WO2022041252A1 - 一种消除3d打印镍基高温合金裂纹的方法 - Google Patents

一种消除3d打印镍基高温合金裂纹的方法 Download PDF

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Publication number
WO2022041252A1
WO2022041252A1 PCT/CN2020/112689 CN2020112689W WO2022041252A1 WO 2022041252 A1 WO2022041252 A1 WO 2022041252A1 CN 2020112689 W CN2020112689 W CN 2020112689W WO 2022041252 A1 WO2022041252 A1 WO 2022041252A1
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nickel
printing
based superalloy
powder
cracks
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French (fr)
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刘祖铭
魏冰
农必重
吕学谦
任亚科
曹镔
艾永康
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Central South University
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • 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
    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • 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
    • B22F2009/0824—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 with a specific atomising fluid
    • 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
    • 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
    • B22F2009/0848—Melting process before atomisation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • the invention provides a method for eliminating cracks in 3D printing nickel-based superalloys, belonging to the technical field of superalloy additive manufacturing.
  • the ⁇ ' phase precipitation strengthening nickel-based superalloy is one of the major breakthroughs in the field of material science. Its strengthening phase is an ordered and coherent intermetallic compound such as ⁇ '-Ni 3 (Al, Ti), usually by casting and deformation processing Or powder forming technology, widely used in advanced aero-engines. However, these techniques cannot directly form parts with complex shapes. 3D printing, or additive manufacturing technology, can directly generate three-dimensional parts with near-net shape size layer by layer from three-dimensional computer-aided design data. It has unique advantages in the preparation of high-performance components with complex shapes. It has been used in titanium alloys, aluminum Alloys, stainless steel and nickel-based alloys and other materials are used.
  • the large temperature gradient, fast cooling rate and repeated remelting in the 3D printing forming process result in high residual stress in the formed parts, and are prone to deformation and cracking, which brings challenges to 3D printing high-quality parts, especially high Al and Ti content.
  • the ⁇ ' phase precipitation strengthens nickel-based superalloys, poor welding performance, and cracking have become the most prominent problems in 3D printing of such alloys.
  • the above patents are all post-processing to eliminate cracks in 3D printed parts.
  • the Chinese patent (CN104988355A) discloses a method for reducing the hot cracking tendency of nickel-based superalloy powder materials for printing, which solves the problem of hot cracking defects by adding a large amount of Hf and/or B elements.
  • the above methods cannot suppress the problems such as cracks generated during printing and/or subsequent heat treatment of 3D printed nickel-based superalloy parts.
  • the present invention proposes for the first time that rare earth microalloying by appropriate amount of rare earth can reduce the cracking sensitivity of ⁇ ' phase precipitation-strengthened nickel-based superalloy 3D printing, widen the 3D printing process window of ⁇ ' phase precipitation-strengthened nickel-based superalloy, and inhibit 3D printing and subsequent
  • the generation of heat treatment cracks is suitable for additive manufacturing of various shapes of parts.
  • the invention proposes a method for eliminating cracks in 3D printing nickel-based superalloys.
  • it is first proposed to carry out rare-earth microalloying by appropriate amount of rare earth to reduce ⁇ '-phase precipitation strengthening.
  • Nickel-based superalloy 3D printing cracking sensitivity widening the ⁇ ' phase precipitation strengthening nickel-based superalloy 3D printing process window, inhibiting 3D printing and subsequent heat treatment cracks, and greatly improving the strength and plasticity of formed parts.
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy.
  • the dense nickel-based superalloy is prepared by 3D printing using nickel-based superalloy powder as raw material; the nickel-based superalloy is calculated in mass percentage, including the following said components.
  • the other non-weldable nickel-based superalloys are selected from one of IN738LC, CM247LC, CMSX-4, René 142, and Hastelloy X; or one of IN718 and IN625 nickel-based superalloys is used as the matrix, and 0.05 -0.18wt% RE.
  • the parameters of the 3D printing are: the laser power is 150-300W, the laser scanning rate is 500-1100mm/s, the spot diameter is 70-110 ⁇ m, the laser scanning distance is 60-120 ⁇ m, the powder layer thickness is 30-50 ⁇ m, and the forming layer is 30-50 ⁇ m thick.
  • the laser scanning direction is rotated by 45°-90°, preferably 67°.
  • the RE is selected from at least one of Sc, Y, La, Ce, and Er.
  • the present invention is a method for eliminating cracks in a 3D printing nickel-based superalloy, where the nickel-based superalloy, in terms of mass percentage, includes the following components ⁇ m.
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy, where RE is Sc; or RE is a mixture of Sc and at least one of Y, La, Ce, and Er.
  • the present invention is a method for eliminating cracks in a 3D printing nickel-based superalloy, wherein the nickel-based superalloy powder is prepared through the following steps.
  • Step 1 Vacuum smelting.
  • the raw materials are dispensed according to the design composition, and the raw materials are put into the crucible of the atomizing pulverizing furnace, and the vacuum melting is carried out by induction heating under the vacuum degree of less than 0.1Pa.
  • Step 2 Degassing.
  • vacuum degassing is performed for 10 to 20 minutes.
  • Step 3 Refinement.
  • the molten mother alloy melt is flowed down through the guide tube at a flow rate of 3.5kg/min ⁇ 5kg/min, and the metal liquid flow is broken into fine droplets with a high-pressure, high-purity inert gas of 3MPa ⁇ 5MPa, and the droplets are cooled and cooled. It solidifies to form spherical powder, which goes into the powder collection tank.
  • the inert gas should be helium, argon, or a mixed gas of argon and helium, with a purity of 99.99 wt %, wherein the oxygen content is less than 0.0001 wt %.
  • nickel-based superalloy powder The oxygen content of the obtained nickel-based superalloy powder is less than or equal to 0.0126wt%, and the sulfur content is less than or equal to 0.0056wt%.
  • nickel-based superalloy powder can also be prepared by plasma rotating electrode atomization method.
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy, wherein the oxygen content of the nickel-based superalloy powder is less than or equal to 0.01wt%, and the sulfur content is less than or equal to 0.004wt%.
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy.
  • the nickel-based superalloy powder is tested for fluidity through 50g/2.5mm aperture, and the result is 15-25 s. Optimized for 15.5-16 s.
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy, and the 3D printing is one of selective laser melting (SLM), electron beam melting (EBM), or coaxial powder feeding laser forming (LENS).
  • SLM selective laser melting
  • EBM electron beam melting
  • LENS coaxial powder feeding laser forming
  • the present invention is a method for eliminating cracks in 3D printing nickel-based superalloy.
  • the parameters of the 3D printing are: laser power of 150-300 W, laser scanning rate of 500-1100 mm/s, spot diameter of 70-110 ⁇ m, and laser scanning spacing of 60 ⁇ 120 ⁇ m, the thickness of the powder layer is 30 to 50 ⁇ m, and the laser scanning direction between the forming layers is rotated by 45° to 90°, preferably 67°.
  • the invention provides a method for eliminating cracks in 3D printing nickel-based superalloy. After the 3D printing is completed, stress relief annealing at 450-650° C. for 0.5-3 hours is performed in a vacuum or an inert gas atmosphere to obtain a product.
  • the invention provides a method for eliminating cracks in 3D printing nickel-based superalloys.
  • the density of the parts is 99.3%-99.5%
  • the room temperature yield strength is 918-935MPa
  • the tensile strength is 1120-1256MPa
  • the elongation is 12.5-14.5 %.
  • the invention provides a method for eliminating cracks in 3D printing nickel-based superalloy, and the prepared alloy powder is supersaturated solid solution alloy powder with uniform composition.
  • 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; there is no segregation of alloy elements.
  • 3D-printed and rapidly solidified parts using this alloy powder have a fine dendritic structure, and the element segregation is limited to the sub-micron level.
  • Trace rare earth elements inhibit the formation of low melting point phases, eliminate low melting point compounds formed by B, Zr, etc., narrow the solidification temperature range, and reduce the cracking sensitivity of ⁇ ' phase precipitation-strengthened nickel-based superalloys, thereby inhibiting the formation of 3D printing cracks .
  • the present invention is aimed at the problem of ⁇ ' phase precipitation strengthening nickel-based superalloy with high Al and Ti content, poor welding performance, and easy cracking during 3D printing.
  • the rare earth microalloying and 3D printing parameters are optimized by a suitable amount of rare earth. It reduces the cracking sensitivity of ⁇ ' phase precipitation-strengthened nickel-based superalloys, eliminates 3D printing cracks, and greatly improves the strength and plasticity of formed parts.
  • supersaturated solid solution superalloy powder is prepared by adding trace amounts of Sc, Y, La, Ce, Er or mixed addition, followed by inert gas atomization or plasma rotating electrode atomization and rapid solidification, and the obtained powder has high sphericity and particle size.
  • the distribution range is narrow, and the impurity elements such as oxygen and sulfur are significantly reduced, which is suitable for 3D printing technology.
  • the present invention reduces the cracking sensitivity of the ⁇ ' phase precipitation strengthened nickel-based superalloy in the process of rapid melting and solidification of 3D printing, and widens the 3D printing process window of the ⁇ ' phase precipitation strengthened nickel-based superalloy.
  • the present invention not only ensures the quality of 3D printing parts, but also controls the generation and accumulation of residual stress in the 3D printing process, and effectively inhibits the generation of cracks in the 3D printing process. .
  • the preparation method of the present invention reduces the component segregation of powder and 3D printing parts, greatly reduces the accumulation of thermal stress in 3D printing, suppresses the generation of solidification cracks and deformation, and improves the quality and mechanical properties of the parts.
  • the present invention uses an appropriate amount of rare earth to microalloy rare earth, eliminates ⁇ ' phase precipitation strengthening nickel-based superalloy 3D printing cracks, greatly improves the strength and plasticity of formed parts, and effectively prevents subsequent processing such as storage cracking between processes and subsequent heat treatment cracking. crack formation during the process.
  • the present invention effectively eliminates the 3D printing cracks of the ⁇ ' phase precipitation-strengthened nickel-based superalloy with high Al and Ti content.
  • the ⁇ ' phase precipitation-strengthened nickel-based superalloy René104 prepared by this method has no cracks in the formed parts.
  • the density exceeds 99.4%
  • the room temperature yield strength and tensile strength reach 935MPa and 1256MPa, respectively, and the elongation exceeds 14.0%.
  • the present invention aims at the problems of ⁇ ' phase precipitation strengthening nickel-based superalloy with high Al and Ti content, poor welding performance and easy cracking during 3D printing.
  • Er or mixed addition for micro-alloying, followed by inert gas atomization or plasma rotating electrode atomization for rapid solidification to prepare supersaturated solid solution superalloy powder reducing the ⁇ ' phase precipitation strengthening nickel-based superalloy 3D printing crack sensitivity, widening ⁇ 'phase precipitation strengthened nickel-based superalloy 3D printing process window, combined with parameter optimization to eliminate 3D printing ⁇ ' phase precipitation strengthened nickel-based superalloy cracks, greatly improve the strength and plasticity of formed parts, and effectively prevent storage cracking between processes and subsequent heat treatment cracking Crack formation during subsequent processing.
  • FIG. 1 is a schematic diagram of scanning strategies adopted in Embodiments 1, 2, and 3 and Comparative Examples 1, 2, and 3.
  • FIG. 1 is a schematic diagram of scanning strategies adopted in Embodiments 1, 2, and 3 and Comparative Examples 1, 2, and 3.
  • FIG. 2 is a microstructure image of the rare earth Sc microalloyed René 104 alloy prepared by SLM in Example 1.
  • FIG. 2 is a microstructure image of the rare earth Sc microalloyed René 104 alloy prepared by SLM in Example 1.
  • Figure 3 is a scanning electron microscope (SEM) photograph of the microstructure of the rare earth Y microalloyed René 104 alloy prepared by SLM in Example 2.
  • FIG. 4 is an SEM photograph of the microstructure of the Sc, Y mixed rare earth microalloyed René 104 alloy prepared by SLM in Example 3.
  • FIG. 4 is an SEM photograph of the microstructure of the Sc, Y mixed rare earth microalloyed René 104 alloy prepared by SLM in Example 3.
  • Figure 5 is a SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Example 4.
  • FIG. 6 is an SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Example 5.
  • FIG. 6 is an SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Example 5.
  • Figure 7 is a SEM photograph of the microstructure of the rare earth Sc microalloyed René 104 alloy prepared by SLM in Comparative Example 1.
  • FIG. 8 is a SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Comparative Example 2.
  • FIG. 8 is a SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Comparative Example 2.
  • FIG. 9 is a SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Comparative Example 3.
  • FIG. 9 is a SEM photograph of the microstructure of the René 104 alloy prepared by SLM in Comparative Example 3.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy, and the mass fraction of rare earth Sc element is 0.08%, and the weight percentage of the alloy is 0.08%.
  • the present invention is used for SLM forming René104 nickel-based superalloy.
  • the sieved René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours. After the substrate is heated to 170° C., the dried powder is dried. Load into the powder supply cylinder and spread powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm. Then enter the printing process, and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained. Then, the printed block and the substrate were subjected to stress relief annealing at 450 °C for 3 h in a vacuum atmosphere.
  • the optimized SLM process parameters are: laser spot diameter 70 ⁇ m, laser power 250W, laser scanning rate 900mm/s, laser scanning spacing 90 ⁇ m, powder layer thickness 40 ⁇ m, using strip scanning strategy, laser scanning between layers The direction is rotated 67°, and the forming strategy is shown in Figure 1.
  • the density of the prepared sample is 99.44%, the yield strength and tensile strength are 918MPa and 1236MPa, respectively, and the elongation is 14.0%.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy, and the mass fraction of rare earth Y element is 0.12%, and the alloy weight percentage is 0.12%.
  • the present invention is used for SLM forming René104 nickel-based superalloy.
  • the sieved René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours. After the substrate is heated to 170° C., the dried powder is dried. Load into the powder supply cylinder and spread powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm. Then enter the printing process, and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained. Then, the printed block together with the substrate was subjected to stress relief annealing at 500 °C for 2 h in argon.
  • the optimized SLM process parameters are: laser spot diameter 70 ⁇ m, laser power 250W, laser scanning rate 900mm/s, laser scanning spacing 90 ⁇ m, powder layer thickness 40 ⁇ m, using strip scanning strategy, laser scanning between layers The direction is rotated 67°, and the forming strategy is shown in Figure 1.
  • the density of the prepared sample is 99.39%, the yield strength and tensile strength are 930MPa and 1224MPa, respectively, and the elongation is 12.8%.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy, and the mass fractions of 0.06% rare earth Sc element and 0.08% rare earth Y element are added, and the alloy weight percentage is .
  • the present invention is used for SLM forming René104 nickel-based superalloy.
  • the sieved René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours. After the substrate is heated to 170° C., the dried powder is dried. Load into the powder supply cylinder and spread powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm. Then enter the printing process, and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained. Then, the printed block and the substrate were subjected to stress relief annealing at 450 °C for 3 h in a vacuum atmosphere.
  • the optimized SLM process parameters are: laser spot diameter 70 ⁇ m, laser power 250W, laser scanning rate 900mm/s, laser scanning spacing 90 ⁇ m, powder layer thickness 40 ⁇ m, using strip scanning strategy, laser scanning between layers The direction is rotated 67°, and the forming strategy is shown in Figure 1.
  • the density of the prepared sample is 99.46%, the yield strength and tensile strength are 935MPa and 1256MPa, respectively, and the elongation is 14.3%.
  • the René 104 alloy bulk was prepared using the 3D printing process parameters used in Example 1 of the Chinese Patent (CN108941560A).
  • the specific parameters of the SLM process are:
  • the laser power is 250W
  • the spot diameter is 0.12mm
  • the scanning speed is 500mm/s
  • the scanning distance is 0.12mm
  • the thickness of the powder layer is 0.03mm.
  • the scanning strategy used by SLM is the strip scanning strategy.
  • Figure 1 shows the schematic diagram of the strip scanning strategy. The scanning method from bottom to top is adopted. The laser scanning direction between adjacent layers is rotated by 67°, and the strip size is 7mm. , the overlap between the strips is 0.11mm, the purpose is to reduce the superposition of residual stress during the printing process.
  • Figure 5 is an SEM photograph of the microstructure of the René 104 alloy.
  • the formed part has a dense structure and no cracks are observed.
  • the density of the prepared René104 alloy is 99.32%, which is better than that of the molded part with a density of 99.18% prepared by SLM in Example 1 of the Chinese Patent (CN108941560A).
  • the yield strength at room temperature is 926MPa and the tensile strength is 1242MPa. , the elongation is 14.2%.
  • the parameters of stress relief annealing are as follows: temperature is 420°C, holding time is 90min, and then cooling with the furnace.
  • spark plasma sintering are: a graphite abrasive tool with a diameter of 40 mm, a heating rate of 60 °C/min, a cooling rate of 60 °C/min, a sintering pressure of 45 MPa, a sintering temperature of 1020 °C, and a holding time of 15 minutes.
  • the final density of the prepared René104 alloy is 99.62%
  • the yield strength at room temperature is 1038MPa
  • the tensile strength is 1394MPa
  • the elongation is 14.5%, which is better than that of the Chinese patent (CN108941560A).
  • the room temperature mechanical properties of the formed parts prepared in Example 1 of the Chinese patent (CN108941560A) are 987 MPa and 1376 MPa, respectively.
  • the René104 alloy bulk was prepared by using the 3D printing process parameters used in Comparative Example 1 of the Chinese Patent (CN108941560B).
  • the specific parameters of the SLM process are:
  • the laser power is 225W
  • the spot diameter is 0.12mm
  • the scanning speed is 600mm/s
  • the scanning distance is 0.11mm
  • the thickness of the powder layer is 0.03mm. (without partition strategy).
  • Figure 6 is a SEM photograph of the microstructure of the René 104 alloy.
  • the structure of the prepared sample is dense and no cracks are observed. After testing, the density of the prepared René104 alloy is 99.2%, the yield strength at room temperature is 913MPa, the tensile strength is 1247MPa, and the elongation is 13.3%.
  • Chinese patent (CN108941560B) compares the printed parts of Example 1.
  • the density of the pre- and post-treatment (stress relief annealing + SPS) after post-treatment (stress relief annealing + SPS) is 98.12% and 99.02%, respectively.
  • the mechanical properties at room temperature are respectively 98.12% and 99.02%. 751MPa and 916MPa.
  • the present invention adopts the 3D printing process parameters of Comparative Example 1 with the most severe cracking and the worst part performance in the Chinese patent (CN108941560B), and can also produce high-quality 3D printing. High-quality, crack-free, and mechanically excellent parts. It shows that the alloy and powder prepared by the present invention can widen the 3D printing process window.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy, and the mass fraction of rare earth Sc element is 0.08%, and the weight percentage of the alloy is 0.08%.
  • the present invention is used for forming René104 nickel-based superalloy by SLM.
  • the screened René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours.
  • the dried powder is packed into Put it into the powder supply tank and spread the powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm.
  • enter the printing process and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained.
  • the printed block and the substrate were subjected to stress relief annealing at 450 °C for 3 h in a vacuum atmosphere.
  • the unoptimized SLM process parameters are: the laser spot diameter is 70 ⁇ m, the laser power is 400 W, the laser scanning rate is 1200 mm/s, the laser scanning spacing is 90 ⁇ m, and the thickness of the powder layer is 30 ⁇ m.
  • the scanning direction is rotated by 67°, and the forming strategy is shown in Figure 1.
  • Fig. 7 show that a small amount of cracks can be observed in the printed parts, the crack length is about 150 ⁇ m, and the crack density is 1.4 ⁇ 0.5 mm/mm 2 .
  • the density of the prepared sample is 90.12%, the yield strength and tensile strength are 893MPa and 1085MPa, respectively, and the elongation is 10.4%.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy without adding rare earth elements, and the weight percentage of the alloy is .
  • the present invention is used for SLM forming René104 nickel-based superalloy.
  • the sieved René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours. After the substrate is heated to 170° C., the dried powder is dried. Load into the powder supply cylinder and spread powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm. Then enter the printing process, and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained. Then, the printed block and the substrate were subjected to stress relief annealing at 450 °C for 3 h in a vacuum atmosphere.
  • the optimized SLM process parameters are: laser spot diameter 70 ⁇ m, laser power 250W, laser scanning rate 900mm/s, laser scanning spacing 90 ⁇ m, powder layer thickness 40 ⁇ m, using strip scanning strategy, laser scanning between layers The direction is rotated by 67°, and the forming strategy is shown in Figure 1.
  • Fig. 8 show that many cracks can be observed in the printed parts, the crack length is 300 ⁇ m, and the crack density is 2.5 ⁇ 0.6 mm/mm 2 .
  • the density of the prepared sample was 98.9%, the yield strength and tensile strength were 786MPa and 918MPa, respectively, and the elongation was 3.9%.
  • the method of the present invention is applied to the following René 104 nickel-based superalloy without adding rare earth elements, and the weight percentage of the alloy is .
  • the present invention is used for SLM forming René104 nickel-based superalloy.
  • the sieved René104 nickel-based superalloy powder is dried in a vacuum drying oven at 120° C. for 4 hours. After the substrate is heated to 170° C., the dried powder is dried. Load into the powder supply cylinder and spread powder, and pass argon or nitrogen into the working chamber until the oxygen content is less than 100ppm. Then enter the printing process, and repeat the steps of powder spreading and laser scanning powder until the printing is completed, and the René104 nickel-based superalloy block is obtained. Then, the printed block and the substrate were subjected to stress relief annealing at 450 °C for 3 h in an argon atmosphere.
  • the unoptimized SLM process parameters are: the laser spot diameter is 70 ⁇ m, the laser power is 400 W, the laser scanning rate is 1200 mm/s, the laser scanning spacing is 90 ⁇ m, and the thickness of the powder layer is 30 ⁇ m.
  • the scanning direction is rotated by 67°, and the forming strategy is shown in Figure 1.
  • the density of the prepared sample is 98.9%, the yield strength and tensile strength are 708MPa and 875MPa, respectively, and the elongation is 2.6%.

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Abstract

一种消除3D打印镍基高温合金裂纹的方法，所述镍基高温合金以质量百分比计，包括下述组分：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％、余量为Ni；或以下列镍基高温合金为基体，向基体加入0.05-0.18wt％的RE，上述镍基高温合金选自IN738LC、CM247LC、CMSX-4、René 142、Hastelloy X、IN718、IN625中的一种，所述RE选自Sc、Y、La、Ce、Er中的至少一种。针对γ'相沉淀强化镍基高温合金3D打印易产生裂纹的问题，上述方法提出通过适量稀土进行稀土微合金化，降低γ'相沉淀强化镍基高温合金3D打印开裂敏感性，扩宽3D打印工艺窗口，抑制3D打印裂纹的产生，大幅提高成形件的强度和塑性，有效预防工序间存放开裂、后续热处理开裂等后续加工过程中裂纹的形成。使用该方法制备的γ'相沉淀强化镍基高温合金René104未见裂纹，致密度超过99.4％，屈服强度和抗拉强度分别达到了935MPa和1256MPa，伸长率超过14.0％。

Description

一种消除3D打印镍基高温合金裂纹的方法 技术领域
本发明提供一种消除3D打印镍基高温合金裂纹的方法，属于高温合金增材制造技术领域。
 背景技术
γ′相沉淀强化镍基高温合金是材料科学领域的重大突破之一，其强化相为有序、连贯的金属间化合物如γ′-Ni 3(Al，Ti)，通常采用铸造、变形加工，或粉末成形技术制备，广泛应用于先进航空发动机。但是，这些技术无法直接成形形状复杂的制件。3D打印，或称增材制造技术，可直接从三维计算机辅助设计数据中逐层生成近净形尺寸的三维零件，在高性能形状复杂构件的制备方面具有独特的优势，已在钛合金、铝合金、不锈钢和镍基合金等材料中得到应用。3D打印成形过程温度梯度大、冷却速度快、反复重熔，使得成形件中残余应力高，易产生变形和开裂，给3D打印成形高质量制件带来了挑战，特别是高Al、Ti含量的γ′相沉淀强化镍基高温合金，焊接性能差，开裂已经成为这类合金3D打印最突出的问题。
针对上述问题，国内外进行了探索性的研究。Catchpole-Smith等[Catchpole-Smith S, et al. Fractal scan strategies for selective laser melting of 'unweldable' nickel superalloys[J]. Additive Manufacturing, 2017, 15:113-122.]研究了3种不同的扫描路径对选区激光熔融（SLM）成形“不可焊” 镍基高温合金开裂的影响，采用不规则形状扫描路径成形的样品，热应力更小且分布均匀，裂纹明显减少，致密度提高了2 ± 0.7%，但不能完全消除裂纹；进一步采用热等静压处理，才能完全消除裂纹。Xu等[Jianjun Xu, et al. The initiation and propagation mechanism of the overlapping zone cracking during laser solid forming of IN738LC superalloy[J].Journal of Alloys and Compounds, 2018, 749: 859-870]将基板加热到700℃及以上，制备出了完全无裂纹的IN738LC镍基高温合金。这种将基板温度提高到700℃及以上更高温度的做法，由于基板温度过高，容易导致晶粒粗大。Han等[Quanquan Han, et al. Additive manufacturing of high-strength crack-free Ni-based Hastelloy X superalloy[J]. Additive Manufacturing, 2019, 30: 100919]通过添加纳米TiC，消除了Hastelloy X镍基高温合金的裂纹。中国专利（CN108941560B）公开了一种消除René104镍基高温合金激光增材制造裂纹的方法，提出通过设计激光成形参数和分区扫描策略，结合去应力退火和放电等离子烧结（SPS）处理，消除成形件内部裂纹的方案，并抑制了烧结过程中晶粒的长大。中国专利（CN108994304B）公开了一种消除金属材料增材制造裂纹，提高力学性能的方法，依次采用特定参数的去应力退火、特定参数的SPS处理，不仅消除了产品的裂纹，还实现了力学性能的大幅度提高。以上专利都是通过后处理来消除3D打印制件的裂纹。中国专利（CN104988355A）公开了一种降低打印用镍基高温合金粉末材料热裂倾向的方法，其通过添加大量的Hf和/或B元素来解决热裂缺陷这一问题。但是，上述方法无法抑制3D打印的镍基高温合金制件在打印和/或后续热处理时产生的裂纹等问题。
本发明首次提出通过适量稀土进行稀土微合金化，降低γ′相沉淀强化镍基高温合金3D打印开裂敏感性，扩宽γ′相沉淀强化镍基高温合金3D打印工艺窗口，抑制3D打印以及后续热处理裂纹的产生，适用于各种形状制件的增材制造。
 技术问题
本发明提出一种消除3D打印镍基高温合金裂纹的方法，针对γ′相沉淀强化镍基高温合金3D打印易产生裂纹问题，首次提出通过适量稀土进行稀土微合金化，降低γ′相沉淀强化镍基高温合金3D打印开裂敏感性，扩宽γ′相沉淀强化镍基高温合金3D打印工艺窗口，抑制3D打印以及后续热处理裂纹的产生，大幅提高成形件的强度和塑性。
 技术解决方案
本发明一种消除3D打印镍基高温合金裂纹的方法，所述致密镍基高温合金是以镍基高温合金粉末为原料，通过3D打印制备；所述镍基高温合金以质量百分比计，包括下述组分。
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%。
或以其他不可焊镍基高温合金为基体，向基体中加入0.05-0.18wt%的RE。
所述其他不可焊镍基高温合金选自IN738LC、CM247LC、CMSX-4、René 142、Hastelloy X中的一种；或以IN718、IN625镍基高温合金中的一种为基体，向基体中加入0.05-0.18wt%的RE。
所述3D打印的参数为：激光功率为150～300W，激光扫描速率500～1100mm/s，光斑直径为70～110μm，激光扫描间距60～120μm，铺粉层厚为30～50μm，成形层之间的激光扫描方向旋转45°-90°，优选为67°。
所述RE选自Sc、Y、La、Ce、Er中的至少一种。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述镍基高温合金以质量百分比计，包括下述组分μm。
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%。
余量为Ni。
本发明一种消除3D打印镍基高温合金裂纹的方法，RE为Sc；或RE为Sc与Y、La、Ce、Er中至少一种的混合。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述镍基高温合金粉末通过以下步骤制备。
步骤一：真空熔炼。
按照设计组分配取原料，并将原料装入雾化制粉炉的坩埚内，在低于0.1Pa的真空度下采用感应加热，进行真空熔炼。
步骤二：脱气。
原料熔化后，真空脱气10min～20min。
步骤三：精炼。
向雾化制粉炉内充入高纯惰性气体至0.1-0.11MPa，将熔融的母合金熔液在1600℃～1650℃温度范围内保温10min～15min。
步骤四：雾化。
将熔融的母合金熔液以3.5kg/min～5kg/min的流速经导流管流下，用3MPa～5MPa的高压、高纯惰性气体将金属液流破碎成细小液滴，液滴经过冷却和凝固，形成球形粉末，进入粉末收集罐中。
步骤五：筛分。
粉末经充分冷却后，在惰性气体保护下使用气流分级和超声震动筛分，得到中粉粒径为53～106μm，细粉粒径为15～53μm的球形镍基高温合金粉末，并进行真空封装。
所述的惰性气体应为氦气、氩气，或氩、氦混合气体，纯度为99.99wt%，其中氧含量小于0.0001wt%。
所得镍基高温合金粉末的氧含量小于等于0.0126wt%，硫含量小于等于0.0056wt%。在工业上应用时，还可以采用等离子旋转电极雾化法制备镍基高温合金粉末。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述镍基高温合金粉末的氧含量小于等于0.01wt%，硫含量小于等于0.004wt%。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述镍基高温合金粉末经50g/2.5mm孔径测试流动性，其结果为15-25 s。经优化后可为15.5-16 s。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述3D打印为选区激光熔融（SLM），或电子束熔化（EBM），或同轴送粉激光成形（LENS）中的一种。
本发明一种消除3D打印镍基高温合金裂纹的方法，所述3D打印的参数为：激光功率为150～300W，激光扫描速率500～1100mm/s，光斑直径为70～110μm，激光扫描间距60～120μm，铺粉层厚为30～50μm，成形层之间的激光扫描方向旋转45°~90°，优选为67°。
本发明一种消除3D打印镍基高温合金裂纹的方法，3D打印完成后，在真空或惰性气体气氛中进行450～650℃保温0.5～3h去应力退火，得到制件。
本发明一种消除3D打印镍基高温合金裂纹的方法，制件的致密度为99.3%~99.5%，室温屈服强度为918~935MPa，抗拉强度为1120~1256MPa，伸长率为12.5~14.5%。
本发明一种消除3D打印镍基高温合金裂纹的方法，所制备的合金粉末为成分均匀的过饱和固溶体合金粉末。该合金粉末采用雾化快速凝固制备，所添加的元素可以超出平衡固溶极限，形成过饱和固溶体；无合金元素偏析。采用该合金粉末进行3D打印快速凝固成形的制件，具有细小树枝晶组织，元素偏析被限制在亚微米级。微量稀土元素抑制了低熔点相的形成，消除了B、Zr等形成的低熔点化合物，缩小凝固温度范围，降低了γ′相沉淀强化镍基高温合金开裂敏感性，从而抑制了3D打印裂纹形成。
 有益效果
（1）本发明针对高Al、Ti含量的γ′相沉淀强化镍基高温合金，焊接性能差，在3D打印过程中容易开裂的问题，通过适量稀土进行稀土微合金化结合3D打印参数优化，降低了γ′相沉淀强化镍基高温合金开裂敏感性，消除3D打印裂纹，大幅提高成形件的强度和塑性。
（2）本发明通过添加微量Sc、Y、La、Ce、Er或混合添加，随后采用惰性气体雾化或等离子旋转电极雾化快速凝固制备过饱和固溶体高温合金粉末，所得粉末球形度高，粒度分布范围窄，同时氧、硫等杂质元素显著降低，适用于3D打印技术。
（3）本发明降低了γ′相沉淀强化镍基高温合金在3D打印快速熔化、凝固过程中的开裂敏感性，扩宽γ′相沉淀强化镍基高温合金3D打印工艺窗口。
（4）本发明通过稀土微合金化和参数优化的协同作用，既保证了3D打印制件质量，也控制了3D打印过程中残余应力的产生和积累，有效抑制了3D打印过程中裂纹的产生。
（5）本发明通过惰性气体雾化或者等离子旋转电极雾化制粉和3D打印快速成形，使元素偏析被限制亚微米级，提高了成分和组织均匀性。
（6）本发明的制备方法减少了粉末和3D打印制件的成分偏析，大大减小了3D打印热应力积累，抑制了凝固裂纹与变形的产生，提高了制件的质量与力学性能。
（7）本发明通过适量稀土进行稀土微合金化，消除γ′相沉淀强化镍基高温合金3D打印裂纹，大幅提高成形件的强度和塑性，有效预防工序间存放开裂、后续热处理开裂等后续加工过程中裂纹的形成。
（8）本发明有效消除了高Al、Ti含量的γ′相沉淀强化镍基高温合金3D打印裂纹，使用本方法制备的γ′相沉淀强化镍基高温合金René104，成形件内未见裂纹，致密度超过99.4%，其室温屈服强度和抗拉强度分别达到了935MPa和1256MPa，伸长率超过14.0%。
综上所述，本发明针对高Al、Ti含量的γ′相沉淀强化镍基高温合金，焊接性能差，3D打印过程中容易开裂的问题，通过添加适量的稀土Sc、Y、La、Ce、Er或混合添加进行微合金化，随后采用惰性气体雾化或者等离子旋转电极雾化快速凝固制备过饱和固溶体高温合金粉末，降低γ′相沉淀强化镍基高温合金3D打印开裂敏感性，扩宽γ′相沉淀强化镍基高温合金3D打印工艺窗口，结合参数优化消除3D打印γ′相沉淀强化镍基高温合金裂纹，大幅提高成形件的强度和塑性，并有效预防工序间存放开裂、后续热处理开裂等后续加工过程中裂纹的形成。
 附图说明
图1为实施例一、二、三和对比例一、二、三采用的扫描策略示意图。
图2为实施例一SLM制备的稀土Sc微合金化René104合金金相组织图像。
图3为实施例二SLM制备的稀土Y微合金化René104合金微观结构扫描电镜（SEM）照片。
图4为实施例三SLM制备的Sc、Y混合稀土微合金化René104合金微观结构SEM照片。
图5为实施例四SLM制备的René104合金微观结构SEM照片。
图6为实施例五SLM制备的René104合金微观结构SEM照片。
图7为对比例一SLM制备的稀土Sc微合金化René104合金微观结构SEM照片。
图8为对比例二SLM制备的René104合金微观结构SEM照片。
图9为对比例三SLM制备的René104合金微观结构SEM照片。
 本发明的实施方式
下面结合附图和具体实施例，对本发明做进一步的阐述。
实施例一。
将本发明方法用于下述René104镍基高温合金，添加质量分数为0.08%稀土Sc元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～0.08Sc～余量为Ni，配制该合金的母合金后采用氩气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金，首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在真空气氛中进行450℃保温3h的去应力退火。
经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率250W，激光扫描速率900mm/s，激光扫描间距90μm，铺粉层厚为40μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图2结果表明，打印成形件没有观察到裂纹。
所制备样品的致密度为99.44%，屈服强度和抗拉强度分别为918MPa、1236MPa，伸长率为14.0%。
实施例二。
将本发明方法用于下述René104镍基高温合金，添加质量分数为0.12%稀土Y元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～0.12Y～余量为Ni，配制该合金的母合金后采用氦气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金，首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在氩气中进行500℃保温2h的去应力退火。
经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率250W，激光扫描速率900mm/s，激光扫描间距90μm，铺粉层厚为40μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图3结果表明，打印成形件没有观察到裂纹。
所制备样品的致密度为99.39%，屈服强度和抗拉强度分别为930MPa、1224MPa，伸长率为12.8%。
实施例三。
将本发明方法用于下述René104镍基高温合金，添加质量分数为0.06%稀土Sc元素和0.08%稀土Y元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～0.06Sc～0.08Y～余量为Ni，配制该合金的母合金后采用氩气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金，首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在真空气氛中进行450℃保温3h的去应力退火。
经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率250W，激光扫描速率900mm/s，激光扫描间距90μm，铺粉层厚为40μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图4结果表明，打印成形件没有观察到裂纹。
所制备样品的致密度为99.46%，屈服强度和抗拉强度分别为935MPa、1256MPa，伸长率为14.3%。
实施例四。
以实施例一制备的合金粉末为原料，采用中国专利（CN108941560A）实施例一中采用的3D打印工艺参数制备René104合金块体。SLM工艺具体参数为。
激光功率为250W，光斑直径为0.12mm，扫描速度为500mm/s，扫描间距为0.12mm，铺粉层厚为0.03mm。
SLM所用扫描策略为条带扫描策略，如图1所示为条带扫描策略示意图，采用由下至上逐层扫描的方式，相邻层之间的激光扫描方向旋转67°，条带大小为7mm，条带间的搭接为0.11mm，目的是减少打印过程中残余应力的叠加。
图5为René104合金的微观结构SEM照片，成形件结构致密，没有观察到裂纹。经检测，所制备的René104合金的致密度为99.32%，优于中国专利（CN108941560A）实施例一采用SLM制备得到的致密度为99.18%的成形件；室温屈服强度为926MPa，抗拉强度为1242MPa，伸长率为14.2%。
对上述成型件，采用中国专利（CN108941560A）实施例一相同的去应力退火和SPS处理。
去应力退火参数为：温度420℃，保温90min，然后随炉冷却。
放电等离子烧结参数为：直径为40mm的石墨磨具，升温速率为60℃/min，降温速率为60℃/min，烧结压力45MPa，烧结温度1020℃，保温时间15min。
经检测，最终所制备的René104合金的致密度为99.62%，室温屈服强度为1038MPa，抗拉强度为1394MPa，伸长率为14.5%，优于中国专利（CN108941560A）实施例一采用SLM制备、并采用去应力退火消除残余应力和SPS消除裂纹制备的成形件的力学性能。所述中国专利（CN108941560A）实施例一制备的成形件的室温力学性能分别为987MPa和1376MPa。
实施例五。
以实施例一制备的合金粉末为原料，采用中国专利（CN108941560B）对比例一中采用的3D打印工艺参数制备René104合金块体。SLM工艺具体参数为。
激光功率为225W，光斑直径为0.12mm，扫描速度为600mm/s，扫描间距为0.11mm，铺粉层厚为0.03mm。（不采用分区策略）。
图6为René104合金的微观结构SEM照片，所制备样品的结构致密，没有观察到裂纹。经检测，所制备的René104合金的致密度为99.2%，室温屈服强度为913MPa，抗拉强度为1247MPa，伸长率为13.3%。
中国专利（CN108941560B）对比例一的打印成形件，经后处理（去应力退火+SPS）前和后处理（去应力退火+SPS）后的致密度分别为98.12%和99.02%，室温力学性能分别为751MPa和916MPa。
对比中国专利（CN108941560B）对比例一的致密度、力学性能，本发明采用中国专利（CN108941560B）中，开裂最严重、制件性能最差的对比例一的3D打印工艺参数，也可以制备出高质量、无裂纹，且力学性能优异制件。表明本发明所制备的合金及粉末，可扩宽3D打印工艺窗口。
对比例一。
将本发明方法用于下述René104镍基高温合金，添加质量分数为0.08%稀土Sc元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～0.08Sc～余量为Ni，配制该合金的母合金后采用氩气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在真空气氛中进行450℃保温3h的去应力退火。
未经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率400W，激光扫描速率1200mm/s，激光扫描间距90μm，铺粉层厚为30μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图7结果表明，打印成形件可以观察到少量裂纹，裂纹长度为150μm左右，裂纹密度为1.4±0.5 mm/mm 2。
所制备样品的致密度为90.12%，屈服强度和抗拉强度分别为893MPa、1085MPa，伸长率为10.4%。
对比例二。
将本发明方法用于下述René104镍基高温合金，不添加稀土元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～余量为Ni，配制该合金的母合金后采用氩气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金，首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在真空气氛中进行450℃保温3h的去应力退火。
经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率250W，激光扫描速率900mm/s，激光扫描间距90μm，铺粉层厚为40μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图8结果表明，打印成形件可以观察到较多裂纹，裂纹长度为300μm，裂纹密度为2.5±0.6 mm/mm 2。
所制备样品的致密度为98.9%，屈服强度和抗拉强度分别为786MPa、918MPa，伸长率为3.9%。
对比例三。
将本发明方法用于下述René104镍基高温合金，不添加稀土元素，该合金重量百分比为。
20.6Co～13Cr～3.4Al～3.9Ti～3.8Mo～2.1W～2.4Ta～0.9Nb～0.05Zr～0.03B～0.04C～余量为Ni，配制该合金的母合金后采用氩气雾化快速凝固制粉，通过气流分级和超声振动筛粉筛出15～53μm的合金粉末。
将本发明用于SLM成形René104镍基高温合金，首先将筛分后的René104镍基高温合金粉末在120℃的真空干燥箱中烘干4h，基板加热到170℃后，将经烘干的粉末装入供粉缸并进行铺粉，往工作腔内通入氩气或氮气至氧含量低于100ppm。之后进入打印程序，不断重复铺粉、激光扫描粉末的步骤，直到打印完成，得到René104镍基高温合金块体。随后对打印好的块体连同基板在氩气气氛中进行450℃保温3h的去应力退火。
未经优化后的SLM工艺参数为：激光光斑直径70μm，激光功率400W，激光扫描速率1200mm/s，激光扫描间距90μm，铺粉层厚为30μm，采用条带扫描策略，逐层之间的激光扫描方向旋转67°，成形策略如图1所示。
图9结果表明，打印成形件可以观察到明显裂纹，裂纹长度接近500μm，裂纹密度为3.7±0.8 mm/mm 2。
所制备样品的致密度为98.9%，屈服强度和抗拉强度分别为708MPa、875MPa，伸长率为2.6%。

Claims (10)

  1. 一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述致密镍基高温合金是以镍基高温合金粉末为原料，通过3D打印制备；所述镍基高温合金以质量百分比计，包括下述组分：
    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%；
    余量为Ni；
    或以其他不可焊镍基高温合金为基体，向基体中加入0.05-0.18wt%的RE；
    所述其他不可焊镍基高温合金选自IN738LC、CM247LC、CMSX-4、René 142、Hastelloy X中的一种；或以IN718、IN625镍基高温合金中的一种为基体，向基体中加入0.05-0.18wt%的RE；
    所述3D打印的参数为：激光功率为150～300W，激光扫描速率500～1100mm/s，光斑直径为70～110μm，激光扫描间距60～120μm，铺粉层厚为30～50μm，成形层之间的激光扫描方向旋转45°-90°；
    所述RE选自Sc、Y、La、Ce、Er中的至少一种。
  2. 根据权利要求1所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述镍基高温合金以质量百分比计，包括下述组分：
    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%；
    余量为Ni。
  3. 根据权利要求1所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：RE为Sc；或RE为Sc与Y、La、Ce、Er中至少一种的混合。
  4. 根据权利要求1所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于；所述镍基高温合金粉末通过以下步骤制备：
    步骤一：真空熔炼
    按设计组分配取原料，并将原料装入雾化制粉炉的坩埚内，在低于0.1Pa的真空度下采用感应加热，进行真空熔炼；
    步骤二：脱气
    原料熔化后，真空脱气10min～20min；
    步骤三：精炼
    向雾化制粉炉内充入高纯惰性气体至0.1-0.11MPa，将熔融的母合金熔液在1600℃～1650℃温度范围内保温10min～15min；
    步骤四：雾化
    将熔融的母合金熔液以3.5kg/min～5kg/min的流速经导流管流下，用3MPa～5MPa的高压、高纯惰性气体将金属液流破碎成细小液滴，液滴经过冷却和凝固，形成球形粉末，进入粉末收集罐中；
    步骤五：筛分
    粉末经充分冷却后，在惰性气体保护下使用气流分级和超声震动筛分，得到中粉粒径为53～106μm，细粉粒径为15～53μm的球形镍基高温合金粉末，并进行真空封装；
    所述的惰性气体应为氦气、氩气，或氩、氦混合气体，纯度为99.99wt%，其中氧含量小于0.0001wt%；
    所得镍基高温合金粉末的氧含量小于等于0.0126wt%，硫含量小于等于0.0056wt%。
  5. 根据权利要求4所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述镍基高温合金粉末的氧含量小于等于0.01wt%，硫含量小于等于0.004wt%。
  6. 根据权利要求4所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述镍基高温合金粉末经50g/2.5mm孔径测试流动性，其结果为15-25 s。经优化后可为15.5-16 s。
  7. 根据权利要求4所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述3D打印为选区激光熔融（SLM），或电子束熔化（EBM），或同轴送粉激光成形（LENS）。
  8. 根据权利要求1所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：所述3D打印的参数为：激光功率为150～300W，激光扫描速率500～1100mm/s，光斑直径为70～110μm，激光扫描间距60～120μm，铺粉层厚为30～50μm，成形层之间的激光扫描方向旋转45°~90°，优选为67°。
  9. 根据权利要求1所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：3D打印完成后，在真空或惰性气体气氛中进行450～650℃保温0.5～3h去应力退火，得到制件。
  10. 根据权利要求9所述的一种消除3D打印镍基高温合金裂纹的方法，其特征在于：制件的致密度为99.3%~99.5%，室温屈服强度为918~935MPa，抗拉强度为1120~1256MPa，伸长率为12.5~14.5%。
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CN115026309A (zh) * 2022-06-13 2022-09-09 西安交通大学 优化激光选区熔化增材镍基高温合金残余应力的原位热处理方法
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CN116604031A (zh) * 2022-09-09 2023-08-18 南昌航空大学 一种提高激光增材制造In 718合金硬度的方法
CN115609006A (zh) * 2022-09-26 2023-01-17 哈尔滨工业大学（威海） 镍基合金粉芯丝材、制备方法及增材制造镍基合金的方法
CN115647369A (zh) * 2022-10-08 2023-01-31 洛阳科威钨钼有限公司 一种利用增材制造技术制备钼合金复杂精密结构件的方法
CN115555555A (zh) * 2022-10-24 2023-01-03 北京工业大学 一种抑制激光增材制造高温合金热裂纹的方法
CN115673338A (zh) * 2022-10-25 2023-02-03 南方科技大学 一种镍基合金的利用双激光实现组织性能定制的粉床熔融成形方法及镍基合金件
CN115815624A (zh) * 2022-12-28 2023-03-21 鑫精合激光科技发展（北京）有限公司 一种激光选区熔化成形方法及烘粉装置
CN116673500A (zh) * 2023-03-13 2023-09-01 南京理工大学 提高增材制造镍基合金薄壁构件强度和塑性的热处理方法
CN116144962A (zh) * 2023-04-17 2023-05-23 北京科技大学 一种高强韧哈氏合金及其制备工艺
CN116516271A (zh) * 2023-04-28 2023-08-01 西安工业大学 一种不产生裂纹的SLM成形Inconel 718合金的热处理方法
CN117380970A (zh) * 2023-06-27 2024-01-12 上海汉邦联航激光科技有限公司 一种gh3625镍基高温合金及其打印方法和应用
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CN116944519A (zh) * 2023-07-31 2023-10-27 华中科技大学 一种高强铁基复合材料的激光3d打印方法及其产品
CN117340270A (zh) * 2023-08-25 2024-01-05 长沙理工大学 一种航空用钛合金扭转疲劳性能的微观组织定量调控方法
CN116944492A (zh) * 2023-09-14 2023-10-27 江西省科学院应用物理研究所 一种高温/高强/高韧异质结构Ti6Al4V合金的制备方法
WO2025148967A1 (zh) * 2024-01-09 2025-07-17 中南大学 一种增材制造用高等轴晶占比镍基高温合金
CN117604329A (zh) * 2024-01-12 2024-02-27 山东大学 用于激光粉末床熔融工艺的镍基高温合金材料及制备方法
CN118046003A (zh) * 2024-02-19 2024-05-17 西南交通大学 一种提高增材制造Hastelloy X合金力学性能的方法
CN117922003A (zh) * 2024-03-21 2024-04-26 东莞理工学院 选择性激光烧结打印机
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