CN115627405A - High-entropy alloy resistant to liquid lead and bismuth corrosion and preparation method thereof - Google Patents
High-entropy alloy resistant to liquid lead and bismuth corrosion and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 98
- 238000005260 corrosion Methods 0.000 title claims abstract description 51
- 230000007797 corrosion Effects 0.000 title claims abstract description 51
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 37
- 239000007788 liquid Substances 0.000 title claims abstract description 36
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005096 rolling process Methods 0.000 claims abstract description 16
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000265 homogenisation Methods 0.000 claims abstract description 6
- 238000010891 electric arc Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000943 NiAl Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention relates to the field of corrosion-resistant alloy materials, in particular to a high-entropy alloy resistant to liquid lead and bismuth corrosion and a preparation method thereof. The high-entropy alloy comprises the following chemical components in percentage by weight: fe:30 to 55 percent; ni:15 to 30 percent; cr:15 to 30 percent; al:5 to 15 percent. The method prepares the alloy plate by electric arc melting and copper mold casting, and the alloy plate is subjected to homogenization treatment, rolling deformation and annealing and aging treatment to obtain the dual-phase structure with the face-centered cubic matrix and the body-centered cubic ordered precipitated phase, and the special structure enables the alloy to have stronger strong plasticity cooperation. In addition, the multilayer oxide film structure of Fe, cr and Al formed in the alloy can inhibit the occurrence of soluble corrosion in a lead-bismuth environment, thereby improving the corrosion performance of the alloy and having important application prospects.
Description
Technical Field
The invention relates to the field of corrosion-resistant alloy materials, in particular to a high-entropy alloy resistant to liquid lead and bismuth corrosion and a preparation method thereof.
Background
The liquid lead bismuth alloy (LBE) has the advantages of excellent neutron performance, chemical inertness, thermophysical performance, radiation resistance and the like, is a first-choice material of a fourth-generation nuclear energy system lead cold fast reactor coolant, and is an important candidate material of an accelerator-driven subcritical system coolant and a spallation target material. However, LBEs can cause severe liquid metal corrosion effects on the structural material, primarily due to the gradual dissolution and mass migration of metal atoms in the structural material into the LBE, as well as the diffusion of the LBE along grain boundaries into the material. The structure material is corroded and damaged, and the safe operation of the lead-cooled fast reactor is influenced. In addition, the concentration of oxygen in the LBE affects the formation of an oxide film on the surface of the structural material, when the oxygen content in the LBE is less than 10 -7 At wt.%, the surface cannot form a complete protective oxide film, and dissolution corrosion will occur; when the LBE oxygen content is higher than 10 -5 In wt.%, the oxide film formed is thick and easily separated from the substrate, and is broken, resulting in severe oxidation corrosion.
The high-entropy alloy generates four effects different from the traditional alloy due to the diversification of the component design, and improves the comprehensive performance of the alloy including the anti-irradiation performance, so that the high-entropy alloy becomes the most potential nuclear structure candidate material. The high-entropy alloy with excellent corrosion resistance is used as a nuclear structure material, so that the method has practical significance.
Disclosure of Invention
The invention mainly aims to provide a high-entropy alloy resistant to liquid lead and bismuth corrosion and a preparation method thereof.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme:
the high-entropy alloy resistant to liquid lead and bismuth corrosion comprises the following chemical components in percentage by weight:
Fe：30～55％；Ni：15～30％；Cr：15～30％；Al：5～15％。
the microstructure of the high-entropy alloy resistant to the corrosion of the liquid lead and bismuth is characterized by a face-centered cubic and body-centered cubic dual-phase structure.
The high-entropy alloy resistant to liquid lead and bismuth corrosion has a face-centered cubic phase which is a disordered structure matrix phase enriched with Fe and Cr.
The body-centered cubic phase of the high-entropy alloy resistant to liquid lead and bismuth corrosion is an ordered B2-NiAl phase and is dispersed in a face-centered cubic matrix phase.
The yield strength of the high-entropy alloy resistant to liquid lead and bismuth corrosion is 450-550 MPa, the tensile strength is 750-860 MPa, and the elongation is 25-35% under the room temperature condition.
The preparation method of the high-entropy alloy resistant to liquid lead and bismuth corrosion comprises the following steps:
(1) Weighing raw materials according to a preset component ratio, preparing an alloy ingot by adopting electric arc melting, and casting into an alloy plate by utilizing a copper mold casting method;
(2) And carrying out homogenization treatment, rolling deformation treatment, annealing and aging treatment on the alloy plate to obtain the FeNiCrAl high-entropy alloy.
The preparation method of the high-entropy alloy resistant to liquid lead and bismuth corrosion comprises the step (1) of pre-vacuumizing a vacuum chamber until the air pressure is lower than 1 x 10 -2 Pa, then filling high-purity argon to make the vacuum chamber pressure 3X 10 4 ～9×10 4 Pa, re-enteringAnd performing arc melting, wherein the melting current is 280-500A, and pouring the alloy melt into a copper mold with a corresponding size to obtain the alloy plate.
The preparation method of the high-entropy alloy resistant to liquid lead and bismuth corrosion comprises the following steps of (2) carrying out homogenization treatment at 1000-1250 ℃, keeping the temperature for 1-4 h, and cooling to room temperature by water; the rolling deformation treatment is room temperature rolling, the rolling direction of the alloy plate is along the length direction, the alloy plate rotates 180 degrees after each pass of rolling, and each pass of rolling is 0.1-0.3 mm until the thickness deformation of the alloy plate is 60-80%.
The preparation method of the high-entropy alloy resistant to liquid lead and bismuth corrosion comprises the following steps of (2) annealing at 900-1100 ℃ for 0.5-2.5 h, and air cooling to room temperature; the aging temperature is 500-900 ℃, the heat preservation time is 1-500 h, and the water is cooled to the room temperature.
The design idea of the invention is as follows:
on one hand, the invention inhibits the occurrence of soluble corrosion by controlling the content of Ni element with high dissolving tendency of liquid lead and bismuth in the high-entropy alloy, and simultaneously, with the addition of Fe, cr and Al, an alumina film with a compact, uniform and stable outer layer and a chromium oxide and iron oxide film as an inner layer are formed. The multi-layer oxide film structure can effectively reduce the diffusion rate of alloy elements and has the effect of inhibiting the dissolution corrosion of structural materials. On the other hand, the face-centered cubic and body-centered cubic dual-phase structures are obtained by cold rolling (60-80%), high-temperature recrystallization annealing (900-1100 ℃ for + 0.5-2.5 h) and low-temperature aging (500-900 ℃ for + 1-500 h) to achieve the strength plastic balance of the alloy.
By means of the technical scheme, the high-entropy alloy resistant to liquid lead and bismuth corrosion at least has the following advantages:
1. the invention discloses a high-entropy alloy resistant to liquid lead and bismuth corrosion, which is a novel alloy design scheme provided for solving the problems of the existing nuclear structure material and can simultaneously meet the performance requirements on high strength and toughness and resistance to liquid lead and bismuth corrosion under the condition of poor oxygen or saturated oxygen.
2. The liquid lead-bismuth corrosion resistant high-entropy alloy has good LBE corrosion resistance, and after the alloy is corroded in LBE at 550 ℃ for 1000 hours, the corrosion rate under the saturated oxygen condition is obviously lower than that under the oxygen-deficient condition.
3. The high-entropy alloy resisting liquid lead and bismuth corrosion has a special two-phase structure, and has the following room-temperature mechanical properties: the yield strength is 450-550 MPa, the tensile strength is 750-860 MPa, and the elongation is 25-35%.
4. The alloy system, the processing method and the heat treatment process of the high-entropy alloy resistant to liquid lead and bismuth corrosion are easy to realize, so that the high-entropy alloy has higher application value in the field of nuclear structure materials.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to make the technical solutions of the present invention practical in accordance with the contents of the specification, the following detailed description is given of preferred embodiments of the present invention with reference to the accompanying drawings.
Drawings
FIG. 1 is an XRD pattern of an example of the invention.
FIG. 2 is a SEM-EDS picture of the surface topography of example 3 of the invention. Fig. 2 (b) is a partially enlarged view of fig. 2 (a).
FIG. 3 is an engineering stress-strain diagram of an embodiment of the present invention.
FIG. 4 is SEM pictures of cross-sectional shapes of corrosion layers of example 2 of the invention after being respectively corroded in liquid lead bismuth at 550 ℃ for 1000 h. In this case, fig. 4 (a) shows the oxygen-deficient concentration, and fig. 4 (b) shows the saturated oxygen concentration.
FIG. 5 is SEM pictures of the cross-sectional shapes of the corrosion layers of example 3 after the corrosion layers are respectively corroded in liquid lead bismuth at 550 ℃ for 1000 hours. In this case, fig. 5 (a) shows the oxygen-deficient concentration, and fig. 5 (b) shows the saturated oxygen concentration.
FIG. 6 is SEM pictures of cross-sectional shapes of corrosion layers of example 4 after being respectively corroded in liquid lead bismuth at 550 ℃ for 1000 h. In fig. 6 (a), the oxygen-deficient concentration is shown, and in fig. 6 (b), the saturated oxygen concentration is shown.
Detailed Description
The embodiments of the present invention will be described in more detail below with reference to the drawings and examples, so that the aspects of the present invention and the advantages of its various aspects can be better understood. However, the specific embodiments and examples described below are for illustrative purposes only and are not limiting of the invention.
In the specific implementation process, the invention provides a high-entropy alloy resistant to liquid lead and bismuth corrosion, and the alloy comprises the following chemical components and micro-morphology and a specific preparation technology:
1. the high-entropy alloy comprises the following chemical components in percentage by weight: fe:30 to 55 percent; ni:15 to 30 percent; cr:15 to 30 percent; al:5 to 15 percent.
2. The microstructure characteristics of the high-entropy alloy are explained as follows:
(1) The microstructure of the alloy is a face-centered cubic and body-centered cubic dual-phase structure.
(2) The face-centered cubic phase is a disordered matrix phase enriched with Fe and Cr.
(3) The body-centered cubic phase is an ordered B2-NiAl phase and is dispersedly distributed in the face-centered cubic matrix phase, and the volume percentage of the body-centered cubic phase is 5-30%.
3. The preparation method of the high-entropy alloy comprises the following steps:
(1) Weighing metal raw materials with purity of more than 99.95wt.% according to a preset component ratio, wherein the alloy chemical components are shown in table 1, and pre-vacuumizing a vacuum chamber to the air pressure of 3.5 × 10 -3 Pa, then filling high-purity argon (the volume purity is 99.999%) to ensure that the pressure of the vacuum chamber is 4 multiplied by 10 4 Pa. The alloy smelting current is 350A, each time of smelting is 3 minutes, the alloy is turned over and smelted again after each time of smelting, and the process is repeated for at least 6 times until the alloy components are uniform; the alloy ingot is melted by electric arc melting and heating, and the alloy melt is rapidly poured into a copper mold with corresponding size by a copper mold casting method to obtain an alloy plate with the size of 60mm multiplied by 24mm multiplied by 4 mm.
(2) Homogenizing the alloy plate, sealing with vacuum quartz tube with pressure of 2 × 10 - 3 Pa, homogenizing at 1100 deg.C for 2h, and cooling with water to room temperature; and (3) rolling the plate into the required thickness by using a double-track rolling mill in a small step length multi-pass mode along a fixed direction at room temperature, wherein each pass is rolled for 0.2mm, and the plate is rolled for 12 passes, namely the thickness of the plate is reduced to 1.6mm from the original 4 mm.
(3) Annealing and aging the cold-rolled plate, sealing the plate by a vacuum quartz tube with the air pressure of 2 x 10 in the vacuum quartz tube -3 Pa, annealing temperature is 1000 ℃, heat preservation time is 1h, and air cooling is carried out to room temperature; the aging temperature is 700 ℃, the heat preservation time is 10h, and the FeNiCrAl high-entropy alloy is obtained after water cooling to room temperature.
TABLE 1 alloy chemistry (wt.%)
| Fe | Ni | Cr | Al | |
| Example 1 | 42.113 | 33.195 | 19.605 | 5.087 |
| Example 2 | 47.207 | 33.075 | 14.650 | 5.068 |
| Example 3 | 52.592 | 27.636 | 14.690 | 5.082 |
| Example 4 | 52.926 | 22.249 | 19.711 | 5.114 |
TABLE 2 Room temperature mechanical properties of high entropy alloys of the examples of the invention
| Yield strength (MPa) | Tensile strength (MPa) | Elongation (%) | |
| Example 1 | 548 | 858 | 31 |
| Example 2 | 496 | 800 | 30 |
| Example 3 | 483 | 786 | 30 |
| Example 4 | 526 | 817 | 29 |
As shown in figure 1, the phase compositions of the high-entropy alloys of the examples 1 to 4 are that four alloys are of a dual-phase face-centered cubic plus body-centered cubic structure, the body-centered cubic phase is an ordered B2-NiAl phase and is distributed in a face-centered cubic matrix phase in a dispersed way, and the volume percentages of the body-centered cubic phase are 29.4%, 15.2%, 42.1% and 20.6% respectively. As shown in FIG. 2, in example 3 Ni and Al-enriched ordered B2 phases are dispersed in Fe and Cr-enriched face-centered cubic matrix phases. Wherein, the matrix phase has good plasticity, the B2 phase can block the slippage of dislocation, and the dual-phase structure can realize good strong plastic balance. By adopting a linear cutting method, a tensile sample with the gauge length of 16mm, the section size of 2.5mm multiplied by 1.5mm and the total length of 38mm is cut from the high-entropy alloy sheet. The room-temperature tensile test was carried out using an Instron model 5582 Universal Material testing machine, with a tensile rate of 1X 10 -3 s -1 The tensile curve of the alloy is shown in figure 3, the room-temperature mechanical properties are listed in table 2, the yield strength of the high-entropy alloy disclosed by the invention is above 480MPa, the tensile strength can reach above 780MPa, and the elongation can be kept above 29%. Respectively in the oxygen deficiency (10) -7 wt.%) or saturated oxygen (10) - 3 wt.%) in liquid lead bismuth at 550 ℃ for 1000h, the high-entropy alloy has the corrosion layer profile shown in fig. 4-6. It can be seen that the high-entropy alloys of examples 2 to 4 of the present invention did not show corrosion under saturated oxygen conditions, whereas under oxygen-deficient conditions, it was found that the degree of corrosion of the high-entropy alloys gradually decreased as the ratio of the Ni content was decreased.
The implementation result shows that the alloy plate is prepared by the arc melting and copper mold casting method, the alloy plate is subjected to homogenization treatment, rolling deformation and annealing and aging treatment, a dual-phase structure with a face-centered cubic matrix and a body-centered cubic ordered precipitated phase is obtained, and the special structure enables the alloy to have stronger strong plasticity cooperation. In addition, the multilayer oxide film structure of Fe, cr and Al formed in the alloy can inhibit the occurrence of soluble corrosion in a lead-bismuth environment, so that the corrosion performance of the alloy is improved, and the alloy has an important application prospect.
The examples are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any obvious modifications, substitutions or variations can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (9)
1. The high-entropy alloy capable of resisting liquid lead and bismuth corrosion is characterized by comprising the following chemical components in percentage by weight:
Fe：30～55％；Ni：15～30％；Cr：15～30％；Al：5～15％。
2. a high entropy alloy resistant to corrosion by liquid lead-bismuth according to claim 1, characterized in that its microstructure is characterized by a face-centered cubic and body-centered cubic dual phase structure.
3. A high entropy alloy resistant to corrosion by liquid lead-bismuth according to claim 2, wherein the face-centered cubic phase is a Fe and Cr enriched disordered structure matrix phase.
4. A high-entropy alloy resistant to corrosion by liquid lead-bismuth according to claim 2, wherein the body-centered cubic phase is an ordered B2-NiAl phase and is dispersed in the face-centered cubic matrix phase.
5. The high-entropy alloy resistant to corrosion by liquid lead and bismuth as claimed in claim 1, wherein the yield strength of the high-entropy alloy at room temperature is 450-550 MPa, the tensile strength is 750-860 MPa, and the elongation is 25-35%.
6. A method for preparing a high-entropy alloy resistant to corrosion by liquid lead-bismuth according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) Weighing raw materials according to a preset component ratio, preparing an alloy ingot by adopting electric arc melting, and casting into an alloy plate by utilizing a copper mold casting method;
(2) And carrying out homogenization treatment, rolling deformation treatment, annealing and aging treatment on the alloy plate to obtain the FeNiCrAl high-entropy alloy.
7. A method for preparing a high-entropy alloy resistant to corrosion by liquid lead and bismuth according to claim 6, wherein in the step (1), the vacuum chamber is pre-evacuated to a pressure lower than 1 x 10 -2 Pa, then filling high-purity argon to make the pressure in the vacuum chamber be 3X 10 4 ～9×10 4 Pa, arc melting is carried out, the melting current is 280-500A, and the alloy melt is poured into a copper mould with a corresponding size to obtain the alloy plate.
8. The method for preparing the high-entropy alloy resistant to liquid lead-bismuth corrosion according to claim 6, wherein in the step (2), the homogenization treatment temperature is 1000-1250 ℃, the heat preservation time is 1-4 h, and the alloy is cooled to room temperature by water; the rolling deformation treatment is room temperature rolling, the rolling direction of the alloy plate is along the length direction, the alloy plate rotates 180 degrees after each pass of rolling, and each pass of rolling is 0.1-0.3 mm until the thickness deformation of the alloy plate is 60-80%.
9. The method for preparing the high-entropy alloy resistant to liquid lead-bismuth corrosion according to claim 6, wherein in the step (2), the annealing temperature is 900-1100 ℃, the heat preservation time is 0.5-2.5 h, and the alloy is air-cooled to room temperature; the aging temperature is 500-900 ℃, the heat preservation time is 1-500 h, and the water is cooled to the room temperature.
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| CN1974816A (en) * | 2006-12-08 | 2007-06-06 | 杭正奎 | High-temperature-resistant nickel-chromium alloy and manufacturing method thereof |
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