CN112210705A - CuCrCoFeNiZrx high-entropy alloy and preparation method thereof - Google Patents
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Abstract
The invention discloses a CuCrCoFeNiZrx high-entropy alloy which comprises the following raw material components in atomic percentage: 5 to 35 percent of Zr, 5 to 25 percent of Fe, 5 to 20 percent of Ni, 5 to 25 percent of Cu, 5 to 35 percent of Cr and 5 to 25 percent of Co, wherein the sum of the atomic percentages of the components is 100 percent; the invention also discloses a preparation method of the high-entropy alloy, which is characterized in that the raw materials are placed in a vacuum arc melting furnace for multiple times of melting from top to bottom according to the melting point to obtain the CuCrCoFeNiZrx high-entropy alloy. The high-entropy alloy prepared by the invention has the advantages of low cost, simple and easily realized process, short smelting period, more uniform structure, fine dendritic crystal and simple single solid solution structure, can be applied to a transition layer of a heterogeneous alloy, and is a high-entropy alloy with great development potential.
Description
Technical Field
The invention belongs to the technical field of alloy preparation, relates to a CuCrCoFeNiZrx high-entropy alloy, and further relates to a preparation method of the CuCrCoFeNiZrx high-entropy alloy.
Background
With the urgent need of national defense science and technology and weaponry for high-strength and high-reliability function and structure integrated heterogeneous composite materials, the connection technology of heterogeneous alloys is more and more extensive, such as the connection of magnesium/aluminum alloy, ceramic/steel, titanium alloy/stainless steel, and the like. Because the physical and chemical properties of the heterogeneous alloy connection are not matched, and intermetallic compounds generated in the heterogeneous alloy joint are hard and brittle intermediate phases, the interface mechanical properties of two heterogeneous materials are directly influenced. Therefore, a good metallurgical bonding joint is formed, which is the premise of improving the use performance of the connection of heterogeneous materials and is also the main research field of interface engineering in the connection of heterogeneous materials. At present, a commonly used means for improving the bonding problem of the connection interface of the heterogeneous material is to add an active alloy interlayer which realizes good metallurgical bonding with the two materials at the bonding surface of the heterogeneous material.
The high-entropy alloy has excellent characteristics which are not possessed by a plurality of traditional alloys, such as high hardness, high-temperature oxidation resistance, wear resistance, temperature resistance and corrosion resistance. Meanwhile, the high entropy effect of the high entropy alloy can inhibit the phase of a brittle intermetallic compound, promote the mixing of elements to form a simple body-centered cubic or face-centered cubic structure or even an amorphous state, and can be used as a transition layer for diffusion metallurgical connection of heterogeneous materials. Therefore, a CuCrCoFeNiZrx high-entropy alloy transition layer is introduced into a heterogeneous alloy joint surface, the interface of a heterogeneous material can be alloyed through an alloy diffusion technology, and the generation of a brittle intermetallic compound phase of the interface is inhibited, so that the strength, hardness, high-temperature oxidation resistance, wear resistance, temperature resistance, corrosion resistance and other properties of the joint interface are greatly improved. However, at present, methods for using the high-entropy alloy as a transition layer for connecting heterogeneous materials are few, so that the research on the high-entropy alloy with good performance has important significance in providing experimental basis and technical support for introducing the high-entropy alloy into the connection of the heterogeneous materials in the future and accelerating the practical application of the high-entropy alloy.
Disclosure of Invention
The invention aims to provide a CuCrCoFeNiZrx high-entropy alloy which has the characteristics of more uniform structure and fine dendritic crystal, has a simple single solid solution structure, and can be better applied to a transition layer of a heterogeneous alloy
The invention also aims to provide a preparation method of the CuCrCoFeNiZrx high-entropy alloy.
The technical scheme adopted by the invention is as follows: the CuCrCoFeNiZrx high-entropy alloy comprises the following raw material components in atomic percentage:
5 to 35 percent of Zr, 5 to 25 percent of Fe, 5 to 20 percent of Ni, 5 to 25 percent of Cu, 5 to 35 percent of Cr and 5 to 25 percent of Co, wherein the sum of the atomic percentages of the components is 100 percent.
The invention is also characterized in that:
cr, Co and Fe are powder with the granularity of 50-400 meshes and the purity of 99.9 percent, Zr is powder with the granularity of 50-400 meshes and the purity of 99.99 percent, and Cu and Ni are cuboid bars with the purity of 99.9 percent.
The other technical scheme adopted by the invention is as follows:
a preparation method of a CuCrCoFeNiZrx high-entropy alloy is specifically implemented according to the following steps:
5-35% of Zr, 5-25% of Fe, 5-20% of Ni, 5-25% of Cu, 5-35% of Cr and 5-25% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%;
and 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, turning over the Cu, Ni and the alloy powder therein for re-melting after the alloy powder between the Cu and the Ni is fully mixed, repeatedly melting for 3-8 times, and taking out the mixture after 5-30min to obtain the CuCrCoFeNiZrx high-entropy alloy.
Another aspect of the invention is also characterized in that:
in the step 1, the Cu bar and the Ni bar are placed in a container filled with alcohol before being weighed, the container is placed in an ultrasonic cleaner for cleaning, and then the container is weighed by an electronic balance with the precision of 0.001g after being dried in vacuum.
The vacuum degree of the vacuum arc melting furnace in the step 2 is 1 multiplied by 10-3～5×10-3Pa。
The current for smelting in the step 2 is 100-300 amperes.
The alcohol concentration is more than 99.7%, and the cleaning time is 20-25 min.
The invention has the beneficial effects that: the method for preparing the alloy has the advantages of low cost, simple process, easy realization and short sintering period. The prepared alloy has high hardness, uniform structure and fine dendritic crystal, has simple single solid solution structure, can be applied to a transition layer of a heterogeneous alloy, and is a high-entropy alloy with great development potential.
Drawings
FIG. 1 is an SEM image of a CuCrCoFeNiZrx high entropy alloy prepared by the method of the present invention;
FIG. 2 is a microhardness curve of a CuCrCoFeNiZrx high entropy alloy prepared by the method of the present invention;
FIG. 3 is a spectrum analysis diagram of CuCrCoFeNiZrx high entropy alloy prepared by the method of the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a CuCrCoFeNiZrx high-entropy alloy which is composed of the following raw material components in atomic percentage:
5 to 35 percent of Zr, 5 to 25 percent of Fe, 5 to 20 percent of Ni, 5 to 25 percent of Cu, 5 to 35 percent of Cr and 5 to 25 percent of Co, wherein the sum of the atomic percentages of the components is 100 percent.
Preferably, Cr, Co and Fe are powder with the granularity of 50-400 meshes and the purity of 99.9 percent, Zr is powder with the granularity of 50-400 meshes and the purity of 99.99 percent, and Cu and Ni are cuboid bars with the purity of 99.9 percent.
The CuCrCoFeNiZrx high-entropy alloy has the following functions:
1: the addition of Zr element increases the hardness and strength of the high-entropy alloy system;
2: the addition of the Ni element increases the capability of the high-entropy alloy system to obtain an FCC phase;
3: the addition of the Cr element increases the melting point of the high-entropy alloy system.
The six elements are all positioned at the adjacent positions of the subgroup of the fourth period in the periodic table of the elements, the atomic radii are similar, the properties are also very similar, and simple solid solution structures can be formed among the six elements.
The invention relates to a preparation method of a CuCrCoFeNiZrx high-entropy alloy, which is implemented according to the following steps:
5-35% of Zr, 5-25% of Fe, 5-20% of Ni, 5-25% of Cu, 5-35% of Cr and 5-25% of Co, wherein the sum of the atomic percentages of the components is 100%, the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, wherein the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before being weighed, the container is placed in an ultrasonic cleaner for cleaning for 20-25min, and then the container is weighed by an electronic balance with the precision of 0.001g after being dried in vacuum;
step 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, and then putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10-3～5×10-3Pa, the current adopted by smelting is 100-300 amperes, the Cu, the Ni and the alloy powder in the Cu and the Ni are overturned and smelted again after the alloy powder in the middle of the Cu and the Ni is fully mixed, the smelting is repeated for 3-8 times, and the alloy powder is taken out after 5-30min after the smelting is finished, so that the CuCrCoFeNiZrx high-entropy alloy is obtained.
The method for preparing the CuCrCoFeNiZrx high-entropy alloy comprises the following steps: the step 1 is used for realizing the optimal proportioning scheme of the high-entropy alloy through the selection of different alloy elements.
The theory is adopted to calculate the entropy, enthalpy, electronegativity difference and atomic radius difference of the high-entropy alloy, and the principle is as follows: the entropy, enthalpy, electronegativity difference, atomic radius difference and the like of the high-entropy alloy are calculated through parameters, and influence on the formation rule of a solid solution phase, a topological close-packed phase and an amorphous phase in the high-entropy alloy and the crystal structure of the solid solution by valence electrons is achieved;
the entropy, the enthalpy, the electronegativity difference and the atomic radius difference of the high-entropy alloy are calculated by adopting a theory, and the method has the advantages that: ensuring that the selected elements have similar crystal structures, small comprehensive atom radius difference and close electronegativity.
The step 2 is used for optimizing the preparation process of the high-entropy alloy by changing various process parameters of vacuum arc melting.
Vacuum arc melting is adopted, and the principle is as follows: an electrothermal metallurgical method for smelting metal by generating an electric arc between an electrode and an electrode or between an electrode and a material to be smelted by using electric energy.
The method for changing various process parameters of vacuum arc melting has the advantages that: the method has the advantages of obtaining a large range of smelting temperature, increasing the smelting times and preventing the smelting samples from being oxidized, thereby realizing the optimization of the high-entropy alloy system smelting process.
FIG. 1 is a scanning electron micrograph of CuCrCoFeNiZr1.5 high entropy alloy prepared by the present invention, and Table 1 shows the energy spectrum analysis of the corresponding region, from Table 1, Cu exists more in the interdendritic region, and the content is 74.08%. The Zr content and the Ni content of the light-color structure part of the dendrite (C) are respectively 21.89 percent and 27.81 percent higher than those of the structure parts of other regions, and the Zr content and the Cr content of the dark-color structure part of the dendrite (B) are increased; as can be seen from FIG. 2, the prepared CuCrCoFeNiZr1.5 high entropy alloy has uniform structure; fig. 2 is a hardness curve of a CuCrCoFeNiZr-based high-entropy alloy, the comprehensive atomic radius difference of the CuCrCoFeNiZrx (x is 1, 1.5, 2) high-entropy alloy is much higher than that of the CuCrCoFeNi alloy, and the large atomic size difference increases lattice distortion in the alloy, so that the hardness of the alloy is improved; fig. 3 is an XRD spectrum of the CuCrCoFeNiZrx (x is 0, 1, 1.5) high-entropy alloy prepared by the present invention, which is a simple multi-phase FCC solid solution structure without complex phases, because of the high entropy mixing effect of the alloy, the high entropy mixing increases the compatibility of each principal element, can significantly reduce the free energy of the system, and inhibits the occurrence of brittle intermetallic compounds, thereby promoting the mixing of elements to form a simple solid solution structure.
TABLE 1 energy spectrum analysis of corresponding region of CuCrCoFeNiZr1.5 high entropy alloy scanning electron micrograph
Example 1
20% of Zr, 25% of Fe, 10% of Ni, 10% of Cu, 10% of Cr and 25% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before weighing, the container is placed in a KQ-50DE type numerical control ultrasonic cleaner for cleaning for 20min, and then the container is weighed by using an electronic balance with the precision of 0.001g after vacuum drying;
step 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, and then putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10- 3And Pa, filling high-purity argon into the sample chamber to normal pressure, adopting the current for smelting at 300 amperes, turning over the Cu and the Ni and the alloy powder therein after the alloy powder between the Cu and the Ni is fully mixed, smelting again for 5 times, repeatedly smelting for 2min each time, and taking out after 10min after smelting is finished to obtain the CuCrCoFeNiZrx high-entropy alloy.
Example 2
10% of Zr, 5% of Fe, 20% of Ni, 25% of Cu, 20% of Cr and 20% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before weighing, the container is placed in a KQ-50DE type numerical control ultrasonic cleaner for cleaning for 22min, and then the container is weighed by using an electronic balance with the precision of 0.001g after vacuum drying;
step 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, and then putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10- 3And Pa, filling high-purity argon into the sample chamber to normal pressure, adopting a smelting current of 250 amperes, turning over the Cu and the Ni and the alloy powder therein after the alloy powder between the Cu and the Ni is fully mixed, smelting for 3 times repeatedly, wherein each time is 1.5min, and taking out after 20min of smelting is finished to obtain the CuCrCoFeNiZrx high-entropy alloy.
Example 3
25% of Zr, 8% of Fe, 15% of Ni, 12% of Cu, 25% of Cr and 15% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before weighing, the container is placed in a KQ-50DE type numerical control ultrasonic cleaner for cleaning for 23min, and then the container is weighed by using an electronic balance with the precision of 0.001g after vacuum drying;
step 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, and then putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10- 3Pa, filling high-purity argon into the sample chamber to normal pressure, adopting a smelting current of 250 amperes, turning over the Cu and the Ni and the alloy powder therein after the alloy powder in the middle of the Cu and the Ni is fully mixed, smelting for 8 times repeatedly, 1min each time, taking out after 25min after smelting is finished, and taking outAnd obtaining the CuCrCoFeNiZrx high-entropy alloy.
Example 4
the alloy is characterized by comprising 14% of Zr, 16% of Fe, 20% of Ni, 10% of Cu, 35% of Cr and 5% of Co, wherein the sum of the atomic percentages of the components is 100%, the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before weighing, the container is placed in a KQ-50DE type numerical control ultrasonic cleaner to be cleaned for 25min, and then the container is weighed by using an electronic balance with the precision of 0.001g after vacuum drying;
step 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, and then putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10- 3And Pa, filling high-purity argon into the sample chamber to normal pressure, adopting the current for smelting at 300 amperes, turning over the Cu and the Ni and the alloy powder therein after the alloy powder between the Cu and the Ni is fully mixed, smelting for 3 times repeatedly, wherein the time is 2 minutes each time, and taking out after 25 minutes after the smelting is finished to obtain the CuCrCoFeNiZrx high-entropy alloy.
Comparative example 1
20% of Zr, 25% of Fe, 10% of Ni, 10% of Cu, 10% of Cr and 25% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%, the Cu and the Ni bars are placed in an alcohol container with the concentration of more than 99.7% before weighing, the container is placed in a KQ-50DE type numerical control ultrasonic cleaner for cleaning for 20min, and then the container is weighed by using an electronic balance with the precision of 0.001g after vacuum drying;
step 2, weighing the raw materials Ni, Zr, Cr and F in the step 1e. Co and Cu are arranged in the order from top to bottom and then placed in a sample groove of a water-cooling copper mold of a vacuum arc melting furnace for melting, wherein the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10- 3And Pa, filling high-purity argon into the sample chamber to normal pressure, adopting a current for smelting of 350 amperes, turning over the Cu and the Ni and the alloy powder therein after the alloy powder between the Cu and the Ni is fully mixed, smelting again for 10 times repeatedly, wherein each time is 1.5min, taking out after 35min after the smelting is finished, and obtaining an alloy ingot without Zr and Cr elements, wherein most of Zr and Cr elements which are easy to burn are burnt under high-current and multiple times of smelting.
Claims (7)
1. The CuCrCoFeNiZrx high-entropy alloy is characterized by comprising the following raw material components in atomic percentage:
5 to 35 percent of Zr, 5 to 25 percent of Fe, 5 to 20 percent of Ni, 5 to 25 percent of Cu, 5 to 35 percent of Cr and 5 to 25 percent of Co, wherein the sum of the atomic percentages of the components is 100 percent.
2. The CuCrCoFeNiZrx high entropy alloy as claimed in claim 1, wherein said Cr, Co and Fe are all powders with 50-400 mesh size and 99.9% purity, said Zr is a powder with 50-400 mesh size and 99.99% purity, and said Cu and Ni are rectangular parallelepiped bars with 99.9% purity.
3. A preparation method of a CuCrCoFeNiZrx high-entropy alloy is characterized by comprising the following steps:
step 1, weighing the following raw materials in atomic percentage:
5-35% of Zr, 5-25% of Fe, 5-20% of Ni, 5-25% of Cu, 5-35% of Cr and 5-25% of Co, wherein the sum of the atomic percentages of the components is 100%, wherein the Cr, the Co and the Fe are powder with the granularity of 50-400 meshes and the purity of 99.9%, the Zr is powder with the granularity of 50-400 meshes and the purity of 99.99%, and the Cu and the Ni are cuboid bars with the purity of 99.9%;
and 2, arranging the raw materials Ni, Zr, Cr, Fe, Co and Cu weighed in the step 1 in sequence from top to bottom, putting the raw materials into a sample groove of a water-cooled copper mold of a vacuum arc melting furnace for melting, turning over the Cu, Ni and the alloy powder therein for re-melting after the alloy powder between the Cu and the Ni is fully mixed, repeatedly melting for 3-8 times, and taking out the mixture after 5-30min to obtain the CuCrCoFeNiZrx high-entropy alloy.
4. The method for preparing the CuCrCoFeNiZrx high-entropy alloy is characterized in that in the step 1, the Cu and Ni bars are placed in a container filled with alcohol before being weighed, the container is placed in an ultrasonic cleaner for cleaning, and then the container is weighed by an electronic balance with the precision of 0.001g after being dried in vacuum.
5. The method for preparing CuCrCoFeNiZrx high entropy alloy according to claim 3, wherein the vacuum degree of the vacuum arc melting furnace in the step 2 is 1 x 10-3～5×10-3Pa。
6. The method for preparing CuCrCoFeNiZrx high entropy alloy according to claim 3, wherein the current for melting in step 2 is 100-300A.
7. The method for preparing the CuCrCoFeNiZrx high-entropy alloy as claimed in claim 4, wherein the alcohol concentration is greater than 99.7%, and the cleaning time is 20-25 min.
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| CN116121619A (en) * | 2023-02-10 | 2023-05-16 | 西北工业大学 | Liquid quenched complex phase alloy based on electrostatic suspension and preparation method thereof |
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| CN113122764A (en) * | 2021-03-19 | 2021-07-16 | 西安理工大学 | Preparation method of CuCrFeCoNixTi high-entropy alloy thin strip |
| CN116121619A (en) * | 2023-02-10 | 2023-05-16 | 西北工业大学 | Liquid quenched complex phase alloy based on electrostatic suspension and preparation method thereof |
| CN116121619B (en) * | 2023-02-10 | 2023-08-29 | 西北工业大学 | Liquid quenched complex phase alloy based on electrostatic suspension and preparation method thereof |
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