CN112877579A - Non-equal atomic ratio high-entropy alloy and method for preparing wire by using same - Google Patents
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Abstract
The invention belongs to the technical field of high-entropy alloy wire materials and preparation, and discloses a non-equal atomic ratio high-entropy alloy wire material and a preparation method thereof, wherein the preparation raw materials are Fe, Mn, Cr and Ni metal particles, and the preparation method comprises the following steps: weighing the metal particles according to a set proportion, and melting and pouring the metal particles in a vacuum induction melting furnace to prepare an unequal atomic ratio high-entropy alloy ingot; homogenizing and heat-treating the as-cast non-equal atomic ratio high-entropy alloy ingot prepared in the initial stage, then carrying out hot-spinning forging to obtain a bar, and then carrying out rolling by an end rolling machine, high-temperature annealing and multi-pass drawing to obtain the wire. The non-equiatomic ratio high-entropy alloy wire prepared by the method is simple in preparation process, and any intermediate annealing treatment and surface treatment are not required to be inserted in the wire drawing process, so that the production process of the wire is greatly simplified.
Description
Technical Field
The invention belongs to a metal material and a preparation technology thereof, and particularly relates to a non-equiatomic ratio high-entropy alloy, a wire material thereof and a preparation method thereof.
Background
The design concept of traditional metal alloys has been to use one or two elements as the main components, such as iron-based, aluminum-based, copper-based, magnesium-based alloys, etc., with a small amount of other elements to improve performance. The properties of the alloy are usually changed by adding a small amount of certain elements in the traditional alloy, for example, aluminum alloy which is a decorative material frequently used in life is used, aluminum is used as a main element, and a small amount of elements such as magnesium, zinc, copper and the like are added into the alloy, so that the alloy has higher strength. The steel materials such as tool steel, stainless steel, spring steel and the like which are used at present are mainly obtained by taking iron element as a main material and adding different other small elements. To date, nearly one hundred alloy systems have been practically developed and popularized, such as iron-based alloys, aluminum-based alloys, magnesium-based alloys, and copper-based alloys. As researchers develop and research traditional alloys deeply, it is difficult to develop new alloy systems from traditional alloy systems. Therefore, the development of new alloy systems has become a necessary requirement for the development of metal materials in society, and the design of single main component materials of traditional alloys has entered the bottleneck period. In the middle of the 90's of the 20 th century, the concept of high entropy alloy (high entropy alloy) was proposed by samourer et al, breaking the conventional model. Such an alloy is defined as an alloy consisting of at least five main elements, each of which is between 5 and 35 atomic percent. Secondly, with the continuous development of high-entropy alloys, the first generation of equimolar single-phase high-entropy alloys have certain limitations, and the second generation of high-entropy alloys have been developed continuously, and mainly refer to a class of high-entropy alloys containing more than four main elements and having a metastable phase structure. Previous studies have shown that high entropy alloys can form simple solid solution structures, rather than intermetallic and other complex compounds, a phenomenon generally attributed to the high configurational entropy of the solid solution state of the high entropy alloy. In addition, the high-entropy alloy also has high hardness, high strength, good thermal stability, excellent wear resistance and oxidation resistance, and has wide engineering application prospect.
Most of the high-entropy alloy materials prepared at present are bulk materials or thin films, and the preparation of the high-entropy alloy wires is only reported. The prior known preparation method of the high-entropy alloy wire is found through the search of the prior art documents that the Chinese patent publication number is CN110538945A, and the publication date is as follows: 2019.12.06, the invention is a refractory high-entropy alloy stranded wire material, and an application and a preparation method thereof, the high-entropy alloy stranded wire material is beneficial to promoting the engineering application of high-entropy alloy in the field of additive manufacturing, but has the possibility of non-uniformity of high-entropy alloy components. The Chinese patent publication number is CN109234601A, and the publication date is: 2019.01.18, the invention is a high-entropy alloy solid wire for electric arc cladding and a preparation method thereof, the preparation process of the high-entropy alloy wire adopts a mechanical alloying technology, then adopts a spray deposition molding technology to prepare an alloy ingot, and then carries out deep cooling drawing on the alloy, and the preparation method is complex and has a long period. In order to solve the technical problem, the development of a high-entropy alloy wire with strong universality and high performance is urgently needed. In addition, the high-entropy alloy has higher strength and excellent wear resistance. Therefore, the high-entropy alloy wire has great potential and can be prepared into a high-strength high-entropy alloy rope stranded wire. The high-entropy alloy wire has high application potential in metal 3D printing technology and on-site repair of industrial major equipment and military equipment.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the prior art, the invention provides a non-equiatomic ratio high-entropy alloy, a wire material thereof, and a preparation method and application thereof.
The technical scheme is as follows: the invention relates to a non-equiatomic ratio high-entropy alloy, which comprises FeaMnbCrcNidIn the formula, a, b, c and d respectively represent the atom percentage content of the corresponding metal elements.
Further preferred is where a is 35, b is 10, c is 20, and d is 35.
The preparation method of the non-equal atomic ratio high-entropy alloy wire comprises the following steps:
(1) preparing metal block particles containing Fe, Mn, Cr and Ni according to atomic percentage;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a vacuum induction smelting furnace;
(3) casting the alloy smelted in the step (2) into ingots, carrying out homogenization treatment in a high-temperature heat treatment furnace, and then taking out and water-quenching to normal temperature;
(4) performing hot rotary forging on the alloy ingot subjected to the homogenization heat treatment in the step (3), forging the alloy ingot into a bar with the diameter of 12-6 mm, wherein the error of the roundness of the section of the bar is 0.2 mm;
(5) annealing the bar obtained in the step (4) at high temperature to eliminate residual internal stress;
(6) and (4) rolling the bar obtained in the step (5) into a bar with the end part corresponding to the size of the drawing die through a rolling end machine at room temperature, and performing multi-pass continuous room-temperature drawing to finally obtain the wire with the diameter of 0.3-2.0 mm.
Wherein, in the step (3), the homogenization heat treatment temperature is 1000-1200 ℃, and the heat treatment time is 5-12 h.
In the step (4), the hot rotary swaging temperature is 900-1100 ℃.
In the step (5), the annealing temperature is 900-1200 ℃, and the annealing time is 10-60 min.
In the step (6), the cross-sectional compression of each pass is 1-30%, and the cross-sectional compression of each pass is preferably 20% in order to ensure the production benefit and the product quality.
The invention also discloses application of the wire serving as a 3D printing wire raw material, a steel electrode and a steel wire rope stranding wire.
Has the advantages that: compared with the prior art, (1) the unequal atomic ratio high-entropy alloy material is prepared from Fe, Mn, Cr and Ni metal block particles, and the cost is greatly reduced compared with the prior high-entropy alloy material which usually contains Co and other noble metal powder; (2) the preparation method of the material adopts vacuum induction melting and casting ingot forming, hot swaging, rolling, heat treatment and wire drawing to prepare the material, particularly, the alloy system does not need intermediate annealing treatment and surface treatment in the room temperature drawing process, and the preparation process is simple; (3) the anisoatomic ratio high-entropy alloy prepared by the method has excellent wire forming capability, and can be used for 3D printing wire raw materials, steel welding rods, wire rope stranding and the like.
Drawings
FIG. 1 is a drawing of a starting wire rod of 6.9mm phi after forging and rolling by an end rolling mill followed by annealing for 10 min;
FIG. 2 is a high-entropy alloy wire with a diameter of 0.45mm finally prepared after multi-pass wire drawing;
FIG. 3 is a view of a forged, annealed 1 hour post-rolling by an end-rolling mill, original wire rod of 6.0mm phi;
FIG. 4 is a high-entropy alloy wire with a diameter of 0.3mm finally prepared after multi-pass wire drawing.
Detailed Description
The present application will be described in detail with reference to specific examples.
Example 1
Composition design and preparation of alloy
Non-equal atomic ratio high-entropy alloy FeaMnbCrcNidAnd a, b, c and d respectively represent the atom percentage content of the corresponding metal element, wherein a is 35, b is 10, c is 20 and d is 35.
The preparation method of the unequal atomic ratio high-entropy alloy wire comprises the following steps:
(1) according to Fe35Mn10Cr20Ni35Preparing metal block particles containing Fe, Mn, Cr and Ni;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a vacuum induction smelting furnace for at least 3 times to ensure the uniformity of alloy components;
(3) casting the alloy smelted in the step (2) into ingots, setting the temperature to be 1000 ℃ in a high-temperature heat treatment furnace, preserving the heat for 12 hours, carrying out homogenization treatment, and then taking out the ingots and carrying out water quenching to normal temperature;
(4) performing hot rotary forging on the alloy ingot subjected to the homogenization heat treatment in the step (3) at 900 ℃, and forging the alloy ingot into a bar with the diameter of 9.5 mm;
(5) rolling the bar material obtained by forging in the step (4) into a bar material with the diameter of 6.9mm by a rolling end machine, and annealing for 10min at the high temperature of 900 ℃ to eliminate residual internal stress; as shown in fig. 1;
(6) and (3) rolling the bar obtained in the step (5) into a bar with the end part corresponding to the size of the drawing die through a rolling end mill at room temperature, and performing multi-pass continuous room-temperature drawing, wherein the section compression ratio of each pass is 20%, and finally obtaining a wire with the diameter of 0.45mm, wherein a product is shown in figure 2.
Example 2
Composition design and preparation of alloy
Non-equiatomic high-entropy alloy, FeaMnbCrcNidAnd a, b, c and d respectively represent the atom percentage content of the corresponding metal element, wherein a is 35, b is 10, c is 20 and d is 35.
The preparation method of the unequal atomic ratio high-entropy alloy wire comprises the following steps:
(1) according to Fe35Mn10Cr20Ni35Preparing metal block particles containing Fe, Mn, Cr and Ni;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a vacuum induction smelting furnace for at least 3 times to ensure the uniformity of alloy components;
(3) casting the alloy smelted in the step (2) into ingots, setting the temperature to be 1000 ℃ in a high-temperature heat treatment furnace, preserving the heat for 12 hours, carrying out homogenization treatment, and then taking out the ingots and carrying out water quenching to normal temperature;
(4) performing hot rotary forging on the alloy ingot subjected to the homogenization heat treatment in the step (3) at 900 ℃, and forging the alloy ingot into a bar with the diameter of 9.5 mm;
(5) rolling the bar material obtained by forging in the step (4) into a bar material with the diameter of 6.0mm by a rolling end machine, and annealing for 60min at the high temperature of 1000 ℃ to eliminate residual internal stress; as shown in fig. 3;
(6) and (3) rolling the bar obtained in the step (5) into a bar with the end part corresponding to the size of the drawing die through a rolling end mill at room temperature, and performing continuous room-temperature drawing for multiple passes, wherein the section reduction rate of each pass is 25%, and finally obtaining a wire with the diameter of phi 0.3mm, wherein a product is shown in figure 4.
Claims (8)
1. A non-equiatomic high-entropy alloy is characterized by the molecular formula of FeaMnbCrcNidIn the formula, a, b, c and d respectively represent the atom percentage of corresponding metal elements, the atom percentage ranges of Fe, Mn and Cr elements are that a is more than or equal to 33 and less than or equal to 36, b is more than or equal to 8 and less than or equal to 12, c is more than or equal to 18 and less than or equal to 22, and the rest is the atom percentage of Ni element.
2. The non-equiatomic high-entropy alloy according to claim 1, preferably has a composition of 35, 10, 20, 35.
3. A method of making wires from a high entropy non-isoatomic ratio alloy as claimed in claim 1 or 2, comprising the steps of:
(1) preparing metal block particles containing Fe, Mn, Cr and Ni according to atomic percentage;
(2) repeatedly smelting the metal block particles prepared in the step (1) in a vacuum induction smelting furnace;
(3) casting the alloy smelted in the step (2) into ingots, carrying out homogenization treatment in a high-temperature heat treatment furnace, and then taking out and water-quenching to normal temperature;
(4) performing hot rotary forging on the alloy ingot subjected to the homogenization heat treatment in the step (3) to forge the alloy ingot into a bar with the diameter of 12-6 mm;
(5) annealing the bar obtained in the step (4) at high temperature to eliminate residual internal stress;
(6) and (4) rolling the bar obtained in the step (5) into a bar with the end part corresponding to the size of the drawing die at room temperature, and performing multi-pass continuous room-temperature drawing to finally obtain the wire with the diameter of 0.3-2.0 mm.
4. The method according to claim 3, wherein in the step (3), the homogenization heat treatment temperature is 1000 ℃ to 1200 ℃ and the heat treatment time is 5 to 12 hours.
5. The method according to claim 3, wherein in the step (4), the swaging temperature is 900 to 1100 ℃.
6. The method according to claim 3, wherein in the step (5), the annealing temperature is 900 to 1200 ℃ and the annealing time is 10 to 60 min.
7. The method of claim 3, wherein in step (6), the cross-sectional reduction at each pass is from 1% to 30%.
8. The method of claim 3, wherein in step (6), the cross-sectional reduction per pass is 20%.
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| CN114657435A (en) * | 2022-02-28 | 2022-06-24 | 东南大学 | Industrial pure single-phase high-entropy alloy and preparation method thereof |
| CN116145003A (en) * | 2022-12-30 | 2023-05-23 | 中核燕龙科技有限公司 | FeCrNiMn high-entropy alloy material and preparation method thereof |
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