CN114351028B - One kind (FeVCrMn) x Ti y Low-activation high-entropy alloy and preparation method thereof - Google Patents
One kind (FeVCrMn) x Ti y Low-activation high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of alloy strengthening and nuclear fusion low-activation structural materials, and particularly discloses a (FeVCrMn) x Ti y Low activation high entropy alloy and method of making the same (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x + y =100, x is more than or equal to 90, and y is less than or equal to 10. (FeVCrMn) x Ti y The low-activation high-entropy alloy is of a single-phase body-centered cubic BCC structure, and the grain size is less than or equal to 200 mu m. (FeVCrMn) x Ti y The hardness of the low-activation high-entropy alloy is more than or equal to 400HV, the elastic modulus is about 200GPa, the room-temperature yield strength is more than or equal to 700MPa, and the room-temperature tensile strength is more than or equal to 1200MPa. Of the invention (FeVCrMn) x Ti y The low-activation high-entropy alloy takes Fe, V, cr and Mn as main components with equal atomic ratio, takes Ti as an adjusting element, and adopts a strengthening method mainly based on solid solution strengthening to achieve high-strength mechanical properties.
Description
Technical Field
The invention belongs to the field of alloy strengthening and nuclear fusion low-activation structural materials, and particularly relates to a (FeVCrMn) x Ti y A low-activation high-entropy alloy and a preparation method thereof.
Background
The service condition of the structural material for the nuclear fusion reactor is very strict, the material is required to have excellent neutron irradiation resistance and high-temperature mechanical property, and the components meet the low activation requirement. The development of structural materials of the fusion reactor is one of key factors influencing the design, construction and commercial use of the fusion reactor. The traditional alloy generally takes one or two alloy elements as the main part, and achieves the required mechanical property requirement by adding trace other elements or assisting different processing techniques, and the mechanical property of the traditional alloy can not be further improved because of the limit of the characteristics of the main elements.
The high-entropy alloy is a novel material design concept, and due to the fact that atomic sizes of different constituent elements are different, crystal lattices of the high-entropy alloy can be seriously distorted and randomly and freely distributed in the crystal lattices, the high-entropy alloy has better mechanical properties than common alloys, and has wide potential application value. The high-entropy alloy has flexible component selection and can fully exert the characteristics of each principal element. Due to the high entropy of mixing, the formation of intermetallic compounds in the material is suppressed and a solid solution structure with a simple structure can be obtained.
The structural material with radiation resistance, high temperature resistance and excellent mechanical property is a fusion reactor key material. The concept of the high-entropy alloy for the fusion reactor provides a thought for developing novel fusion materials. In terms of selection of alloying elements, the low activation requirement needs to be met.
Therefore, there is a need to develop a low-activation high-entropy alloy as a novel fusion material for a nuclear fusion reactor.
Disclosure of Invention
The invention aims to provide a (FeVCrMn) x Ti y A low-activation high-entropy alloy and its preparing process features that Fe, V, cr and Mn are used as the main components of atomic ratio, ti is used as regulating element, and the strengthening method mainly including solid solution strengthening is used to obtain high-strength mechanical performance.
The technical scheme for realizing the purpose of the invention is as follows: one kind (FeVCrMn) x Ti y Low activation high entropy alloy, (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x + y =100, x is more than or equal to 90, and y is less than or equal to 10.
Said (FeVCrMn) x Ti y The low-activation high-entropy alloy is a single-phase body-centered cubic BCC structure, and the grain size is less than or equal to 200 mu m.
Said (FeVCrMn) x Ti y The hardness of the low-activation high-entropy alloy is more than or equal to 400HV, the elastic modulus is about 200GPa, and the yield strength at room temperature is more than or equal to700MPa and the room-temperature tensile strength is more than or equal to 1200MPa.
Said (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x =95 and y =5.
The (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x =98, y =2.
One kind of preparation (FeVCrMn) x Ti y A method of low activation of a high entropy alloy, the method comprising the steps of:
step 1, weighing raw materials of elementary substance elements of Fe, V, cr, mn and Ti according to the atomic percentage of each element, and putting the raw materials into a water-cooled copper crucible of a vacuum arc melting furnace;
and 2, carrying out vacuum arc melting on the raw materials of the Fe, V, cr, mn and Ti simple substance elements which are put into a water-cooled copper crucible of the vacuum arc melting furnace.
The step 2 specifically comprises the following steps: vacuumizing the vacuum chamber to less than or equal to 5 multiplied by 10 -3 Pa, filling high-purity argon to a vacuum bin with the pressure of-0.8 to-0.6 MPa, smelting current of 350 to 450A, and introducing cooling water during smelting; repeatedly smelting the front and back surfaces of the alloy ingot for 3-5 times, keeping for 3-6 minutes each time, keeping the alloy in a liquid state for 10-30 minutes, and finally cooling to obtain (FeVCrMn) x Ti y And (3) low-activation high-entropy alloy ingot casting.
The beneficial technical effects of the invention are as follows:
1. of the invention (FeVCrMn) x Ti y The hardness of the low-activation high-entropy alloy is more than or equal to 400HV, the elastic modulus is about 200GPa, the room-temperature yield strength is more than or equal to 700MPa, the room-temperature tensile strength is more than or equal to 1200MPa, and the strength of the low-activation high-entropy alloy is far higher than that of the existing fusion reactor low-activation structural material such as low-activation ferrite/martensite steel and vanadium alloy, so that the low-activation high-entropy alloy is a novel low-activation high-entropy alloy fusion reactor structural material with excellent mechanical properties.
2. The preparation method has simple preparation steps and easy operation, the preparation period of the high-entropy alloy is as low as 3 hours, and the solid solution strengthening (FeVCrMn) with uniform components can be prepared by only one step of vacuum arc melting in the operation process x Ti y And (3) low-activation high-entropy alloy ingot casting.
3. The metal elements used for preparing the material are all low-activation elements, namely the induced radioactivity of the material after neutron irradiation in a future fusion reactor is low, so that the irradiation resistance test period of the material after the neutron irradiation can be further shortened, and the radioactive waste treatment time and the cyclic utilization period of the material can be shortened after the operation of the future fusion reactor is finished.
Drawings
FIG. 1 shows a composition of (FeVCrMn) according to the present invention 95 Ti 5 X-ray diffraction (XRD) pattern of the low activation high entropy alloy of (a);
FIG. 2 shows a composition of (FeVCrMn) according to the present invention 95 Ti 5 The microstructure of the low-activation high-entropy alloy of (4) is observed by a Scanning Electron Microscope (SEM);
FIG. 3 shows a composition of (FeVCrMn) according to the present invention 95 Ti 5 A microstructure observed by a Transmission Electron Microscope (TEM) of the low activation high entropy alloy of (a) a matrix high resolution TEM image, (b) a Ti-rich phase TEM image, (c) a spectrum of a Ti-rich phase;
FIG. 4 shows a composition of (FeVCrMn) according to the present invention 95 Ti 5 The true stress-strain curve (room temperature) of the low activation high entropy alloy of (a);
FIG. 5 shows a composition of (FeVCrMn) according to the present invention 98 Ti 2 The XRD pattern of the low-activation high-entropy alloy;
FIG. 6 shows a composition of (FeVCrMn) according to the present invention 98 Ti 2 The microstructure of the low-activation high-entropy alloy of (2) is observed by SEM;
FIG. 7 shows a composition of (FeVCrMn) according to the present invention 98 Ti 2 A microstructure of the low activation high entropy alloy of (a) a matrix high resolution TEM image, (b) a Ti-rich phase TEM image, and (c) a spectrum of the Ti-rich phase;
FIG. 8 shows a composition of (FeVCrMn) according to the present invention 98 Ti 2 The true stress-strain curve (room temperature) of the low activation high entropy alloy of (2).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
The invention discloses a low-activation high-entropy alloy, which comprises the following components (FeVCrMn) x Ti y In the chemical formula, x + y =100, x is more than or equal to 90, and y is less than or equal to 10. Wherein Fe, V, cr and Mn are the main components with equal atomic ratio
Ti is an adjusting element, and the atomic percentage is y percent. Wherein Fe, V, cr, mn and Ti are the main elements of the traditional fusion reactor structural materials such as low-activation ferrite/martensite steel and vanadium alloy. The mechanical property of high strength is achieved by adopting a strengthening method mainly of solid solution strengthening.
The solid solution strengthening low-activation high-entropy alloy has a single-phase Body Centered Cubic (BCC) structure, and the grain size is less than or equal to 200 mu m. The hardness is more than or equal to 400HV, the elastic modulus is about 200GPa, the room-temperature yield strength is more than or equal to 700MPa, and the room-temperature tensile strength is more than or equal to 1200MPa. The strength of the low-activation high-entropy alloy is far higher than that of the existing fusion reactor low-activation structural materials such as low-activation ferrite/martensite steel and vanadium alloy.
The solid solution strengthening low-activation high-entropy alloy can be (FeVCrMn) 98 Ti 2 And the alloy comprises 24.5% of Fe, V, cr and Mn in atomic fraction and 2% of Ti in atomic fraction.
A further preferred component of the solid solution strengthened low activation high entropy alloy may also be (FeVCrMn) 95 Ti 5 The alloy comprises 23.75 atomic percent of Fe, V, cr and Mn and 5 atomic percent of Ti. The increase of Ti content can obviously reduce the grain size of the alloy and improve the strength of the alloy.
The method for preparing the solid solution strengthening low-activation high-entropy alloy comprises the following steps:
1) Weighing raw material particles of Fe, V, cr, mn and Ti simple substance elements with the purity of more than or equal to 99.95 percent according to the atomic ratio, and putting the raw material particles into a water-cooled copper crucible of a vacuum arc melting furnace;
2) Vacuum arc melting is carried out. Vacuumizing the vacuum bin of the smelting furnace to less than or equal to 5 multiplied by 10 -3 Pa, then filling high-purity argon with the purity of more than or equal to 99.999 percent into the vacuum bin at the pressure of-0.8 to-0.6MPa. High-purity argon is used as protective gas and an arc medium, the smelting current is 350-450A, and cooling water is introduced during smelting to prevent the water-cooled copper plate from being melted by overheating. In order to homogenize the components and the structure of the alloy, the front and back surfaces of an alloy ingot are repeatedly smelted for 3 to 5 times, each time is kept for 3 to 6 minutes, the time of the alloy in a liquid state is 10 to 30 minutes in total, and finally the alloy ingot is cooled to obtain (FeVCrMn) x Ti y And (3) casting a low-activation high-entropy alloy ingot.
Example 1
A solid solution strengthened low-activation high-entropy alloy comprises (FeVCrMn) 95 Ti 5 Contains 23.75% of Fe, V, cr and Mn in atomic fraction and 5% of Ti in atomic fraction. Weighing raw material particles of Fe, V, cr, mn and Ti simple substance elements with the purity of more than or equal to 99.95 percent according to the atomic ratio, and putting the raw material particles into a water-cooled copper crucible of a vacuum arc melting furnace; vacuumizing the vacuum bin of the smelting furnace to less than or equal to 4 multiplied by 10 -3 Pa, and then filling high-purity argon with the purity of more than or equal to 99.999 percent until the pressure of the vacuum bin is-0.7 MPa. High-purity argon is used as a protective gas and an arc medium, the smelting current is 400A, and cooling water is fed during smelting to prevent the water-cooled copper plate from being melted by overheating. In order to homogenize the alloy components and the structure, the front and back sides of the alloy ingot are repeatedly smelted for 4 times, each time, the alloy ingot is kept for 5 minutes, and the total time of the alloy in a liquid state is 20 minutes. Finally cooling to obtain (FeVCrMn) 95 Ti 5 And (3) casting a low-activation high-entropy alloy ingot.
Measured by Archimedes drainage method (FeVCrMn) 95 Ti 5 The density of the low-activation high-entropy alloy is 7.008g/cm 3 . The hardness was measured by means of a micro Vickers hardness tester, model HVS-1000A, at about 510HV. DX-2700X-ray diffractometer pair (FeVCrMn) 95 Ti 5 Phase analysis is carried out on the low-activation high-entropy alloy, the result is shown in figure 1, and according to the lattice diffraction extinction law, diffraction peaks in a map can be determined to respectively correspond to (110), (200) and (211) crystal faces of a Body Centered Cubic (BCC) structure, (FeVCrMn) 95 Ti 5 The low activation high entropy alloy is a single phase BCC lattice structure. Calculating the lattice constant of the Bragg equation of lambda =2dsin theta
The lattice constant of the alloy is different from that of pure metal, which shows that the atoms of the alloy elements cause lattice distortion to play a role in solid solution strengthening.
The composition prepared in this example was observed by Scanning Electron Microscope (SEM) to be (FeVCrMn) 95 Ti 5 The microstructure of the low-activation high-entropy alloy of (1) is shown in FIG. 2, (FeVCrMn) 95 Ti 5 The microstructure of the low-activation high-entropy alloy is equiaxed crystal with elements uniformly distributed. As shown in FIG. 2, the Zeiss Auriga field emission scanning electron microscope is adopted to observe that the grain size is 20-70 μm, the average size is about 40 μm, the grains are finer, and the alloy structure is more uniform. The composition prepared in this example was observed by Transmission Electron Microscopy (TEM) to be (FeVCrMn) 95 Ti 5 The microstructure of the low-activation high-entropy alloy is shown in FIG. 3, wherein (a) is a matrix high-resolution TEM image, (b) is a Ti-rich phase TEM image, and (c) is a Ti-rich phase energy spectrum image. Various alloy elements are dissolved in a metal matrix, different atoms are mutually dissolved in a solid solution, serious lattice distortion is caused, and the strength of the high-entropy alloy is improved mainly in a solid solution strengthening mode. The alloy matrix component is 3.9Ti-24.1V-23.2Cr-22.5Mn-26.3Fe, and is similar to the design component. Among them, ti-rich phase with a size of about 1 μm is occasionally found, which has a composition of 10.5Ti-15.4V-16.5Cr-24.8Mn-32.9Fe (wt.%), contains slightly higher Ti and Fe contents than the matrix, is a high-entropy alloy phase with slightly segregated components, and plays a strengthening role like the matrix.
The composition prepared in this example was found to be (FeVCrMn) by cylindrical planar indentation test 95 Ti 5 The room temperature true stress-strain curve of the low activation high entropy alloy of (2) is shown in fig. 4. Calculated by a plane indentation test related theoretical formula (FeVCrMn) 95 Ti 5 The elastic modulus of the alloy is about 198GPa, the yield strength is about 1040MPa, the tensile strength is 1640MPa, the strain hardening index is 0.198, and the strain hardening coefficient is 2760. The strength of the high-entropy alloy is far higher than that of the existing fusion reactor low-activation structural materials such as low-activation ferrite/martensite steel and vanadium alloy (the room-temperature tensile strength is only 500-700 MPa).
Example 2
A solid solution strengthened low-activation high-entropy alloy comprises (FeVCrMn) 98 Ti 2 The alloy comprises 24.5 atomic percent of Fe, V, cr and Mn and 2 atomic percent of Ti. Weighing raw material particles of Fe, V, cr, mn and Ti simple substance elements with the required weight purity of more than or equal to 99.95 percent according to the atomic ratio, and putting the raw material particles into a water-cooled copper crucible of a vacuum arc melting furnace; vacuumizing the vacuum bin of the smelting furnace to 3.5 multiplied by 10 -3 Pa, and then filling high-purity argon with the purity of more than or equal to 99.999 percent until the pressure of the vacuum bin is-0.8 MPa. High-purity argon is used as a protective gas and an arc medium, the smelting current is 390A, and cooling water is fed during smelting to prevent the water-cooled copper plate from being melted by overheating. In order to homogenize the alloy components and the structure, the front and back sides of the alloy ingot are repeatedly smelted for 5 times, each time, the alloy ingot is kept for 3 minutes, and the total time of the alloy in a liquid state is 15 minutes. Finally cooling to obtain (FeVCrMn) 95 Ti 5 And (3) low-activation high-entropy alloy ingot casting.
Measured by Archimedes drainage method (FeVCrMn) 98 Ti 2 The density of the low-activation high-entropy alloy is 7.053g/cm 3 . The hardness was measured to be about 430HV using a micro Vickers hardness tester type HVS-1000A. DX-2700X-ray diffractometer pair (FeVCrMn) 98 Ti 2 And carrying out phase analysis on the low-activation high-entropy alloy. As shown in FIG. 5, according to the lattice diffraction extinction law, the diffraction peaks in the spectrum can be determined to correspond to the (110), (200) and (211) crystal planes of the BCC structure, respectively, (FeVCrMn) 98 Ti 2 The low activation high entropy alloy is a single phase Body Centered Cubic (BCC) lattice structure. From the Bragg equation, λ =2dsin θ, the lattice constant is calculated as
The lattice constant of the alloy is different from that of pure metal, which shows that the atoms of the alloy elements cause lattice distortion to play a role in solid solution strengthening.
As shown in FIG. 6, observation was performed using a Zeiss Auriga field emission scanning electron microscope (FeVCrMn) 98 Ti 2 The microstructure of the low-activation high-entropy alloy is equiaxial crystal with uniformly distributed elements, and the grain size is 20-200 mu mThe average size is about 120 mu m, the crystal grains are finer, and the alloy structure is more uniform.
FIG. 7 shows (FeVCrMn) 98 Ti 2 The TEM microstructure of the alloy is (a) a matrix high-resolution TEM image, (b) a Ti-rich phase TEM image, and (c) a Ti-rich phase energy spectrum image. Wherein, the Ti-rich phase component is 96Ti-1.95V-0.8Cr-0.07Mn-0.62Fe (wt.%), and compared with the matrix component of 0.71Ti-25.7V-27.9Cr-20.1Mn-25.6Fe (wt.%), the Ti-rich phase can be a precipitated phase, but the Ti content is very high, and the Ti-rich phase also has certain toughening effect on the alloy.
The room temperature true stress strain-curve is shown in FIG. 8, and is calculated by the related theoretical formula of plane indentation test, (FeVCrMn) 98 Ti 2 The elastic modulus of the alloy is about 202GPa, the yield strength is about 760MPa, the tensile strength is about 1290MPa, the strain hardening index is 0.204, and the strain hardening coefficient is 2180. The strength of the high-entropy alloy is far higher than that of the existing fusion reactor low-activation structural materials such as low-activation ferrite/martensite steel and vanadium alloy.
The present invention has been described in detail with reference to the drawings and examples, but the present invention is not limited to the examples, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. The present invention may be practiced without these particulars.
Claims (6)
1. One kind (FeVCrMn) x Ti y The low-activation high-entropy alloy is characterized in that (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, fe, V, cr and Mn are equal atomic ratio, x + y =100, x is more than or equal to 90 and less than 100, y is more than 0 and less than or equal to 10; (FeVCrMn) x Ti y The low-activation high-entropy alloy is a single-phase body-centered cubic BCC structure, and the grain size is less than or equal to 200 mu m.
2. A compound of claim 1 in the form of a (FeVCrMn) x Ti y A low activation high entropy alloy, characterized in that (FeVCrMn) x Ti y The hardness of the low-activation high-entropy alloy is more than or equal to 400HV, the elastic modulus is 200GPa, the room-temperature yield strength is more than or equal to 700MPa, and the room-temperature resistance isThe tensile strength is more than or equal to 1200MPa.
3. A compound of claim 1 (FeVCrMn) x Ti y Low activation high entropy alloy, characterized in that (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x =95 and y =5.
4. A compound of claim 1 (FeVCrMn) x Ti y Low activation high entropy alloy, characterized in that (FeVCrMn) x Ti y In the chemical formula of the low-activation high-entropy alloy, x =98,y =2.
5. One kind of preparation (FeVCrMn) x Ti y Method for low activation of high entropy alloys, for a (FeVCrMn) according to claim 1 x Ti y A low activation high entropy alloy, characterized in that the method comprises the steps of:
step 1, weighing raw materials of elementary substance elements of Fe, V, cr, mn and Ti according to the atomic percentage of each element, and putting the raw materials into a water-cooled copper crucible of a vacuum arc melting furnace;
and 2, carrying out vacuum arc melting on the raw materials of the Fe, V, cr, mn and Ti simple substance elements which are put into a water-cooled copper crucible of the vacuum arc melting furnace.
6. A process according to claim 5 (FeVCrMn) x Ti y The method for low-activation high-entropy alloy is characterized in that the step 2 specifically comprises the following steps: vacuumizing the vacuum chamber to less than or equal to 5 multiplied by 10 -3 Pa, filling high-purity argon to a vacuum bin with the pressure of-0.8 to-0.6 MPa, smelting current of 350 to 450A, and introducing cooling water during smelting; repeatedly smelting the front and back surfaces of the alloy ingot for 3-5 times, keeping for 3-6 minutes each time, keeping the alloy in a liquid state for 10-30 minutes in total, and finally cooling to obtain (FeVCrMn) x Ti y And (3) low-activation high-entropy alloy ingot casting.
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