CN111961893A - High-strength high-plasticity high-entropy alloy and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-entropy alloy with high strength and high plasticity and a preparation method thereof, belonging to the technical field of metal materials and manufacturing. The high-entropy alloy preparation raw materials comprise Co, Cr, Fe and Ni metal particles and Al-10Er (the mass fraction of Er is 10%) intermediate alloy particles, and the preparation method specifically comprises the following steps: the metal particles are weighed according to a set proportion, melted in a high-vacuum arc melting furnace and then solidified in a copper mold to prepare the high-entropy alloy, and an alloy block needs to be repeatedly melted in order to ensure the uniformity of alloy components in the melting process. Homogenizing the initially prepared as-cast high-entropy alloy in a high-temperature heat treatment furnace, then performing water quenching, rolling the high-entropy alloy ingot at the temperature of 500-800 ℃, and cooling the rolled sample with air to obtain the high-strength high-plasticity high-entropy alloy. The high-entropy alloy prepared by the invention has excellent mechanical property and simple preparation process.
Description
Technical Field
The invention relates to a high-entropy alloy with high strength and high plasticity and a preparation method thereof, belonging to the technical field of metal materials and preparation thereof.
Background
Conventional alloys are generally based on one or two elements, with small amounts of other elements being added to meet certain performance requirements. With the further development of the alloy design concept, in the beginning of the 21 st century, Taiwan scholars break through the traditional alloy design concept and firstly propose the design concept of 'high-entropy alloy', namely, the number of main elements in the alloy is not less than 5, and the molar ratio of each main element is between 5% and 35%. The high-entropy alloy has a high-entropy effect, can form a simple solid solution structure, does not generate complex intermetallic compounds, has the phase number far lower than the phase number predicted by an equilibrium phase law, shows the characteristics of high strength, high hardness, high temperature softening resistance, high temperature oxidation resistance, corrosion resistance and the like, and has important significance for the promotion of metallurgy and material industry.
Early research on high-entropy alloys focused on the design of alloy components, i.e., the influence of the types and contents of constituent elements on the microstructure and properties of high-entropy alloys. Researchers can optimize the performance of the alloy through reasonable element addition or proportion, and the performance of the alloy can reach or even exceed that of the traditional alloy materials, such as stainless steel, nickel-based high-temperature alloy and the like. The types of alloys explored in recent years are increasing, the relationship between the structure and the performance of the high-entropy alloy is gradually clarified, but the pure blending of macro-components cannot support the further pursuit of high performance. It is known that the high-entropy alloy with single-phase FCC structure has better plasticity, but the yield strength of the high-entropy alloy generally does not exceed 300MPa, and the yield strength of the BCC structure with single phase can reach 1GPa, but the plasticity of the high-entropy alloy is very poor. The practical application of the high-entropy alloy is greatly limited, so that the development of the high-entropy alloy with good comprehensive mechanical properties is of great significance.
In recent years, researchers have focused on the search for trace element additions and their transformation mechanisms. Research on Al at high temperature0.5The deformation mechanism of FeCoNiCrMn high-entropy alloy is found to be Al at 900 DEG C0.5The FeCoNiCrMn high-entropy alloy is simultaneously subjected to work hardening and dynamic recovery in the thermal deformation process, and the strength and the plasticity are simultaneously improved. Zhang et al prepared CoCrFeNiY by a vacuum arc melting method, explored the influence of rare earth Y element on the mechanical properties of CoCrFeNi high-entropy alloy, found that when the addition amount is 0.3, the hardness is optimal, increased from 146HV to 400HV, the yield strength is increased from 202MPa to 1440 MPa, and the plasticity is reduced to 2.3%, and obtained the main alloyThis is due to the combined action of solid solution strengthening and second phase strengthening. The CoCrFeNi high-entropy alloy has a single FCC phase, has very good corrosion resistance, high temperature resistance and plasticity, but has lower strength, and the improvement of the performance of the CoCrFeNi high-entropy alloy through different modes is a hot problem of current research.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the prior art, the invention provides a high-strength high-plasticity high-entropy alloy and a preparation method thereof.
The technical scheme is as follows: the high-strength high-plasticity high-entropy alloy disclosed by the invention contains metal elements such as Co, Cr, Fe, Ni, Al and Er, wherein the Al and Er elements are added in an intermediate alloy form, and the mass percent of Er in the intermediate alloy is 10%, namely Al-10 Er.
Preferably, the molar ratio of Co, Cr, Fe, Ni and Al in the intermediate alloy is 1:1:1:1: 0.05.
The preparation method of the high-strength high-plasticity high-entropy alloy comprises the following steps:
(1) preparing metal block particles of Fe, Cr, Co, Ni and Al-10 Er;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a high-purity Ar gas environment of a high-vacuum arc melting furnace, and cooling and solidifying the metal block particles in a copper mold to form an ingot;
(3) carrying out high-temperature homogenization heat treatment on the alloy ingot smelted in the step (2), and then taking out and water-quenching to normal temperature;
(4) and (4) rolling the alloy ingot subjected to the homogenization heat treatment in the step (3), and then air-cooling to room temperature to obtain the high-strength high-plasticity high-entropy alloy material.
In the step (1), Al- (10) wt.% Er master alloy metal block particles are adopted for Al-Er combined microalloying, and the master alloy is added to improve the distribution uniformity of elements in the alloy and reduce the burning loss during smelting. And trace Al and Er elements are added to form an intermetallic compound rich in Al and Er in the matrix alloy so as to improve the mechanical property of the alloy.
Preferably, in the step (1), the molar ratio of the Co, Cr, Fe, Ni and Al in the intermediate alloy is 1:1:1:1: 0.05.
In the step (3), the high-temperature homogenization heat treatment temperature is 950-1050 ℃, the heat preservation is carried out for 8-15h, and the gas environment is air.
In the step (4), the rolling directions are consistent, the rolling temperature is 500-.
According to the invention, by adding trace Al and Er elements, the solid solution strengthening, the fine grain strengthening and the dispersion strengthening of the high-entropy alloy are promoted, and meanwhile, the CoCrFeNi high-entropy alloy is rolled, so that the strength and the plasticity of the material can be obviously improved through the work hardening and the dynamic recovery in the rolling process, and a large number of crack defects in cold rolling are reduced.
The tensile strength of the alloy prepared by the method is 690-760MPa, and the elongation is 19-23%.
Has the advantages that: (1) the invention rolls the high-entropy alloy at medium temperature, the rolling temperature is 500-800 ℃, the energy consumption can be effectively reduced, and the preparation cost is reduced; (2) the addition of the trace elements does not damage the FCC structure, and the grains are refined, so that Al-Er-rich intermetallic compounds are easily formed, and the effects of fine grain strengthening and dispersion strengthening are promoted; (3) the electric arc melting is the most widely researched alloy melting process route at present, the method is simple and easy to operate, and the prepared high-entropy alloy has more excellent plasticity and higher tensile strength.
Drawings
FIG. 1 is a metallographic microstructure of example 1 (homogeneous CoCrFeNi high-entropy alloy);
FIG. 2 is a metallographic microstructure of example 2 (homogenized state of the high-entropy alloy of the present invention);
FIG. 3 is a metallographic microstructure of the alloy of example 3 (in the rolled state at 650 ℃ C. of the high-entropy alloy of the invention);
FIG. 4 is a metallographic microstructure of the alloy of example 4 (in a rolled state at 800 ℃ C. of the high-entropy alloy of the invention);
FIG. 5 is a comparison of tensile stress-strain curves for examples 1-4.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Respectively removing oxide skins on the surfaces of the Co, Cr, Fe and Ni metals by using fine sand paper, and then performing ultrasonic cleaning by using absolute ethyl alcohol to obtain clean metal blocks; weighing 70g of mixed raw materials according to a molar ratio of 1:1:1: 1;
(2) repeatedly smelting the weighed raw materials in a high-purity Ar gas environment of a high-vacuum arc melting furnace;
(3) and (3) keeping the alloy ingot smelted in the step (2) at 1000 ℃ for 12h, carrying out homogenization heat treatment, taking out, and carrying out water quenching to normal temperature to obtain the homogenized high-entropy alloy.
The experimental results are as follows:
the high-entropy alloy prepared by the method is subjected to rough grinding step by using abrasive paper of different models, the abrasive paper is subjected to fine grinding to obtain a #1600, then the high-entropy alloy is subjected to mechanical polishing until the surface of the high-entropy alloy has no obvious scratch, a metallographic corrosive agent is used for corroding the alloy, a microscopic structure of the alloy is observed by using an MV5000 metallographic microscope, and the result is shown in figure 1, and the homogenized alloy structure is coarse isometric crystal.
The tensile property test of the high-entropy alloy block material is carried out by using a CMT5105 electronic universal testing machine, and the test result is shown in figure 5. The tensile strength of the homogenized sample without the Al-10Er intermediate alloy is 396MPa, and the elongation is 52.6%.
Example 2
(1) Respectively removing oxide skins on the surfaces of Co, Cr, Fe, Ni and Al-10Er by using fine sand paper, and then carrying out ultrasonic cleaning by using absolute ethyl alcohol to obtain clean metal blocks; weighing 70g of mixed raw materials according to a molar ratio of 1:1:1:1: 0.05;
(2) repeatedly smelting the weighed raw materials in a high-purity Ar gas environment of a high-vacuum arc melting furnace;
(3) and (3) keeping the alloy ingot smelted in the step (2) at 1000 ℃ for 12h, carrying out homogenization heat treatment, taking out, and carrying out water quenching to normal temperature to obtain the homogenized high-entropy alloy.
The experimental results are as follows:
the high-entropy alloy prepared by the method is subjected to rough grinding step by using abrasive paper of different types, the abrasive paper is subjected to fine grinding to be #1600, then mechanical polishing is carried out until the surface of the alloy has no obvious scratch, a metallographic corrosive agent is used for corroding the alloy, a microscopic structure of the alloy is observed by using an MV5000 metallographic microscope, and the result is shown in figure 2, and the grain size of the alloy structure is obviously reduced compared with that of the alloy prepared by the comparative example.
The tensile property test of the high-entropy alloy block material is carried out by using a CMT5105 electronic universal testing machine, and the test result is shown in figure 5. The tensile strength of the homogenized sample was 439MPa, and the elongation was 51.4%.
Example 3
A preparation method of a high-strength high-plasticity high-entropy alloy comprises the following specific steps:
(1) respectively removing oxide skins on the surfaces of Co, Cr, Fe, Ni and Al-10Er by using fine sand paper, and then carrying out ultrasonic cleaning by using absolute ethyl alcohol to obtain clean metal blocks; weighing 70g of mixed raw materials according to a molar ratio of 1:1:1:1: 0.05;
(2) repeatedly smelting the weighed raw materials in a high-purity Ar gas environment of a high-vacuum arc melting furnace;
(3) keeping the alloy ingot smelted in the step (2) at 1000 ℃ for 12h, carrying out homogenization heat treatment, taking out, and carrying out water quenching to normal temperature to obtain a homogenized high-entropy alloy;
(4) and (4) cutting the alloy ingot subjected to the homogenization heat treatment in the step (3) into a sample with the thickness of 16 multiplied by 4mm, rolling at 650 ℃ for 4 times, wherein the reduction amount is 0.5mm each time, the total deformation amount is 50%, and air cooling to room temperature to obtain the high-strength high-plasticity high-entropy alloy material.
The experimental results are as follows:
the high-entropy alloy prepared by the method is subjected to rough grinding step by using abrasive paper of different models, the abrasive paper is finely ground to #1600, then the high-entropy alloy is subjected to mechanical polishing until the surface of the high-entropy alloy has no obvious scratch, the alloy is corroded by using a metallographic corrosive agent, the microstructure of the alloy is observed by using an MV5000 metallographic microscope, the result is shown in figure 3, the crystal grains of a sample rolled at 650 ℃ are obviously crushed, a fibrous structure is formed inside the sample, no crack defect is seen, and the alloy is mainly subjected to deformation strengthening.
The tensile property test of the high-entropy alloy block material prepared under different process conditions is carried out by utilizing a CMT5105 electronic universal tester, and the test result is shown in figure 5. The tensile strength of a sample of the high-entropy alloy is 759MPa and the elongation is 19.8% after the high-entropy alloy is rolled at 650 ℃.
Example 4
A preparation method of a high-strength high-plasticity high-entropy alloy comprises the following specific steps:
(1) respectively removing oxide skins on the surfaces of Co, Cr, Fe, Ni and Al-10Er by using fine sand paper, and then carrying out ultrasonic cleaning by using absolute ethyl alcohol to obtain clean metal blocks; weighing 70g of mixed raw materials according to a molar ratio of 1:1:1:1: 0.05;
(2) repeatedly smelting the weighed raw materials in a high-purity Ar gas environment of a high-vacuum arc melting furnace;
(3) keeping the alloy ingot smelted in the step (2) at 1000 ℃ for 12h, carrying out homogenization heat treatment, taking out, and carrying out water quenching to normal temperature to obtain a homogenized high-entropy alloy;
(4) and (4) cutting the alloy ingot subjected to the homogenization heat treatment in the step (3) into a sample with the thickness of 16 multiplied by 4mm, rolling at 800 ℃ for 4 times, wherein the reduction amount of each time is 0.5mm, the total deformation amount is 50%, and air cooling to room temperature to obtain the high-strength high-plasticity high-entropy alloy material.
The experimental results are as follows:
the high-entropy alloy prepared by the method is subjected to rough grinding step by using abrasive paper of different types, the abrasive paper is subjected to fine grinding to be #1600, then mechanical polishing is carried out until the surface of the alloy has no obvious scratch, a metallographic corrosive agent is used for corroding the alloy, a microscopic structure of the alloy is observed by using an MV5000 metallographic microscope, the result is shown in figure 4, fine isometric crystals are generated at the crystal boundary of a sample rolled at 800 ℃, and the alloy is subjected to dynamic recovery in the rolling process.
The tensile property test of the high-entropy alloy block material prepared under different process conditions is carried out by utilizing a CMT5105 electronic universal tester, and the test result is shown in figure 5. The tensile strength of a sample of the high-entropy alloy is 692MPa and the elongation is 22.9% after the high-entropy alloy is rolled at 800 ℃.
The results of the examples are summarized:
according to the invention, the Al-Er combined microalloying high-entropy alloy is used for promoting the effects of fine grain strengthening and dispersion strengthening, and simultaneously controlling the rolling temperature, so that the hot working deformation and the recovery recrystallization are carried out simultaneously, the grain size is regulated and controlled, the segregation and the defects are eliminated, and the comprehensive mechanical property of the material is improved. In the embodiment 3, the tensile strength of the sample rolled at 800 ℃ reaches 692MPa, the elongation reaches 22.9 percent, and the sample has excellent comprehensive mechanical properties.
Claims (8)
1. The high-entropy alloy with high strength and high plasticity is characterized by containing metal elements of Co, Cr, Fe, Ni, Al and Er, wherein the Al and Er elements are added in the form of intermediate alloy Al-10 Er.
2. A high strength and high plasticity high entropy alloy as claimed in claim 1, wherein the molar ratio of Co, Cr, Fe, Ni, Al in the master alloy is 1:1:1:1: 0.05.
3. A high-strength high-plasticity high-entropy alloy as claimed in claim 2, wherein the tensile strength is 690-760MPa, and the elongation is 19-23%.
4. The method for preparing the high-strength high-plasticity high-entropy alloy as claimed in claim 1, which is characterized by comprising the following steps:
(1) preparing metal block particles of Fe, Cr, Co, Ni and Al-10 Er;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a high-purity Ar gas environment of a high-vacuum arc melting furnace, and cooling and solidifying the metal block particles in a copper mold to form an ingot;
(3) carrying out high-temperature homogenization heat treatment on the alloy ingot smelted in the step (2), and then taking out and water-quenching to normal temperature;
(4) and (4) rolling the alloy ingot subjected to the homogenization heat treatment in the step (3), and then air-cooling to room temperature to obtain the high-strength high-plasticity high-entropy alloy material.
5. A method for preparing a high-strength high-plasticity high-entropy alloy according to claim 4, wherein in the step (1), the molar ratio of the Co, the Cr, the Fe, the Ni and the Al in the intermediate alloy is 1:1:1:1: 0.05.
6. A preparation method of a high-strength high-plasticity high-entropy alloy according to claim 4, wherein in the step (3), the high-temperature homogenization heat treatment temperature is 950-1050 ℃, the temperature is kept for 8-15h, and the gas environment is air.
7. The method for preparing the high-strength high-plasticity high-entropy alloy as claimed in claim 4, wherein in the step (4), the rolling directions are consistent, the rolling temperature is 500-800 ℃, and the deformation amount is 50%.
8. The method for preparing a high-entropy alloy with high strength and high plasticity as claimed in claim 4, wherein the prepared alloy has a tensile strength of 690-760MPa and an elongation of 19-23%.
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| CN112899531A (en) * | 2021-01-19 | 2021-06-04 | 江苏大学 | High-entropy alloy particle reinforced aluminum-based composite material and magnetic field auxiliary preparation method |
| CN113430406A (en) * | 2021-05-21 | 2021-09-24 | 中国科学院金属研究所 | Precipitation strengthening CoCrNiAlNb multi-principal-element alloy and preparation method thereof |
| CN114324146A (en) * | 2021-12-31 | 2022-04-12 | 华侨大学 | Method for predicting dynamic scratch elastic recovery |
| CN114395717A (en) * | 2021-12-14 | 2022-04-26 | 北京科技大学 | Co-Ni-Cr-Fe-W high-density high-plasticity high-entropy alloy and preparation method thereof |
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| CN114395717A (en) * | 2021-12-14 | 2022-04-26 | 北京科技大学 | Co-Ni-Cr-Fe-W high-density high-plasticity high-entropy alloy and preparation method thereof |
| CN114395717B (en) * | 2021-12-14 | 2023-02-17 | 北京科技大学 | Co-Ni-Cr-Fe-W high-density high-plasticity high-entropy alloy and preparation method thereof |
| CN114324146A (en) * | 2021-12-31 | 2022-04-12 | 华侨大学 | Method for predicting dynamic scratch elastic recovery |
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