CN115491532B - High corrosion-resistant high-entropy alloy and preparation method thereof - Google Patents
High corrosion-resistant high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high corrosion-resistant high-entropy alloy and a preparation method thereof, belonging to the technical field of corrosion-resistant alloy materials and preparation thereof. A high corrosion resistant high entropy alloy, characterized by: comprises Nb, ti, cr, A, zr metal elements, and in atom percent, nb: 18-22%, ti: 18-22%, cr: 18-22%, A: 18-22%, zr: 18-22% of unavoidable impurities; the A is V or Mo. The high corrosion resistance high entropy alloy and the preparation method thereof are adopted, and the prepared alloy has high strength, excellent corrosion resistance, simple preparation process, convenient operation and wide popularization and application.
Description
Technical Field
The invention relates to a high corrosion-resistant high-entropy alloy and a preparation method thereof, belonging to the technical field of corrosion-resistant alloy materials and preparation thereof.
Background
Because the titanium alloy has better corrosion resistance in seawater, the titanium alloy is an ideal equipment manufacturing material in a marine environment, and the use of the titanium alloy can greatly improve the fighting capacity of naval vessels and equipment, reduce the maintenance cost and prolong the service life. Titanium alloys have been widely used in naval vessels, deep submarines, and other equipment by the united states, russia, and chinese naval. Pressure-resistant housings, seawater pipes, other valves, etc. used in civil marine facilities are often made of titanium alloys.
The high-entropy alloy has a plurality of advantages as a novel hot alloy in recent years, such as high thermodynamic mixing entropy, slow dynamic diffusion, large structural lattice distortion, and 'cocktail' effect in performance. Since taiwan She Junwei teaches in 1996 a new concept of high-entropy alloy, high-entropy alloy has received extensive attention from researchers at home and abroad. Researchers have conducted different studies on the structure and properties of high-entropy alloys, starting from different alloy composition systems. The application of high-entropy alloys to marine corrosion-resistant materials is one of the hot spot directions of international research. However, many of the existing high-entropy alloys are difficult to meet the requirements of marine environments.
CN114951634a discloses a wear-resistant and corrosion-resistant coating of high-entropy alloy and a preparation method thereof, and the method comprises the following specific steps: the method comprises the steps of preparing coating powder by adopting 17-22% of cobalt, 17-22% of chromium, 17-22% of nickel, 17-22% of copper and the balance of aluminum in atomic percentage, wherein the crystal of the coating powder is of a body-centered cubic lattice structure; the coating powder is coated on a substrate, and a gradient solid solution is formed at the interface of the substrate and the coating. The method has the following defects: although the corrosion resistance of the material is improved, the bending strength, the bending elastic modulus and the hardness metallographic effect are poor.
Disclosure of Invention
The first technical problem solved by the invention is to provide a high corrosion-resistant high-entropy alloy.
A high corrosion resistant high entropy alloy, characterized by: comprises Nb, ti, cr, A, zr metal elements, and in atom percent, nb: 18-22%, ti: 18-22%, cr: 18-22%, A: 18-22%, zr: 18-22% of unavoidable impurities; the A is V or Mo. Wherein, the high-entropy alloy comprises HCP hexagonal close-packed solid solution, BCC body-centered cubic solid solution and LAVES structure precipitated phase.
Wherein the high-entropy alloy comprises HCP hexagonal close-packed solid solution, BCC body-centered cubic solid solution and LAVES structure precipitated phase; wherein, the HCP hexagonal close-packed solid solution content in the high-entropy alloy is 45-49%, the BCC body-centered cubic solid solution content is 45-49% and the precipitated phase content of the LAVES structure is 2-8%.
The second technical problem to be solved by the invention is to provide a preparation method of the high corrosion-resistant high-entropy alloy, which comprises the following steps:
a. respectively taking five metal raw materials of Nb, ti, cr, V, zr and Nb, ti, cr, mo, zr with the purity of 99.95 percent and the metal particle size of 1-5 mm, uniformly mixing according to the atomic percentage of the high corrosion resistance high entropy alloy, and pressing into a blank;
b. vacuum non-consumable arc melting is performed.
Wherein the pressing pressure in the step a is 25-35 MPa.
Preferably, in the step a, the pressing pressure is 30MPa.
Wherein the smelting operation comprises the following steps:
carrying out argon cleaning on a water-cooled copper crucible smelting furnace, vacuumizing until the pressure in the smelting furnace is lower than 0.0009Pa, then filling argon so that the pressure in the furnace reaches 5-10 Pa, vacuumizing until the pressure in the smelting furnace is lower than 0.0009Pa, and starting smelting;
the voltage is 380V during smelting, the current is 500-600A, and the smelting time is five minutes; after smelting, closing the current, cooling to 1000 ℃, reversing the ingot casting direction, and loading the current 500A again for smelting for 5 minutes; repeating the step for at least 8 times, wherein the smelting process is accompanied by magnetic stirring, and the stirring current is 5A;
cooling to below 400 ℃ along with the furnace, wherein the cooling rate is 50-100 ℃/min, and then air cooling to room temperature.
The invention has the beneficial effects that:
1. according to the high corrosion-resistant high-entropy alloy and the preparation method thereof, the prepared high corrosion-resistant high-entropy alloy has high hardness and bending strength, strong interatomic binding force, high melting point and co-coordination of solid solution strengthening and precipitation strengthening, and is beneficial to improving the material strength.
2. According to the high corrosion-resistant high-entropy alloy and the preparation method thereof provided by the invention, the prepared high corrosion-resistant high-entropy alloy has strong corrosion resistance, no macroscopic change is caused when the alloy is corroded in aqua regia for 4 hours, and the electrochemical test result is 2 orders of magnitude smaller than the corrosion current density of the conventional TA2 titanium alloy, so that the alloy can be used as a corrosion-resistant material of naval equipment.
3. According to the high corrosion-resistant high-entropy alloy and the preparation method thereof, the vacuum non-consumable arc melting is adopted, the market supply of required equipment is sufficient, new equipment is not required to be developed, the energy consumption is low, the melting time can be completed within half an hour, the cost is effectively reduced, the preparation process is convenient to operate, the preparation of large-size cast ingots can be realized, and the method is suitable for industrial production and has good economic benefit.
Drawings
FIG. 1 is an ingot diagram of a high corrosion resistant NbTiCrVZr (left) and NbTiCrMoZr (right) high entropy alloy of the present invention.
FIG. 2 is an X-ray diffraction pattern of the high corrosion resistant NbTiCrVZr (left) and NbTiCrMoZr (right) high entropy alloys of the present invention.
FIG. 3 is a microscopic gold phase diagram of the high corrosion resistant NbTiCrVZr (left) and NbTiCrMoZr (right) high entropy alloys of the present invention.
FIG. 4 is an electrochemical polarization curve of a highly corrosion-resistant NbTiCrVZr, nbTiCrMoZr high-entropy alloy and a TA1 titanium alloy of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The examples were conducted under conventional conditions, except that the specific conditions were not specified.
Example 1 preparation of the NbTiCrVZr high entropy alloy according to the invention
Five metal elements Nb, ti, cr, V, zr with the purity of 99.95 percent and the average size of metal particles of 4mm are respectively taken, and according to the atomic percent, nb:20%, ti:20%, cr:20%, V:20%, zr:20%. The high-entropy alloy ingredients are mixed and pressed, the pressure is 30MPa, and then vacuum non-consumable arc melting is carried out. Carrying out primary argon cleaning on a water-cooled copper crucible smelting furnace, vacuumizing to the pressure of 0.0008Pa in the smelting furnace, then filling argon to enable the pressure in the furnace to reach 6Pa, vacuumizing to the pressure of 0.0008Pa in the smelting furnace, and starting smelting; the voltage is 380V and the current is 550A during smelting, and the smelting time is five minutes; after smelting, closing the current, cooling to 1000 ℃, reversing the ingot casting direction, and loading the current 550A again for smelting for 5 minutes; repeating the step for 8 times, wherein the smelting process is accompanied by magnetic stirring, and the stirring current is 5A; cooling to 350 ℃ along with the furnace, wherein the cooling rate is 90-100 ℃/min, and then air cooling to room temperature. Finally, the obtained cast ingot is cut and characterized.
Example 2 preparation of the NbTiCrMoZr high entropy alloy according to the invention
Five metal elements Nb, ti, cr, mo, zr with the purity of 99.95 percent and the average size of metal particles of 4mm are respectively taken, and according to the atomic percent, nb:20%, ti:20%, cr:20%, mo:20%, zr:20%. The high-entropy alloy ingredients are mixed and pressed, the pressure is 30MPa, and then vacuum non-consumable arc melting is carried out. Carrying out primary argon cleaning on a water-cooled copper crucible smelting furnace, vacuumizing to the pressure of 0.0008Pa in the smelting furnace, then filling argon to enable the pressure in the furnace to reach 6Pa, vacuumizing to the pressure of 0.0008Pa in the smelting furnace, and starting smelting; the voltage is 380V and the current is 550A during smelting, and the smelting time is five minutes; after smelting, closing the current, cooling to 1000 ℃, reversing the ingot casting direction, and loading the current 550A again for smelting for 5 minutes; repeating the step for 8 times, wherein the smelting process is accompanied by magnetic stirring, and the stirring current is 5A; cooling to 350 ℃ along with the furnace, wherein the cooling rate is 90-100 ℃/min, and then air cooling to room temperature. Finally, the obtained cast ingot is cut and characterized.
The ingot diagrams of the high corrosion resistant NbTiCrVZr (left) and NbTiCrMoZr (right) high entropy alloys of the present invention prepared in examples 1 and 2 are shown in FIG. 1. The X-ray diffraction patterns of the high-corrosion-resistance NbTiCrVZr (left) and NbTiCrMoZr (right) high-entropy alloys of the invention prepared in examples 1 and 2 are shown in FIG. 2. Microscopic gold phase diagrams of the high-corrosion-resistance NbTiCrVZr (left) and NbTiCrMoZr (right) high-entropy alloys of the invention prepared in examples 1 and 2 are shown in FIG. 3. The electrochemical polarization curves of the high corrosion resistance NbTiCrVZr, nbTiCrMoZr high entropy alloy and the TA1 titanium alloy of the invention prepared in examples 1 and 2 are shown in FIG. 4.
The NbTiCrVZr high-entropy alloy prepared in example 1 comprises BCC body-centered cubic solid solution, HCP hexagonal close-packed solid solution and LAVES phase. After arc melting, the high-corrosion-resistance NbTiCrVZr high-entropy alloy of the invention forms HCP hexagonal close-packed solid solution with the main element Ti, also forms BCC1 body-centered cubic solid solution with the main element Nb and Ti and BCC2 body-centered cubic solid solution with the main element V, and forms Cr 2 Nb is the LAVES phase of the prototype. Wherein the HCP is hexagonal close-packed (BCC is body-centered-cubic (body-centered-cubic), and the LAVES is hexagonal close-packed (hexagonal close-packed). As can be seen from the metallographic microscopic diagram, the morphology of the NbTiCrVZr high entropy combination is mainly three colors: white, gray and black, whichIn which the white areas are mainly HCP phases, the gray areas are mainly BCC phases, and the black interstitial areas are mainly LAVES phases. Nb, ti, cr, V, zr, the five elements form a substitutional solid solution, the solid solution strengthening effect is enhanced, and the interstitial phase pinning grain boundary improves the strength and the hardness of the material. The NbTiCrVZr high-entropy alloy integrally presents equiaxial flaky grain and precipitated phase morphology.
The NbTiCrMoZr high entropy alloy prepared in example 2 forms BCC body centered cubic solid solutions with Mo and Nb elements as the main components, respectively, corresponding to the two cleavage peaks at the 40 ° position in the XRD spectrum. At the same time, HCP solid solution mainly containing Ti is formed, and Mo is also formed 2 Zr is the LAVES phase of the prototype. As can be seen from the microscopic schematic diagram of the NbTiCrMoZr high-entropy alloy phase, the structure of the alloy is in a dendritic wafer shape, and the color of the alloy can be divided into white and gray areas. Wherein, the gray area is mainly BCC phase, the white area is HCP phase, and the LAVES phase is dispersed in the white area. Nb, ti, cr, mo, zr, the HCP and BCC solid solution is formed by the replacement of five elements, so that the solid solution strengthening effect is achieved. The NbTiCrMoZr high-entropy alloy is in a dendritic wafer-shaped structure as a whole.
The NbTiCrVZr, nbTiCrMoZr high-entropy alloy prepared in examples 1 and 2 was tested for flexural strength, flexural modulus, and hardness (measured using a vickers hardness tester). The results are shown in Table 1, the bending strength, the bending modulus and the hardness of the NbTiCrMoZr and NbTiCrVZr high-entropy alloy are as follows, and the bending strength of the NbTiCrMoZr and NbTiCrMoZr high-entropy alloy respectively reaches 165.59 MPa and 157.09MPa, and the hardness of the NbTiCrMoZr and NbTiCrMoZr high-entropy alloy respectively 683HV and 582HV.
TABLE 1
| Sample preparation | Measurement of temperature (. Degree. C.) | Bending resistanceIntensity (MPa) | Flexural modulus of elasticity (MPa) | Hardness (HV) |
| NbTiCrVZr | 25 | 165.59 | 22288.65 | 683 |
| CrNbTMoZr | 25 | 157.09 | 11144.32 | 582 |
The electrochemical corrosion characteristics of the NbTiCrVZr, nbTiCrMoZr high-entropy alloy were tested using 3.0% NaCl solution as the etchant and titanium alloy TA1 as the comparative group, and the polarization curves are shown in fig. 4. Referring to Table II, the electrochemical properties of the CrNbTiMoZr, nbTiCrVZr high-entropy alloy and the titanium TA1 alloy are indicated, and compared with the titanium alloy TA1, the corrosion current densities of the NbTiCrVZr and the NbTiCrMoZr high-entropy alloys reach 4.15E-08, 8.77E-08 and 1.22E-06A/cm respectively 2 The corrosion current of the NbTiCrVZr and NbTiCrMoZr high-entropy alloy is two orders of magnitude smaller than that of the titanium alloy TA2, and therefore the NbTiCrVZr and NbTiCrMoZr high-entropy alloy exhibits excellent corrosion resistance.
TABLE 2
| Material | Corrosion voltage (V) | Corrosion current (A/cm) 2 ) |
| High entropy alloy NbTiCrVZr | -0.15522 | 4.15E-08 |
| High-entropy alloy NbTiCrMoZr | -0.05974 | 8.77E-08 |
| Titanium alloy TA1 | -0.47875 | 1.22E-06 |
The present embodiment is merely illustrative of the invention and not intended to be limiting, and those skilled in the art will make modifications or improvements on the basis of the present invention after reading the description of the invention, but are protected by the patent laws within the scope of the claims of the present invention.
Claims (3)
1. A high corrosion resistant high entropy alloy, characterized by: comprises Nb, ti, cr, A, zr metal elements, and in atom percent, nb: 18-22%, ti: 18-22%, cr: 18-22%, V: 18-22%, zr: 18-22% of unavoidable impurities; the high-entropy alloy comprises HCP hexagonal close-packed solid solution, BCC body-centered cubic solid solution and LAVES structure precipitated phase; wherein, the HCP hexagonal close-packed solid solution content in the high entropy alloy is 45-49%, the BCC body-centered cubic solid solution content is 45-49% and the precipitated phase content of the LAVES structure is 2-8%;
the preparation method of the high corrosion resistance high entropy alloy comprises the following steps:
a. respectively taking Nb, ti, cr, V, zr five metal raw materials with the purity of 99.95 percent and the metal particle size of 1-5 mm, uniformly mixing according to the atomic percentage of the high corrosion-resistant high-entropy alloy, and pressing into a blank;
b. carrying out vacuum non-consumable arc melting; the smelting operation comprises the following steps:
carrying out argon cleaning on a water-cooled copper crucible smelting furnace, vacuumizing until the pressure in the smelting furnace is lower than 0.0009Pa, then filling argon so that the pressure in the furnace reaches 5-10 Pa, vacuumizing until the pressure in the smelting furnace is lower than 0.0009Pa, and starting smelting;
the voltage is 380V during smelting, the current is 500-600A, and the smelting time is five minutes; after smelting, closing the current, cooling to 1000 ℃, reversing the ingot casting direction, and loading the current 500A again for smelting for 5 minutes; repeating the step for at least 8 times, wherein the smelting process is accompanied by magnetic stirring, and the stirring current is 5A;
cooling to below 400 ℃ along with the furnace, wherein the cooling rate is 50-100 ℃/min, and then air cooling to room temperature.
2. The method for preparing the high corrosion-resistant high-entropy alloy according to claim 1, wherein: the pressing pressure in the step a is 25-35 MPa.
3. The method for preparing the high corrosion-resistant high-entropy alloy according to claim 2, wherein: the pressing pressure in step a was 30MPa.
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| JP2018145456A (en) * | 2017-03-02 | 2018-09-20 | 株式会社日立製作所 | Alloy member, manufacturing method of the alloy member and manufactured article using the alloy member |
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| CN114032544A (en) * | 2021-11-15 | 2022-02-11 | 昆明理工大学 | Refractory high-entropy alloy coating and preparation method thereof |
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| US20190024198A1 (en) * | 2017-07-19 | 2019-01-24 | The Industry & Academic Cooperation In Chungnam National University (Iac) | Precipitation Hardening High Entropy Alloy and Method of Manufacturing the Same |
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| JP2018145456A (en) * | 2017-03-02 | 2018-09-20 | 株式会社日立製作所 | Alloy member, manufacturing method of the alloy member and manufactured article using the alloy member |
| CN107488804A (en) * | 2017-08-04 | 2017-12-19 | 北京航空航天大学 | A kind of superhigh intensity, hardness and corrosion-resistant CrMnFeVTi high-entropy alloys and preparation method thereof |
| CN109161776A (en) * | 2018-10-10 | 2019-01-08 | 湘潭大学 | A kind of porous high-entropy alloy of pre-alloyed CrMoNbTiZr and preparation method thereof |
| EP3670684A1 (en) * | 2018-12-18 | 2020-06-24 | Casa Maristas Azterlan | High wear resistant high entropy alloy and preparation thereof |
| CN114645177A (en) * | 2020-12-21 | 2022-06-21 | 武汉苏泊尔炊具有限公司 | Corrosion-resistant alloy, preparation method thereof and cooking utensil |
| CN114032544A (en) * | 2021-11-15 | 2022-02-11 | 昆明理工大学 | Refractory high-entropy alloy coating and preparation method thereof |
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