CN114807719A - Laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement - Google Patents
Laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement Download PDFInfo
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Abstract
The invention relates to a laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement, and belongs to the field of additive manufacturing of high-entropy alloys. The method aims to solve the problem that grains are easy to be large in the AlxCoFeNi high-entropy alloy as-cast sample structure; the invention utilizes a Laser Melting Deposition (LMD) additive manufacturing method, analyzes the hole distribution condition in a 3D printing sample by an X-ray computed tomography (X-CT) imaging technology, screens and optimizes the process parameter range according to the principle that the porosity is lower than 10 percent: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, the interlayer cooling time is 120-185 s, and a high-entropy alloy sample with high surface precision, high density, uniform components and refined structure is successfully prepared. Compared with an as-cast sample, the sample prepared by the LMD method has uniform components, the crystal grains are greatly refined, and the tensile yield strength and the breaking strain at room temperature can be improved by 27 percent to the maximum.
Description
Technical Field
The invention relates to a laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement, and belongs to the field of additive manufacturing of high-entropy alloys.
Background
High entropy alloys were produced by Taiwan scientists leaf of China, all in 1995. Different from the traditional alloy with one or two main elements, the high-entropy alloy has a plurality of main elements, so that the high-entropy alloy has a high-entropy effect, a delayed diffusion effect, a lattice distortion effect and a cocktail effect, and under the comprehensive action of the effects, the high-entropy alloy generally has a simple solid solution phase structure such as a body-centered cubic structure (BCC), a face-centered cubic structure (FCC), a close-packed hexagonal structure (HCP) and the like, and simultaneously has excellent mechanical properties such as high hardness, high strength, high wear resistance and the like, thereby becoming a hotspot in the field of metal material research. At present, the method for preparing the high-entropy alloy mainly comprises vacuum arc melting, powder metallurgy and the like, but the cast alloy prepared by the method has simple shape, has higher requirements on the fluidity, the melting point and the like of the alloy, has high cooling speed, forms coarse structure grains, is easy to generate segregation, and cannot thoroughly eliminate the problem of uneven component distribution even repeatedly remelting for many times, thereby greatly influencing the performance of the high-entropy alloy and severely limiting the industrial application of the high-entropy alloy.
The AlxCoFeNi series high-entropy alloy has been researched, the alloy enhances the overall performance of the alloy by adding Al element into CoFeNi ternary alloy, and with the addition of the Al element, the alloy can generate the phase transformation of FCC-FCC + BCC-BCC, and the hardness and the strength of the alloy are increased. The research is mainly to improve the alloy performance through a series of post-treatment methods such as heat treatment, rolling and the like on the basis of an as-cast state, and the processes are complicated, so that resources and time are greatly consumed, and the industrial application cost is greatly increased. Laser Melting Deposition (LMD), as a new additive manufacturing technology, is an additive manufacturing method that uses laser as an energy source and melts metal powder fed synchronously according to a preset path to deposit the metal powder layer by layer until molding. The method has the advantages that the metal workpiece with uniform components, fine tissue, complex geometric shape and high dimensional precision can be rapidly prepared, the subsequent processing process is omitted, and the preparation efficiency is high. Because the laser additive manufacturing process is controlled by various process parameters, such as laser power, spot diameter, scanning speed and the like, each parameter and different parameter combinations have different influences on the structure and performance of the workpiece, for example, too much laser power can cause overheating of the workpiece and even burn through the workpiece, and too little laser power can cause incomplete melting of powder, thereby reducing the compactness of the workpiece; too large a scanning speed may result in low temperatures and incomplete melting of the powder, while too small a scanning speed may result in too much concentration of laser heat, thereby creating overheating problems. If the process parameters are not properly selected, the effect of laser additive manufacturing is affected, and even the structure and the performance of the high-entropy alloy are deteriorated. Therefore, it is a main research trend to optimize the process parameters to obtain high-entropy alloys with fine microstructures and better mechanical properties.
Disclosure of Invention
The invention aims to solve the problem of large grains easily appearing in the as-cast sample structure of the AlxCoFeNi high-entropy alloy, and provides a laser melting deposition method for realizing the grain refinement of the AlxCoFeNi high-entropy alloy. The laser melting deposition method provided by the invention optimizes process parameters, can realize the refinement of AlxCoFeNi high-entropy alloy structure, and can simultaneously improve the strength and the plasticity.
The purpose of the invention is realized by the following technical scheme;
an AlxCoFeNi high-entropy alloy comprises four elements of aluminum (Al), cobalt (Co), iron (Fe) and nickel (Ni), wherein the atomic percent of Al is 3.1-9.1%, the atomic percent of Co is 30.3-32.3%, the atomic percent of Fe is 30.3-32.3%, and the atomic percent of Ni is 30.3-32.3%; the four elements are composed in a single phase Face Centered Cubic (FCC) structure.
A laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement comprises the following steps:
the method comprises the following steps: placing the AlxCoFeNi high-entropy alloy spherical powder in a drying box of printing equipment, drying for 1-2 hours, carrying out air blowing cleaning on a powder feeder, and then filling the high-entropy alloy powder;
the AlxCoFeNi high-entropy alloy spherical powder comprises four elements of aluminum (Al), cobalt (Co), iron (Fe) and nickel (Ni), wherein the atomic percent of Al is 3.1-9.1%, the atomic percent of Co is 30.3-32.3%, the atomic percent of Fe is 30.3-32.3%, and the atomic percent of Ni is 30.3-32.3%;
step two: mechanically polishing a 316 stainless steel substrate until the substrate is bright and free of impurities, sealing the equipment, introducing argon with the purity of 99.999 wt% into a processing chamber, and controlling the oxygen water content of the processing chamber to be not more than 50 ppm;
step three: the process parameters of laser melting deposition are preliminarily set as follows: the laser power is 1800-2600W, the scanning speed is 540-900 mm/min, the powder feeding speed is 4-9 g/min, the diameter of a light spot is 1.5-4 mm, the thickness of the layer is 0.3-0.6 mm, the scanning distance is 2-3.5 mm, and the interlayer cooling time is 60-200 s;
step four: adjusting the height between the laser beam and the 316 stainless steel substrate, and printing the laser beam layer by layer according to a preset scanning path under the protection of high-purity argon according to the process parameters in the third step;
step five: and observing the layer-by-layer deposition capability and the forming quality of the sample constantly in the printing process, detecting the pore distribution of the workpiece by an X-CT (X-ray computed tomography) technology, and obtaining the optimal process parameters according to the principle of low porosity as follows: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, and the interlayer cooling time is 120-185 s;
step six: and printing according to the optimized process parameters to obtain a thin-wall sample with high surface precision, high density and uniform tissue components, and cutting the printed thin-wall sample from the substrate by using a linear cutting method to obtain a molded high-entropy alloy sample.
The particle size range of the spherical powder in the first step is 45-105 μm.
In the fourth step, the initial distance from the laser nozzle to the substrate is 17-18 mm, and the distance from the laser nozzle to each layer in the layer-by-layer printing process is kept at 17-18 mm.
In the fourth step, the scanning path of the laser beam is unidirectional scanning, and the interlayer scanning direction rotates by 180 degrees.
The preferable parameter condition in the fifth step is that the porosity of the workpiece is less than 10%.
Advantageous effects
1. Compared with an as-cast sample obtained by arc melting, the AlxCoFeNi high-entropy alloy printed by the optimized process parameters has the advantages of high density, uniform tissue components, refined grains, higher room-temperature tensile yield strength and plasticity.
2. The laser melting deposition method provided by the invention is simple to operate and high in efficiency, and the printed sample is high in dimensional accuracy and good in surface quality, so that a large number of surface layers are not required to be cut off in the subsequent sampling analysis, and the material utilization rate is improved.
Drawings
FIG. 1 is an Optical Microscope (OM) view of an Al0.1CoFeNi high-entropy alloy prepared by arc melting and laser melting deposition; wherein, the picture (a) is an alloy structure picture prepared by arc melting, and the picture (b) is an alloy structure picture prepared by laser melting deposition.
FIG. 2 is an Optical Microscope (OM) diagram of the preparation of Al0.2CoFeNi high-entropy alloy by electric arc melting and laser melting deposition; wherein, the picture (a) is an alloy structure picture prepared by arc melting, and the picture (b) is an alloy structure picture prepared by laser melting deposition.
FIG. 3 is an Optical Microscope (OM) view of an Al0.3CoFeNi high-entropy alloy prepared by arc melting and laser melting deposition; wherein, the picture (a) is an alloy structure picture prepared by arc melting, and the picture (b) is an alloy structure picture prepared by laser melting deposition.
FIG. 4 is a room temperature tensile engineering stress-strain curve for preparing AlxCoFeNi high entropy alloy by arc melting and laser melting deposition; wherein, the graph (a) is Al0.1CoFeNi high-entropy alloy, the graph (b) is Al0.2CoFeNi high-entropy alloy, and the graph (c) is Al0.3CoFeNi high-entropy alloy.
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
Example 1
The present example is an al0.1cofeni high entropy alloy, which is composed of four elements, i.e., Al, Co, Fe, Ni, etc., wherein the relative atomic percentage content of Al is 3.1%, the relative atomic percentage content of Co is 32.3%, the relative atomic percentage content of Fe is 32.3%, and the relative atomic percentage content of Ni is 32.3%.
The purity of the metal raw materials such as Al, Co, Fe, Ni and the like is higher than 99.99 wt%;
the laser melting deposition preparation method of the Al0.1CoFeNi high-entropy alloy comprises the following steps:
the method comprises the following steps: taking 1Kg of Al0.1CoFeNi high-entropy alloy prealloy powder with the particle size range of 45-105 mu m, putting the powder into a drying oven, and drying for 1-2 hours, so as to ensure that the powder with good fluidity and enough dryness is obtained, and avoid the adhesion of the powder due to water. Cleaning a powder feeder of the printing equipment until no other impurities exist, and adding 1Kg of dried alloy powder for later use.
Step two: a316 stainless steel substrate is selected as a printing substrate, an oxidation layer on the surface of the substrate is polished by a grinding machine until the surface is bright, and impurities are blown off. Closing the processing chamber of the equipment, introducing high-purity argon with the purity of 99.999 wt%, and strictly controlling the oxygen water content of the processing chamber to be not more than 50ppm so as to prevent the material from being oxidized during printing.
Step three: in order to further screen out the optimized process parameters, printing is firstly carried out in a wider parameter range, so the process parameters of laser melting deposition are preliminarily set as follows: the laser power is 1800-2600W, the scanning speed is 540-900 mm/min, the powder feeding speed is 4-9 g/min, the diameter of a light spot is 1.5-4 mm, the thickness of the layer is 0.3-0.6 mm, the scanning distance is 2-3.5 mm, and the interlayer cooling time is 60-200 s;
step four: adjusting the height between the laser beam and a 316 stainless steel substrate to be 17-18 mm, and printing the laser beam layer by layer according to a preset scanning path under the protection of high-purity argon according to preliminary process parameters;
step five: and (3) observing the layer-by-layer deposition capability and the forming quality of the sample constantly in the printing process, detecting the hole distribution condition of the workpiece by an X-ray computed tomography (X-CT) technology after forming, and directly rejecting a corresponding process parameter group if the workpiece has obvious large-size defects. According to the principle that the distribution concentration degree of the holes in the sample is low, the hole volume is small, the number of the holes is small, and the porosity is lower than 10%, comparing and screening the initial process parameters to obtain the optimal process parameters: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, and the interlayer cooling time is 120-185 s;
step six: and printing according to the optimized process parameters to obtain a thin-wall sample with high surface precision, high density and uniform tissue components, and cutting the printed thin-wall sample from the substrate by using a linear cutting method to obtain a molded high-entropy alloy sample.
Example 2
The Al0.2CoFeNi high-entropy alloy is composed of four elements including Al, Co, Fe, Ni and the like, wherein the relative atomic percent content of Al is 6.1%, the relative atomic percent content of Co is 31.3%, the relative atomic percent content of Fe is 31.3%, and the relative atomic percent content of Ni is 31.3%.
The purity of the metal raw materials such as Al, Co, Fe, Ni and the like is higher than 99.99 wt%;
the laser melting deposition preparation method of the Al0.2CoFeNi high-entropy alloy comprises the following steps:
the method comprises the following steps: taking 1Kg of Al0.2CoFeNi high-entropy alloy prealloy powder with the particle size range of 45-105 mu m, putting the powder into a drying oven, and drying for 1-2 hours, so as to ensure that the powder with good fluidity and enough dryness is obtained, and avoid the adhesion of the powder due to water. Cleaning a powder feeder of the printing equipment until no other impurities exist, and adding 1Kg of dried alloy powder for later use.
Step two: a316 stainless steel substrate is selected as a printing substrate, an oxidation layer on the surface of the substrate is polished by a grinding machine until the surface is bright, and impurities are blown off. Closing the processing chamber of the equipment, introducing high-purity argon with the purity of 99.999 wt%, and strictly controlling the oxygen water content of the processing chamber to be not more than 50ppm so as to prevent the material from being oxidized during printing.
Step three: in order to further screen out the optimized process parameters, printing is firstly carried out in a wider parameter range, so that the process parameters of laser melting deposition are preliminarily set as follows: the laser power is 1800-2600W, the scanning speed is 540-900 mm/min, the powder feeding speed is 4-9 g/min, the diameter of a light spot is 1.5-4 mm, the thickness of the layer is 0.3-0.6 mm, the scanning distance is 2-3.5 mm, and the interlayer cooling time is 60-200 s;
step four: adjusting the height between the laser beam and a 316 stainless steel substrate to be 17-18 mm, and printing the laser beam layer by layer according to a preset scanning path under the protection of high-purity argon according to preliminary process parameters;
step five: and (3) observing the layer-by-layer deposition capability and the forming quality of the sample constantly in the printing process, detecting the hole distribution condition of the workpiece by an X-ray computed tomography (X-CT) technology after forming, and directly rejecting a corresponding process parameter group if the workpiece has obvious large-size defects. According to the principle that the distribution concentration degree of the holes in the sample is low, the hole volume is small, the number of the holes is small, and the porosity is lower than 10%, comparing and screening the initial process parameters to obtain the optimal process parameters: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, and the interlayer cooling time is 120-185 s;
step six: and printing according to the optimized process parameters to obtain a thin-wall sample with high surface precision, high density and uniform tissue components, and cutting the printed thin-wall sample from the substrate by using a linear cutting method to obtain a molded high-entropy alloy sample.
Example 3
The alloy is an Al0.3CoFeNi high-entropy alloy and is composed of Al, Co, Fe, Ni and other four elements, wherein the relative atomic percent content of Al is 9.1%, the relative atomic percent content of Co is 30.3%, the relative atomic percent content of Fe is 30.3%, and the relative atomic percent content of Ni is 30.3%.
The purity of the metal raw materials such as Al, Co, Fe, Ni and the like is higher than 99.99 wt%;
the laser melting deposition preparation method of the Al0.3CoFeNi high-entropy alloy comprises the following steps:
the method comprises the following steps: taking 1Kg of Al0.3CoFeNi high-entropy alloy prealloy powder with the particle size range of 45-105 mu m, putting the Al0.3CoFeNi high-entropy alloy prealloy powder into a drying box, and drying for 1-2 hours, so that powder with good fluidity and enough dryness is ensured to be obtained, and adhesion of the powder due to water is avoided. Cleaning a powder feeder of the printing equipment until no other impurities exist, and adding 1Kg of dried alloy powder for later use.
Step two: a316 stainless steel substrate is selected as a printing substrate, an oxidation layer on the surface of the substrate is polished by a grinding machine until the surface is bright, and impurities are blown off. Closing the processing chamber of the equipment, introducing high-purity argon with the purity of 99.999 wt%, and strictly controlling the oxygen water content of the processing chamber to be not more than 50ppm so as to prevent the material from being oxidized during printing.
Step three: in order to further screen out the optimized process parameters, printing is firstly carried out in a wider parameter range, so that the process parameters of laser melting deposition are preliminarily set as follows: the laser power is 1800-2600W, the scanning speed is 540-900 mm/min, the powder feeding speed is 4-9 g/min, the diameter of a light spot is 1.5-4 mm, the thickness of the layer is 0.3-0.6 mm, the scanning distance is 2-3.5 mm, and the interlayer cooling time is 60-200 s;
step four: adjusting the height between the laser beam and a 316 stainless steel substrate to be 17-18 mm, and printing the laser beam layer by layer according to a preset scanning path under the protection of high-purity argon according to preliminary process parameters;
step five: and (3) observing the layer-by-layer deposition capability and the forming quality of the sample constantly in the printing process, detecting the hole distribution condition of the workpiece by an X-ray computed tomography (X-CT) technology after forming, and directly rejecting a corresponding process parameter group if the workpiece has obvious large-size defects. According to the principle that the distribution concentration degree of the holes in the sample is low, the hole volume is small, the number of the holes is small, and the porosity is lower than 10%, comparing and screening the initial process parameters to obtain the optimal process parameters: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, and the interlayer cooling time is 120-185 s;
step six: and printing according to the optimized process parameters to obtain a thin-wall sample with high surface precision, high density and uniform tissue components, and cutting the printed thin-wall sample from the substrate by using a linear cutting method to obtain a molded high-entropy alloy sample.
The AlxCoFeNi samples obtained by the arc melting and the laser melting deposition method were subjected to Optical Microscope (OM) characterization and room temperature tensile mechanical property test, as shown in fig. 1 to 4, respectively. Experiments show that: the as-cast structure has coarse grains of 500 to 600 μm as shown in (a) of FIGS. 1 to 3; the high-entropy alloy microstructure prepared by the laser melting deposition method has equiaxial grains as small as-50 μm, as shown in (b) of fig. 1-3; the room temperature yield strength, tensile strength, and strain at break of the alloy prepared by the laser melting deposition method were all higher than those of the corresponding alloy as-cast sample, as shown in fig. 4.
The foregoing is a description of the preferred embodiments of the present invention. It should be noted that the present invention is not limited to the above embodiments, and any modifications, equivalent replacements, or improvements that can be made to the present invention are included in the protection scope of the present invention when the scope of the claims, the summary of the invention, and the accompanying drawings are satisfied.
Claims (7)
1. A laser melting deposition method for realizing AlxCoFeNi high-entropy alloy grain refinement is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: placing the AlxCoFeNi high-entropy alloy spherical powder in a drying box of printing equipment, drying for 1-2 hours, carrying out air blowing cleaning on a powder feeder, and then filling the high-entropy alloy powder;
the AlxCoFeNi high-entropy alloy spherical powder comprises four elements of aluminum, cobalt, iron and nickel, wherein the atomic percent of Al is 3.1-9.1%, the atomic percent of Co is 30.3-32.3%, the atomic percent of Fe is 30.3-32.3%, and the atomic percent of Ni is 30.3-32.3%;
step two: mechanically polishing a 316 stainless steel substrate until the substrate is bright and free of impurities, sealing the equipment, introducing argon with the purity of 99.999 wt% into a processing chamber, and controlling the oxygen water content of the processing chamber to be not more than 50 ppm;
step three: the process parameters of laser melting deposition are preliminarily set as follows: the laser power is 1800-2600W, the scanning speed is 540-900 mm/min, the powder feeding speed is 4-9 g/min, the diameter of a light spot is 1.5-4 mm, the thickness of the layer is 0.3-0.6 mm, the scanning distance is 2-3.5 mm, and the interlayer cooling time is 60-200 s;
step four: adjusting the height between the laser beam and the 316 stainless steel substrate, and printing the laser beam layer by layer according to a preset scanning path according to the process parameters optimized on the basis of the third step under the protection of high-purity argon; and obtaining a thin-wall sample with high surface precision, high density and uniform tissue components, and cutting the printed thin-wall sample from the substrate by using a linear cutting method to obtain a formed high-entropy alloy sample.
2. The method of claim 1, wherein: fourthly, the optimized process parameters are as follows: the laser power is 2000-2500W, the scanning speed is 600-850 mm/min, the powder feeding speed is 5-7 g/min, the diameter of a light spot is 2-3.5 mm, the thickness of the layer is 0.4-0.55 mm, the scanning distance is 2-2.5 mm, and the interlayer cooling time is 120-185 s.
3. The method of claim 1, wherein: the granularity of the spherical powder in the first step is 45-105 μm.
4. The method of claim 1, wherein: in the fourth step, the initial distance from the laser nozzle to the substrate is 17-18 mm, and the distance from the laser nozzle to each layer in the layer-by-layer printing process is kept to be 17-18 mm.
5. The method of claim 1, wherein: in the fourth step, the scanning path of the laser beam is unidirectional scanning, and the interlayer scanning direction rotates by 180 degrees.
6. The method of claim 1, wherein: the selection condition of the optimized parameters in the fourth step is that the porosity of the workpiece is lower than 10%.
7. An AlxCoFeNi high entropy alloy produced by the method of any one of claims 1 to 6, characterized in that: the single-phase face-centered cubic (FCC) structure is composed of four elements of aluminum, cobalt, iron and nickel.
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| CN117230336A (en) * | 2023-09-19 | 2023-12-15 | 上海大学 | Method for preparing high-entropy alloy |
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