CN114836667A - Light high-temperature high-entropy alloy and preparation process of rod material thereof - Google Patents
Light high-temperature high-entropy alloy and preparation process of rod material thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of high-entropy alloy rod material preparation, and particularly relates to a light high-temperature high-entropy alloy and a rod material preparation process thereof, wherein the alloy consists of the following raw materials in atomic percentage: ti22-25 at.%, Sc22-25 at.%, Zr22-25 at.%, Nb0-17 at.%, V17-25 at.%; scandium and niobium elements are sequentially added on the basis of the TiZrV alloy, the mechanical property of the as-cast alloy is improved by adjusting the proportion of the metal elements, the alloy structure is adjusted by hot extrusion and annealing treatment, and the performance of the alloy material is further regulated and controlled, so that the requirements of different use environments are met, the application range of the light high-temperature high-entropy alloy is widened, the process is simple, and the method is suitable for large-scale industrial application.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy rod material preparation, and particularly relates to a light high-temperature high-entropy alloy and a rod material preparation process thereof.
Background
The high-entropy alloy is independently proposed in 2004 by the leaf of Taiwan scholars in China and the Cantor of English scholars respectively as a new alloy design concept, and a new example is provided for designing the metal alloy with remarkable performance. Due to the unique element composition and the high entropy effect, lattice distortion effect, slow diffusion effect and 'cocktail' effect, they have many excellent mechanical and functional properties, such as high hardness, high strength, excellent oxidation resistance, wear resistance, corrosion resistance, irradiation resistance, soft magnetic properties, thermoelectric properties, catalytic properties, etc., which can meet many challenging applications. The Ti-containing light high-temperature high-entropy alloy has the advantages of excellent specific strength, excellent strong plasticity harmony, high-temperature stability, specific hardness, corrosion resistance and the like, is widely researched by researchers, and has wide application prospects in the fields of aerospace, ships, rail transit and the like.
However, the development of the light high-entropy alloy at present has many factors, which limit the large-scale industrial application of the light high-entropy alloy, wherein the mechanical property of the light high-entropy alloy material is still to be improved, and the regulation and control rule of the mechanical property of the light high-entropy alloy material is unclear, so that the improvement of the mechanical property of the alloy is not regular, a systematic guidance method is lacked, and the light high-entropy alloy material cannot flexibly adapt to the requirements of different application environments; in addition, most of the traditionally prepared light high-entropy alloy is cast ingots, the size and the structure of the cast ingots are not uniform, and the process for processing and applying the cast ingots is not mature; therefore, the invention provides a novel light high-temperature high-entropy alloy system which has excellent mechanical properties, and realizes regular adjustment of the mechanical properties of an alloy material through the process of processing the alloy into a rod material, and promotes large-scale industrial application of the alloy through the processed rod material product.
Disclosure of Invention
In order to solve the technical problems, the invention provides a light high-temperature high-entropy alloy and a preparation process of a rod material thereof, provides a novel light high-temperature high-entropy alloy, sequentially adds scandium and niobium elements on the basis of TiZrV alloy, improves the mechanical property of the as-cast alloy by adjusting the proportion of the metal elements, and severely limits the large-scale industrial application of the alloy due to the nonuniformity of the size and the structure of an ingot.
The invention is realized by the following technical scheme.
A light high-temperature high-entropy alloy is composed of the following raw materials in atomic percentage: ti 22-25 at.%, Sc 22-25 at.%, Zr 22-25 at.%, Nb 0-17 at.%, V17-25 at.%.
Preferably, the alloy consists of the following raw materials in atomic percentage: ti 22 at.%, Sc 22 at.%, Zr 22 at.%, Nb 17 at.%, V17 at.%; the alloy forms BCC and HCP solid solution structures in an as-cast state, is changed into FCC, BCC and HCP solid solution structures after hot extrusion, and is then annealed. After the annealing treatment, the microstructure undergoes a significant change, which is that annealing can induce eutectoid reactions and solid phase separation in the pre-existing supersaturated or quasi-supersaturated structures, resulting in the microstructure tending to grow into cellular crystals, and the striped precipitated phases produced by hot extrusion gradually disappear, and therefore, BCC-rich, HCP-rich and FCC-rich structures are formed.
The preparation process of the rod material of the light high-temperature high-entropy alloy comprises the following steps:
respectively weighing the following raw materials in atomic percentage: ti 22-25 at.%, Sc 22-25 at.%, Zr 22-25 at.%, Nb 0-17 at.%, V17-25 at.%; smelting the weighed blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent into alloy ingots; and casting the alloy ingot into an alloy bar by a vacuum induction melting method, and extruding the alloy bar into an alloy bar by a heat consolidation press.
Preferably, the extrusion process is specifically:
heating the alloy bar from room temperature to 900 ℃ under the inert gas atmosphere, carrying out heat preservation annealing for 24h, and cooling the alloy bar to room temperature by water; and then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for 1h at 900 ℃, and then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into the alloy bar.
More preferably, in the extrusion process, the temperature rise rate is 10 ℃/min.
Preferably, the method further comprises the following steps: under the inert gas atmosphere, the temperature of the alloy rod is raised from room temperature to 400-1000 ℃, then the alloy rod is annealed for 24 hours in a heat preservation way, and finally furnace cooling or water cooling is carried out to the room temperature.
More preferably, the temperature increase rate is 10 ℃/min when the alloy rod material is annealed.
Preferably, the diameter of the alloy rod material is 7-16mm, and the length of the alloy rod material is 30-100 cm.
Compared with the prior art, the invention has the following beneficial effects:
according to the light high-entropy alloy rod material provided by the invention, scandium and niobium elements are sequentially added on the basis of the TiZrV alloy, and the mechanical property of the as-cast alloy is improved by adjusting the proportion of the metal elements;
The TiZrV ingot is of a BCC structure, a large number of HCP structures are formed after Sc is added, and an FCC structure is formed along with the addition of Nb and subsequent hot extrusion annealing, namely, an as-cast alloy sample of the light high-entropy alloy presents a multi-phase solid solution structure of BCC and HCP, and an extruded alloy sample and an annealed alloy sample present a multi-phase solid solution structure of FCC, BCC and HCP;
the grain size and the precipitate property of the FCC, BCC and HCP multiphase solid solution are regulated and controlled through a subsequent hot extrusion and annealing process, so that the performance of the alloy material is regulated and controlled, the application prospect of the high-entropy alloy material is expanded, and the regulation and control method is simple and is suitable for large-scale industrial application;
the light high-temperature high-entropy alloy rod material prepared by the method is simple to prepare, low in cost, simple and effective in performance regulation and control, has great potential in the application fields of aerospace and ships and warships, and is expected to become a high-performance high-entropy component when being used as a structural material of the aerospace and ships and warships.
Drawings
FIG. 1 is the appearance of a sample of example 4 of the present invention;
in FIG. 2, (a) is an XRD pattern of the samples of comparative example 1 and examples 1-2; (b) XRD patterns for the samples of examples 3-8.
FIG. 3, (a) is a microstructure of an alloy rod prepared in example 3 of the present invention; (b) the microstructure of the alloy rod prepared in example 4; (c) the microstructure of the alloy rod subjected to the annealing treatment at 1000 ℃ in example 8 is shown;
FIG. 4, (a) is a tensile engineering stress-strain plot at room temperature for the samples of comparative example 1 and examples 1-2; (b) tensile engineering stress-strain curves at room temperature for the samples of examples 3-8.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
A light high-temperature high-entropy alloy is composed of the following raw materials in atomic percentage: ti 22-25 at.%, Sc 22-25 at.%, Zr 22-25 at.%, Nb 0-17 at.%, V17-25 at.%.
Preferably, the alloy consists of the following raw materials in atomic percentage: ti 22 at.%, Sc 22 at.%, Zr 22 at.%, Nb 17 at.%, V17 at.%;
The preparation process of the rod material of the light high-temperature high-entropy alloy comprises the following steps: smelting the weighed blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent into alloy ingots; casting an alloy ingot into an alloy bar by a vacuum induction melting method, extruding the alloy bar into an alloy rod by a heat consolidation press, and then annealing the rod; the prepared rod material has a diameter of 7-16mm and a length of 30-100 cm.
The invention adds scandium and niobium elements in turn on the basis of TiZrV alloy, improves the mechanical property of the as-cast alloy by adjusting the proportion of the metal elements, and seriously limits the large-scale industrial application of the as-cast alloy due to the nonuniformity of the size and the structure of the cast ingot.
The specific implementation process is as follows:
comparative example 1
A ternary medium entropy alloy ingot is composed of equal atoms TiZrV, namely the atomic proportions of the alloy are Ti (33.33 at.%), Zr (33.33 at.%), and V (33.33 at.%). The high-entropy alloy is prepared by smelting blocky Ti, Zr and V with the purity of more than or equal to 99.99 percent.
The synthesis method of the ternary medium entropy alloy ingot comprises the following steps:
s1, preparing ingredients
Treating the surface of each metal simple substance raw material, removing an oxide layer, carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and then respectively calculating the mass of each metal simple substance according to the atomic proportions of Ti (33.33 at.%), Zr (33.33 at.%), and V (33.33 at.%) of each metal simple substance by using 35g of the total mass and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
Example 1
A light high-temp high-entropy alloy contains Ti 25 Sc 25 Zr 25 V 25 I.e. the atomic proportions of the alloy are Sc (25 at.%), Ti (25 at.%), Zr (25 at.%), and V (25 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, Zr and V with the purity of more than or equal to 99.99 percent.
The synthesis method of the high-entropy alloy ingot comprises the following steps:
s1, preparing the ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic proportions of Sc (25 at.%), Ti (25 at.%), Zr (25 at.%), and V (25 at.%) of each metal simple substance by using 35g of the total mass and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the smelting current is 330A each time, and each time of smeltingThe time is 70 s.
Example 2
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, Zr, Nb and V with the purity of more than or equal to 99.99 percent.
The synthesis method of the high-entropy alloy ingot comprises the following steps:
s1, preparing ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
Example 3
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy bar comprises the following steps:
s1, preparing the ingredients
Treating the surface of each metal simple substance raw material to remove an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and then respectively calculating the mass of each metal simple substance according to the atomic ratio Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%) of the total mass of 35g and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current was 330A for each melting time of 70 s.
S3 preparation of alloy rod
And (4) placing the alloy ingot obtained in the step (S2) in a crucible of a vacuum induction melting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar material with the length of 8cm and the diameter of 30 mm.
Example 4
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy rod material comprises the following steps:
s1, preparing the ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
S3 preparation of alloy rod
And (3) placing the alloy ingot obtained in the step (S2) in a crucible in a vacuum induction smelting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar with the length of 8cm and the diameter of 30 mm.
S4 preparation of light high-temperature high-entropy alloy rod material
And (3) preparing the antioxidant light high-entropy alloy rod material from the alloy rod obtained in the step S3 by adopting a thermal consolidation pressure forming machine, specifically, sealing the light high-entropy alloy rod material obtained in the step S3 in a container filled with 0.5 atmosphere of inert gas, heating the temperature from room temperature to 900 ℃ at the speed of 10 ℃/min, then carrying out heat preservation and annealing for 24h, and finally carrying out water cooling to the room temperature. And then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element at 900 ℃ for one hour, then placing the sealing element in a corresponding die to extrude at the extrusion speed of 25mm/s until all materials are extruded into a bar, and obtaining the antioxidant light high-entropy alloy bar (as shown in figure 1, the maximum scale of a straight ruler is 40 cm).
Example 5
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy rod material comprises the following steps:
s1, preparing ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
S3 preparation of alloy rod
And (3) placing the alloy ingot obtained in the step (S2) in a crucible in a vacuum induction smelting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar with the length of 8cm and the diameter of 30 mm.
S4 preparation of light high-temperature high-entropy alloy rod material
And (3) preparing the antioxidant light high-entropy alloy rod material from the alloy rod obtained in the step S3 by adopting a thermal consolidation pressure forming machine, specifically, sealing the light high-entropy alloy rod material obtained in the step S3 in a container filled with 0.5 atmosphere of inert gas, heating the temperature from room temperature to 900 ℃ at the speed of 10 ℃/min, then carrying out heat preservation and annealing for 24h, and finally carrying out water cooling to the room temperature. And then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for one hour at 900 ℃, then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into a bar, and obtaining the antioxidant light high-entropy alloy bar.
S5, and carrying out subsequent annealing process treatment on the light high-temperature high-entropy alloy rod material
And sealing the light high-entropy alloy rod material obtained in the step S4 in a quartz tube filled with 0.5 atmosphere of inert gas, raising the temperature from room temperature to 400 ℃ at the speed of 10 ℃/min, annealing at the temperature of 400 ℃ for 24 hours, and furnace-cooling to room temperature.
Example 6
A light high-temperature high-entropy alloy contains Ti as its component 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy rod material comprises the following steps:
s1, preparing the ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
S3 preparation of alloy rod
And (3) placing the alloy ingot obtained in the step (S2) in a crucible in a vacuum induction smelting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar with the length of 8cm and the diameter of 30 mm.
S4 preparation of light high-temperature high-entropy alloy rod material
And (3) preparing the antioxidant light high-entropy alloy rod material from the alloy rod obtained in the step S3 by adopting a thermal consolidation pressure forming machine, specifically, sealing the light high-entropy alloy rod material obtained in the step S3 in a container filled with 0.5 atmosphere of inert gas, heating the temperature from room temperature to 900 ℃ at the speed of 10 ℃/min, then carrying out heat preservation and annealing for 24h, and finally carrying out water cooling to the room temperature. And then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for one hour at 900 ℃, then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into a bar, and obtaining the antioxidant light high-entropy alloy bar.
S5, and carrying out subsequent annealing process treatment on the light high-temperature high-entropy alloy rod material
And sealing the light high-entropy alloy rod material obtained in the step S4 in a quartz tube filled with 0.5 atmosphere of inert gas, raising the temperature from room temperature to 600 ℃ at the speed of 10 ℃/min, annealing at the temperature of 600 ℃ for 24 hours, and furnace-cooling to room temperature.
Example 7
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic proportions of the alloy are Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), respectively. The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy rod material comprises the following steps:
s1, preparing the ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
S3 preparation of alloy rod
And (3) placing the alloy ingot obtained in the step (S2) in a crucible in a vacuum induction smelting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar with the length of 8cm and the diameter of 30 mm.
S4 preparation of light high-temperature high-entropy alloy rod material
And (3) preparing the antioxidant light high-entropy alloy rod material from the alloy rod obtained in the step S3 by adopting a thermal consolidation pressure forming machine, specifically, sealing the light high-entropy alloy rod material obtained in the step S3 in a container filled with 0.5 atmosphere of inert gas, heating the temperature from room temperature to 900 ℃ at the speed of 10 ℃/min, then carrying out heat preservation and annealing for 24h, and finally carrying out water cooling to the room temperature. And then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for one hour at 900 ℃, then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into a bar, and obtaining the antioxidant light high-entropy alloy bar.
S5, and carrying out subsequent annealing process treatment on the light high-temperature high-entropy alloy rod material
And sealing the light high-entropy alloy rod material obtained in the step S4 in a quartz tube filled with 0.5 atmosphere of inert gas, raising the temperature from room temperature to 800 ℃ at the speed of 10 ℃/min, annealing at the temperature of 800 ℃ for 24 hours, and furnace-cooling to room temperature.
Example 8
A light high-temp high-entropy alloy contains Ti 22 Sc 22 Zr 22 Nb 17 V 17 I.e. the atomic ratio of the alloy is Sc (22 a) t.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), V (17 at.%). The high-entropy alloy is prepared by smelting blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent.
The synthesis method of the light high-temperature high-entropy alloy rod material comprises the following steps:
s1, preparing ingredients
Processing the surface of each metal simple substance raw material, removing an oxide layer, respectively carrying out ultrasonic cleaning on each raw material by using an acetone cleaning solution, and respectively calculating the mass of each metal simple substance according to the atomic ratio of Sc (22 at.%), Ti (22 at.%), Zr (22 at.%), Nb (17 at.%), and V (17 at.%), wherein the total mass is 35g, and weighing;
s2 preparation of alloy ingot
Placing the metal simple substances prepared in S1 into a water-cooled copper crucible of an electric arc furnace in sequence by adopting an electric arc melting method, and vacuumizing the electric arc furnace to 2.0 multiplied by 10 -3 Pa, then argon was introduced to 0.5 atmosphere. Repeatedly overturning and smelting for 5 times under the protection of high-purity argon to obtain an alloy ingot with uniform components; wherein, the repeated overturning smelting of the raw materials is carried out by utilizing a high-frequency electric arc; the melting current of each time is 330A, and the melting time of each time is 70 s.
S3 preparation of alloy rod
And (3) placing the alloy ingot obtained in the step (S2) in a crucible in a vacuum induction smelting furnace, melting the alloy ingot into liquid by using an induction coil, and then pouring the alloy liquid into a mold to obtain the antioxidant light high-entropy alloy bar with the length of 8cm and the diameter of 30 mm.
S4 preparation of light high-temperature high-entropy alloy rod material
And (3) preparing the antioxidant light high-entropy alloy rod material from the alloy rod obtained in the step S3 by adopting a thermal consolidation pressure forming machine, specifically, sealing the light high-entropy alloy rod material obtained in the step S3 in a container filled with 0.5 atmosphere of inert gas, heating the temperature from room temperature to 900 ℃ at the speed of 10 ℃/min, then carrying out heat preservation and annealing for 24h, and finally carrying out water cooling to the room temperature. And then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for one hour at 900 ℃, then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into a bar, and obtaining the antioxidant light high-entropy alloy bar.
S5, and carrying out subsequent annealing process treatment on the light high-temperature high-entropy alloy rod material
And sealing the light high-entropy alloy rod material obtained in the step S4 in a quartz tube filled with 0.5 atmosphere of inert gas, raising the temperature from room temperature to 1000 ℃ at the speed of 10 ℃/min, annealing at the temperature of 1000 ℃ for 24 hours, and furnace-cooling to room temperature.
We compared TiZrV ingot and Ti provided in comparative example 1 and examples 1-8 25 Sc 25 Zr 25 V 25 Ingot and Ti 22 Sc 22 Zr 22 Nb 17 V 17 Ingot and Ti 22 Sc 22 Zr 22 Nb 17 V 17 Cast rod and Ti 22 Sc 22 Zr 22 Nb 17 V 17 The performance of the light high-entropy alloy rod material is characterized, and fig. 2 is an XRD (X-ray diffraction) spectrum of the samples of the comparative example 1 and the examples 1-8, wherein the samples of the materials of the comparative example 1 and the examples 1-8 are correspondingly marked as T1-T9. From FIG. 2(a) it can be seen that the TiZrV ingot is BCC structure and after addition of Sc a large amount of HCP structure is formed, and from FIG. 2(b) it can be seen that with addition of Nb and subsequent hot extrusion annealing an FCC structure is formed, thus Ti in example 1 25 Sc 25 Zr 25 V 25 Ingot and Ti in examples 2 and 3 22 Sc 22 Zr 22 Nb 17 V 17 The as-cast state of (A) shows a multiphase solid solution structure of BCC and HCP, Ti in examples 4 to 8 22 Sc 22 Zr 22 Nb 17 V 17 The as-extruded and as-annealed alloy samples exhibited heterogeneous solid solution structures of FCC, BCC and HCP.
Ti 22 Sc 22 Zr 22 Nb 17 V 17 SEM images of the as-cast state, the extruded state and the annealing treatment of the high-entropy alloy are respectively shown in (a), (b) and (c) of FIG. 3, and EDS data are shown in Table 1. As shown in FIG. 3(a), Ti 22 Sc 22 Zr 22 Nb 17 V 17 High entropy alloy as-cast, found wholeThe individual microstructures are dominated by bright near equiaxed dendrites, worm-like bright particles, lamellar bright precipitates, near hexagonal spot precipitates, and intergranular structures. In our example, an irregular eutectic microstructure occurs, not only due to kinetic supercooling, but also due to relatively large thermal supercooling. Under such non-equilibrium solidification conditions, uncoupled eutectic growth is typically induced, resulting in an irregular eutectic microstructure. According to the EDS data of table 1, bright near equiaxed dendrites are rich in Ti, Zr, Nb, and V, the intergranular structure is rich in Sc, Zr, and Nb, and the near hexagonal spot precipitates are rich in Sc and Zr.
As shown in FIG. 3(b), after heat treatment at 900 ℃ and hot extrusion, the alloy structure had a distinct orientation, with a large number of refined grains formed in the extrusion direction. The alloy is mainly divided into bright near equiaxed dendrites (B1), intergranular structures (B2) (intergranular distribution white grid-like structure), near hexagonal spot precipitates (B3), striped precipitates (B4) and white grid phase (B5). To observe the composition of the phases, EDS analysis was performed. As shown in fig. 3(B) and listed in table 1, in our case, region B1 is rich in Ti, Nb, and V; regions B2 and B4 were rich in Sc and Zr, but lower in Ti, Nb, and V; region B3 is Sc-rich; the elements of region B5(BCC) are relatively uniformly distributed. Thus hot extruding Ti at 900 deg.C 22 Sc 22 Zr 22 Nb 17 V 17 High entropy alloys can induce a large amount of microstructural transformation. The homogeneously distributed Sc-rich phase is due to the increased dislocation density at higher deformation rates increasing the nucleation sites and diffusivity of the precipitate-forming elements. It was confirmed that the FCC zone (B3) had the highest Sc concentration and the BCC zone had the highest TiNbV concentration, while the FCC zone was depleted of TiNbV. Thus, the FCC phase contains a higher concentration of Sc, while the TiZrNbV element is low. The BCC phase contains higher concentrations of TiNbV, while the Sc and Zr concentrations, especially Sc, are reduced. From the Sc-Ti binary phase diagram, Ti has limited solid-state solubility in Sc, which may result in lower Sc concentrations in the BCC phase. EDS shows that high concentrations of Sc are accompanied by low contents of Ti, Zr, Nb and V. Thus the presence of Ti, Zr, Nb and V stabilizes the FCC structure of Sc. The region in which the Sc, Zr and Ti, Sc, Zr, Nb and V-rich elements are uniformly distributed is the HCP structure.
As shown in fig. 3(C), after annealing, 4 regions of different morphologies, i.e., C1, C2, C3, and C4, were observed, which were greatly different from the as-cast and extruded states. The microstructure tends to grow into a cellular structure, and the streak-like precipitated phase caused by the hot extrusion disappears, and the corresponding element distribution is shown in table 1. In summary, a 24h 1000 degree incubation can result in eutectoid reactions and solid phase separation in the already present supersaturated or quasi-supersaturated structures, leading to the formation of TiNbV (BCC) -rich, ScZr (HCP) -rich, Sc (FCC) -rich and C4 (transition HCP) -rich structures.
TABLE 1 EDS data (at.%) for as-cast and hot extruded
The samples obtained in comparative example 1 and examples 1 to 8 were subjected to a room temperature tensile test. FIG. 4 is a graph of tensile engineering stress-strain curves at room temperature for the samples of comparative example 1 and examples 1-8, wherein the samples of comparative example 1 and examples 1-8 are labeled T1-T8, and Table 2 shows the results of performance tests at room temperature for the alloy samples obtained from comparative example 1 and examples 1-8.
TABLE 2 results of performance test at room temperature of alloy samples obtained in comparative example 1 and examples 1 to 8
As can be seen from the results in table 2, firstly, compared with the TiZrV alloy ingot in comparative example 1, after the Sc element is added in example 1, the yield strength and tensile strength of the ingot are both improved, which proves that the mechanical properties of the alloy material can be improved by the addition of the Sc element, and further, after the Nb element is continuously added in example 2, the yield strength and tensile strength of the alloy ingot are further improved, which indicates that the solid solution strengthening effect of the alloy is more obvious with the increase of the Nb element; although the mechanical properties of the cast ingot are good in the examples 1 and 2, the cast ingot cannot be applied to large-scale industrialization, and in order to expand the application range, in the example 3, casting is carried out on the basis of the example 2, and in the process of processing the cast ingot, compared with the cast ingot, certain mechanical loss is inevitable and reasonable in order to improve the industrial application of the cast ingot; furthermore, in example 4, the alloy material of example 3 is hot extruded, BCC, FCC and HCP phases are formed in the alloy, the yield strength and tensile strength of the alloy material are improved compared with those of example 3, and the plastic strain is also improved, i.e. the hot extrusion can improve the comprehensive mechanical properties of the alloy;
Influence of annealing on the material, Ti 22 Sc 22 Zr 22 Nb 17 V 17 The yield strength of the high-entropy alloy in an extrusion state, namely a sample T5 room temperature is 936MPa, and the yield strength of the high-entropy alloy after annealing at 400 ℃ (sample T6) reaches 957MPa, although the strength is slightly improved, the plasticity is obviously reduced. When the annealing temperature is gradually increased from 600 ℃ to 1000 ℃ (T7-T9), the plasticity of the sample is obviously improved by about 2 times compared with the extrusion state, and the tensile strength is not greatly changed. This indicates that long high temperature annealing is beneficial to improve tensile strength and plasticity. Meanwhile, the mechanical property of the material can be adjusted by annealing after the extrusion treatment, and the alloy with the required property can be obtained by selecting proper annealing temperature and annealing time according to the actual use requirement, for example, if the application environment with the requirements on tensile strength and plasticity is adopted, the high-temperature and long-time annealing treatment can be selected, such as 1000 ℃; if the requirement on plasticity is not great, the properties such as yield strength, tensile strength and the like are used in an important way, and annealing treatment can be carried out at a lower temperature, such as 400 ℃; according to the environment requirement, the mechanical property of the alloy material can be changed through annealing treatment, the alloy with the required target property can be obtained, the adjusting method is simple, the alloy property can be changed more flexibly, the alloy can be processed into a rod structure, and the application range of the alloy is further greatly widened. The theoretical density of the alloy is 5.412g/cm 3 And the alloy has high strength, can be used as a novel metal structure material to exert the advantage of high specific strength, and replaces the traditional aluminum alloy and steel to realize the aim of light weight of aerospace, ship, naval vessel and vehicle equipment.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (10)
1. The light high-temperature high-entropy alloy is characterized by comprising the following raw materials in atomic percentage: ti 22-25 at.%, Sc 22-25 at.%, Zr 22-25 at.%, Nb 0-17 at.%, V17-25 at.%.
2. The light-weight high-temperature high-entropy alloy according to claim 1, wherein the alloy consists of the following raw materials in atomic percent: ti 22 at.%, Sc 22 at.%, Zr 22 at.%, Nb 17 at.%, V17 at.%.
3. The lightweight, high temperature, high entropy alloy of claim 2, wherein the alloy forms BCC and HCP solid solution structures in an as-cast state, undergoes hot extrusion to become FCC, BCC and HCP solid solution structures, and is then annealed, whereby eutectoid or quasi-supersaturated structures in the matrix undergo eutectoid reaction and solid phase separation, resulting in the formation of BCC-rich, HCP-rich and FCC-rich structures.
4. The preparation process of the rod material of the light high-temperature high-entropy alloy according to claim 1, characterized by comprising the following steps:
respectively weighing the following raw materials in atomic percentage: ti 22-25 at.%, Sc 22-25 at.%, Zr 22-25 at.%, Nb 0-17 at.%, V17-25 at.%; smelting the weighed blocky Sc, Ti, V, Zr and Nb with the purity of more than or equal to 99.99 percent into alloy ingots; casting the alloy ingot into an alloy bar by a vacuum induction melting method; and extruding the alloy bar material into the alloy bar material by a hot consolidation press.
5. The preparation process of the rod material of the light high-temperature high-entropy alloy as claimed in claim 4, wherein the extrusion process is specifically as follows:
heating the alloy bar from room temperature to 900 ℃ under the inert gas atmosphere, carrying out heat preservation annealing for 24h, and cooling the alloy bar to room temperature by water; and then sealing the annealed alloy bar by using a steel sleeve to prepare a sealing element with the length of 10cm and the diameter of 50mm, preserving the temperature of the sealing element for 1h at 900 ℃, and then placing the sealing element in a corresponding die for extrusion at the extrusion speed of 25mm/s until all materials are extruded into the alloy bar.
6. The process for preparing a rod material of a light-weight high-temperature high-entropy alloy according to claim 5, wherein in the extrusion process, the temperature rise rate is 10 ℃/min.
7. The preparation process of the rod material of the light-weight high-temperature high-entropy alloy as claimed in claim 4, further comprising: under the atmosphere of inert gas, the temperature of the alloy rod is raised to 400-1000 ℃ from room temperature, then the annealing treatment is carried out, and finally furnace cooling or water cooling is carried out to the room temperature.
8. The process for preparing the rod material of the light-weight high-temperature high-entropy alloy as claimed in claim 7, wherein the heat-preserving annealing is carried out at 400-1000 ℃ for 24 h.
9. The process for preparing a rod material of a light-weight high-temperature high-entropy alloy according to claim 7, wherein when the alloy rod material is annealed, the temperature rise rate is 10 ℃/min.
10. The process for preparing a rod material of a light-weight high-temperature high-entropy alloy according to claim 4, wherein the diameter of the alloy rod material is 7-16mm, and the length of the alloy rod material is 30-100 cm.
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