CN113523282A - A method for preparing fine equiaxed titanium alloys by 3D printing - Google Patents
A method for preparing fine equiaxed titanium alloys by 3D printing Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000010146 3D printing Methods 0.000 title claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 57
- 239000013078 crystal Substances 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000010936 titanium Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
- 238000009689 gas atomisation Methods 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910008487 TiSn Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
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- 239000000463 material Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
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- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
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- 230000003068 static effect Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 6
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- 238000005242 forging Methods 0.000 description 3
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- 229910052718 tin Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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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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- 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
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- Y02P10/00—Technologies related to metal processing
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Abstract
本发明涉及钛合金材料加工制备领域，具体是一种通过3D打印制备细小等轴晶钛合金的方法，本发明提出了采用激光增材制造技术制备出快速凝固的TA7钛合金，利用材料内部储存的大量畸变能，后通过合适的热处理使合金发生静态再结晶实现晶粒细化，本发明涉及的钛合金的化学成分为：Al 2.5～6.5％，Sn 0.5～4％，Ti余量(按重量百分比计)。首先按照合金成分制备出预合金粉末；然后采用激光选区熔化成形技术制备成钛合金材料；最后将钛合金材料置于真空热处理炉内在700～1000℃温度范围保温1～4h后炉冷，经过充分静态再结晶后得到细小等轴晶的钛合金材料。采用本发明可以研制出具有细小等轴晶的复杂结构钛合金构件，大幅度提升构件的疲劳、断裂韧性等性能。The invention relates to the field of processing and preparation of titanium alloy materials, in particular to a method for preparing small equiaxed titanium alloys by 3D printing. The invention proposes to use a laser additive manufacturing technology to prepare a rapidly solidified TA7 titanium alloy, and utilize the internal storage of the material. A large amount of distortion energy is obtained, and then the alloy is statically recrystallized to achieve grain refinement through appropriate heat treatment. weight percent). Firstly, the pre-alloyed powder is prepared according to the alloy composition; then the titanium alloy material is prepared by laser selective melting and forming technology; finally, the titanium alloy material is placed in a vacuum heat treatment furnace at a temperature range of 700-1000 °C for 1-4 hours, and then the furnace is cooled. After static recrystallization, a titanium alloy material with fine equiaxed crystals is obtained. By adopting the invention, complex structure titanium alloy components with fine equiaxed crystals can be developed, and the properties such as fatigue and fracture toughness of the components can be greatly improved.
Description
The technical field is as follows:
the invention relates to the field of additive manufacturing titanium alloy material processing and preparation, in particular to a method for preparing a fine isometric crystal titanium alloy through 3D printing.
Background art:
the titanium alloy has the characteristics of high specific strength, low density, good corrosion resistance and the like, and is widely applied to the fields of ships, petrochemical industry, aerospace and medical treatment. In recent years, with the development of aerospace related technologies, the requirements on materials are higher and higher, and especially the requirements on the toughness matching of a light structural material which can play a significant weight reduction role are more and more strict. Meanwhile, based on the requirement of improving the performance of the novel equipment, the complexity of the structure and the shape of the novel high-performance device is higher and higher. The 3D printing technique is a metal material processing technique using high energy beam to scan and melt metal powder or wire point by point, scan and overlap line by line, and scan and stack layer by layer, which can realize direct forming of complex structures and shapes, but the molten metal is up to 10 a during processing4～107The cooling rate of K/s is solidified, so that the structure of the formed metal material is an unbalanced ultra-fast solidification structure, the alloy has high strength and low toughness, and the performance stability of the component is obviously influenced. Due to the effect of the temperature gradient in the process, the prepared alloy presents a columnar crystal characteristic along the printing direction, so that the alloy presents serious anisotropy and the performance of a 3D printing sample is influenced.
For titanium alloy components with complex structures and shapes, the structure and performance of the alloy cannot be improved through a conventional hot working process, the structure uniformity is the premise of realizing stable and reliable performance of the components and is the urgent need of high-performance equipment, and therefore the forming technology of the titanium alloy components with the complex structures and fine isometric crystal structures becomes a key technology which needs to be solved urgently in the field of aerospace. The urgent need exists.
The invention content is as follows:
in order to solve the above problems, an object of the present invention is to provide a method for preparing a fine isometric crystal titanium alloy by 3D printing, first preparing prealloyed powder according to alloy components; then preparing a titanium alloy material by adopting a selective laser melting forming technology; and finally, placing the titanium alloy material in a vacuum heat treatment furnace, preserving heat for 1-4 h at the temperature of 700-1000 ℃, cooling the furnace, and fully and statically recrystallizing to obtain the fine isometric crystal titanium alloy material. The invention can realize the structural uniformity of a complex component and simultaneously improve the toughness of the alloy, and has important significance for realizing the obdurability matching of materials and solving the requirement of heavy components in the aerospace field.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for preparing a fine isometric crystal titanium alloy through 3D printing comprises the following chemical components in percentage by weight: 2.5-6.5% of Al, 0.5-4% of Sn and the balance of Ti; firstly, prealloying powder is prepared by a crucible-free induction melting gas atomization method, and the prealloying powder is used for preparing a titanium alloy material in a laser selective melting 3D printing mode; then, the titanium alloy material is placed in a vacuum heat treatment furnace, the temperature is raised to 700-1000 ℃ in a vacuum environment, the temperature is kept for 1-4 hours at the temperature, and then the titanium alloy material is naturally cooled to room temperature and taken out of the furnace.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the preferable content range of the Al element is 4.0-6.0 wt.%.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the preferable content range of the Sn element is 1.5-3.5 wt.%.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the titanium alloy material prepared in the mode of selective laser melting and 3D printing is a solid sample, a porous sample or a component with a complex structure.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the cross section and the longitudinal section of the titanium alloy material after heat treatment are both isometric crystal tissues.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the raw material of Ti element is sponge titanium, the raw material of Al element is pure aluminum, and the raw material of Sn element is TiSn alloy.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, materials are mixed according to required alloy components, pre-alloyed powder is prepared through a crucible-free induction melting gas atomization method, and the particle size range of the powder is 15-53 mu m.
According to the method for preparing the fine isometric crystal titanium alloy through 3D printing, the room-temperature tensile property of the prepared titanium alloy material is as follows: tensile strength Rm750 to 950MPa, yield strength Rp0.2700 to 800MPa, and 15 to 25% elongation A.
The design idea of the invention is as follows:
the invention provides a method for preparing rapidly solidified TA7 titanium alloy by adopting a laser additive manufacturing technology, which utilizes a large amount of distortion energy stored in the alloy in the non-equilibrium solidification process to lead the alloy to generate static recrystallization through proper heat treatment so as to realize grain refinement. In addition, the invention fully utilizes the coupling in the aspects of alloy components, process, heat treatment and the like, and can realize the structural uniformity control of complex components.
The invention has the advantages and beneficial effects that:
the invention relates to a method for preparing a fine isometric crystal titanium alloy through 3D printing, the preferable titanium alloy components and heat treatment system improve the anisotropy of the alloy and simultaneously improve the toughness of the alloy, and the mechanical property of the alloy is not greatly changed after heat treatment in the heat treatment range. By adopting the method, the high-strength high-toughness non-anisotropic comprehensive equiaxial-structure titanium alloy can be obtained, and a new approach support is provided for the application of the 3D printing titanium alloy in the fields of aerospace and the like.
Description of the drawings:
fig. 1 shows the original metallographic microstructure of the titanium alloy with a cross section (a) and a longitudinal section (b) printed in a 3D mode.
FIG. 2 is an original metallographic microstructure of a cross section (a) and a longitudinal section (b) of the titanium alloy which is subjected to 3D printing after heat treatment at 800 ℃.
FIG. 3 is an original metallographic microstructure of a cross section (a) and a longitudinal section (b) of the titanium alloy which is 3D printed after the heat treatment at 900 ℃.
The specific implementation mode is as follows:
in the specific implementation process, the 3D printing titanium alloy material is prepared according to required alloy components, raw materials such as sponge titanium and the like are uniformly mixed and then pressed into an electrode, the electrode is subjected to vacuum consumable melting and then forged and rolled to prepare bar material suitable for a crucible-free induction melting gas atomization method to prepare pre-alloy powder, and the pre-alloy powder is prepared into the titanium alloy material by adopting a 3D printing mode of selective laser melting. And (3) keeping the temperature of the titanium alloy material in a vacuum heat treatment furnace at 700-1000 ℃ for 1-4 h, and then cooling the furnace to obtain the titanium alloy material with comprehensive isometric crystals. Compared with the toughness of the original 3D printing titanium alloy material, the toughness of the comprehensive equiaxed titanium alloy material is improved, and meanwhile, the mechanical properties of the alloy are not greatly influenced by different heat treatments.
The present invention is further illustrated in detail by comparative examples and examples below.
Comparative example 1
The specific process of this comparative example is: the titanium alloy comprises the following chemical components in percentage by weight: 5.3 percent of Al, 2.7 percent of Sn and the balance of Ti. The method comprises the steps of uniformly mixing raw materials such as sponge titanium and the like, pressing an electrode, forging and rolling the electrode after vacuum consumable melting to prepare pre-alloy powder suitable for a bar material prepared by a crucible-free induction melting gas atomization method, wherein the granularity of the pre-alloy powder is 15-53 mu m, and the pre-alloy powder is prepared into a titanium alloy sample by adopting a 3D printing mode of selective laser melting.
Fig. 1 is an original metallographic microstructure of a cross section (a) and a longitudinal section (b) of the titanium alloy which are printed in a 3D mode, and it can be seen from fig. 1 that the cross section of the titanium alloy structure of the comparative example is an original printing island-shaped morphology, and the longitudinal section is columnar crystals along a vertical printing direction.
Example 1
In this embodiment, the titanium alloy comprises the following chemical components in percentage by weight: 5.3 percent of Al, 2.7 percent of Sn and the balance of Ti. The method comprises the steps of uniformly mixing raw materials such as sponge titanium and the like, pressing an electrode, forging and rolling the electrode after vacuum consumable melting to prepare pre-alloy powder suitable for a bar material prepared by a crucible-free induction melting gas atomization method, wherein the granularity of the pre-alloy powder is 15-53 mu m, and the pre-alloy powder is prepared into a titanium alloy sample by adopting a 3D printing mode of selective laser melting. And heating the 3D printed titanium alloy sample to 800 ℃ in a vacuum environment, then preserving the heat for 2h at the temperature, and then cooling in a furnace to obtain the final titanium alloy sample.
FIG. 2 shows that the original metallographic microstructure of the cross section (a) and the longitudinal section (b) of the titanium alloy is printed in a 3D mode after heat treatment at 800 ℃, the island-shaped appearance of the cross section in the original 3D printing state disappears to present an isometric crystal appearance, the columnar crystal appearance of the longitudinal section disappears to present an isometric crystal appearance, and the size of the obtained fine isometric crystal is 50 μm.
Example 2
In this embodiment, the titanium alloy comprises the following chemical components in percentage by weight: 5.3 percent of Al, 2.7 percent of Sn and the balance of Ti. The method comprises the steps of uniformly mixing raw materials such as sponge titanium and the like, pressing an electrode, forging and rolling the electrode after vacuum consumable melting to prepare pre-alloy powder suitable for a bar material prepared by a crucible-free induction melting gas atomization method, wherein the granularity of the pre-alloy powder is 15-53 mu m, and the pre-alloy powder is prepared into a titanium alloy sample by adopting a 3D printing mode of selective laser melting. And heating the 3D printed titanium alloy sample to 900 ℃ in a vacuum environment, then preserving the heat for 2h at the temperature, and then cooling in a furnace to obtain the final titanium alloy sample.
FIG. 3 shows that the original metallographic microstructure of the cross section (a) and the longitudinal section (b) of the titanium alloy is printed in a 3D mode after the heat treatment at 900 ℃, the island-shaped appearance of the cross section in the original 3D printing state disappears to present an isometric crystal appearance, the columnar crystal appearance of the longitudinal section disappears to present an isometric crystal appearance, and the size of the obtained fine isometric crystal is 50 μm.
The performance of the 3D printed titanium alloy samples obtained in comparative example 1 and examples 1-2 was tested, and the results are shown in table 1 below.
Table 1 shows the properties of the 3D-printed titanium alloy samples obtained in comparative example 1 and examples 1 to 2
As can be seen from Table 1, the properties of the heat-treated 3D printed titanium alloy sample obtained by the method of the invention can be obviously improved by heat treatment, and the mechanical properties of the titanium alloy sample are not greatly changed after different heat treatments, so that an effective solution is provided for the practical application of the titanium alloy sample.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (8)
1. A method for preparing a fine isometric crystal titanium alloy through 3D printing is characterized in that the titanium alloy comprises the following chemical components in percentage by weight: 2.5-6.5% of Al, 0.5-4% of Sn and the balance of Ti; firstly, prealloying powder is prepared by a crucible-free induction melting gas atomization method, and the prealloying powder is used for preparing a titanium alloy material in a laser selective melting 3D printing mode; then, the titanium alloy material is placed in a vacuum heat treatment furnace, the temperature is raised to 700-1000 ℃ in a vacuum environment, the temperature is kept for 1-4 hours at the temperature, and then the titanium alloy material is naturally cooled to room temperature and taken out of the furnace.
2. The method for preparing fine equiaxed titanium alloy by 3D printing as claimed in claim 1, wherein the preferred content of Al element ranges from 4.0 to 6.0 wt.%.
3. The method for preparing fine equiaxed titanium alloy by 3D printing as claimed in claim 1, wherein the preferred content of Sn element ranges from 1.5 to 3.5 wt.%.
4. The method for preparing the fine isometric crystal titanium alloy through 3D printing according to claim 1, wherein the titanium alloy material prepared by the mode of selective laser melting 3D printing is a solid sample, a porous sample or a component with a complex structure.
5. The method for preparing the fine equiaxed titanium alloy through 3D printing according to claim 1, wherein the cross section and the longitudinal section of the titanium alloy material after heat treatment are equiaxed structures.
6. The method for preparing a fine isometric crystal titanium alloy according to claim 1, wherein the raw material of Ti element is sponge titanium, the raw material of Al element is pure aluminum, and the raw material of Sn element is TiSn alloy.
7. The method for preparing a fine isometric crystal titanium alloy according to claim 6, wherein the pre-alloyed powder is prepared by a crucible-free induction melting gas atomization method according to the required alloy components, and the particle size of the powder is 15-53 μm.
8. The method for preparing the fine isometric crystal titanium alloy through 3D printing according to claim 1, wherein the room-temperature tensile property of the prepared titanium alloy material is as follows: tensile strength Rm750 to 950MPa, yield strength Rp0.2700 to 800MPa, and 15 to 25% elongation A.
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| CN115446329A (en) * | 2022-09-08 | 2022-12-09 | 辽宁五寰特种材料与智能装备产业技术研究院有限公司 | SLM (selective laser melting) technology-based high-strength Ti-Al-V-based alloy 3D printing manufacturing method |
| CN115446329B (en) * | 2022-09-08 | 2024-04-19 | 辽宁五寰特种材料与智能装备产业技术研究院有限公司 | High-strength Ti-Al-V based alloy 3D printing manufacturing method based on SLM technology |
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