CN115838889A - Quaternary high-entropy alloy powder and preparation method thereof - Google Patents
Quaternary high-entropy alloy powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses quaternary high-entropy alloy powder and a preparation method thereof, and belongs to the technical field of high-entropy alloy powder metallurgy. The invention provides a high-specific-strength transition metal quaternary high-entropy alloy containing FeCrAlTi, which utilizes the characteristic of lower quality of transition metal in the fourth period and Ti element to regulate and control the hardness and specific strength of the high-entropy alloy, and prepares and obtains quaternary high-entropy alloy powder with low density, high hardness and high specific strength. And Ti and Al elements are dissolved in BCC crystal lattices by utilizing the high kinetic energy impact of high-energy ball milling and the lattice inclusion of Fe-Cr alloy to form uniformly dispersed high-entropy alloy powder.
Description
Technical Field
The invention relates to quaternary high-entropy alloy powder and a preparation method thereof, in particular to high-specific-strength transition metal quaternary high-entropy alloy powder with high structural stability and a preparation method thereof, and belongs to the technical field of high-entropy alloy powder metallurgy.
Background
High Entropy Alloys (HEAs) are a new class of alloy materials, and due to their composition and component concentration controllability, are potential metal materials that can replace traditional alloy materials. At present, the reported high-entropy alloy is mainly divided into a body-centered cubic (bcc) structure and a face-centered cubic (fcc) structure, and the structure configuration of the high-entropy alloy can be regulated and controlled by regulating and controlling the concentration of a certain element in the high-entropy alloy. With the widening of the application field of the high-entropy alloy material, the high-entropy alloy material has more applications in the fields of aerospace, aviation and the like. However, the aerospace field has higher requirements on the density of materials, and the purposes of improving the overall energy consumption ratio and controlling the operation cost are achieved by reducing the density of the materials. However, the existing high-entropy alloy system is difficult to balance the relation between strength and quality, and the specific strength of the high-entropy alloy system is difficult to exceed that of part of the traditional high-specific-strength alloy. Therefore, the high-entropy alloy with high structural stability and high specific strength and the preparation method thereof are provided, and are necessary to meet the severe requirements of the existing aerospace field on materials.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides high-structure-stability high-specific-strength transition metal quaternary high-entropy alloy powder and a preparation method thereof.
The technical scheme of the invention is as follows:
one of the purposes of the invention is to provide high-specific strength transition metal quaternary high-entropy alloy powder with high structural stability, which comprises the following components in atomic percentage: 20-30.77% of Fe, 20-30.77% of Cr, 20-30.77% of Al and 7.69-40% of Ti7, wherein the atomic mole percentage ratio of Fe, cr and Al is 1:1:1, and the sum of the atomic percentages of the components is 100at%.
Further defined, the atomic mole percent ratio of Fe, cr, al, and Ti is 1:1:1:2.
further defined, the atomic mole percent ratio of Fe, cr, al, and Ti is 1:1:1:1.5.
further defined, the atomic mole percent ratio of Fe, cr, al, and Ti is 1:1:1:0.5.
further limited, the quaternary high-entropy alloy powder is of a single-phase BCC structure.
The invention also aims to provide a preparation method of the high-structure-stability high-specific-strength transition metal quaternary high-entropy alloy powder.
Further limit, the grain diameter of the iron powder, the chromium powder, the aluminum powder and the titanium powder is 15-150 mu m.
Further limited, the purity of the iron powder, the chromium powder, the aluminum powder and the titanium powder is more than or equal to 99.99wt.%.
Further limiting, the ratio of the mass of the zirconia balls to the total mass of the raw materials is (5-40): 1.
further limit, the diameter of the zirconia ball is 2 mm-20 mm.
Further limiting, the high-energy ball milling rotating speed is 300 rpm-800 rpm.
Further limiting, the high-energy ball milling treatment mode is an intermittent type, the operation is stopped for 0-30 min every 5-60 min, and the total treatment time is not less than 40h.
Further, the high-energy ball milling treatment can be carried out by using steel balls instead of zirconia balls.
The invention provides a high-specific-strength transition metal quaternary high-entropy alloy containing FeCrAlTi, which utilizes the characteristic of lower quality of transition metal in the fourth period and Ti element to regulate and control the hardness and specific strength of the high-entropy alloy. And Ti and Al elements are dissolved in BCC crystal lattices by utilizing the high kinetic energy impact of high-energy ball milling and the lattice inclusion of Fe-Cr alloy to form uniformly dispersed high-entropy alloy powder. Compared with the prior art, the method has the following advantages:
(1) The transition metal quaternary high-entropy alloy with high specific strength is prepared by utilizing the low density characteristics of the transition metals Fe, cr, ti and Al and the high hardness properties of Cr and Ti. In addition, ti also has excellent environmental corrosion resistance, and the corrosion resistance of the transition metal quaternary high-entropy alloy is effectively improved.
(2) The high-entropy alloy provided by the invention realizes the balance of mass and hardness, and has the characteristics of low density, high hardness and corrosion resistance.
Drawings
FIG. 1 is an XRD pattern of FeCrAlTi quaternary high-entropy alloy powder prepared by different examples;
FIG. 2 is an SEM image of a FeCrAlTi quaternary high entropy alloy powder prepared in example 1;
FIG. 3 is an EDS diagram of FeCrAlTi quaternary high entropy alloy powder prepared in example 1;
FIG. 4 is a theoretical model of FeCrAlTi quaternary high-entropy alloy powder prepared by the present invention, wherein (a) Ti-0.5 and (b) Ti-2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
(1) The preparation method comprises the following steps of (1) carrying out FeCrAlTi quaternary high-entropy alloy powder proportioning according to a molar ratio: 20% of Fe, 20% of Cr, 20% of Al and 40% of Ti, and weighing the metal powder by adopting an electronic balance.
The sources of the respective metal element powders are listed in the following table
| Name (R) | Molecular formula | Purity of | Particle size/. Mu.m | Manufacturer of the product |
| Iron powder | Fe | 99.99％ | 20 | Shanghai climbing nano powder |
| Chromium powder | Cr | 99.99％ | 20 | Shanghai climbing nano powder |
| Aluminum powder | Al | 99.99％ | 20 | Shanghai climbing nano powder |
| Titanium powder | Ti | 99.99％ | 20 | Shanghai climbingNano powder of field |
(2) And (3) mixing the total mass of the weighed metal powder and the mass of the zirconia balls according to the ratio of 1:15 are put into a zirconia ball-milling tank after being proportioned according to the mass ratio. Wherein the zirconia balls have a size of 2 μm.
(3) And (3) performing ball milling by using a planetary ball mill, wherein the ball milling rotation speed is 400rpm, the ball milling mode is intermittent, the operation is stopped for 20min every 25min, and the total processing time is 40h, so that FeCrAlTi high-entropy alloy powder, namely Ti-2 for short, is obtained.
Characterization and testing:
(1) XRD tests and results are shown in a Ti-2 curve in figure 1, and prove that the obtained powder is a high-entropy alloy, and the high-entropy alloy powder Ti-2 is a single BCC phase.
(2) The SEM test results show in fig. 2, and it can be seen from fig. 2 that the sizes of alloy particles in the visual field are different, because the high degree of disorder of high entropy causes a slight difference in the element contents at different positions, which causes the hardness to change, and thus the morphology and particle size are different under the same process. However, the comparison shows that the phenomenon does not influence the practical use. And the EDS characterization results are shown in fig. 3, fig. 3 also further demonstrates that there are subtle differences in the distribution of elements at different locations, but that the elements are uniformly distributed as a whole. It is shown that a stable quaternary high-entropy alloy powder has been formed by high-energy ball milling.
Example 2:
(1) The four-element high-entropy alloy powder of FeCrAlTi is prepared according to the molar ratio: 30.77% of Fe, 30.77% of Cr, 30.77% of Al30.77% and 7.69% of Ti, and weighing the metal powder by using an electronic balance.
The sources of the respective metal element powders are listed in the following table
| Name(s) | Molecular formula | Purity of | Particle size/. Mu.m | Manufacturer of the product |
| Iron powder | Fe | 99.99％ | 25 | Shanghai climbing nano powder |
| Chromium powder | Cr | 99.99％ | 25 | Shanghai climbing nano powder |
| Aluminum powder | Al | 99.99％ | 25 | Shanghai climbing nano powder |
| Titanium powder | Ti | 99.99％ | 25 | Shanghai climbing nano powder |
(2) And (3) mixing the total mass of the weighed metal powder and the mass of the zirconia balls according to the ratio of 1:10 are put into a zirconia ball milling tank after being mixed according to the mass ratio. Wherein the zirconia balls have a size of 13 μm.
(3) And (3) performing ball milling by using a planetary ball mill, wherein the ball milling rotation speed is 450rpm, the ball milling mode is intermittent, the operation is stopped for 10min every 20min, and the total processing time is 50h, so that FeCrAlTi high-entropy alloy powder, namely Ti-1.5 for short, is obtained.
Characterization and testing:
(1) XRD test and the result are shown in the curve Ti-1.5 in figure 1, which proves that the obtained powder is high entropy alloy, and the high entropy alloy powder Ti-1.5 is single BCC phase.
Example 3:
(1) The four-element high-entropy alloy powder of FeCrAlTi is prepared according to the molar ratio: 26.67% of Fe, 26.67% of Cr, 26.67% of Al26.67% and 19.99% of Ti, and weighing the metal powder by using an electronic balance.
The sources of the respective metal element powders are listed in the following table
| Name (R) | Molecular formula | Purity of | Particle size/. Mu.m | Manufacturer of the product |
| Iron powder | Fe | 99.99％ | 45 | Shanghai climbing nano powder |
| Chromium powder | Cr | 99.99％ | 45 | Shanghai climbing nano powder |
| Aluminum powder | Al | 99.99％ | 45 | Shanghai climbing nano powder |
| Titanium powder | Ti | 99.99％ | 45 | Shanghai climbing nano powder |
(2) And (3) mixing the total mass of the weighed metal powder and the mass of the zirconia balls according to the ratio of 1:20 are put into a ball milling tank after being proportioned according to the mass ratio. Wherein the size of the stainless steel ball is 6 μm.
(3) And (3) performing ball milling by using a planetary ball mill, wherein the ball milling rotation speed is 500rpm, the ball milling mode is intermittent, the operation is stopped for 0min every 15min, and the total processing time is 20h, so that FeCrAlTi high-entropy alloy powder, namely Ti-1 for short, is obtained.
Characterization and testing:
(1) XRD test and the result are shown in a Ti-1 curve in figure 1, and the obtained powder is proved to be a high-entropy alloy, and the high-entropy alloy powder Ti-1 is a single BCC phase.
Example of effects:
comparing different curves in fig. 1, it can be seen that the process conditions provided by the present invention can successfully prepare high entropy alloy powder mainly having BCC structure, and the alloying degree can be changed by adjusting the ball milling time, for example, some small peaks disappear, indicating that the alloying degree is increased. And under the same ball milling process, the half-peak width of the sample of example 1 is the largest and the peak intensity is also the lowest. Due to the lattice distortion effect of the high entropy alloy, the refraction angle of the X-ray changes, thus showing changes in intensity and peak width. This also indicates that the degree of alloying is optimal at this concentration.
The density of the quaternary high-entropy alloy powder obtained by different examples is tested according to the requirements of GB/T5161-201, the powder density test results are shown in the following table 1, and the density of the coating is reduced along with the increase of the Ti content. This is because Ti itself is a low-density alloy, and an increase in the content thereof is effective in reducing the density of the high-entropy alloy powder.
The hardness of the quaternary high-entropy alloy powder obtained in different examples is tested according to the requirements of SIS 110178-1964, and the results are shown in the following table 1, and the hardness of the high-entropy alloy powder is increased along with the increase of Ti. This is because Ti, a high hardness metal, can increase the overall hardness by the cocktail effect of the high entropy alloy, and therefore the hardness increases with increasing Ti content. As can be seen from table 1, the quaternary high-entropy alloy powder obtained in the above examples has high specific strength (specific strength refers to the ratio of density to hardness).
TABLE 1
| Examples of the invention | Density (g/cm) 3 ) | Hardness (HB) |
| 1 | 5.1 | 115 |
| 2 | 6 | 110 |
| 3 | 6.5 | 105 |
The quaternary high-entropy alloy powder obtained in the above example was placed in 3.5wt.% NaCl for 200h, and the mass change rate before and after corrosion was calculated. The results of the rate of change of the corrosion quality of the high-entropy alloy powder are shown in table 2 below, and it can be seen from table 2 that the corrosion resistance increases with the increase of the Ti content. This is because Ti can rapidly form a dense oxide film in a corrosive environment, thereby preventing corrosion from continuing.
TABLE 2
| Examples of the invention | Change in mass (%) |
| 1 | 1.7 |
| 2 | 2.3 |
| 3 | 4.9 |
The theoretical model for preparing the high-entropy alloy powder with the specific strength FeCrAlTi is shown in figure 4, and the structural model of the high-entropy alloy powder with the specific strength FeCrAlTi shows that the structure of the whole alloy system is still stable with the increase of Ti element.
The above embodiments are merely preferred embodiments of the present invention, and the present invention is not limited to the above embodiments, and modifications and changes thereof may be made by those skilled in the art within the scope of the claims of the present invention.
Claims (10)
1. A quaternary high-entropy alloy powder, characterized by comprising, in atomic percent: 20-30.77% of Fe, 20-30.77% of Cr, 20-30.77% of Al and 7.69-40% of Ti, wherein the atomic mole percentage ratio of Fe, cr and Al is 1:1:1, and the sum of the atomic percentages of the components is 100at%.
2. The quaternary high-entropy alloy powder of claim 1, wherein the quaternary high-entropy alloy powder has a single-phase BCC structure.
3. A preparation method of the quaternary high-entropy alloy powder of claim 1, characterized by mixing raw materials of iron powder, chromium powder, aluminum powder and titanium powder, placing the mixture into a ball milling tank, adding zirconia balls, and carrying out high-energy ball milling treatment to obtain the quaternary high-entropy alloy powder with a single-phase BCC structure.
4. The method for preparing quaternary high-entropy alloy powder according to claim 1, wherein the particle sizes of the iron powder, the chromium powder, the aluminum powder, and the titanium powder are 15 to 150 μm.
5. The method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein the purity of the iron powder, the chromium powder, the aluminum powder and the titanium powder is not less than 99.99wt.%.
6. The method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein a ratio of a mass of the zirconia balls to a total mass of the raw materials is (5-40): 1.
7. the method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein the zirconia balls have a diameter of 2 to 20mm.
8. The method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein the rotation speed of the high-energy ball mill is 300rpm to 800rpm.
9. The method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein the high-energy ball milling treatment mode is an intermittent type, the operation is stopped for 0-30 min every 5-60 min, and the total treatment time is not less than 40h.
10. The method for preparing the quaternary high-entropy alloy powder according to claim 1, wherein a high-energy ball milling treatment is performed by using steel balls instead of zirconia balls.
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| US20170369970A1 (en) * | 2016-06-22 | 2017-12-28 | National Tsing Hua University | High-entropy superalloy |
| CH714802A2 (en) * | 2018-03-20 | 2019-09-30 | Swatch Group Res & Dev Ltd | High entropy alloys for dressing components. |
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| US20170369970A1 (en) * | 2016-06-22 | 2017-12-28 | National Tsing Hua University | High-entropy superalloy |
| CH714802A2 (en) * | 2018-03-20 | 2019-09-30 | Swatch Group Res & Dev Ltd | High entropy alloys for dressing components. |
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