CN113025865B - Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy - Google Patents
Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy Download PDFInfo
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Abstract
The invention belongs to the technical field of metal materials, and particularly discloses a preparation method of an AlCoCrFeNi series two-phase structure high-entropy alloy. Wherein, the content of the in-situ autogenous face-centered cubic phase is increased, and the plasticity of the body-centered cubic-based high-entropy alloy is effectively improved. The method is different from the method of directly introducing the FCC phase by adjusting the components, avoids complex processing technology, can obtain the comprehensive mechanical property with high strength and high plasticity by only carrying out simple heat treatment on the as-cast alloy, not only improves the processability of the alloy, but also has great practical application potential.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to a preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy.
Background
The high-entropy alloy is one of hot spots in the research field of metal materials in recent years, generally consists of multiple elements in equal atomic ratio or near equal atomic ratio, has large development space and strong designability. It has been found that the high-entropy alloy has excellent properties of high strength, high hardness, good wear resistance and corrosion resistance, excellent low-temperature performance, irradiation resistance, high-temperature softening resistance and the like, and is a novel metal structure material with great development potential.
Due to the contradictory relationship between strength and plasticity, developing advanced materials with both high strength and high plasticity has been a challenging research focus, including high-entropy alloys. Despite the chemical disorder of the high entropy alloy atomic arrangement, the crystal structure is clear, and the Face Centered Cubic (FCC) and Body Centered Cubic (BCC) are common. Among them, the FCC type high-entropy alloy has low strength but good plasticity, while the BCC type high-entropy alloy generally has extremely high strength and hardness but poor plasticity and work hardening capability, which severely limits its practical application.
Researches show that the classical dislocation theory is still suitable for mechanical property analysis and regulation of the high-entropy alloy. In general, plastic deformation of FCC and BCC crystals proceeds mainly by dislocation glide. Under the condition of smaller stress, the dislocation can start along the closest arrangement surface, and various methods can be adopted to block the dislocation motion to realize alloy strengthening, including solid solution strengthening, fine crystal strengthening, second phase strengthening and the like. In addition, the mechanical property of the FCC high-entropy alloy can be improved through mechanisms such as deformation phase transformation (TRIP effect) or deformation twin crystal (TWIP effect) in a strain process.
However, although the slip system of BCC crystals is not less (sometimes more) than that of FCC crystals, the slip resistance is large because the slip direction per slip plane is small and the close packing plane atomic density and the plane spacing are also small. Considering the effect of grain boundary in alloy, even under the action of higher stress, large-area dislocation cooperative sliding between grains is difficult to realize, and local stress concentration occurs at the early stage of deformation to cause material instability, which is the root cause of high strength and poor plasticity of the BCC high-entropy alloy. That is, the key of the plasticity improvement of the BCC high-entropy alloy is to effectively delay the early stress during deformationThe force is concentrated. At present, the effective method comprises the steps of directly obtaining as-cast high-entropy alloy with FCC and BCC dual-phase structures by regulating and controlling alloy components, however, dendritic crystal growth and element segregation in the solidification process can cause the as-cast alloy microstructure to be uneven, the process is difficult to control, and the alloy strength can be obviously reduced while the alloy plasticity is improved; the eutectic high-entropy alloy better solves the problem of component segregation, can obtain a FCC and BCC two-phase layered eutectic structure, has strain mainly concentrated in a soft FCC phase region during deformation, and has good comprehensive mechanical properties, such as AlCoCrFeNi2.1(ii) a By adjusting the stability of BCC phase, the local stress concentration in the deformation process is relieved based on a mode of strain-induced phase transformation, and the plasticity of the alloy is improved, such as insoluble Ti35Zr27.5Hf27.5NbTa5And TaxHfZrTi; by introducing small-sized interstitial atoms such as oxygen elements, a nanostructure ordered oxygen complex completely coherent with the matrix is formed, so that a dislocation slip mode is changed from plane slip to wave slip mainly based on cross slip, dislocation proliferation and uniform deformation are promoted, and alloy plasticity is improved; the BCC with a completely coherent interface and a fine crystal structure of ordered body-centered cubic phase (B2) are obtained through regulation, the dislocation motion and the formation of cracks are hindered, and the strength and the plasticity of the alloy are improved. At present, the plasticity of the alloy can be improved by eutectic high-entropy structure, TRIP effect, interstitial solid solution and the like.
The literature (A.Munitz, S.Salhov, S.Hayun, N.Frage, Heat treatment images of the micro-structure and mechanical properties of AlCoCrFeNi high entry alloy, Journal of Alloys and Compounds,2016,683:221-230.) reports that the dendrite region and the intergranular region of the equiatomic ratio AlCoCrFeNi high entropy alloy undergo significant phase transformation during Heat treatment, the compressive elongation of the alloy in the Heat treatment state is increased, but the elongation of the alloy during tensile testing is poor because the alloy still shows a fine crystalline structure (containing nano-sedimentary phase).
The research object of the method is the as-cast high-entropy alloy, and the universality and the systematicness of the method need further intensive research. In fact, the high-entropy alloy takes dozens of metal elements as main component sources, the properties of the organization structure and the phase are different, and the designability is extremely strong, so that the research of diversified plastic regulation schemes is very necessary.
Disclosure of Invention
The invention aims to provide a preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy, which aims to solve the problems in the prior art.
According to the invention, through a heat treatment process, the microstructure of the alloy is regulated and controlled by using metastable state phase transition, and the plasticity of the body-centered cubic-based high-entropy alloy is effectively improved. The method is different from the method of directly introducing FCC phase by adjusting components, avoids complex treatment process, can obtain high-strength and high-plasticity comprehensive mechanical property by simply carrying out heat treatment on the as-cast alloy, not only improves the processability of the alloy, but also has great practical application potential.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy, which comprises the following steps:
firstly, preparing a high-entropy alloy ingot by adopting a vacuum arc melting method, then preparing the high-entropy alloy ingot into a high-entropy alloy casting bar by adopting a vacuum melting and pouring method, and carrying out heat treatment for 1-3 hours at the temperature of 1000-1200 ℃ to regulate and control the microstructure of the high-entropy alloy casting bar, thus obtaining the AlCoCrFeNi series dual-phase structure high-entropy alloy in a heat treatment state.
The high-entropy alloy ingot is AlCoCrFeNi series high-entropy alloy, and the high-entropy alloy ingot comprises the following components in atomic percentage: co: 20.91-22.31 wt%, Cr: 18.45-19.68 wt%, Fe: 19.82-21.14 wt%, Ni: 26.66 to 31.24 weight percent, and the balance of Al, wherein the sum of the atomic percentages of the components is 100 percent.
When AlCoCrFeNi high-entropy alloy is subjected to heat treatment, the disordered body-centered cubic phase can be decomposed into a sigma phase and a face-centered cubic phase at the temperature of more than 600 ℃, and the sigma phase can be decomposed into an FCC phase and a B2 phase again at the temperature of more than 950 ℃. Generally, topologically close-packed sigma phases are one of the most common intermetallic compounds that can improve alloy strength, but can significantly reduce alloy plasticity. However, if the sigma phase is only a transition phase and can be decomposed to precipitate a soft FCC phase by heat treatment, the plasticity of the BCC-based high-entropy alloy can be improved.
As further optimization of the invention, the preparation of the high-entropy alloy ingot by adopting the vacuum arc melting method specifically comprises the following steps:
(a) weighing metal raw materials according to a proportion, and putting the metal raw materials into a groove of a water-cooling copper mold in a vacuum arc melting furnace;
(b) vacuumizing the arc melting furnace to 3 x 10-3Pa, filling protective gas to 1.6 × 103Pa, repeating the process for 5 times to fully remove oxygen in the furnace cavity;
(c) melting high-purity metal by adopting a vacuum arc melting process to obtain an ingot, turning the ingot and then melting again, repeating the process for 5 times, cooling, polishing by using abrasive paper, ultrasonically cleaning by using absolute ethyl alcohol, and drying to obtain the high-entropy alloy ingot.
As further optimization of the invention, the method for preparing the high-entropy alloy cast ingot into the high-entropy alloy cast rod by adopting the vacuum melting and pouring method specifically comprises the following steps:
(1) placing the high-entropy alloy cast ingot on a casting mold in a vacuum arc melting furnace;
(2) vacuumizing the arc melting furnace to 3 x 10-3Pa, filling protective gas to 1.6 × 103Pa, repeating the process for 5 times to fully remove oxygen in the furnace cavity;
(3) and melting the high-entropy alloy cast ingot by adopting a vacuum arc melting process, wherein the current is 280A, and the molten cast ingot spontaneously flows into a copper mold and is cooled to obtain the high-entropy alloy cast rod.
As a further optimization of the present invention, the heat treatment process specifically includes the following steps:
and (3) putting the high-entropy alloy cast rod into a vacuum atmosphere furnace for heat treatment and air cooling to obtain the thermal treatment AlCoCrFeNi series two-phase structure high-entropy alloy.
As a further optimization of the invention, the current of the vacuum arc melting process in the step (b) is 150-280A, wherein the current is controlled to be 150-180A for slowly melting high-purity metal in the 1 st melting, and the current is controlled to be 250-280A in the 2 nd-5 th melting.
As a further optimization of the invention, the drying temperature in the step (c) is 50-80 ℃.
As a further optimization of the present invention, the shielding gas is high purity argon.
As a further optimization of the invention, the vacuum atmosphere furnace is an argon atmosphere.
The high-entropy alloy cast rod is represented by a coarse dendritic structure and mainly consists of an ordered body-centered cubic phase and a disordered body-centered cubic phase. In the heat treatment process, the disordered body-centered cubic phase is transformed into the ordered body-centered cubic phase and the face-centered cubic phase, the microstructure is changed, and the coarse dendritic crystal structure disappears and is transformed into a two-phase network structure consisting of the face-centered cubic phase and the body-centered cubic phase. The in-situ autogenous face-centered cubic phase content is increased, the plasticity of the AlCoCrFeNi series high-entropy alloy with the dual-phase structure in the heat treatment state is obviously improved, the elongation can be improved from 1.3 percent to 8.5 percent, the breaking strength is slightly reduced, and the comprehensive mechanical property is good.
The invention discloses the following technical effects:
the invention provides a preparation method of an AlCoCrFeNi series dual-phase structure high-entropy alloy, which is characterized in that the microstructure of a body-centered cubic base as-cast high-entropy alloy is directly regulated and controlled through a high-temperature heat treatment process, so that the plasticity of the alloy is obviously improved, higher strength is reserved, and the heat-treated AlCoCrFeNi series dual-phase structure high-entropy alloy with good comprehensive mechanical properties is obtained. The method provided by the invention improves the microstructure of the BCC-based as-cast high-entropy alloy through a simple heat treatment process, can effectively improve the phenomenon of nonuniform structure caused by element segregation in the solidification process, and is beneficial to preparing large-size high-performance high-entropy alloy structural materials.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a structural analysis diagram of a high-entropy alloy cast rod prepared in example 1, wherein a is a microstructure observation diagram of the high-entropy alloy cast rod, and b is a partial enlarged diagram;
FIG. 2 shows the microstructure and phase analysis results of the 650 ℃ heat-treated AlCoCrFeNi-based two-phase structure high-entropy alloy obtained in comparative example 1. Wherein a is an observation image of a microstructure of the heat-treated high-entropy alloy, B is a transmission electron microscope image of a dendritic crystal region, c is an electron diffraction image corresponding to the structure of the B image, d is a transmission electron microscope image of an intercrystalline region, e is an electron diffraction image of a B2 phase in d, and f is an electron diffraction image of an FCC phase in d;
FIG. 3 is a structural analysis chart of a 1100 ℃ heat-treated AlCoCrFeNi-based two-phase high-entropy alloy obtained in example 1. Wherein a is a microstructure picture, and b is a partial enlarged view;
FIG. 4 shows the transmission electron microscope analysis results of the microstructure of the 1100 ℃ heat-treated AlCoCrFeNi-based high-entropy alloy with a two-phase structure obtained in example 1. Wherein a is a microstructure diagram, B is a B2 phase electron diffraction diagram in a, and c is an FCC phase electron diffraction diagram in a;
FIG. 5 is a differential thermal analysis result of the high-entropy alloy cast rod obtained in step (5) of example 1, which includes two temperature increase and decrease cycle test curves;
FIG. 6 shows XRD diffraction patterns of the high-entropy alloy cast bar obtained in example 1, the AlCoCrFeNi series high-entropy alloy having a two-phase structure in a heat-treated state at 1100 deg.C, and the AlCoCrFeNi series high-entropy alloy having a two-phase structure in a heat-treated state at 650 deg.C obtained in comparative example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
(1) High-purity metals with the purity of 99.99 percent are selected as raw materials, including aluminum, cobalt, chromium, iron and nickel, according to the following ratio of Co: 20.91 wt.%, Cr: 18.45 wt.%, Fe: 19.82 wt.%, Ni: 31.24 wt.% and the balance of Al, placing the corresponding metal in a copper crucible of vacuum arc melting equipment, and vacuumizing the arc melting furnace to 3 x 10 by sequentially adopting a mechanical pump and a molecular pump-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, the process was repeated 5 times to sufficiently remove oxygen from the furnace chamber.
(2) The high-purity metal is smelted by adopting a vacuum arc smelting process to obtain an ingot, the ingot is turned over by a mechanical arm in the process and then smelted again, and the operation is repeated for 5 times to ensure that the alloy components are uniform. And in the 1 st smelting, the current is controlled to be 170A to slowly melt the high-purity metal, and in the 2 nd to 5 th smelting, the current is controlled to be 280A.
(3) Removing an oxide layer on the surface of the high-entropy alloy cast ingot by using sand paper, ultrasonically cleaning by using absolute ethyl alcohol, and drying at 70 ℃.
(4) Placing the high-entropy alloy cast ingot subjected to surface treatment on a casting mold in a vacuum arc melting furnace, and vacuumizing the arc melting furnace to 3 multiplied by 10 by adopting a mechanical pump and a molecular pump in sequence-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, the process was repeated 5 times to sufficiently remove oxygen from the furnace chamber.
(5) And melting the high-entropy alloy cast ingot by adopting a vacuum arc melting process, wherein the current is 280A, and the molten cast ingot spontaneously flows into a copper mold to obtain the high-entropy alloy cast rod.
(6) Putting the high-entropy alloy cast rod into a vacuum atmosphere furnace, firstly vacuumizing to below 10Pa, introducing argon for 30 minutes to remove oxygen, carrying out heat preservation and heat treatment at 1100 ℃ for 3 hours, taking out and air-cooling to obtain the AlCoCrFeNi series two-phase structure high-entropy alloy in the heat treatment state.
Comparative example 1
The preparation method is the same as that of example 1, except that the heat preservation heat treatment temperature in the step (6) is 650 ℃, and the AlCoCrFeNi series two-phase structure high-entropy alloy in the heat treatment state is obtained.
Experimental example 1
The microstructure of the high-entropy alloy cast rod obtained in step 5 of example 1 was observed, and the result is shown in FIG. 1. Wherein, fig. 1b is an enlarged view of the white square area in fig. 1 a. As shown in FIG. 1, the as-cast high-entropy alloy is a typical dendritic structure, the dendritic region is a two-phase nanostructure, and the intergranular region is dominated by the FCC phase.
The microstructure of the 650 ℃ heat-treated AlCoCrFeNi-based two-phase structure high-entropy alloy obtained in comparative example 1 was observed, and the result is shown in FIG. 2. As can be seen from FIG. 2a, the dendrite region of the alloy in the 650 ℃ heat-treated state precipitates a new flocculent phase, which is the FCC phase. Fig. 2B & c demonstrate that the dendritic region consists primarily of disordered BCC and ordered B2 nano-biphase, which is consistent with the as-cast alloy dendritic region (see fig. 1B). FIG. 2d shows the microstructure of the interdendritic region, consisting of ordered B2 phase and FCC phase, the corresponding electron diffraction patterns of the two phases being shown in FIGS. 2e & f.
The microstructure of the 1100 ℃ heat-treated AlCoCrFeNi-based two-phase high-entropy alloy obtained in example 1 was observed, and the results are shown in FIG. 3. As can be seen from FIG. 3, the AlCoCrFeNi series high-entropy alloy with the two-phase structure in the high-temperature heat treatment state is a two-phase structure and consists of two phases of FCC and B2, and the corresponding electron diffraction patterns of the microstructure and the phase of the transmission electron microscope are shown in FIG. 4. Therefore, the cast body-centered cubic high-entropy alloy can be converted into a two-phase structure after high-temperature heat treatment.
The differential thermal analysis of the high-entropy alloy cast rod obtained in the step (5) of example 1 is carried out, and the result is shown in fig. 5, and the comparison of the two temperature rise curves shows that the alloy does have irreversible solid-state phase transition behavior near 600 ℃ in the temperature rise process. This is consistent with the results of fig. 2, where the dendritic region of the 650 ℃ hot worked alloy precipitates the FCC phase.
XRD diffraction analysis was performed on the high-entropy alloy cast bar (As-cast) obtained in example 1, the AlCoCrFeNi series high-entropy alloy having the two-phase structure in the heat-treated state at 1100 deg.C, and the AlCoCrFeNi series high-entropy alloy having the two-phase structure in the heat-treated state at 650 deg.C obtained in comparative example 1, respectively, and the results are shown in FIG. 6. As is clear from FIG. 6, the 650 ℃ heat-treated AlCoCrFeNi-based two-phase structure high-entropy alloy obtained in comparative example 1 had sigma phase precipitation. Compared with a high-entropy alloy cast rod and a 650 ℃ heat treatment state AlCoCrFeNi series high-entropy alloy with a two-phase structure, the diffraction peak relative strength of the FCC phase of the 1100 ℃ heat treatment state AlCoCrFeNi series high-entropy alloy with a two-phase structure is enhanced, which shows that the content of the FCC phase of the 1100 ℃ heat treatment state AlCoCrFeNi series high-entropy alloy obtained in example 1 is increased. This is consistent with microstructure analysis, the high entropy alloy cast rod is BCC dendritic structure morphology (figure 1), after 1100 ℃ heat treatment, the dendritic structure morphology disappears, and the alloy is converted into FCC + B2 two-phase structure.
Wherein the diffraction spots marked with white circles in fig. 2c & e and fig. 4B correspond to the diffraction of the (100) crystal plane of ordered B2.
From the above, after the BCC-based AlCoCrFeNi high-entropy alloy is subjected to high-temperature heat treatment, on one hand, the alloy microstructure is changed from a typical dendritic structure into a more uniform dual-phase structure, on the other hand, the content of the FCC phase of the alloy is increased, the FCC phase is more prone to plane dislocation slip, and finally, the plasticity of the alloy is improved.
Example 2
The specific process was the same as in example 1 except that the heat treatment time in step (6) was 2 hours.
Example 3
The specific process was the same as in example 1 except that the heat treatment time in step (6) was 1 hour.
Example 4
The specific process was the same as example 1 except that the heat treatment temperature in step (6) was 1000 ℃ and the heat treatment time was 2 hours.
Experimental example 2
Mechanical property tests were performed on the as-cast high-entropy alloy cast bar prepared in the step (5) of example 1 and the heat-treated AlCoCrFeNi-based two-phase structure high-entropy alloys prepared in examples 1 to 4, and the results are shown in table 1. As can be seen from Table 1, the plasticity of the body-centered cubic AlCoCrFeNi system as-cast high-entropy alloy can be effectively improved by heat treatment, the elongation can be improved from 1.3% to 8.5%, and the method can be used for preparing a metal structure material with large size and good comprehensive mechanical properties.
TABLE 1
Example 5
(1) High-purity metals with the purity of 99.99 percent are selected as raw materials, including aluminum, cobalt, chromium, iron and nickel, according to the following ratio of Co: 21.36 wt.%, Cr: 18.85 wt.%, Fe: 20.24 wt.%, Ni: 29.78 wt.%, the balance being Al, placing the corresponding metal in a copper crucible of vacuum arc melting equipment, and vacuumizing the arc melting furnace to 3 × 10 by sequentially adopting a mechanical pump and a molecular pump-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, the process was repeated 5 times to sufficiently remove oxygen from the furnace chamber.
(2) The high-purity metal is smelted by adopting a vacuum arc smelting process to prepare the high-entropy alloy ingot, the ingot is turned over by a mechanical arm in the process and then smelted again, and the operation is repeated for 5 times to ensure that the alloy components are uniform. Wherein, during the 1 st smelting, the current is controlled to be 160A to slowly melt the high-purity metal, and during the 2 nd to 5 th smelting, the current is controlled to be 270A.
(3) Removing an oxide layer on the surface of the high-entropy alloy cast ingot by using sand paper, ultrasonically cleaning by using absolute ethyl alcohol, and drying at 80 ℃.
(4) Placing the high-entropy alloy cast ingot subjected to surface treatment on a casting mold in a vacuum arc melting furnace, and vacuumizing the arc melting furnace to 3 multiplied by 10 by adopting a mechanical pump and a molecular pump in sequence-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, the process was repeated 5 times to sufficiently remove oxygen from the furnace chamber.
(5) And melting the high-entropy alloy cast ingot by adopting a vacuum arc melting process, wherein the current is 280A, and the molten cast ingot spontaneously flows into a copper mold to obtain the high-entropy alloy cast rod.
(6) Putting the high-entropy alloy cast rod into a vacuum atmosphere furnace, firstly vacuumizing to below 10Pa, introducing argon for 30 minutes to remove oxygen, carrying out heat preservation and heat treatment at 1100 ℃ for 2 hours, taking out and air-cooling to obtain the AlCoCrFeNi series two-phase structure high-entropy alloy in the heat treatment state.
Example 6
The specific process was the same as example 5 except that the heat treatment time in step (6) was 3 hours.
Example 7
The specific process is the same as example 5 except that the heat treatment temperature in step (6) is 1200 ℃ and the time is 1 hour.
Experimental example 3
Mechanical property tests were performed on the high-entropy alloy cast rod prepared in the step (5) of example 5 and the thermally-treated AlCoCrFeNi-based two-phase structure high-entropy alloy prepared in examples 5 to 7, and the results are shown in Table 2.
TABLE 2
Example 8
(1) High-purity metals with the purity of 99.99 percent are selected as raw materials, including aluminum, cobalt, chromium, iron and nickel, according to the following ratio of Co: 22.31%, Cr: 19.68%, Fe: 21.24%, Ni: 26.6Weighing corresponding metals in a proportion of 6 percent and the balance of Al, placing the metals in a copper crucible of vacuum arc melting equipment, and vacuumizing an arc melting furnace to 3 multiplied by 10 by adopting a mechanical pump and a molecular pump in sequence-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, the process was repeated 5 times to sufficiently remove oxygen from the furnace chamber.
(2) The high-purity metal is smelted by adopting a vacuum arc smelting process to prepare the high-entropy alloy ingot, the ingot is turned over by a mechanical arm in the process and then smelted again, and the operation is repeated for 5 times to ensure that the alloy components are uniform. And in the 1 st smelting, the current is controlled to be 150A to slowly melt the high-purity metal, and in the 2 nd to 5 th smelting, the current is controlled to be 280A.
(3) Removing an oxide layer on the surface of the high-entropy alloy cast ingot by using sand paper, ultrasonically cleaning by using absolute ethyl alcohol, and drying at 50 ℃.
(4) Placing the high-entropy alloy cast ingot subjected to surface treatment on a casting mold in a vacuum arc melting furnace, and vacuumizing the arc melting furnace to 3 multiplied by 10 by adopting a mechanical pump and a molecular pump in sequence-3Pa, filling high-purity argon to 1.6 multiplied by 103Pa, repeating the process for 5 times to fully remove oxygen in the furnace cavity;
(5) and melting the high-entropy alloy cast ingot by adopting a vacuum arc melting process, wherein the current is 280A, and the molten cast ingot spontaneously flows into a copper mold to obtain the high-entropy alloy cast rod.
(6) Putting the high-entropy alloy cast rod into a vacuum atmosphere furnace, firstly vacuumizing to below 10Pa, introducing argon for 30 minutes to remove oxygen, carrying out heat preservation and heat treatment at 1100 ℃ for 2 hours, taking out and air-cooling to obtain the AlCoCrFeNi series two-phase structure high-entropy alloy in the heat treatment state.
Example 9
The specific process was the same as in example 8 except that the heat treatment time was 3 hours.
Example 10
The specific process was the same as example 8 except that the heat treatment temperature was 1200 ℃ and the heat treatment time was 2 hours.
Experimental example 4
Mechanical property tests were performed on the high-entropy alloy cast rod prepared in the step (5) of example 8 and the thermally-treated AlCoCrFeNi-based two-phase structure high-entropy alloy prepared in examples 8 to 10, and the results are shown in Table 3.
TABLE 3
Comparative example 2
This example is based on the document "Ultrafine-grained dual phase Al0.45CoCrFeNi high-entry alloys, J.Hou, X.Shi, J.Qiao, Y.Zhang, P.K.Liaw, Y.Wu, Materials and Design, 2019' discloses that an as-cast alloy is obtained through a vacuum arc melting and casting process, and is subjected to homogenization treatment at 1250 ℃ for 5 hours to obtain Al with FCC and BCC dual-phase structures0.45CoCrFeNi high entropy alloy.
Comparative example 3
This example is based on the document "Ultrafine-grained dual phase Al0.45CoCrFeNi high-even alloys, J.Hou, X.Shi, J.Qiao, Y.Zhang, P.K.Liaw, Y.Wu, Materials and Design, 2019' discloses that an as-cast alloy is obtained through a vacuum arc melting and casting process, homogenized at 1250 ℃ for 5h, cold rolled (70% deformation), and heat treated at 700 ℃ for 1h to obtain Al with FCC and BCC dual-phase structures0.45CoCrFeNi high entropy alloy.
Test example 5
The properties of the high-entropy alloys prepared in example 1 and comparative examples 2 to 3 were subjected to mechanical property tests, and the results are shown in table 4.
TABLE 4
| Examples | Yield strength (MPa) | Breaking Strength (MPa) | Elongation (%) |
| Example 1 | 560 | 1073 | 8.5 |
| Comparative example 2 | 300 | 590 | 30 |
| Comparative example 3 | 1200 | 1460 | 2.4 |
The high-entropy alloy of AlCoCrFeNi with equal atomic ratio is proved to be a typical BCC type high-entropy alloy, and the microstructure is a typical dendritic morphology. It was shown by studies to consist of an ordered B2 phase and a disordered BCC phase, with dendritic regions dominated by the B2 phase and intergranular regions dominated by the disordered BCC phase. Therefore, the alloy has high strength but poor plasticity, and the application prospect of the alloy as a structural material is severely limited.
At present, the comprehensive mechanical properties of AlCoCrFeNi series high-entropy alloy can be adjusted and controlled by changing the alloy content, for example, the content of Al element is reduced to convert the cast alloy into BCC and FCC dual-phase alloy. Table 4 comparative example 2 is a high entropy alloy of a dual phase structure obtained by reducing the Al content, compared with the mechanical properties of the alloy obtained in example 1, and although the plasticity is better, the strength of the alloy is lower. Comparative example 3 is a dual phase structure obtained by cold rolling and annealing heat treatment based on the alloy obtained in comparative example 2, and the alloy has high strength but poor plasticity. The starting point of the invention is different, and the microstructure and the mechanical property of the BCC-based AlCoCrFeNi high-entropy alloy are directly regulated and controlled based on a metastable phase decomposition method in a heat treatment process. By analysis and introduction of the embodiment 1, the invention can find that the elongation percentage of the alloy can be increased to 8.5 percent after heat treatment from 1.3 percent of the as-cast state at most through a simple high-temperature heat treatment process, and the improvement is obvious.
According to the invention, the microstructure of the as-cast alloy is changed by properly adjusting the alloy components, the main phase of the alloy intercrystalline region is converted into a stable FCC phase, the dendritic crystal region undergoes solid phase transition in the heat treatment process (shown in figure 2a), the heat treatment state dual-phase structure is finally obtained, and the alloy plasticity is remarkably improved. Therefore, different from the related process technologies reported in the past, the method provided by the invention aims at the BCC type AlCoCrFeNi series high-entropy alloy, regulates and controls the microstructure and mechanical property of the alloy by virtue of the metastable phase transition nature of the disordered BCC phase, really regulates and controls the tensile mechanical property of the as-cast alloy, and obviously improves the elongation.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (7)
1. A preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy is characterized by comprising the following steps:
firstly, preparing a high-entropy alloy ingot by adopting a vacuum arc melting method, then preparing the high-entropy alloy ingot into a high-entropy alloy casting bar by adopting a vacuum melting and pouring method, and carrying out heat treatment at the temperature of 1000-1200 ℃ for 1-3 hours to regulate and control the microstructure of the high-entropy alloy casting bar so as to obtain the AlCoCrFeNi series dual-phase structure high-entropy alloy in a heat treatment state;
the high-entropy alloy cast ingot comprises the following components in atomic percentage: co: 20.91-22.31 wt%, Cr: 18.45-19.68 wt%, Fe: 19.82-21.14 wt%, Ni: 26.66 to 31.24 weight percent, the balance being Al, and the sum of the atomic percentages of the components being 100 percent;
and (3) putting the high-entropy alloy cast rod into a vacuum atmosphere furnace for heat treatment and air cooling to obtain the thermal treatment AlCoCrFeNi series two-phase structure high-entropy alloy.
2. The preparation method of the AlCoCrFeNi-based two-phase structure high-entropy alloy as claimed in claim 1, wherein the preparation of the high-entropy alloy ingot by using a vacuum arc melting method specifically comprises the following steps:
(a) weighing metal raw materials according to a proportion, and putting the metal raw materials into a vacuum arc melting furnace;
(b) vacuumizing the arc melting furnace to 3 x 10-3Pa, filling protective gas to 1.6 × 103Pa, the process was repeated 5 times;
(c) melting high-purity metal by adopting a vacuum arc melting process to obtain an ingot, turning the ingot and then melting again, repeating the process for 5 times, cooling, polishing by using abrasive paper, ultrasonically cleaning by using absolute ethyl alcohol, and drying to obtain the high-entropy alloy ingot.
3. The preparation method of the AlCoCrFeNi-series two-phase structure high-entropy alloy as claimed in claim 1, wherein the method of vacuum melting and pouring is adopted to prepare the high-entropy alloy ingot into the high-entropy alloy cast rod, and the method specifically comprises the following steps:
(1) placing the high-entropy alloy cast ingot in a vacuum arc melting furnace;
(2) vacuumizing the arc melting furnace to 3 x 10-3Pa, filling protective gas to 1.6 × 103Pa, the process was repeated 5 times;
(3) and melting the high-entropy alloy cast ingot by adopting a vacuum arc melting process, wherein the current is 280A, and cooling to obtain the high-entropy alloy cast rod.
4. The method for preparing the high-entropy alloy with the dual-phase structure of the AlCoCrFeNi system as claimed in claim 2, wherein the current of the vacuum arc melting process in the step (c) is 150-280A.
5. The method for preparing the high-entropy alloy of the dual-phase structure of AlCoCrFeNi series as claimed in claim 2, wherein the drying temperature in the step (c) is 50-80 ℃.
6. The method for preparing the high-entropy alloy of the dual-phase structure of AlCoCrFeNi series as claimed in claim 2 or 3, wherein the protective gas is argon.
7. The method for preparing the high-entropy alloy of the dual-phase structure of AlCoCrFeNi series according to claim 1, wherein the vacuum atmosphere furnace is an argon atmosphere.
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