CN115305402A - Al-Co-V-Fe-Ni biphase high-strength-toughness high-entropy alloy and preparation method thereof - Google Patents
Al-Co-V-Fe-Ni biphase high-strength-toughness high-entropy alloy and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 14
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
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Abstract
The invention belongs to the technical field of high-entropy alloy and preparation thereof, and discloses an Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy and a preparation method thereof, wherein the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy comprises the following elements in percentage by mol: 10-14% Al, 13-18% Co, 15-20% V, 24-30% by weight Fe, 24-30% Ni, the total mole percentage of all the elemental constituents being 100%, and the dual phase in the dual phase high toughness high entropy alloy being the BCC phase and the FCC phase. The Al-Co-V-Fe-Ni two-phase high-entropy alloy prepared by the invention has a compact two-phase structure and excellent tensile mechanical property, the ultimate tensile strength is more than or equal to 1000MPa, and the elongation is more than or equal to 20%.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy and preparation thereof, in particular to Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy and a preparation method thereof.
Background
The high-entropy alloy has been proposed to date, has generated a great influence in the field of metal materials, has obtained a series of research results, and has still received great attention from researchers to date. However, the current application of the high-entropy alloy is rarely reported, and the fundamental reason is that the high-entropy alloy is a single solid solution phase. Common high entropy alloys are mainly divided into single solid solution FCC phase and single solid solution BCC phase. The FCC phase has high elongation but low strength, and the BCC phase has high strength and hardness but poor plasticity. Therefore, to achieve a synergistic increase in strength and plasticity is a significant challenge for high entropy alloy engineering applications.
In recent years, the scholars propose a novel high-entropy alloy, namely a eutectic high-entropy alloy, which comprises an FCC + BCC two-phase microstructure and is considered to have great potential in realizing obdurability matching of the high-entropy alloy. The eutectic high-entropy alloy reported at present is AlCoCrFeNi 2.1 ，CoCrFeNiMo 1.2 CoFeNiVZrx, and the like. However, the composition system of eutectic high entropy alloys is still not perfect so far. Therefore, how to design and develop a high-entropy alloy with dual-phase, high toughness and high entropy becomes a problem which needs to be solved urgently.
Therefore, the invention provides an Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy and a preparation method thereof.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides an Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy and a preparation method thereof.
The Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy and the preparation method thereof are realized by the following technical scheme:
the first purpose of the invention is to provide an Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy, which comprises the following elements in percentage by mole:
10％～14％Al、13％～18％Co、15％～20％V、24％～30％Fe、24％～30％Ni；
the total mole percentage of all elemental constituents is 100%.
Furthermore, the two phases in the two-phase high-strength high-entropy alloy are a BCC phase and an FCC phase.
Further, the phase of the FCC phase is Fe2AlV, and the phase of the BCC is AlNi3.
The second purpose of the invention is to provide a preparation method of the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy, which comprises the following steps:
and 2, placing the weighed metal raw materials in a vacuum arc melting furnace, sequentially performing gas purification treatment and vacuum-pumping treatment, and then performing melting treatment to obtain the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy.
Further, the purity of each of the metal raw materials was 99.99wt%.
Further, the particle size of each of the metal materials is 3 to 5mm.
Further, the gas purification treatment is as follows: vacuumizing the vacuum arc furnace to 5-8 Pa, filling argon to the pressure of-0.09 MPa to-0.08 MPa, vacuumizing again, and repeating for at least three times to finish the furnace body purification treatment.
Further, the vacuum degree of the vacuum pumping treatment is less than or equal to 3 multiplied by 10 -3 Pa。
Further, the smelting treatment comprises the following steps: firstly, starting arc with 50-55A of smelting current, then smelting with 300-500A of smelting current until the metal raw material is completely melted, and then adding 8-10A of induced current to magnetically stir for 30-50 s, thus finishing the primary smelting treatment.
Further, the smelting process is repeated at least 5 times.
Compared with the prior art, the invention has the following beneficial effects:
the invention fully considers the interaction among elements, fully considers the atomic radius and the physicochemical parameters of the elements, forms a stable second phase on the basis of ensuring the strength to generate a compact BCC/FCC dual-phase structure, and ensures the realization of the strong toughness cooperative matching of the material.
The Al-Co-V-Fe-Ni two-phase high-entropy alloy prepared by the invention has a compact two-phase structure; the Al-Co-V-Fe-Ni two-phase high-entropy alloy prepared by the invention has excellent tensile mechanical property, the ultimate tensile strength is more than or equal to 1000MPa, and the elongation is more than or equal to 20%; moreover, the raw materials of the selected alloy elements have no volatility, so that the condition that the smelting equipment is damaged due to the addition of volatile elements in the smelting process is avoided.
The invention adopts a vacuum arc melting method to melt each metal simple substance, and in the melting process, all the metal simple substances are fully contacted, so that elements with the same crystal structure or close atomic sizes are easy to dissolve mutually, and Fe, V elements and part of Al elements form an FCC phase with a phase of Fe2AlV together, while Ni and the rest Al elements form a BCC phase with a phase of AlNi3, and two phases which are uniformly distributed are typical eutectic structures, thereby obviously improving the obdurability of the material.
Drawings
FIG. 1 is a stress-strain curve of the high entropy alloy prepared in example 1;
FIG. 2 is a stress-strain curve of the high entropy alloy prepared in example 2;
FIG. 3 is an optical microstructure photograph of the high entropy alloy prepared in example 1;
FIG. 4 is a photograph of the optical microstructure of the high entropy alloy prepared in example 2;
FIG. 5 is a scanning electron micrograph of the high entropy alloy prepared in example 1;
FIG. 6 is a scanning electron micrograph of the high entropy alloy prepared in example 2;
FIG. 7 is the XRD phase detection result of the high entropy alloy prepared by example 1;
FIG. 8 is a schematic positional view of the TEM electron diffraction pattern calibration of the high-entropy alloy prepared in example 1;
FIG. 9 is a TEM electron diffraction pattern calibration analysis of the FCC phase in the left circle of FIG. 8;
FIG. 10 shows the results of a nominal analysis of the TEM electron diffraction pattern of the BCC phase at the right circle in FIG. 8.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1
The embodiment provides an Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy, wherein two phases in the two-phase high-toughness high-entropy alloy are a BCC phase and an FCC phase, and the two-phase high-toughness high-entropy alloy comprises the following elements in percentage by mol: 13% of Al, 15% of Co, 18% of V, 27% of Fe and 27% of Ni.
The preparation method of the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy of the embodiment is as follows:
step one, respectively weighing metal raw materials corresponding to each element component according to the proportioning relation for later use;
it should be noted that the present invention does not limit the specific composition of each metal material as long as the respective metal elements can be provided in the respective contents. In this example, metals Al, co, V, fe, and Ni having a purity of 99.99Wt% and a particle diameter of 3mm are preferably used as the metal raw materials.
Secondly, placing the weighed metal Al, co, V, fe and Ni into a vacuum arc melting furnace, then closing a furnace door, and sequentially performing gas purification treatment and vacuum-pumping treatment;
the present invention is not limited to a specific embodiment of the gas purification treatment, and may be any gas purification treatment as long as other interfering gases in the vacuum arc melting furnace can be discharged. In this embodiment, the following processes may be optionally employed for gas purification: and vacuumizing the vacuum arc furnace to 5-8 Pa, filling argon until the pressure displayed by a pressure gauge is-0.09 MPa, vacuumizing again, and repeating for three times to finish furnace body purification treatment, so that the phenomena of material oxidation and the like in the smelting process are prevented, and the quality of the material is improved.
It should be noted that the present invention is not limited to the specific embodiment of the vacuum process and the specific degree of vacuum, as long as the degree of vacuum in the vacuum arc furnace can be controlled to 3 × 10 -3 Pa or less. In this embodiment, the following process may be optionally adopted for vacuum-pumping treatment: after the furnace body is purified, a molecular pump is started to carry out vacuum pumping operation, and the vacuum pumping is carried out until the vacuum degree is 3 multiplied by 10 -3 Pa meets the preparation requirement of the high-entropy alloy.
Step three, carrying out vacuum-pumping treatment and then carrying out smelting treatment to obtain the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy;
the invention is not limited to the specific mode of the melting treatment, and the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy of the invention can be obtained as long as the raw materials of each metal element can be completely melted to form a uniform liquid component and then be re-solidified into a solid state. In this embodiment, vacuum arc melting is preferably adopted, and a water-cooled copper mold is adopted for cooling, and in order to ensure more uniform melting of the material, the melting treatment is specifically performed by the following processes in this embodiment: firstly, starting arc with 50A of smelting current, then smelting with 300A of smelting current until the metal raw materials are completely melted, then adding 8A of induced current and magnetically stirring for 30s to finish one-time smelting treatment, repeating the smelting treatment for 5 times in the embodiment, and after 30min after the smelting is finished, discharging gas and opening a furnace door to obtain the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy in the embodiment.
Example 2
The embodiment provides an Al-Co-V-Fe-Ni dual-phase high-toughness high-entropy alloy, wherein dual phases in the dual-phase high-toughness high-entropy alloy comprise a BCC phase and a FCC phase, and the dual-phase high-toughness high-entropy alloy comprises the following elements in percentage by mol: 12% of Al, 16% of Co, 17% of V, 27% of Fe and 28% of Ni.
The preparation method of the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy of the embodiment is as follows:
step one, respectively weighing metal raw materials corresponding to each element component according to the proportioning relation for later use;
it should be noted that the present invention does not limit the specific composition of each metal material as long as the respective metal elements can be provided in the respective contents. In this example, metals Al, co, V, fe, and Ni having a purity of 99.99Wt% and a particle diameter of 4mm are preferably used as the metal raw materials.
Secondly, placing the weighed metal Al, co, V, fe and Ni into a vacuum arc melting furnace, then closing a furnace door, and sequentially performing gas purification treatment and vacuum-pumping treatment;
the present invention is not limited to a specific embodiment of the gas purification treatment, and other interfering gases in the vacuum arc melting furnace may be discharged. In this embodiment, the following processes may be optionally adopted for gas purification: and (3) vacuumizing the vacuum arc furnace to 5Pa, filling an argon pressure gauge to display-0.09 MPa, vacuumizing again, and repeating for three times to finish the furnace body purification treatment.
It should be noted that the present invention is not limited to the specific embodiment of the vacuum process and the specific degree of vacuum, as long as the degree of vacuum in the vacuum arc furnace can be controlled to 3 × 10 -3 Pa or less. In this embodiment, the following process may be optionally adopted for vacuum-pumping treatment: after the furnace body is purified, a molecular pump is started to carry out vacuum pumping operation, and the vacuum pumping is carried out until the pressure is 1 multiplied by 10 -3 And after Pa, the preparation requirement of the high-entropy alloy is met.
Step three, carrying out vacuum-pumping treatment and then carrying out smelting treatment to obtain the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy;
it should be noted that the invention does not limit the specific mode of the melting treatment, as long as the raw materials of each metal element can be completely melted to form a uniform liquid component, and then solidified into a solid state again, so as to obtain the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy. In this embodiment, the following process is preferably used for the melting treatment: firstly, carrying out arc striking by using 52A smelting current, then smelting by using 350A smelting current until metal raw materials are completely melted, then adding 9A induced current to carry out magnetic stirring for 35s, thus completing one-time smelting treatment, repeating the smelting treatment for 5 times in the embodiment, and after the smelting is completed, deflating and opening a furnace door after 32min, thus obtaining the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy in the embodiment.
Example 3
The embodiment provides an Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy, wherein two phases in the two-phase high-toughness high-entropy alloy are a BCC phase and an FCC phase, and the two-phase high-toughness high-entropy alloy comprises the following elements in percentage by mol: 10% Al, 13% Co, 17% V, 30% Fe, 30% Ni.
And the preparation method of the embodiment is different from that of the embodiment 1 in that:
in this example, the particle size of each metal raw material was 5mm.
In this example, the following process was used for gas purification: vacuumizing the vacuum arc furnace to 8Pa, introducing argon until the pressure indicated by the pressure gauge is-0.08 MPa, vacuumizing again, and repeating for three times to complete the furnace body purification treatment
In this example, the following process was used for vacuum treatment: after the furnace body is purified, a molecular pump is started to carry out vacuum pumping operation, and the vacuum pumping is carried out until the vacuum degree is 1 multiplied by 10 -3 Pa, meeting the preparation requirement of the high-entropy alloy.
In this example, the smelting process was carried out by the following process: firstly, carrying out arc striking by using a smelting current of 53A, then smelting by using a smelting current of 400A until the metal raw material is completely molten, then adding an induced current of 9A, magnetically stirring for 40s, thus completing one-time smelting treatment, repeating the smelting treatment for 6 times in the embodiment, and after the smelting is completed, discharging gas and opening a furnace door to obtain the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy in the embodiment.
Example 4
The embodiment provides an Al-Co-V-Fe-Ni dual-phase high-toughness high-entropy alloy, wherein dual phases in the dual-phase high-toughness high-entropy alloy comprise a BCC phase and a FCC phase, and the dual-phase high-toughness high-entropy alloy comprises the following elements in percentage by mol: 14% Al, 18% Co, 20% V, 24% Fe, 24% Ni.
And the preparation method of the embodiment is different from that of the embodiment 1 in that:
in this example, the particle size of each metal material was 5mm.
In this example, the following process was used for gas purification: and vacuumizing the vacuum arc furnace to 8Pa, filling argon until the pressure displayed by a pressure gauge is-0.08 MPa, vacuumizing again, and repeating for three times to finish the furnace body purification treatment.
In this example, the following process was used for vacuum treatment: after the furnace body is purified, a molecular pump is started to carry out vacuum pumping operation, and the vacuum pumping is carried out until the vacuum degree is 3 multiplied by 10 -3 Pa, meeting the preparation requirement of the high-entropy alloy.
In this example, the smelting process was carried out by the following process: firstly, striking an arc by using 55A of smelting current, then smelting by using 500A of smelting current until metal raw materials are completely molten, then adding 10A of induction current to magnetically stir for 50s, namely finishing one-time smelting treatment, repeating the smelting treatment for 5 times in the embodiment, and discharging gas and opening a furnace door after 40min after the smelting is finished, namely obtaining the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy in the embodiment.
Example 5
This example differs from example 1 only in that:
the biphase high-strength, high-toughness and high-entropy alloy of the embodiment comprises the following elements in percentage by mole: 12% Al, 17% Co, 15% V, 28% Fe, 28% Ni.
Test section
(I) tensile Property test
The invention respectively carries out stress-strain tests on the two-phase high-strength high-toughness high-entropy alloy prepared in the example 1 and the example 2 according to the test method in GB T228.1-2021 part 1 of the metal material tensile test, and the test results are respectively shown in the figure 1 and the figure 2.
It can be seen that: the ultimate tensile strength of the two-phase high-strength high-toughness high-entropy alloy in the embodiment 1 and the embodiment 2 is more than or equal to 1000MPa, and the elongation is more than or equal to 20%.
(II) topography testing
The optical microstructures of the two-phase high-strength high-toughness high-entropy alloy prepared in example 1 and example 2 are respectively tested, and the test results are respectively shown in fig. 3 and fig. 4. It can be seen that: the two-phase high-strength and high-toughness high-entropy alloy prepared in the embodiment 1 and the embodiment 2 is a two-phase structure distributed like a lamella, and the two-phase high-strength and high-toughness high-entropy alloy is successfully prepared by the method.
The scanning electron microstructures of the two-phase high-toughness high-entropy alloy prepared in example 1 and example 2 are respectively tested, and the test results are respectively shown in fig. 5 and fig. 6. It can be seen that: the microstructures of the two-phase high-strength high-toughness high-entropy alloy prepared in the embodiment 1 and the embodiment 2 are compact two-phase structures, and the results show that the two-phase high-strength high-toughness high-entropy alloy is successfully prepared by the method.
(III) XRD test
The invention takes Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy obtained in example 1 as an example, XRD phase detection analysis is carried out on the alloy, and the result is shown in figure 7.
As can be seen from fig. 7: the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy prepared by the method has a BCC phase and FCC phase two-phase structure.
(IV) TEM Electron diffraction Pattern calibration
Taking Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy obtained in example 1 as an example, TEM electron diffraction pattern calibration analysis is respectively carried out on an FCC phase (shown as a position at a left circle in FIG. 8) and a BCC phase (shown as a position at a right circle in FIG. 8) of the Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy obtained in example 1, and the results are shown in FIGS. 9 and 10.
FIG. 9 shows the results of a TEM electron diffraction pattern calibration analysis of FCC phase, and FIG. 10 shows the results of a TEM electron diffraction pattern calibration analysis of BCC phase. As can be seen from fig. 9 and 10: in the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy prepared by the invention, the FCC phase is Fe2AlV, and the BCC phase is AlNi3. The two phases which are uniformly distributed are typical eutectic structures, and the toughness of the material is obviously improved.
It is to be understood that the above-described embodiments are only a few embodiments of the present invention, and not all embodiments. 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.
Claims (9)
1. The Al-Co-V-Fe-Ni two-phase high-toughness high-entropy alloy is characterized by comprising the following elements in percentage by mole:
10％～14％Al、13％～18％Co、15％～20％V、24％～30％Fe、24％～30％Ni；
the total mole percentage of all elemental constituents is 100%.
2. The dual-phase high-toughness high-entropy alloy of claim 1, wherein the dual phases in the dual-phase high-toughness high-entropy alloy are a BCC phase and an FCC phase.
3. A preparation method of the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy as claimed in claim 1 or 2, which is characterized by comprising the following steps:
step 1, respectively weighing all metal raw materials, namely metal Al, co, V, fe and Ni according to the proportioning relation for later use;
and 2, placing the weighed metal raw materials in a vacuum arc melting furnace, sequentially performing gas purification treatment and vacuum-pumping treatment, and then performing melting treatment to obtain the Al-Co-V-Fe-Ni two-phase high-strength-toughness high-entropy alloy.
4. The method of claim 3, wherein each of said metal feedstock has a purity of 99.99wt%;
the particle size of each metal raw material is 3-5 mm.
5. The production method according to claim 3, wherein in step 2, the respective metal materials are added in the order of Al, V, co, fe, ni.
6. The method of claim 3, wherein the gas purification process is: vacuumizing the vacuum arc furnace to 5-8 Pa, filling argon to the pressure of-0.09-0.08 MPa, vacuumizing again, and repeating for at least three times to finish the furnace body purification treatment.
7. The method according to claim 3, wherein the degree of vacuum of the evacuation treatment is 3 x 10 or less -3 Pa。
8. The method of claim 3, wherein the smelting process is: firstly, starting arc with 50-55A of smelting current, then smelting with 300-500A of smelting current until the metal raw material is completely melted, and then adding 8-10A of induced current to magnetically stir for 30-50 s, thus finishing the primary smelting treatment.
9. The method of claim 3, wherein the smelting process is repeated at least 5 times.
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| CN113981292A (en) * | 2021-10-28 | 2022-01-28 | 西北工业大学 | High-entropy alloy with excellent strong plasticity and preparation method thereof |
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| KR20200041630A (en) * | 2018-10-12 | 2020-04-22 | 포항공과대학교 산학협력단 | High entropy alloy and manufacturing method of the same |
| CN113025865A (en) * | 2021-03-03 | 2021-06-25 | 北方工业大学 | Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy |
| CN113981292A (en) * | 2021-10-28 | 2022-01-28 | 西北工业大学 | High-entropy alloy with excellent strong plasticity and preparation method thereof |
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