CN110592457A - Rare earth element high-entropy alloy material and preparation method thereof - Google Patents
Rare earth element high-entropy alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a rare earth element high-entropy alloy material and a preparation method thereof, belonging to the field of materials. The alloy material is a close-packed hexagonal high-entropy alloy consisting of 14 rare earth elements, the composition of the alloy material is ScYLaCePrNdSmGdTbDyHoErTmLu, and each element is smelted according to an equal atomic ratio. The invention adopts 14 rare earth elements of scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium and lutetium to prepare the high-entropy alloy, is characterized by taking a higher component number and a material crystal as a single-phase close-packed hexagonal structure, has the mechanical property and the lattice constant meeting the high-entropy alloy mixing law, and has solid solution strengthening to a certain degree, and the whole experimental process is simple to operate and easy to implement.
Description
Technical Field
The invention relates to a rare earth element high-entropy alloy material and a preparation method thereof, belonging to the field of materials.
Background
The high-entropy alloy is proposed and researched by the previous 90 th century by the samsung maiden et al, and the main idea is to design the alloy by multiple elements and break through a shackle with a single element as a main component in the traditional alloy. The high-entropy alloy is a solid solution consisting of five or more elements, each element accounts for 5-35% of the total atomic number, and the high-entropy alloy has no main component because the content of one element is more than 50%. The types of the alloys are divided according to the mixed entropy, and the mixed entropy of the high-entropy alloys（RAs gas mole constant).
Previous studies have shown that: the performance of high entropy alloys can use the mixing law to explain the phenomenon of measured value deviation caused by complex polymerization systems in the alloy. As explained generally, since the components exhibit their respective properties after being mixed, the average value of the property contribution of each component to the population is the property exhibited by the alloy, and the mixing law plays an important role whether it is a pure metal element or an alloy obtained by mixing. Many experiments have shown that the results obtained using the mixing law have a small difference between the measured and calculated values. The calculation formula is as follows:
in the formula (I), the compound is shown in the specification,c i express componentiThe percentage of the atomic content of (A) is,p i express componentiA certain property of (2).
The content of the current study shows: the high-entropy alloy material has excellent characteristics superior to the traditional alloy, such as good mechanical property, wear resistance, corrosion resistance, thermal stability and irradiation resistance, and has important theoretical research value and application prospect. However, the research on the single-phase hexagonal close-packed rare earth high-entropy alloy materials and how to use the mixing law to predict the performance data of the high-entropy alloy is still in the initial stage. The relationship between the organization structure and the performance of the rare earth high-entropy alloy with the hexagonal close-packed structure and the prediction of the performance and the organization between the component and the alloy system according to the mixing law have far-reaching significance for the research work of materials.
Disclosure of Invention
The invention aims to provide a rare earth element high-entropy alloy material and a preparation method thereof, and fills the blank of high-element unidirectional close-packed hexagonal high-entropy alloy. The material is a high-entropy alloy material with a new component.
According to the theoretical basis, the phase structure, the atomic radius, the electronegativity, the chemical property and the like of lanthanide rare earth elements are very similar, so that the rare earth elements can be selected to form an approximate ideal solid solution, and the solid solubility of the alloy is very high. The invention adds new elements into the original alloy of 5 elements to prepare the 14-element rare earth high-entropy alloy. And observing whether the prepared alloy is in a single-phase close-packed hexagonal structure or not, and establishing a brand new alloy model.
The invention provides a rare earth element high-entropy alloy material which is a 14-component rare earth element close-packed hexagonal structure high-entropy alloy, the composition of the rare earth element high-entropy alloy is ScYLaCePrNdSmdTdBDyHoErTmLu, each element is smelted according to equal atomic ratio, and the composition elements of the rare earth element high-entropy alloy material are scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium and lutetium.
In the materials, the purity of each element of the selected raw materials is not lower than 99.9%.
The formula for calculating the mixing law between each alloy component and the whole body is as follows:
in the formula (I), the compound is shown in the specification,c i express componentiThe percentage of the atomic content of (A) is,p i express componentiA certain property of (2).
The high-entropy alloy material is prepared by smelting in a high-vacuum non-consumable arc smelting furnace, and the preparation method comprises the following steps:
(1) weighing 14 rare earth element raw materials according to equal atomic ratio;
(2) sequentially putting the raw materials of each element into a copper mold crucible of an arc melting furnace according to the sequence of low melting point to high melting point, and then vacuumizing until the vacuum degree is lower than 1.5 multiplied by 10-3Filling argon with the purity of 99.9 percent into the reactor under the MPa till the pressure in the non-consumable arc melting furnace is 0.5 MPa;
(3) arc striking smelting, wherein the current is 50-150A during smelting, the smelting is repeated for 4-5 times, and the furnace body of the smelting furnace is cleaned immediately after each smelting; after the smelting is finished, suction casting is not needed, and the rare earth element high-entropy alloy material is obtained after the copper mold crucible in the furnace is cooled to room temperature.
The high-entropy alloy material obtained by the invention has the alloy yield strength of 204MPa, the fracture strength of 850MPa, the plastic strain of 20.1 percent and the micro Vickers hardness of 111 HV. The unexpected exception of the lattice constant of the alloy occurs, according to the mixing law, the lattice constant ratio c/a value of the alloy is 2.1109, but the actual ratio is 1.5799, because the lattice constant of praseodymium element and samarium element in the alloy is large, the calculated value is large, and the actual experimental value meets the lattice constant of a close-packed hexagonal structure and meets the mixing effect of the high-entropy alloy.
The invention has the beneficial effects that:
the invention adopts 14 rare earth elements of scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium and lutetium to prepare the high-entropy alloy, is characterized by taking a higher component number and a material crystal as a single-phase close-packed hexagonal structure, has the mechanical property and the lattice constant meeting the high-entropy alloy mixing law, and has solid solution strengthening to a certain degree, and the whole experimental process is simple to operate and easy to implement.
Drawings
FIG. 1 is an X-ray diffraction spectrum of the 14-component rare earth element high-entropy alloy prepared in example 1. All diffraction peaks in the figure correspond to a single-phase close-packed hexagonal structure;
FIG. 2 is a metallographic structure (500 times) of the 14-component rare earth element high-entropy alloy prepared in example 1;
FIG. 3 shows the metallographic structure (1000 times) of the high-entropy alloy of 14 elements of rare earth elements prepared in example 1
FIG. 4 is a microstructure diagram of the 14-element rare earth high-entropy alloy prepared in example 1 under a scanning electron microscope;
FIG. 5 shows the composition distribution under a scanning electron microscope of the 14-component rare earth high-entropy alloy prepared in example 1;
FIG. 6 is the true stress-strain curve under room temperature compression condition of the 14-component rare earth high-entropy alloy prepared in example 1.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
Example 1:
the method for manufacturing the ScYLaCePrNdSmGdTbDyHoErTmLu high-entropy alloy material by adopting the arc melting process comprises the following steps:
(1) weighing 14 rare earth element raw materials according to equal atomic ratio.
(2) Sequentially putting raw materials of various elements (Ce, La, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Y, Er, Sc, Tm and Lu) into a crucible of a copper mold of an arc melting furnace according to the sequence of low melting point to high melting point, and then vacuumizing until the vacuum degree is lower than 1.5 multiplied by 10-3And (MPa), filling argon with the purity of 99.9 percent until the pressure in the non-consumable arc melting furnace is 0.5 MPa.
(3) And (3) arc striking smelting, wherein the current is 150A during smelting, the smelting is repeated for 5 times, and the smelting furnace body is cleaned immediately after each smelting. After the smelting is finished, suction casting is not needed, and the rare earth element high-entropy alloy material is obtained after the copper mold crucible in the furnace is cooled to room temperature.
In the embodiment, acrylic cold setting powder is adopted to set a sample with the size of phi 3mm multiplied by 3mm in the sample into an observation sample with the size of phi 20mm multiplied by 10mm, and European standard 240 is selected in sequence#，400#，600#，800#，1000#，1200#，1500#And 2000#And grinding the surface of the sample by using metallographic abrasive paper, and then mechanically polishing the sample until the surface is free from scratches.
An X-ray diffraction analyzer is adopted to measure the diffraction pattern of the high-entropy alloy, the scanning angle is 20-80 degrees, and the scanning speed is 3 degrees/min. The results of the analysis are shown in FIG. 1. The XRD analysis result shows that the phase composition of the alloy is single-phase close-packed hexagonal solid solution.
The high-entropy alloy material prepared by the embodiment is prepared by adding 100ml of HNO containing nitric acid32.5ml, HCl1.5ml, HF1ml hydrofluoric acid and 95ml deionized water are corroded by the corrosive agent and observed under a Leica electron metallographic microscope, the structure observation under a 500-time objective lens is shown in figure 2, and the structure observation under a 1000-time objective lens is shown in figure 3. It can be seen that the alloy is a single-phase dendritic structure, the grains are approximately uniformly distributed in a visual field, the sizes of the grains are relatively uniform, the grain boundaries are quite clear and can be obviously observed, and substances are precipitated and mixed in the grains and on the grain boundaries, and the substances may be oxides of elements.
The high-entropy alloy material prepared by the embodiment is prepared by adding 100ml of HNO containing nitric acid32.5ml, HCl1.5ml, HF1ml hydrofluoric acid and 95ml deionized water are corroded by the corrosive agent and then are observed under a TESCAN-LYRA3 scanning electron microscope, and the observation is shown in figure 4. In FIG. 4, the high-entropy alloy material is composed of dendrites with uniform sizes, and strip-shaped texture precipitation can be seen on grain boundaries. In fig. 5, the distribution of 14 components in the measured area is uniform, oxygen element segregates on the grain boundary, which may be caused by that the atoms at the grain boundary deviate from the equilibrium position, and the higher kinetic energy causes the energy of the grain boundary to be higher than that in the interior of the grain, where the atoms are in an unstable state and are easy to combine with the oxygen element to form oxide.
In this example, a round bar-shaped high-entropy alloy material with a size of phi 3mm × 6mm was prepared, and the compression property was measured at room temperature by using an Instron-5969 multifunctional material tester. The compression ratio of the 14-component rare earth element high-entropy alloy material prepared by the experiment reaches 20.1%. And testing the Vickers hardness of the material by using an MH-600 microhardness tester. During testing, the load of the tester is set to be 200g, the load retention time is set to be 15s, and the Vickers hardness value of the high-entropy alloy material prepared by the embodiment is 111 HV.
Fig. 6 is a real stress-strain curve of the 14-component rare earth high-entropy alloy material prepared by the embodiment under the room-temperature compression condition, and the alloy prepared by the experiment has good room-temperature compression performance, the yield strength reaches 204MPa, and the fracture strength reaches 850 MPa.
The rare earth element high-entropy alloy obtained by the experimental mode has higher compressive strength and compression molding property and excellent comprehensive mechanical property.
Claims (4)
1. A rare earth element high-entropy alloy material is characterized in that: the high-entropy alloy is a close-packed hexagonal structure high-entropy alloy consisting of 14 rare earth elements, and comprises ScYLACEPNdSmGdTbDyHoErTmLu, wherein each element is smelted according to an equal atomic ratio, and the elements comprise scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, gadolinium, terbium, dysprosium, holmium, erbium, thulium and lutetium.
2. A rare earth element high entropy alloy material according to claim 1, characterized in that: the purity of each element is not less than 99.9%.
3. A preparation method of the rare earth element high-entropy alloy material of any one of claims 1 ~ 2, wherein the rare earth element high-entropy alloy material is prepared by smelting in a high-vacuum non-consumable arc smelting furnace, and the method comprises the following steps:
(1) weighing 14 rare earth element raw materials according to equal atomic ratio;
(2) sequentially putting the raw materials of each element into a copper mold crucible of an arc melting furnace according to the sequence of low melting point to high melting point, and then vacuumizing until the vacuum degree is lower than 1.5 multiplied by 10-3Filling argon with the purity of 99.9 percent into the non-consumable arc melting furnace until the pressure in the non-consumable arc melting furnace is 0.5 MPa;
(3) arc striking smelting, wherein the current is 50-150A during smelting, the smelting is repeated for 4-5 times, and the furnace body of the smelting furnace is cleaned immediately after each smelting; after the smelting is finished, suction casting is not needed, and the rare earth element high-entropy alloy material is obtained after the copper mold crucible in the furnace is cooled to room temperature.
4. The method for preparing a rare earth element high-entropy alloy material according to claim 3, characterized in that: the properties of the obtained high-entropy alloy material are as follows: the yield strength of the alloy reaches 204MPa, the breaking strength is 850MPa, the plastic strain reaches 20.1 percent, and the micro Vickers hardness reaches 111 HV.
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Cited By (2)
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| CN115436134A (en) * | 2022-09-23 | 2022-12-06 | 国标（北京）检验认证有限公司 | Metallographic structure characterization method of high-purity yttrium target material |
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Application publication date: 20191220 |