CN114807770A - High-strength and high-toughness multilevel heterogeneous FeCrNiAl-based alloy material and preparation method thereof - Google Patents
High-strength and high-toughness multilevel heterogeneous FeCrNiAl-based alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength and high-toughness multilevel heterogeneous FeCrNiAl-based alloy material and a preparation method thereof; the alloy material comprises the following components in atomic percentage: 40-60%, Cr: 15-35%, Ni: 10-30%, Al: 5-15% and the content of other elements is less than or equal to 5%. According to the invention, multiple strengthening mechanisms are introduced simultaneously through structure regulation and process optimization, so that the yield strength of the alloy is improved by more than 2.5 times compared with that of the as-cast coarse-grain alloy, and the alloy has good tensile plasticity. The preparation method of the invention is casting and deformation heat treatment, and the multi-grade isomeric alloy material jointly composed of a multi-scale FCC matrix phase, a multi-scale B2 and a sigma reinforcing phase is obtained. The heterogeneous microstructure of the invention effectively improves the strength of the material and keeps good tensile plasticity, meets the urgent requirements of high strength and high toughness of advanced structural materials, has simple and efficient preparation process, and is suitable for the requirement of large-scale production.
Description
Technical Field
The invention belongs to the technical field of high-performance alloy materials, and particularly relates to a high-strength and high-toughness multilevel heterogeneous FeCrNiAl-based alloy material and a preparation method thereof.
Technical Field
The performance of the nuclear fuel cladding, which serves as a first safety barrier for a nuclear reactor, is directly related to the reliability and safety of the operation of the nuclear reactor. Zirconium alloy is the only cladding material adopted by the current light water reactor nuclear fuel element. However, in 2011 of nuclear accidents in fukushima of japan, the zirconium alloy cladding reacts with high-temperature cooling water, generating a large amount of heat and hydrogen, causing core melting and hydrogen explosion, exposing fatal defects of the zirconium alloy. Therefore, the development of accident-tolerant fault-tolerant type nuclear fuel cladding material for the nuclear reactor is urgently needed by various countries, and a larger safety margin is provided under the condition of a serious accident so as to improve the safety and the reliability of the operation of the nuclear reactor.
Among the current numerous candidate materials, the FeCrNiAl alloy has excellent corrosion resistance, high-temperature steam oxidation resistance and good radiation resistance due to the contained elements such as Al and Cr, and meanwhile, the raw materials and the preparation process of the FeCrNiAl alloy have good economy and maturity, so the FeCrNiAl alloy is one of the most promising accident-resistant cladding materials at present. On the other hand, the severe use environment requires that the wall thickness of the FeCrNiAl alloy cladding tube needs to be reduced to be less than 0.4mm, which puts forward the severe requirement on the mechanical property of the FeCrNiAl alloy cladding tube, but the FeCrNiAl alloy reported in the prior art rarely has both high strength (yield strength is more than or equal to 900MPa) and high plasticity (elongation after fracture is more than or equal to 15%). Therefore, a novel FeCrNiAl-based alloy and a preparation process thereof need to be developed, so that the strength and the plasticity of the alloy are greatly improved, and the harsh requirement of an accident-resistant cladding material of a nuclear reactor is met.
Heterostructural alloys (heterostructural alloys) refer to alloys that have significant structural differences within the alloy from one region to another. The regional interface in the heterostructure alloy generates obvious strain gradient during deformation, and the heterostructure interface forms a large amount of geometrical dislocation to coordinate deformation, so that effective back stress strengthening is induced, and the alloy has excellent combination of high strength and high plasticity. In recent years, research teams such as Luoke, Wuxianlei, Zhu Yuan and the like have succeeded in preparing copper alloy, steel and titanium alloy with heterostructure, and the introduction of heterostructure into alloy has become one of important ideas for preparing high-performance alloy Materials (Science (2014)345, 1455-. However, the idea of constructing the heterostructure is not applied in the FeCrNiAl-based alloy, so that the preparation of the FeCrNiAl-based alloy material with multilevel isomerism can not only greatly improve the strong plasticity of the alloy system, meet the rigorous requirements of the nuclear fuel cladding tube on mechanical properties, but also provide reference value for preparing other high-performance alloy materials.
Disclosure of Invention
The invention discloses a high-toughness multistage isomeric FeCrNiAl-based alloy and a preparation method thereof, aiming at the problem that the FeCrNiAl-based alloy needs to improve the mechanical property urgently. The invention carries out simple plastic deformation and two-step processing of heat treatment on the alloy cast ingot to obtain a heterostructure microstructure composed of a multi-scale FCC matrix, a multi-scale B2 and a sigma reinforcing phase, so that the heterostructure microstructure generates back stress induced strengthening, strong precipitated phase dispersion strengthening and effective grain boundary strengthening, a multi-phase and multi-scale multi-stage heterogeneous FeCrNiAl-based alloy material is constructed, and the preparation of the high-performance alloy material with high strength and high plasticity, low cost and short process is realized.
The purpose of the invention is realized by the following technical scheme:
a high-strength and high-toughness multistage-isomeric FeCrNiAl-based alloy material comprises the following components in atomic percentage (at.%): 40-60%, Cr: 15-35%, Ni: 10-30%, Al: 5-15% and the content of other elements is less than or equal to 5%.
Preferably, the other element includes at least one of Mn, Ti, Co, and C.
Preferably, the high-toughness multi-stage isomeric FeCrNiAl-based alloy is of a multi-phase structure and comprises an FCC matrix phase, a B2 reinforcing phase and a sigma reinforcing phase; wherein the sum of the volume fractions of the B2 reinforcing phase and the sigma reinforcing phase is 5-25%, and the B2 reinforcing phase and the sigma reinforcing phase are uniformly dispersed in the alloy.
Preferably, the grain sizes of the matrix phase and the reinforcing phase of the high-toughness multistage-isomeric FeCrNiAl-based alloy material present multi-scale gradient distribution of nanocrystalline, ultrafine grain and fine grain.
Preferably, the yield strength sigma of the high-strength and high-toughness multistage-isomeric FeCrNiAl-based alloy 0.2 850-1200 MPa, tensile strength sigma UTS 1100-1500 MPa, and the elongation after fracture is more than or equal to 15%.
The preparation method of the high-strength and high-toughness multistage-isomerism FeCrNiAl-based alloy material adopts a casting, plastic deformation and heat treatment process, and comprises the following steps of:
(1) preparing raw materials according to the following atomic percentages: fe: 40-60%, Cr: 15-35%, Ni: 10-30%, Al: 5-15%, and the content of other elements is less than or equal to 5%;
(2) placing the prepared raw materials in a smelting furnace, repeatedly smelting for 3-6 times to ensure that the components are uniformly distributed, and cooling to obtain an alloy block;
(3) performing plastic deformation treatment on the alloy block obtained in the step (2), wherein the total deformation is controlled to be 60-95%;
(4) and (4) carrying out annealing heat treatment on the FeCrNiAl-based alloy subjected to plastic deformation treatment obtained in the step (3) to obtain the high-strength and high-toughness multistage heterogeneous FeCrNiAl-based alloy material.
Preferably, the raw material is an elemental block or powder.
Preferably, the smelting process in the step (2) comprises vacuum arc smelting, vacuum induction smelting and suspension smelting.
Further preferably, the vacuum arc melting is specifically: and in the smelting process, firstly, vacuumizing to 3Pa, introducing high-purity argon, vacuumizing, repeatedly washing the furnace twice to ensure a high-purity vacuum environment, smelting induction current of 300-400A, carrying out electromagnetic stirring in the alloy smelting process, smelting for 4-5 times, and then casting into a copper mold to be cooled to obtain an alloy ingot.
Preferably, the plastic deformation process of step (3) is a cold rolling or forging process.
Further preferably, the number of cold rolling is 5-15, and the total deformation is 60-95%; the forging ratio of the forging process is 3-10.
Preferably, the total deformation amount in the step (3) is 75-90%.
Preferably, the temperature of the annealing heat treatment in the step (4) is 700-1100 ℃, and the time is 0.5-6 hours.
Further preferably, the temperature of the annealing heat treatment in the step (4) is 800 to 1000 ℃.
After plastic deformation and heat treatment, the high-strength high-plasticity multistage isomeric FeCrNiAl high-entropy alloy is obtained, the microstructure of the alloy consists of a multi-scale FCC matrix phase, a multi-scale B2 and a sigma reinforcing phase, the tensile strength is greatly improved, and the alloy has high plasticity and excellent comprehensive mechanical properties.
Compared with the prior art, the invention has the following advantages:
(1) the invention can obtain a multi-scale FCC phase matrix by utilizing two simple steps of plastic deformation and heat treatment, introduces a multi-scale B2 precipitated phase and a multi-scale sigma precipitated phase which are dispersed, and realizes high strength and high plasticity by carrying out cooperative reinforcement by a plurality of mechanisms.
(2) The room-temperature tensile yield strength can reach 850-1200 MPa, the tensile strength can reach 1100-1500 MPa, the elongation after fracture can reach 15-35%, and the requirements of advanced structural materials on high strength and high toughness are met.
(3) The method has the advantages of low raw material cost and simple preparation process flow, can obtain the FeCrNiAl-based alloy material with multilevel isomerism by a process convenient to operate, and can provide extra back stress reinforcement for the alloy by a heterostructure so as to greatly improve the strength and plasticity of the alloy. Compared with the as-cast coarse-grain FeCrNiAl alloy, the FeCrNiAl-based alloy prepared by the method has the advantages that the yield strength is improved by more than 3 times, the tensile strength is improved by more than 2 times, and meanwhile, the quite good plasticity is kept.
Drawings
FIG. 1 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 XRD pattern of the alloy.
FIG. 2 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 Low power Scanning Electron Microscope (SEM) images of the alloy material.
FIG. 3 shows the high strength and toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 High power Scanning Electron Microscope (SEM) images of the alloy material.
FIG. 4 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 Room temperature tensile stress-strain curves of the alloy materials.
FIG. 5 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 Scanning electron microscope image of the alloy material.
FIG. 6 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 High power scanning electron microscope image of the alloy material.
FIG. 7 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 Room temperature tensile stress-strain curves of the alloy materials.
FIG. 8 is the multistage isomeric Fe prepared in example 3 41 Cr 23 Ni 23 Al 12 Scanning electron microscope image of the alloy material.
FIG. 9 is the multistage isomeric Fe prepared in example 3 41 Cr 23 Ni 23 Al 12 High power scanning electron microscope image of the alloy material.
FIG. 10 is the multistage isomeric Fe prepared in example 3 41 Cr 23 Ni 23 Al 12 Room temperature tensile stress-strain curves of the alloy materials.
Detailed Description
In order that the invention may be more readily understood, reference is now made to the following description, taken in conjunction with the accompanying drawings and examples, of the specific embodiments of the invention, but the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The high-strength and high-toughness multi-stage heterogeneous Fe is prepared by the embodiment 40 Ni 30 Cr 20 Al 10 The preparation method of the alloy material specifically comprises the following steps:
(1) preparing raw materials by adopting element blocks according to the following atomic percentages: fe: 40%, Ni: 30%, Cr: 20%, Al: 10 percent and the block purity is more than or equal to 99.9wt percent.
(2) And (3) putting the prepared raw materials into vacuum arc melting. And in the smelting process, firstly, vacuumizing to 3Pa, introducing high-purity argon, vacuumizing, repeatedly washing the furnace twice to ensure a high-purity vacuum environment, smelting induction current of 400A, carrying out electromagnetic stirring in the alloy smelting process, smelting for 4 times, and then casting into a water-cooled copper mold for cooling to obtain an alloy ingot.
(3) And (3) carrying out multi-pass (10-pass) cold rolling deformation treatment on the alloy obtained in the step (2), wherein the single-pass reduction amount is controlled to be about 10%, and the total deformation amount is controlled to be 80%.
(4) And (3) keeping the temperature of the alloy obtained in the step (3) at 830 ℃ for 2 hours, and then cooling to room temperature.
FIG. 1 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 XRD pattern of the alloy.
FIG. 2 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 Low power Scanning Electron Microscope (SEM) images of the alloy material.
FIG. 3 shows the high strength and toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 High power Scanning Electron Microscope (SEM) images of the alloy material.
FIG. 4 shows the high-toughness multi-stage isomeric Fe prepared in example 1 40 Ni 30 Cr 20 Al 10 Room temperature tensile stress-strain curves of the alloy materials.
As can be seen from the figure: this example prepares a multi-stage isomeric Fe 40 Ni 30 Cr 20 Al 10 The alloy material has a microstructure composed of a multi-scale FCC matrix phase, a multi-scale B2 and a sigma reinforcing phase, wherein the sizes of the FCC matrix phase and the B2 and sigma reinforcing phase are in multi-scale gradient distribution (composed of nano-crystals, ultra-fine crystals and fine crystals). The room-temperature tensile yield strength, the tensile strength and the elongation after fracture are respectively 1199MPa, 1368MPa and 19.3 percent, and the comprehensive mechanical property is excellent.
Example 2
The high-strength and high-toughness multi-stage heterogeneous Fe is prepared by the embodiment 55 Cr 18 Ni 17 Al 8 Co 2 The preparation method of the alloy material specifically comprises the following steps:
(1) preparing raw materials by adopting element blocks according to the following atomic percentages: fe: 55%, Cr: 18%, Ni: 17%, Al: 8%, Co: 2 percent and the block purity is more than or equal to 99.9 wt.%.
(2) And (3) putting the prepared raw materials into vacuum arc melting. And in the smelting process, firstly, vacuumizing to 3Pa, introducing high-purity argon, vacuumizing, repeatedly washing the furnace twice to ensure a high-purity vacuum environment, smelting induction current of 380A, carrying out electromagnetic stirring in the alloy smelting process, repeatedly smelting for 5 times, and carrying out suction casting on the alloy in a water-cooling copper mold to obtain an ingot.
(3) And (3) carrying out multiple (8) cold rolling deformation treatments on the alloy obtained in the step (2), wherein the pressing amount of a single pass is controlled to be about 10%, and the total deformation is controlled to be 75%.
(4) And (3) keeping the temperature of the alloy obtained in the step (3) at 880 ℃ for 0.5 hour, and then cooling to room temperature.
FIG. 5 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 Scanning electron microscope image of the alloy material.
FIG. 6 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 High power scanning electrode for alloy materialMirror image.
FIG. 7 is the multistage isomeric Fe prepared in example 2 55 Cr 18 Ni 17 Al 8 Co 2 Room temperature tensile stress-strain curves of the alloy materials.
As can be seen from the figure: this example prepares a multi-stage isomeric Fe 55 Cr 18 Ni 17 Al 8 Co 2 The alloy material has a microstructure composed of a multi-scale FCC matrix phase, a multi-scale B2 and a sigma reinforcing phase, wherein the sizes of the FCC matrix phase and the B2 and sigma reinforcing phase are in multi-scale gradient distribution (composed of nano-crystals, ultra-fine crystals and fine crystals). The room-temperature tensile yield strength, the tensile strength and the elongation after fracture are respectively 1106MPa, 1208MPa and 18.3 percent, and the comprehensive mechanical property is excellent.
Example 3
The high-strength high-plasticity multi-stage heterogeneous Fe is prepared by the following steps 42 Cr 23 Ni 23 Al 12 The preparation method of the alloy material specifically comprises the following steps:
(1) preparing raw materials by adopting element blocks according to the following atomic percentages: fe: 42%, Cr: 23%, Ni: 23%, Al: 12 percent and the block purity is more than or equal to 99.9wt percent.
(2) And (3) putting the prepared raw materials into vacuum arc melting. And in the smelting process, firstly, vacuumizing to 3Pa, introducing high-purity argon, vacuumizing, repeatedly washing the furnace for three times to ensure a high-purity vacuum environment, wherein the smelting induced current is 380A, carrying out electromagnetic stirring in the alloy smelting process, smelting for 4 times, and carrying out suction casting in a copper mold to obtain an alloy ingot.
(3) And (3) carrying out multi-pass (8-pass) cold rolling deformation treatment on the alloy obtained in the step (2), wherein the pressing amount of a single pass is controlled to be about 10%, and the total deformation is controlled to be 70%.
(4) And (4) keeping the temperature of the alloy obtained in the step (3) at 920 ℃ for 0.7 hour, and then cooling to room temperature.
FIG. 8 is the multistage isomeric Fe prepared in example 3 41 Cr 23 Ni 23 Al 12 Scanning electron microscope image of the alloy material.
FIG. 9 is a schematic representation of the multistage catalyst prepared in example 3Form Fe 41 Cr 23 Ni 23 Al 12 High power scanning electron microscope image of the alloy material.
FIG. 10 is the multistage isomeric Fe prepared in example 3 41 Cr 23 Ni 23 Al 12 Room temperature tensile stress-strain curves of the alloy materials.
As can be seen from the figure: this example prepares a multi-stage isomeric Fe 42 Cr 23 Ni 23 Al 12 The alloy material has a microstructure composed of a multi-scale FCC matrix phase, a multi-scale B2 and a sigma reinforcing phase, wherein the sizes of the FCC matrix phase and the B2 and sigma reinforcing phase are in multi-scale gradient distribution (composed of nano-crystals, ultra-fine crystals and fine crystals). The room-temperature tensile yield strength, the tensile strength and the elongation after fracture are 1036MPa, 1203MPa and 17.3 percent respectively, and the comprehensive mechanical property is excellent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, and equivalents thereof are intended to be included in the scope of the present invention.
Claims (10)
1. A high-strength-toughness multi-stage isomeric FeCrNiAl-based alloy material is characterized by comprising the following components in percentage by atom: 40-60%, Cr: 15-35%, Ni: 10-30%, Al: 5-15% and the content of other elements is less than or equal to 5%.
2. The high-toughness multi-stage isomeric FeCrNiAl-based alloy material according to claim 1, wherein the other elements comprise at least one of Mn, Ti, Co and C.
3. The high-toughness multi-stage isomeric FeCrNiAl-based alloy material according to claim 1, wherein the high-toughness multi-stage isomeric FeCrNiAl-based alloy has a multi-phase structure comprising an FCC matrix phase and a B2 reinforcement phase and a sigma reinforcement phase; wherein the sum of the volume fractions of the B2 reinforcing phase and the sigma reinforcing phase is 5-25%, and the B2 reinforcing phase and the sigma reinforcing phase are uniformly dispersed in the alloy.
4. The high-toughness multi-stage isomeric FeCrNiAl-based alloy material according to claim 1, wherein the grain sizes of the matrix phase and the reinforcement phase of the high-toughness multi-stage isomeric FeCrNiAl-based alloy material exhibit a multi-scale gradient distribution of "nanocrystalline + ultrafine crystalline + fine crystalline".
5. The high-toughness multistage-isomeric FeCrNiAl-based alloy material according to claim 1, wherein the yield strength σ of the high-toughness multistage-isomeric FeCrNiAl-based alloy is 0.2 850-1200 MPa, tensile strength sigma UTS 1100-1500 MPa, and the elongation after fracture is more than or equal to 15%.
6. The preparation method of the high-strength-and-toughness multistage-isomeric FeCrNiAl-based alloy material disclosed by any one of claims 1 to 5 is characterized by adopting a casting, plastic deformation and heat treatment process and comprising the following steps of:
(1) preparing raw materials according to the following atomic percentages: fe: 40-60%, Cr: 15-35%, Ni: 10-30%, Al: 5-15%, and the content of other elements is less than or equal to 5%;
(2) placing the prepared raw materials in a smelting furnace, repeatedly smelting for 3-6 times to ensure that the components are uniformly distributed, and cooling to obtain an alloy block;
(3) performing plastic deformation treatment on the alloy block obtained in the step (2), wherein the total deformation is controlled to be 60-95%;
(4) and (4) carrying out annealing heat treatment on the FeCrNiAl-based alloy subjected to plastic deformation treatment obtained in the step (3) to obtain the high-strength and high-toughness multistage heterogeneous FeCrNiAl-based alloy material.
7. The preparation method of the high-toughness multistage-isomeric FeCrNiAl-based alloy material according to claim 6, wherein the smelting process in the step (2) comprises vacuum arc smelting, vacuum induction smelting and suspension smelting.
8. The method for preparing the high-toughness multistage-isomeric FeCrNiAl-based alloy material according to claim 6, wherein the plastic deformation treatment in the step (3) is a cold rolling or forging process.
9. The preparation method of the high-strength-toughness multistage-isomeric FeCrNiAl-based alloy material according to claim 8, wherein the cold rolling is performed for 5-15 passes, and the total deformation is 60-95%; the forging ratio of the forging process is 3-10.
10. The preparation method of the high-toughness multistage-isomeric FeCrNiAl-based alloy material according to claim 6, wherein the annealing heat treatment in the step (4) is performed at 700-1100 ℃ for 0.5-6 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115491561A (en) * | 2022-08-23 | 2022-12-20 | 西安工业大学 | High-toughness high-conductivity three-component alloy for diesel engine cylinder cover and preparation method thereof |
| CN115821144A (en) * | 2022-12-12 | 2023-03-21 | 华南理工大学 | High-strength-toughness low-cost cast FeMnNiCrAl alloy with precipitation-strengthened heterogeneous layered structure and preparation method thereof |
| CN115821144B (en) * | 2022-12-12 | 2024-05-17 | 华南理工大学 | High-strength and high-toughness low-cost casting FEMNNICRAL alloy with precipitation-strengthening heterogeneous lamellar structure and preparation method thereof |
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| CN115821144A (en) * | 2022-12-12 | 2023-03-21 | 华南理工大学 | High-strength-toughness low-cost cast FeMnNiCrAl alloy with precipitation-strengthened heterogeneous layered structure and preparation method thereof |
| CN115821144B (en) * | 2022-12-12 | 2024-05-17 | 华南理工大学 | High-strength and high-toughness low-cost casting FEMNNICRAL alloy with precipitation-strengthening heterogeneous lamellar structure and preparation method thereof |
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