CN113751724B - Heat treatment method for GH4099 alloy component formed by selective laser melting - Google Patents
Heat treatment method for GH4099 alloy component formed by selective laser melting Download PDFInfo
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- CN113751724B CN113751724B CN202111310804.8A CN202111310804A CN113751724B CN 113751724 B CN113751724 B CN 113751724B CN 202111310804 A CN202111310804 A CN 202111310804A CN 113751724 B CN113751724 B CN 113751724B
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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
- 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
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/25—Process efficiency
Abstract
The invention provides a heat treatment method for forming a GH4099 alloy component by selective laser melting, which is characterized in that the GH4099 alloy component is prepared by selective laser melting technology; heating the GH4099 alloy and the substrate from room temperature to 450-550 ℃, preserving heat for 1.5-2 h, performing stress relief annealing, and cooling to room temperature; heating the GH4099 alloy from room temperature to 1130-1170 ℃, preserving heat for 1.5-2 h, and cooling to room temperature; and heating the GH4099 alloy from room temperature to 740-810 ℃, preserving heat for 8-10 h, and cooling to room temperature. The GH4099 alloy after heat treatment does not deform and crack, columnar crystals in an alloy structure are converted into isometric crystals, the size of carbides at a crystal boundary is inhibited, small-sized gamma' phase particles with extremely high volume fraction dispersion distribution are separated out in the crystals, and the GH4099 alloy has excellent strength and plasticity.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing engineering, and particularly relates to a heat treatment method for forming a GH4099 alloy component by selective laser melting.
Background
The GH4099 alloy is a nickel-base superalloy containing a gamma' phase (Ni3Al, Ti) as a main strengthening phase, and further contains a certain content of carbides in the structure to play a role in strengthening grain boundaries. The alloy contains Co, Mo, W and other elements with high content to play a role in solid solution strengthening, so that the high-temperature service performance of the alloy can be improved to a great extent, the alloy can be used for a long time below 900 ℃, and the maximum working temperature can reach 1000 ℃. The alloy has stable structure and good cold and hot processing forming and welding performance, and is suitable for manufacturing high-temperature plate bearing structural members such as an aircraft engine combustion chamber, an afterburner and the like.
The unique 'point-line-plane-body' gradually-superposed processing mode and the highly-free forming parameters of the Selective Laser Melting (SLM) technology have outstanding advantages in the aspects of part manufacturing integration, structural lightweight design, material composition gradient, shape function complexity and the like. Provides a brand-new solution for the manufacture of complex parts in the fields of aerospace, mold manufacturing and the like. However, in the SLM forming process, the micro molten pool is rapidly solidified under a very high temperature gradient, so that a large number of unstable structures such as vacancies, dislocations, subgrains and the like are contained in the alloy microstructure, and very high residual stress exists in the microstructure, which causes the formed part to have the mechanical property characteristics of high strength and low plasticity, and especially, the problem that the SLM forming part is insufficient in high temperature plasticity is always a problem to be solved. The mechanical property of the SLM forming GH4099 alloy must be regulated by subsequent heat treatment, but the original structure state of the SLM forming alloy is greatly different from that of the traditional casting, forging and rolling GH4099 alloy, so the existing heat treatment system is not suitable for the heat treatment of the SLM forming GH4099 alloy. At present, after SLM forming GH4099 alloy parts are subjected to heat treatment, the parts are deformed or cracked, and the phenomena of low high-temperature strength and serious insufficient high-temperature plasticity exist.
Disclosure of Invention
In order to solve the technical problems, the invention provides a heat treatment method for forming a GH4099 alloy component by selective laser melting, which is suitable for a heat treatment process for preparing thin-wall or solid parts by SLM forming the GH4099 alloy, and the heat treatment method is used for regulating and controlling the grain state, the carbide content at the grain boundary and the size and the content of an intragranular gamma' phase of the SLM forming GH4099 alloy, so that excellent high-temperature mechanical properties are finally obtained, and the heat-treated parts are not deformed or cracked.
The invention provides a heat treatment method for forming a GH4099 alloy component by selective laser melting, which comprises the following steps:
step S1, preparing a GH4099 alloy component by adopting a laser selective melting technology;
step S2, heating the GH4099 alloy component melted in the selected laser area prepared in the step S1 and the substrate from room temperature to 450-550 ℃ at the speed of 5-15 ℃/min, preserving heat for 1.5-2 h, performing stress relief annealing, and cooling to room temperature after heat preservation;
and step S3, cutting the GH4099 alloy member obtained in step S2 from the substrate by selective laser melting, and then carrying out solution heat treatment: heating the GH4099 alloy component melted in the selected laser area obtained in the step S2 from room temperature to 1130-1170 ℃ at the speed of 10-20 ℃/min, preserving heat for 1.5-2 h, and cooling to room temperature after heat preservation;
step S4, aging heat treatment: and (5) heating the GH4099 alloy component melted in the selected laser area obtained in the step (S3) from room temperature to 740-810 ℃ at the speed of 10-20 ℃/min, preserving heat for 8-10 h, and cooling to room temperature after heat preservation.
Preferably, when the cooling is performed to room temperature in step S2, step S3, and step S4, the cooling method used is inert gas cooling or air cooling.
The invention has the following beneficial effects:
the heat treatment method for forming the GH4099 alloy component by selective laser melting is suitable for thin-wall parts and solid parts prepared by forming the GH4099 alloy by SLM (selective laser melting); after stress relief annealing heat treatment, the thin wall and the solid part are not deformed and cracked; then, after solution heat treatment, columnar crystals in the GH4099 alloy structure are converted into isometric crystals, dendritic crystals in original crystal grains are completely eliminated, the crystal grains are completely recrystallized, original distortion energy is completely released, a large number of twin crystals are formed in the structure, the size of carbides at grain boundaries is inhibited, and the improvement of the plasticity of the GH4099 alloy is facilitated; finally, after aging heat treatment, gamma' phase particles which are small in size and have extremely high volume fraction dispersion distribution are separated out from the crystal, so that the GH4099 alloy after heat treatment has high strength. The average size of the obtained gamma' phase in crystal is less than 20nm, and the volume fraction is higher than 50%. The high-temperature mechanical property of the GH4099 alloy after heat treatment is remarkably improved, the yield strength is more than 400 MPa at 900 ℃, the elongation is more than 25%, and the strength and plasticity are well matched.
According to the invention, through the good cooperation of the heat treatment system, the SLM-formed GH4099 alloy is free from deformation and cracking, the structural integrity of parts is ensured, and meanwhile, the SLM-formed GH4099 alloy has excellent strength and plasticity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description are only some embodiments of the present invention.
FIG. 1 shows (a) the molten pool morphology, (b) the molten pool internal dendrite morphology of the original texture of the SLM-formed GH4099 alloy prepared in step S1 of example 1;
FIG. 2 shows (a) an inverse pole figure and (b) a grain orientation expansion figure of the original structure of the SLM-formed GH4099 alloy prepared at step S1 in example 1;
FIG. 3 shows (c) a reverse pole diagram and (d) a grain orientation expansion diagram of an SLM-formed GH4099 alloy after stress annealing and solution heat treatment in example 1;
FIG. 4 is a microstructure of an SLM-formed GH4099 alloy after stress annealing and solution heat treatment in example 1;
FIG. 5 is a graph of the distribution of the gamma prime phase in the SLM-formed GH4099 alloy structure after treatment according to example 1;
FIG. 6 is a stress-strain curve of SLM-formed GH4099 alloy after processing in example 1 under 900 deg.C tension.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a heat treatment method for forming a GH4099 alloy component by selective laser melting, which comprises the following steps:
and step S1, preparing the GH4099 alloy component by adopting a selective laser melting technology.
And S2, heating the GH4099 alloy component melted in the selected laser area prepared in the step S1 and the substrate from room temperature to 450-550 ℃ at the speed of 5-15 ℃/min, preserving heat for 1.5-2 h, performing stress relief annealing, cooling to room temperature after heat preservation, and cooling by adopting an inert gas cooling or air cooling mode.
And step S3, cutting the GH4099 alloy member obtained in step S2 from the substrate by selective laser melting, and then carrying out solution heat treatment: and (4) heating the GH4099 alloy component melted in the selected laser area obtained in the step (S2) from room temperature to 1130-1170 ℃ at the speed of 10-20 ℃/min, preserving heat for 1.5-2 h, cooling to room temperature after heat preservation, and cooling by adopting an inert gas cooling or air cooling mode.
Step S4, aging heat treatment: and (5) heating the GH4099 alloy component melted in the selected laser area obtained in the step (S3) from room temperature to 740-810 ℃ at the speed of 10-20 ℃/min, preserving heat for 8-10 h, cooling to room temperature after heat preservation, and cooling by adopting an inert gas cooling or air cooling mode.
Example 1
The embodiment provides a heat treatment method for forming a GH4099 alloy component by selective laser melting, which comprises the following steps:
and step S1, preparing GH4099 alloy component samples by adopting a Selective Laser Melting (SLM) technology. GH4099 alloy spherical powder with the particle size of 15-53 mu m is used as a forming material, and is formed by selective laser melting equipment, wherein the forming parameters are laser power of 350W, laser scanning speed of 1100 mm/s, powder spreading thickness of 40 mu m, scanning interval of 90 mu m, scanning strategy is strip-type bidirectional scanning, interlayer rotation is 67 DEG, and the substrate is preheated to 80 ℃. Wherein the size of the specimen for the detection of the microstructure is 10 mm. times.10 mm, and the size of the tensile specimen is determined in accordance with GH/T4338-2006.
And step S2, heating the GH4099 alloy component sample prepared in the step S1 and the substrate from room temperature to 500 ℃ at the speed of 5 ℃/min, preserving heat for 2h, performing stress relief annealing, and cooling the sample to room temperature by air after the heat preservation is finished.
And step S3, subsequently, cutting the GH4099 alloy component sample obtained in the step S2 from the substrate by using a wire cutting device, and then placing the cut GH4099 alloy component sample in a heat treatment furnace for solution heat treatment: and (4) heating the GH4099 alloy component sample obtained in the step S2 from room temperature to 1150 ℃ at the speed of 15 ℃/min, then carrying out heat preservation for 1.5h, and cooling the air to room temperature after finishing the heat preservation.
Step S4, aging heat treatment: and (4) heating the GH4099 alloy component sample obtained in the step S3 from room temperature to 750 ℃ at a speed of 15 ℃/min, then carrying out heat preservation for 8h, and carrying out air cooling to room temperature after the heat preservation is finished. And then grinding and polishing a GH4099 alloy component sample obtained after heat treatment, observing a microstructure after metallographic corrosion, and then performing high-temperature tensile verification at 900 ℃.
The GH4099 alloy structure formed by the SLM is shown in figure 1 (a), the lap joint between molten pools is tight, no crack and hole defect exists, and the material is nearly compact; the dendrites in submicron level are uniformly distributed in the molten pool as shown in FIG. 1 (b). The crystal grains in the morphological structure are irregularly shaped columnar crystals growing along the forming direction, as shown in fig. 2 (a). Using the grain orientation expansion map obtained by EBSD (electron back scattering diffraction), as shown in fig. 2 (b), it can be seen that a large number of subgrain boundaries exist inside the original grains of the SLM-formed GH4099 alloy, and the average orientation difference inside the grains is 2.55 °.
After the stress relief annealing and the solution heat treatment of the embodiment, the crystal grains of the SLM-formed GH4099 alloy are transformed into isometric crystals, a large number of twin crystals are generated, and no crack or crack is generated, as shown in FIG. 3 (c); small-angle grain boundaries in the GH4099 alloy grains are eliminated, a large number of twin grain boundaries are formed, the grain orientation expansion diagram obtained by EBSD (electron back scattering diffraction) is shown in fig. 3 (d), the average orientation difference in the grains is 0.42 degrees, which means that the grains are completely recrystallized, so that residual stress in the grains caused by extremely high cooling speed in the SLM forming process is released, and the matrix is softened, which is favorable for greatly improving the plasticity of the material. And as can be seen from fig. 4, the size of the carbide at the grain boundary is less than 1 μm, and the precipitation of the carbide is greatly inhibited, which is beneficial to relieving the premature failure of the material under the high-temperature stretching condition due to the overhigh local stress of the grain boundary.
FIG. 5 shows the gamma-prime phase precipitated from the alloy structure after the stress relief annealing, solution heat treatment and aging heat treatment of this example, and it can be seen that the average size of the gamma-prime phase is 15nm and the volume fraction is 60. + -.6%. The precipitation of the gamma' phase in the alloy with small size and high density is beneficial to the improvement of the high-temperature strength of the alloy.
Finally, the SLM-formed GH4099 alloy after heat treatment in this embodiment is subjected to 900 ℃ tensile verification, and as can be seen from fig. 6, compared with the SLM-formed GH4099 alloy after being treated by the heat treatment system (1100 ℃x1 h, 800 ℃x8 h) adopted by the conventional formed GH4099 alloy, the SLM-formed GH4099 alloy after being treated by the heat treatment system (1150 ℃x1.5 h, 750 ℃x8 h) in this embodiment greatly improves the plasticity of the material without sacrificing the strength of the material, which is beneficial to effective regulation and control of the microstructure of the SLM-formed GH4099 alloy by the heat treatment system provided in this embodiment. The problem that the high-temperature plasticity of the GH4099 alloy formed by the SLM is difficult to meet the use requirement is solved.
In the embodiment, the GH4099 alloy grains formed by selective laser melting are completely recrystallized, the grains are transformed from columnar grains to isometric grains, the precipitation of large-size carbides at grain boundaries is inhibited, the average size of the obtained intragranular gamma' phase is less than 20nm, and the volume fraction is higher than 50%. The high-temperature mechanical property of the GH4099 alloy after heat treatment is remarkably improved, the yield strength is more than 400 MPa at 900 ℃, the elongation is more than 25%, and the strength and plasticity are well matched.
According to the technical scheme, the heat treatment method for forming the GH4099 alloy component by selective laser melting provided by the embodiment is suitable for thin-wall parts and solid parts prepared by SLM forming of the GH4099 alloy; after stress relief annealing heat treatment, the thin wall and the solid part are not deformed and cracked; then, after solution heat treatment, columnar crystals in the GH4099 alloy structure are converted into isometric crystals, dendritic crystals in original crystal grains are completely eliminated, the crystal grains are completely recrystallized, original distortion energy is completely released, a large number of twin crystals are formed in the structure, the size of carbides at grain boundaries is inhibited, and the improvement of the plasticity of the GH4099 alloy is facilitated; finally, after aging heat treatment, gamma' phase particles which are small in size and have extremely high volume fraction dispersion distribution are separated out from the crystal, so that the GH4099 alloy after heat treatment has higher strength; by the good cooperation of the heat treatment system, the SLM-formed GH4099 alloy is free of deformation and cracking, the structural integrity of parts is guaranteed, and the SLM-formed GH4099 alloy has excellent strength and plasticity.
The embodiments of the present invention have been described in detail through the embodiments, but the description is only exemplary of the embodiments of the present invention and should not be construed as limiting the scope of the embodiments of the present invention. The scope of protection of the embodiments of the invention is defined by the claims. In the present invention, the technical solutions described in the embodiments of the present invention or those skilled in the art, based on the teachings of the embodiments of the present invention, design similar technical solutions to achieve the above technical effects within the spirit and the protection scope of the embodiments of the present invention, or equivalent changes and modifications made to the application scope, etc., should still fall within the protection scope covered by the patent of the embodiments of the present invention.
Claims (1)
1. A heat treatment method for forming GH4099 alloy components by selective laser melting, the method is characterized by comprising the following steps:
step S1, preparing a GH4099 alloy component by adopting a laser selective melting technology;
step S2, heating the GH4099 alloy component melted in the selected laser area prepared in the step S1 and the substrate from room temperature to 450-550 ℃ at the speed of 5-15 ℃/min, preserving heat for 1.5-2 h, performing stress relief annealing, cooling to room temperature after heat preservation, wherein the cooling mode is inert gas cooling or air cooling;
and step S3, cutting the GH4099 alloy member obtained in step S2 from the substrate by selective laser melting, and then carrying out solution heat treatment: heating the GH4099 alloy component melted in the selected laser area obtained in the step S2 from room temperature to 1130-1170 ℃ at the speed of 10-20 ℃/min, preserving heat for 1.5-2 h, cooling to room temperature after heat preservation, wherein the cooling mode is inert gas cooling or air cooling;
step S4, aging heat treatment: and (5) heating the GH4099 alloy component melted in the selected laser area obtained in the step (S3) from room temperature to 740-750 ℃ at the speed of 10-20 ℃/min, preserving heat for 8-10 h, cooling to room temperature after heat preservation, wherein the cooling mode is inert gas cooling or air cooling.
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| CN115261754B (en) * | 2022-07-22 | 2023-04-18 | 南昌航空大学 | Laser composite additive manufacturing twin-crystal structure nickel-based high-temperature alloy integral heat treatment method |
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