CN112011713A - Method for eliminating cracks of 3D printing nickel-based superalloy - Google Patents
Method for eliminating cracks of 3D printing nickel-based superalloy Download PDFInfo
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Abstract
The invention provides a method for eliminating cracks of a 3D printing nickel-based superalloy, and belongs to the technical field of superalloy additive manufacturing. Aiming at the problem that cracks are easy to generate in gamma '-phase precipitation strengthening nickel-based high-temperature alloy 3D printing, the invention firstly provides rare earth microalloying through a proper amount of rare earth, reduces the cracking sensitivity of the gamma' -phase precipitation strengthening nickel-based high-temperature alloy 3D printing, widens a 3D printing process window, inhibits the generation of 3D printing cracks, greatly improves the strength and plasticity of a formed piece, and effectively prevents the formation of cracks in the subsequent processing processes such as storage cracking and subsequent heat treatment cracking in working procedures. The gamma' -phase precipitation-strengthened nickel-based high-temperature alloy Ren 104 prepared by the method has no cracks, the compactness is over 99.4 percent, the yield strength and the tensile strength respectively reach 935MPa and 1256MPa, and the elongation rate is over 14.0 percent.
Description
Technical Field
The invention provides a method for eliminating cracks of a 3D printing nickel-based superalloy, and belongs to the technical field of superalloy additive manufacturing.
Background
The gamma ' phase precipitation strengthening nickel-base high-temperature alloy is one of the great breakthroughs in the field of material science, and the strengthening phase of the gamma ' phase precipitation strengthening nickel-base high-temperature alloy is an ordered and coherent intermetallic compound such as gamma ' -Ni3(Al, Ti), which is generally produced by casting, deformation processing, or powder forming techniques, is widely used in advanced aircraft engines. However, these techniques do not allow the direct formation of complex shaped articles. 3D printing, or additive manufacturing technology, can directly generate three-dimensional parts with near net shape dimensions layer by layer from three-dimensional computer aided design data, has unique advantages in the preparation of high-performance complex-shaped components, and is applied to materials such as titanium alloy, aluminum alloy, stainless steel, nickel-based alloy and the like. The 3D printing forming process is large in temperature gradient, high in cooling speed and repeated in remelting, so that the formed part is high in residual stress and easy to deform and crack, and the 3D printing forming high-quality parts are challenged, and particularly, the gamma' phase precipitation strengthening nickel-based high-temperature alloy with high Al and Ti contents is poor in welding performance, and cracking is the most prominent problem in 3D printing of the alloy.
Exploratory studies have been conducted at home and abroad to address the above problems. The influence of 3 different scanning paths on cracking of a Selective Laser Melting (SLM) formed 'unweldable' nickel-based high-temperature alloy is researched by catching pole-Smith and the like [ catching pole-Smith S, et al, sectional scan scales for selective laser melting of 'unweldable' nickel superalloys [ J ]. Additive Manufacturing,2017,15: 113. 122.], a sample formed by adopting an irregular scanning path has smaller thermal stress and uniform distribution, cracks are obviously reduced, the density is improved by 2 +/-0.7%, but the cracks cannot be completely eliminated; further hot isostatic pressing is used to completely eliminate the cracks. Xu et al [ Jianjun Xu, et al, the initiation and propagation mechanism of the overlapping zone cracking laser soluble formation of IN738LC superalloys [ J ] Journal of Alloys and Compounds,2018,749: 859-. Such a method of raising the substrate temperature to 700 ℃ or higher tends to cause coarsening of crystal grains due to an excessively high substrate temperature. Han et al (Quanquan Han, et al, Additive Manufacturing of high-strength crack-free Ni-based Hastelloy X super alloy J. Additive Manufacturing,2019,30: 100919) eliminate cracking of Hastelloy X nickel-based superalloy by adding nano TiC. Chinese patent (CN108941560B) discloses a method for eliminating laser additive manufacturing cracks of Ren 104 nickel-based superalloy, and proposes a scheme of eliminating cracks inside a formed part by designing laser forming parameters and a partition scanning strategy and combining stress relief annealing and Spark Plasma Sintering (SPS) treatment, and inhibiting the growth of crystal grains in the sintering process. Chinese patent (CN108994304B) discloses a method for eliminating metal material additive manufacturing cracks and improving mechanical properties, which adopts stress relief annealing with specific parameters and SPS treatment with specific parameters in sequence, thereby not only eliminating the cracks of products, but also greatly improving the mechanical properties. All the above patents are to eliminate cracks of 3D printed products by post-processing. Chinese patent (CN104988355A) discloses a method for reducing the hot cracking tendency of nickel-base superalloy powder materials for printing by adding large amounts of Hf and/or B elements to solve the problem of hot cracking defects. However, the above method cannot suppress the problems of cracks and the like generated during the printing and/or the subsequent heat treatment of the 3D printed nickel-base superalloy articles.
The invention firstly proposes that rare earth microalloying is carried out through a proper amount of rare earth, the 3D printing cracking sensitivity of the gamma '-phase precipitation strengthening nickel-based superalloy is reduced, the 3D printing process window of the gamma' -phase precipitation strengthening nickel-based superalloy is widened, the generation of 3D printing and subsequent heat treatment cracks is inhibited, and the rare earth microalloying method is suitable for additive manufacturing of workpieces in various shapes.
Disclosure of Invention
The invention provides a method for eliminating cracks of a 3D printing nickel-based high-temperature alloy, aiming at the problem that cracks are easily generated in the 3D printing of a gamma ' phase precipitation strengthening nickel-based high-temperature alloy, the rare earth microalloying is carried out through a proper amount of rare earth for the first time, the 3D printing cracking sensitivity of the gamma ' phase precipitation strengthening nickel-based high-temperature alloy is reduced, the 3D printing process window of the gamma ' phase precipitation strengthening nickel-based high-temperature alloy is widened, the generation of 3D printing and subsequent heat treatment cracks is inhibited, and the strength and the plasticity of a formed part are greatly improved.
The invention relates to a method for eliminating cracks of a 3D printing nickel-based superalloy, wherein the compact nickel-based superalloy is prepared by 3D printing by taking nickel-based superalloy powder as a raw material; the nickel-based superalloy comprises the following components in percentage by mass:
Co：14-23％；
Cr：11-15％；
Al：2-5％；
Ti：3-6％；
Mo：2.7-5％；
W：0.5-3％；
Ta：0.5-4％；
Nb：0.25-3％；
Zr：0.02-0.06％；
B：0.01-0.05％；
C：0.0015-0.1％；
RE：0.05-0.18wt％；
or taking other non-weldable nickel-based high-temperature alloy as a matrix, and adding 0.05-0.18 wt% of RE into the matrix;
the other non-weldable nickel-base superalloy is selected from one of IN738LC, CM247LC, CMSX-4, Ren 142 and Hastelloy X; or one of IN718 and IN625 nickel-base high-temperature alloys is taken as a matrix, and 0.05-0.18 wt% of RE is added into the matrix;
the parameters of the 3D printing are as follows: the laser power is 150-300W, the laser scanning speed is 500-1100 mm/s, the spot diameter is 70-110 μm, the laser scanning interval is 60-120 μm, the powder spreading layer thickness is 30-50 μm, and the laser scanning direction between the forming layers rotates 45-90 degrees, preferably 67 degrees;
and the RE is at least one selected from Sc, Y, La, Ce and Er.
The invention discloses a method for eliminating cracks of a 3D printing nickel-based superalloy, which comprises the following components in percentage by mass:
Co：20.6％；
Cr：13％；
Al：3.4％；
Ti：3.9％；
Mo：3.8％；
W：2.1％；
Ta：2.4％；
Nb：0.9％；
Zr：0.05％；
B：0.03％；
C：0.04％；
RE：0.06-0.18wt％；
the balance being Ni.
The invention relates to a method for eliminating cracks of a 3D printing nickel-based superalloy, wherein RE is Sc; or RE is the mixture of Sc and at least one of Y, La, Ce and Er.
The invention discloses a method for eliminating cracks of a 3D printing nickel-based superalloy, which comprises the following steps:
the method comprises the following steps: vacuum melting
Taking raw materials according to the distribution of a design group, filling the raw materials into a crucible of an atomization powder making furnace, and carrying out vacuum melting by adopting induction heating under the vacuum degree lower than 0.1 Pa;
step two: degassing of gases
After the raw materials are melted, vacuum degassing is carried out for 10min to 20 min;
step three: refining
Filling high-purity inert gas into the atomization powder making furnace to 0.1-0.11MPa, and preserving the temperature of the molten master alloy melt within the temperature range of 1600-1650 ℃ for 10-15 min;
step four: atomization
The molten master alloy solution flows down through a flow guide pipe at the flow rate of 3.5 kg/min-5 kg/min, the metal liquid flow is crushed into fine liquid drops by high-pressure and high-purity inert gas of 3 MPa-5 MPa, and the liquid drops are cooled and solidified to form spherical powder and enter a powder collecting tank;
step five: sieving
Fully cooling the powder, performing air classification and ultrasonic vibration screening under the protection of inert gas to obtain spherical nickel-based high-temperature alloy powder with the medium powder particle size of 53-106 microns and the fine powder particle size of 15-53 microns, and performing vacuum packaging;
the inert gas is helium gas, argon gas or argon-helium mixed gas, the purity is 99.99 wt%, and the oxygen content is less than 0.0001 wt%;
the oxygen content of the obtained nickel-based superalloy powder is less than or equal to 0.0126 wt%, and the sulfur content is less than or equal to 0.0056 wt%. In industrial application, the nickel-based superalloy powder can also be prepared by adopting a plasma rotary electrode atomization method.
The invention discloses a method for eliminating cracks of 3D printing nickel-based superalloy, wherein the oxygen content of nickel-based superalloy powder is less than or equal to 0.01 wt%, and the sulfur content of nickel-based superalloy powder is less than or equal to 0.004 wt%.
The invention discloses a method for eliminating cracks of 3D printing nickel-based superalloy, wherein the nickel-based superalloy powder is tested for fluidity through a pore size of 50g/2.5mm, and the result is 15-25 s. The optimized time can be 15.5-16 s.
The invention discloses a method for eliminating cracks of 3D printing nickel-based superalloy, wherein the 3D printing is one of Selective Laser Melting (SLM), Electron Beam Melting (EBM) or coaxial powder feeding laser forming (LENS).
The invention discloses a method for eliminating cracks of 3D printing nickel-based superalloy, wherein the 3D printing parameters are as follows: the laser power is 150-300W, the laser scanning speed is 500-1100 mm/s, the spot diameter is 70-110 μm, the laser scanning interval is 60-120 μm, the powder spreading layer thickness is 30-50 μm, and the laser scanning direction between the forming layers rotates 45-90 degrees, preferably 67 degrees.
The invention relates to a method for eliminating cracks of a 3D printing nickel-based high-temperature alloy, which is characterized in that after 3D printing is finished, stress relief annealing is carried out for 0.5-3 hours at 450-650 ℃ in vacuum or inert gas atmosphere to obtain a workpiece.
According to the method for eliminating cracks of the 3D printing nickel-based high-temperature alloy, the compactness of a workpiece is 99.3% -99.5%, the room-temperature yield strength is 918-935 MPa, the tensile strength is 1120-1256 MPa, and the elongation is 12.5-14.5%.
The invention relates to a method for eliminating cracks of a 3D printing nickel-based superalloy, and the prepared alloy powder is supersaturated solid solution alloy powder with uniform components. The alloy powder is prepared by atomization and rapid solidification, and the added elements can exceed the equilibrium solid solution limit to form a supersaturated solid solution; no alloy element segregation. The 3D printing fast solidification formed workpiece has fine dendritic crystal structure and element segregation limited in submicron level. The trace rare earth elements inhibit the formation of low-melting-point phases, eliminate low-melting-point compounds formed by B, Zr and the like, narrow the range of solidification temperature, and reduce the cracking sensitivity of the gamma' -phase precipitation-strengthened nickel-based superalloy, thereby inhibiting the formation of 3D printing cracks.
The invention has the advantages and positive effects that:
(1) aiming at the problems that the gamma '-phase precipitation strengthening nickel-based high-temperature alloy with high Al and Ti contents is poor in welding performance and easy to crack in the 3D printing process, rare earth microalloying is carried out by proper amount of rare earth in combination with optimization of 3D printing parameters, cracking sensitivity of the gamma' -phase precipitation strengthening nickel-based high-temperature alloy is reduced, 3D printing cracks are eliminated, and strength and plasticity of a formed part are greatly improved;
(2) according to the invention, the supersaturated solid solution high-temperature alloy powder is prepared by adding trace amounts of Sc, Y, La, Ce and Er or mixing and adding, and then adopting inert gas atomization or plasma rotating electrode atomization for rapid solidification, the obtained powder has high sphericity and narrow particle size distribution range, and meanwhile, impurity elements such as oxygen, sulfur and the like are remarkably reduced, so that the supersaturated solid solution high-temperature alloy powder is suitable for a 3D printing technology;
(3) the cracking sensitivity of the gamma '-phase precipitation strengthening nickel-based superalloy in the 3D printing rapid melting and solidification process is reduced, and the 3D printing process window of the gamma' -phase precipitation strengthening nickel-based superalloy is widened;
(4) according to the invention, through the synergistic effect of rare earth microalloying and parameter optimization, the quality of a 3D printing workpiece is ensured, the generation and accumulation of residual stress in the 3D printing process are also controlled, and the generation of cracks in the 3D printing process is effectively inhibited;
(5) according to the invention, through inert gas atomization or plasma rotating electrode atomization powder preparation and 3D printing rapid forming, element segregation is limited to a submicron level, and the uniformity of components and tissues is improved;
(6) the preparation method reduces the component segregation of the powder and the 3D printing workpiece, greatly reduces the 3D printing thermal stress accumulation, inhibits the generation of solidification cracks and deformation, and improves the quality and mechanical property of the workpiece;
(7) according to the invention, rare earth microalloying is carried out through a proper amount of rare earth, so that 3D printing cracks of the gamma' -phase precipitation strengthening nickel-based superalloy are eliminated, the strength and plasticity of a formed part are greatly improved, and the formation of cracks in subsequent processing processes such as storage cracking and subsequent heat treatment cracking among working procedures is effectively prevented;
(8) the invention effectively eliminates 3D printing cracks of the gamma '-phase precipitation strengthening nickel-based high-temperature alloy with high Al and Ti contents, the gamma' -phase precipitation strengthening nickel-based high-temperature alloy Ren 104 prepared by the method has no cracks in a formed part, the density is over 99.4 percent, the room-temperature yield strength and the tensile strength respectively reach 935MPa and 1256MPa, and the elongation is over 14.0 percent.
In summary, the invention aims at the problems that the gamma '-phase precipitation strengthening nickel-based high-temperature alloy with high Al and Ti contents is poor in welding performance and easy to crack in the 3D printing process, microalloying is carried out by adding a proper amount of rare earth Sc, Y, La, Ce and Er or carrying out mixed addition, and then supersaturated solid solution high-temperature alloy powder is prepared by inert gas atomization or plasma rotating electrode atomization and rapid solidification, so that the 3D printing cracking sensitivity of the gamma' -phase precipitation strengthening nickel-based high-temperature alloy is reduced, the 3D printing process window of the gamma '-phase precipitation strengthening nickel-based high-temperature alloy is widened, the crack of the 3D printing gamma' -phase precipitation strengthening nickel-based high-temperature alloy is eliminated by combining parameter optimization, the strength and the plasticity of a formed piece are greatly improved, and the crack formation in the subsequent processing processes such as storage cracking in the working procedures.
Drawings
Fig. 1 is a schematic diagram of scanning strategies used in examples one, two and three and comparative examples one, two and three.
FIG. 2 is an image of the metallographic structure of a rare earth Sc microalloyed Ren 104 alloy prepared by SLM of example.
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the microstructure of the rare earth Y microalloyed Ren 104 alloy prepared by the SLM of example two.
FIG. 4 is an SEM photograph of the microstructure of a Sc and Y mixed rare earth microalloyed Ren 104 alloy prepared by the three SLMs in the example.
FIG. 5 is an SEM photograph of the microstructure of a Ren 104 alloy prepared by a four-SLM according to an example
FIG. 6 is an SEM photograph of the microstructure of a Ren 104 alloy prepared by a five-SLM example
FIG. 7 is an SEM photograph of the microstructure of a rare earth Sc microalloyed Ren 104 alloy prepared by comparative example one SLM.
FIG. 8 is an SEM image of the microstructure of a Ren 104 alloy prepared by an SLM according to the second comparative example.
FIG. 9 is an SEM image of the microstructure of a Ren 104 alloy prepared by a third SLM comparative example.
Detailed Description
The invention is further illustrated with reference to the following figures and specific examples.
The first embodiment is as follows:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and rare earth Sc elements with the mass fraction of 0.08 percent are added, and the weight percentage of the alloy is as follows:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-0.08 Sc-the balance being Ni, preparing the master alloy of the alloy, then adopting argon atomization rapid solidification to prepare powder, and screening out alloy powder with the particle size of 15-53 mu m by airflow classification and ultrasonic vibration powder screening.
The method is used for SLM forming of the Ren 104 nickel-based high-temperature alloy, firstly, screened Ren 104 nickel-based high-temperature alloy powder is dried in a vacuum drying box at 120 ℃ for 4 hours, a substrate is heated to 170 ℃, the dried powder is filled into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 450 ℃ for 3h in a vacuum atmosphere.
The optimized SLM process parameters are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 250W, the laser scanning speed is 900mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 40 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results in fig. 2 show that no cracks were observed in the printed forms.
The density of the prepared sample is 99.44%, the yield strength and the tensile strength are 918MPa and 1236MPa respectively, and the elongation is 14.0%.
Example two:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and rare earth Y element with the mass fraction of 0.12 percent is added, and the weight percentage of the alloy is as follows:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-0.12Y and the balance of Ni, preparing the master alloy of the alloy, atomizing by helium gas, rapidly solidifying and preparing powder, and screening out alloy powder with the particle size of 15-53 mu m by airflow classification and ultrasonic vibration sieve powder.
The method is used for SLM forming of the Ren 104 nickel-based high-temperature alloy, firstly, screened Ren 104 nickel-based high-temperature alloy powder is dried in a vacuum drying box at 120 ℃ for 4 hours, a substrate is heated to 170 ℃, the dried powder is filled into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 500 ℃ for 2h under argon.
The optimized SLM process parameters are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 250W, the laser scanning speed is 900mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 40 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results in fig. 3 show that no cracks were observed in the printed forms.
The density of the prepared sample is 99.39%, the yield strength and the tensile strength are 930MPa and 1224MPa respectively, and the elongation is 12.8%.
Example three:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and the rare earth Sc element with the mass fraction of 0.06 percent and the rare earth Y element with the mass fraction of 0.08 percent are added, and the alloy comprises the following components in percentage by weight:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-0.06 Sc-0.08Y, and the balance being Ni, preparing the master alloy of the alloy, then adopting argon atomization rapid solidification to prepare powder, and screening out alloy powder with the particle size of 15-53 mu m through airflow classification and ultrasonic vibration screening.
The method is used for SLM forming of the Ren 104 nickel-based high-temperature alloy, firstly, screened Ren 104 nickel-based high-temperature alloy powder is dried in a vacuum drying box at 120 ℃ for 4 hours, a substrate is heated to 170 ℃, the dried powder is filled into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 450 ℃ for 3h in a vacuum atmosphere.
The optimized SLM process parameters are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 250W, the laser scanning speed is 900mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 40 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results of fig. 4 show that no cracks were observed in the printed forms.
The density of the prepared sample is 99.46%, the yield strength and the tensile strength are 935MPa and 1256MPa respectively, and the elongation is 14.3%.
Example four:
the alloy powder prepared in the first example is used as a raw material, and 3D printing process parameters adopted in the first example of Chinese patent (CN108941560A) are adopted to prepare a Ren 104 alloy block. The specific parameters of the SLM process are as follows:
the laser power is 250W, the diameter of a light spot is 0.12mm, the scanning speed is 500mm/s, the scanning interval is 0.12mm, and the thickness of a powder layer is 0.03 mm.
The scanning strategy used by the SLM is a stripe scanning strategy, as shown in fig. 1, which is a schematic diagram of the stripe scanning strategy, a mode of scanning layer by layer from bottom to top is adopted, the laser scanning direction between adjacent layers is rotated by 67 °, the size of a stripe is 7mm, and the lap joint between the stripes is 0.11mm, so as to reduce the superposition of residual stress in the printing process.
FIG. 5 is an SEM image of the microstructure of the Ren 104 alloy, the structure of the formed piece is dense, and no cracks are observed. Through detection, the density of the prepared Ren 104 alloy is 99.32 percent, which is superior to that of a formed piece with the density of 99.18 percent, which is prepared by adopting an SLM in the first embodiment of Chinese patent (CN 108941560A); the yield strength at room temperature is 926MPa, the tensile strength is 1242MPa, and the elongation is 14.2%.
The molded article was subjected to the same stress relief annealing and SPS treatment as in the example of chinese patent (CN 108941560A).
The stress relief annealing parameters are as follows: keeping the temperature at 420 ℃ for 90min, and then cooling along with the furnace.
The discharge plasma sintering parameters are as follows: the graphite grinding tool with the diameter of 40mm has the heating rate of 60 ℃/min, the cooling rate of 60 ℃/min, the sintering pressure of 45MPa, the sintering temperature of 1020 ℃ and the heat preservation time of 15 min.
Through detection, the compactness of the finally prepared Ren é 104 alloy is 99.62%, the yield strength at room temperature is 1038MPa, the tensile strength is 1394MPa, and the elongation is 14.5%, which is superior to the mechanical properties of a formed piece prepared by adopting SLM (SLM), adopting stress-relief annealing to relieve residual stress and adopting SPS to eliminate cracks in the first embodiment of Chinese patent (CN 108941560A). The room-temperature mechanical properties of the formed piece prepared in the first embodiment of the Chinese patent (CN108941560A) are 987MPa and 1376MPa respectively.
Example five:
the alloy powder prepared in the first example is used as a raw material, and 3D printing process parameters adopted in the first comparative example of Chinese patent (CN108941560B) are adopted to prepare a Ren 104 alloy block. The specific parameters of the SLM process are as follows:
the laser power is 225W, the diameter of a light spot is 0.12mm, the scanning speed is 600mm/s, the scanning interval is 0.11mm, and the thickness of a powder layer is 0.03 mm. (without using a partitioning strategy)
FIG. 6 is a SEM image of the microstructure of the Ren 104 alloy, and the prepared sample is compact in structure and no crack is observed. Through detection, the prepared Ren é 104 alloy has the compactness of 99.2%, the room-temperature yield strength of 913MPa, the tensile strength of 1247MPa and the elongation of 13.3%.
The printed forming piece of the comparative example I of Chinese patent (CN108941560B) has densities of 98.12% and 99.02% before and after post-treatment (stress relief annealing + SPS), and room-temperature mechanical properties of 751MPa and 916MPa respectively.
Compared with the density and the mechanical property of the comparative example I in the Chinese patent (CN108941560B), the invention adopts the 3D printing process parameters of the comparative example I which has the most serious cracking and the worst product performance in the Chinese patent (CN108941560B), and can also prepare the product with high quality, no crack and excellent mechanical property. The alloy and the powder prepared by the method can widen the 3D printing process window.
Comparative example one:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and rare earth Sc elements with the mass fraction of 0.08 percent are added, and the weight percentage of the alloy is as follows:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-0.08 Sc-the balance being Ni, preparing the master alloy of the alloy, then adopting argon atomization rapid solidification to prepare powder, and screening out alloy powder with the particle size of 15-53 mu m by airflow classification and ultrasonic vibration powder screening.
The screened Ren 104 nickel-based high-temperature alloy used for SLM forming is dried for 4 hours in a vacuum drying box at 120 ℃, the substrate is heated to 170 ℃, the dried powder is loaded into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 450 ℃ for 3h in a vacuum atmosphere.
The SLM process parameters after optimization are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 400W, the laser scanning speed is 1200mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 30 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results in FIG. 7 show that a small number of cracks were observed in the printed article, the crack length was about 150 μm, and the crack density was 1.4. + -. 0.5mm/mm2。
The density of the prepared sample is 90.12%, the yield strength and the tensile strength are 893MPa and 1085MPa respectively, and the elongation is 10.4%.
Comparative example two:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and rare earth elements are not added, and the alloy comprises the following components in percentage by weight:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-the balance being Ni, preparing the master alloy of the alloy, then adopting argon atomization to rapidly solidify and prepare powder, and screening out 15-53 mu m of alloy powder through airflow classification and ultrasonic vibration powder screening.
The method is used for SLM forming of the Ren 104 nickel-based high-temperature alloy, firstly, screened Ren 104 nickel-based high-temperature alloy powder is dried in a vacuum drying box at 120 ℃ for 4 hours, a substrate is heated to 170 ℃, the dried powder is filled into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 450 ℃ for 3h in a vacuum atmosphere.
The optimized SLM process parameters are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 250W, the laser scanning speed is 900mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 40 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results in FIG. 8 show that more cracks were observed in the printed forms, the crack length was 300 μm and the crack density was 2.5. + -. 0.6mm/mm2。
The density of the prepared sample is 98.9%, the yield strength and the tensile strength are 786MPa and 918MPa respectively, and the elongation is 3.9%.
Comparative example three:
the method is used for the following Ren 104 nickel-based high-temperature alloy, and rare earth elements are not added, and the alloy comprises the following components in percentage by weight:
20.6 Co-13 Cr-3.4 Al-3.9 Ti-3.8 Mo-2.1W-2.4 Ta-0.9 Nb-0.05 Zr-0.03B-0.04C-the balance being Ni, preparing the master alloy of the alloy, then adopting argon atomization to rapidly solidify and prepare powder, and screening out 15-53 mu m of alloy powder through airflow classification and ultrasonic vibration powder screening.
The method is used for SLM forming of the Ren 104 nickel-based high-temperature alloy, firstly, screened Ren 104 nickel-based high-temperature alloy powder is dried in a vacuum drying box at 120 ℃ for 4 hours, a substrate is heated to 170 ℃, the dried powder is filled into a powder supply cylinder and spread, and argon or nitrogen is introduced into a working cavity until the oxygen content is lower than 100 ppm. And then, entering a printing program, and continuously repeating the steps of powder paving and laser powder scanning until the printing is finished to obtain the Ren 104 nickel-based superalloy block. The printed block together with the substrate was then stress relieved annealed at 450 ℃ for 3h in an argon atmosphere.
The SLM process parameters after optimization are as follows: the diameter of a laser spot is 70 micrometers, the laser power is 400W, the laser scanning speed is 1200mm/s, the laser scanning interval is 90 micrometers, the powder spreading layer thickness is 30 micrometers, a stripe scanning strategy is adopted, the laser scanning direction between layers rotates 67 degrees, and the forming strategy is shown in figure 1.
The results in FIG. 9 show that significant cracks were observed in the printed forms with crack lengths approaching 500 μm and crack densities of 3.7. + -. 0.8mm/mm2。
The density of the prepared sample is 98.9%, the yield strength and the tensile strength are 708MPa and 875MPa respectively, and the elongation is 2.6%.
Claims (10)
1. A method for eliminating cracks of 3D printing nickel-based superalloy is characterized by comprising the following steps: the compact nickel-based superalloy is prepared by 3D printing by taking nickel-based superalloy powder as a raw material; the nickel-based superalloy comprises the following components in percentage by mass:
Co：14-23％；
Cr：11-15％；
Al：2-5％；
Ti：3-6％；
Mo：2.7-5％；
W：0.5-3％；
Ta：0.5-4％；
Nb：0.25-3％；
Zr：0.02-0.06％；
B：0.01-0.05％；
C：0.0015-0.1％；
RE：0.05-0.18wt％；
the balance being Ni;
or taking other non-weldable nickel-based high-temperature alloy as a matrix, and adding 0.05-0.18 wt% of RE into the matrix;
the other non-weldable nickel-base superalloy is selected from one of IN738LC, CM247LC, CMSX-4, Ren 142 and Hastelloy X; or one of IN718 and IN625 nickel-base high-temperature alloys is taken as a matrix, and 0.05-0.18 wt% of RE is added into the matrix;
the parameters of the 3D printing are as follows: the laser power is 150-300W, the laser scanning speed is 500-1100 mm/s, the spot diameter is 70-110 μm, the laser scanning interval is 60-120 μm, the powder spreading layer thickness is 30-50 μm, and the laser scanning direction between the forming layers rotates by 45-90 degrees;
and the RE is at least one selected from Sc, Y, La, Ce and Er.
2. The method for eliminating cracks in 3D printed nickel-base superalloy according to claim 1, wherein: the nickel-based superalloy comprises the following components in percentage by mass:
Co：20.6％；
Cr：13％；
Al：3.4％；
Ti：3.9％；
Mo：3.8％；
W：2.1％；
Ta：2.4％；
Nb：0.9％；
Zr：0.05％；
B：0.03％；
C：0.04％；
RE：0.06-0.18wt％；
the balance being Ni.
3. The method for eliminating cracks in 3D printed nickel-base superalloy according to claim 1, wherein: RE is Sc; or RE is the mixture of Sc and at least one of Y, La, Ce and Er.
4. The method for 3D printing nickel-base superalloy crack mitigation according to claim 1, wherein; the nickel-based superalloy powder is prepared by the following steps:
the method comprises the following steps: vacuum melting
Distributing and taking raw materials according to a design group, filling the raw materials into a crucible of an atomization powder making furnace, and carrying out vacuum melting by adopting induction heating under the vacuum degree lower than 0.1 Pa;
step two: degassing of gases
After the raw materials are melted, vacuum degassing is carried out for 10min to 20 min;
step three: refining
Filling high-purity inert gas into the atomization powder making furnace to 0.1-0.11MPa, and preserving the temperature of the molten master alloy melt within the temperature range of 1600-1650 ℃ for 10-15 min;
step four: atomization
The molten master alloy solution flows down through a flow guide pipe at the flow rate of 3.5 kg/min-5 kg/min, the metal liquid flow is crushed into fine liquid drops by high-pressure and high-purity inert gas of 3 MPa-5 MPa, and the liquid drops are cooled and solidified to form spherical powder and enter a powder collecting tank;
step five: sieving
Fully cooling the powder, performing air classification and ultrasonic vibration screening under the protection of inert gas to obtain spherical nickel-based high-temperature alloy powder with the medium powder particle size of 53-106 microns and the fine powder particle size of 15-53 microns, and performing vacuum packaging;
the inert gas is helium gas, argon gas or argon-helium mixed gas, the purity is 99.99 wt%, and the oxygen content is less than 0.0001 wt%;
the oxygen content of the obtained nickel-based superalloy powder is less than or equal to 0.0126 wt%, and the sulfur content is less than or equal to 0.0056 wt%.
5. The method for eliminating cracks in 3D printing nickel-based superalloy according to claim 4, wherein the method comprises the following steps: the nickel-based superalloy powder has an oxygen content of 0.01 wt% or less and a sulfur content of 0.004 wt% or less.
6. The method for eliminating cracks in 3D printing nickel-based superalloy according to claim 4, wherein the method comprises the following steps: the nickel-base superalloy powder has a flowability measured by a 50g/2.5mm pore size, and the result is 15-25 s. The optimized time can be 15.5-16 s.
7. The method for eliminating cracks in 3D printing nickel-based superalloy according to claim 4, wherein the method comprises the following steps: the 3D printing is selected area laser melting (SLM), or Electron Beam Melting (EBM), or coaxial powder laser forming (LENS).
8. The method for eliminating cracks in 3D printed nickel-base superalloy according to claim 1, wherein: the parameters of the 3D printing are as follows: the laser power is 150-300W, the laser scanning speed is 500-1100 mm/s, the spot diameter is 70-110 μm, the laser scanning interval is 60-120 μm, the powder spreading layer thickness is 30-50 μm, and the laser scanning direction between the forming layers rotates 45-90 degrees, preferably 67 degrees.
9. The method for eliminating cracks in 3D printed nickel-base superalloy according to claim 1, wherein: and after the 3D printing is finished, performing stress relief annealing at 450-650 ℃ for 0.5-3 h in vacuum or inert gas atmosphere to obtain a workpiece.
10. The method for eliminating cracks in 3D printed nickel-base superalloy according to claim 9, wherein: the density of the workpiece is 99.3% -99.5%, the room-temperature yield strength is 918-935 MPa, the tensile strength is 1120-1256 MPa, and the elongation is 12.5-14.5%.
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| CN115121811B (en) * | 2022-06-29 | 2024-03-12 | 中国航发动力股份有限公司 | Welding method of powder-spreading 3D printer casing and engine casing |
| CN115609009A (en) * | 2022-09-20 | 2023-01-17 | 天津大学 | Method for eliminating printing cracks of solid solution strengthened nickel-based superalloy in additive manufacturing |
| CN117001014A (en) * | 2023-10-07 | 2023-11-07 | 苏州倍丰智能科技有限公司 | Rapid development method of cracking-free metal material for 3D printing |
| CN117001014B (en) * | 2023-10-07 | 2024-01-05 | 苏州倍丰智能科技有限公司 | Rapid development method of cracking-free metal material for 3D printing |
| CN117245084A (en) * | 2023-11-20 | 2023-12-19 | 中航迈特增材科技(北京)有限公司 | High-strength temperature-resistant aluminum alloy powder for 3D printing and preparation method and application thereof |
| CN117245084B (en) * | 2023-11-20 | 2024-01-16 | 中航迈特增材科技(北京)有限公司 | High-strength temperature-resistant aluminum alloy powder for 3D printing and preparation method and application thereof |
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| CN112011713B (en) | 2021-11-23 |
| WO2022041252A1 (en) | 2022-03-03 |
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