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CN-121972649-A - High-temperature-resistant and radiation-resistant alloy material for nuclear power and preparation method thereof

CN121972649ACN 121972649 ACN121972649 ACN 121972649ACN-121972649-A

Abstract

The invention discloses a high-temperature-resistant and radiation-resistant alloy material for nuclear power and a preparation method thereof, belongs to the technical field of alloy preparation, and is used for solving the technical problems that the high-temperature resistance and the radiation resistance of the alloy material for nuclear power in the prior art are to be further improved; according to the invention, a multiphase composite system consisting of an yttrium-rich interface activation framework, a nickel-iron extension-defect interlayer phase and high-entropy core-shell pinning particles is constructed, in-situ combination of metal-ceramic-high-entropy three phases is realized in the hot pressing and micro-oxygen regulation and control process, a stable interface and a high-efficiency defect regulation and control network are formed on a microscopic scale by the structure, and the tissue compactness, interface combination strength and high-temperature structural stability of the alloy are remarkably improved, so that the material shows high strength, high plasticity and excellent radiation resistance under room temperature, high temperature and radiation environment.

Inventors

  • HUANG ZHI
  • MIN KAI
  • ZHANG QINGHUA

Assignees

  • 江苏裕隆特种金属材料科技有限公司

Dates

Publication Date
20260505
Application Date
20251224

Claims (9)

  1. 1. The alloy material for nuclear power is characterized by comprising the following raw materials, by weight, 7-8 parts of yttrium-rich interface activation framework, 2 parts of nickel-iron extension-defect interlayer phase, 1 part of high-entropy core-shell pinning particles, 15-18 parts of dispersing agent and 1-2 parts of silica sol; wherein the dispersing agent is obtained by mixing deionized water and absolute ethyl alcohol according to the dosage ratio of 2mL to 1 mL; The preparation method of the yttrium-rich interface activation framework comprises the following steps: A1, placing a titanium zirconium boron oxide network body in a gas-solid reaction furnace, introducing mixed gas, heating to 900-1100 ℃, preserving heat for 2-3 hours, switching to nitrogen, cooling to 80 ℃, discharging, grinding and sieving to obtain a titanium zirconium carbon boron interpenetrating polymer skeleton with the particle size of 30-50 mu m; A2, placing the titanium-zirconium-carbon-boron interpenetrating framework in a tubular furnace in a controllable oxygen potential environment, introducing oxygen/nitrogen mixed gas to enable oxygen partial pressure to be 10 -4 -10 -3 atm, heating to 650-800 ℃ at 2-4 ℃ per minute, preserving heat for 1-2h, and cooling to 120 ℃ along with the furnace after the heat preservation is finished, and discharging to obtain the yttrium-rich interface activation framework.
  2. 2. The alloy material for nuclear power, which is resistant to high temperature and irradiation, according to claim 1, wherein in the step A1, the mixed gas is obtained by mixing hydrogen, methane and nitrogen according to a volume ratio of 2-3:2-3:14-16, and in the step A2, the oxygen/nitrogen mixed gas is obtained by mixing oxygen and nitrogen according to a volume ratio of 1:5000.
  3. 3. The high-temperature-resistant and radiation-resistant alloy material for nuclear power according to claim 1, wherein the preparation method of the titanium zirconium boron oxide network body comprises the following steps: Adding citric acid and deionized water into a reaction kettle, stirring and dissolving, introducing nitrogen for protection, sequentially adding titanium isopropoxide, zirconium nitrate and yttrium nitrate hexahydrate into the reaction kettle, adjusting the pH value of a system to be 6.8-7.8 by using ethylenediamine, keeping the temperature of the reaction kettle at 30-40 ℃, keeping the temperature and stirring for 2-4 hours, and continuing to age at room temperature for 12-24 hours to obtain titanium-zirconium-yttrium polynuclear complex gel; And B2, mixing the titanium-zirconium-yttrium polynuclear coordination gel with boric acid, uniformly spreading the mixture in a crucible, transferring the crucible into a tube furnace, introducing nitrogen/hydrogen mixed gas, and calcining to obtain the titanium-zirconium-boron-oxygen network body.
  4. 4. The alloy material for nuclear power, which is resistant to high temperature and radiation, according to claim 3, wherein in the step B1, the dosages of citric acid, deionized water, titanium isopropoxide, zirconium nitrate and yttrium nitrate hexahydrate are respectively 5-10g:240-300mL:12-18g:18-28g:3-5g, in the step B2, the dosage ratio of the titanium zirconium yttrium polynuclear complex gel to boric acid is 30g:1-2g, wherein the nitrogen/hydrogen mixed gas is obtained by mixing nitrogen and hydrogen according to the volume ratio of 93:7, the calcination operation is that a tube furnace is heated to 350-450 ℃ at 2-3 ℃ per min, the temperature is kept for 1-2h, the temperature is further raised to 500-650 ℃ and the temperature is kept for 2-4h.
  5. 5. The alloy material for nuclear power, which is resistant to high temperature and irradiation, according to claim 1, wherein the preparation method of the nickel-iron extension-defect interlayer phase comprises the following steps: adding deionized water and dimethylformamide into a reaction kettle, stirring, adding nickel nitrate hexahydrate and ferric nitrate nonahydrate, introducing nitrogen for protection, using saturated ammonia water to adjust the pH value of a system to be 9.5-10.5, then dropwise adding a 30wt% hydrogen peroxide aqueous solution into the reaction kettle, controlling the temperature of the reaction kettle to be 30-50 ℃, keeping the temperature, stirring for 4-6 hours, standing and aging for 8-12 hours, and performing aftertreatment to obtain a nickel-iron lamellar intercalation body; And C2, adding the ferronickel lamellar intercalation body and deionized water into a reaction kettle for overtime, introducing nitrogen for protection, reducing the temperature of the reaction kettle to 5-10 ℃, adding 3-5wt% of sodium borohydride aqueous solution into the reaction kettle, heating the reaction kettle to 20-30 ℃, preserving heat, stirring for 1-2h, and performing post treatment to obtain a ferronickel extension-defect interlayer phase.
  6. 6. The alloy material for nuclear power, which is resistant to high temperature and radiation according to claim 5, wherein in the step C1, the dosage ratio of deionized water, dimethylformamide, nickel nitrate hexahydrate, ferric nitrate nonahydrate and 30wt% of hydrogen peroxide aqueous solution is 75-100mL:10-15mL:5-8g:2-3 mL, and in the step C2, the dosage ratio of the nickel iron lamellar intercalation body, deionized water and 3-5wt% of sodium borohydride aqueous solution is 4-6g:15-20mL:10mL.
  7. 7. The alloy material for nuclear power, which is resistant to high temperature and irradiation, according to claim 1, wherein the preparation method of the high-entropy core-shell pinning particles comprises the following steps: Adding nickel chloride hexahydrate, chromium chloride hexahydrate, ammonium heptamolybdate tetrahydrate, sodium tungstate dihydrate, yttrium nitrate hexahydrate and deionized water into a reaction kettle, introducing nitrogen for protection, using saturated ammonia water to adjust the pH value of a reaction system to be 8.4-8.6, keeping the temperature of the reaction kettle at 30-40 ℃, keeping the temperature and stirring for 2-4 hours, aging at room temperature for 12-18 hours, and performing post treatment to obtain nickel-chromium-molybdenum-tungsten-yttrium co-precipitation nano-cores; And D2, uniformly mixing the nickel-chromium-molybdenum-tungsten-yttrium co-deposited nano-cores, urea, boric acid and deionized water, loading into a crucible, transferring the crucible into a tube furnace, introducing nitrogen for protection, calcining in sections, cooling to room temperature along with the furnace after calcining, and grinding and dispersing to obtain the high-entropy core-shell pinning particles.
  8. 8. The alloy material for nuclear power, which is resistant to high temperature and radiation, according to claim 7, wherein in the step D1, the dosage ratio of nickel chloride hexahydrate, chromium chloride hexahydrate, ammonium heptamolybdate tetrahydrate, sodium tungstate dihydrate, yttrium nitrate hexahydrate and deionized water is 10-18g, 8-14g, 6-10g, 4-8g, 300-500mL, the dosage ratio of nickel-chromium-molybdenum-tungsten-yttrium co-precipitation nano-core, urea, boric acid and deionized water is 4-6g, 12-18g, 0.1-0.2g, 2-4mL, the sectional calcination operation is that the temperature is raised to 120 ℃ for 40min at 3 ℃ per min, then to 380 ℃ for 60min, and finally to 800 ℃ for 2-3h.
  9. 9. The method for preparing the alloy material for nuclear power, which is resistant to high temperature and irradiation, according to any one of claims 1 to 8, comprising the following steps: S1, adding an yttrium-rich interface activated framework, a nickel iron extension-defect interlayer phase and high-entropy core-shell pinning particles into a ball milling tank, adding a dispersing agent, introducing nitrogen for protection, performing ball milling for 30-60min, adding silica sol, performing ball milling for 20-30min, and performing vacuumizing and defoaming for 5-10min to obtain a forming material; S2, pouring the forming material into a blank, placing the blank in a drying oven at 80-120 ℃, preserving heat for 1-2h to obtain a dry blank, placing the dry blank in a tubular furnace at 300-400 ℃ under nitrogen atmosphere, preserving heat for 1-2h, and performing hot-pressing calcination to obtain the alloy material.

Description

High-temperature-resistant and radiation-resistant alloy material for nuclear power and preparation method thereof Technical Field The invention relates to the technical field of alloy preparation, in particular to a high-temperature-resistant and radiation-resistant alloy material for nuclear power and a preparation method thereof. Background With the development of nuclear energy devices to the high power density and long service life, high temperature resistant structural materials become the key for ensuring the safe operation of equipment, conventional nuclear power alloys mainly comprise austenitic stainless steel, nickel-based superalloys, iron-based superalloys and the like, and the materials have certain strength and creep resistance under high temperature conditions, and in recent years, the high temperature stability of the materials is obviously improved by solid solution strengthening, dispersion strengthening, grain boundary engineering and other methods, so that important support is provided for the operation of advanced reactors and nuclear fusion devices; At the same time, the problem of structural stability in an irradiation environment is attracting a great deal of attention, and high-energy neutron irradiation can cause dislocation, vacancy clusters and bubble aggregation, thereby causing embrittlement and performance degradation of materials, researchers explore from the directions of alloy component design, interface structure optimization, multiphase compounding and the like, develop various anti-irradiation alloys with defect adsorption and energy dissipation capacity, and provide a new research foundation for material application under high-temperature high-irradiation service conditions. At present, the high-temperature-resistant and radiation-resistant alloy for nuclear power is prepared by adopting the traditional smelting, powder metallurgy or dispersion strengthening process, and the method can improve the strength and stability of the material to a certain extent, but has limitations in element distribution uniformity and interface combination, and phase separation and abnormal growth of crystal grains are easy to occur in the high-temperature sintering process, so that the tissue density is insufficient, the interface binding force is reduced, and the overall mechanical property and long-term service reliability of the material are affected; in addition, the traditional alloy system has limited defect evolution control capability in an irradiation environment, and is easy to generate phenomena such as vacancy aggregation, bubble nucleation, dislocation loop coarsening and the like, so that irradiation embrittlement and intensity attenuation are induced, and therefore, the traditional preparation process is difficult to realize collaborative solid solution and interface stable regulation and control of multiple elements on a microscopic scale, and forms restriction on the irradiation resistance and high-temperature comprehensive performance improvement of materials. In view of the technical drawbacks of this aspect, a solution is now proposed. Disclosure of Invention The invention aims to provide a high-temperature-resistant and radiation-resistant alloy material for nuclear power and a preparation method thereof, which are used for solving the technical problems that the high-temperature resistance and the radiation resistance of the alloy material for nuclear power in the prior art are to be further improved. The invention aims at realizing the technical scheme that the alloy material for nuclear power resistant to high temperature and radiation comprises the following raw materials, by weight, 7-8 parts of yttrium-rich interface activation framework, 2 parts of nickel-iron extension-defect interlayer phase, 1 part of high-entropy core-shell pinning particles, 15-18 parts of dispersing agent and 1-2 parts of silica sol; wherein the dispersing agent is obtained by mixing deionized water and absolute ethyl alcohol according to the dosage ratio of 2mL to 1 mL; The preparation method of the yttrium-rich interface activation framework comprises the following steps: A1, placing a titanium zirconium boron oxide network body in a gas-solid reaction furnace, introducing mixed gas, heating to 900-1100 ℃, preserving heat for 2-3 hours, switching to nitrogen, cooling to 80 ℃, discharging, grinding and sieving to obtain a titanium zirconium carbon boron interpenetrating polymer skeleton with the particle size of 30-50 mu m; A2, placing the titanium-zirconium-carbon-boron interpenetrating framework in a tubular furnace in a controllable oxygen potential environment, introducing oxygen/nitrogen mixed gas to enable oxygen partial pressure to be 10 -4-10-3 atm, heating to 650-800 ℃ at 2-4 ℃ per minute, preserving heat for 1-2h, and cooling to 120 ℃ along with the furnace after the heat preservation is finished, and discharging to obtain the yttrium-rich interface activation framework. The re