CN115125462A - Heat treatment method for improving stability of structure and performance of titanium alloy manufactured by laser additive - Google Patents

Heat treatment method for improving stability of structure and performance of titanium alloy manufactured by laser additive Download PDF

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Publication number
CN115125462A
CN115125462A CN202210517723.3A CN202210517723A CN115125462A CN 115125462 A CN115125462 A CN 115125462A CN 202210517723 A CN202210517723 A CN 202210517723A CN 115125462 A CN115125462 A CN 115125462A
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titanium alloy
heat treatment
additive manufacturing
laser additive
laser
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CN202210517723.3A
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Chinese (zh)
Inventor
刘欢
龙平
张洁
夏英男
杨玉乐
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Shanghai Hangyi High Tech Development Research Institute Co ltd
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Shanghai Hangyi High Tech Development Research Institute Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/64Treatment of workpieces or articles after build-up by thermal means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/68Cleaning or washing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y40/00Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20Post-treatment, e.g. curing, coating or polishing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a heat treatment method for improving the stability of the structure and performance of a laser additive manufacturing titanium alloy, which comprises the following steps: cleaning stains on the surface and residual metal powder inside the titanium alloy component manufactured by laser additive manufacturing; placing the cleaned titanium alloy component for laser material increase manufacturing in a vacuum heat treatment furnace, and carrying out first-stage isothermal annealing heat treatment; and carrying out isothermal annealing heat treatment on the obtained laser additive manufacturing titanium alloy component at the second stage. The method can effectively improve the plasticity and impact toughness of the TA15 titanium alloy manufactured by the additive, and provides a new solution for optimizing the performance of the titanium alloy member manufactured by the additive; compared with the common heat treatment annealing process, the invention can effectively improve the stability of the material structure and performance.

Description

Heat treatment method for improving structure and performance stability of laser additive manufacturing titanium alloy
Technical Field
The invention relates to a heat treatment method for improving the structure and performance stability of a laser additive manufactured near-alpha titanium alloy, and belongs to the technical field of metal laser additive manufacturing.
Background
The titanium alloy has the characteristics of high specific strength, good corrosion resistance, good high-temperature performance and the like, is widely applied to manufacturing important structural components with high working temperature and complex stress, such as airplane partition frames, wall plates, reinforcements and the like, and has large forging processing difficulty due to the characteristics of narrow forming temperature range, easy local overheating and the like. The laser additive manufacturing technology has the characteristics of short period, high flexibility, quick response and the like, and provides an effective way for the quick manufacturing of titanium alloy parts. However, the rapid melting characteristic of the technology enables the deposition state to obtain a supersaturated acicular martensite structure which is usually metastable, so that the titanium alloy sample has lower plasticity and toughness and needs further heat treatment to improve the microstructure and mechanical properties.
The common annealing heat treatment can promote martensite to decompose to form alpha phase and beta phase, but the formed alpha phase and beta phase structure has the phenomenon of uneven morphology and thickness distribution, which causes the mechanical property of the titanium alloy subjected to the common annealing heat treatment to be unstable. The isothermal annealing heat treatment completes the phase transformation of beta → alpha + beta at a fixed temperature, and ensures the uniformity of the structure and the stability of the performance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the TA15 titanium alloy member manufactured by the laser additive manufacturing method has the problems of poor structure and performance stability, low plasticity, low toughness and the like.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a heat treatment method for improving the stability of the structure and the performance of a laser additive manufacturing titanium alloy comprises the following steps:
step 1): cleaning stains on the surface and residual metal powder inside the titanium alloy component manufactured by laser additive manufacturing;
step 2): placing the cleaned laser additive manufacturing titanium alloy component in a vacuum heat treatment furnace, and carrying out first-stage isothermal annealing heat treatment;
step 3): and 2) carrying out isothermal annealing heat treatment of the second stage on the laser additive manufacturing titanium alloy component obtained in the step 2).
The heat preservation time in the step 2) and the step 3) depends on the maximum wall thickness of the component, and the larger the wall thickness is, the longer the heat preservation time is.
Preferably, the preparation process for laser additive manufacturing the titanium alloy component in the step 1) is a Selective Laser Melting (SLM) or a Laser Melting Deposition (LMD).
Preferably, the method for cleaning stains on the surface of the titanium alloy component manufactured by laser additive manufacturing in the step 1) comprises the following steps: the furnace chamber is wiped by alcohol and non-woven fabrics, so that stains are prevented from evaporating and polluting the furnace chamber in the heat treatment process.
Preferably, the method for cleaning residual metal powder inside the titanium alloy component manufactured by laser additive manufacturing in step 1) comprises the following steps: and the high-pressure air gun is used for cleaning until no powder flows out of the component, so that the powder is prevented from being heated and agglomerated in the heat treatment process to block the internal flow channel of the component.
Preferably, the first-stage isothermal annealing heat treatment in the step 2) specifically comprises: heating to the beta-phase transition temperature T at a heating rate of 2-4 ℃/min β ~(T β And keeping the temperature for 2 to 4 hours at minus 50 ℃.
Preferably, the second-stage isothermal annealing heat treatment in step 3) specifically includes: furnace cooling to 550 ℃ ~ (T) at cooling rate of 2-4 ℃/min β And (4) keeping the temperature at minus 50 ℃ for 2 to 4 hours, and cooling to the normal temperature along with the furnace.
Due to the over-high cooling speed of the laser additive manufacturing technology, the microstructure of the titanium alloy sample manufactured by the laser additive manufacturing technology is that supersaturated acicular martensite is distributed on beta columnar dendrite, and the martensite is promoted to be completely transformed through isothermal annealing heat treatment to form uniform alpha-phase and beta-phase structures. The purpose of the first-stage isothermal annealing heat treatment is as follows: promoting the martensite phase to be completely transformed into beta and alpha phases; the purpose of the isothermal annealing heat treatment of the second stage is: the tissue transformation process from the beta phase to the alpha phase is ensured to be completed at a fixed temperature, so that the uniformity of the tissue, including the distribution content, the tissue form and the size uniformity of the alpha phase and the beta phase, is ensured.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention can effectively improve the plasticity and impact toughness of the TA15 titanium alloy manufactured by the additive, and provides a new solution for optimizing the performance of the titanium alloy member manufactured by the additive;
(2) compared with the common heat treatment annealing process, the invention can effectively improve the stability of the structure and the performance of the material.
Drawings
FIGS. 1 and 2 are microstructure topography images of TA15 titanium alloy components manufactured by laser additive manufacturing in example 1 at different magnifications;
FIG. 3 is a microstructure topography of a laser additive manufactured TA15 titanium alloy component obtained in example 1;
FIG. 4 is a microstructure topography of a laser additive manufactured TA15 titanium alloy component obtained in comparative example 1;
FIG. 5 is a microstructure topography of a TA15 titanium alloy component manufactured by laser additive manufacturing in example 2;
FIG. 6 is a graph of the tensile strength of a laser additive manufactured TA15 titanium alloy part for different heat treatment conditions in example 2;
FIG. 7 is the post-fracture elongation of a TA15 titanium alloy component produced by laser additive manufacturing under different heat treatment conditions in example 2;
FIG. 8 is an illustration of the impact properties of laser additive manufactured TA15 titanium alloy components under different heat treatment conditions in example 2.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1
A heat treatment method for improving the stability of the structure and performance of a laser additive manufactured titanium alloy comprises the following steps:
(1) a TA15 titanium alloy sample piece (a forming state sample for short) is formed by adopting a laser powder bed melting technology (SLM), a laser is adopted as a semiconductor laser, the adopted additive manufacturing equipment is Renishaw AM400, and the additive manufacturing forming process parameters are as follows: the laser power is 200w, the exposure time is 50 mus, the laser spot diameter is 70 um, the spot spacing is 65 um, the powder layer thickness is 30 um, and the scanning spacing is 120 um.
(2) And cleaning the formed sample, cleaning residual metal powder in a powder cleaning box by using a high-pressure air gun, and cleaning stains on the surface of the sample by using alcohol.
(3) Isothermal annealing heat treatment: placing the cleaned forming sample piece into a vacuum heat treatment furnace, vacuumizing to keep the pressure in the furnace at 6.67X 10 -4 ~6.67×10 -3 And Pa, heating to 900 ℃ at the heating rate of 2 ℃/min, preserving heat for 2 hours, then reducing the temperature to 550 ℃ in a furnace cooling mode, preserving heat for 2 hours, and then furnace cooling to room temperature to obtain the isothermal annealing heat treatment state sample.
As shown in FIGS. 1 and 2, the TA15 titanium alloy structure manufactured by laser additive manufacturing is a martensite structure with different sizes, the martensite structure is distributed in a needle-shaped form, and the length of the martensite structure is different from 40 to 100 micrometers. The tensile test results show that the tensile strength of transverse and longitudinal samples of the additive manufacturing TA15 titanium alloy is 1227 +/-38 MPa and 1219 +/-32 MPa respectively, the elongation is 12.3% +/-1.3% and 8.7% +/-2.9% respectively, and the impact work is 19 +/-1J and 18 +/-3J respectively.
As shown in FIG. 3, after isothermal heat treatment at 900 deg.C, 2h +550 deg.C and 2h, the microstructure of the material is uniformly distributed, and the shape and size of the basket-shaped structure are relatively uniform. At this time, the tensile strengths of the samples in the transverse direction and the longitudinal direction were 1032. + -.6 MPa and 1038. + -.3 MPa, respectively, the elongations were 16.0%. + -. 0.8% and 17.0%. + -. 0.0%, respectively, and the impact powers were 40. + -. 1J and 38. + -. 1J, respectively. It follows that isothermal annealing heat treatment can greatly improve the elongation and impact properties of the as-formed material.
Comparative example 1
Comparative example 1 differs from example 1 in that step (3) employs a normal annealing heat treatment: placing the cleaned forming sample piece into a vacuum heat treatment furnace, vacuumizing to keep the pressure in the furnace at 6.67X 10 -4 ~6.67×10 -3 Heating to 900 ℃ at the heating rate of 2 ℃/min in Pa, preserving heat for 2 hours, and then cooling to room temperature along with the furnaceAnd obtaining a common annealed sample.
As shown in FIG. 4, after heat treatment at 900 ℃ for 2h, the microstructure of the material is a basket-shaped structure consisting of an alpha phase and a beta phase, at the moment, the shape and the size of the alpha phase in the basket-shaped structure are not uniformly distributed, the size of the thinner alpha phase is 2.9 μm, and the thicker alpha phase can reach 12.5 μm. At this time, the tensile strengths of the samples in the transverse direction and the longitudinal direction were 1018. + -.3 MPa and 974. + -.17 MPa, respectively, the elongations were 17.6%. + -. 1.0% and 6.8%. + -. 4.9%, respectively, and the impact powers were 29. + -. 7J and 31. + -. 3J, respectively. It can be seen that the strength of the material after the ordinary annealing heat treatment is reduced and the plasticity and impact properties are slightly improved compared with the formed sample.
Example 2
A heat treatment method for improving the stability of the structure and performance of a titanium alloy manufactured by laser additive manufacturing comprises the following steps:
(1) a TA15 titanium alloy sample piece (a forming state sample for short) is formed by adopting a laser powder bed melting technology (SLM), a laser is adopted as a semiconductor laser, the adopted additive manufacturing equipment is Renishaw AM400, and the additive manufacturing forming process parameters are as follows: the laser power is 200W, the exposure time is 50 mu s, the laser spot diameter is 70 mu m, the dot spacing is 65 mu m, the powder layer thickness is 30 mu m, and the scanning spacing is 120 mu m.
(2) Cleaning the formed sample, cleaning residual metal powder in a powder cleaning box by using a high-pressure air gun, and cleaning stains on the surface of the sample by using alcohol.
(3) Placing the cleaned forming sample piece into a vacuum heat treatment furnace, vacuumizing to keep the pressure in the furnace at 6.67X 10 -4 ~6.67×10 -3 And heating to 900 ℃ at the heating rate of 2 ℃/min in Pa, preserving heat for 2 hours, then reducing the temperature to 850 ℃ in a furnace cooling mode, preserving heat for 2 hours, and then furnace cooling to room temperature to obtain the isothermal annealing heat treatment state sample.
As shown in FIG. 5, after isothermal heat treatment at 900 deg.C, 2h +850 deg.C and 2h, the microstructure of the material is uniformly distributed, and the form and size of the basket-shaped structure are relatively uniform. At this time, the tensile strengths of the samples in the transverse direction and the longitudinal direction were 1018. + -.9 MPa and 1026. + -.3 MPa, respectively, the elongations were 16.3%. + -. 0.3% and 16.4%. + -. 0.5%, respectively, and the impact powers were 41. + -.1J and 42. + -.1J, respectively.
In conclusion, the TA15 titanium alloy microstructure manufactured by the laser additive manufacturing method is an acicular martensite structure with nonuniform size; after ordinary annealing heat treatment, the TA15 titanium alloy microstructure manufactured by laser additive is converted into a net basket alpha phase and a beta phase; after isothermal annealing heat treatment, the structural uniformity of the basket-shaped alpha phase and the basket-shaped beta phase is obviously improved, and correspondingly, the plasticity, the impact property and the performance stability of the material are obviously improved.
The tensile strength, elongation and work of impact of additive manufactured TA15 titanium alloy under different heat treatment conditions are shown in fig. 6-8. It can be found that the elongation and impact energy after fracture of the sample in the isothermal annealing heat treatment state are significantly increased compared with those of the sample in the formed state and the sample in the normal annealing state, and at this time, the tensile strength, elongation and impact energy of the sample are very stable, and the difference between the properties of the transverse sample and the longitudinal sample is small because the microstructure of the sample in the isothermal annealing heat treatment state is highly uniform.
Test results show that the plasticity, toughness and stability of structure and performance of the material can be obviously improved through the specific isothermal annealing heat treatment step.

Claims (6)

1. A heat treatment method for improving the stability of the structure and the performance of a titanium alloy manufactured by laser additive manufacturing is characterized by comprising the following steps of:
step 1): cleaning stains on the surface and residual metal powder inside the titanium alloy component manufactured by laser additive manufacturing;
step 2): placing the cleaned laser additive manufacturing titanium alloy component in a vacuum heat treatment furnace, and carrying out first-stage isothermal annealing heat treatment;
step 3): and 2) carrying out isothermal annealing heat treatment of the second stage on the laser additive manufacturing titanium alloy component obtained in the step 2).
2. The heat treatment method for improving the structural and performance stability of the laser additive manufacturing titanium alloy component according to claim 1, wherein the preparation process of the laser additive manufacturing titanium alloy component in the step 1) is a selective laser melting technology or a laser melting deposition technology.
3. The heat treatment method for improving the structural stability and the performance stability of the laser additive manufacturing titanium alloy component according to claim 1, wherein the method for cleaning the stains on the surface of the laser additive manufacturing titanium alloy component in the step 1) comprises the following steps: wiping with alcohol and non-woven fabric.
4. The heat treatment method for improving the structural stability and the performance stability of the laser additive manufacturing titanium alloy component according to claim 1, wherein the method for cleaning the residual metal powder in the laser additive manufacturing titanium alloy component in the step 1) comprises the following steps: and (4) cleaning by using a high-pressure air gun until no powder flows out of the interior of the component.
5. The heat treatment method for improving the structural and performance stability of the laser additive manufacturing titanium alloy according to claim 1, wherein the first-stage isothermal annealing heat treatment in the step 2) is specifically: heating to the beta-phase transition temperature T at a heating rate of 2-4 ℃/min β ~(T β And keeping the temperature for 2 to 4 hours at minus 50 ℃.
6. The heat treatment method for improving the structural and performance stability of the laser additive manufacturing titanium alloy according to claim 1, wherein the second-stage isothermal annealing heat treatment in the step 3) is specifically: furnace cooling to 550 ℃ ~ (T) at cooling rate of 2-4 ℃/min β And (4) keeping the temperature at minus 50 ℃ for 2 to 4 hours, and cooling to the normal temperature along with the furnace.
CN202210517723.3A 2022-05-13 2022-05-13 Heat treatment method for improving stability of structure and performance of titanium alloy manufactured by laser additive Pending CN115125462A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116586635A (en) * 2023-05-17 2023-08-15 成都科宁达科技有限公司 Method for improving bonding performance of TC4 titanium alloy gold porcelain through selective laser cladding

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116586635A (en) * 2023-05-17 2023-08-15 成都科宁达科技有限公司 Method for improving bonding performance of TC4 titanium alloy gold porcelain through selective laser cladding
CN116586635B (en) * 2023-05-17 2024-01-19 成都科宁达科技有限公司 Method for improving bonding performance of TC4 titanium alloy gold porcelain through selective laser cladding

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