CN115478201A - CoNiV-based medium-entropy alloy containing dual ordered phases and preparation method thereof - Google Patents
CoNiV-based medium-entropy alloy containing dual ordered phases and preparation method thereof Download PDFInfo
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- CN115478201A CN115478201A CN202211130258.4A CN202211130258A CN115478201A CN 115478201 A CN115478201 A CN 115478201A CN 202211130258 A CN202211130258 A CN 202211130258A CN 115478201 A CN115478201 A CN 115478201A
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Abstract
The invention relates to the technical field of metal materials, in particular to a CoNiV-based medium-entropy alloy containing double ordered phases and a preparation method thereof. The invention provides a CoNiV-based medium entropy alloy, the chemical composition of which is (CoNiV) 1‑x‑y Al x Ti y In terms of atom mole percentage content, the value range of x is 0.5-3%; the value range of y is 0.5-2%; the CoNiV-based medium entropy alloy comprises L1 2 Short range ordered phase and L1 1 A short-range ordered phase; the above-mentioned L1 2 The size of the short-range ordered phase is 1-5 nm; the above-mentioned L1 1 The size of the short-range ordered phase is less than 1nm. The CoNiV-based medium entropy alloy provided by the invention has higher obdurability in a low-temperature environmentHigh.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a CoNiV-based medium-entropy alloy containing double ordered phases and a preparation method thereof.
Background
The CoNiV-based medium entropy alloy is a newly-appeared novel single-phase face-centered cubic alloy, has excellent properties such as normal-temperature strong plasticity balance, low-temperature resistance, hydrogen embrittlement resistance and the like, is a structural material for hydrogen energy equipment with great application potential, and has great application in the fields of aerospace, transportation and the like. How to further improve the mechanical property of the CoNiV-based medium entropy alloy is a difficult problem to be solved at present.
At present, the introduction of a proper precipitated phase into the medium-entropy alloy becomes one of effective ways for enhancing the strength, wherein Al and Ti are added to introduce L1 2 The coherent precipitated phase can greatly improve the strength of the CoNiV-based medium entropy alloy. However, conventional L1 2 The introduction of the long-range ordered precipitated phase causes local stress concentration in the CoNiV-based medium entropy alloy, so that the plasticity of the CoNiV-based medium entropy alloy in a low-temperature environment is sharply reduced.
Disclosure of Invention
In view of the above, the present invention aims to provide a CoNiV-based entropy alloy containing a dual ordered phase and a preparation method thereof, and the CoNiV-based entropy alloy provided by the present invention has high toughness in a low temperature environment.
In order to achieve the above object, the present invention provides a CoNiV-based entropy alloy containing a double ordered phase, the chemical composition of which is (CoNiV) 1-x-y Al x Ti y The value range of x is 0.5-3% by atomic mol percentage; the value range of y is 0.5-2%;
the CoNiV-based medium entropy alloy comprises L1 2 Short range ordered phase sum L1 1 Short range ordered phase, said L1 2 The size of the short-range ordered phase is 1-5 nm; the above-mentioned L1 1 The size of the short-range ordered phase is less than 1nm.
The invention also provides a preparation method of the CoNiV-based medium entropy alloy, which comprises the following steps:
smelting alloy raw materials corresponding to the chemical element composition of the CoNiV-based medium entropy alloy to obtain a pre-alloyed ingot;
sequentially carrying out annealing treatment, deformation treatment, solid solution treatment and aging treatment on the pre-alloyed ingot to obtain the CoNiV-based medium entropy alloy;
the temperature of the aging treatment is 600-850 ℃, and the heat preservation time of the aging treatment is 0.5-5 h.
Preferably, the annealing temperature is 1000-1200 ℃, and the heat preservation time is 20-25 h; the annealing is performed in an argon atmosphere.
Preferably, the manner of deformation treatment comprises cold rolling.
Preferably, the temperature of the solution treatment is 1000-1100 ℃, and the holding time of the solution treatment is 1-60 min.
Preferably, the rate of temperature increase to the temperature of the solution treatment is 5 to 10 ℃/min.
Preferably, the rate of temperature increase to the temperature of the aging treatment is 5 to 10 ℃/min.
The invention provides a CoNiV-based medium entropy alloy containing double ordered phases, and the chemical composition of the CoNiV-based medium entropy alloy is (CoNiV) 1-x-y Al x Ti y The value range of x is 0.5-3% by atomic mol percentage; the value range of y is 0.5-2%; the CoNiV-based medium entropy alloy comprises L1 2 Short range ordered phase and L1 1 A short-range ordered phase; the above-mentioned L1 2 The size of the short-range ordered phase is 1-5 nm; the above-mentioned L1 1 The size of the short-range ordered phase is less than 1nm. The invention avoids other intermetallic compounds by controlling the dosage of Al and Ti elements in the above range. L1 2 The short range ordered phase is rich in Al and Ti elements, and L1 1 The short-range ordered phase is rich in Co, ni and V elements. The scale of the dual nanometer short-range ordered phase is controlled below 5nm through a reasonable heat treatment process, and a good precipitation strengthening effect can be achieved. At the same timeWhen the stress reaches a certain level, the dislocation easily cuts through two short-range orders, thus comparing with the traditional L1 2 The invention can not affect the plastic deformation while improving the strength. Therefore, the CoNiV-based medium entropy alloy still has higher obdurability in a low temperature state.
The invention also provides a preparation method of the CoNiV-based medium entropy alloy, which comprises the following steps:
smelting alloy raw materials corresponding to the chemical element composition of the CoNiV-based medium entropy alloy to obtain a pre-alloyed ingot; and sequentially carrying out annealing treatment, deformation treatment, solid solution treatment and aging treatment on the pre-alloyed ingot to obtain the CoNiV-based medium entropy alloy. The invention obtains the short-range ordered strengthening phase with two scales below 5nm by limiting the aging temperature and time. Therefore, the CoNiV-based medium entropy alloy still has higher obdurability in a low-temperature state.
Drawings
FIG. 1 is a photograph prepared in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 An X-ray diffraction result graph of the medium-entropy alloy;
FIG. 2 is a photograph prepared in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 L1 in the medium entropy alloy 2 Transmission electron microscopy images of short-range ordered phases;
FIG. 3 is prepared as in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 L1 in the medium entropy alloy 1 Transmission electron microscopy images of short-range ordered phases.
FIG. 4 is prepared as in example 2 (CoNiV) 95 Al 3 Ti 2 Transmission electron microscopy images of the medium entropy alloy.
Detailed Description
The invention provides a CoNiV-based medium entropy alloy containing double ordered phases, and the chemical composition of the CoNiV-based medium entropy alloy is (CoNiV) 1-x-y Al x Ti y The value range of x is 0.5-3% by atomic mol percentage; the value range of y is 0.5-2%; the CoNiV-based medium entropy alloy comprises L1 2 Short range ordered phase and L1 1 A short-range ordered phase; the above-mentionedL1 2 The size of the short-range ordered phase is 1-5 nm; the size of the short-range ordered phase is less than 1nm.
In the present invention, the chemical composition of the CoNiV-based intermediate entropy alloy is (CoNiV) 1-x-y Al x Ti y The value range of x is 0.5-3%, preferably 1-2%; the value range of y is 0.5-2%, preferably 1-1.5%.
In the present invention, said L1 2 The size of the short-range ordered phase is 1 to 5nm, preferably 2 to 3nm. In the present invention, said L1 1 The size of the short-range ordered phase is < 1nm, more preferably 0.1 to 0.5nm.
The invention also provides a preparation method of the CoNiV-based medium entropy alloy, which comprises the following steps:
smelting the alloy raw material for the second time corresponding to the chemical element composition of the CoNiV-based medium entropy alloy to obtain a pre-alloyed ingot;
and sequentially carrying out annealing treatment, deformation treatment, solid solution treatment and aging treatment on the pre-alloyed ingot to obtain the CoNiV-based medium entropy alloy.
According to the invention, the chemical elements corresponding to the CoNiV-based medium entropy alloy are melted for the second time to obtain a pre-alloyed ingot.
In the invention, the purity of the alloy raw material is preferably more than or equal to 99.9%. The invention has no special requirement on the source of the raw materials, and the raw materials with the sources known by the technicians in the field can be adopted.
In the present invention, the temperature of the melting is preferably 1800 to 2100 ℃, more preferably 1900 to 2000 ℃. In the invention, the raw materials are preferably repeatedly smelted, and the smelting frequency is preferably 6 to 8 times. In the invention, the time for each smelting is preferably 30-60 s, and the repeated smelting of the raw materials is beneficial to more uniform alloy components.
After obtaining the ingot, the pre-alloyed ingot is sequentially subjected to annealing treatment, deformation treatment, solid solution treatment and aging treatment to obtain the CoNiV-based intermediate entropy alloy.
In the invention, the temperature of the annealing treatment is preferably 1000-1200 ℃, and more preferably 1100 ℃; the time is preferably 20 to 25 hours, more preferably 24 hours. In the present invention, the annealing treatment is preferably performed in an argon atmosphere.
In the present invention, it is preferable to further perform water quenching after the annealing treatment, and the water quenching is not particularly limited in the present invention and may be performed by a method well known in the art.
In the present invention, the deformation treatment mode includes cold rolling. In the present invention, the deformation amount of the deformation treatment is preferably 75 to 85%, more preferably 80%.
In the present invention, the temperature of the solution treatment is preferably 1000 to 1100 ℃, more preferably 1010 to 1070 ℃, and the time of the solution treatment is preferably 1 to 60min, more preferably 2 to 20min. In the present invention, the rate of temperature increase to the solution treatment temperature is preferably 5 to 10 ℃/min, and more preferably 8 to 9 ℃/min. In the present invention, the solution treatment is preferably performed in a muffle furnace.
In the present invention, it is preferable to further perform water quenching after the solution treatment, and the water quenching is not particularly limited in the present invention, and may be performed by a water quenching operation well known to those skilled in the art.
In the invention, the temperature of the aging treatment is preferably 600-850 ℃, and more preferably 650-800 ℃; the time for the aging treatment is preferably 0.5 to 5 hours, and more preferably 2 to 3 hours. In the present invention, the rate of temperature increase to the temperature for the aging treatment is preferably 5 to 10 ℃/min, and more preferably 8 to 9 ℃/min. In the present invention, the aging treatment is preferably performed in a muffle furnace.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(CoNiV) 96 Al 1.5 Ti 1.5 System of (1)Preparing:
according to atomic mole percentage, the metal V, the metal Co, the metal Ni, the metal Al and the metal Ti are mixed according to the ratio of V:32.3%, co:32.3%, ni:32.3 percent of Al, 1.5 percent of Al and 1.5 percent of Ti (the purity of each raw material is 99.9 percent), and the total mass is 120g.
Putting the raw materials into an electric arc melting furnace, repeatedly melting for 6 times, wherein the melting temperature is 2000 ℃ each time, and the melting time is 30s each time, so as to obtain the pre-alloyed ingot.
Heating a muffle furnace to 1100 ℃ at a speed of 10 ℃/min, then placing the pre-alloyed ingot into the furnace for annealing treatment for 24 hours, carrying out water quenching after annealing, carrying out wire cutting on the water-quenched alloy to obtain alloy sheets with the length, width and height of 100 x 20 x 10mm respectively, and then carrying out cold rolling on the obtained alloy sheets with the rolling amount of 80%.
And (3) carrying out solution treatment on the alloy sheet after cold rolling at the temperature of 1100 ℃ for 5min, and then carrying out water quenching.
Aging the alloy sheet after water quenching at 800 deg.C for 2h, and air cooling to room temperature to obtain (VCoNi) 94 Al 4 Ti 2 And (3) medium-entropy alloy.
FIG. 1 is a photograph prepared in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 The X-ray diffraction result diagram of the medium entropy alloy is shown in figure 1: the alloy matrix is of a face-centered cubic structure.
FIG. 2 is a photograph prepared in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 L1 in the medium entropy alloy 2 Transmission electron microscopy images of short-range ordered phases; FIG. 3 is prepared as in example 1 (CoNiV) 97 Al 1.5 Ti 1.5 L1 in the medium entropy alloy 1 The transmission electron microscopy images of the short-range ordered phase are shown in FIGS. 2 to 3: the alloy contains L1 2 Short range ordered phase and L1 1 Short range ordered phase two-stage ordered phase, L1 2 Short range order phase scale of 1-5 nm and L1 1 The size of the short-range ordered phase is below 1nm.
The invention also relates to (CoNiV) prepared in example 1 97 Al 1.5 Ti 1.5 The intermediate entropy alloy is subjected to drawingThe stretching test method comprises the following steps: flat dog-bone-shaped tensile specimens were cut from the said test specimens of the mid-entropy alloy material by wire cutting. The gauge length, width and thickness of the tensile specimen were 8mm, 1.8mm and 1.2mm, respectively. Under the conditions of room temperature and 77K (-196.15 ℃), a universal Testing machine (Care Material Testing System) was used at 10 deg.C -3 s -1 The uniaxial tensile test was performed at a fixed strain rate of (2). Each tensile test was repeated three times to ensure data reproducibility, test results: at room temperature, the (CoNiV) 97 Al 1.5 Ti 1.5 The medium entropy alloy has excellent tensile strength and ductility, the (CoNiV) 97 Al 1.5 Ti 1.5 The medium entropy alloy exhibits ultra-high yield strength and ultimate tensile strength of 1.0GPa and 1.5GPa, respectively, and an elongation of approximately 37.3%. Example 1 prepared the resulting (CoNiV) at a temperature of 77K (-196.15 deg.C) 97 Al 1.5 Ti 1.5 The yield strength and the ultimate tensile strength of the medium-entropy alloy are 1.2GPa and 1.85GPa respectively, and the elongation is improved to 43 percent.
Example 2
(CoNiV) 95 Al 3 Ti 2 Preparing the medium entropy alloy by mixing metal V, metal Co, metal Ni, metal Al and metal Ti according to the atomic mole percentage: 31.7%, co:31.7%, ni:31.7% of Al, 3% of Ti and 2% of Ti (purity of raw material: 99.9%) in a total mass of 150g to obtain (CoNiV) 95 Al 3 Ti 2 And (3) medium-entropy alloy.
FIG. 4 is prepared as in example 2 (CoNiV) 95 Al 3 Ti 2 Transmission electron microscopy of medium entropy alloy containing L1 2 Short range ordered phase and L1 1 Short range ordered phase two-stage ordered phase, L1 2 Short range order phase scale of 1-5 nm and L1 1 The size of the short-range ordered phase is below 1nm.
The invention also relates to (CoNiV) prepared in example 2 95 Al 3 Ti 2 The medium entropy alloy is subjected to tensile test (CoNiV) 95 Al 3 Ti 2 The medium entropy alloy exhibits ultra-high yield strength and ultimate tensile strength of 1.15GPa and 1.62GPa, respectively, and approximately 32.3% elongation. Example 2 prepared the resulting (CoNiV) at a temperature of 77K (-196.15 deg.C) 95 Al 3 Ti 2 The yield strength and the ultimate tensile strength of the medium-entropy alloy are 1.3GPa and 1.95GPa respectively, and the elongation is improved to 38%.
Compared with other reported medium entropy alloys or transformation induced plasticity steels, dual phase steels and even martensitic steels, (CoNiV) 1-x-y Al x Ti y (x = 0.5-3%, y = 0.5-2%) the medium entropy alloy material has excellent combination of low temperature tensile strength and ductility, and has potential as a structural material in the field of low temperature engineering.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. A CoNiV-based entropy alloy containing double ordered phases is characterized in that the chemical composition of the CoNiV-based entropy alloy is (CoNiV) 1-x-y Al x Ti y The value range of x is 0.5-3% by atomic mol percentage; the value range of y is 0.5-2%;
the CoNiV-based medium entropy alloy comprises L1 2 Short range ordered phase and L1 1 A short-range ordered phase; the above-mentioned L1 2 The size of the short-range ordered phase is 1-5 nm; the above-mentioned L1 1 The size of the short-range ordered phase is less than 1nm.
2. The method for preparing CoNiV-based intermediate entropy alloy according to claim 1, comprising the steps of:
smelting alloy raw materials corresponding to the chemical element composition of the CoNiV-based medium entropy alloy in claim 1 to obtain a pre-alloyed ingot;
sequentially carrying out annealing treatment, deformation treatment, solid solution treatment and aging treatment on the pre-alloyed ingot to obtain the CoNiV-based medium-entropy alloy;
the temperature of the aging treatment is 600-850 ℃, and the heat preservation time of the aging treatment is 0.5-5 h.
3. The preparation method according to claim 2, characterized in that the annealing temperature is 1000-1200 ℃ and the holding time is 20-25 h; the annealing is performed in an argon atmosphere.
4. A method of manufacturing according to claim 2, wherein the deformation process comprises cold rolling.
5. The method according to claim 2, wherein the temperature of the solution treatment is 1000 to 1100 ℃ and the holding time of the solution treatment is 1 to 60min.
6. The production method according to claim 5, wherein a rate of temperature rise to the solution treatment temperature is 5 to 10 ℃/min.
7. The production method according to claim 2, wherein the rate of temperature increase to the temperature for the aging treatment is 5 to 10 ℃/min.
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| CN115948671A (en) * | 2023-02-17 | 2023-04-11 | 南京理工大学 | Material and method for further refining nanocrystalline grains through low-temperature annealing |
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| CN112048682A (en) * | 2020-08-31 | 2020-12-08 | 华东理工大学 | Processing heat treatment process for medium-entropy alloy plate |
| CN112853237A (en) * | 2021-01-05 | 2021-05-28 | 中北大学 | Preparation method of high-yield-strength CoCrNi-based medium-entropy alloy |
| CN114457270A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | L12Medium-entropy alloy with particles strongly plasticized and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112048682A (en) * | 2020-08-31 | 2020-12-08 | 华东理工大学 | Processing heat treatment process for medium-entropy alloy plate |
| CN112853237A (en) * | 2021-01-05 | 2021-05-28 | 中北大学 | Preparation method of high-yield-strength CoCrNi-based medium-entropy alloy |
| CN114457270A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | L12Medium-entropy alloy with particles strongly plasticized and preparation method thereof |
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| XUEFEI CHEN等: ""Direct observation of chemical short-range order in a medium-entropy alloy"" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115948671A (en) * | 2023-02-17 | 2023-04-11 | 南京理工大学 | Material and method for further refining nanocrystalline grains through low-temperature annealing |
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