CN114411035B - Precipitation strengthening type medium-entropy alloy suitable for laser additive manufacturing and preparation method thereof - Google Patents
Precipitation strengthening type medium-entropy alloy suitable for laser additive manufacturing and preparation method thereof Download PDFInfo
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Abstract
The invention provides a precipitation-strengthened type medium entropy alloy suitable for laser additive manufacturing and a preparation method thereof, wherein the precipitation-strengthened type medium entropy alloy is Ni a Co b Cr c Al d M e Wherein M is one or more elements of Ti, ta, nb and Mo, a, b, c, d and e respectively represent the mole percentage of the corresponding elements, b =20% -40%, c =20% -25%, d>1％，e>0，d+e<7%, a + b + c + d + e =100%. The precipitation-strengthened type intermediate entropy alloy is prepared by adopting a selective laser melting forming technology or a three-dimensional laser forming technology, so that the preparation of the novel precipitation-strengthened type intermediate entropy alloy with high compactness, no crack and excellent comprehensive mechanical properties is realized.
Description
Technical Field
The invention relates to the technical field of laser additive manufacturing of metal materials, in particular to a precipitation-strengthened type medium-entropy alloy suitable for laser additive manufacturing and a preparation method thereof.
Background
The high/medium entropy alloy adopts a brand-new alloy design strategy and adopts a plurality of main elements with equal concentration or near equal concentration as alloy elements, shows excellent combination of strength, ductility and fracture toughness, and has wide structuralization and functionalization application prospects. The high/medium entropy alloy with the FCC structure shows good toughness but the strength is generally low, and the application requirement of structural materials is difficult to meet.
The traditional preparation method of the high/medium entropy alloy mainly adopts electric arc melting, has the defects of single shape and size, easy occurrence of composition segregation, shrinkage porosity, shrinkage cavity and the like, is difficult to form a fully-compact high-performance high/medium entropy alloy part with a complex structure, and greatly limits the further application and development of the high/medium entropy alloy.
The laser additive manufacturing technology is based on the principle that materials accumulate point by point, line by line and layer by layer, and achieves near-net forming of complex structures or customized parts through the rapid action of high-energy laser beams and metal powder and extremely high manufacturing flexibility. The technology has the advantages of high material utilization rate, high flexibility in the manufacturing process, short period, uniform and fine microstructure and the like, and provides huge potential for preparing high/medium entropy alloy components with excellent comprehensive performance, high precision, full compactness and complex shapes. However, high temperature gradients and large cooling rates during additive manufacturing often result in high thermal residual stresses and are prone to metallurgical defects such as cracks. Particularly for precipitation-strengthened high/medium entropy alloys, defects such as liquefaction cracking, strain aging cracking and the like are easily generated in the printing process, and the structural integrity and the comprehensive performance of the component are influenced. Therefore, designing a precipitation-strengthened high/medium entropy alloy suitable for laser additive manufacturing is a key problem to be solved urgently in the field.
Disclosure of Invention
The invention aims to overcome the defects of the traditional preparation method of the high/medium entropy alloy, provides the precipitation strengthening type medium entropy alloy suitable for laser additive manufacturing and the preparation method thereof, and realizes the preparation of the novel precipitation strengthening type medium entropy alloy which is high in compactness, free of cracks and excellent in comprehensive mechanical property.
The invention is realized by the following technical scheme:
precipitation-strengthened type medium-entropy alloy suitable for laser additive manufacturing, wherein the precipitation-strengthened type medium-entropy alloy is Ni a Co b Cr c Al d M e Wherein M is one or more elements of Ti, ta, nb and Mo, a, b, c, d and e respectively represent the mol percent of the corresponding elements, and b =20%-40％，c＝20％-25％，d>1％，e>0，d+e<7％，a+b+c+d+e＝100％。
Preferably, the preparation is carried out by using a selective laser melting forming technology.
Further, the method comprises the following steps:
According to the mol percent of the alloy powder as claimed in claim 1, taking metal raw materials corresponding to each element, preparing the medium-entropy alloy prealloy spherical powder by a vacuum gas atomization method, sieving and drying to obtain the medium-entropy alloy powder;
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into a file with an STL format, importing the file into construction software of selective laser melting forming equipment, and carrying out layering treatment; and introducing high-purity argon to ensure that the oxygen content in the forming cabin is lower than 300ppm, and melting and forming the medium-entropy alloy powder layer by layer according to the set technological parameters and scanning strategy for selective laser melting and forming to prepare the medium-entropy alloy component.
Further, the technological parameters of selective laser melting forming are as follows: the laser power P is 160-360W, the scanning speed v is 600-1000 mm/s, the scanning interval h is 60-80 μm, the powder layer thickness t is 30-50 μm, the spot diameter is 80 μm, and the energy density VED range is 140J/mm 3 <VED<240J/mm 3 Wherein VED = P/vht.
Further, the scanning strategy is 67 ° rotation scanning, reciprocating interlaced scanning or 45 ° rotation sector scanning.
Further, the method also comprises the following heat treatment steps: and heating the medium-entropy alloy component to 600-800 ℃, preserving heat for 12h or more and t or less than 480h, and cooling by water after heat preservation is finished to obtain the heat-treated medium-entropy alloy.
Preferably, the preparation is carried out by using a laser stereolithography technology.
Further, the method comprises the following steps:
According to the mol percent of the alloy powder as claimed in claim 1, taking metal raw materials corresponding to each element, preparing the medium-entropy alloy prealloy spherical powder by a vacuum gas atomization method, sieving and drying to obtain the medium-entropy alloy powder;
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into an STL format, transmitting the STL format to laser three-dimensional forming equipment, setting printing process parameters and a laser scanning path, transmitting the medium-entropy alloy powder into a molten pool formed by high-energy laser beams in the laser three-dimensional forming equipment, and printing to obtain the medium-entropy alloy component by depositing raw materials on a base material point by point, line by line and layer by layer.
Further, the printing process parameters are as follows: the laser power is 2 KW-3.5 KW, the scanning speed is 300-800 mm/min, the powder feeding speed is 5-8g/min, the Z-axis lifting amount is 0.4-1.0mm, the overlapping rate is 50%, the spot diameter is 3mm, and the scanning path is a reciprocating interweaving scanning path.
Further, the method also comprises the following heat treatment steps: and heating the medium-entropy alloy component to 600-800 ℃, preserving the heat for 3h or more and t or less than 480h, and cooling by water after the heat preservation is finished to obtain the heat-treated medium-entropy alloy.
Compared with the prior art, the invention has the following beneficial effects:
the invention designs precipitation strengthening type medium entropy alloy suitable for laser additive manufacturing, namely Ni a Co b Cr c Al and Ti, ta, nb or Mo elements are added into the matrix in a multi-principal component mode, so that the generation of a gamma 'phase is promoted, and the strengthening effect of a gamma' precipitated phase is obviously enhanced. The sum of Al, ti, ta, nb and Mo is regulated to be less than 7 percent, so that on one hand, the problems of poor formability in the additive manufacturing process and the like caused by a gamma' phase with high volume fraction are solved, namely, the high susceptibility of the alloy to liquefaction cracking, strain aging cracking and the like in laser additive manufacturing is reduced; on the other hand, a gamma' precipitate phase having an excellent strengthening effect can be obtained. The invention is according toThe formula respectively adopts the selective laser melting forming technology and the three-dimensional laser forming technology to realize the preparation of the novel precipitation-strengthened type medium-entropy alloy with high compactness, no crack and excellent comprehensive mechanical property.
Furthermore, the generation of a gamma' precipitated phase is promoted by carrying out heat treatment on a laser additive manufacturing sample, and a non-uniform structure with partial recrystallization is obtained, so that the comprehensive mechanical property of the precipitation strengthening type entropy alloy designed by the invention is greatly improved, and the further strengthening and toughening of the entropy alloy in laser additive manufacturing are realized.
Drawings
FIG. 1 shows selective laser melting of Ni 35 Co 35 Cr 25 Ti 3 Al 2 The shape of the medium-entropy alloy powder.
FIG. 2 shows Ni prepared by selective laser melting in example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 A medium entropy alloy block sample.
FIG. 3 shows Ni prepared by selective laser melting in example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 The density of the medium entropy alloy is along with the change rule of the energy density of the body.
FIG. 4 shows Ni prepared by casting and selective laser melting in example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Scanning electron microscope pictures of the medium entropy alloy, wherein (a) is an as-cast state and (b) is a as-deposited state.
FIG. 5 shows Ni formed by selective melting of as-cast and laser-formed Ni according to example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Room temperature tensile stress-strain curves for the mid-entropy alloys.
FIG. 6 shows selective laser melting of Ni in example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Scanning electron microscope picture (a) and transmission electron microscope selected area electron diffraction picture (b) of the medium entropy alloy after 600 ℃/12h heat treatment.
FIG. 7 shows selective laser melting of Ni according to example 1 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 And (3) carrying out room-temperature tensile stress-strain curves on the medium-entropy alloy after different heat treatment temperatures and times.
FIG. 8 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 The shape of the medium-entropy alloy powder.
FIG. 9 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 A medium entropy alloy block sample.
FIG. 10 shows Ni prepared with different laser powers in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Room temperature tensile stress-strain curves for the mid-entropy alloys.
FIG. 11 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Microstructure characteristics of the medium entropy alloy.
FIG. 12 shows the preparation of Ni by using the optimized laser stereolithography process parameters in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Room temperature tensile stress-strain curves for the mid-entropy alloys.
FIG. 13 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Scanning electron microscope pictures of the medium entropy alloy after heat treatment.
FIG. 14 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 And (3) the microhardness of the medium-entropy alloy after heat treatment.
FIG. 15 shows laser stereolithography of Ni in example 2 of the present invention 35 Co 35 Cr 25 Ti 3 Al 2 Room temperature tensile stress-strain curve of the medium entropy alloy after 700 ℃/3h heat treatment (LSF-HT).
Detailed Description
For a further understanding of the invention, reference will now be made to the following examples, which are provided to illustrate further features and advantages of the invention, and are not intended to limit the scope of the invention as set forth in the following claims.
The precipitation-strengthened medium-entropy alloy with excellent strong plasticity suitable for laser additive manufacturing comprises Ni as an alloy component a Co b Cr c Al d M e Wherein a, b, c, d, e represent the mole percentages of the respective elements, a is the balance, b =20-40at.%, c =20-25at.%, d>1at.％，e>0，d+e<7at.%, a + b + c + d + e =100at.%, the trace elements M comprise one or more components of Ti, ta, nb, mo. The selected medium-entropy alloy is pre-alloyed spherical powder prepared by a vacuum gas atomization method or a plasma rotating electrode method, and the purity of the pre-alloyed spherical powder is more than 99.9%.
The invention provides a preparation method of the laser selective melting forming technology of the precipitation strengthening type medium entropy alloy, which comprises the following steps:
1. preparation and pretreatment of medium-entropy alloy powder
Proportioning according to the mole percentage of each element in the nominal chemical components of the medium-entropy alloy, preparing medium-entropy alloy pre-alloyed spherical powder by a vacuum gas atomization method, and sieving the pre-alloyed spherical powder, wherein the particle size of the powder is 15-53 mu m. The oxygen content and nitrogen content are less than 300ppm, preferably 131ppm and 53ppm. Before selective laser melting, the pre-alloyed spherical powder is dried at 80 ℃ for 4 hours to remove water in the powder, and then the powder is placed in a powder feeding cylinder of selective laser melting equipment.
2. Surface treatment of substrates
Selecting a stainless steel or carbon steel substrate, polishing the surface to be deposited, cleaning the surface with acetone and alcohol in sequence to remove surface oil stains, then drying the surface oil stains, and mounting the substrate on a forming platform and leveling the substrate. Prior to printing, the substrate is preheated to 100-200 ℃, preferably 200 ℃.
3. Selective laser melting of Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing three-dimensional solid model on computer, converting into STL format file, and introducing into laser selection areaIn the build software of the melt forming apparatus, a layering process is performed. The technological parameters of selective laser melting and forming are as follows: the laser power P is 160-360W, the scanning speed v is 600-1000 mm/s, the scanning interval h is 60-80 μm, the powder layer thickness t is 30-50 μm, the spot diameter is 80 μm, and the scanning strategy can select 67-degree rotary scanning, reciprocating interweaving scanning and 45-degree rotary partition scanning paths. Before printing, high-purity argon gas with the purity of 99.99wt.% is introduced, so that the oxygen content in the forming chamber is lower than 300ppm. According to the set technological parameters and scanning path of selective laser melting and forming, ni is added a Co b Cr c Al d M e And melting and forming the medium-entropy alloy pre-alloyed spherical powder layer by layer to prepare a block sample. The invention adopts a selective laser melting and forming mode to prepare Ni a Co b Cr c Al d M e Separating out strengthened medium entropy alloy, selecting optimized laser selective melting forming technological parameter, namely high volume energy density VED (140J/mm) 3 <VED<240J/mm 3 VED = P/vht), the compactness of the printing alloy can be greatly improved, the comprehensive mechanical property of the printing alloy is further improved, and the integrated precision forming of the precipitation-strengthened type medium-entropy alloy complex structural member with high compactness, no crack and excellent performance is realized.
The invention also provides a preparation method of the laser three-dimensional forming technology of the precipitation-strengthened type medium-entropy alloy, which comprises the following steps:
1. preparation and pretreatment of medium-entropy alloy powder
Proportioning according to the mole percentage of each element in the nominal chemical components of the medium-entropy alloy, preparing medium-entropy alloy pre-alloyed spherical powder by a vacuum gas atomization method, and sieving the pre-alloyed spherical powder, wherein the particle size of the powder is 45-150 mu m. The oxygen content and nitrogen content are less than 300ppm, preferably 131ppm and 53ppm. Before carrying out a laser three-dimensional forming experiment, drying the powder to avoid the influence of moisture adsorbed in the powder on material forming, and then placing the powder into a powder feeder of laser three-dimensional forming equipment.
2. Surface treatment of substrates
Selecting a stainless steel or carbon steel substrate, polishing the surface to be deposited, sequentially cleaning the surface to be deposited with acetone and alcohol to remove surface oil stains, blow-drying, and fixing the substrate on a forming platform.
3. Laser stereolithography of Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model on a computer according to the geometric shape of the medium-entropy alloy component, converting the three-dimensional solid model into an STL format, transmitting the STL format to laser forming equipment, setting printing process parameters and a laser scanning path, transmitting medium-entropy alloy spherical powder into a molten pool formed by high-energy laser beams through a coaxial powder-transmitting nozzle under the control of a numerical control system, and realizing the forming of the complex component with a specific shape and size by depositing raw materials on a base material point by point, line by line and layer by layer. The technological parameters of the laser three-dimensional forming are as follows: the laser power is 2 KW-3.5 KW, the scanning speed is 300-800 mm/min, the powder feeding speed is 5-8g/min, the Z-axis lifting amount is 0.4-1.0mm, the overlapping rate is 50%, the diameter of a light spot is 3mm, and the scanning strategy selects reciprocating interweaving scanning, namely in the same deposition layer, the scanning path is S-shaped, adjacent deposition layers rotate 90 degrees in the scanning direction. The laser three-dimensional forming process adopts high-purity argon as a protective gas and a powder-carrying gas, and the oxygen content is lower than 2000ppm in the printing process. According to the set technological parameters and scanning path of laser three-dimensional forming, ni is added a Co b Cr c Al d M e And melting and forming the medium-entropy alloy powder layer by layer to prepare a block sample. By optimizing the laser power, the scanning speed, the powder feeding speed and the Z-axis lifting amount, the quality of the printing alloy can be improved, the microstructure can be optimized, the comprehensive mechanical property can be further improved, and the integrated precise forming of the precipitation-strengthened type medium-entropy alloy complex structural part which is full-compact, free of defects and excellent in comprehensive property can be realized.
The invention also provides Ni prepared by the laser additive manufacturing technology a Co b Cr c Al d M e The heat treatment method of the precipitation strengthening type medium entropy alloy comprises the following steps:
in the present invention, to promote high volume fraction precipitated phase productionRaw and paired laser additive manufacturing of Ni a Co b Cr c Al d M e And carrying out heat treatment on the precipitation strengthening type intermediate entropy alloy. The heat treatment preferably comprises: ni prepared by laser additive manufacturing a Co b Cr c Al d M e Heating the precipitation strengthening type medium-entropy alloy to 600-800 ℃, preserving heat, selecting time t which is not less than 12h and not more than 480h (selective laser melting forming) or t which is not less than 3h and not more than 480h (laser three-dimensional forming), and cooling with water after heat preservation is finished to obtain the medium-entropy alloy after heat treatment. Additive manufacturing of Ni by laser a Co b Cr c Al d M e The medium-entropy alloy is subjected to heat treatment, so that the precipitation of a precipitated phase with a high volume fraction can be effectively promoted, an incompletely recrystallized structure is obtained, and the laser additive manufacturing of Ni is further optimized a Co b Cr c Al d M e The comprehensive mechanical property of the medium-entropy alloy realizes the preparation of the high-strength high-toughness medium-entropy alloy.
Example 1
A precipitation strengthening type intermediate entropy alloy suitable for laser additive manufacturing has a chemical formula of Ni 35 Co 35 Cr 25 Ti 3 Al 2 (ii) a Wherein, the proportion of each element is mole percentage. The selected medium entropy alloy is gas atomization prealloy spherical powder, and the purity is more than 99.9%.
In this example 1, the formation process of the entropy alloy prepared by the selective laser melting technology is as follows:
1. preparation and pretreatment of medium-entropy alloy powder
Proportioning the molar ratios of the elements in the nominal chemical components of the medium-entropy alloy, preparing medium-entropy alloy prealloy spherical powder by a vacuum gas atomization method, sieving the prealloy powder, and selecting the powder with the grain diameter of 15-53 mu m, wherein the typical form of the powder is shown in figure 1. The oxygen content was 131ppm and the nitrogen content was 53ppm. Before the selective laser melting, the powder is dried at 80 ℃ for 4 hours to remove the water in the powder. Then the powder is placed in a powder feeding cylinder of selective laser melting equipment.
2. Surface treatment of substrates
Selecting a 316L stainless steel substrate, polishing a surface to be deposited, cleaning the surface with acetone and alcohol in sequence to remove surface oil stains, then drying the surface oil stains, and mounting the substrate on a forming platform and leveling the substrate. Prior to printing, the substrate was preheated to 200 ℃.
3. Selective laser melting and forming of Ni 35 Co 35 Cr 25 Ti 3 Al 2 Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model on a computer, converting the three-dimensional solid model into a file in an STL format, and importing the file into construction software of selective laser melting forming equipment for layering processing. The technological parameters of selective laser melting and forming are as follows: the laser power is 160-360W, the scanning speed is 600-1000 mm/s, the scanning interval is 60-80 μm, the powder layer thickness is 30-50 μm, the spot diameter is 80 μm, and the scanning strategy is 67-degree rotary scanning. Before printing, high-purity argon gas with the purity of 99.99wt.% is introduced, so that the oxygen content in the forming chamber is lower than 300ppm.
The laser power, the scanning rate and the scanning interval were adjusted by the parameters shown in table 1, and a selective laser melting molding experiment was performed with a fixed powder layer thickness of 30 μm, so as to obtain a selective laser melting molding sample as shown in fig. 2. And the density of the sample is tested, and the result is shown in figure 3.
TABLE 1 Experimental parameters
The optimum process parameters were determined by the experiments shown in table 1: the laser power is 320W, the scanning speed is 1000mm/s, the scanning interval is 70 μm, and the powder layer thickness is 30 μm.
4. Tissue characterization and performance test of selective laser melting forming sample
Observing the microstructure of the formed sample with Scanning Electron Microscope (SEM) under optimized laser selective melting parameters4 (b), the alloy has good forming quality, no defects such as cracks and the like are observed, and the relative density of a formed part is more than 99.6 percent through testing. Compared with an as-cast structure (prepared by a vacuum arc melting method), the Ni prepared by selective laser melting deposition 35 Co 35 Cr 25 Ti 3 Al 2 The microstructure of the precipitation strengthening type medium entropy alloy is finer and more uniform. EXAMPLE 1 Selective laser melting of Ni Using optimized Process parameters 35 Co 35 Cr 25 Ti 3 Al 2 The room-temperature yield strength of the medium-entropy alloy (SLM) is 671MPa, the tensile strength is 913MPa, the elongation is 36 percent, and the hardness is 310HV. The strength is much higher than the as-cast condition, and the tensile plasticity is equivalent to the as-cast condition, as shown in FIG. 5, wherein Ni 35 Co 35 Cr 25 Ti 3 Al 2 The yield strength of the medium-entropy alloy as-Cast state (Cast) is 342MPa, the tensile strength is 648MPa, and the elongation is 38%.
5. Selective laser melting of Ni 35 Co 35 Cr 25 Ti 3 Al 2 Medium entropy alloy heat treatment
Promoting selective laser melting forming of Ni by aging treatment 35 Co 35 Cr 25 Ti 3 Al 2 The generation of the precipitated phase of the medium-entropy alloy realizes further strengthening and toughening. In the present invention, the heat treatment comprises forming Ni by using the optimal laser selective melting parameters 35 Co 35 Cr 25 Ti 3 Al 2 And heating the medium-entropy alloy to 600-800 ℃, preserving the heat for 12h or more and t or 480h or less, and cooling by water after the heat preservation is finished to obtain the heat-treated medium-entropy alloy.
Three sets of experiments were carried out, one set of experiments with a heat treatment at 600 ℃ for 12h, another set of experiments with a heat treatment at 700 ℃ for 12h, and a further set of experiments with a heat treatment at 700 ℃ for 480h.
FIG. 6 shows selective laser melting of Ni 35 Co 35 Cr 25 Ti 3 Al 2 The scanning electron microscope picture (a) and the transmission electron microscope selected region electron diffraction picture (b) of the medium entropy alloy after 600 ℃/12h heat treatment can be observed from the picture 6 (a) that the sedimentary structure is partially recrystallized, and the pictureDiffraction spots of the FCC phase and the gamma' -precipitated phase were observed simultaneously in the sample No. 6 (b). Selective laser melting and forming of Ni 35 Co 35 Cr 25 Ti 3 Al 2 The room temperature tensile property test of the medium entropy alloy heat treatment sample is carried out, the result is shown in figure 7, the result shows that the strength is greatly improved after the heat treatment, the yield strength can reach 1098MPa after the deposition state is subjected to the heat treatment at 700 ℃/480h, the tensile strength is 1466MPa, the elongation is 25%, and the room temperature tensile property is the highest level of the laser additive manufacturing high/medium entropy alloy.
Example 2
A precipitation strengthening type intermediate entropy alloy suitable for laser additive manufacturing has a chemical formula of Ni 35 Co 35 Cr 25 Ti 3 Al 2 (ii) a Wherein, the proportion of each element is mole percentage. The selected medium entropy alloy is gas atomization prealloy spherical powder, and the purity is more than 99.9%.
In this embodiment 2, the formation process of the entropy alloy prepared by the laser stereo forming technology is as follows:
1. preparation and pretreatment of medium-entropy alloy powder
Proportioning the molar ratio of each element in the nominal chemical components of the medium-entropy alloy, preparing medium-entropy alloy prealloy spherical powder by a vacuum atomization method, sieving the prealloy spherical powder, and selecting powder with the particle size of 45-150 mu m, wherein the typical morphology of the powder is shown in figure 8. The oxygen content was 131ppm and the nitrogen content was 53ppm. Before carrying out a laser three-dimensional forming experiment, drying the powder to avoid the influence of moisture adsorbed in the powder on material forming, and then placing the powder in a powder feeder of laser three-dimensional forming equipment.
2. Surface treatment of substrates
Selecting a 316L stainless steel substrate, polishing a surface to be deposited, cleaning with acetone and alcohol in sequence to remove surface oil stains, blow-drying, and fixedly clamping the substrate on a forming platform.
3. Laser stereolithography of Ni 35 Co 35 Cr 25 Ti 3 Al 2 Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model on a computer according to the geometric shape of the medium-entropy alloy component, converting the three-dimensional solid model into an STL format, transmitting the STL format to laser forming equipment, setting printing process parameters and a laser scanning path, transmitting medium-entropy alloy powder into a molten pool formed by high-energy laser beams through a coaxial powder-transmitting nozzle under the control of a numerical control system, and realizing the forming of the complex component with a specific shape and size by depositing raw materials on a base material point by point, line by line and layer by layer. The technological parameters of the laser three-dimensional forming are as follows: the laser power is 2 KW-3.5 KW, the scanning speed is 300-800 mm/min, the powder feeding speed is 5-8g/min, the Z-axis lifting amount is 0.4-1.0mm, the overlapping rate is 50%, the spot diameter is 3mm, the scanning strategy selects reciprocating interweaving scanning, namely, in the same deposition layer, the scanning path is S-shaped, and the adjacent deposition layers rotate 90 degrees in the scanning direction. The laser three-dimensional forming process adopts high-purity argon as a protective gas and a powder-carrying gas, and the oxygen content is lower than 2000ppm in the printing process.
And adjusting the laser power, the scanning speed, the powder feeding speed and the Z-axis lifting amount to perform optimal process exploration, and printing block samples with different linear energy densities, wherein the specifically adopted process parameters are shown in table 2.
Table 2 specific experimental parameters for example 2
Ni is prepared by adopting the laser three-dimensional forming process parameters 35 Co 35 Cr 25 Ti 3 Al 2 A typical macro-morphology of a medium-entropy bulk alloy sample is shown in FIG. 9. The room temperature tensile property test was performed on each of the 3 samples, and the results are shown in FIG. 10. Through the mechanical property test result, the optimal process parameters are determined: the laser power is 2800W, the scanning speed is 300mm/min, the powder feeding speed is 5g/min, the Z-axis lifting amount is 0.5mm, and the overlapping rate is 50%.
4. Tissue characterization and performance test of laser stereolithography sample
Visualization of the shaped samples under optimum parameters using electron back-scattered diffraction (EBSD) and Scanning Electron Microscopy (SEM)As shown in FIG. 11, the microstructure was good in the alloy forming quality, and no defects such as cracks, voids, and fusion failure were observed. And Ni prepared by adopting laser stereolithography 35 Co 35 Cr 25 Ti 3 Al 2 A small amount of γ' nanoscale precipitated phase was present in the intermediate entropy alloy structure, as shown in fig. 11 (b). Laser stereoforming Ni prepared by adopting optimized process parameters 35 Co 35 Cr 25 Ti 3 Al 2 The room-temperature mechanical properties of the medium-entropy alloy are shown in fig. 12, the yield strength along the construction direction (longitudinal direction) is 723MPa, the tensile strength is 1078MPa, the elongation is 39%, and the hardness is 355HV; yield strength was 566MPa, tensile strength was 1011MPa, elongation was 47%, and hardness was 284HV in the scanning direction (transverse direction). Compared with the traditional casting method, the Ni prepared by adopting the laser three-dimensional forming method 35 Co 35 Cr 25 Ti 3 Al 2 The medium entropy alloy sample has high strong plastic bonding.
5. Laser stereolithography of Ni 35 Co 35 Cr 25 Ti 3 Al 2 And (4) carrying out medium-entropy alloy heat treatment.
Further promoting laser stereolithography Ni by aging treatment 35 Co 35 Cr 25 Ti 3 Al 2 The generation of the precipitated phase of the medium-entropy alloy realizes further strengthening and toughening. In the invention, the heat treatment mode comprises the step of carrying out laser three-dimensional forming on Ni under the optimal process parameters 35 Co 35 Cr 25 Ti 3 Al 2 And heating the medium-entropy alloy to 700 ℃, preserving the heat for 3h, and cooling by water after the heat preservation is finished to obtain the heat-treated medium-entropy alloy.
FIG. 13 shows laser stereolithography of Ni 35 Co 35 Cr 25 Ti 3 Al 2 Compared with the original sedimentary structure, the volume fraction of a precipitated phase is obviously increased by a high-power scanning electron microscope picture of the medium-entropy alloy after 700 ℃/3h heat treatment. FIG. 14 shows Ni prepared with different laser powers 35 Co 35 Cr 25 Ti 3 Al 2 The change rule of microhardness of the medium-entropy alloy after heat treatment. Is subjected to heat treatmentThen, the hardness is obviously improved due to the generation of precipitated phases with high volume fraction, and the hardness of a sample with the laser power of 2.8KW after being subjected to heat treatment at 700 ℃/3h is about 415HV. FIG. 15 shows Ni with a laser power of 2.8KW 35 Co 35 Cr 25 Ti 3 Al 2 The tensile property of the medium-entropy alloy after 700 ℃/3h heat treatment is that the yield strength is 808MPa, the tensile strength is 1168MPa, and the elongation is 32%, compared with a sedimentary sample, the strength of the medium-entropy alloy is remarkably improved due to the generation of precipitated phases.
Claims (6)
1. The precipitation-strengthened type intermediate entropy alloy is suitable for laser additive manufacturing, and is characterized in that the precipitation-strengthened type intermediate entropy alloy is Ni a Co b Cr c Al d M e Wherein M is one or more elements of Ti, ta, nb and Mo, a, b, c, d and e respectively represent the mole percentage of the corresponding elements, b =20% -40%, c =20% -25%, d> 1%，e >0，d+e < 7%，a+b+c+d+e=100%；
The precipitation strengthening type intermediate entropy alloy is prepared by adopting a selective laser melting forming technology; the method comprises the following steps:
step 1, preparing and pretreating intermediate entropy alloy powder
According to the mole percentage, taking metal raw materials corresponding to each element, preparing medium-entropy alloy prealloy spherical powder by adopting a vacuum gas atomization method, sieving and drying to obtain medium-entropy alloy powder;
step 2, selective laser melting and forming Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into a file in an STL format, importing the file into construction software of selective laser melting forming equipment, and carrying out layering treatment; introducing high-purity argon to ensure that the oxygen content in the forming cabin is lower than 300ppm, and melting and forming the medium-entropy alloy powder layer by layer according to the set technological parameters and scanning strategy for selective laser melting and forming to prepare a medium-entropy alloy component;
selective laser melting forming toolThe technological parameters are as follows: the laser power P is 160-360W, the scanning speed v is 600-1000 mm/s, the scanning interval h is 60-80 mu m, the powder layer thickness t is 30-50 mu m, the spot diameter is 80 mu m, and the energy and mass density VED range is 140J/mm 3 < VED < 240J/mm 3 Wherein VED = P/vht;
or the precipitation strengthening type medium entropy alloy is prepared by adopting a laser three-dimensional forming technology; the method comprises the following steps:
step 1, preparing and pretreating medium-entropy alloy powder
According to the mole percentage, taking metal raw materials corresponding to each element, preparing medium-entropy alloy prealloy spherical powder by adopting a vacuum gas atomization method, sieving and drying to obtain medium-entropy alloy powder;
step 2 laser stereolithography of Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into an STL format, transmitting the STL format to laser three-dimensional forming equipment, setting printing process parameters and a laser scanning path, transmitting medium-entropy alloy powder into a molten pool formed by high-energy laser beams in the laser three-dimensional forming equipment, and printing to obtain the medium-entropy alloy component in a mode of depositing raw materials on a base material point by point, line by line and layer by layer;
the printing process parameters are as follows: the laser power is 2 kW-3.5 kW, the scanning speed is 300-800 mm/min, the powder feeding speed is 5-8g/min, the Z-axis lifting amount is 0.4-1.0mm, the lap joint rate is 50%, the spot diameter is 3mm, and the scanning path is a reciprocating interweaving scanning path.
2. The method for preparing the precipitation-strengthened type entropy alloy suitable for laser additive manufacturing of claim 1, wherein the method is prepared by a selective laser melting forming technology; the method comprises the following steps:
step 1, preparing and pretreating intermediate entropy alloy powder
According to the mol percent of the alloy powder as claimed in claim 1, taking metal raw materials corresponding to each element, preparing the medium-entropy alloy prealloy spherical powder by a vacuum gas atomization method, sieving and drying to obtain the medium-entropy alloy powder;
step 2, selective laser melting and forming Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into a file with an STL format, importing the file into construction software of selective laser melting forming equipment, and carrying out layering treatment; introducing high-purity argon to ensure that the oxygen content in the forming cabin is lower than 300ppm, and melting and forming the medium-entropy alloy powder layer by layer according to the set technological parameters and scanning strategy for selective laser melting and forming to prepare a medium-entropy alloy component;
the technological parameters of selective laser melting and forming are as follows: the laser power P is 160-360W, the scanning speed v is 600-1000 mm/s, the scanning interval h is 60-80 μm, the powder layer thickness t is 30-50 μm, the spot diameter is 80 μm, and the energy density VED range is 140J/mm 3 < VED < 240J/mm 3 Wherein VED = P/vht.
3. The preparation method of the precipitation-strengthened type entropy alloy suitable for laser additive manufacturing according to claim 2, is characterized in that the scanning strategy is 67 degree rotation scanning, reciprocating interlaced scanning or 45 degree rotation divisional scanning.
4. The method for preparing a precipitation-strengthened entropy alloy suitable for laser additive manufacturing of claim 2, further comprising a heat treatment step of: and (3) heating the medium-entropy alloy component to 600-800 ℃, keeping the temperature for 12h or less and t or less than 480h, and cooling by water after the temperature is kept, so as to obtain the heat-treated medium-entropy alloy.
5. The method for preparing the precipitation-strengthened type entropy alloy suitable for laser additive manufacturing of claim 1, wherein the precipitation-strengthened type entropy alloy is prepared by a laser stereolithography technique; the method comprises the following steps:
step 1, preparing and pretreating intermediate entropy alloy powder
According to the mol percent of the alloy powder as claimed in claim 1, taking metal raw materials corresponding to each element, preparing the medium-entropy alloy prealloy spherical powder by a vacuum gas atomization method, sieving and drying to obtain the medium-entropy alloy powder;
step 2 laser stereolithography of Ni a Co b Cr c Al d M e Precipitation strengthening type medium entropy alloy
Establishing a three-dimensional solid model according to the geometric shape of the medium-entropy alloy component to be prepared, converting the three-dimensional solid model into an STL format, transmitting the STL format to laser three-dimensional forming equipment, setting printing process parameters and a laser scanning path, transmitting medium-entropy alloy powder into a molten pool formed by high-energy laser beams in the laser three-dimensional forming equipment, and printing to obtain the medium-entropy alloy component in a mode of depositing raw materials on a base material point by point, line by line and layer by layer;
the printing process parameters are as follows: the laser power is 2 kW-3.5 kW, the scanning speed is 300-800 mm/min, the powder feeding speed is 5-8g/min, the Z-axis lifting amount is 0.4-1.0mm, the lap joint rate is 50%, the spot diameter is 3mm, and the scanning path is a reciprocating interweaving scanning path.
6. The method of preparing a precipitation-strengthened entropy alloy suitable for laser additive manufacturing of claim 5, further comprising a heat treatment step of: and (3) heating the medium-entropy alloy component to 600-800 ℃, preserving heat for 3h or more and t or less than 480h, and cooling by water after heat preservation to obtain the heat-treated medium-entropy alloy.
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