CN114799204B - Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity - Google Patents
Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity Download PDFInfo
- Publication number
- CN114799204B CN114799204B CN202210683465.6A CN202210683465A CN114799204B CN 114799204 B CN114799204 B CN 114799204B CN 202210683465 A CN202210683465 A CN 202210683465A CN 114799204 B CN114799204 B CN 114799204B
- Authority
- CN
- China
- Prior art keywords
- laser
- powder
- additive manufacturing
- nickel
- laser additive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
-
- 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]
-
- 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
- B22F10/80—Data acquisition or data processing
- B22F10/85—Data acquisition or data processing for controlling or regulating additive manufacturing processes
-
- 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
-
- 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
- B33Y50/00—Data acquisition or data processing for additive manufacturing
- B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
-
- 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
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- 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
Abstract
The invention discloses a method for reducing brittle Laves phase in laser additive manufacturing nickel-based superalloy and improving strong plasticity, which comprises the following steps: s1, wet mixing nano carbon powder and nickel-based high-temperature alloy powder, drying and cooling; s2, starting a laser additive manufacturing and forming test and obtaining process parameters of laser additive manufacturing and forming; and S3, performing a laser additive forming test to obtain a non-defective high-density sedimentary sample, and performing microstructure analysis and mechanical property test on the sedimentary sample. According to the invention, a small amount of carbon element is introduced into the nickel-based high-temperature alloy powder and technological parameters of laser additive forming manufacturing are regulated, so that the carbon element plays a role in reducing the content of a brittle Laves phase in the nickel-based high-temperature alloy, the formation of the brittle Laves phase with chain-shaped distribution among dendrites in a deposited sample is effectively avoided, the content of the brittle Laves phase is reduced, and the dispersion distribution of small-size carbides is controlled, so that the room-temperature mechanical property of the nickel-based high-temperature alloy manufactured by laser additive manufacturing is improved.
Description
Technical Field
The invention relates to the technical field of nickel-based superalloy preparation and laser additive manufacturing, in particular to a method for reducing a brittle Laves phase in laser additive manufacturing of a nickel-based superalloy and improving strong plasticity.
Background
The nickel-based high-temperature alloy has good high-temperature mechanical property and excellent oxidation resistance and corrosion resistance, and is widely applied to heat end parts of aerospace engines, gas turbines and the like. At present, 30 to 45 percent of hot end parts of aeroengines and gas turbines are formed by forging and adding and subtracting materials by a machine, so that great waste of high-temperature alloy is caused. In addition, the high-temperature alloy has the characteristics of difficult deformation, difficult processing and the like, so that the processing of high-temperature alloy parts with complex structures becomes more difficult, the functional and light-weight characteristics of partial structures are sacrificed due to the consideration of the existing processing process limitations in the actual design and manufacturing process of parts, and the innovative development of the aeroengine and gas turbine technology is severely restricted. The laser additive manufacturing technology shows wide application prospects in the manufacturing of complex components in the fields of aerospace, power energy and the like gradually due to the advantages of digital manufacturing of free entities, no mold, short period, high-performance complex component integrated forming and the like.
However, due to the influence of high-temperature alloy components and laser additive manufacturing process characteristics, micro-segregation of alloy elements during solidification can cause the formation of continuously distributed chain brittle phases among dendrites, such as Laves and the like. The existence of the brittle phase can seriously reduce the mechanical property of the alloy, and on one hand, a large amount of solid solution strengthening and precipitation strengthening elements can be consumed to reduce the strengthening effect; on the other hand, the brittle phase can become a crack initiation source and an expansion channel in the stress process, and the toughness of the alloy is reduced. It is therefore necessary to improve the mechanical properties of the alloy by reducing the continuously distributed brittle phases in laser additive manufacturing of nickel-base superalloys by a suitable process. The adoption of high-temperature solid solution heat treatment can fully dissolve the brittle phase, thereby improving the toughness of the alloy, but the treatment process can generate recrystallization to reduce the dislocation density, so that the yield strength of the alloy is obviously reduced, and the improvement of the comprehensive mechanical property of the alloy is not facilitated.
Disclosure of Invention
The invention mainly aims to solve the technical problems that brittle phases distributed in a continuous chain shape exist among dendrites in a deposited sample of a laser additive manufactured nickel-based high-temperature alloy in the prior art to reduce the mechanical property of the alloy, and the subsequent high-temperature solid solution treatment can seriously reduce the yield strength of the alloy to influence the strengthening and toughening effect of the alloy, and provides a method for reducing the brittle Laves phases in the laser additive manufactured nickel-based high-temperature alloy and improving the strong plasticity of the alloy.
The invention provides a method for reducing brittle Laves phase and improving strong plasticity in a laser additive manufacturing nickel-based high-temperature alloy, which comprises the following steps:
s1, wet mixing nano carbon powder and nickel-based high-temperature alloy powder in absolute ethyl alcohol according to a mass ratio, drying, and cooling to obtain carbon-containing nickel-based high-temperature alloy powder;
s2, putting carbon-containing nickel-based superalloy powder into a powder feeder, filling argon gas serving as inert protective gas into a laser additive manufacturing forming bin, starting a laser additive manufacturing forming test after the oxygen content in the forming bin is reduced to 50ppm, and obtaining technological parameters of laser additive manufacturing forming;
and S3, performing a laser additive forming test on the carbon-containing nickel-based superalloy powder obtained in the step S1 according to the laser additive manufacturing forming process parameters in the step S2 to obtain a defect-free high-density deposition-state sample, and performing microstructure analysis and mechanical property test on the deposition-state sample to determine the influence rule of the introduction of the carbon element on the volume fraction and distribution characteristics of the brittle Laves phase and the improvement of the alloy strong plasticity.
In some embodiments of the present invention, in step S1, the mass ratio of the nano carbon powder to the nickel-based superalloy powder is (0.5-4): (996-999.5), preferably (1-2): (998-999).
In some embodiments of the present invention, in step S1, the nano carbon powder is selected from graphite powder with a particle size of 40-60 nm; the nickel-based superalloy powder is selected from a solid solution strengthening type nickel-based superalloy or a precipitation strengthening type nickel-based superalloy; the particle size of the nickel-based superalloy powder in the coaxial powder feeding type directional energy deposition process is 50-150 mu m, and the particle size of the nickel-based superalloy powder in the selective laser melting process is 15-53 mu m.
In some embodiments of the invention, in step S1, wet mixing is performed in absolute ethanol by using a planetary ball mill, the rotation speed of the planetary ball mill is 120-200 r/min during powder mixing, the planetary ball mill rotates forwards for 3-5 min, stops for 30S and rotates backwards for 3-5 min, and the wet mixing time is 3-6 h; the drying is carried out in a vacuum drying oven at the temperature of 110-130 ℃ for 4-6 h.
In some embodiments of the invention, in step S2, the laser additive manufacturing process is selected from a co-axial powder-fed directional energy deposition process or a selective laser melting process.
In some embodiments of the present invention, in step S2, the type of laser used in the CO-fed energy deposition process is CO 2 The laser, the fiber laser or the semiconductor laser, the optimized technological parameters are as follows: the laser power is 1000-3000W, the diameter of a light spot is 2-5 mm, the scanning speed is 10-30 mm/s, the powder feeding amount is 8-20 g/min, the powder carrying gas flow is 4-10L/min, the lap joint rate is 40-60%, and the lifting amount is 0.4-0.6mm; the energy distribution of the laser is Gaussian distribution or bimodal distribution, and the protective gas and the powder carrier are argon gas in the forming process.
In some embodiments of the present invention, in step S2, the laser used in the selective laser melting process is a fiber laser, and the optimized process parameters are: the laser power is 180-300W, the spot diameter is 50-100 mu m, the scanning speed is 300-1200 mm/s, the scanning interval is 60-100 mu m, the powder laying thickness is 30-50 mu m, the used laser can be continuous laser or pulse laser, and the wavelength is 1060 nm.
In some embodiments of the present invention, in step S3, when the coaxial powder feeding directional energy deposition process is adopted for the laser additive manufacturing and forming, a laser scanning mode in a layer is a unidirectional scanning or a reciprocating scanning, and a laser scanning path between layers may be a cross scanning or a reciprocating scanning.
In some embodiments of the present invention, in step S3, when the selective laser melting process is used for laser additive manufacturing forming, the scanning manner in the layer is unidirectional scanning or reciprocating scanning, and the rotation angle between the layers is any one of 0 °, 90 ° or 67 °.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a small amount of carbon element is introduced into the nickel-based high-temperature alloy powder and technological parameters of laser additive forming manufacturing are regulated, so that the carbon element plays a role in reducing the content of a brittle Laves phase in the nickel-based high-temperature alloy, the formation of the brittle Laves phase with chain-shaped distribution among dendrites in a deposited sample is effectively avoided, the content of the brittle Laves phase is reduced, the dispersion distribution of small-size carbides is controlled, mechanical property test is performed on the deposited sample, the influence rule of the introduction of the carbon element on the improvement of the alloy strong plasticity is determined, and the effect of improving the room-temperature mechanical property of the nickel-based high-temperature alloy manufactured by laser additive manufacturing is achieved.
Drawings
FIG. 1 is an electron microscope photograph of the laser additive manufacturing nickel-based superalloy powder.
FIG. 2 is a microstructure diagram of Ni-based superalloy as-deposited after addition of 0.1% carbon (mass%) in example 1 of the present invention.
FIG. 3 is a microstructure diagram of Ni-based superalloy as-deposited after addition of 0.2% carbon (mass%) in example 2 of the present invention.
Fig. 4 is a microstructure diagram of the ni-based superalloy deposited after the addition of 0.4% c (mass%) in example 3 according to the present invention.
FIG. 5 is a photograph of the as-deposited microstructure of the carbon-free additive nickel-based superalloy prepared by laser additive manufacturing in comparative example 1 according to the present invention.
FIG. 6 is a microstructure diagram of Ni-based superalloy deposited with 0.6% C (mass%) addition in comparative example 2.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention.
Room temperature mechanical properties (yield strength, tensile strength, elongation) test method: sampling a tensile sample from a sedimentary sample, wherein the shape of the sample is plate-shaped, the gauge length is 20mm, the width and the thickness are respectively 6mm and 2mm, the moving speed of a cross beam of a stretcher in the stretching process is 1mm/min, in order to accurately measure the elastic modulus and the yield strength, a extensometer with the length of 10mm is used for measuring the deformation of the sample in the stretching process to calculate the engineering strain in the stretching process, and the residual elongation stress sigma is specified r0.2 The specific measurement method is the percentage of the elongation of a gauge length section of the sample after fracture and the initial gauge length.
Example 1
A method for reducing brittle Laves phase and improving strong plasticity in a laser additive manufacturing nickel-based high-temperature alloy, taking Inconel 625 nickel-based high-temperature alloy as an example, the alloy components are 63.59 Ni-21.5 Cr-8.5Mo-3.5 Nb-2.0 Fe-0.2 Ti-0.2 Al-0.5 Si-0.01C (mass percent), and the addition amount of carbon element in the alloy is 0.1% (mass percent);
s1: taking 1g of graphite powder with the particle size of 50nm and 999g of spherical Inconel 625 alloy powder with the particle size of 50-150 mu m (shown in figure 1), putting the graphite powder and the spherical Inconel 625 alloy powder into a stainless steel ball milling tank, adding absolute ethyl alcohol, putting the ball milling tank into a planetary ball mill for ball milling, wherein the ball milling process parameters are as follows: the rotating speed is 160r/min, the rotation is stopped for 30s after 5min, and then the rotation is carried out for 5min, and the whole powder mixing process lasts for 4h; after the powder mixing is finished, taking out the ball milling tank, placing the ball milling tank in a vacuum drying oven for drying treatment after the absolute ethyl alcohol is volatilized, setting the drying temperature to be 120 ℃, setting the drying duration time to be 6 hours, placing the ball milling tank in a vacuum environment after drying, and cooling the ball milling tank to room temperature to obtain carbon-containing nickel-based superalloy powder;
s2: putting the powder dried in the step S1 into a powder feeder, filling argon gas serving as inert protective gas into a laser additive manufacturing forming bin, and starting a forming test after the oxygen content in the forming bin is reduced to 50 ppm; the optimized laser additive manufacturing process parameters are as follows: the laser power is 2000W, the diameter of a light spot is 5 mm, the scanning speed is 30 mm/s, the powder feeding amount is 15 g/min, the powder carrying airflow is 8L/min, the lap joint rate is 50%, and the lifting amount is 0.6 mm. Wherein the type of the used laser is a fiber laser, and the maximum output power is 10000W;
s3: carrying out a block forming test on the carbon-containing nickel-based superalloy powder obtained in the step S1 according to the optimized process parameters in the step S2, wherein the laser scanning path between layers is cross scanning, and the size of a formed sample is 80 multiplied by 10 multiplied by 20mm; cutting a sample along the deposition direction in a linear cutting mode to prepare a metallographic phase, sequentially grinding the surface of the sample by using #80, #180, #400, #1000 and #2000 SiC abrasive paper, and polishing; to observe the macroscopic and microscopic structure of the bulk sample, the polished sample was etched with an etchant (6 mL HCl + 2 mL H2O + 1g CrO) 3 ) Carrying out chemical corrosion; the dendrite morphology and the distribution characteristics of the second phase were analyzed using an optical microscope (OM, leica Microsystem DM-3000) and a field emission scanning electron microscope (FE-SEM, HITACHI SU 8010) as shown in fig. 2: from fig. 2, it can be seen that the macroscopic structure is still columnar dendrite, the content of chain Laves phase continuously distributed among dendrites is reduced, and the particulate carbide is dispersedly distributed, which indicates that the addition of trace carbon element has the effect of inhibiting the chain Laves phase, and brings beneficial effect on the strengthening and toughening of the material. The test data of yield strength, tensile strength and elongation of the prepared laser additive manufacturing nickel-based superalloy are shown in table 1.
Example 2
A method for reducing brittle Laves phase and improving strong plasticity in a laser additive manufacturing nickel-based high-temperature alloy, taking Inconel 625 nickel-based high-temperature alloy as an example, the alloy components are 63.59 Ni-21.5 Cr-8.5Mo-3.5 Nb-2.0 Fe-0.2 Ti-0.2 Al-0.5 Si-0.01C (mass percent), and the addition amount of carbon element in the alloy is 0.2 percent (mass percent);
s1: taking 2g of graphite powder with the particle size of 50nm and 998g of spherical Inconel 625 alloy powder with the particle size of 50-150 mu m (shown in figure 1), putting the graphite powder and the spherical Inconel 625 alloy powder into a stainless steel ball milling tank, adding absolute ethyl alcohol, putting the ball milling tank into a planetary ball mill for ball milling, wherein the ball milling process parameters are as follows: the rotating speed is 160r/min, the rotation is stopped for 30s after 5min, and then the rotation is carried out for 5min, and the whole powder mixing process lasts for 4h; after the powder mixing is finished, taking out the ball milling tank, placing the ball milling tank in a vacuum drying oven for drying treatment after the anhydrous ethanol volatilizes, setting the drying temperature to be 120 ℃, setting the drying duration time to be 6 hours, placing the ball milling tank in a vacuum environment after drying, and cooling the ball milling tank to room temperature;
s2: putting the powder dried in the step S1 into a powder feeder, filling argon as inert protective gas into a laser additive manufacturing forming bin, and starting a forming test after the oxygen content in the forming bin is reduced to 50 ppm; the optimized laser additive manufacturing process parameters are as follows: the laser power is 2000W, the diameter of a light spot is 5 mm, the scanning speed is 30 mm/s, the powder feeding amount is 15 g/min, the powder carrying airflow is 8L/min, the lap joint rate is 50%, and the lifting amount is 0.6 mm. Wherein the type of the used laser is a fiber laser, and the maximum output power is 10000W;
s3: carrying out a block forming test on the carbon-containing nickel-based superalloy powder obtained in the step S1 according to the optimized process parameters in the step S2, wherein the laser scanning path between layers is cross scanning, and the size of a formed sample is 80 multiplied by 10 multiplied by 20mm; cutting a sample along the deposition direction by adopting a linear cutting mode to prepare a metallographic phase, sequentially grinding the surface of the sample by using #80, #180, #400, #1000 and #2000 SiC abrasive paper, and polishing; to observe the macroscopic and microscopic structure of the bulk sample, the polished sample was etched with an etchant (6 mL HCl + 2 mL H2O + 1g CrO) 3 ) And carrying out chemical corrosion. The dendrite morphology and the distribution characteristics of the second phase were analyzed using an optical microscope (OM, leica Microsystem DM-3000) and a field emission scanning electron microscope (FE-SEM, HITACHI SU 8010) as shown in fig. 3: from fig. 3, it can be seen that the macroscopic structure is still columnar dendrite, the content of chain Laves phase continuously distributed among dendrites is reduced compared with the reference group without adding carbon element, and compared with example 1, the particulate carbide is still dispersed and distributed but the content thereof is gradually increased, which indicates that the addition of trace carbon element plays a role in inhibiting the chain Laves phase, and brings beneficial effect on the toughening of the material. The test data of yield strength, tensile strength and elongation of the prepared laser additive manufacturing nickel-based superalloy are shown in table 1.
Example 3
A method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity, taking Inconel 625 nickel-based high-temperature alloy as an example, the alloy components are 63.59 Ni-21.5 Cr-8.5Mo-3.5 Nb-2.0 Fe-0.2 Ti-0.2 Al-0.5 Si-0.01C (mass percent), and the addition amount of carbon element in the alloy is 0.4 percent (mass percent);
s1: taking 4g of graphite powder with the particle size of 50nm and 996g of spherical Inconel 625 alloy powder with the particle size of 50-150 mu m (shown in figure 1), putting the graphite powder and the spherical Inconel 625 alloy powder into a stainless steel ball milling tank, adding absolute ethyl alcohol, putting the ball milling tank into a planetary ball mill for ball milling, wherein the ball milling technological parameters are as follows: the rotating speed is 160r/min, the rotation is stopped for 30s after 5min, and then the rotation is carried out for 5min, and the whole powder mixing process lasts for 4h; after the powder mixing is finished, taking out the ball milling tank, placing the ball milling tank in a vacuum drying oven for drying treatment after the anhydrous ethanol volatilizes, setting the drying temperature to be 120 ℃, setting the drying duration to be 6 hours, placing the ball milling tank in a vacuum environment after drying, and cooling the ball milling tank to room temperature;
s2: and (3) putting the powder dried in the step (S1) into a powder feeder, filling argon gas serving as inert protective gas into a laser additive manufacturing forming bin, and starting a forming test after the oxygen content in the forming bin is reduced to 50 ppm. The optimized laser additive manufacturing process parameters are as follows: the laser power is 2000W, the diameter of a light spot is 5 mm, the scanning speed is 30 mm/s, the powder feeding amount is 15 g/min, the powder carrying airflow is 8L/min, the lapping rate is 50%, and the lifting amount is 0.6 mm. Wherein the type of the used laser is a fiber laser, and the maximum output power is 10000W;
s3: and (3) carrying out a block forming test on the carbon-containing nickel-based superalloy powder obtained in the step (S1) according to the optimized process parameters in the step (S2), wherein the laser scanning path between layers is cross scanning, and the size of a formed sample is 80 multiplied by 10 multiplied by 20mm. Cutting a sample along the deposition direction in a linear cutting mode to prepare a metallographic phase, sequentially grinding the surface of the sample by using #80, #180, #400, #1000 and #2000 SiC abrasive paper, and polishing; to observe the macroscopic and microscopic structure of the bulk sample, the polished sample was etched with an etchant (6 mL HCl + 2 mL H2O + 1g CrO) 3 ) Carrying out chemical corrosion; using an optical microscope (OM, leica Microsystem DM-3000) anda field emission scanning electron microscope (FE-SEM, HITACHI SU 8010) was used to analyze the dendrite morphology and the distribution characteristics of the second phase, as shown in fig. 4: from fig. 4, it can be seen that the macroscopic structure is still columnar dendrite, the content of chain Laves phase continuously distributed between dendrites is reduced compared with the reference group without adding carbon element, and compared with examples 1 and 2, the content of carbide is still dispersed but gradually increased, and the size of carbide is increased, which indicates that the addition of trace carbon element plays a role in inhibiting the chain Laves phase, and brings beneficial effect on the toughening of the material. The test data of yield strength, tensile strength and elongation of the prepared laser additive manufacturing nickel-based superalloy are shown in table 1.
Comparative example 1
The inhibiting effect of the added carbon element on the Laves phase is analyzed in a comparative way by taking the Inconel 625 nickel-based high-temperature alloy without the added carbon element as a reference group, and the alloy composition is 63.59 Ni-21.5 Cr-8.5Mo-3.5 Nb-2.0 Fe-0.2 Ti-0.2 Al-0.5 Si-0.01C (mass percent);
s1: placing spherical Inconel 625 alloy powder (shown in figure 1) with the particle size of 50-150 mu m in a vacuum drying oven for drying treatment, setting the drying temperature at 120 ℃, setting the drying duration time at 6h, and placing in a vacuum environment after drying to cool to room temperature;
s2: and (2) putting the powder dried in the step (S1) into a powder feeder, filling argon as inert protective gas into a laser additive manufacturing forming bin, and starting a forming test after the oxygen content in the forming bin is reduced to 50 ppm. The optimized laser additive manufacturing process parameters are as follows: the laser power is 2000W, the diameter of a light spot is 5 mm, the scanning speed is 30 mm/s, the powder feeding amount is 15 g/min, the powder carrying airflow is 8L/min, the lap joint rate is 50%, and the lifting amount is 0.6 mm. Wherein the type of the used laser is a fiber laser, and the maximum output power is 10000W;
s3: carrying out a block forming test on the nickel-based superalloy powder obtained in the step S1 according to the process parameters optimized in the step S2, wherein the laser scanning path between layers is cross scanning, and the size of a formed sample is 80 multiplied by 10 multiplied by 20mm; cutting a sample along the deposition direction by adopting a linear cutting mode to prepare a metallographic phase, and sequentially using SiC sands of #80, #180, #400, #1000 and #2000Grinding the surface of the sample by using paper, and polishing; to observe the macroscopic and microscopic structure of the bulk sample, the polished sample was etched with an etchant (6 mL HCl + 2 mL H2O + 1g CrO) 3 ) Carrying out chemical corrosion; the dendrite morphology and the distribution characteristics of the second phase were analyzed using an optical microscope (OM, leica Microsystem DM-3000) and a field emission scanning electron microscope (FE-SEM, HITACHI SU 8010) as shown in FIG. 6: from fig. 6, it can be seen that the Inconel 625 alloy without the added carbon element has a macrostructure of columnar dendrites, and dendritic phases are continuously distributed chain Laves phases, and the chain Laves phases seriously reduce the plasticity of the material. The test data of the yield strength, tensile strength and elongation of the prepared laser additive manufacturing nickel-based superalloy are shown in table 1.
Comparative example 2
When the addition amount of carbon element in the alloy is large, a large amount of carbide which is continuously distributed is formed, and the plasticity of the material is adversely affected. In addition, the content of carbon element in the conventional high temperature alloy is usually below 0.5% (mass percent), so the addition amount of carbon element in the alloy needs to be strictly controlled. Taking an Inconel 625 nickel-based superalloy as an example, the alloy components are 63.59 Ni-21.5 Cr-8.5Mo-3.5 Nb-2.0 Fe-0.2 Ti-0.2 Al-0.5 Si-0.01C (mass percent), and the addition amount of carbon in the alloy is 0.6% (mass percent) as a comparative example of the influence of the addition of excessive carbon on the laser additive manufacturing of the nickel-based superalloy structure.
S1: taking 6g of graphite powder with the particle size of 50nm and 994g of spherical Inconel 625 alloy powder with the particle size of 50-150 mu m (shown in figure 1), putting the graphite powder and the spherical Inconel 625 alloy powder into a stainless steel ball milling tank, adding absolute ethyl alcohol, putting the ball milling tank into a planetary ball mill for ball milling, wherein the ball milling process parameters are as follows: the rotating speed is 160r/min, the powder is positively rotated for 5min, then the powder is stopped for 30s and reversely rotated for 5min, and the whole powder mixing process lasts for 4h; after the powder mixing is finished, taking out the ball milling tank, placing the ball milling tank in a vacuum drying oven for drying treatment after the anhydrous ethanol volatilizes, setting the drying temperature to be 120 ℃, setting the drying duration to be 6 hours, placing the ball milling tank in a vacuum environment after drying, and cooling the ball milling tank to room temperature;
s2: and (3) putting the powder dried in the step (S1) into a powder feeder, filling argon gas serving as inert protective gas into a laser additive manufacturing forming bin, and starting a forming test after the oxygen content in the forming bin is reduced to 50 ppm. The optimized laser additive manufacturing process parameters are as follows: the laser power is 2000W, the diameter of a light spot is 5 mm, the scanning speed is 30 mm/s, the powder feeding amount is 15 g/min, the powder carrying airflow is 8L/min, the lapping rate is 50%, and the lifting amount is 0.6 mm. Wherein the type of the used laser is a fiber laser, and the maximum output power is 10000W;
s3: carrying out a block forming test on the carbon-containing nickel-based superalloy powder obtained in the step S1 according to the optimized process parameters in the step S2, wherein the laser scanning path between layers is cross scanning, and the size of a formed sample is 80 multiplied by 10 multiplied by 20mm; cutting a sample along the deposition direction in a linear cutting mode to prepare a metallographic phase, sequentially grinding the surface of the sample by using #80, #180, #400, #1000 and #2000 SiC abrasive paper, and polishing; in order to observe the macroscopic and microscopic structure of the bulk sample, the polished sample was etched with an etchant (6 mL HCl + 2 mL H2O + 1g CrO) 3 ) Carrying out chemical corrosion; the dendrite morphology and the distribution characteristics of the second phase were analyzed using an optical microscope (OM, leica Microsystem DM-3000) and a field emission scanning electron microscope (FE-SEM, HITACHI SU 8010) as shown in fig. 5: as can be seen from fig. 5, compared with the reference group without carbon element, the macroscopic structure is still columnar dendrite, the content of chain Laves phase continuously distributed among dendrites is reduced, and compared with examples 1, 2 and 3, the content of carbide is gradually increased, the size is gradually increased, and the morphology is gradually changed from granular to film-shaped, which shows that the addition of trace carbon element has the effect of inhibiting the chain Laves phase, but when the content of carbon is high, film-shaped carbide is formed, which has adverse effect on the plasticity of the material, so the content of carbon element in the alloy is strictly controlled. The test data of yield strength, tensile strength and elongation of the prepared laser additive manufacturing nickel-based superalloy are shown in table 1.
TABLE 1
| Yield Strength (YS)/MPa | Tensile Strength (UTS)/MPa | Elongation (δ)/%) | |
| Example 1 | 321.2 | 713.1 | 77.80 |
| Example 2 | 332.3 | 720.3 | 59.63 |
| Example 3 | 343.7 | 725.7 | 53.95 |
| Comparative example 1 | 316.7 | 696.6 | 49.65 |
| Comparative example 2 | 338.9 | 730.6 | 26.26 |
The above-described embodiments of the present invention are merely examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications in light of the above examples may be apparent to those skilled in the art. Not all embodiments are exemplified in detail herein. Obvious changes and modifications of the present invention are also within the scope of the present invention.
Claims (8)
1. A method for reducing brittle Laves phase and improving strong plasticity in a laser additive manufacturing nickel-based superalloy is characterized by comprising the following steps:
s1, wet mixing nano carbon powder and nickel-based high-temperature alloy powder in absolute ethyl alcohol according to a mass ratio, drying, and cooling to obtain carbon-containing nickel-based high-temperature alloy powder;
s2, putting carbon-containing nickel-based superalloy powder into a powder feeder, filling argon gas serving as inert protective gas into a laser additive manufacturing forming bin, starting a laser additive manufacturing forming test after the oxygen content in the forming bin is reduced to 50ppm, and obtaining technological parameters of laser additive manufacturing forming;
s3, performing a laser additive forming test on the carbon-containing nickel-based superalloy powder obtained in the step S1 according to the process parameters of laser additive manufacturing forming in the step S2 to obtain a defect-free high-density deposition-state sample, and performing microstructure analysis and mechanical property test on the deposition-state sample to determine the influence rule of introduction of carbon element on the volume fraction and distribution characteristics of a brittle Laves phase and improvement of alloy strong plasticity;
in the step S1, the mass compound ratio of the nano carbon powder to the nickel-based superalloy powder is (1-2): (998-999);
in the step S1, the nano carbon powder is selected from graphite powder with the particle size of 40-60 nm.
2. The method for reducing brittle Laves phase and improving ductility in laser additive manufacturing ni-based superalloy as claimed in claim 1, wherein the ni-based superalloy powder is selected from a solution strengthened ni-based superalloy or a precipitation strengthened ni-based superalloy; the particle size of the nickel-based superalloy powder in the coaxial powder feeding type directional energy deposition process is 50-150 mu m, and the particle size of the nickel-based superalloy powder in the selective laser melting process is 15-53 mu m.
3. The method for reducing the brittle Laves phase and improving the strong plasticity of the laser additive manufacturing nickel-based superalloy according to claim 1, wherein in the step S1, the wet mixing is performed by a planetary ball mill in absolute ethyl alcohol, the rotation speed of the planetary ball mill is 120-200 r/min during powder mixing, 30S is stopped after 3-5 min of forward rotation, and then 3-5 min of reverse rotation is performed, and the wet mixing time is 3-6 h; the drying is carried out in a vacuum drying oven at the temperature of 110-130 ℃ for 4-6 h.
4. The method for reducing the brittle Laves phase and improving the strong plasticity of the laser additive manufacturing nickel-base superalloy as claimed in claim 1, wherein in the step S2, the laser additive manufacturing forming is selected from a coaxial powder feeding type directional energy deposition process or a selective laser melting process; the type of the laser used in the coaxial powder feeding type directional energy deposition process is CO 2 The laser, the fiber laser or the semiconductor laser, the optimized technological parameters are as follows: the laser power is 1000-3000W, the diameter of a light spot is 2-5 mm, the scanning speed is 10-30 mm/s, the powder feeding amount is 8-20 g/min, the powder carrying gas flow is 4-10L/min, the lap joint rate is 40-60%, and the lifting amount is 0.4-0.6mm; the energy distribution of the laser is Gaussian distribution or bimodal distribution, and the shielding gas and the powder carrier are argon gas in the forming process; the laser used in the selective laser melting process is a fiber laser, and the optimized process parameters are as follows: the laser power is 180-300W, the spot diameter is 50-100 mu m, the scanning speed is 300-1200 mm/s, the scanning interval is 60-100 mu m, the powder laying thickness is 30-50 mu m, the used laser can be continuous laser or pulse laser, and the wavelength is 1060 nm.
5. The method for reducing the brittle Laves phase and improving the strong plasticity of the laser additive manufacturing ni-based superalloy as claimed in claim 4, wherein in step S2, the coaxial powder feeding type orientationThe laser type used in the energy deposition process is CO 2 The laser, the fiber laser or the semiconductor laser, the optimized technological parameters are as follows: the laser power is 1000-3000W, the diameter of a light spot is 2-5 mm, the scanning speed is 10-30 mm/s, the powder feeding amount is 8-20 g/min, the powder carrying gas flow is 4-10L/min, the lap joint rate is 40-60%, and the lifting amount is 0.4-0.6mm; the energy distribution of the laser is Gaussian distribution or bimodal distribution, and the protective gas and the powder carrier are argon gas in the forming process.
6. The method for reducing the brittle Laves phase and improving the plasticity of the ni-based superalloy manufactured by the laser additive manufacturing method according to claim 4, wherein in the step S2, the laser used in the selective laser melting process is a fiber laser, and the optimized process parameters are as follows: the laser power is 180-300W, the spot diameter is 50-100 mu m, the scanning speed is 300-1200 mm/s, the scanning interval is 60-100 mu m, the powder laying thickness is 30-50 mu m, the used laser can be continuous laser or pulse laser, and the wavelength is 1060 nm.
7. The method for reducing the brittle Laves phase and improving the toughness of the ni-based superalloy by laser additive manufacturing according to claim 1 or 5, wherein in step S3, when the coaxial powder feeding type directional energy deposition process is adopted for laser additive manufacturing forming, the laser scanning mode in the layer is unidirectional scanning or reciprocating scanning, and the laser scanning path between layers can be cross scanning or reciprocating scanning.
8. The method for reducing the brittle Laves phase and improving the plasticity of the ni-based superalloy manufactured by the laser additive manufacturing according to claim 1 or 6, wherein in the step S3, when the selective laser melting process is adopted for the laser additive manufacturing forming, the scanning mode in the layer is a unidirectional scanning or a reciprocating scanning, and the rotation angle between the layers is any one of 0 °, 90 ° or 67 °.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210683465.6A CN114799204B (en) | 2022-06-17 | 2022-06-17 | Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210683465.6A CN114799204B (en) | 2022-06-17 | 2022-06-17 | Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114799204A CN114799204A (en) | 2022-07-29 |
| CN114799204B true CN114799204B (en) | 2022-12-27 |
Family
ID=82522146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210683465.6A Active CN114799204B (en) | 2022-06-17 | 2022-06-17 | Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114799204B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4093454A (en) * | 1975-12-18 | 1978-06-06 | Mitsubishi Kinzoku Kabushiki Kaisha | Nickel-base sintered alloy |
| CN105112708A (en) * | 2015-09-16 | 2015-12-02 | 华中科技大学 | Rapid manufacturing method for laser remelting scanning carbide dispersion strengthened aluminum alloy |
| CN106077647A (en) * | 2016-07-27 | 2016-11-09 | 湖南大学 | A kind of laser gain material controls the method for fragility Laves phase during manufacturing nickel base superalloy |
| CN111500898A (en) * | 2020-06-19 | 2020-08-07 | 北京钢研高纳科技股份有限公司 | Nickel-based superalloy, method for producing same, component and use |
| CN113477940A (en) * | 2021-05-20 | 2021-10-08 | 暨南大学 | Method for manufacturing graphene reinforced nickel-based composite material through laser additive manufacturing and graphene reinforced nickel-based composite material |
| CN114480893A (en) * | 2021-12-31 | 2022-05-13 | 中南大学 | Method for reducing additive manufacturing cracks of nickel-based superalloy and nickel-based superalloy |
-
2022
- 2022-06-17 CN CN202210683465.6A patent/CN114799204B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4093454A (en) * | 1975-12-18 | 1978-06-06 | Mitsubishi Kinzoku Kabushiki Kaisha | Nickel-base sintered alloy |
| CN105112708A (en) * | 2015-09-16 | 2015-12-02 | 华中科技大学 | Rapid manufacturing method for laser remelting scanning carbide dispersion strengthened aluminum alloy |
| CN106077647A (en) * | 2016-07-27 | 2016-11-09 | 湖南大学 | A kind of laser gain material controls the method for fragility Laves phase during manufacturing nickel base superalloy |
| CN111500898A (en) * | 2020-06-19 | 2020-08-07 | 北京钢研高纳科技股份有限公司 | Nickel-based superalloy, method for producing same, component and use |
| WO2021254480A1 (en) * | 2020-06-19 | 2021-12-23 | 北京钢研高纳科技股份有限公司 | Nickel-based superalloy and manufacturing method therefor, and component and application |
| CN113477940A (en) * | 2021-05-20 | 2021-10-08 | 暨南大学 | Method for manufacturing graphene reinforced nickel-based composite material through laser additive manufacturing and graphene reinforced nickel-based composite material |
| CN114480893A (en) * | 2021-12-31 | 2022-05-13 | 中南大学 | Method for reducing additive manufacturing cracks of nickel-based superalloy and nickel-based superalloy |
Non-Patent Citations (1)
| Title |
|---|
| Rene104镍基高温合金选区激光熔化成形及开裂行为;段然曦等;《中国有色金属学报》;20180815;第28卷(第08期);第1568-1578页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114799204A (en) | 2022-07-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Basak et al. | Microstructure of nickel-base superalloy MAR-M247 additively manufactured through scanning laser epitaxy (SLE) | |
| Huang et al. | Simultaneously enhanced strength-ductility of AlCoCrFeNi2. 1 eutectic high-entropy alloy via additive manufacturing | |
| Lapin | TiAl-based alloys: Present status and future perspectives | |
| Qi et al. | Thermal expansion control of composite coatings on 42CrMo by laser cladding | |
| Ma et al. | Microstructures and mechanical properties of Ti6Al4V-Ti48Al2Cr2Nb alloys fabricated by laser melting deposition of powder mixtures | |
| Teng et al. | Effects of processing temperatures on FGH4097 superalloy fabricated by hot isostatic pressing: microstructure evolution, mechanical properties and fracture mechanism | |
| Hu et al. | Effects of TiC addition on microstructure, microhardness and wear resistance of 18Ni300 maraging steel by direct laser deposition | |
| Lu et al. | Evolution of interface carbide diamond brazed with filler alloy containing Cr | |
| Xia et al. | Circular oscillating laser melting deposition of nickel-based superalloy reinforced by WC: Microstructure, wear resistance and electrochemical properties | |
| Li et al. | Effects of WC particles on microstructure and mechanical properties of 316L steel obtained by laser melting deposition | |
| Das et al. | Direct laser fabrication of superalloy cermet abrasive turbine blade tips | |
| Xu et al. | Effect of B4C nanoparticles on microstructure and properties of laser cladded IN625 coating | |
| Zhang et al. | Combined effects of heat treatment and TiB2 content on the high-temperature tensile performance of TiB2-modified Ni-based GH3230 alloy processed by laser powder bed fusion | |
| Li et al. | In-situ fabrication of Ti2AlNb-based alloy through double-wire arc additive manufacturing | |
| CN113305285A (en) | Nickel-based superalloy metal powder for additive manufacturing | |
| Gong et al. | Microstructures of Inconel 718 by selective laser melting | |
| Sun et al. | Microstructure and properties of Inconel 718 matrix composite coatings reinforced with submicron TiC particles prepared by laser cladding | |
| Lu et al. | Effect of Cu-P-Sn on brazing diamond with Ni-based filler alloy | |
| Wei et al. | Microstructural evolution and mechanical properties of carbon nanotubes–reinforced TZM composites synthesized by powder metallurgy | |
| Yu et al. | High strength and toughness of in-situ TiC/In718 functionally gradient material by using Ti3AlC2 as a precursor | |
| Kong et al. | Additive manufacturing of high-strength Inconel 718 alloy through the addition of Ti2AlC MAX particles | |
| Liu et al. | Pulsed laser cladding on IN718 alloy using pre-coated CrCoNi-TiC/SiC powders for enhancing wear resistance | |
| CN114799204B (en) | Method for reducing brittle Laves phase in laser additive manufacturing nickel-based high-temperature alloy and improving strong plasticity | |
| Darolia et al. | Overview of NiAl alloys for high temperature structural applications | |
| CN114480901B (en) | Method for manufacturing nickel-based superalloy performance through carbide reinforced additive, nickel-based superalloy powder and application of nickel-based superalloy powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |