CN111826573A - Precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and preparation method thereof - Google Patents
Precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and preparation method thereof Download PDFInfo
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- CN111826573A CN111826573A CN202010611439.3A CN202010611439A CN111826573A CN 111826573 A CN111826573 A CN 111826573A CN 202010611439 A CN202010611439 A CN 202010611439A CN 111826573 A CN111826573 A CN 111826573A
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
Abstract
The invention discloses a precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and a preparation method thereof, belonging to the field of high-entropy alloys. The high-entropy alloy is composed of four elements of Fe, Ni, Mn and Cu according to an equimolar proportion. The preferred preparation method of the high-entropy alloy comprises the following steps: firstly, smelting the prepared raw materials in an electric arc furnace under the protection of vacuum argon, and then carrying out drop casting, homogenizing annealing, cold rolling and aging to obtain the precipitation strengthening type high-entropy alloy without the sigma phase precipitation tendency. The optimal values of the room-temperature yield strength and the tensile strength of the precipitation-strengthened high-entropy alloy without the sigma phase precipitation tendency can reach 825MPa and 933MPa respectively, the elongation is more than 15%, and the mechanical property index of the precipitation-strengthened high-entropy alloy can be adjusted by using aging parameters. The precipitation strengthening type high-entropy alloy without the sigma phase precipitation tendency has excellent comprehensive mechanical properties at room temperature.
Description
Technical Field
The invention belongs to the field of high-entropy alloy preparation, and particularly relates to a precipitation-strengthened high-entropy alloy without a sigma phase precipitation tendency and a preparation method thereof.
Background
High-entropy alloys (HEAs) have been proposed to subvert the understanding of traditional alloys. Due to the cocktail effect of high entropy alloys, one can need to blend the alloy components to achieve the desired properties, which greatly opens the way researchers design new materials. High entropy alloys generally refer to alloy systems in which five or more alloying elements are combined in (near) equal atomic ratios, on the basis of which a number of new alloy systems with unique properties have been proposed. Wherein the alloy system with a face-centered cubic structure (FCC) has excellent toughness/plasticity and is considered to have great application potential. However, the alloy systems are widely added with strengthening element Cr, such as a very representative CrMnFeCoNi high-entropy alloy.
A large number of researches show that in the medium-temperature aging process of the CrMnFeCoNi high-entropy alloy, Cr element is easy to induce and separate out a brittle sigma (sigma) phase and/or other compounds, so that the comprehensive mechanical property is reduced. If the precipitation tendency of brittle phases and compounds can be eliminated, the method is greatly helpful for improving the comprehensive mechanical properties of the material.
How to ensure the strength and/or plasticity of the material while eliminating the precipitation tendency of brittle phases and compounds becomes a problem to be solved at present.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and a preparation method thereof, aiming at only taking four pure metal materials of Fe, Ni, Mn and Cu as raw materials on the premise of not adding Cr, and realizing the purposes of eliminating the precipitation tendency of a brittle (sigma) phase and other compounds and ensuring the strength and/or toughness of the material through the improvement of process steps and process parameters.
In order to achieve the above object, according to one aspect of the present invention, a method for preparing a precipitation-strengthened high-entropy alloy without a sigma phase precipitation tendency is provided, wherein four pure metal materials of Fe, Ni, Mn, and Cu in equal molar ratio are subjected to smelting, drop casting, homogenizing annealing, cold rolling, and aging annealing in sequence to obtain the precipitation-strengthened high-entropy alloy without a sigma phase precipitation tendency; wherein the content of the first and second substances,
the parameter range of the homogenizing annealing is 910-1050 ℃, and the temperature is kept for 12-48 h; the temperature range of the aging annealing is 800-900 ℃, and the time range is 0.5-1 h.
Further, Mn is placed at the bottommost layer of the crucible during smelting, and Fe, Ni and Cu are stacked above Mn layer by layer from bottom to top according to the sequence of melting points from low to high.
Further, the smelting method comprises the following steps: smelting in an electric arc smelting furnace under the protection of negative pressure and argon atmosphere.
Further, the electric arc melting furnace is vacuumized and then backfilled with argon to 5 multiplied by 104And Pa, repeatedly vacuumizing and backfilling argon twice, and then smelting.
Further, cold rolling 80-90% of deformation.
Further, the steel sheet was cold-rolled by 85% deformation.
Further, the parameters of homogenizing annealing are 1000 ℃ and 12 hours; the parameters of the aging annealing are that the temperature is kept for 1h at 800 ℃ or 1h at 850 ℃.
Further, after homogenizing and aging annealing, the steel is rapidly cooled in a water-cooling quenching mode.
In order to achieve the above object, according to another aspect of the present invention, there is provided a precipitation-strengthened high-entropy alloy free from a tendency to precipitate a sigma phase, obtained by the production method as described in any one of the foregoing.
In general, compared with the prior art, the above technical solution contemplated by the present invention can obtain the following beneficial effects:
1. the precipitation strengthening type high-entropy alloy prepared by the method does not contain Cr, and the precipitation tendency of a brittle sigma phase is eliminated; meanwhile, through the combination of a homogenization process and an aging annealing process, the yield strength of the obtained high-entropy alloy at room temperature reaches 474 MPa-825 MPa, the tensile strength reaches 730 MPa-933 MPa, and the elongation rate can reach 15% -29%, so that the high-entropy alloy belongs to the high-entropy alloy with good comprehensive mechanical properties and has a good application prospect.
2. The homogenization parameter range is 910-1050 ℃, the heat preservation is carried out for 12-48 h, the alloy components can be uniformly distributed, and meanwhile, the alloy components have proper grain sizes, so that the elongation is improved, the uniformity of the subsequent aging annealing treatment phase formation is improved, and the integral strength is improved. Too low a homogenization temperature or too short a time results in insufficient homogenization of the components, while too high a homogenization temperature or too long a time results in too large grains, making it difficult to obtain a suitable grain size by cold rolling, resulting in a reduction in elongation and a weakening of the overall strength after the aging annealing treatment. On the basis of ensuring the homogenization of alloy components and the proper particle size, the comprehensive performance of the product can be regulated and controlled through an aging annealing process, the temperature range of the aging annealing process is 800-900 ℃, and the comprehensive mechanical performance of the product obtained by matching with the homogenization treatment process is the best when the time range is 0.5-1 h.
3. Mn is placed at the bottommost layer of the crucible during smelting, Fe, Ni and Cu are stacked layer by layer from bottom to top above the Mn according to the sequence of melting points from low to high, so that materials with low melting points can be preferentially and rapidly melted to cover the Mn, the evaporation capacity of the Mn is reduced to the maximum extent, and the Mn loss is reduced.
4. The argon gas reaction atmosphere of negative pressure not only can provide protective atmosphere, and argon gas can also arouse electric arc, helps the electric arc to smelt to go on, and the negative pressure can also form self-sealing effect, ensures that whole reaction environment is isolated with external, avoids the material oxidation.
5. And (3) cold rolling 80-90% of deformation on the basis of homogenizing annealing treatment, which is beneficial to refining crystal grains and improving the comprehensive mechanical property after aging annealing.
6. The parameters of homogenizing annealing are 1000 ℃, 12h and 85% of deformation of cold rolling, the parameters of aging annealing are that the strength of the product obtained when the product is kept at 800 ℃ for 1h is the highest, the yield strength at room temperature is 825MPa, the tensile strength is 933MPa, and the elongation at break is 15%; the parameters of homogenizing annealing are 1000 ℃, 12h and 85% of cold rolling deformation, the parameters of aging annealing are that the elongation of the product is highest when the temperature is kept at 850 ℃ for 1h, the yield strength at room temperature is 474MPa, the tensile strength is 730MPa, and the elongation at break is 29%.
7. After homogenization and aging annealing, the steel is rapidly cooled in a water-cooling quenching mode, so that the precipitation of brittle phases and compounds can be further inhibited, and the reduction of comprehensive mechanical properties can be further avoided.
Drawings
FIG. 1 is a graph comparing the stress-strain relationship in tensile tests for precipitation-strengthened high-entropy alloys without the tendency to precipitate the sigma phase prepared in examples 1 and 2;
FIG. 2 is an XRD diffractogram of the precipitation-strengthened high-entropy alloy having no tendency to precipitate the sigma phase prepared in example 1;
FIG. 3 is a room temperature tensile fracture morphology map of the precipitation-strengthened high-entropy alloy without the tendency of sigma phase precipitation prepared in example 1, wherein (a) is a fracture map, and (b) is an enlarged view of the fracture morphology;
fig. 4 is an SE SEM image of the precipitation-strengthened high-entropy alloy having no tendency to precipitate the σ phase, which was obtained in example 1, wherein (a) is an SE SEM image at 0.5h, and (b) is an SE SEM image at 1 h.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The molecular formula of the high-entropy alloy prepared by the embodiment is MnFeNiCu. Preferably, the purity of each of the constituent elements is 99.9% or more to minimize the introduction of impurities.
The Fe, Ni and Cu materials are weighed by a precision balance, and the weighed raw materials are put into absolute ethyl alcohol for ultrasonic cleaning and full drying to remove other impurities attached to the surface. Due to the characteristic that Mn element is easy to oxidize, the Mn raw material is cleaned twice by using 10 vol.% nitric acid alcohol solution before being weighed, then is cleaned once by using absolute ethyl alcohol in an ultrasonic cleaner, is weighed by using a precision balance after being dried and is put into smelting equipment to be smelted as soon as possible.
The pretreated alloy raw materials are sequentially put into a magnesium oxide crucible of a smelting furnace, Mn is put at the bottommost layer of the crucible, and the evaporation capacity is reduced to the maximum extent. Preferably, in order to fully remove air and form negative pressure self-sealing effect, the smelting furnace is vacuumized and then backfilled with argon gas by about 5X 104Pa, repeating the steps twice and then smelting. And keeping the temperature for 5 minutes after the metal is completely melted, and ensuring that the alloy is uniformly distributed. And after full smelting, pouring the molten metal into a high-purity graphite mold in an argon atmosphere to obtain a cylindrical metal ingot. Then the final alloy is obtained after drop casting, homogenizing annealing at 1000 ℃ for 12h, cold rolling for 85% of deformation and aging annealing at 800 ℃ for 1 h.
The alloy obtained in the example is an FCC phase, precipitates are dispersed and uniformly distributed in crystal grains, no enrichment is caused at crystal boundary, and the alloy is strengthened. The room temperature yield strength is 825MPa, the tensile strength is 933MPa, and the elongation at break is 15%. The precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency prepared by the example has excellent comprehensive mechanical properties.
Example 2
The molecular formula of the high-entropy alloy prepared by the embodiment is MnFeNiCu. Preferably, the purity of each of the constituent elements is 99.9% or more to minimize the introduction of impurities.
The Fe, Ni and Cu materials are weighed by a precision balance, and the weighed raw materials are put into absolute ethyl alcohol for ultrasonic cleaning and full drying to remove other impurities attached to the surface. Due to the characteristic that Mn element is easy to oxidize, the Mn raw material is cleaned twice by using 10 vol.% nitric acid alcohol solution before being weighed, then is cleaned once by using absolute ethyl alcohol in an ultrasonic cleaner, is weighed by using a precision balance after being dried and is put into smelting equipment to be smelted as soon as possible.
The pretreated alloy raw materials are sequentially put into a magnesium oxide crucible of a smelting furnace, Mn is put at the bottommost layer of the crucible, and the evaporation capacity is reduced to the maximum extent. Preferably, in order to fully remove air and form negative pressure self-sealing effect, the smelting furnace is vacuumized and then backfilled with argon gas by about 5X 104Pa, repeating the steps twice and then smelting. Vacuumizing the smelting furnace, and backfilling with argon gas about 5X 104Pa, repeating the steps twice and then smelting. And keeping the temperature for 5 minutes after the metal is completely melted, and ensuring that the alloy is uniformly distributed. And after full smelting, pouring the molten metal into a high-purity graphite mold in an argon atmosphere to obtain a cylindrical metal ingot. Then the final alloy is obtained after drop casting, homogenizing annealing at 1000 ℃ for 12h, cold rolling for 85% of deformation and aging annealing at 850 ℃ for 1 h.
The alloy obtained in this example also has a precipitate dispersed and distributed to strengthen the alloy matrix. The room temperature yield strength is 474MPa, the tensile strength is 730MPa, and the elongation at break is 29%. The precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency prepared by the embodiment is reduced in strength, but the elongation is greatly improved, and the regulation and control effect of aging parameters on performance is reflected.
In conclusion, the prepared precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency has good comprehensive mechanical properties. And the mechanical property of the high-entropy alloy is regulated and controlled by changing the aging parameters.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A preparation method of a precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency is characterized in that four pure metal materials of Fe, Ni, Mn and Cu in equal molar ratio are sequentially subjected to smelting, drop casting, homogenizing annealing, cold rolling and aging annealing to obtain the precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency; wherein the content of the first and second substances,
the parameter range of the homogenizing annealing is 910-1050 ℃, and the temperature is kept for 12-48 h; the temperature range of the aging annealing is 800-900 ℃, and the time range is 0.5-1 h.
2. The preparation method of claim 1, wherein Mn is placed at the bottommost layer of the crucible during smelting, and Fe, Ni and Cu are stacked layer by layer from bottom to top in the sequence of melting points from low to high above Mn.
3. The method of claim 2, wherein the smelting process is: smelting in an electric arc smelting furnace under the protection of negative pressure and argon atmosphere.
4. The method of claim 3, wherein the arc melting furnace is evacuated and backfilled with argon to 5 x 104And Pa, repeatedly vacuumizing and backfilling argon twice, and then smelting.
5. The method of claim 1, wherein the cold rolling is performed for a deformation amount of 80% to 90%.
6. The method of claim 5, wherein the cold rolling is performed at a strain level of 85%.
7. The method according to claim 6, wherein the parameters of the homogenizing anneal are 1000 ℃, 12 h; the parameters of the aging annealing are that the temperature is kept for 1h at 800 ℃ or 1h at 850 ℃.
8. The method according to any one of claims 1 to 7, wherein the homogenizing annealing and the aging annealing are both followed by rapid cooling by water-cooling quenching.
9. A precipitation-strengthened high-entropy alloy free from a tendency to precipitate a sigma phase, which is obtained by the production method according to any one of claims 1 to 8.
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Cited By (9)
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| CN112501569A (en) * | 2020-12-18 | 2021-03-16 | 哈尔滨工业大学（深圳） | Surface gradient high-entropy alloy layer and preparation method thereof |
| CN112962036A (en) * | 2021-02-03 | 2021-06-15 | 中国科学院力学研究所 | Preparation method of layered nano heterogeneous precipitation hardening high-entropy alloy |
| CN113430444A (en) * | 2021-06-18 | 2021-09-24 | 哈尔滨工程大学 | High-plasticity high-strength high-entropy alloy and preparation method thereof |
| CN113528921A (en) * | 2021-06-23 | 2021-10-22 | 沈阳航空航天大学 | C-containing high-performance multi-principal-element high-entropy alloy and preparation method thereof |
| CN113637885A (en) * | 2021-07-19 | 2021-11-12 | 哈尔滨工程大学 | Multicomponent FeNiCoAlTiZr super elastic alloy and preparation method thereof |
| CN113718152A (en) * | 2021-08-25 | 2021-11-30 | 哈尔滨工程大学 | High-temperature-resistant low-density Ni-Co-Cr-Fe-Al-Ti high-entropy alloy and preparation method thereof |
| CN113751722A (en) * | 2021-08-17 | 2021-12-07 | 温州大学 | Method for preparing FCC phase high-entropy alloy with high strength and high toughness |
| CN114086049A (en) * | 2021-11-17 | 2022-02-25 | 沈阳航空航天大学 | 2.0GPa grade CoCrNi-based medium entropy alloy with ultrahigh yield strength and plasticity and preparation method thereof |
| CN116855811A (en) * | 2023-07-05 | 2023-10-10 | 华中科技大学 | Zero-expansion dual-phase high-entropy alloy and preparation method thereof |
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| CN112501569A (en) * | 2020-12-18 | 2021-03-16 | 哈尔滨工业大学（深圳） | Surface gradient high-entropy alloy layer and preparation method thereof |
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| CN113430444A (en) * | 2021-06-18 | 2021-09-24 | 哈尔滨工程大学 | High-plasticity high-strength high-entropy alloy and preparation method thereof |
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| CN113751722A (en) * | 2021-08-17 | 2021-12-07 | 温州大学 | Method for preparing FCC phase high-entropy alloy with high strength and high toughness |
| CN113718152A (en) * | 2021-08-25 | 2021-11-30 | 哈尔滨工程大学 | High-temperature-resistant low-density Ni-Co-Cr-Fe-Al-Ti high-entropy alloy and preparation method thereof |
| CN114086049A (en) * | 2021-11-17 | 2022-02-25 | 沈阳航空航天大学 | 2.0GPa grade CoCrNi-based medium entropy alloy with ultrahigh yield strength and plasticity and preparation method thereof |
| CN116855811A (en) * | 2023-07-05 | 2023-10-10 | 华中科技大学 | Zero-expansion dual-phase high-entropy alloy and preparation method thereof |
| CN116855811B (en) * | 2023-07-05 | 2024-02-02 | 华中科技大学 | Zero-expansion dual-phase high-entropy alloy and preparation method thereof |
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