CN112981210B - Nuclear medium-entropy alloy system and preparation method and application thereof - Google Patents
Nuclear medium-entropy alloy system and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nuclear medium-entropy alloy system and a preparation method and application thereof, and belongs to the technical field of medium-entropy alloy materials and preparation thereof. The FeCrV system consists of four low-activation elements of Fe, Cr, V and M (one of Ti, Mn, Ni and Zn), wherein the atomic molar ratio of Fe, Cr, V and M is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5. The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV-series medium-entropy alloy material for the nuclear is prepared by raw material treatment and material weighing proportioning and adopting a magnetic suspension (a metal raw material sample is not in contact with a crucible) arc melting mode and annealing heat treatment. The low-activation FeCrV system entropy alloy material shows excellent high-temperature thermal stability, high strength and high toughness. The medium entropy alloy is expected to be applied to ADS spallation target windows, subcritical reactor cores, fusion reactors, fourth generation nuclear fission reactor cores and structural materials or coating materials in strong acid environments or liquid metal environments.
Description
Technical Field
The invention belongs to the technical field of high/medium entropy alloy materials and preparation thereof, and particularly relates to a nuclear FeCrV (FeCrVM) system with low activation, high temperature resistance, high strength and high toughnessxM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), and a preparation method and application thereof.
Background
Nuclear energy is a low-carbon clean energy with high energy density. In China and even all over the world, the rapid development of nuclear energy is regarded as an important way to overcome the shortage of fossil energy and the treatment of environmental pollution. The service behavior of materials in extreme environments is one of the main bottlenecks restricting the use and development of nuclear energy, and the feasibility, safety and economy of a nuclear energy system are determined by material problems.
The innovation of nuclear power technology brings great promotion of nuclear energy utilization rate and safety, and simultaneously, a more severe working condition environment puts higher requirements on materials. For example, the fusion reactor first wall material (the material directly facing the plasma) needs to meet several stringent requirements: low tritium retention and penetration, excellent neutron irradiation resistance (100dpa), plasma irradiation resistance, low activation, high temperature resistance, thermal shock resistance and the like. Likewise, the in-core structural materials of fourth generation nuclear fission reactors will be subject to extremely harsh operating conditions of higher temperature, pressure and neutron flux. Therefore, developing (candidate) engineering materials that can be used in advanced nuclear energy systems such as fusion reactors, fourth generation nuclear fission reactors or accelerator driven subcritical reactor systems (ADS) is a key work in driving nuclear energy development and application.
At present, widely used steel and alloy materials and newly proposed candidate structural materials expected to be applied to future advanced nuclear energy systems have various problems, and cannot completely meet the working condition requirements of advanced nuclear energy systems such as fusion reactors, fourth-generation nuclear fission reactors and accelerator driven subcritical systems (ADS). For example: t91, 316L, 15-15Ti steel and alloy materials have the problems of insufficient high-temperature strength, non-low activation (more transmutation products after irradiation and high radioactivity level), irradiation creep, embrittlement and the like; intrinsic safety issues of Zr alloys (zirconium water reaction at high temperature to produce hydrogen); the problem of irradiation embrittlement of Fe-based RAFM steel under 0-10 dpa; the mass production process and the cost control of ODS steel, and the like; SiC, ZrO2Poor toughness of ceramic materials, difficult processing and the like; although the toughness of SiC fiber composite materials and the like is partially enhanced, multiple problems of poor thermal conductivity, composite interface combination and the like are brought. These typical problems have greatly restricted the possible applications of the above materials in future advanced nuclear power systems. The material of the high/medium entropy alloy (HEAS/MEAs) has unique high mixed entropy effect in thermodynamics and crystallographyThe special high/medium entropy alloy material has the advantages of high strength, high toughness, high hardness, high temperature resistance, high pressure resistance, corrosion resistance, irradiation resistance and the like through special component design and preparation, so that the high/medium entropy alloy (HEAS/MEAs) material has a good application prospect in the aspect of future advanced nuclear energy system candidate materials.
At present, the development of high/medium entropy alloy materials for nuclear applications is still in the beginning. Although some high/medium entropy alloy material systems are reported and researched, the high/medium entropy alloy material systems related to the articles and the patents often contain non-low activation elements such as Al, Cu and the like; in addition, the refractory high/medium entropy alloy material system designed aiming at the high strength of the material has extremely high strength performance at high temperature, but the toughness is often very poor.
Disclosure of Invention
One of the purposes of the invention is to provide a FeCrV-series medium-entropy alloy material system with low activation, high temperature resistance, high strength and high toughness.
The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV system intermediate entropy alloy material system provided by the invention consists of three low-activation elements Fe, Cr and V, wherein the atomic molar ratio of Fe, Cr and V is 1:1:1 in sequence,
furthermore, the low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV system intermediate entropy alloy material system can also comprise a fourth low-activation element M, wherein the atomic molar ratio of Fe, Cr, V and M is 1:1:1: x in sequence, x is more than or equal to 0 and less than or equal to 0.5, and M is any one of Ti, Mn, Ni and Zn.
The FeCrV-series medium entropy alloy has the performances of low neutron reaction cross section (low activation), high temperature resistance (above 1500 ℃), high strength (the yield strength reaches 1100 MPa-1525 MPa, the ultimate strength reaches 1700 MPa-2200 MPa) and high toughness (the elongation at break reaches 25% -35%).
The invention also aims to provide a preparation method of the FeCrV intermediate entropy alloy material system with low activation, high temperature resistance, high strength and high toughness.
The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV intermediate entropy alloy material system provided by the invention is prepared by a method comprising the following steps:
1) raw material treatment and material weighing and proportioning
Taking Fe, Cr and V metal simple substances as raw materials, and weighing the raw materials according to the atomic molar ratio of Fe, Cr and V of 1:1: 1;
or the like, or, alternatively,
taking Fe, Cr, V and M metal simple substances as raw materials, and weighing the materials according to the atomic molar ratio of Fe, Cr, V and M of 1:1:1: x (x is more than or equal to 0 and less than or equal to 0.5);
2) vacuum magnetic suspension arc melting
Placing the weighed metal raw materials into a non-consumable vacuum magnetic suspension induction melting furnace, vacuumizing, filling argon, and melting in a high-purity argon atmosphere of 50 Pa;
3) annealing heat treatment
And after the smelting is finished, maintaining a high-purity argon atmosphere of 50Pa, naturally cooling to room temperature, sealing the button-shaped as-cast alloy in a quartz tube filled with the high-purity argon, and performing annealing thermal aging treatment at the temperature of 800-1500 ℃ for 24-72 h to obtain the FeCrV-series intermediate entropy alloy with low activation, high temperature resistance, high strength and high toughness.
In the step 1) of the method, Fe, Cr, V and M metal simple substance blocks with the purity of more than 99.9 wt% are used as raw materials, and impurities and oxides on the surfaces of the Fe, Cr, V and M metal simple substance blocks are removed by sanding; then ultrasonically cleaning the mixture by sequentially using acetone, alcohol and deionized water, drying the mixture, and proportioning and weighing the mixture;
the ultrasonic power density adopted by the ultrasonic cleaning is 0.8W/cm2The frequency is 33Hz, and the ultrasonic cleaning time can be 5 min;
proportioning and weighing materials by adopting a high-precision balance, wherein the precision of the high-precision balance can be 0.0001 g;
in the step 2) of the method, a smelting mode that a metal raw material sample is not in contact with a crucible is adopted, so that the purity of reactants is ensured to avoid introducing other impurities in the smelting process;
the tool in step 2)The physical exercise is as follows: placing the weighed metal raw materials into a non-consumable vacuum magnetic suspension induction melting furnace, vacuumizing the non-consumable vacuum magnetic suspension arc melting furnace in which the melting raw materials are placed, and reducing the vacuum degree to 3 multiplied by 10 when the vacuum degree is reduced-3And when the pressure is Pa, filling argon, when the vacuum degree is 50Pa, stopping filling argon, repeating the steps, putting a furnace chamber of the smelting furnace in a high-purity (99.99 wt%) argon atmosphere with the vacuum degree of 50Pa, opening a smelting control switch, starting smelting, wherein the smelting current of the non-consumable vacuum arc smelting furnace is 170-220A, the single-time smelting time is 50-70 s, so that the metal simple substance raw materials are completely molten and uniformly mixed, then closing the smelting control switch, and repeatedly turning over and smelting for 5-7 times through the same method and flow after the alloy cast ingot is naturally cooled and solidified.
Wherein, a mechanical pump and a molecular pump are combined to vacuumize a non-consumable vacuum magnetic suspension arc melting furnace for placing melting raw materials;
through repeated turnover smelting, the metal elements can be fully and uniformly mixed to form a solid solution structure, so that composition segregation is avoided.
The invention further aims to provide application of the FeCrV-series medium-entropy alloy material with low activation, high temperature resistance, high strength and high toughness in nuclear energy systems (fields) and strong acid environments or liquid metal environments.
The application specifically comprises the following steps: 1) as spallation target window or spallation target structural material for accelerator driven subcritical reactor systems (ADS), and fuel cladding/assembly material for subcritical reactor core or coating material thereof;
2) the material is used as a first wall material facing plasma of a fusion reactor system or as a coating material thereof;
3) as core fuel cladding/assembly structural material or as coating material for fourth generation nuclear fission reactors;
4) used as the container material of strong acid solution and the liquid metal (wrapping) structure material or as the coating material thereof.
The invention has the beneficial effects that:
(1) compared with the traditional steel such as T91, S316, 15-15Ti steel and the likeAnd alloys, the FeCrV system (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), the entropy alloy material adopts low activation elements such as Fe, Cr, V, M (Ti, Mn, Ni and Zn) and the like, the nuclear reaction section of the entropy alloy material to particles such as high-energy protons, neutrons and the like is smaller, the generated transmutation activation products are fewer, and the induced radioactivity of the nuclear energy device using the entropy alloy system in the FeCrV system as a structural material is greatly reduced. Low activation characteristic, is FeCrV system (FeCrVM)xM is one of important characteristics and nuclear application bases of the entropy alloy, wherein x is more than or equal to 0 and less than or equal to 0.5.
(2) Compared with traditional steel and alloy such as T91, S316 and the like, the FeCrV system (FeCrVM) of the inventionxM is Ti, Mn, Ni and Zn, x is more than or equal to 0 and less than or equal to 0.5), the usage amount of Cr element and V element is greatly increased, and the atomic molar ratio of the three elements of Fe, Cr and V is about 1:1:1 to form the three-principal-element alloy. A large number of metallurgical research results show that the high temperature resistance and the corrosion resistance of the traditional Fe-based steel and the traditional alloy can be improved due to the increased content of Cr and V elements. For the invention, the FeCrV mid-entropy alloy with larger Cr and V contents has extremely excellent high-temperature stability and acid corrosion resistance; and adding a small amount of M (Ti, Mn, Ni, Zn) elements with the molar ratio of x being more than or equal to 0 and less than or equal to 0.5 to FeCrV system (FeCrVM)xM ═ Ti, Mn, Ni, and Zn, x is 0 or more and 0.5 or less) and the grain size, crystal orientation, precipitates, grain boundaries, and the like of the entropy alloy material are adjusted to achieve the effects of high strength, high toughness, radiation resistance, and the like. The designed component distribution ratio and the high/medium entropy alloy material performance adjustable cocktail effect calculated by a thermodynamic phase diagram are FeCrV systems (FeCrVM)xM is one of important characteristics and nuclear application bases of the entropy alloy, wherein x is more than or equal to 0 and less than or equal to 0.5.
(3) FeCrV line (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, x is more than or equal to 0 and less than or equal to 0.1), when the content of the doping element M is small (x is more than or equal to 0 and less than or equal to 0.1), the entropy alloy has a single Body Centered Cubic (BCC) structure and does not have a second phase; and when the content of the M element is more than 0.1, the FeCrV system (FeCrVM) of the inventionx，M＝Ti、Mn、Ni、Zn，0.1<x is less than or equal to 0.5) the medium entropy alloy has a BCC + Laves two-phase structure which is essentially BCC + Laves doublePhase (Fe)1-2xCrV phase and MxFe2xPhase) coherent solid solution structure which overall exhibits the atomic structural features of BCC lattice order and chemical protogen disorder arrangement. Compared with the reported face-centered cubic (FCC) high-entropy alloy (such as FeCoNiCr-based high-entropy alloy), the material with the BCC structure and the BCC + Laves two-phase structure is more resistant to irradiation, and has stronger holding capacity for nuclear reaction transmutation gas elements such as H, He and the like. The lattice order and chemical element disorder arrangement of the BCC structure and the BCC + Laves two-phase structure are FeCrV system (FeCrVM)xM is one of important characteristics and nuclear application bases of the entropy alloy, wherein x is more than or equal to 0 and less than or equal to 0.5.
(4) Specifically, the FeCrV system (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, x is more than or equal to 0 and less than or equal to 0.5) and has the characteristics of good high temperature resistance, high strength, high toughness, radiation resistance, acid corrosion resistance and the like.
Through thermogravimetry/differential thermal analysis and X-ray diffraction tests, when the highest test temperature reaches 1500 ℃, the mass change of the sample is within 0.05 percent, and the sample always keeps the original body-centered cubic BCC structure or BCC + Laves two-phase structure and is very stable. This means that FeCrV intermediate entropy alloys are difficult to oxidize and decompose at high temperatures, and have extremely excellent high-temperature thermal stability (high temperature resistance). Through series tests of compression mechanics, the yield strength of the entropy alloy in the FeCrV system reaches 1100 MPa-1525 MPa, the ultimate strength reaches 1700 MPa-2200 MPa, and the elongation at break reaches 25% -35%; for comparison, the T91 steel had a yield strength of 625MPa, an ultimate strength of 800MPa, and an elongation at break of 22%. Obviously, compared with the traditional steel such as T91 and other materials, the intermediate entropy alloy of the FeCrV system has the characteristics of ultrahigh strength and high toughness, and the toughness of the intermediate entropy alloy is not weakened or even increased while the strength is greatly improved. Through acid corrosion and metallographic corrosion experiments, the traditional medium carbon alloy steel (such as TiV alloy steel) is added with picric acid (C) in dilute hydrochloric acid (HCl)6H3N3O7) The obvious over-corrosion phenomenon (the grain boundary is completely corroded and penetrated) is already shown after 2min of corrosion in a weakly acidic corrosion solution, while the surface of the entropy alloy in the FeCrV system can not be corroded at all even if the surface of the entropy alloy in the acidic corrosion solution with the same formula is corroded for 30minIn aqua regia (concentrated hydrochloric acid (HCl) and concentrated nitric acid (HNO)3) The mixture is composed of 3:1 in volume ratio) strong acid corrosive liquid, or obvious grain boundaries can not be corroded for 60min, which shows that the FeCrV intermediate entropy alloy shows extremely excellent acid corrosion resistance.
(5) FeCrV line (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), is prepared by a vacuum induction/arc melting method, and has relatively simple preparation method and production process, thereby facilitating the large-scale production of the intermediate entropy alloy material in the FeCrV system and effectively reducing the production cost, which is one of the nuclear application bases.
The application prospect of the invention is as follows:
(1) FeCrV line (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), the medium entropy alloy is expected to be applied to a spallation target window or a spallation target structural material of an accelerator-driven subcritical reactor system (ADS), and a fuel cladding/component material of a subcritical reactor core or a coating material thereof to resist extreme working condition environments of high temperature (400-1000 ℃), strong neutron/proton mixed spectrum irradiation (10 dpa/year) and high local stress (about 600 MPa-800 MPa at most).
(2) FeCrV line (FeCrVM) of the present inventionxAnd M is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), and the alloy has the excellent characteristics of low tritium retention, excellent neutron/plasma irradiation resistance, low activation, high temperature resistance, thermal shock resistance and the like, and is expected to be applied to a first wall material facing plasma of a future fusion reactor system or used as a coating of the first wall material.
(3) FeCrV line (FeCrVM) of the present inventionxAnd M is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5), and the medium-entropy alloy has excellent characteristics of low activation, high temperature resistance, high strength (high pressure resistance), high toughness, neutron irradiation resistance and the like, and is expected to be applied to structural materials of reactor core fuel cladding/components and the like of fourth-generation nuclear fission reactors or used as coating materials of the structural materials.
(4) FeCrV line (FeCrVM) of the present inventionxM is Ti, Mn, Ni and Zn, x is more than or equal to 0 and less than or equal to 0.5), and is expected to be applied to strong acid and liquid metal corrosion resistance due to extremely excellent acid and liquid metal corrosion resistanceSolution container materials and liquid metal (cladding) construction materials or as coating materials therefor.
Aiming at the background of material requirements of an advanced nuclear energy system, the components of an alloy material are designed and prepared by smelting through the neutron screening low-activation element analysis, the thermodynamic phase diagram calculation and the like, a FeCrV system intermediate entropy alloy system which gives consideration to low activation, high temperature resistance, high strength, high toughness and acid corrosion resistance is developed, and the possible application range of the intermediate entropy alloy system in ADS, a fusion reactor and a fourth-generation fission reactor is given by combining the performance tests and the characteristics of typical force, heat, irradiation resistance, corrosion resistance and the like.
Drawings
FIG. 1 shows FeCrV and FeCrVTi prepared in examples 1 and 3 of the present invention0.1And (3) an X-ray diffraction pattern of the medium-entropy alloy material.
FIG. 2 shows FeCrVMn prepared in example 7 and example 8 of the present invention0.3And FeCrVNi0.1And (3) an X-ray diffraction pattern of the medium-entropy alloy material.
FIG. 3 shows FeCrVTi prepared in example 3 of the present invention0.1And (3) a surface topography image of the medium-entropy alloy material observed by a Scanning Electron Microscope (SEM).
FIG. 4 is a Transmission Electron Microscope (TEM) observation result of the entropy alloy material in FeCrV prepared in example 1 of the present invention, wherein A is a local TEM image of the entropy alloy in FeCrV, B, C and D are EDS energy spectrum surface scanning distribution diagrams for the A region, and E is an EDS element energy spectrum analysis result for the A region.
FIG. 5 is a graph showing the thermogravimetric/differential thermal analysis of the entropy alloy material in FeCrV prepared in example 1 of the present invention, the sample mass percentage varies with temperature.
FIG. 6 shows FeCrVTi prepared in examples 1, 2, 3, 4, 5 and 6xEngineering stress-strain curve diagram in the compression mechanical property test of the medium entropy alloy material.
FIG. 7 is a comparison of the metallographic corrosion results of the photograph of the entropy alloy in FeCrV and the medium carbon alloy steel prepared in example 1 of the present invention (A is the entropy alloy in FeCrV, and B is the medium carbon alloy in TiV).
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
The invention provides a FeCrV system intermediate entropy alloy material system with low activation, high temperature resistance, high strength and high toughness, which consists of three low-activation elements Fe, Cr and V, wherein the atomic molar ratio of Fe, Cr and V is 1:1:1 in sequence,
furthermore, the low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV system intermediate entropy alloy material system can also comprise a fourth low-activation element M, wherein the atomic molar ratio of Fe, Cr, V and M is 1:1:1: x in sequence, x is more than or equal to 0 and less than or equal to 0.5, and M is any one of Ti, Mn, Ni and Zn.
The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV intermediate entropy alloy material system provided by the invention is prepared by a method comprising the following steps:
1) raw material treatment and material weighing and proportioning
Taking Fe, Cr, V and M metal simple substances as raw materials, and weighing the materials according to the atomic molar ratio of Fe, Cr, V and M of 1:1:1: x (x is more than or equal to 0 and less than or equal to 0.5); taking Fe, Cr and V metal simple substances as raw materials, and weighing the raw materials according to the atomic molar ratio of Fe, Cr and V of 1:1: 1;
or the like, or, alternatively,
taking Fe, Cr, V and M metal simple substances as raw materials, and weighing the materials according to the atomic molar ratio of Fe, Cr, V and M of 1:1:1: x (x is more than or equal to 0 and less than or equal to 0.5);
2) vacuum magnetic suspension arc melting
Placing the weighed metal raw materials into a non-consumable vacuum magnetic suspension induction melting furnace, vacuumizing, filling argon, and melting in a high-purity argon atmosphere of 50 Pa;
3) annealing heat treatment
And after the smelting is finished, maintaining a high-purity argon atmosphere of 50Pa, naturally cooling to room temperature, sealing the button-shaped as-cast alloy in a quartz tube filled with the high-purity argon, and performing annealing thermal aging treatment at the temperature of 800-1500 ℃ for 24-72 h to obtain the FeCrV-series intermediate entropy alloy with low activation, high temperature resistance, high strength and high toughness.
The invention also provides application of the FeCrV intermediate entropy alloy material with low activation, high temperature resistance, high strength and high toughness in a nuclear energy system (field) and a strong acid environment or a liquid metal environment.
Aiming at the background of material requirements of an advanced nuclear energy system, the components of an alloy material are designed and prepared by smelting through the neutron screening low-activation element analysis, the thermodynamic phase diagram calculation and the like, a FeCrV system intermediate entropy alloy system which gives consideration to low activation, high temperature resistance, high strength, high toughness and acid corrosion resistance is developed, and the possible application range of the intermediate entropy alloy system in ADS, a fusion reactor and a fourth-generation fission reactor is given by combining the performance tests and the characteristics of typical force, heat, irradiation resistance, corrosion resistance and the like.
Example 1
The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV intermediate entropy alloy for the core consists of three low-activation elements Fe, Cr and V, wherein the atomic molar ratio of Fe, Cr and V is 1:1: 1. The preparation method of the FeCrV entropy alloy specifically comprises the following steps:
firstly, removing impurities and oxides on the surfaces of Fe, Cr, V and M metal simple substance blocks with the purity of more than 99.9 wt% by sanding; then sequentially cleaning with acetone, alcohol and deionized water in an ultrasonic cleaner for 5min (ultrasonic power density of 0.8W/cm)2And the frequency is 33Hz), and clean Fe, Cr, V and M metal simple substances are obtained for later use after being dried by a blower. The spare metal simple substance is proportioned and weighed by a high-precision balance (the precision is 0.0001g), wherein the mass percentages of Fe, Cr and V are 35.17%, 32.75% and 32.08% in sequence. The mass of the ingot contained in the water-cooled copper crucible used for the experiment is 10g (the specific ingot mass can be set according to the needs of experiment operators and the equipment capacityAnd (3) determining, namely weighing the Fe, Cr and V metal simple substances according to the mass percentage multiplied by the total mass of the cast ingot, namely 3.517g, 3.275g and 3.208g in sequence, and then placing the weighed Fe, Cr and V metal simple substances in a non-consumable vacuum magnetic suspension induction/electric arc melting furnace.
Step 2, vacuumizing and filling argon: the mechanical pump and the molecular pump are combined to vacuumize a non-consumable vacuum magnetic suspension arc melting furnace for placing melting raw materials, and when the vacuum degree is reduced to 3 multiplied by 10-3When Pa, closing the mechanical pump, the molecular pump and the valve; then, an argon filling valve is opened, argon filling is started, and when the vacuum degree is 50Pa, the argon filling valve is closed. The steps are repeated for five times, and finally the furnace chamber of the smelting furnace is placed in a high-purity (99.99 wt%) argon atmosphere with the vacuum degree of 50 Pa.
Step 3, smelting and annealing heat treatment: based on the above-mentioned condition of high-purity argon atmosphere of 50Pa, a melting control switch was turned on to start melting. The smelting current of the non-consumable vacuum arc smelting furnace is about 190A, the single smelting time is usually 60s, so that metal simple substances Fe, Cr and V are completely molten and uniformly mixed, then a smelting control switch is closed, and after the alloy cast ingot is naturally cooled and solidified, the alloy cast ingot is repeatedly turned and smelted by the same method, 60s are smelted each time, and 5-7 times are smelted in total. Through repeated turnover smelting, the four elements can be fully and uniformly mixed to form a solid solution structure, so that composition segregation is avoided. After the smelting is finished, maintaining a high-purity argon atmosphere of 50Pa, naturally cooling to room temperature in a water-cooled copper crucible, sealing the button-shaped cast alloy in a quartz tube filled with the high-purity argon, and carrying out annealing thermal aging treatment at 1000 ℃ for 24 h. So far, the preparation of FeCrV intermediate entropy alloy is completed.
Example 2
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVTi for nucleus0.05The medium-entropy alloy consists of four low-activation elements of Fe, Cr, V and Ti, wherein the atomic molar ratio of the Fe, Cr, V and Ti is 1:1:1: 0.05. FeCrVTi0.05The preparation method of the medium entropy alloy specifically comprises the steps of example 1.
The present embodiment is different from embodiment 1 in that: fe. The mass percentages of Cr, V and Ti are 34.65%, 32.26%, 31.60% and 1.48% in sequence, namely the metal simple substances of Fe, Cr, V and Ti are weighed to be 3.465g, 3.226g, 3.160g and 0.148g in sequence.
Otherwise as in example 1 FeCrVTi0.05And finishing the preparation of the medium-entropy alloy. .
Example 3
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVTi for nucleus0.1The medium-entropy alloy consists of four low-activation elements of Fe, Cr, V and Ti, wherein the atomic molar ratio of the Fe, Cr, V and Ti is 1:1:1: 0.1. FeCrVTi0.1The preparation method of the medium entropy alloy specifically comprises the steps of example 1.
The present embodiment is different from embodiment 1 in that: fe. The mass percentages of Cr, V and Ti are 34.14%, 31.79%, 31.14% and 2.93% in sequence, namely weighing the elementary metals of Fe, Cr, V and Ti as 3.414g, 3.179g, 3.114g and 0.293g in sequence.
Otherwise as in example 1 FeCrVTi01And finishing the preparation of the medium-entropy alloy.
Example 4
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVTi for nucleus0.2The medium-entropy alloy consists of four low-activation elements of Fe, Cr, V and Ti, wherein the atomic molar ratio of the Fe, Cr, V and Ti is 1:1:1: 0.2. FeCrVTi0.2The preparation method of the medium entropy alloy specifically comprises the steps of example 1.
The present embodiment is different from embodiment 1 in that: fe. The mass percentages of Cr, V and Ti are 33.17%, 30.89%, 30.26% and 5.69% in sequence, namely the simple metals of Fe, Cr, V and Ti are weighed to be 3.317g, 3.089g, 3.026g and 0.569g in sequence.
Otherwise as in example 1 FeCrVTi0.2And finishing the preparation of the medium-entropy alloy.
Example 5
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVTi for nucleus0.3The medium-entropy alloy consists of four low-activation elements of Fe, Cr, V and Ti, wherein the atomic molar ratio of the Fe, Cr, V and Ti is 1:1:1: 0.3. FeCrVTi0.3Preparation method of medium-entropy alloyThe method specifically comprises the steps of example 1.
The present embodiment is different from embodiment 1 in that: fe. The mass percentages of Cr, V and Ti are 32.26%, 30.03%, 29.42% and 8.29% in sequence, namely the simple metals of Fe, Cr, V and Ti are weighed to be 3.226g, 3.003g, 2.942g and 0.829g in sequence.
Otherwise as in example 1 FeCrVTi0.3And finishing the preparation of the medium-entropy alloy.
Example 6
The low-activation, high-temperature-resistant, high-strength and high-toughness FeCrV intermediate entropy alloy for the core consists of three low-activation elements Fe, Cr and V, wherein the atomic molar ratio of Fe, Cr and V is 1:1: 1. The preparation method of the FeCrV entropy alloy specifically comprises the steps of the method in the embodiment 1.
The present embodiment is different from embodiment 1 in that: directly taking out the button-shaped as-cast FeCrV mid-entropy alloy from the water-cooled copper crucible without annealing thermal aging treatment at 1000 ℃.
Otherwise, FeCrV was prepared as in example 1 without aging.
Example 7
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVMn for nucleusxThe medium-entropy alloy consists of four low-activation elements Fe, Cr, V and Mn, wherein the atomic molar ratio of the four elements Fe, Cr, V and Mn is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5. FeCrVMnxThe preparation method of the medium entropy alloy specifically comprises the steps of 1-6.
The present embodiment is different from embodiments 1 to 6 in that: the Ti element is replaced by the Mn element, and the corresponding weighing mass is also changed (but always follows the relationship that the atomic molar ratio of the four elements of Fe, Cr, V and Mn is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5).
FeCrVMn, as in examples 1-6xAnd finishing the preparation of the medium entropy alloy and the non-aging material thereof.
Example 8
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVNi for coresxThe medium entropy alloy consists of four low-activation elements of Fe, Cr, V and Ni, wherein the Fe, Cr, V, Ni and Cr are selected from the group consisting of Cu, Ni, and Ni, wherein the Fe, Cr, V, and Ni are selected from the group,The atomic molar ratio of the four elements of Ni is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5. FeCrVNixThe preparation method of the medium entropy alloy specifically comprises the steps of 1-6.
The present embodiment is different from embodiments 1 to 6 in that: the Ti element is changed into the Ni element, and the corresponding weighing mass is also changed (but always follows the relationship that the atomic molar ratio of the four elements of Fe, Cr, V and Ni is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5).
FeCrVNi as in examples 1 to 6xAnd finishing the preparation of the medium entropy alloy and the non-aging material thereof.
Example 9
Low-activation, high-temperature-resistant, high-strength and high-toughness FeCrVZn for nucleusxThe medium-entropy alloy consists of four low-activation elements Fe, Cr, V and Zn, wherein the atomic molar ratio of the four elements Fe, Cr, V and Zn is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5. FeCrVZnxThe preparation method of the medium entropy alloy specifically comprises the steps of 1-6.
The present embodiment is different from embodiments 1 to 6 in that: the Ti element is replaced by the Zn element, and the corresponding weighing mass is also changed (but always follows the relationship that the atomic molar ratio of the four elements of Fe, Cr, V and Zn is 1:1:1: x, and x is more than or equal to 0 and less than or equal to 0.5).
FeCrVZn as in examples 1 to 6xAnd finishing the preparation of the medium entropy alloy and the non-aging material thereof.
Aiming at FeCrV and FeCrVTi prepared in example 1 and example 3 of the invention0.1The results of X-ray diffraction (XRD) tests on the medium-entropy alloy material are shown in figure 1, and FeCrV and FeCrVTi prepared by the method0.1The medium entropy alloys are all standard Body Centered Cubic (BCC) structures. In fact, for all FeCrV lines (FeCrVM)xM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.1), and the BCC structure is presented according to the rule.
FeCrVMn prepared according to example 7 and example 8 of the invention0.3And FeCrVNi0.1The results of X-ray diffraction (XRD) tests on the medium-entropy alloy material are shown in FIG. 2, and when the content of the doping element M (Ni in the embodiment) is small (X is more than or equal to 0 and less than or equal to 0.1), the medium-entropy alloy material has a single body coreCubic (BCC) structure; and FeCrVMn when the content of the doping element M (Mn in this example) is more than 0.10.3Similar in structure, the FeCrV system (FeCrVM) of the present inventionx，M＝Ti、Mn、Ni、Zn，0.1<x is less than or equal to 0.5) the medium entropy alloys have a BCC + Laves two-phase structure.
Aiming at FeCrVTi prepared in embodiment 3 of the invention0.1The Scanning Electron Microscope (SEM) surface topography of the medium entropy alloy material is shown in FIG. 3. The photograph is universal and similar to the surface shown in FIG. 3, and the FeCrV system (FeCrVM) prepared by smeltingxM is Ti, Mn, Ni and Zn, and x is more than or equal to 0 and less than or equal to 0.5).
The Transmission Electron Microscope (TEM) observation result of the entropy alloy material in FeCrV prepared in example 1 of the present invention is shown in fig. 4, where a is a transmission observation region, B, C and D are X-ray characteristic element energy spectra (EDS) of the a region, respectively, and E is a result of performing surface scanning EDS on the a region. EDS energy spectrum and transmission electron microscope results show that: the prepared FeCrV system entropy alloy has the element components and proportion completely consistent with the designed target, and the elements are uniformly distributed without other impurities or impure phases, segregation, casting defects and the like.
The thermogravimetric test is carried out on the FeCrV entropy alloy material prepared in the embodiment 1 of the invention, and the specific test result is shown in FIG. 5, wherein the temperature is increased from room temperature to 1500 ℃, and the mass percentage of the FeCrV entropy alloy sample is basically kept unchanged, which shows that the FeCrV high/intermediate entropy alloy material has good high-temperature thermal stability and can resist high temperature.
Aiming at FeCrVTi prepared in example 1, example 2, example 3, example 4, example 5 and example 6 of the inventionxThe medium entropy alloy material is subjected to a mechanical compression test, and a specific test result is shown in fig. 6, wherein the yield strength of the medium entropy alloy material reaches 1100-1525 MPa, the ultimate strength of the medium entropy alloy material reaches 1700-2200 MPa, and the elongation at break of the medium entropy alloy material reaches 25% -35%, which shows that the FeCrV high/medium entropy alloy material has excellent high strength and high toughness.
The result of metallographic corrosion observation of the entropy alloy in FeCrV prepared in example 1 of the present invention is shown in fig. 7. At the contrast knotIn FIG. 7 (B), medium carbon alloy steel (TiV alloy steel) is treated with picric acid (C) in dilute hydrochloric acid (HCl)6H3N3O7) The obvious over-corrosion phenomenon (the grain boundary is completely corroded and penetrated) is already shown after 2min of corrosion in a weakly acidic corrosive solution, but the entropy alloy in FeCrV is added with picric acid (C) in dilute hydrochloric acid (HCl) with the same proportion6H3N3O7) The corrosion in weakly acidic corrosive liquid for 60min still has no corrosion phenomenon, even in aqua regia (concentrated hydrochloric acid (HCl) and concentrated nitric acid (HNO)3Mixture composed of 3:1 in volume ratio) strong acid corrosive liquid, or no obvious grain boundary can be corroded for 60min, as shown in fig. 7 (a), which shows that the FeCrV series high/medium entropy alloy of the invention shows good corrosion resistance.
Claims (5)
1. A FeCrV system intermediate entropy alloy material system with low activation, high temperature resistance, high strength and high toughness is composed of three low activation elements of Fe, Cr and V, wherein the atomic molar ratio of Fe, Cr and V is 1:1:1 in sequence; the FeCrV system entropy alloy material system also comprises a fourth low-activation element M, wherein the atomic molar ratio of Fe, Cr, V and M is 1:1:1: x in sequence, x is more than 0.1 and less than or equal to 0.5, M is any one of Ni and Zn, and the FeCrV system entropy alloy material system has a BCC + Laves two-phase structure.
2. The method for preparing the FeCrV system medium entropy alloy material system with low activation, high temperature resistance, high strength and high toughness of claim 1 comprises the following steps:
1) raw material treatment and material weighing and proportioning
Taking Fe, Cr, V and M metal simple substances as raw materials, weighing the materials according to the atomic molar ratio of Fe, Cr, V and M of 1:1:1: x, wherein x is more than 0.1 and less than or equal to 0.5, wherein M is any one of Ni and Zn,
2) vacuum magnetic suspension arc melting
Placing the weighed metal raw materials into a non-consumable vacuum magnetic suspension induction melting furnace, vacuumizing, filling argon, and melting in a high-purity argon atmosphere of 50 Pa;
3) annealing heat treatment
And after the smelting is finished, maintaining a high-purity argon atmosphere of 50Pa, naturally cooling to room temperature, sealing the button-shaped as-cast alloy in a quartz tube filled with the high-purity argon, and performing annealing thermal aging treatment at the temperature of 800-1500 ℃ for 24-72 h to obtain the FeCrV-series intermediate entropy alloy with low activation, high temperature resistance, high strength and high toughness.
3. The method for preparing the FeCrV system medium entropy alloy material system with low activation, high temperature resistance, high strength and high toughness according to claim 2, is characterized in that: the operation of step 2) is: placing the weighed metal raw materials into a non-consumable vacuum magnetic suspension induction melting furnace, vacuumizing the non-consumable vacuum magnetic suspension arc melting furnace in which the melting raw materials are placed, and reducing the vacuum degree to 3 multiplied by 10 when the vacuum degree is reduced-3And when the pressure is Pa, filling argon, when the vacuum degree is 50Pa, stopping filling argon, repeating the steps, putting a furnace chamber of the smelting furnace in a high-purity argon atmosphere with the vacuum degree of 50Pa, opening a smelting control switch, starting smelting, wherein the smelting current of the non-consumable vacuum arc smelting furnace is 170-220A, the single smelting time is 50-70 s, completely and uniformly melting and mixing the metal simple substance raw materials, then closing the smelting control switch, and repeatedly turning and smelting the alloy ingot by the same method and flow after the alloy ingot is naturally cooled and solidified, wherein the total smelting time is 5-7 times.
4. The use of a low activation, high temperature resistant, high strength, high toughness FeCrV system of an entropic alloy material system of claim 1 in a nuclear energy system or in a strongly acidic environment or in a liquid metal environment.
5. The use of a low activation, high temperature resistant, high strength, high toughness FeCrV system entropy alloyed material system as claimed in claim 4, wherein: the application is as follows:
1) the material is used as a spallation target structural material, a subcritical reactor core assembly material or a coating material of the core assembly material of an accelerator-driven subcritical reactor system;
2) the material is used as a first wall material facing plasma of a fusion reactor system or a coating material of the first wall material facing plasma;
3) as a core fuel cladding for a fourth generation nuclear fission reactor or as a coating material for a core fuel cladding for a fourth generation nuclear fission reactor;
4) a coating material for a strongly acidic solution container material, a liquid metal-clad structural material or a liquid metal-clad structural material.
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