 25mm.
Further, in the step S2, argon is used for protection during the forming process of the tantalum-tungsten alloy component, and the oxygen content in the forming chamber is controlled within 100ppm, so as to solve the problem that the plasticity of the alloy material is reduced due to too high oxygen content, thereby affecting the mechanical properties.
Further, in step S3, the parameters of the heat treatment are: heat treatment at 1500 deg.c for 2 hr and furnace cooling.
Further, the method also comprises the steps of cleaning, grinding and sand blasting the cut test piece.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the invention, by reasonably designing laser forming parameters, the tantalum-tungsten alloy component without defects such as poor interlayer bonding, air holes and cracks can be formed, and the TaW alloy manufactured based on additive is higher in cost-effectiveness ratio, lower in processing cost and higher in efficiency than the TaW alloy material adopting traditional powder metallurgy.
2. According to the invention, the tantalum-tungsten alloy test piece prepared by reasonably designing the heat treatment parameters has higher mechanical property.
3. The invention can print the model machines with different shapes according to different support structure designs and linear cutting modes.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a diagram of the gold phase of the printed underfill in TAW deposition state under SEM microscope in example 1;
FIG. 2 is a schematic diagram of the structure of inner filling in printing according to example 1;
FIG. 3 is a schematic diagram of the structure of a printed grid support of example 1;
FIG. 4 is a schematic view of the structure of an outer ring printed in embodiment 1;
FIG. 5 is a schematic structural view of a printed structure according to example 1;
FIG. 6 is a schematic view of the structures of the upper and lower surfaces printed in example 1;
FIG. 7 is a sample of a flat plate of the TaW alloy material prepared in example 2;
FIG. 8 is a sample of a square cavity of TaW alloy material prepared in example 2;
FIG. 9 is a sample of a flat plate with mounting holes of the TaW alloy material prepared in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and the accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limiting the present invention.
Example 1:
the present embodiment takes TA88W12 alloy as an example:
a tantalum-tungsten alloy preparation process based on selective laser melting forming comprises the following steps:
s1, pretreating tantalum-tungsten powder and a base material:
before forming, TAW powder is delivered from a warehouse, the particle size range of the powder is selected from 10-60 μm according to the requirements of material powder such as titanium alloy, high-temperature alloy, aluminum alloy and the like, and the flowability, particle size distribution, spherical percentage, hollow percentage and chemical components of the raw material powder are detected;
before forming, preparing a base material: tungsten with the thickness of 20mm is used as a base material, and the base material is fixed by a high-strength screw; wiping the base material with alcohol, mounting the base material and leveling;
s2, adopting selective laser melting and forming to obtain a tantalum-tungsten alloy component, wherein selective laser melting and forming parameters are shown in Table 1, argon is adopted for protection in the tantalum-tungsten alloy forming process, and the oxygen content in a forming chamber is controlled within 100ppm so as to solve the problem that the plasticity of an alloy material is reduced due to overhigh oxygen content in the forming chamber, so that the mechanical property is influenced;
the structures of the inner filling, the grid support, the outer ring and the structural body printed in this embodiment are shown in fig. 2 to 5, the structures of the printed upper surface and the printed lower surface are shown in fig. 6, wherein the upper part of fig. 6 is the upper surface structure, and the metallographic detection result after the inner filling is formed is shown in fig. 1: through metallographic microstructure observation, the metallographic structure in a deposition state is mainly in scanning shapes at different angles, the defects of cracks, air holes, poor fusion and the like do not exist in the metallographic structure, and the density meets the quality requirement;
s3, carrying out heat treatment on the formed tantalum-tungsten alloy component, wherein the parameters of the heat treatment are as follows: heat treatment is carried out for 2h at 1500 ℃, and then furnace cooling is carried out;
s4, cutting the tantalum-tungsten alloy component after heat treatment to separate the base material from the test piece;
s5, cleaning oil stains on the surface of the sample; the sample is subjected to support removal treatment, and the surface of the part cannot be knocked or damaged; polishing the part; performing sand blasting treatment on the surface of the part (fine sand is required, the granularity is more than or equal to 50 meshes), uniformly blasting sand on the surface, and preventing the surface of the part from being knocked or damaged; visual inspection shows that no cracks and pits exist; the surface color of the formed piece is metallic; according to the accessory blank drawing, detecting the detectable size of the part by using a vernier caliper and a three-dimensional scanner; and cleaning the sample and warehousing.
The mechanical properties of the test pieces prepared in this example are shown in table 4:
TABLE 4 mechanical properties of selective laser melting of Ta-W alloy
The TaW alloy material sample prepared in this example is shown in FIGS. 7-9; fig. 7 shows Φ 50 × 0.5 plate, fig. 8 shows square cavity 50 × 0.5, and fig. 9 shows 80 × 0.5 plate (with mounting hole M3.5).
Density of TaW alloy material sample 17 + -0.2 g/cm 3 Wherein the mass fraction of W is 12%, the mass fraction of Ta is 88%, the thermal conductivity is 47-52W/(m multiplied by K), the thermal expansion coefficient is 4-6 multiplied by 10 < -6 >/K, the tensile strength Rm is more than 800MPa, the yield strength Rp0.2 is more than 800MPa, and the elongation A is 8%.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A tantalum-tungsten alloy preparation process based on selective laser melting forming is characterized by comprising a forming process, wherein the forming process adopts selective laser melting forming to obtain a tantalum-tungsten alloy component, and parameters of selective laser melting forming are as follows:
the power of the inner filling is 265W, the speed is 800mm/s, the track spacing is 0.08mm, the additional outer ring is 140W and 300mm/s, and the outer ring is 100W and 300mm/s; the power of the structure is 240W, the speed is 1300mm/s, and the track spacing is 0.11mm; the power of the grid support is 150W, and the speed is 1500mm/s; the power of the upper surface is 170W, the speed is 1000mm/s, the track spacing is 0.04mm, the additional outer ring is 215W and 1200mm/s, and the outer ring is 135W and 1300mm/s; the power of the lower surface was 170W, the speed was 1800mm/s, the track pitch was 0.05mm, the additional outer circles were 180W and 1200mm/s, and the outer circles were 110W and 1500mm/s.
2. The process for preparing tantalum-tungsten alloy based on selective laser melting forming of claim 1, further comprising a post-treatment process, wherein the post-treatment process comprises the step of carrying out heat treatment on the tantalum-tungsten alloy component, and the parameters of the heat treatment are as follows: heat treatment at 1500 deg.C for 2h, and furnace cooling.
3. The process for preparing the tantalum-tungsten alloy based on the selective laser melting forming of claim 2, wherein the post-treatment process further comprises a cutting treatment of the tantalum-tungsten alloy component after the heat treatment, so that the base material and the test piece are separated.
4. The preparation process of the tantalum-tungsten alloy based on the selective laser melting forming is characterized by comprising the following steps of:
s1, pretreating tantalum-tungsten powder and a base material;
s2, adopting selective laser melting forming to obtain a tantalum-tungsten alloy component;
s3, carrying out heat treatment on the formed tantalum-tungsten alloy component;
and S4, cutting the tantalum-tungsten alloy component after heat treatment to separate the base material from the test piece.
5. The process for preparing the tantalum-tungsten alloy based on the selective laser melting forming of claim 4, wherein in the step S1, the particle size of the tantalum-tungsten powder is 10-60 μm.
6. The process for preparing the tantalum-tungsten alloy based on the selective laser melting forming of claim 4, wherein in the step S1, the thickness of the base material is 15 mm-25 mm.
7. The process for preparing tantalum-tungsten alloy based on selective laser melting forming of claim 4, wherein in step S2, argon gas is used for protection during the forming process of the tantalum-tungsten alloy component, and the oxygen content in the forming chamber is controlled within 100 ppm.
8. The process for preparing tantalum-tungsten alloy based on selective laser melting forming of claim 4, wherein in step S3, the parameters of the heat treatment are as follows: heat treatment at 1500 deg.C for 2h, and furnace cooling.
9. The process for preparing tantalum-tungsten alloy based on selective laser melting forming of claim 4, further comprising cleaning, grinding and sand blasting the cut test piece.
10. A tantalum-tungsten alloy produced by the production process as set forth in any one of claims 1 to 9.
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