CN111575596B - Irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel and preparation method thereof - Google Patents
Irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
The invention belongs to the technical field of nuclear structure materials and preparation thereof, and particularly relates to irradiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel and a preparation method thereof. Aims to provide a radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel with high strength and high elongation and a preparation method thereof, and the preparation method comprises the following steps: firstly, preparing raw materials according to components and mole percentage; placing the raw materials in a copper crucible, vacuumizing, filling argon, and starting to smelt; rolling the ingot obtained by smelting into a plate with the thickness of 2mm by different processes; then solid solution aging and ion irradiation treatment are carried out. According to the invention, through alloy component design, the Cu-rich nanocluster reinforced alloy is precipitated through aging and is used as a radiation induced defect trap to improve the irradiation resistance, so that the Cu-rich nanocluster reinforced alloy can resist high-dose ion irradiation exceeding 50dpa, has excellent irradiation resistance, and has good application prospects in the field of nuclear structure materials, especially steel for pressure vessels.
Description
Technical Field
The invention belongs to the technical field of nuclear structure materials and preparation thereof, and particularly relates to irradiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel and a preparation method thereof.
Background
One of the most important problems in nuclear energy applications is the nuclear safety problem, and the safety stability of nuclear engineering structural materials is a key factor for determining whether nuclear power plants, mobile nuclear power and future fusion reactors can safely operate. In the long-term operation process of a nuclear reactor, because strong particles such as neutrons and the like irradiate materials to cause the cascade displacement of material atoms to form vacancies and interstitial atoms and promote the segregation of solute atoms in alloys to form material defects such as atomic clusters and the like, if a large number of vacancy defects are gathered, a serious material swelling effect can occur, so that the stability of the mechanical properties of a structural material is influenced, and finally, the material fails due to the irradiation induced brittleness and the like, so that the potential hazard on the safety of the nuclear reactor and the moving nuclear power is greatly formed.
The pressure vessel is a critical component of nuclear reactors, whose embrittlement is primarily due to radiation-induced microstructural changes in the material, the effect of which on embrittlement depends on the material composition, the initial microstructure and the irradiation conditions. The existing research considers that the main causes of hardening and embrittlement are the precipitation phase of intragranular nanometer scale caused by neutron irradiation, matrix damage, the segregation of impurities in grain boundary and the interaction of the precipitation phase and the matrix damage and the impurities, so that the ductile-brittle transition temperature (DBTT) is increased to cause embrittlement. Among the above causes of irradiation embrittlement, it is currently widely believed that a precipitated phase "precipitation of a nano-sized Cu precipitate cluster of high density in particular hinders dislocation glide" is dominant. However, several other types of steel are strengthened by copper-rich nano-phases of similar or slightly larger size, such as High Strength Low Alloy (HSLA) steel and Precipitation Hardening (PH) stainless steel, with high strength and excellent ductility without embrittlement. The invention innovatively takes the copper-rich nanocluster as a defect trap to absorb irradiation-induced defects and solute atoms and improve irradiation resistance. The traditional nuclear structure material can only bear the irradiation dose of less than 10dpa and is not embrittled, while the alloy material developed by the invention can resist the high-dose ion irradiation of more than 50dpa and still keeps good strength and plasticity and toughness without embrittlement.
In patent document CN 105239010 a, a Cr-Y-O nanocluster oxide dispersion strengthened low activation steel is disclosed, in which oxide nanoclusters are dispersed and distributed, and not only have excellent mechanical properties, but also have low activation properties and good radiation swelling resistance, but the cost of the nanoclusters is different from that of the steel of the present invention. The patent of publication No. CN 109594009A reports that the creep endurance time of the obtained anti-radiation low-activation steel under the loading condition of 550 ℃ and 195MPa exceeds 5000h, and the cost of the nanophase is different from that of the patent.
Disclosure of Invention
The invention aims to provide a radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel with high strength and high elongation. The invention also aims to provide a preparation method of the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel.
In order to realize the purpose of the invention, the technical scheme is as follows:
the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel comprises the following components in percentage by mass: 0.5 to 4.0 percent of Cu0.5 to 6.0 percent of Ni0.5 to 6.0 percent of Mn0.2 to 2.0 percent of Cr0.1 to 1.5 percent of Mo0.2 to 1.5 percent of Al0 to 0.5 percent of Nb0 to 0.5 percent of the balance of iron.
A preparation method of irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel comprises the following steps:
the method comprises the following steps: the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel is prepared from the following raw materials in percentage by mass: 0.5-4.0% of Cu0.5-6.0% of Ni0.5-6.0%, 0.2-2.0% of Mn0.1-1.5% of Cr0.1-1.5%, 0.2-1.5% of Mo0. 0-0.5%, 0.5% of Nb 0-0.5%, and the balance of iron;
step two: placing the alloy raw material in a crucible, vacuumizing to 1 × 10-2Introducing argon to 0.01-0.1MPa after the pressure is higher than MPa;
step three: high vacuum arc melting is adopted, repeated melting is carried out for 2-10 times, and alloy bars with the diameter of 20mm are formed in a water-cooling copper mould through suction casting;
step four: hot rolling the alloy bar to a thickness of 10mm at 900-1100 ℃, pressing down 10% in a single pass, and preserving heat for 0.25-1 h after hot rolling; then, cold rolling the sample to the thickness of 2mm, wherein each pass is 0.4-0.6 mm;
step five: solid solution aging treatment;
step six: and (5) ion irradiation.
The temperature of the solution treatment is 880-1000 ℃, and the solution time is 30-180 min; the aging temperature is 475-600 ℃, and the aging time is 2-1200 min.
The ion irradiation of the implanted Au2+The energy of the ions is 3-9 MeV, and the injection amount is 1.0 multiplied by 1014~1.0×1017ions/cm2, dpa is 40-75.
The invention has the beneficial effects that:
according to the invention, through alloy component design, the Cu-rich nanocluster reinforced alloy is precipitated through aging and is used as a radiation induced defect trap to improve the irradiation resistance, so that the Cu-rich nanocluster reinforced alloy can resist high-dose ion irradiation exceeding 50dpa, has excellent irradiation resistance, and has good application prospects in the field of nuclear structure materials, especially steel for pressure vessels.
Drawings
FIG. 1 shows the microstructure aged at 500 ℃ for 2 min;
FIG. 2 shows the microstructure after 1h ageing at 500 ℃;
FIG. 3 shows the microstructure aged at 500 ℃ for 20 hours;
FIG. 4 is a graph of hardness at 500 ℃ versus time;
FIG. 5 is an engineering stress-strain curve of solid solution and treatment at different aging times at 500 ℃;
FIG. 6 is a graph of nanoindentation hardness before and after irradiation of samples in a solid solution state and in various aging states;
FIG. 7 is a graph showing the variation of Young's modulus before and after irradiation of samples in a solid solution state and in various aging states;
FIG. 8 is a graph of Cu-rich nanocluster distribution in a peak-aged un-irradiated copper-rich nanocluster strengthened steel;
FIG. 9 shows Au in a peak aged state2+And (3) distributing the Cu-rich and Ni-rich nanocluster in the copper-rich nanocluster strengthened steel after irradiation.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to the accompanying drawings.
The invention belongs to the technical field of nuclear structure materials and preparation thereof, and particularly relates to irradiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel and a preparation method thereof. Aims to provide the irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel with high strength and high elongation and the preparation method thereof.
In order to realize the purpose of the invention, the technical scheme is as follows:
the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel comprises the following components in percentage by mass: 0.5 to 4.0 percent of Cu0.5 to 6.0 percent of Ni0.5 to 6.0 percent of Mn0.2 to 2.0 percent of Cr0.1 to 1.5 percent of Mo0.2 to 1.5 percent of Al0 to 0.5 percent of Nb0 to 0.5 percent of the balance of iron.
A preparation method of irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel comprises the following steps:
the method comprises the following steps: the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel is prepared from the following raw materials in percentage by mass: 0.5-4.0% of Cu0.5-6.0% of Ni0.5-6.0%, 0.2-2.0% of Mn0.1-1.5% of Cr0.1-1.5%, 0.2-1.5% of Mo0. 0-0.5%, 0.5% of Nb 0-0.5%, and the balance of iron;
step two: the alloy raw material is placed in a crucible, the crucible is vacuumized to be more than 1 x 10 < -2 > MPa, and then argon is filled to be 0.01 to 0.1 MPa.
Step three: high vacuum arc melting is adopted, repeated melting is carried out for 2-10 times, and alloy bars with the diameter of 20mm are formed in a water-cooling copper mould through suction casting;
step four: hot rolling the alloy bar to 10mm at 900-1100 ℃, pressing down 10% in a single pass, and keeping the temperature for 0.25-1 h after hot rolling; then, cold rolling the sample to 2mm, wherein each pass is 0.4-0.6 mm;
step five: solid solution aging treatment;
step six: and (5) ion irradiation.
The temperature of the solution treatment is 880-1000 ℃, and the solution time is 30-180 min; the aging temperature is 475-600 ℃, and the aging time is 2-1200 min.
The ion irradiation of the implanted Au2+The energy of the ions is 3-9 MeV, and the injection amount is 1.0 multiplied by 1014~1.0×1017ions/cm2Dpa is 40-75.
As will be further described below in the following,
the chemical components of the Cu-rich nanocluster strengthened steel in the embodiment are as follows by mass percent: 2.25% of Cu2, 4.17% of Ni0.97% of Mn0.97%, 0.46% of C, 0.85% of Mo0, 0.01% of Al0.06% of Nb0.06% of Fe, and the balance of Fe. The specific process comprises the following steps:
(1) smelting: the designed components are weighed and proportioned according to mass percent, alloy smelting is carried out in a high vacuum arc melting furnace, the alloy smelting is carried out for 5 times repeatedly, magnetic stirring is adopted to ensure that elements are uniformly mixed in the second time, and the alloy rod with the diameter of 20mm is formed in a water-cooled copper crucible by suction casting.
(2) Rolling: the alloy rods are subjected to hot rolling treatment, the alloy rods are hot rolled to be 10mm thick at 1000 ℃, the pressing amount is 10% in a single pass, and the temperature is kept for 1min after the hot rolling. The samples were then cold rolled to a thickness of 2mm, 0.5mm per pass.
(3) And (3) heat treatment: and (3) carrying out solid solution and heat preservation on the rolled sample at 900 ℃ for 30min, and then carrying out water cooling. The aging temperature is 500 deg.C, and the holding time is 2min, 60min and 1200 min.
(4) Ion irradiation: subjecting the samples in solid solution state, 500 deg.C under-aging, peak aging and over-aging states to ion irradiation, and adopting 6MeV Au2+Irradiating with a fluence of 1X 1016ion/cm2The irradiation depth is about 800nm, and the peak damage is near 400nm and reaches about 70 dpa.
The microstructure of the copper-rich nanocluster strengthened steel subjected to solid solution and different aging time treatments is lath ferrite, and as shown in figures 1-3, the aging treatment at 500 ℃ has almost no influence on the microstructure and the grain size. Hardness and tensile properties after solid solution and 500 ℃ aging are shown in FIGS. 4 and 5, the hardness is highest at 340HV at 1h of aging, the corresponding yield strength is 979MPa, the tensile strength is 1023MPa, and the elongation is 24%. Selecting solid solution, underaging, peak aging and overaging samples to carry out Au2+The samples in the ion irradiated, solid solution and underaged states hardened due to precipitation of nanoclusters, the peak aged and overaged samples softened due to coarsening of nanoclusters, and the irradiation had little effect on young's modulus, as shown in fig. 6-7. Three-dimensional atom probe characterization is carried out on the sample before and after peak-aged state irradiation, as shown in fig. 8 and 9, it is found that the preset Cu-rich nanoclusters can be used as irradiation induced defect traps to absorb solute atoms so as to improve irradiation resistance, and can resist high-dose ion irradiation exceeding 50 dpa.
In conclusion, the invention belongs to the technical field of nuclear structure materials and preparation thereof, and particularly relates to irradiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel and a preparation method thereof. Aims to provide the irradiation-resistant Cu-containing nanocluster reinforced high-strength low-alloy steel with high strength and high elongation and the preparation method thereof. The method comprises the following steps of firstly preparing raw materials according to components and mole percentage; placing the raw materials in a copper crucible, vacuumizing, filling argon, and starting to smelt; rolling the ingot obtained by smelting into a plate with the thickness of 2mm by different processes; then solid solution aging and ion irradiation treatment are carried out. According to the invention, through alloy component design, the Cu-rich nanocluster reinforced alloy is precipitated through aging and is used as a radiation induced defect trap to improve the irradiation resistance, so that the Cu-rich nanocluster reinforced alloy can resist high-dose ion irradiation exceeding 50dpa, has excellent irradiation resistance, and has good application prospects in the field of nuclear structure materials, especially steel for pressure vessels.
Claims (1)
1. The preparation method of the irradiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel is characterized by comprising the following steps of:
the method comprises the following steps: the radiation-resistant Cu-containing nanocluster reinforced high-strength low alloy steel is prepared from the following raw materials in percentage by mass: 2.25% of Cu2.17%, 4.17% of Ni0.97%, 0.46% of Cr0.85%, 0.01% of Al0.06%, and the balance of Fe;
step two: placing the alloy raw material in a crucible, vacuumizing to 1 × 10-2Introducing argon to 0.01-0.1MPa after the pressure is higher than MPa;
step three: high vacuum arc melting is adopted, repeated melting is carried out for 5 times, and alloy bars with the diameter of 20mm are formed in a water-cooling copper mould through suction casting;
step four: alloy bar material is placed at 1000oC, hot rolling to a thickness of 10mm, pressing 10% in a single pass, and keeping the temperature for 1h after hot rolling; then, cold rolling the sample to 2mm thickness, 0.5mm per pass;
step five: solid solution aging treatment; the solution treatment temperature is 900 DEG CoC, solid solution time is 30 min; aging temperature is 500oC, aging for 60 min;
step six: ion irradiation; the ion irradiation of the implanted Au2+The energy of the ion is 6MeV, and the fluence is 1X 1016ion/cm2Dpa is 70.
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