CN117025992A - Preparation method of high-strength high-plasticity VCONi medium-entropy alloy at low temperature - Google Patents
Preparation method of high-strength high-plasticity VCONi medium-entropy alloy at low temperature Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
Abstract
The invention provides a preparation method of an entropy alloy in high-strength high-plasticity VCoNi at low temperature, which comprises the following steps: (1) Proportioning V, co and Ni according to a preset mass percentage, sequentially placing the mixture into a crucible, repeatedly smelting and cooling to obtain a medium-entropy alloy material; (2) Carrying out solution treatment on the prepared medium-entropy alloy material in a vacuum environment, and then processing the medium-entropy alloy material to an initial plate thickness through hot forging treatment to obtain a plate; (3) Rolling the plate subjected to hot forging treatment at high temperatures in different directions, rolling to obtain a preset rolling reduction, and mechanically grinding and decontaminating the surface of the plate to obtain a high-entropy alloy material; (4) And carrying out ordered annealing treatment and cooling treatment of a preset cooling rate on the prepared high-entropy alloy material to finally obtain the multi-level heterogeneous medium-entropy alloy material. The invention has reasonable conception and can solve the technical bottleneck problem that the yield strength of low-temperature steel and traditional FCC medium/high-entropy alloy in the prior art is still lower in low-temperature environment.
Description
Technical Field
The invention relates to the field of mechanical properties of advanced structural materials, in particular to a preparation method of an entropy alloy in high-strength high-plasticity VCoNi at low temperature.
Background
With the development of modern industry and technology, mechanical equipment has more service scenes in a low-temperature environment, and higher requirements are put on strong plastic matching of novel structural materials for ensuring structural application safety and light weight of the materials. In recent years, single-phase face-centered cubic (FCC) medium/high entropy alloys exhibit excellent low temperature (4-77K) stretch plasticity (. Epsilon.) u ) And fracture toughness (K) IC ) Drawing extensive attention from the academic and engineering community. Recently, a new single-phase FCC VCoNi entropy alloy has been reported that produces significant lattice distortion and chemical short-range order by incorporating V atoms of larger size. The entropy alloy in VCoNi has excellent mechanical properties, such as room temperature strong plastic matching, high Wen Xiachao plasticity, hydrogen embrittlement resistance and the like, and is a novel structural material with great application potential in the fields of aerospace, transportation and the like. However, low temperature steels and FCC medium/high entropy alloys, which exhibit excellent low temperature environment, have tensile yield strength (σ y ) All the lower (< 0.5 GPa), is always the biggest bottleneck limiting the practical application. In addition, advanced high strength steels with ultra-high yield strength at room temperature inevitably undergo ductile-brittle transition at low temperatures, resulting in severe loss of plasticity. Therefore, the problem to be solved is how to further improve the mechanical properties under low temperature environment, especially to maintain high plasticity under ultra-high strength.
In order to improve the tensile plasticity of high-strength metal materials as much as possible, based on microstructure design taking "plastic strain gradient" as a starting point, heterogeneous strain hardening strategies have been proposed in recent years. Isomerization is a microstructure formed by orderly constructing a region with obvious difference between two mechanical properties of strength and plasticity, and is considered to be an effective hardening strategy capable of considering both the strength and the plasticity of a metal material. The heterogeneous deformation induced additional strain hardening is utilized, the isomerism improves the uniform stretching plasticity and the synergistic relationship between the strength and the stretching plasticity, and the heterogeneous deformation induced additional strain hardening is particularly suitable for high-strength materials. In addition, the stacking fault energy of the FCC medium/high entropy alloy is further reduced in a low temperature environment, which can generate additional deformation mechanisms such as stacking fault, deformation twin crystal, close packed hexagonal structure (HCP) phase transformation and the like, thereby continuously improving the strain hardening capacity. Therefore, by combining the existing isomerism strengthening strategy and combining the intrinsic excellent deformability of the high-entropy alloy in FCC, a synergistic strengthening mechanism is realized, and the novel high-strength high-plasticity FCC medium-entropy alloy at low temperature is expected to be designed.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength high-plasticity VCoNi medium-entropy alloy at low temperature, which is reasonable in conception, and utilizes the combination of alloying treatment, pre-deformation processing and heat treatment technology to prepare the VCoNi medium-entropy alloy with the tensile yield strength of approximately 2.2 GPa and the tensile uniform elongation of approximately 20 percent at low temperature, so as to solve the technical bottleneck problem that the yield strength of low-temperature steel and traditional FCC medium/high-entropy alloy in the prior art is still lower in a low-temperature environment.
In order to solve the technical problems, the preparation method of the entropy alloy in the high-strength high-plasticity VCoNi at low temperature provided by the invention specifically comprises the following steps:
(1) V, co and Ni are adopted as alloy raw materials and are proportioned according to a preset mass percentage, then the alloy raw materials are put into a crucible according to the sequence of melting points of all alloy elements from low to high, and the alloy raw materials are repeatedly smelted by a vacuum arc furnace and cooled along with the furnace to obtain a medium-entropy alloy material in the form of an ingot;
(2) Carrying out solution treatment on the medium-entropy alloy material prepared in the step (1) in a vacuum environment within a preset annealing temperature-time range, and then processing the medium-entropy alloy material to an initial plate thickness through hot forging treatment to obtain a plate;
(3) Carrying out high-temperature rolling on the sheet subjected to the hot forging treatment in the step (2), then carrying out cold rolling at the liquid nitrogen temperature to obtain a preset rolling reduction, and carrying out mechanical grinding and decontamination treatment on the surface of the cold-rolled sheet obtained after the cold rolling to obtain a high-entropy alloy material;
(4) And (3) orderly annealing the high-entropy alloy material prepared in the step (3) within a preset temperature-time range, and then cooling at a preset cooling rate to finally obtain the multi-stage heterogeneous medium-entropy alloy material.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: the medium entropy alloy material of the step (1) is expressed as V x Co y Ni z X, y and z are mole percentages of chemical elements V, co and Ni respectively; and the V is x Co y Ni z The ratio of the amounts of the substances of V, co and Ni elements is x: y: z= (0.8-1.2): (0.5-1.5).
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: the V is x Co y Ni z The ratio of the amounts of the substances of V, co and Ni elements is specifically x:y:z.apprxeq.1:1:1.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: in the smelting process, each alloy raw material is repeatedly smelted for 10 times under the protection of high-purity argon, so that the uniformity of chemical components and microstructures is ensured, each alloy raw material is melted into alloy liquid under the conditions of low loss and high uniform mixing state, and then the alloy liquid is naturally cooled in a vacuum smelting furnace to achieve the aim of slow forming.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps of: in a vacuum environment, the temperature is 1373-1473K, and the time is 2-4 h.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: the reduction of the hot forging treatment in the step (2) is not more than 75%.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: in the step (3), cold rolling is carried out for as many times as possible at the liquid nitrogen temperature, the rolling reduction of each time is controlled to be 0.05mm, and simultaneously, the cold rolled strip is kept stand in a liquid nitrogen tank for 5min before and after each time of rolling for full cooling; the foregoing process is repeated to finally achieve a reduction of greater than 90%.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: in the step (4), short-time annealing treatment is carried out at the recrystallization temperature of more than 50-100 ℃; in the step (4), during the cooling treatment at a preset cooling speed, the sample is not subjected to tube sealing vacuum treatment before being subjected to heat treatment in a muffle furnace, the sample is directly placed on a crucible sheet, and then the sample is rapidly thrown into liquid nitrogen directly to obtain the cooling speed of 1000 ℃/s as fast as possible.
The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature comprises the following steps: the annealing treatment temperature is 880-950 ℃ and the annealing treatment time is 30-600s.
The invention also has the following advantages:
(1) VCoNi alloy is FCC+L1 2 Unlike the conventional nano-scale L1, the dual-phase alloy of (2) 2 Nano precipitated phase, second phase L1 in the alloy 2 Is a large-size intermetallic compound and can play the following key roles: (a) Large-sized lamellar L1 2 Penetrating the crystal grains, dividing the equiaxed ultrafine crystal into two parts, and enabling the Hall-Petch effect to be exerted to the greatest extent, thereby realizing high yield strength of record level; (b) L1 2 The internal part has high density of layer errors, nano twin crystals and HCP phases with only a few atomic layers, thus having intrinsic high strength; (c) L1 2 The catalyst has a coherent interface with an FCC matrix, a large number of dislocation plugs are accumulated at the two-phase interface, and L1 2 The method can coordinate deformation through rotation, so that the early cracking of an interface is avoided, and the method has a certain isomerism toughening effect, so that the plasticity of the material is improved;
(2) The FCC matrix is of an ultrafine grain structure, and the average grain size is smaller than 1.5 mu m;
(3) The sub-nano scale chemical short-range ordered structure in the FCC matrix can play a role similar to that of a precipitated phase, generate an additional strain field to obviously block dislocation movement, and further realize synergistic stiffening;
(4) The mechanical properties of the alloy with the record level at low temperature (77K and 4K) are far superior to those of other high-performance alloys, such as stainless steel, FCC medium/high entropy alloy, high manganese steel and the like;
(5) The alloy has good hot processing and cold processing properties;
(6) "Cold reduction per pass 0.0 in step (3)"5mm "and" standing cold rolled strip in liquid nitrogen tank for 5min before and after cold rolling for sufficient cooling "is key to obtain high density dislocation and stacking fault (high yield strength) in initial structure," recrystallization temperature 50-100deg.C above for short time annealing "in step (4) and" throwing sample directly into liquid nitrogen to obtain cooling rate 1000 ℃/s as fast as possible "is to obtain large size L1 simultaneously 2 Intermetallic compounds and small-scale chemical short-range ordered structures.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are some embodiments of the invention and that other drawings may be obtained from these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an XRD pattern of an alloy prepared by the method for preparing an entropy alloy in high strength and high plasticity VCoNi at low temperature according to examples 1 and 2 of the present invention;
FIG. 2 is an EBSD quality chart (a), an IFFT lattice image (b) and a room/low temperature mechanical property chart (c) of an alloy prepared by the preparation method of the entropy alloy in the high-strength and high-plasticity VCONi at low temperature in the embodiment 1 of the invention;
fig. 3 is an EBSD mass map (a), an IFFT lattice image (b) and a chamber/low temperature mechanical property map (c) of the alloy prepared by the preparation method of the entropy alloy in high strength and high plasticity VCoNi at low temperature in example 2 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further illustrated by the following examples.
Example 1
As shown in fig. 1, the preparation method of the entropy alloy in the high-strength and high-plasticity vcon at low temperature provided in this embodiment 1 specifically includes the following steps:
s101, taking V, co and Ni elements as alloy raw materials and proportioning according to near-equiatomic ratio, then putting the alloy raw materials into a crucible according to the sequence of melting points of all the alloy elements from low to high, repeatedly smelting for 10 times by a vacuum arc furnace, and cooling along with the furnace to obtain the intermediate entropy alloy material in the form of a non-hole cast ingot with uniform components.
S102, performing solution treatment on the medium-entropy alloy material prepared in the step S101 in a vacuum environment at 1200 ℃/24/h, and then processing the medium-entropy alloy material into a plate with the thickness of 30 mm by performing hot forging treatment processes in different directions.
S103, performing high-temperature rolling at 1150 ℃ on the plate obtained after the hot forging treatment in the step S102, performing multi-pass cold rolling processing with the rolling reduction of 0.05mm in each pass at the liquid nitrogen temperature, wherein the final rolling reduction is 95%, and performing mechanical grinding processing and decontamination treatment on the surface of the cold-rolled plate obtained after the cold rolling processing.
S104, carrying out ordered annealing treatment (namely selecting heat treatment time and temperature capable of generating small-size chemical short-range ordered CSRO and large-size L12 intermetallic compounds, wherein CSRO and L12 are ordered structures) on the high-entropy alloy material treated in the step S103 at a preset speed of 900 ℃/2.5 min, then rapidly placing the high-entropy alloy material in liquid nitrogen to obtain a cooling speed of 1000 ℃/S as fast as possible, and finally obtaining the multi-stage heterogeneous medium-entropy alloy VCoNi (HS 1 )。
The green curve in FIG. 1 is the VCoNi (HS) prepared in example 1 1 ) X-ray diffraction result of the medium entropy alloy shows that the alloy is FCC+L1 2 A two-phase structure.
FIG. 2 (a) shows VCoNi (HS) prepared in example 1 1 ) The EBSD mass diagram in the medium entropy alloy can be seen from the figure: the alloy contains FCC ultra-fine grain matrix (average grain size of 0.42 μm) and L1 2 Intermetallic compound (average thickness was 0.12 μm). At the same time, there is also a chemical short-range ordered structure with a size below 1nm, fig. 2 (b).
The invention also relates to the intermediate entropy alloy VCoNi (HS) prepared in the example 1 1 ) Tensile testing was performed, fig. 2 (c). The length, width and thickness of the tensile specimen gauge length were 10mm, 4.0mm and 1.0mm, respectively. A standard tester (MTS model SANS UTM 5305S) was used at 298K (25 ℃), 77K (-196 ℃) and 4K (-269 ℃) temperatures, respectivelyUniaxial tensile test was performed at quasi-static tensile rate of (c). Each tensile test was repeated three times to ensure reproducibility of the tensile curve. In FIG. 2 (c) is VCoNi (HS) 1 ) Room/low temperature mechanical properties of (c). In 298K, VCoNi (HS 1 ) Yield strength (sigma) of medium entropy alloy y ) Tensile strength (sigma) u ) And uniform elongation (e) u ) 2.01GPa, 2.03GPa and 16%, respectively. With decreasing temperature, in 77K, σ y 、σ u And e u Further up to 2.21 GPa, 2.31 GPa and 19%. In addition, a strong plastic match at 4K and 77K approach, saw tooth rheological behavior occurs. VCoNi (HS) 1 ) The medium-entropy alloy has the most excellent strong plastic matching at present in low-temperature environments (4K and 77K), exceeds the alloy materials reported in all documents, and has very wide application scenes.
Example 2
The preparation method of the entropy alloy in the high-strength high-plasticity VCoNi at low temperature provided in the embodiment 2 specifically comprises the following steps:
s201, adopting V, co and Ni elements as alloy raw materials and proportioning according to near-equiatomic ratio, then putting the alloy raw materials into a crucible according to the sequence of the melting points of the elements from low to high, repeatedly smelting for 10 times by a vacuum arc furnace, and cooling along with the furnace to obtain the intermediate entropy alloy material in the form of a non-hole cast ingot with uniform components.
S202, performing solution treatment on the medium-entropy alloy material in a vacuum environment of 1200 ℃/24/h, and then processing the medium-entropy alloy material into a plate with the thickness of 30 mm by performing hot forging processes in different directions.
S203, performing high-temperature rolling at 1150 ℃ on the plate subjected to the hot forging treatment, performing multi-pass cold rolling with the rolling reduction of 0.05mm per pass at the liquid nitrogen temperature, wherein the final rolling reduction is 95%, and performing mechanical grinding and decontamination treatment on the surface of the cold-rolled plate.
S204, carrying out ordered annealing treatment on the treated high-entropy alloy material at a preset speed of 880 ℃/10 min, then rapidly placing the high-entropy alloy material in liquid nitrogen to obtain a cooling speed (1000 ℃/S) as fast as possible, and finally obtaining the multistage heterogeneous medium-entropy alloy VCoNi (HS) 2 )。
The yellow curve in FIG. 1 is the VCoNi (HS) prepared in example 2 2 ) X-ray diffraction result of the medium entropy alloy shows that the alloy is FCC+L1 2 A two-phase structure.
In FIG. 3, (a) is VCoNi (HS) prepared in example 2 2 ) The EBSD mass diagram in the medium entropy alloy can be seen from the figure: the alloy contains FCC ultra-fine grain matrix (average grain size of 1.26 μm) and L1 2 Intermetallic compound (average thickness: 0.38 μm) and small-sized sigma precipitate phase (average diameter: 10 nm). In fig. 3 (b) it is shown that the alloy also has a chemical short range order structure with a size below 1 nm.
In FIG. 3 (c) is VCoNi (HS) 2 ) Room/low temperature mechanical properties of (c). In 298K, VCoNi (HS 2 ) Sigma of medium entropy alloy y 、σ u And e u 1.57 GPa, 1.82 GPa and 24.8%, respectively. With decreasing temperature, in 77K, σ y 、σ u And e u Further improved to 1.79 GPa, 2.12 GPa and 24.1%. In addition, a strong plastic match at 4K, similar to 77K, also exhibits a saw tooth rheological behavior.
The invention utilizes the combination of alloying treatment, pre-deformation processing and heat treatment technology to prepare the VCoNi medium entropy alloy with the tensile yield strength of approximately 2.2 GPa and the tensile uniform elongation of approximately 20 percent at low temperature, which is used for solving the technical bottleneck problem that the yield strength of low-temperature steel and traditional FCC medium/high entropy alloy in the prior art is still lower in low-temperature environment.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. The preparation method of the high-strength high-plasticity VCONi medium-entropy alloy at low temperature is characterized by comprising the following steps of:
(1) V, co and Ni are adopted as alloy raw materials and are proportioned according to a preset mass percentage, then the alloy raw materials are put into a crucible according to the sequence of melting points of all alloy elements from low to high, and the alloy raw materials are repeatedly smelted by a vacuum arc furnace and cooled along with the furnace to obtain a medium-entropy alloy material in the form of an ingot;
(2) Carrying out solution treatment on the medium-entropy alloy material prepared in the step (1) in a vacuum environment within a preset annealing temperature-time range, and then processing the medium-entropy alloy material to an initial plate thickness through hot forging treatment to obtain a plate;
(3) Carrying out high-temperature rolling on the sheet subjected to the hot forging treatment in the step (2), then carrying out cold rolling at the liquid nitrogen temperature to obtain a preset rolling reduction, and carrying out mechanical grinding and decontamination treatment on the surface of the cold-rolled sheet obtained after the cold rolling to obtain a high-entropy alloy material;
(4) And (3) orderly annealing the high-entropy alloy material prepared in the step (3) within a preset temperature-time range, and then cooling at a preset cooling rate to finally obtain the multi-stage heterogeneous medium-entropy alloy material.
2. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the method comprises the following steps: the medium entropy alloy material of the step (1) is expressed as V x Co y Ni z X, y and z are mole percentages of chemical elements V, co and Ni respectively; and the V is x Co y Ni z The ratio of the amounts of the substances of V, co and Ni elements is x: y: z= (0.8-1.2): (0.5-1.5): (0.5~1.5)。
3. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 2, wherein the method comprises the following steps: the V is x Co y Ni z The ratio of the amounts of the substances of V, co and Ni elements is specifically x:y:z.apprxeq.1:1:1.
4. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the method comprises the following steps: in the smelting process, each alloy raw material is repeatedly smelted for 10 times under the protection of high-purity argon, so that the uniformity of chemical components and microstructures is ensured, each alloy raw material is melted into alloy liquid under the conditions of low loss and high uniform mixing state, and then the alloy liquid is naturally cooled in a vacuum smelting furnace to achieve the aim of slow forming.
5. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the annealing treatment conditions in the step (2) are as follows: in a vacuum environment, the temperature is 1373-1473K, and the time is 2-4 h.
6. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the method comprises the following steps: the reduction of the hot forging treatment in the step (2) is not more than 75%.
7. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the method comprises the following steps: in the step (3), cold rolling is carried out for as many times as possible at the liquid nitrogen temperature, the rolling reduction of each time is controlled to be 0.05mm, and simultaneously, the cold rolled strip is kept stand in a liquid nitrogen tank for 5min before and after each time of rolling for full cooling; the foregoing process is repeated to finally achieve a reduction of greater than 90%.
8. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 1, wherein the method comprises the following steps: in the step (4), short-time annealing treatment is carried out at the recrystallization temperature of more than 50-100 ℃; in the step (4), during the cooling treatment at a preset cooling speed, the sample is not subjected to tube sealing vacuum treatment before being subjected to heat treatment in a muffle furnace, the sample is directly placed on a crucible sheet, and then the sample is rapidly thrown into liquid nitrogen directly to obtain the cooling speed of 1000 ℃/s as fast as possible.
9. The method for preparing the entropy alloy in the high-strength and high-plasticity VCoNi at low temperature as claimed in claim 8, wherein the method comprises the following steps: the annealing treatment temperature is 880-950 ℃ and the annealing treatment time is 30-600s.
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