CN116287929A - High-strength high-plasticity CrCoNi-based multi-principal element alloy and preparation method thereof - Google Patents
High-strength high-plasticity CrCoNi-based multi-principal element alloy and preparation method thereof Download PDFInfo
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- 238000000265 homogenisation Methods 0.000 claims abstract description 14
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- 239000000203 mixture Substances 0.000 claims abstract description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The invention discloses a high-strength high-plasticity L1 2 Co-lattice nano precipitation strengthening CrCoNi-based multi-principal element alloy with elemental composition of (CrCoNi) according to atomic ratio 100‑a‑b Al a Ti b Wherein Cr, co and Ni have equal atomic ratio of 4.5-5.5,4.5-5.5. The CrCoNi-based multi-element alloy contains high-density L1 2 Coherent nano precipitated phase structure (Ni, co) 3 (Al, ti), the preparation method comprises: according to atomic ratio (CrCoNi) 100‑a‑b Al a Ti b Weighing a required amount of metal simple substance raw materials, smelting, and carrying out solution homogenization treatment for 1-4 hours at 1100-1300 ℃ on the obtained multi-principal element alloy raw ingot; rolling the multi-principal element alloy subjected to solution homogenization annealing by adopting a multipass cold rolling process, wherein the total thinning amount is 80% -85%;carrying out recrystallization annealing treatment for 1-30min at 1100-1300 ℃ on the rolled multi-principal element alloy; and carrying out isothermal aging heat treatment at 600-650 ℃ on the multi-principal element alloy after recrystallization annealing for 1-3h.
Description
Technical Field
The invention relates to the technical field of high-performance multi-principal element alloy, in particular to a high-strength high-plasticity L1 2 A coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy and a preparation method thereof.
Background
As an advanced structural metal material, the multi-principal element alloy has good application prospect in the fields of national defense and military industry and aerospace due to excellent high strength, ductility, fracture toughness, wear resistance and corrosion resistance, and has been widely studied in recent years.
The mechanical properties of the metallic structural material directly determine the structural stability and service performance of the device. The strength and the ductility are two most basic and important mechanical properties in the metal structural materials, and how to break through the inversion relation of the two mechanical properties and realize the strong plastic coordination of the materials are forever subjects in the research of the metal structural materials.
Single phase CrCoNi medium entropy alloys with FCC structure typically have high tensile ductility and excellent toughness, but their room temperature strength is typically very low. Second phase strengthening is a strategy that is considered to be very effective to substantially increase the strength of materials, which is useful in a number of applications including composite materials, but the strength is usually increased by this strategy at the expense of plasticity. The main reason of the strong plastic mutual exclusion is that the uneven plastic deformation caused by the introduction of the second phase with huge difference in matching with the matrix interface causes the dislocation to excessively plug at the two-phase interface so as to cause local stress concentration, so that cracks are initiated at the interface of the reinforcing phase and the matrix too early so as to cause plastic instability.
The patent specification with publication number CN 112853237A discloses a high yield strength CoCrNi-based medium entropy alloy, and the preparation method comprises selecting (CoCrNi) Al 3 Ti 3 Performing hot rolling, homogenizing annealing, hot rolling and cold rolling (total deformation is 60%), and recrystallization annealing at 900 ℃ for 1-2 h and 6Aging and heat preserving at 00 deg.c for 8-9 hr. (CoCrNi) Al prepared by the method of the patent technology 3 Ti 3 The elongation at break of the medium-entropy alloy is less than 35%, and although the tensile yield strength and the ultimate tensile strength of more than 1000MPa can be realized, the elongation at break is obviously reduced (less than 20%) correspondingly, and if the elongation at break of more than 30% is to be realized, the tensile yield strength cannot reach 1000MPa.
The patent specification with publication number CN 115233077A discloses a high-aluminum high-titanium content nano coherent precipitation reinforced CoCrNi-based medium entropy alloy, the composition of which is Co 37 Cr 14 Ni 37 Al 6 Ti 6 It contains high-density nano coherent precipitation structure (Ni, co, cr) 3 (Al, ti) nano coherent precipitated phase (Ni, co, cr) 3 (Al, ti) in L1 2 The phases exist in the form of phases. The preparation method comprises the steps of carrying out homogenization heat treatment, rolling (thickness reduction of 40% -70%), recrystallization heat treatment at 1000-1050 ℃ for 1.5-60min, aging heat treatment and the like on the suction cast medium entropy alloy plate. Co prepared by the technical method 37 Cr 14 Ni 37 Al 6 Ti 6 Although the elongation at break of the alloy can reach more than 40%, the corresponding tensile yield strength cannot reach 1000MPa, and the ultimate tensile strength cannot reach 1400MPa.
Therefore, developing a coherent nano precipitation strengthening multi-principal element alloy with high strength and high plasticity is an important scientific problem in the field of the prior structural multi-principal element alloy.
Disclosure of Invention
Aiming at the technical problems and the defects in the prior art, the invention provides a high-strength high-plasticity L1 2 The coherent nano precipitation strengthening CrCoNi-based multi-element alloy and the preparation method thereof solve the problems of unmatched toughness and uncoordinated strength of the CrCoNi-based multi-element alloy in the prior art.
The specific technical scheme is as follows:
high-strength high-plasticity L1 2 Co-lattice nano precipitation strengthening CrCoNi-based multi-principal element alloy, and high strength and high plasticity L1 2 Strong coherent nano precipitationThe element composition of the chemical CrCoNi-based multi-principal element alloy is (CrCoNi) according to the atomic ratio 100-a-b Al a Ti b Wherein Cr, co and Ni have equal atomic ratio of 4.5-5.5,4.5-5.5.
The high strength and high plasticity L1 2 Co-lattice nano precipitation strengthening CrCoNi-based multi-principal element alloy containing high-density L1 2 Coherent nano precipitated phase structure (Ni, co) 3 (Al, ti), its preparation method includes:
step 3, rolling the multi-principal element alloy subjected to solution homogenization annealing by adopting a multipass cold rolling process, wherein the total thinning amount is 80% -85%, and the thinning amount is favorable for refining alloy grains, so that the finally obtained alloy has high strength and high plasticity;
and 5, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 600-650 ℃, and the heat preservation time is 1-3h.
In a preferred embodiment, the high strength and high plasticity L1 2 The element composition of the coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy is (CrCoNi) according to the atomic ratio 90 Al 5 Ti 5 I.e. a=b=5.
Preferably, in the step 1, the mass fraction purity of the metal simple substance raw material is greater than or equal to 99.95%.
Preferably, in step 1, the metal simple substance raw material is polished to remove surface oxide skin before smelting.
Preferably, in step 1, the smelting specifically includes: and (3) putting the metal simple substance raw material into a vacuum arc melting furnace for melting under the argon protection atmosphere, wherein the melting current is kept at 400-500A, electromagnetic stirring is added in the melting process, and the melting is repeated for 4-6 times.
Preferably, the solution homogenizing treatment, the recrystallization annealing treatment and the isothermal aging heat treatment are all followed by cooling the multi-principal element alloy to room temperature by water quenching.
Most preferred L1 with high strength and high plasticity 2 The preparation method of the coherent nano precipitation strengthening CrCoNi-based multi-principal alloy comprises the following steps:
step 3, rolling the multi-principal element alloy subjected to solution homogenization treatment by adopting a multipass cold rolling process, wherein the total thinning amount is 85%;
and 5, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 600 ℃, and the heat preservation time is 2 hours.
The high-strength and high-plasticity L1 thus obtained 2 The room temperature tensile yield strength 1006MPa, the room temperature ultimate tensile strength 1460MPa and the elongation at break of 40.5 percent of the coherent nano precipitation strengthening CrCoNi-based multi-element alloy have excellent strong plastic matching at room temperature.
Compared with the prior art, the invention has the beneficial effects that:
the invention adds a small amount of L1 into CrCoNi multi-principal element matrix alloy with equal mole ratio of Cr, co and Ni 2 Nano precipitated phase forming elements Al and Ti to obtain L1 2 Coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy. Compared with the prior FCC system multi-principal element alloy, the invention obtains L1 2 The coherent nano precipitation strengthening CrCoNi-based multi-element alloy has better strength-plasticity matching, and the preparation method of the high-strength high-plasticity L12 coherent nano precipitation strengthening CrCoNi-based multi-element alloy provided by the invention is simple and convenient to operate, and has potential advantages for mass production of multi-element alloy with excellent mechanical properties and engineering application popularization.
The alloy prepared by the invention can meet the application scenes of most structural materials, and has great engineering application prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern of the CrCoNi-based multi-component alloy prepared in example 1.
FIG. 2 is a high angle annular dark field scanning transmission electron microscope (HAADF-STEM) characterization and atomic scale EDS profile (EDS-mapping) of the interfacial precipitation phase atomic resolution of the CrCoNi-based multi-principal component alloy prepared in example 1.
FIG. 3 is a plot of room temperature quasi-static tensile engineering stress versus engineering strain for the CrCoNi-based multi-principal component alloy prepared in example 1.
FIG. 4 is a plot of room temperature quasi-static tensile engineering stress versus engineering strain for the CrCoNi-based multi-principal component alloy prepared in comparative example 1.
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of a CrCoNi-based multi-component alloy prepared in comparative example 2.
Detailed Description
The invention will be further elucidated with reference to the drawings and to specific embodiments. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention.
The methods of operation, under which specific conditions are not noted in the examples below, are generally in accordance with conventional conditions, or in accordance with the conditions recommended by the manufacturer.
Example 1
High-strength high-plasticity L1 2 The preparation method of the coherent nano precipitation strengthening CrCoNi-based multi-principal alloy specifically comprises the following steps:
step 3, placing the metal simple substance raw material weighed in the step 2 into a vacuum arc melting furnace for melting under the protection of high-purity argon; wherein the smelting current is kept at 450A, electromagnetic stirring is added in the smelting process, and the smelting is repeated for 5 times, so as to obtain a multi-principal element alloy original cast ingot;
step 7, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 600 ℃, and the heat preservation time is 2 hours;
it should be noted that the solution homogenizing treatment, the recrystallization treatment and the isothermal aging heat treatment are all followed by cooling the multi-principal element alloy to room temperature by water quenching.
In order to determine the phase composition of the multi-principal component alloy prepared in this example, an X-ray diffraction test was performed on the multi-principal component alloy prepared in this example, and the obtained test spectrum is shown in fig. 1, and only characteristic peaks of the FCC structure are seen in the spectrum, but no diffraction peaks of other phases are seen.
To examine whether the multi-principal component alloy prepared in this example is precipitated at the interface with fine deleterious phases such as Sigma phase and Hesl phase which are difficult to characterize by XRDuer, the structure at the interface was subjected to atomic-resolution high-angle annular dark-field scanning transmission electron microscope (HAADF-STEM) characterization and atomic-level EDS-mapping characterization, and the results are shown in FIG. 2, from which it is clear that the interface precipitated phase is chromium-depleted L1 2 Ordered phases (Ni, co) 3 (Al, ti) and a chromium-rich BCC phase.
In order to determine the room temperature mechanical properties of the multi-element alloy prepared in this example, a room temperature quasi-static tensile test was performed on the multi-element alloy prepared in this example, and the obtained tensile engineering stress-engineering strain curve is shown in fig. 3, from which it is known that the multi-element alloy prepared in this example has a room temperature tensile yield strength of 1006MPa, a room temperature ultimate tensile strength of 1460MPa, and a fracture elongation of 40.5%, so that the multi-element alloy prepared in this example has excellent strong plastic matching at room temperature.
Comparative example 1
The preparation method of the CrCoNi-based multi-principal element alloy specifically comprises the following steps:
step 3, placing the metal simple substance raw material weighed in the step 2 into a vacuum arc melting furnace for melting under the protection of high-purity argon; wherein the smelting current is kept at 450A, electromagnetic stirring is added in the smelting process, and the smelting is repeated for 5 times, so as to obtain a multi-principal element alloy original cast ingot;
step 7, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 900 ℃, and the heat preservation time is 0.5h;
it should be noted that the solution homogenizing treatment, the recrystallization treatment and the isothermal aging heat treatment are all followed by cooling the multi-principal element alloy to room temperature by water quenching.
In order to determine the room temperature mechanical properties of the multi-principal element alloy prepared in this comparative example, room temperature quasi-static tensile test was performed on the multi-principal element alloy prepared in this comparative example, and the resulting tensile engineering stress-engineering strain curve is shown in fig. 4, from which it is known that the room temperature tensile yield strength 1120MPa, the room temperature ultimate tensile strength 1563MPa, and the elongation at break were only 17%, whereby the room temperature mechanical properties of the multi-principal element alloy prepared in this comparative example were slightly improved but the plasticity was greatly reduced, relative to the multi-principal element alloy prepared in example 1.
Comparative example 2
step 3, placing the metal simple substance raw material weighed in the step 2 into a vacuum arc melting furnace for melting under the protection of high-purity argon; wherein the smelting current is kept at 450A, electromagnetic stirring is added in the smelting process, and the smelting is repeated for 5 times, thus obtaining a multi-principal element alloy original cast ingot (CrCoNi) 86 Al 7 Ti 7 ;
And 4, carrying out solution homogenization annealing treatment after smelting, wherein the annealing temperature is 1200 ℃, the heat preservation time is 2 hours, and then cooling the multi-principal element alloy to room temperature by adopting a water quenching mode.
As a result of SEM characterization in FIG. 5, (CrCoNi) 86 Al 7 Ti 7 A large amount of Sigma phase, which is a detrimental precipitated phase that causes brittleness of the grain boundary, is precipitated at the grain boundary.
Further, it will be understood that various changes and modifications may be made by those skilled in the art after reading the foregoing description of the invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Claims (8)
1. High-strength high-plasticity L1 2 The coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy is characterized in that the high-strength high-plasticity L1 2 The element composition of the coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy is (CrCoNi) according to the atomic ratio 100-a- b Al a Ti b Wherein Cr, co and Ni have equal atomic ratio of 4.5-5.5,4.5-5.5;
the high strength and high plasticity L1 2 Co-lattice nano precipitation strengthening CrCoNi-based multi-principal element alloy containing high-density L1 2 Coherent nano precipitated phase structure (Ni, co) 3 (Al, ti), its preparation method includes:
step 1, according to the atomic ratio (CrCoNi) 100-a-b Al a Ti b Weighing a required amount of metal simple substance raw materials, and smelting to obtain a multi-principal element alloy original ingot;
step 2, carrying out solution homogenization annealing treatment on the multi-principal element alloy original cast ingot after smelting, wherein the annealing temperature is 1100-1300 ℃, and the heat preservation time is 1-4 hours;
step 3, rolling the multi-principal element alloy subjected to solution homogenization treatment by adopting a multipass cold rolling process, wherein the total thinning amount is 80% -85%;
step 4, carrying out recrystallization annealing treatment on the rolled multi-principal element alloy, wherein the annealing temperature is 1100-1300 ℃, and the heat preservation time is 1-30min;
and 5, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 600-650 ℃, and the heat preservation time is 1-3h.
2. The high-strength high-plasticity L1 as claimed in claim 1 2 The coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy is characterized in that the high-strength high-plasticity L1 2 The element composition of the coherent nano precipitation strengthening CrCoNi-based multi-principal element alloy is (CrC) according to the atomic ratiooNi) 90 Al 5 Ti 5 。
3. High-strength high-plasticity L1 2 The preparation method of the coherent nano precipitation strengthening CrCoNi-based multi-principal-element alloy is characterized by comprising the following steps of:
step 1, according to the atomic ratio (CrCoNi) 100-a-b Al a Ti b Wherein Cr, co and Ni are taken in an equal atomic ratio, a is more than or equal to 4.5 and less than or equal to 5.5,4.5, b is more than or equal to 5.5, and the required amount of metal simple substance raw materials are weighed and smelted to obtain a multi-principal element alloy original cast ingot;
step 2, carrying out solution homogenization annealing treatment on the multi-principal element alloy original cast ingot after smelting, wherein the annealing temperature is 1100-1300 ℃, and the heat preservation time is 1-4 hours;
step 3, rolling the multi-principal element alloy subjected to solution homogenization treatment by adopting a multipass cold rolling process, wherein the total thinning amount is 80% -85%;
step 4, carrying out recrystallization annealing treatment on the rolled multi-principal element alloy, wherein the annealing temperature is 1100-1300 ℃, and the heat preservation time is 1-30min;
step 5, carrying out isothermal aging heat treatment on the multi-principal element alloy subjected to recrystallization annealing, wherein the annealing temperature is 600-650 ℃, and the heat preservation time is 1-3h, thus obtaining the high-strength high-plasticity L1 2 Co-lattice nano precipitation strengthening CrCoNi-based multi-principal element alloy containing high-density L1 2 Coherent nano precipitated phase structure (Ni, co) 3 (Al,Ti)。
4. A method according to claim 3, wherein in step 1, a=b=5.
5. The method according to claim 3, wherein in the step 1, the mass fraction purity of the metal simple substance raw material is 99.95% or more.
6. The method according to claim 3, wherein in step 1, the elemental metal raw material is polished to remove surface scale before smelting.
7. The method according to claim 3, wherein in step 1, the smelting specifically comprises: and (3) putting the metal simple substance raw material into a vacuum arc melting furnace for melting under the argon protection atmosphere, wherein the melting current is kept at 400-500A, electromagnetic stirring is added in the melting process, and the melting is repeated for 4-6 times.
8. The method according to claim 3, wherein the solution homogenizing treatment, the recrystallization annealing treatment, and the isothermal aging heat treatment are all followed by cooling the multi-component alloy to room temperature by water quenching.
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CN117248169A (en) * | 2023-08-23 | 2023-12-19 | 河南省科学院材料研究所 | Optimizing L1 2 Preparation process of phase precipitation strengthening high-entropy alloy |
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CN117248169A (en) * | 2023-08-23 | 2023-12-19 | 河南省科学院材料研究所 | Optimizing L1 2 Preparation process of phase precipitation strengthening high-entropy alloy |
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