CN116716528B - High-strength plastic nanoparticle precipitation strengthening medium-entropy alloy and preparation method thereof - Google Patents
High-strength plastic nanoparticle precipitation strengthening medium-entropy alloy and preparation method thereof Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 35
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- 229910000601 superalloy Inorganic materials 0.000 description 2
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Abstract
The invention discloses a high-strength plastic nanoparticle precipitation strengthening intermediate entropy alloy and a preparation method thereof, wherein the molecular formula is as follows: ni 2.1CoCrFe0.5Nb0.2, the alloy has stable single-phase face-centered cubic structure at high temperature, and nano-scale gamma' phase with D0 22 structure can be precipitated through low temperature aging. Manufactured by laser additive manufacturing, then solution treated and aged. The prepared intermediate entropy alloy has no micropores and microcracks, uniform structure, compact structure and high elongation. After the alloy is subjected to solution treatment at 1100 ℃ for 2 hours, the elements of the alloy are uniformly distributed, the element segregation is eliminated, and the effect of solid solution is achieved. In the aging treatment at 650 ℃, the gamma' phase with a D0 22 structure is gradually increased, alloy strength and hardness are gradually improved, plasticity is reduced, time efficiency reaches 120h, strength reaches a peak value, comprehensive mechanical property is optimal, yield strength is 1005MPa, ultimate strength is 1240MPa, and tensile elongation is 20%. Provides a theoretical basis for preparing the entropy alloy in high-strength plasticity in additive manufacturing.
Description
Technical Field
The invention belongs to the field of alloys, and particularly relates to a high-strength plastic nano particle precipitation strengthening medium entropy alloy and a preparation method thereof.
Background
The intermediate entropy alloy is a novel alloy which contains 3 or more main elements, the entropy value is more than or equal to 1.5R and more than or equal to deltaS and more than or equal to 1R, and the novel alloy is composed of the same molar ratio or near-molar ratio. The medium entropy alloy composed of a plurality of main elements not only has unexpected simple phase composition, but also has good performance, and is attracting attention. In the past decades, significant progress has been made in the research of composition design, phase selection, mechanical and functional properties, deformation mechanisms, processing methods, and the like of medium entropy alloys. Among the different processing methods, additive manufacturing is considered as an advanced manufacturing method and is a promising technique for preparing medium entropy alloys. Additive manufacturing is based on a combination of computer science and material processing and forming techniques, showing great potential in rapidly manufacturing large parts with complex shapes and obtaining alloys with fine structure and excellent mechanical properties. At the same time, the diversity and variability of mid-entropy alloy compositions gives more opportunities for additive manufacturing applications, but existing limited alloy systems are used for additive manufacturing, and the mechanical properties obtained are still not ideal, such as Ti-6Al-4v, in718, 316L. Thus, there is a need to develop more high performance alloy formulations for additive manufacturing.
Additive manufacturing has significant advantages: (1) the freedom degree of geometric design and optimization is high; (2) The functional combination and the parts are integrated, so that the assembly is reduced, and the performance and the reliability are improved; (3) the utilization rate and the energy efficiency of the material are improved; (4) is suitable for customization and small-scale production; (5) shortening the production and lead time of the product. Therefore, aerospace is a key market driver for additive manufacturing development, as high-value parts thereof often require multiple varieties of small-volume production, highly integrated complex structures, and rapid and efficient manufacturing processes. In the direct laser deposition material-increasing technology, since coaxial powder feeding is adopted, metal powder is instantly melted, alloy is quickly solidified, the medium-entropy alloy is composed of a plurality of elements, and the characteristics of melting point, shrinkage rate and the like among the elements are different, the massive high-entropy alloy prepared by material-increasing manufacturing has macroscopic cracks and micropores in a plurality of basic researches, so that the formability is poor.
In order to improve the strength of single-phase high-entropy alloy prepared by additive manufacturing, a great deal of work is done. For example, a hierarchical metastable microstructure is achieved; doping a small amount of interstitial atoms into a single-phase matrix; the second nanoparticle is added to the single phase matrix. However, these methods all exhibit a moderate strength reinforcing effect. Recently, it has been reported that precipitation strengthening exhibits a better strengthening effect in medium entropy alloys than other strengthening mechanisms, and that Al/Ti alloys and Nb alloys have successfully incorporated and developed two types of precipitation hardening medium entropy alloys, γ' phase and γ "phase, respectively.
Disclosure of Invention
In order to solve the technical problems, a first object of the present invention is to provide a high-strength plastic nano particle precipitation strengthening mid-entropy alloy, and a second object is to provide a preparation method of the alloy.
In order to achieve the first object, the present invention provides the following technical solutions: the high-strength plastic nanoparticle precipitation strengthening medium entropy alloy is characterized by having the following molecular formula: ni 2.1CoCrFe0.5Nb0.2, the alloy has a stable single-phase face-centered cubic structure at high temperatures, and a nanoscale gamma' phase with a D0 22 structure.
The invention aims at obtaining good mechanical properties, takes CoCrFeNi systems which are the most basic, fully researched and single and stable in structure as a matrix, adds typical precipitation hardening Nb elements in nickel-based superalloy, and designs a medium-entropy alloy formula for additive manufacturing.
The second object of the present invention is achieved by: the preparation method of the high-strength plastic nanoparticle precipitation strengthening medium entropy alloy is characterized by comprising the following steps of:
1) Preparing powder, namely selecting spherical powdery raw materials Ni, co, cr, fe and Nb prepared by a plasma rotating electrode process according to a mole ratio of 21:10:10:5:2, uniformly mixing the materials in proportion;
2) Ball milling of the powder, namely placing the mixed powder into a ball milling tank for ball milling;
3) Placing the powder after ball milling and mixing in a vacuum dryer for drying at 120 ℃ for more than 4 hours;
4) In a laser additive manufacturing machine, adopting a coaxial nozzle to send powder, and preparing a bulk deposition state medium entropy alloy by taking 304 plates as substrate materials in an argon atmosphere;
5) Solid solution treatment, namely solid solution treatment is carried out on the prepared blocky medium-entropy alloy at 1100 ℃, direct water quenching and cooling treatment are carried out,
6) And aging the intermediate entropy alloy after solid solution at 650 ℃.
3. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 2, which is characterized in that: the purity of Ni, co, cr, fe and Nb in the alloy feedstock is greater than 99.5wt%.
In the scheme, the method comprises the following steps: the grinding ball mass and the powder mass are proportioned according to the ratio of 5:1, the ball milling rotating speed is 350r/min, and the ball milling is carried out for 4 hours.
In the scheme, the method comprises the following steps: the laser additive manufacturing machine is provided with a 6KW continuous wave fiber laser and an automatic feeding device of a double powder feeder.
In the scheme, the method comprises the following steps: in step 4), laser power: 1200W, 20g/min of powder feeding amount, and scanning rate: 20mm/s, layer height: 0.40mm, and the laser spot diameter is 3.2mm.
In the scheme, the method comprises the following steps: in step 4), the thickness of the entropy alloy in the as-deposited state is 0.4-0.5mm.
In the scheme, the method comprises the following steps: the solution treatment time is 2h.
In the scheme, the method comprises the following steps: aging treatment time is 24-148h.
According to the invention, the optimal manufacturing process parameters of the medium entropy alloy system additive manufacturing are obtained by optimizing laser power, light spot diameter, powder feeding speed, scanning speed and Z-direction layer height.
Compared with the prior art, the invention has the beneficial effects that:
NiCoCrFe is the most basic and well-studied alloy system with a single and stable FCC structure, nb element addition for nanoparticle gamma "phase precipitation strengthening. The invention provides a design strategy combining total valence electron concentration and phase diagram simulation, which is used for designing gamma' phase in medium entropy alloy. When the total valence electron concentration value of the intermediate entropy alloy is less than 8.4, a brittle Lives phase is easy to form at high temperature, and a sample is easy to crack under the thermal environment of additive manufacturing. When the total valence electron concentration value of the intermediate entropy alloy is more than 8.4, a single-phase face-centered cubic structure is formed at high temperature, and gamma' phase with a D0 22 structure is precipitated at low temperature. The Ni 2.1CoCrFe0.5Nb0.2 intermediate entropy alloy developed by the invention has a stable single-phase face-centered cubic structure at high temperature, can precipitate a nano-scale gamma' phase with a D0 22 structure through low-temperature aging, and improves the strength of the intermediate entropy alloy.
The high-strength plastic intermediate entropy alloy which is not subjected to solid solution and aging treatment has uniform structure, compact structure, no micropores and microcracks, has yield strength, tensile strength and elongation of 278MPa, 720MPa and 50 percent respectively, exceeds the very high level of other manufacturing methods, and widens the conventional intermediate entropy alloy formula system for additive manufacturing.
After the alloy is subjected to solution treatment at 1100 ℃ for 2 hours, the elements of the alloy are uniformly distributed, dendrites disappear and are converted into columnar crystals, the effect of solid solution is achieved, the yield and tensile strength are respectively reduced to 257MPa and 647MPa, and the tensile elongation is increased to 58%. In the aging treatment, the alloy strength and hardness are gradually improved along with the increase of time, the plasticity is reduced, when the aging time reaches 120 hours, the alloy strength reaches a peak value, the comprehensive mechanical property is optimal, the yield strength is 1005MPa, the ultimate strength is 1240MPa, and the tensile elongation is 20%.
Drawings
FIG. 1 shows the phase diagram calculations for the entropy alloys in NiCoCrFNb of the different compositions, niCoCrFeNb 0.2 alloy, (b) Ni 1.6CoCrFeNb0.2 alloy, and (c) Ni 2.1CoCrFe0.5Nb0.2.
FIG. 2 is a morphology diagram of an entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared by laser additive manufacturing according to the present invention.
Fig. 3 is a SEM image of (a 1) as-deposited, (b 1) as-solid solution and (c 1) as-aged 120h, and XRD detection results of (a 2) as-deposited, (b 2) as-solid solution and (c 2) as-aged 120h in the microstructure map and XRD detection results of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention.
FIG. 4 is a graph of the as-deposited surface scanning energy spectrum of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention.
FIG. 5 shows the EBSD analysis results of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention, the particle size distribution of (a 1) as-deposited (not solution treated), (b 1) as-solid solution (not aging treated), (c 1) as-aged for 120h, (a 2) as-deposited, (b 2) as-solid solution, and (c 2) as-aged for 120 h.
FIG. 6 shows TEM analysis results of 120h aging state of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention.
FIG. 7 is a graph showing the hardness test results of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention at different time intervals.
FIG. 8 is a tensile test result of different time-lapse of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention.
Detailed Description
The invention is further described below with reference to examples.
Example 1
A high-strength plastic nano particle precipitation strengthening medium entropy alloy,
The alloy with molecular formula NiCoCrFeNb 0.2、Ni1.6CoCrFeNb0.2、Ni2.1CoCrFe0.5Nb0.2 is designed and prepared according to the following method:
1) Preparing powder, namely selecting spherical powdery raw materials Ni, co, cr, fe and Nb prepared by a plasma rotating electrode process according to a mole ratio of 21:10:10:5:2, uniformly mixing the materials in proportion; the purity of Ni, co, cr, fe and Nb in the alloy feedstock is greater than 99.5wt%.
2) Ball milling is carried out on the powder, the mixed powder is placed in a ball milling tank for ball milling, the mass of the grinding balls and the mass of the powder are proportioned according to the ratio of 5:1, the ball milling rotating speed is 350r/min, and the ball milling is carried out for 4 hours.
3) And (3) placing the powder subjected to ball milling and mixing in a vacuum dryer, and drying at 120 ℃ for more than 4 hours.
4) In a laser additive manufacturing machine, powder is fed by adopting a coaxial nozzle, and under the argon atmosphere, 304 plates are used as substrate materials to prepare the bulk-state entropy alloy, wherein the thickness of the bulk-state entropy alloy in the deposition state is 0.4-0.5mm. The laser additive manufacturing machine is provided with a 6KW continuous wave fiber laser and an automatic feeding device of a double powder feeder. Laser power: 1200W, 20g/min of powder feeding amount, and scanning rate: 20mm/s, layer height: 0.40mm, and the laser spot diameter is 3.2mm.
5) And (3) carrying out solution treatment, namely directly carrying out water quenching and cooling treatment on the entropy alloy in the prepared bulk Ni 2.1CoCrFe0.5Nb0.2 at 1100 ℃ for 2 hours.
6) Aging the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 after solid solution at 650 ℃ for 24h, 48h, 72h, 96h, 112h, 120h and 148h respectively
The test pieces were tested for hardness and tensile properties.
Fig. 1 shows the phase diagram calculations of the entropy alloys in NiCoCrFNb of the different compositions, (a) NiCoCrFeNb 0.2 alloy, (b) Ni 1.6CoCrFeNb0.2 alloy, and (c) Ni 2.1CoCrFe0.5Nb0.2, as can be seen from fig. 1: the OVEC values of the entropy alloys in NiCoCrFeNb 0.2 and Ni 1.6CoCrFeNb0.2 were 8.09 and 8.33, respectively, and the OVEC values of these two alloy components were below 8.4, and therefore the D0 22 structure could not be formed mainly. FIG. 1 (a) shows a calculated phase diagram of the entropy alloy in NiCoCrFeNb 0.2, indicating the presence of Laves phases during laser deposition. FIG. 1 (b) shows simulation results of the phase diagram of the entropy alloy in Ni 1.6CoCrFeNb0.2, indicating that the Laves phase decreases with increasing Ni content. Finally, the entropy alloy composition in Ni 2.1CoCrFe0.5Nb0.2 with OVEC being 8.54 is designed, and the simulation result of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 is shown in FIG. 1 (c), wherein a single-phase FCC structure is formed in the laser deposition process, and gamma' phase is separated out in the subsequent aging treatment, and Laves phase disappears. Meanwhile, fig. 1 (c) provides a theoretical reference for solid solution and aging heat treatment of the as-deposited alloy.
Fig. 2 is a morphology diagram of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared by laser additive manufacturing according to the present invention, and it can be seen from fig. 2: the bulk medium entropy alloy is regular in shape, free of collapse and free of cracks and oxidation on the surface.
FIG. 3 shows the microstructure morphology and XRD detection results of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention, (a 1) as deposited state, (b 1) as solid solution state and (c 1) as SEM image of 120 hours aging, (a 2) as deposited state, (b 2) as solid solution state and (c 2) as XRD detection results of 120 hours aging state. As can be seen from fig. 3: (a 1) shows that the microstructure of the as-deposited alloy exhibits a dendritic microstructure. (b 1) shows the microstructure of the alloy after solution treatment, dendrite decomposition. (c 1) shows the microstructure of the alloy after aging, with tiny particles present in the grains. (a 2-c2) shows the XRD patterns of Ni 2.1CoCrFe0.5Nb0.2 in the three treatment states, respectively, clearly showing that all samples have a single FCC crystal structure, and it can be further seen that, despite the presence of the particulate phase on the matrix, only a single phase is shown after aging treatment. Although precipitation of the gamma "phase or dissolution of the Nb-rich phase may result in a change in the Nb element distribution, the particulate phase is too fine to be detected by XRD, which does not ultimately result in a significant change in the lattice parameter.
As can be seen from fig. 4: panels (b-e) show elemental mapping scans of Ni, co, cr and Fe, with uniform distribution of these elements in the microstructure, whereas panel (f) shows non-uniform distribution of Nb elements.
FIG. 5 shows the particle size distribution of (a 1) as-deposited, (b 1) as-solid solution and (c 1) as-aged 120h IPF, of (a 2) as-deposited, (b 2) as-solid solution and (c 2) as-aged 120h EBSD analysis of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention. As can be seen from the figures: graph (a 1) shows the IPF plot of the as-deposited alloy and graph (a 2) shows the corresponding grain size distribution with an average size of 54.42 μm. Graph (b 1) shows the IPF plot of the solid solution alloy and graph (b 2) shows the corresponding particle size distribution with an average particle size of 58.89 μm. Graph (c 1) shows the IPF plot of the 120h aged alloy and graph (c 2) shows the corresponding grain size distribution with an average size of 62.08 μm.
FIG. 6 shows TEM analysis results of 120h aging state of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention. As can be seen from the figures: the uniformly distributed precipitate with different crystal orientations is mainly disc-shaped. According to the DF image, the volume fraction of the precipitated phase is about 15%, the length is about 9.8nm and the width is about 3.2nm. (b 1) shows three variants of the gamma "phase, marked with three different yellow symbols, with a crystal orientation relationship between the matrix and the gamma" phase of < 001 > m//[001]γ″ and {100} m//{100}γ″.
FIG. 7 is a graph showing the hardness test results of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention at different time intervals. As can be seen from the figures: as the aging time increases, the hardness tends to increase, reaching a peak of 481HV at 120 h.
FIG. 8 is a tensile test result of different time-lapse of the entropy alloy in Ni 2.1CoCrFe0.5Nb0.2 prepared according to the present invention. As can be seen from the figures: the yield strength of the as-deposited entropy alloy is about 278MPa, the tensile strength is about 720MPa, and the elongation at break is about 50%. After solution treatment, the samples showed a better ductility of about 58% but a slight decrease in strength of about 647MPa. After various time aging treatments, the strength of the test sample is obviously improved, and especially after aging for 120 hours, the yield strength and the ultimate tensile strength respectively reach 1005MPa and 1240MPa.
After the alloy is subjected to solution treatment at 1100 ℃ for 2 hours, the elements of the alloy are uniformly distributed, dendrites disappear and are converted into columnar crystals, the effect of solid solution is achieved, the yield and tensile strength are respectively reduced to 257MPa and 647MPa, and the tensile elongation is increased to 58%. In the aging treatment, the strength and hardness of the alloy are gradually improved along with the increase of time, the plasticity is reduced, when the aging time reaches 120 hours, the strength of the alloy reaches a peak value, the comprehensive mechanical property is optimal, the yield strength is 1005MPa, the ultimate strength is 1240MPa, and the tensile elongation is 20%, so that the alloy is the highest level reported at present.
Claims (9)
1. The high-strength plastic nanoparticle precipitation strengthening medium entropy alloy is characterized by having the following molecular formula: ni 2.1CoCrFe0.5Nb0.2, the alloy has a stable single-phase face-centered cubic structure at high temperatures, and a nanoscale gamma '' phase with a D0 22 structure.
2. The preparation method of the high-strength plastic nanoparticle precipitation strengthening medium entropy alloy is characterized by comprising the following steps of:
1) Preparing powder, namely selecting spherical powdery raw materials Ni, co, cr, fe and Nb prepared by a plasma rotating electrode process according to a mole ratio of 21:10:10:5:2, uniformly mixing the materials in proportion;
2) Ball milling of the powder, namely placing the mixed powder into a ball milling tank for ball milling;
3) Placing the powder after ball milling and mixing in a vacuum dryer to be dried for more than 4 hours at 120 ℃;
4) In a laser additive manufacturing machine, adopting a coaxial nozzle to send powder, and preparing a bulk deposition state medium entropy alloy by taking 304 plates as substrate materials in an argon atmosphere;
5) Solid solution treatment, namely solid solution treatment is carried out on the prepared blocky medium-entropy alloy at 1100 ℃, direct water quenching and cooling treatment are carried out,
6) And aging the intermediate entropy alloy after solid solution at 650 ℃.
3. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 2, which is characterized in that: the purity of Ni, co, cr, fe and Nb in the alloy feedstock is greater than 99.5wt%.
4. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 3, which is characterized in that: the grinding ball mass and the powder mass are proportioned according to the ratio of 5:1, the ball milling rotating speed is 350 r/min, and the ball milling is 4: 4 h.
5. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 4, which is characterized in that: the laser additive manufacturing machine is provided with a 6KW continuous wave fiber laser and an automatic feeding device of a double powder feeder.
6. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 5, which is characterized in that: in step 4), laser power: 1200W, 20g/min of powder feeding amount, and scanning rate: 20mm/s, layer height: 0.40mm, and the laser spot diameter is 3.2mm.
7. The method for preparing the high-strength plastic nanoparticle precipitation strengthening medium entropy alloy according to claim 6, which is characterized in that: in step 4), the thickness of the entropy alloy in the as-deposited state is 0.4-0.5mm.
8. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 7, which is characterized in that: the solution treatment time is 2h.
9. The method for preparing the high-strength plastic nanoparticle precipitation strengthening mid-entropy alloy according to claim 8, which is characterized in that: aging treatment time is 24-148h.
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