CN113832416A - Method for regulating and controlling sigma phase of high-entropy alloy by using magnetic field - Google Patents
Method for regulating and controlling sigma phase of high-entropy alloy by using magnetic field Download PDFInfo
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Abstract
The invention discloses a method for regulating and controlling a sigma phase of a high-entropy alloy by using a magnetic field, which comprises the following steps: placing the high-entropy alloy block prepared by smelting in a quartz glass tube, and placing the sample-carrying quartz glass tube filled with the high-entropy alloy block in a uniform magnetic field of an excitation coil; and heating the sample-carrying quartz glass tube, applying a 0-30T magnetic field in a temperature range of the heating temperature for the generation and disappearance of the sigma phase of the high-entropy alloy, and carrying out quenching after keeping the temperature for a period of time to obtain the high-entropy alloy block body treated by the magnetic field. The invention makes the magnetic field act on the phase change process of the high-entropy alloy, regulates and controls the generation and disappearance of sigma phase through the magnetic field treatment, and changes the microstructure, the mechanical property and the magnetic property of the alloy. The method is simple and feasible, and opens up a new way for the organization formation and defect control of the high-entropy alloy and the improvement of the metallurgical quality by adopting the electromagnetic field.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy material treatment, and particularly relates to a method for regulating and controlling a sigma phase of a high-entropy alloy by using a magnetic field.
Background
The conventional alloy is mainly composed of one or two metal elements, and is obtained by adding a small amount of other alloying elements to obtain an alloy with certain special properties, such as iron-based steel materials, aluminum-based aluminum alloys, nickel-based alloys and the like. The high-entropy alloy is a brand-new alloy system proposed since 2004, and generally consists of five or more alloy components, wherein the atomic percent of each component is between 5 and 35 percent, and the existence of trace elements with the atomic percent less than 5 percent is allowed. The addition of more principal elements will result in alloys composed of more phases, including ordered phases, complex intermetallics (σ and Laves, etc.) and even face-centered cubic (FCC), body-centered cubic (BCC), Hexagonal Close Packed (HCP) derived ordered structures. These unique structures determine that the high-entropy alloy has excellent properties such as high hardness, high strength, high wear resistance, excellent high-temperature and low-temperature properties, good fatigue and creep properties and the like.
The sigma phase is a defect that is widely present in nickel-base superalloys and stainless steels (ZHao J C, Larsen M, Ravikumar V. phase prediction and time-temperature-transformation diagramm of HastelloyX [ J ]. Materials Science and engineering A,2000,293: 112-. The brittle phase can obviously deteriorate the mechanical property of the alloy and influence the use of the alloy. Currently, the researchers found that the sigma phase also widely exists in the high-entropy alloy after the medium-temperature treatment. Taking AlCoCrFeNi high-entropy alloy as an example, the generation and disappearance of sigma phase can occur in the thermal treatment at about 610 ℃ and 990 ℃, and the mechanical property and the magnetic property are obviously changed: the BCC phase transforms into the FCC and sigma phases upon heat treatment at 610 deg.C, whereas the sigma phase transforms into the FCC and BCC phases upon heat treatment at 990 deg.C (ZHao C D, Li J, LiuY, et al. Tally mechanical and magnetic properties of AlCoCrFeNi high-entry alloy via phase transformation [ J ]. Journal of materials Science and Technology,2021,73: 83-90). At present, a method for regulating sigma phase and improving material performance is very urgent to find.
Disclosure of Invention
In order to solve the problem that the sigma phase of the high-entropy alloy is widely existed after medium-temperature treatment in the prior art, so that the mechanical property and the magnetic property of the high-entropy alloy are influenced, the invention provides a method for regulating the sigma phase of the high-entropy alloy by using a magnetic field.
The strong magnetic field, as a non-contact high-energy physical field, can generate magnetization energy, Lorentz force, magnetization force and the like on a substance, and the control of tissue formation and defects through the synergistic action of heat, electricity, magnetism and force can serve as a method for obtaining the electromagnetic field to improve the metallurgical quality. In the existing research, the magnetic properties of new and old phases of steel in the phase change process are different, and the magnetization energy applied by a strong magnetic field can change the phase change thermodynamics of the steel, so that the initial temperature of the phase change is increased. The high-entropy alloy has the transformation of ferromagnetic BCC phase and paramagnetic sigma phase and FCC (fluid catalytic cracking) phase at medium temperature and above, so that the phase change of the sigma phase of the high-entropy alloy can be regulated and controlled by a magnetic field, and the magnetic property and the mechanical property of the high-entropy alloy can be improved.
According to the invention, the magnetic field directly acts on the phase change process of the high-entropy alloy, the structure morphology of the high-entropy alloy evolves after being regulated and controlled by the strong magnetic field, and the magnetic property and the mechanical property of the high-entropy alloy are regulated and controlled due to the inhibition of the generation and disappearance of the sigma phase, so that a foundation is laid for the structure property optimization and the engineering application of the high-entropy alloy.
The invention is realized by the following technical scheme:
the method for regulating and controlling the sigma phase of the high-entropy alloy by using the magnetic field comprises the following steps:
placing the high-entropy alloy block prepared by smelting in a quartz glass tube, and placing the sample-carrying quartz glass tube filled with the high-entropy alloy block in a uniform magnetic field of an excitation coil;
and heating the sample-carrying quartz glass tube, applying a 0-30T magnetic field in a temperature range of the heating temperature for the generation and disappearance of the sigma phase of the high-entropy alloy, and carrying out quenching after keeping the temperature for a period of time to obtain the high-entropy alloy block body treated by the magnetic field.
As further illustration of the invention, the high-entropy alloy is AlCoCrFeNi high-entropy alloy.
As a further explanation of the present invention, the rate of temperature rise during heating is 1 to 90K/min.
As a further illustration of the invention, the temperature interval for the generation and disappearance of the sigma phase of the high-entropy alloy is specifically 500-1200 ℃.
As a further illustration of the invention, the time of the heat preservation is 0.5h to 100 h.
As a further explanation of the present invention, in the magnetic field processing, the excitation coil is electrically excited by an excitation power supply so that a required magnetic field strength is obtained at a maximum uniform magnetic field.
As further illustration of the invention, the preparation process of the high-entropy alloy block is as follows:
the method comprises the steps of taking a multi-principal-element intermediate alloy with the purity of 99.95% and a high-purity simple substance with the purity of 99.99% as raw materials, proportioning by atomic ratio of target components, smelting the raw materials by adopting a vacuum induction smelting method to obtain a high-entropy alloy ingot, and then cutting the high-entropy alloy ingot into high-entropy alloy blocks.
As a further explanation of the present invention, the smelting of the raw materials by using the vacuum induction smelting method comprises the following processes:
firstly, putting the raw materials into a vacuum induction melting furnace, vacuumizing to below 10Pa, heating to 400 ℃, preserving heat for 4-6 hours to remove water vapor, then filling the furnace body with Ar gas, circulating for three times, finally, quickly heating the furnace body to 1550 ℃, preserving heat for 15 minutes, and then pouring in a steel die to obtain the high-entropy alloy ingot.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention makes the magnetic field act on the phase change process of the high-entropy alloy, regulates and controls the generation and disappearance of sigma phase through the magnetic field treatment, and changes the microstructure, the mechanical property and the magnetic property of the alloy. The method is simple and feasible, and opens up a new way for the organization formation and defect control of the high-entropy alloy and the improvement of the metallurgical quality by adopting the electromagnetic field.
Drawings
FIG. 1 is a schematic view of the apparatus used in the high-entropy alloy high-intensity magnetic field solidification experiment provided by the invention.
FIG. 2 is a picture of the morphology of the AlCoCrFeNi high-entropy alloy sample in the absence of a magnetic field and after being processed by a 10T magnetic field; the different treatment conditions in the figure are respectively: (a)610 ℃ -0T, (b)610 ℃ -10T; (c)990 ℃ -0T, (d)990 ℃ -10T.
FIG. 3 is an XRD curve of AlCoCrFeNi high-entropy alloy samples after being processed by no magnetic field and 10T magnetic field.
FIG. 4 is a compressive stress-strain curve of AlCoCrFeNi high-entropy alloy samples after being processed without a magnetic field and a 10T magnetic field.
FIG. 5 is a hysteresis loop of AlCoCrFeNi high-entropy alloy sample after being processed by no magnetic field and 10T magnetic field.
FIG. 6 is a simplified flow chart of a method for controlling the sigma phase of a high-entropy alloy by using a magnetic field according to an embodiment of the present invention.
In the figure: 1. a water cooling machine; 2. a compressor; 3. an excitation power supply; 4. a superconducting magnet; 5. a quartz tube; 6. a copper sleeve; 7. a copper end cap; 8. a heat-insulating layer; 9. a water-cooling layer; 10. a sample; 11. a heating body; 12. a tray; 13. an insulating refractory disc; 14. a thermocouple fixing plate; 15. a thermocouple; 16. a heating power supply; 17. an continental controller; 18. a computer; 19. an infrared probe; 20. a test tube clamp; 21. a balance.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
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. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Fig. 6 is a simplified flow chart of a method for regulating a sigma phase of a high-entropy alloy by using a magnetic field according to an embodiment of the present invention, and as shown in fig. 6, the present invention provides a method for regulating a sigma phase of a high-entropy alloy by using a magnetic field, including:
step 1: placing the high-entropy alloy block prepared by smelting in a quartz glass tube, and placing the sample-carrying quartz glass tube filled with the high-entropy alloy block in a uniform magnetic field of an excitation coil;
step 2: and heating the sample-carrying quartz glass tube, applying a 0-30T magnetic field in a temperature range of the heating temperature for the generation and disappearance of the sigma phase of the high-entropy alloy, and carrying out quenching after keeping the temperature for a period of time to obtain the high-entropy alloy block body treated by the magnetic field.
In the step 1, the preparation process of the high-entropy alloy block is as follows:
the method comprises the steps of taking a multi-principal-element intermediate alloy with the purity of 99.95% and a high-purity simple substance with the purity of 99.99% as raw materials, mixing the raw materials according to the atomic ratio of target components, smelting the raw materials by adopting a vacuum induction smelting method to obtain a high-entropy alloy ingot, and then cutting the high-entropy alloy ingot into high-entropy alloy blocks.
In order to ensure the purity and cleanliness of the raw materials, the following cleaning pretreatment processes are carried out before vacuum induction melting: removing the line cutting mark, performing ultrasonic cleaning with acetone for 10min-20min, removing dust and oil stain on the surface of the intermediate alloy, and drying in a drying oven.
The raw materials are smelted by adopting a vacuum induction smelting method, and the smelting method comprises the following steps:
firstly, putting the raw materials into a vacuum induction melting furnace, vacuumizing to below 10Pa, heating to 400 ℃, preserving heat for 4-6 hours to remove water vapor, then filling the furnace body with Ar gas, circulating for three times, finally, quickly heating the furnace body to 1550 ℃, preserving heat for 15 minutes, and then pouring in a steel die to obtain the high-entropy alloy ingot. The high-entropy alloy ingot is preferably a large-volume high-entropy alloy ingot of 3-20 kg.
In order to test the structure and the performance of the high-entropy alloy conveniently, the size of the high-entropy alloy block is within phi 30mm multiplied by 40 mm.
The magnetic field treatment process of the step 2 comprises the following specific steps: firstly, putting a quartz glass tube filled with a high-entropy alloy block in a uniform magnetic field of an excitation coil, and electrifying and exciting the excitation coil through an excitation power supply to enable the maximum uniform magnetic field to reach the required magnetic field intensity: 0-30T. And then heating and preserving heat of the high-entropy alloy block in the quartz glass tube by a heating power supply according to a set program, and finally quenching to obtain the high-entropy alloy block treated by the magnetic field.
During the magnetic field heat treatment, the heating rate is 1-90K/min, the temperature range of the generation and disappearance of the sigma phase of the high-entropy alloy is 500-1200 ℃, the heat preservation time is 0.5-100 h, and then quenching is carried out to obtain the high-entropy alloy block body after the magnetic field treatment.
The technical scheme of each embodiment of the invention is implemented by a magnetic field material processing device. The technical scheme of the magnetic field material processing device is disclosed in the invention with the application number of 201910364023.3. As shown in fig. 1, the device comprises a water cooling machine 1, a compressor 2, an excitation power supply 3, a superconducting magnet 4, a quartz tube 5, a copper sleeve 6, an insulating layer 8, a water cooling layer 9, a heating body 11, a thermocouple fixing plate 14 and a thermocouple 14. Wherein: the water cooler 1 is connected with the compressor 2; the compressor is connected with the input end and the output end of a liquid nitrogen cooling pipe orifice of the superconducting magnet. The excitation power supply 3 is connected to the superconducting magnet 4.
The lower end of the quartz tube 5 penetrates through the copper sleeve 6 and is arranged in the heating body; the upper end of the thermocouple 15 penetrates through the thermocouple fixing plate 14 and is arranged in the heating body; and a distance of 10-20 mm is formed between the lower end face of the quartz tube and the upper end face of the thermocouple. The heating body is positioned in the heat preservation layer 8, and a distance of 10-20 mm is formed between the outer circumferential surface of the heating body and the inner circumferential surface of the heat preservation layer. The heat-insulating layer is positioned in the water-cooling layer 9, and the outer circumferential surface of the heat-insulating layer is attached to the inner circumferential surface of the water-cooling layer; the length of the heat-insulating layer is the same as that of the water-cooling layer. The water-cooling layer is positioned in the superconducting magnet 4, and the outer circumferential surface of the water-cooling layer is attached to the inner circumferential surface of the superconducting magnet; the lower end face of the positioning boss at the upper end of the water cooling layer is attached to the upper end face of the superconducting magnet. A copper end cover 7 is arranged in an inner hole at the upper end of the heat-insulating layer.
A tray 12 is fixed below the superconducting magnet 4; the insulating fireproof disc 13 is arranged in a clamping groove on the upper surface of the tray 12; the central hole of the tray is in clearance fit with the outer circumferential surface of the heating body; the insulating fire-resistant disc is fixedly connected to the outer circumferential surface of the heating body through clay. And the flange at the upper end of the copper end cover is attached to the end faces of the heat-insulating layer and the water-cooling layer. The copper sleeve is arranged on the spigot at the hole of the central hole on the upper end surface of the copper end cover. The infrared probe 19, the test tube holder 20 and the balance 21 constitute a balance magnetic susceptibility measurement system. When the balance magnetic susceptibility is measured, the copper sleeve on the quartz tube is removed, the top end of the test tube clamp is connected with the balance through the hook, and the bottom end of the test tube clamp is connected with the quartz tube through the nylon bolt, so that the quartz tube is freely suspended. The infrared probe and the balance are connected with a computer through a lead and a conversion interface.
A through groove is formed in the shell of the heating body, and the width of the through groove is 7 mm; the upper end of the through groove is a spiral groove, and the lower end of the through groove is a vertical groove; the distance between the notch at the top end of the spiral groove and the upper end surface of the heating body is 30 mm; the notch of the vertical groove penetrates through the lower end face of the heating body. The ratio of the axial vertical length of the spiral groove to the axial length of the vertical groove is 1: 1.5. The spiral angle of the spiral groove is 25 degrees, and the vertical distance between the center distances of the adjacent spiral grooves in the width direction is 40 mm. The outer diameter of the small outer diameter end of the copper bush 6 is the same as the inner diameter of the copper end cover; four radial threaded holes are uniformly distributed on the large outer diameter end, and each threaded hole is communicated with the central hole of the copper sleeve; the aperture of the central hole of the copper sleeve is the same as the outer diameter of the quartz tube, and the copper sleeve and the quartz tube are in clearance fit. After the quartz tube is arranged in the central hole of the copper sleeve, bolts are arranged in the threaded holes to fasten the quartz tube. The thermocouple fixing plate 14 is a triangular plate, a thermocouple through hole is formed in the geometric center of the thermocouple fixing plate, and screw holes for connecting the tray are formed in three corners of the thermocouple fixing plate.
The center of the tray 12 is provided with a mounting hole of a heating body. The upper surface of the tray is provided with an axially protruding ring, and the inner diameter of the ring is the same as the outer diameter of the insulating refractory disc. Screw holes for fixedly connecting with the superconducting magnet are uniformly distributed on the outer edge of the tray surface; the tray surface is provided with screw holes distributed in a triangular shape and used for connecting the thermocouple fixing plate. The mass measuring range of the balance in the balance magnetic susceptibility measuring system is 650g at most; the quartz tube can accommodate a specimen of phi 30 mm.
The position from the upper surface of the superconducting magnet 4 to the 460mm deep hole of the inner cavity of the superconducting magnet is the position of a uniform magnetic field, the gradient of the magnetic field at the position is 0, and the strength of the uniform magnetic field can reach 10T at most. The position 330mm down from the upper surface of the superconducting magnet is the position with the maximum magnetic field gradient, and the gradient magnetic field at the position can reach 300T at most2/m。
Two preferred examples will be specifically described below.
Example 1:
the high-entropy alloy in the embodiment is AlCoCrFeNi, the heat treatment temperature is 610 ℃, and the magnetic field intensity is 0T and 10T
The embodiment provides a method for regulating and controlling an AlCoCrFeNi high-entropy alloy sigma phase by utilizing magnetic field treatment, which comprises the following steps of:
step one, preparing an alloy:
firstly, preparing alloy raw materials. Selecting FeCoCr, Ni2Al intermediate alloy (purity 99.95%) and high-purity Al, Co, Cr, Fe and Ni (purity 99.99%) as raw materials, wherein Al, Co, Cr, Fe and Ni are solid elementary raw materials. The raw materials are mixed according to the atomic ratio of Al, Co, Cr, Fe and Ni being 1:1:1:1:1, the raw materials are mechanically polished to remove linear cutting marks, ultrasonic cleaning is carried out for 10min by acetone, and then the raw materials are placed in a drying oven to be dried.
And secondly, smelting the alloy. Preheating a furnace body, then placing the raw materials into a crucible of a vacuum induction smelting furnace, heating to 400 ℃ in vacuum below 10Pa, preserving heat for 4 hours, filling argon into the smelting chamber, closing an argon filling valve after the pressure in the furnace reaches 0.05MPa, circulating for three times, quickly heating the furnace body to 1550 ℃ under the argon condition, preserving heat for 15 minutes, and then pouring in a steel mould. Finally obtaining 7kg of AlCoCrFeNi large-volume high-entropy alloy cast ingot.
And step two, placing the sample. The AlCoCrFeNi high-entropy alloy block to be regulated is placed in a quartz glass tube with the outer diameter of 18mm and the inner diameter of 16mm, and is placed in a uniform magnetic field region of an excitation coil. In order to test the structure, phase type and performance of the AlCoCrFeNi high-entropy alloy conveniently, the size of the AlCoCrFeNi high-entropy alloy block is phi 13mm multiplied by 16 mm.
And step three, treating by a strong magnetic field. The magnetic field treatment process is implemented by an excitation power supply and a heating power supply, and the excitation power supply is used for electrifying and exciting the excitation coil to enable the maximum uniform magnetic field to reach the required magnetic field intensity (0T and 10T). Heating, insulating and quenching AlCoCrFeNi high-entropy alloy blocks in the quartz glass tube by a heating power supply according to a set program. The heating rate during heating is 10K/min, the temperature is kept for 10h at the heating temperature of 610 ℃, and then quenching is carried out to obtain the AlCoCrFeNi high-entropy alloy block body after high-intensity magnetic field treatment.
A1 mm slice of the AlCoCrFeNi high-entropy alloy sample subjected to magnetic field treatment is cut along a direction parallel to a magnetic field by using linear cutting to observe a microstructure, a 1.5mm slice is cut for XRD (X-ray diffraction) test, and a cylinder with phi 4mm multiplied by 4mm is cut for magnetic property test. Simultaneously cutting a cylinder with the diameter of 4mm multiplied by 8mm, and adopting a CMT5025 electronic universal mechanical testing machine produced by American national Patty company to test the room temperature compression performance with the strain rate of 5 multiplied by 10-4s-1The test result is as follows:
the microstructure of the AlCoCrFeNi high-entropy alloy sample treated by the non-magnetic field and the 10T magnetic field is shown in FIG. 2, the structure evolution of a grain boundary region occurs under the condition of no magnetic field at 610 ℃ (FIG. 2a), but the structure evolution does not occur after the 10T magnetic field is applied (FIG. 2 c).
FIG. 3 is an XRD curve of AlCoCrFeNi high-entropy alloy sample treated by a magnetic field-free and a 10T magnetic field, and the peak intensity of a sigma phase is weakened relative to that under the magnetic field-free condition after the 10T magnetic field is applied at 610 ℃.
Fig. 4 and 5 show the compressive stress-strain curves and hysteresis loops of the AlCoCrFeNi high-entropy alloy samples after the magnetic field-free treatment and the 10T magnetic field treatment, respectively, and the results are shown in table 1. After a 10T magnetic field is applied at 610 ℃, the strength and the plasticity are simultaneously improved, and the saturation magnetization is improved.
Example 2:
the high-entropy alloy in the embodiment is AlCoCrFeNi, the heat treatment temperature is 990 ℃, and the magnetic field intensity is 0T and 10T
The embodiment provides a method for regulating and controlling an AlCoCrFeNi high-entropy alloy sigma phase by utilizing magnetic field treatment, which comprises the following steps of:
step one, preparing an alloy:
firstly, preparing alloy raw materials. Selecting FeCoCr, Ni2Al intermediate alloy (purity 99.95%) and high-purity Al, Co, Cr, Fe and Ni (purity 99.99%) as raw materials, wherein Al, Co, Cr, Fe and Ni are solid elementary raw materials. The raw materials are mixed according to the atomic ratio of Al, Co, Cr, Fe and Ni being 1:1:1:1:1, the raw materials are mechanically polished to remove linear cutting marks, ultrasonic cleaning is carried out for 10min by acetone, and then the raw materials are placed in a drying oven to be dried.
And secondly, smelting the alloy. Preheating a furnace body, then placing the raw materials into a crucible of a vacuum induction smelting furnace, heating to 400 ℃ in vacuum below 10Pa, preserving heat for 4 hours, filling argon into the smelting chamber, closing an argon filling valve after the pressure in the furnace reaches 0.05MPa, circulating for three times, quickly heating the furnace body to 1550 ℃ under the argon condition, preserving heat for 15 minutes, and then pouring in a steel mould. Finally obtaining 7kg of AlCoCrFeNi large-volume high-entropy alloy cast ingot.
And step two, placing the sample. The AlCoCrFeNi high-entropy alloy block to be regulated is placed in a quartz glass tube with the outer diameter of 18mm and the inner diameter of 16mm, and is placed in a uniform magnetic field region of an excitation coil. In order to test the structure, phase type and performance of the AlCoCrFeNi high-entropy alloy conveniently, the size of the AlCoCrFeNi high-entropy alloy block is phi 13mm multiplied by 16 mm.
And step three, treating by a strong magnetic field. The magnetic field treatment process is implemented by an excitation power supply and a heating power supply, and the excitation power supply is used for electrifying and exciting the excitation coil to enable the maximum uniform magnetic field to reach the required magnetic field intensity (0T and 10T). Heating, insulating and quenching AlCoCrFeNi high-entropy alloy blocks in the quartz glass tube by a heating power supply according to a set program. The heating rate during heating is 10K/min, the temperature is kept for 10h at the heating temperature of 990 ℃, and then quenching is carried out to obtain the AlCoCrFeNi high-entropy alloy block body after high-intensity magnetic field treatment.
A1 mm slice of the AlCoCrFeNi high-entropy alloy sample subjected to magnetic field treatment is cut along a direction parallel to a magnetic field by using linear cutting to observe a microstructure, a 1.5mm slice is cut for XRD (X-ray diffraction) test, and a cylinder with phi 4mm multiplied by 4mm is cut for magnetic property test. Simultaneously cutting a cylinder with the diameter of 4mm multiplied by 8mm, and adopting a CMT5025 electronic universal mechanical testing machine produced by American national Patty company to test the room temperature compression performance with the strain rate of 5 multiplied by 10-4s-1The test result is as follows:
the microstructure of the AlCoCrFeNi high-entropy alloy sample treated by the magnetic field-free and the 10T magnetic field is shown in figure 2, the structure is flat under the condition of no magnetic field at 990 ℃ (figure 2b), and the structure is changed from flat to long after the 10T magnetic field is applied (figure 2 d).
FIG. 3 is an XRD curve of AlCoCrFeNi high-entropy alloy sample after being processed by a magnetic field-free and a 10T magnetic field, wherein a sigma phase peak does not exist after being processed by the magnetic field-free at 990 ℃, and the sigma phase peak appears after the 10T magnetic field is applied.
Fig. 4 and 5 show the compressive stress-strain curves and hysteresis loops of the AlCoCrFeNi high-entropy alloy samples after the magnetic field-free treatment and the 10T magnetic field treatment, respectively, and the results are shown in table 1. After applying a 10T magnetic field at 990 ℃, the strength and plasticity are reduced and the magnetic properties are deteriorated.
TABLE 1 mechanical and magnetic properties of AlCoCrFeNi high entropy alloy under various processing conditions
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A method for regulating and controlling a sigma phase of a high-entropy alloy by using a magnetic field is characterized by comprising the following steps:
placing the high-entropy alloy block prepared by smelting in a quartz glass tube, and placing the sample-carrying quartz glass tube filled with the high-entropy alloy block in a uniform magnetic field of an excitation coil;
and heating the sample-carrying quartz glass tube, applying a 0-30T magnetic field in a temperature range of the heating temperature for the generation and disappearance of the sigma phase of the high-entropy alloy, and carrying out quenching after keeping the temperature for a period of time to obtain the high-entropy alloy block body treated by the magnetic field.
2. The method for regulating sigma phase of high-entropy alloy by using magnetic field as claimed in claim 1, wherein the high-entropy alloy is AlCoCrFeNi high-entropy alloy.
3. The method for regulating the sigma phase of the high-entropy alloy by using the magnetic field as claimed in claim 1, wherein the heating rate is 1-90K/min.
4. Method for modulating sigma phase of high entropy alloy by magnetic field according to claim 1, characterized in that the temperature interval for generation and disappearance of sigma phase of high entropy alloy is in particular 500-1200 ℃.
5. The method for regulating sigma phase of high-entropy alloy by using magnetic field according to claim 1, wherein the holding time is 0.5h-100 h.
6. A method for regulating sigma phase of high-entropy alloy by using magnetic field according to claim 1, wherein the magnetic field treatment is performed by energizing the exciting coil by an exciting power supply so that the required magnetic field intensity is achieved at the maximum uniform magnetic field.
7. The method for regulating sigma phase of high-entropy alloy by using magnetic field according to claim 1, wherein the high-entropy alloy block is prepared by the following steps:
the method comprises the steps of taking a multi-principal-element intermediate alloy with the purity of 99.95% and a high-purity simple substance with the purity of 99.99% as raw materials, mixing the raw materials according to the atomic ratio of target components, smelting the raw materials by adopting a vacuum induction smelting method to obtain a high-entropy alloy ingot, and then cutting the high-entropy alloy ingot into high-entropy alloy blocks.
8. The method for regulating and controlling the sigma phase of the high-entropy alloy by using the magnetic field as claimed in claim 7, wherein the smelting of the raw material by using a vacuum induction smelting method comprises the following steps:
firstly, putting the raw materials into a vacuum induction melting furnace, vacuumizing to below 10Pa, heating to 400 ℃, preserving heat for 4-6 hours to remove water vapor, then filling the furnace body with Ar gas, circulating for three times, finally, quickly heating the furnace body to 1550 ℃, preserving heat for 15 minutes, and then pouring in a steel die to obtain the high-entropy alloy ingot.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418588A (en) * | 2022-09-15 | 2022-12-02 | 西北工业大学 | Magnetic field deep supercooling treatment method for improving toughness of cobalt-based high-temperature alloy |
| CN115927943A (en) * | 2022-08-16 | 2023-04-07 | 重庆化工职业学院 | Method for preparing high-hardness high-toughness CrMnFeNi-based high-entropy alloy by doping Si and B |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756412A (en) * | 2017-03-16 | 2017-05-31 | 西北工业大学 | One kind prepares Al0.5The method of CoCrFeNi high-entropy alloys |
| CN107267838A (en) * | 2017-05-11 | 2017-10-20 | 东北大学 | It is a kind of to prepare the method with high tough fine grain high-entropy alloy using pyromagnetic coupling |
| CN109972066A (en) * | 2019-05-05 | 2019-07-05 | 西北工业大学 | The method for improving AlCoCrCuFeNi high-entropy alloy power magnetic property using magnetic field |
| CN109971980A (en) * | 2019-05-05 | 2019-07-05 | 西北工业大学 | The method for improving CrCoNi medium entropy alloy mechanical property using magnetic field |
| CN110093522A (en) * | 2019-05-05 | 2019-08-06 | 西北工业大学 | AlCoCrFeNi is improved using magnetic field2.1The method of eutectic high-entropy alloy mechanical property |
| WO2020118802A1 (en) * | 2018-12-10 | 2020-06-18 | 北京理工大学 | Lightweight high-entropy alloy having high strength and high plasticity and preparation method therefor |
| CN113025865A (en) * | 2021-03-03 | 2021-06-25 | 北方工业大学 | Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy |
-
2021
- 2021-10-28 CN CN202111266032.2A patent/CN113832416A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756412A (en) * | 2017-03-16 | 2017-05-31 | 西北工业大学 | One kind prepares Al0.5The method of CoCrFeNi high-entropy alloys |
| CN107267838A (en) * | 2017-05-11 | 2017-10-20 | 东北大学 | It is a kind of to prepare the method with high tough fine grain high-entropy alloy using pyromagnetic coupling |
| WO2020118802A1 (en) * | 2018-12-10 | 2020-06-18 | 北京理工大学 | Lightweight high-entropy alloy having high strength and high plasticity and preparation method therefor |
| CN109972066A (en) * | 2019-05-05 | 2019-07-05 | 西北工业大学 | The method for improving AlCoCrCuFeNi high-entropy alloy power magnetic property using magnetic field |
| CN109971980A (en) * | 2019-05-05 | 2019-07-05 | 西北工业大学 | The method for improving CrCoNi medium entropy alloy mechanical property using magnetic field |
| CN110093522A (en) * | 2019-05-05 | 2019-08-06 | 西北工业大学 | AlCoCrFeNi is improved using magnetic field2.1The method of eutectic high-entropy alloy mechanical property |
| CN113025865A (en) * | 2021-03-03 | 2021-06-25 | 北方工业大学 | Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy |
Non-Patent Citations (6)
| Title |
|---|
| 张伟强: "《固态金属及合金中的相变》", 31 May 2016 * |
| 曾鹏等: "热处理温度对Al_xCoCrFeNi系高熵合金组织和硬度的影响", 《上海金属》 * |
| 王康康 等: "高熵合金的研究进展", 《中国重型装备》 * |
| 简天真: "热处理及强磁场对FeCoNiAlxCr系高熵合金组织及性能的影响", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
| 赵晨东 等: "强磁场作用下AlxCoCrFeNi高熵合金相变机制及力-磁性能研究", 《第五届全国电磁冶金与强磁场材料科学年会论文集》 * |
| 龙琼等: "高熵合金耐蚀性研究的现状及最新进展", 《电镀与涂饰》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115927943A (en) * | 2022-08-16 | 2023-04-07 | 重庆化工职业学院 | Method for preparing high-hardness high-toughness CrMnFeNi-based high-entropy alloy by doping Si and B |
| CN115418588A (en) * | 2022-09-15 | 2022-12-02 | 西北工业大学 | Magnetic field deep supercooling treatment method for improving toughness of cobalt-based high-temperature alloy |
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