CN116904828A - Second-phase reinforced high-entropy alloy and preparation method thereof - Google Patents
Second-phase reinforced high-entropy alloy and preparation method thereof Download PDFInfo
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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Abstract
A second-phase reinforced high-entropy alloy and a preparation method thereof belong to the technical field of metal materials. The high-entropy alloy takes CoCrNi as a matrix, and realizes the purpose of second phase strengthening through microalloying of two elements of Al and Nb. The atomic ratio expression of the high-entropy alloy is Co a Cr b Ni c Al d Nb e Subscripts correspond to the respective atomic percent contents of the alloying elements, wherein a=20 to 35, b=10 to 25, c=35 to 50, d=1 to 8, respectivelyE=1 to 8, a+b+c+d+e=100. The high-entropy alloy promotes massive submicron D0 by adjusting the element proportion of the CoCrNi matrix and adjusting the addition of trace element Nb 19 Phase formation, the high entropy alloy consisting essentially of an FCC phase and D0 19 Phase composition, nb-rich D0 19 The second phase is mainly distributed in FCC crystal boundary, the grain size can be controlled between several micrometers and tens micrometers by regulating the content of the second phase in the crystal boundary, the high-entropy alloy has good strength and plasticity, and the requirement of modern industry on the mechanical property of novel metal materials can be met.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to a second-phase reinforced high-entropy alloy and a preparation method thereof.
Background
The traditional alloy usually takes a single component as a main component, and the aim of regulating and controlling the performance is achieved by adding trace alloy elements (such as Ti-based alloy, al-based alloy, ni-based superalloy and the like). The high-entropy alloy is used as a new alloy which is developed recently, and is composed of five or more elements according to an equal atomic ratio or near equal atomic ratio, and the atomic percentage of each main element is generally 5% -35%. The configurational entropy is an important factor that makes high entropy alloys prone to form solid solutions with face-centered cubic structures (FCC), body-centered cubic structures (BCC) or close-packed hexagonal structures (HCP). The unique high entropy effect, delayed diffusion effect, lattice distortion effect and cocktail effect of the high entropy alloy lead the high entropy alloy to show excellent performances such as excellent low temperature plasticity, good wear resistance and corrosion resistance and good irradiation resistance. High entropy alloys of FCC structure typically have good plasticity at room temperature, but lower tensile strength; while the high-entropy alloy with the BCC or HCP structure has higher strength at room temperature, the plasticity is poor, and the engineering application of the high-entropy alloy is limited by the mismatch of strength and plasticity. Therefore, how to improve the tensile strength and the plasticity of the high-entropy alloy simultaneously so as to achieve excellent matching of the strength and the plasticity has important significance for engineering and industrialization of the high-entropy alloy in the future.
Most researches are now developing new high-entropy alloy systems, and research results of traditional metal materials show that micro-alloying can play a role in improving alloy structure and mechanical properties. And the research on how to regulate and control the structure of the novel high-entropy alloy through microalloying and improve the mechanical property at the same time is less. The second phase strengthening is an effective way of strengthening the high-entropy alloy, and the problems that the size of the second phase is difficult to control, the distribution of the second phase is uneven and the like still exist at present, so that the comprehensive performance of the existing high-entropy alloy needs to be further improved, and the preparation process of the existing high-entropy alloy needs to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the second-phase reinforced high-entropy alloy and the preparation method thereof, and the high-entropy alloy can realize that submicron Nb-rich second phases are uniformly distributed on a matrix to obviously reinforce the matrix, and the prepared high-entropy alloy has clear process route, strong repeatability, excellent mechanical property and strong safety and is expected to have excellent potential in the engineering application field.
A second-phase reinforced high-entropy alloy takes a CoCrNi medium-entropy alloy as a matrix, and realizes the purpose of second-phase reinforcement through microalloying of two elements of Al and Nb, wherein the atomic ratio expression of the high-entropy alloy is Co a Cr b Ni c Al d Nb e Subscripts correspond to the respective mole percentages of the alloying elements, wherein a=20at.% to 35at.%, b=10at.% to 25at.%, c=35at.% to 50at.%, d=1at.% to 8at.%, e=1at.% to 8at.%, and a+b+c+d+e=100deg.at.%.
Further, the second phase strengthening type high-entropy alloy Co a Cr b Ni c Al d Nb e The preferred composition of the alloy satisfies the following conditions: wherein a=25at.% to 30at.%, b=15at.% to 12at.%, c=44at.% to 48at.%, d=3at.% to 5at.%, and e=3at.% to 5at.%.
The preparation method of the second-phase reinforced high-entropy alloy is characterized by comprising the following specific preparation steps:
step one, preparing raw materials: according to the proportion of the designed components, the Co, cr, ni, al, nb element in the alloy components with the purity of more than 99.9 percent in the market is adopted for proportioning after oxide scale is removed;
step two, alloy smelting and homogenization treatment: in a smelting furnace protected by introducing argon, starting electromagnetic stirring, and repeatedly smelting after the prepared alloy raw materials are melted to obtain an initial alloy ingot; heating the master alloy ingot to a complete melting state under the protection of argon, and performing suction casting molding to obtain a high-entropy alloy ingot; under the protection of argon, placing the cast high-entropy alloy ingot into a muffle furnace for heat preservation and homogenization treatment;
step three, thermal deformation and cold deformation: carrying out thermal deformation on the homogenized alloy ingot at a certain temperature window; pickling and peeling the alloy ingot after thermal deformation, and then carrying out cold deformation;
step four, annealing and aging heat treatment: annealing heat treatment is carried out on the material after cold deformation, and then aging heat treatment is carried out to control D0 19 The size and distribution of the phases are used for obtaining the second-phase reinforced high-entropy alloy.
Further, in the second step, the smelting furnace is a vacuum arc smelting furnace or an induction smelting furnace; and performing alloy casting molding by suction casting of a vacuum arc melting furnace or casting of a vacuum induction melting furnace.
Further, the homogenization treatment in the second step is to preserve heat for more than 12 hours at 1150-1200 ℃, and water quenching is performed after the heat preservation is finished.
Further, in the step three, the thermal deformation process is that hot forging or hot rolling deformation is carried out at a temperature window of 1000-1200 ℃, and the deformation amount is 50-60%; and in the third step, cold rolling or drawing deformation is carried out at room temperature, and the deformation amount is 70-80%.
Further, the annealing treatment in the fourth step is water quenching after annealing for 0.5 to 4 hours at 800 to 1200 ℃; the aging treatment is water quenching after aging for 0-48 h at 500-900 ℃; the annealing treatment and the aging treatment are mainly used for controlling precipitation D0 19 The size and distribution of the phases, and the ageing treatment can be omitted according to the production requirements.
Further, the structure of the prepared high-entropy alloy mainly comprises FCC phase and bulk D0 rich in Nb 19 The second phase is formed, and the grain size can be controlled between a few micrometers and tens of micrometers by regulating precipitation and dissolution of the second phase at the grain boundary.
The technical key points of the invention are as follows:
the formation of Fe-rich equal second phases is completely eradicated on the tissue; and the CoCrNi is used as a matrix, so that the high strength and the excellent breaking elongation can be inherited.
The patent office website is issued with an invention patent with the application number of CN2017108248422.2, wherein the atomic percent of each element in the high-entropy alloy is Ni 30at percent to 42at percent, co 17at percent to 30at percent, fe 17at percent to 30at percent, cr10at percent to 20at percent, al 8at percent to 10at percent and Nb 1.0at percent to 4.5at percent. Wherein, ni is preferably 35at.% to 42at.%, and Nb is preferably 1.5at.% to 2at.%. "
In contrast, the invention reduces the aluminum content in the high-entropy alloy, improves the niobium content, removes the iron element in the alloy, greatly improves the performance of the high-entropy alloy, and respectively reaches 934MPa and 1323MPa when the elongation at break is more than 32%, and 1189MPa and 1454MPa when the elongation at break is 12.8%.
The reason for this is that the reduction of aluminum content, the increase of niobium content and the removal of iron element in the high-entropy alloy promote the massive submicron D0 19 The phase is evenly precipitated at the grain boundary, so that the grain size can be controlled between a few micrometers and tens of micrometers by regulating the content of the second phase at the grain boundary, and the alloy has the strengthening effects of solid solution strengthening, fine grain strengthening, dislocation strengthening, second phase particle precipitation strengthening and the like, thereby remarkably improving the mechanical properties of the high-entropy alloy.
Advantages of the invention
The invention adopts the unique proportioning of five-component CoCrNiAlNb, and obtains the second-phase reinforced high-entropy alloy through alloy smelting and homogenization, thermal deformation and cold deformation, annealing and aging heat treatment, the alloy is corrosion-resistant alloy, the higher Ni element content can effectively improve the solid solubility of the alloy to form an FCC matrix, and the formation of Fe-rich equal second phases is stopped on the tissue; and the CoCrNi is used as a matrix, so that the structure can inherit good strength and excellent breaking elongation, and the addition of trace element Nb promotes blockinessSubmicron D0 19 The phases are uniformly precipitated at the grain boundary, and the high-entropy alloy mainly comprises FCC phases and Nb-rich D0 19 The second phase is formed, the grain size can be controlled between a few microns and tens of microns by regulating the content of the second phase in the grain boundary, and the alloy has the strengthening effects of solid solution strengthening, fine grain strengthening, dislocation strengthening, second phase particle precipitation strengthening and the like, so that the mechanical property of the alloy can be remarkably improved; the alloy prepared by the method has the advantages of excellent and stable performance, simple preparation flow, strong safety, moderate price of alloy raw materials and very good prospect of being applied as a structural component in the field of engineering application.
Drawings
Fig. 1 is an SEM tissue diagram of the high-entropy alloy 1 prepared in example 1 of the present invention.
Fig. 2 is an SEM tissue diagram of the high-entropy alloy 2 prepared in example 2 of the present invention.
Fig. 3 is an SEM tissue diagram of the high-entropy alloy 3 prepared in example 3 of the present invention.
FIG. 4 is a graph showing the static tensile engineering stress-strain curves of the high-entropy alloys 1 to 3 prepared in examples 1 to 3 according to the present invention.
Detailed Description
Example 1
Step one, the preparation component is Co 27 Cr 18 Ni 45 Al 5 Nb 5 (at%) alloy, wherein the footmark of each element is the atomic percent of each element, and smelting in a vacuum arc smelting furnace with argon atmosphere to obtain a high-entropy alloy master alloy ingot; placing the smelted master alloy ingot above a suction casting die, and performing suction casting molding in a vacuum arc melting furnace with argon atmosphere to obtain a high-entropy alloy suction cast ingot; and (3) carrying out vacuum tube sealing on the high-entropy alloy suction cast ingot, filling argon, homogenizing at 1200 ℃ for 12 hours, and then carrying out water quenching.
Step two, hot rolling and thinning the cast ingot subjected to homogenization treatment by 60% at the initial temperature of 1150 ℃; and (3) removing the oxide skin, and then rolling and thinning at room temperature to obtain the high-entropy alloy cold-rolled sheet. Step three, carrying out water quenching on the cold-rolled plate after heat preservation for 1h at 950 ℃ to obtain a high-entropy alloy 1; step four, the high-entropy alloy 1 sheet is processed by an electric spark processing methodDog bone-shaped tensile specimens having a thickness of about 1mm were cut out, and the gauge length, width and thickness of the tensile specimens were 10mm,3mm and 1mm, respectively, using a common tester (CMT 4305) at 1X 10 -3 s -1 Static tensile testing was performed at a fixed strain rate.
Experimental test analysis:
experiments show that the high-entropy alloy 1 prepared in the embodiment is mainly composed of FCC phase and Nb-rich D0 as shown in an SEM (scanning electron microscope) tissue diagram of FIG. 1 19 The phase is constituted and the FCC grains are of an incompletely recrystallized structure. From the tensile test results of FIG. 4, the high-entropy alloy 1 has a yield strength of 1189MPa, a tensile strength of 1454MPa, and an elongation at break of 12.8%.
Example 2
Step one, the preparation component is Co 27 Cr 18 Ni 45 Al 5 Nb 5 (at%) alloy, wherein the footmark of each element is the atomic percent of each element, and smelting in a vacuum arc smelting furnace with argon atmosphere to obtain a high-entropy alloy master alloy ingot; placing the smelted master alloy ingot above a suction casting die, and performing suction casting molding in a vacuum arc melting furnace with argon atmosphere to obtain a high-entropy alloy suction cast ingot; and (3) carrying out vacuum tube sealing on the high-entropy alloy suction cast ingot, filling argon, homogenizing at 1200 ℃ for 12 hours, and then carrying out water quenching.
Step two, hot rolling and thinning the cast ingot subjected to homogenization treatment by 60% at the initial temperature of 1150 ℃; and (3) removing the oxide skin, and then rolling and thinning at room temperature to obtain the high-entropy alloy cold-rolled sheet. Step three, carrying out water quenching on the cold-rolled plate after heat preservation for 1h at 1100 ℃ to obtain a high-entropy alloy 2; cutting a dog-bone-shaped tensile sample with the thickness of about 1mm from the high-entropy alloy 2 sheet by an electric spark machining method, wherein the length, the width and the thickness of a gauge length of the tensile sample are 10mm,3mm and 1mm respectively, and a common testing machine (CMT 4305) is adopted to carry out the test at the speed of 1X 10 -3 s -1 Static tensile testing was performed at a fixed strain rate.
Experimental test analysis:
the high-entropy alloy 2 prepared in this example was subjected to experimental detection, and as can be seen from the SEM tissue diagram of fig. 2,the high-entropy alloy 2 prepared by the method mainly comprises FCC phase and Nb-rich D0 19 The phase is constituted and the FCC grains are fully recrystallized. As can be seen from the tensile test results of FIG. 4, the high-entropy alloy 2 has a yield strength of 553MPa, a tensile strength of 1022MPa, and an elongation at break of 37.3%.
Example 3
Step one, the preparation component is Co 28 Cr 19 Ni 46 Al 3.5 Nb 3.5 (at%) alloy, wherein the footmark of each element is the atomic percent of each element, and smelting in a vacuum arc smelting furnace with argon atmosphere to obtain a high-entropy alloy master alloy ingot; placing the smelted master alloy ingot above a suction casting die, and performing suction casting molding in a vacuum arc melting furnace with argon atmosphere to obtain a high-entropy alloy suction cast ingot; and (3) carrying out vacuum tube sealing on the high-entropy alloy suction cast ingot, filling argon, homogenizing at 1200 ℃ for 12 hours, and then carrying out water quenching.
Step two, hot rolling and thinning the cast ingot subjected to homogenization treatment by 60% at the initial temperature of 1150 ℃; and (3) removing the oxide skin, and then rolling and thinning at room temperature to obtain the high-entropy alloy cold-rolled sheet. Step three, carrying out water quenching on the cold-rolled plate after heat preservation for 1h at 1100 ℃, and then carrying out water quenching after aging for 24h at 700 ℃ to obtain a high-entropy alloy 3;
cutting a dog-bone-shaped tensile sample with the thickness of about 1mm from the high-entropy alloy 3 sheet by an electric spark machining method, wherein the length, the width and the thickness of a gauge length of the tensile sample are 10mm,3mm and 1mm respectively, and a common testing machine (CMT 4305) is adopted to carry out the test at the speed of 1X 10 -3 s -1 Static tensile testing was performed at a fixed strain rate.
Experimental test analysis:
experiments show that the high-entropy alloy 3 prepared in the embodiment mainly comprises FCC phase and is rich in Nb D0 as shown in SEM organization chart of FIG. 3 19 The second phase is substantially redissolved at 1100 ℃ and FCC grains follow D0 19 The phase dissolves back and grows. From the tensile test results of FIG. 4, it is found that the high-entropy alloy 3 has a yield strength of 934MPa, a tensile strength of 1323MPa, and an elongation at break of 35.2%.
In conclusion, the second-phase reinforced high-entropy alloy and the preparation method thereof are simple and feasible, the second-phase reinforced high-entropy alloy obtained by the method is excellent and stable in performance, simple in preparation process, high in safety, and very expected to be applied as a structural component in the field of engineering application, and the used raw materials are nontoxic and harmless, moderate in price and low in industrial investment.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the scope of the embodiments described above. All changes, substitutions and modifications which may be made without departing from the spirit of the invention are intended to be within the scope of the invention.
Claims (8)
1. A second-phase reinforced high-entropy alloy is characterized in that the high-entropy alloy takes a CoCrNi medium-entropy alloy as a matrix, the purpose of second-phase reinforcement is realized through microalloying of two elements of Al and Nb, and the atomic ratio expression of the high-entropy alloy is Co a Cr b Ni c Al d Nb e Subscripts correspond to the respective mole percentages of the alloying elements, wherein a=20at.% to 35at.%, b=10at.% to 25at.%, c=35at.% to 50at.%, d=1at.% to 8at.%, e=1at.% to 8at.%, and a+b+c+d+e=100deg.at.%.
2. The second-phase strengthened high-entropy alloy of claim 1, wherein: second phase strengthened high entropy alloy Co a Cr b Ni c Al d Nb e The alloy composition satisfies the following conditions: wherein a=25at.% to 30at.%, b=15at.% to 12at.%, c=44at.% to 48at.%, d=3at.% to 5at.%, and e=3at.% to 5at.%.
3. The method for producing a second-phase strengthened high-entropy alloy according to claim 1 or 2, characterized by comprising the steps of:
step one, preparing raw materials: according to the proportion of the designed components, the Co, cr, ni, al, nb element in the alloy components with the purity of more than 99.9 percent in the market is adopted for proportioning after oxide scale is removed;
step two, alloy smelting and homogenization treatment: in a smelting furnace protected by introducing argon, starting electromagnetic stirring, and repeatedly smelting after the prepared alloy raw materials are melted to obtain an initial alloy ingot; heating the master alloy ingot to a complete melting state under the protection of argon, and performing suction casting molding to obtain a high-entropy alloy ingot; under the protection of argon, placing the cast high-entropy alloy ingot into a muffle furnace for heat preservation and homogenization treatment;
step three, thermal deformation and cold deformation: carrying out thermal deformation on the homogenized alloy ingot at a certain temperature window; pickling and peeling the alloy ingot after thermal deformation, and then carrying out cold deformation;
step four, annealing and aging heat treatment: annealing heat treatment is carried out on the material after cold deformation, and then aging heat treatment is carried out to control D0 19 The size and distribution of the phases are used for obtaining the second-phase reinforced high-entropy alloy.
4. The method of producing a second-phase strengthened high-entropy alloy according to claim 2, wherein: the smelting furnace in the second step is a vacuum arc smelting furnace or an induction smelting furnace; and performing alloy casting molding by suction casting of a vacuum arc melting furnace or casting of a vacuum induction melting furnace.
5. The method of producing a second-phase strengthened high-entropy alloy according to claim 2, wherein: and step two, the homogenization treatment is carried out at 1150-1200 ℃ for more than 12 hours, and water quenching is carried out after the heat preservation is finished.
6. The method of producing a second-phase strengthened high-entropy alloy according to claim 2, wherein: the thermal deformation process in the third step is to perform hot forging or hot rolling deformation at a temperature window of 1000-1200 ℃, wherein the deformation amount is 50-60%; and in the third step, cold rolling or drawing deformation is carried out at room temperature, and the deformation amount is 70-80%.
7. Preparation of the second-phase strengthened high-entropy alloy according to claim 2The method is characterized in that: the annealing treatment in the fourth step is water quenching after annealing for 0.5 to 4 hours at 800 to 1200 ℃; the aging treatment is water quenching after aging for 0-48 h at 500-900 ℃; the annealing treatment and the aging treatment are mainly used for controlling precipitation D0 19 The size and distribution of the phases, and the ageing treatment can be omitted according to the production requirements.
8. The method for producing a second-phase strengthened high-entropy alloy according to claim 2, wherein the structure of the high-entropy alloy produced is mainly composed of an FCC phase and a bulk D0 rich in Nb 19 The second phase is formed, and the grain size can be controlled between a few micrometers and tens of micrometers by regulating precipitation and dissolution of the second phase at the grain boundary.
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