CN115717215B - Stainless steel ladle shell tube material for lead-bismuth fast reactor fuel assembly and preparation method thereof - Google Patents

Stainless steel ladle shell tube material for lead-bismuth fast reactor fuel assembly and preparation method thereof Download PDF

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CN115717215B
CN115717215B CN202211447039.9A CN202211447039A CN115717215B CN 115717215 B CN115717215 B CN 115717215B CN 202211447039 A CN202211447039 A CN 202211447039A CN 115717215 B CN115717215 B CN 115717215B
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stainless steel
steel ladle
tube material
lead
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CN115717215A (en
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陈敏莉
徐杨
王旻
马颖澈
陈刘涛
石林
梁田
郝宪朝
易昊钰
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Institute of Metal Research of CAS
China General Nuclear Power Corp
China Nuclear Power Technology Research Institute Co Ltd
CGN Power Co Ltd
Lingao Nuclear Power Co Ltd
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Institute of Metal Research of CAS
China General Nuclear Power Corp
China Nuclear Power Technology Research Institute Co Ltd
CGN Power Co Ltd
Lingao Nuclear Power Co Ltd
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    • Y02E30/30Nuclear fission reactors

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Abstract

The invention discloses a stainless steel ladle shell tube material for a lead bismuth fast reactor fuel assembly and a preparation method thereof; the cladding material comprises the elements Fe, cr, ni, mn, ti, mo, al, C, si, B, wherein the mass percentages of the elements in the material are respectively: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0% or less of Al or less than 0.3%, and the mass percentage ratio Ti/C of Ti to C is (4-6): 1; the balance being Fe; the preparation method comprises the following steps: and (3) performing vacuum induction melting and vacuum arc self-weight melting to obtain an alloy ingot, forging and rolling the alloy ingot to obtain the stainless steel ladle shell tube. The stainless steel shell and tube material provided by the invention has good room temperature and high temperature mechanical properties and excellent lead-bismuth liquid metal corrosion resistance.

Description

Stainless steel ladle shell tube material for lead-bismuth fast reactor fuel assembly and preparation method thereof
Technical Field
The invention relates to the technical field of nuclear materials, in particular to a stainless steel cladding tube for a lead-bismuth fast reactor fuel assembly and a preparation method thereof.
Background
The fuel assembly is one of the most central components of a lead-based reactor, and the working environment is severe. Because of its direct contact with liquid lead-based coolants, the fuel assembly structural materials are required to be resistant to high temperatures, irradiation, and also to have excellent resistance to liquid metal corrosion. The 15Cr-15Ni series Ti-containing austenitic stainless steel has good tissue stability, excellent processing performance, high use temperature, maximum radiation damage resistant dosage of 150dpa, good application prospect and is one of main candidate structural materials of the lead-based fast reactor cladding tube. But the current application experience of 15-15Ti alloy is mostly from sodium-cooled fast reactor. The coolant used in lead-based fast stacks (lead and lead bismuth eutectic alloy) is more corrosive than sodium cooled fast stacks. Therefore, if the 15-15Ti alloy is used as a lead-based fast reactor cladding tube material, the liquid metal corrosion resistance of the 15-15Ti alloy needs to be further optimized and improved.
In order to improve the corrosion resistance of 15-15Ti austenitic stainless steel, it is common to modify or add Si, ti, mn, al or other alloying elements. The design of the material components for improving the corrosion performance of lead and bismuth often affects other important properties of the material, such as mechanical properties, irradiation tissue stability and the like. The composition ranges of 15-15Ti are not unified at home and abroad, and a stainless steel ladle shell tube material with corrosion resistance, uniform structure and excellent surface quality for a lead-based reactor fuel assembly and a preparation method thereof are required to be developed on the basis of not affecting important structural material characteristics such as mechanical property, welding property and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a stainless steel cladding tube for a lead-bismuth fast reactor fuel assembly and a preparation method thereof.
The technical scheme adopted for solving the technical problems is as follows: a stainless steel ladle casing tube material for a lead-bismuth fast reactor fuel assembly, which comprises the following elements Fe, cr, ni, mn, ti, mo, al, C, si, B by mass percent: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0% or less of Al or less than 0.3%, and the mass percentage ratio Ti/C of Ti to C is (4-6): 1; the balance being Fe.
Preferably, the total mass percent of all impurity elements of the stainless steel ladle shell and tube material is not higher than 0.03%; among the impurity elements, the mass percent of P is not higher than 0.01%, the mass percent of N is not higher than 0.003%, the mass percent of S is not higher than 0.0015%, and the mass percent of O is not higher than 0.0015%.
The preparation method of the stainless steel ladle casing pipe material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 15-20%; the proportion of the raw materials meets the mass percentage of the elements: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0% or less of Al or less than 0.3%, and the mass percentage ratio Ti/C of Ti to C is (4-6): 1; the balance being Fe; the mass percentage of the polysilicon is 0.3-0.5%;
s2, vacuum induction melting: adding polysilicon twice, firstly, placing partial polysilicon, nickel plate, pure iron, molybdenum strip and metal chromium into a reaction container, vacuumizing and refining; adding carbon and metal aluminum, stopping power transmission after the carbon and the metal aluminum are melted, introducing protective gas, re-transmitting power, adding the rest polysilicon, metal manganese, ferroboron and sponge titanium at a first preset temperature, stirring, adjusting the temperature of molten steel to a second preset temperature, and pouring into a mold to obtain an alloy ingot casting primary body;
s3, vacuum arc consumable remelting: cutting off the shrinkage cavity part of the alloy ingot casting primary body obtained in the step S2, and carrying out vacuum arc consumable remelting to obtain a consumable remelting ingot;
s4, forging: upsetting-drawing and homogenizing the consumable remelting cast ingot obtained in the step S3 to obtain an alloy forging rod;
s5, rolling the pipe: and (3) processing the alloy forging rod obtained in the step (S4) into a tube blank, performing multi-pass cold rolling and heat treatment, and finally performing pre-deformation cold rolling to obtain the stainless steel shell tube.
Preferably, in the step S2, vacuum is pumped until the vacuum degree is less than or equal to 5.0Pa, and refining is carried out for 10-20min at 1300-1700 ℃.
Preferably, in the step S2, the shielding gas is argon; the first preset temperature is 1350-1400 ℃; the second preset temperature is 1500-1550 ℃.
Preferably, in the step S3, the shrinkage cavity is cut off by 50-80mm.
Preferably, in the step S4, 20-40% upsetting-drawing pre-deformation and homogenization treatment are performed, and then upsetting-drawing is performed for 2-5 times, wherein the final deformation is 30-40%; wherein the temperature of the homogenization treatment is 1150-1200 ℃, and the heat preservation time of the homogenization treatment is 11-12h.
Preferably, in the step S4, the diameter of the alloy forging bar is 45-55mm; in the step S5, the outer diameter of the tube blank is 40-50mm, and the wall thickness is 4-5mm.
Preferably, in the step S5, the tube blank is subjected to solution treatment before cold rolling, wherein the temperature of the solution treatment is 1050-1100 ℃, and the time of the solution treatment is 20-40min.
Preferably, in the step S5, the number of cold rolling passes is 8-15; the deformation amount of the pre-deformation cold rolling is 15-25%, and the feeding amount is 1-2mm/min.
Preferably, in the step S5, the heat treatment includes an intermediate heat treatment and a final heat treatment; wherein the temperature of the intermediate heat treatment is 1050-1100 ℃, and the time of the intermediate heat treatment is 10-30min; the temperature of the final heat treatment is 1030-1080 ℃, and the time of the final heat treatment is 8-15min.
The invention has the beneficial effects that:
the invention provides a stainless steel ladle tube material for a lead-bismuth fast reactor fuel assembly, which improves the structural uniformity of alloy cast ingots, improves the oxidation resistance of the stainless steel ladle tube material and reduces inclusions in the material by reducing the Mn content, adjusting the Al content and strictly controlling the N content.
The invention provides a preparation method of a stainless steel ladle shell tube material for a lead-bismuth fast reactor fuel assembly, which can more accurately control the content of chemical elements in the stainless steel ladle shell tube material, better reduce the content of impurity elements and improve the tissue uniformity and cold and hot processing performance of the material. The forging is performed by adopting a method of multiple upsetting deformation and homogenization treatment, so that segregation of the cast ingot in the solidification process is eliminated, and an excellent deformation structure without strip structure and macroscopic defects is obtained. The stainless steel ladle shell tube material has good room temperature and high temperature mechanical properties and excellent lead-bismuth liquid metal corrosion resistance, and can better meet the material selection requirement of a lead-bismuth fast reactor fuel assembly.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a microstructure of an alloy wrought bar of example 1 of the present invention;
FIG. 2 is a microstructure of an alloy wrought bar of example 2 of the present invention;
FIG. 3 is a microstructure of a stainless steel cladding tube of example 1 of the present invention;
FIG. 4 is a microstructure of a stainless steel cladding tube of example 2 of the present invention;
FIG. 5 is a graph showing the results of the lead bismuth corrosion test in example 1 of the present invention;
FIG. 6 is a graph showing the results of the lead bismuth corrosion test in example 2 of the present invention;
FIG. 7 is a graph showing the results of lead bismuth corrosion tests on stainless steel 15-15 Ti.
Detailed Description
The present invention will be further described in detail with reference to the following examples, which are only for explaining the present invention and are not to be construed as limiting the scope of the present invention, for the purpose of making a clearer understanding of the technical features, objects and effects of the present invention.
The stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the elements of Fe (iron), cr (chromium), ni (nickel), mn (manganese), ti (titanium), mo (molybdenum), al (aluminum), C (carbon), si (silicon) and B (boron), wherein the mass percentages of the elements in the material are as follows: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0% or less of Al or less than 0.3%, and the mass percentage ratio Ti/C of Ti to C is (4-6): 1; the balance being Fe.
It should be noted that the ratio of Ti to C in mass percent is (4-6): 1, i.e., ti/C may be 4:1, 4.5:1, 4.67:1, 5:1, 5.6:1, 6:1, etc., without limitation. In addition, the rest elements refer to elements except Cr, ni, mn, ti, mo, al, C, si and B in the stainless steel raw material, namely Fe which is a basic metal element of the stainless steel ladle tube material.
The total mass percentage of all impurity elements of the stainless steel shell and tube material is not higher than 0.03%; among the impurity elements, P (phosphorus) is not more than 0.01% by mass, N (nitrogen) is not more than 0.003% by mass, S (sulfur) is not more than 0.0015% by mass, and O (oxygen) is not more than 0.0015% by mass. Wherein, the mass percentages of P, N, S and O are controlled within the corresponding ranges, and are not particularly limited herein.
Mn element is an element for stabilizing austenite, can stabilize a single-phase austenite matrix of the alloy and improve the tensile plasticity of the alloy, but has strong volatility, is easy to form component fluctuation in the smelting process, and is unsuitable for excessively high content. Therefore, in order to improve the structural uniformity of the alloy ingot without affecting the alloy performance, the mass percentage of Mn element in the invention is 1.0-1.2%.
In order to improve the oxidation resistance of the stainless steel shell and tube material, the invention adds Al element with the mass percentage of 0-0.3 percent.
The N element is a main source of inclusion TiN, the N content is strictly controlled below 0.003 percent by mass, and the number of the inclusions is reduced, so that the performance of the stainless steel ladle shell and tube material is improved.
The preparation method of the stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: polysilicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium are used as raw materials, and the proportions among the raw materials satisfy the mass percentages of the elements: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0% or less of Al or less than 0.3%, and the mass percentage ratio Ti/C of Ti to C is (4-6): 1; the balance being Fe.
Wherein the mass percentage of boron element in the ferroboron is 15-20%; when the consumption of pure iron is calculated, firstly, the consumption of the ferroboron alloy is calculated according to the mass percentage of boron in the stainless steel shell and tube material of 0.003-0.004%, then the content of iron element in the ferroboron alloy is determined, and finally, the consumption of pure iron is calculated.
The mass percentage of the polysilicon is 0.3-0.5%.
S2, vacuum induction melting: adding polysilicon twice, firstly, placing partial polysilicon, nickel plate, pure iron, molybdenum strip and metal chromium into a reaction container, vacuumizing and refining; and adding carbon and metal aluminum, stopping power transmission after the carbon and the metal aluminum are melted, introducing protective gas, re-transmitting power, adding the rest polysilicon, the metal manganese, the ferroboron and the titanium sponge at a first preset temperature, stirring, adjusting the temperature of molten steel to a second preset temperature, and pouring into a mold to obtain an alloy ingot casting primary body.
Preferably, in the above steps, after the raw materials are added for the first time, vacuum is pumped to a vacuum degree of less than or equal to 5.0Pa, and refining is carried out for 10-20min at 1300-1700 ℃. After the material is added again, argon gas can be used as shielding gas to be introduced, and the first preset temperature can be 1350-1400 ℃ and the second preset temperature can be 1500-1550 ℃.
Specifically, vacuum induction melting: adding polysilicon twice, firstly placing partial polysilicon, nickel plate, pure iron, molybdenum strip and chromium in crucible of vacuum induction furnace, vacuum-pumping the furnace until vacuum degree is less than or equal to 5.0Pa (vacuum degree is less than or equal to 5.0Pa, and the vacuum degree is not limited), refining at 1300-1700 deg.C for 10-20min; and adding carbon and aluminum, stopping power transmission after the carbon and aluminum are melted, introducing shielding gas argon, re-transmitting power, adding the rest polysilicon, manganese, ferroboron and sponge titanium at 1350-1400 ℃, stirring, adjusting the temperature of molten steel to 1500-1550 ℃, and pouring into a mould to obtain an alloy ingot casting primary body.
In the smelting process, the polysilicon is added in two times, wherein the first time is used for deoxidizing, and the second time is used for better controlling the Si content in the stainless steel material. In order to avoid the reaction of metal raw materials in the smelting process, inert gas is selected as the shielding gas, and argon is selected as the shielding gas in consideration of smelting effect and economy. The loss of the metal raw material is small in the state of argon and lower first preset temperature (1350-1400 ℃), and oxidization is not easy to occur; and because the ambient pressure is high, the molten steel is not easy to overflow, and the content of the stainless steel is convenient to control.
S3, vacuum arc consumable remelting: and (2) cutting off the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2), and carrying out vacuum arc consumable remelting to obtain a consumable remelting ingot casting.
Preferably, in the above step, the shrinkage cavity is cut off by 50-80mm.
Specifically, vacuum arc consumable remelting: and (2) cutting the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2) by 50-80mm, and carrying out vacuum arc consumable remelting in a consumable furnace as a remelting electrode to obtain a consumable remelting ingot. And (3) performing head and tail cutting, surface peeling and cutting treatment after the cast ingot is cooled. The head and tail cutting aims at removing shrinkage cavities of steel ingots and non-compact parts of materials, the peeling treatment surface defects provide good conditions for subsequent forging, and the cutting treatment aims at facilitating the forging and obtaining more uniform deformed tissues. The head and tail cutting, surface peeling and cutting are all the prior art and are not described in detail herein.
S4, forging: upsetting-drawing and homogenizing the consumable remelting cast ingot obtained in the step S3 to obtain an alloy forging rod.
Preferably, in the steps, 20-40% upsetting-drawing pre-deformation and homogenization treatment are carried out, and then upsetting-drawing is carried out for 2-5 times, wherein the final deformation is 30-40%; wherein the homogenization temperature is 1150-1200 ℃, and the homogenization heat preservation time is 11-12h.
Specifically, forging: performing 20-40% upsetting-drawing pre-deformation on the consumable remelting cast ingot obtained in the step S3, performing homogenization treatment at 1150-1200 ℃ for 11-12 hours, and repeatedly performing upsetting for 2-5 times, wherein the final upsetting deformation is 30-40%, so as to obtain an alloy forging rod with the diameter of 45-55mm; the forged bar has no carbide and fine grain structure distributed in a strip shape, and the grain size is more than grade 3.
S5, rolling the pipe: and (3) processing the alloy forging rod obtained in the step (S4) into a tube blank, performing multi-pass cold rolling and heat treatment, and finally performing pre-deformation cold rolling to obtain the stainless steel shell tube.
Preferably, the alloy forging bar is processed to form a tube blank with an outer diameter of 40-50mm and a wall thickness of 4-5mm. In the steps, the number of cold rolling passes is 8-15; the deformation amount of the pre-deformation cold rolling is 15-25%, and the feeding amount is 1-2mm/min; the heat treatment comprises intermediate heat treatment and final heat treatment, wherein the temperature of the intermediate heat treatment is 1050-1100 ℃, and the time of the intermediate heat treatment is 10-30min; the final heat treatment temperature is 1030-1080 ℃, and the final heat treatment time is 8-15min.
Further, the pipe blank is subjected to solution treatment before cold rolling, wherein the temperature of the solution treatment is 1050-1100 ℃, and the time of the solution treatment is 20-40min.
Specifically, pipe rolling: processing the alloy forging rod obtained in the step S4 into a tube blank with the outer diameter of 40-50mm and the wall thickness of 4-5mm, and carrying out solid solution treatment at 1050-1100 ℃ in an atmosphere protection furnace for 20-40min; then performing 8-15 times of cold rolling deformation, wherein the intermediate heat treatment temperature is 1050-1100 ℃ and the time is 10-30min, and the final heat treatment is performed in an atmosphere protection roller type continuous heat treatment furnace, and the treatment temperature is 1030-1080 ℃ and the time is 8-15min; the deformation amount of the pre-deformation cold rolling is 15-25%, the feeding amount is 1-2mm/min, and finally the stainless steel cladding tube with the average grain size of 7-9 grades is obtained. The size of the stainless steel ladle tube is selected and set according to actual requirements, and is not limited herein.
The preparation method comprises the steps of obtaining an alloy cast ingot by adopting a vacuum induction smelting and vacuum arc consumable remelting process, cogging the cast ingot by adopting a forging mode of repeated upsetting deformation and high-temperature homogenization treatment to obtain an alloy forged bar, preparing a tube blank by adopting machining, carrying out multi-pass cold rolling and heat treatment, and finally applying 15-25% cold working pre-deformation by adopting a cold rolling process to obtain the stainless steel ladle shell tube.
Austenitic stainless steel materials for lead bismuth fast reactors, such as austenitic stainless steel 15-15Ti, prepared by the prior art are not ideal in lead bismuth corrosion resistance, and the prior art does not accurately control alloy elements, particularly microelements such as nitrogen, carbon and the like in the preparation process of the stainless steel materials.
The invention can accurately control the element content in the stainless steel ladle tube material, improves the tissue uniformity of the cast ingot, reduces the number of inclusions and improves the oxidation resistance and cold and hot processing performance of the material by reducing the Mn content, adjusting the Al content and strictly controlling the N content. The invention can ensure that the solidification segregation of the cast ingot is eliminated, and excellent deformation tissue without strip tissue and macroscopic defect is obtained. Compared with similar stainless steel, the stainless steel ladle tube material prepared by the invention has good room temperature and high temperature mechanical properties and excellent lead bismuth liquid metal corrosion resistance, and can better meet the material selection requirement of a lead bismuth fast reactor fuel assembly.
The following is described by way of specific examples:
example 1
A stainless steel ladle casing tube material for a lead-bismuth fast reactor fuel assembly, which comprises the following elements Fe, cr, ni, mn, ti, mo, C, si, B by mass percent: 0.06% of C, 16.00% of Cr, 15.00% of Ni, 1.20% of Mn, 0.36% of Ti, 1.50% of Mo, 0.40% of Si, 0.003% of B and 65.477% of Fe. The total mass percentage of all impurity elements of the stainless steel shell and tube material is not higher than 0.03%; among the impurity elements, the mass percentage of P is not higher than 0.01%, the mass percentage of N is not higher than 0.003%, the mass percentage of S is not higher than 0.0015%, and the mass percentage of O is not higher than 0.0015%.
The preparation method of the stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 17%; the proportion of the raw materials meets the mass percentage of the elements: 0.06% of C, 16.00% of Cr, 15.00% of Ni, 1.20% of Mn, 0.36% of Ti, 1.50% of Mo, 0.40% of Si, 0.003% of B and 65.477% of Fe.
S2, vacuum induction melting: adding polysilicon twice, firstly, placing part of polysilicon, nickel plate, pure iron, molybdenum strip and chromium in a crucible of a vacuum induction furnace, vacuumizing the furnace until the vacuum degree is less than or equal to 5.0Pa, and refining for 15min at 1500 ℃; and adding carbon and aluminum, stopping power transmission after the carbon and aluminum are melted, introducing shielding gas argon, re-transmitting power, adding the rest polysilicon, manganese, ferroboron and titanium sponge at 1370 ℃, stirring, adjusting the temperature of molten steel to 1525 ℃, and pouring into a mould to obtain an alloy ingot casting primary body.
S3, vacuum arc consumable remelting: and (2) cutting the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2) by 60mm, and carrying out vacuum arc consumable remelting in a consumable furnace as a remelting electrode to obtain a consumable remelting ingot. And (3) performing head and tail cutting, surface peeling and cutting treatment after the cast ingot is cooled.
S4, forging: and (3) heating the consumable remelting cast ingot obtained in the step (S3) to 1200 ℃ for heat preservation for 2 hours, then carrying out 40% upsetting-drawing pre-deformation, then carrying out homogenization treatment at 1200 ℃ for 12 hours, and repeatedly carrying out upsetting for 2 times, wherein the final deformation of upsetting is 40%, thus obtaining the alloy forging rod with the diameter of 50 mm.
S5, rolling the pipe: processing the alloy forging rod obtained in the step S4 into a tube blank with the outer diameter of 42mm and the wall thickness of 4.5mm, and carrying out solution treatment at 1080 ℃ for 30min in an atmosphere protection furnace; then carrying out 10-pass cold rolling deformation, wherein the intermediate heat treatment temperature is 1080 ℃, the time is 20min, and the final heat treatment is carried out in an atmosphere protection roller type continuous heat treatment furnace, the treatment temperature is 1060 ℃ and the time is 12min; the deformation amount of the pre-deformation cold rolling is 20%, and the feeding amount is 1.5mm/min, so that the stainless steel ladle shell tube is obtained.
Example 2
A stainless steel ladle casing tube material for a lead-bismuth fast reactor fuel assembly, which comprises the following elements Fe, cr, ni, mn, ti, mo, al, C, si, B by mass percent: 0.06% of C, 16.00% of Cr, 15.00% of Ni, 1.20% of Mn, 0.36% of Ti, 1.50% of Mo, 0.2% of Al, 0.40% of Si, 0.003% of B and 65.277% of Fe. The total mass percentage of all impurity elements of the stainless steel shell and tube material is not higher than 0.03%; among the impurity elements, the mass percentage of P is not higher than 0.01%, the mass percentage of N is not higher than 0.003%, the mass percentage of S is not higher than 0.0015%, and the mass percentage of O is not higher than 0.0015%.
The preparation method of the stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 17%; the proportion of the raw materials meets the mass percentage of the elements: 0.06% of C, 16.00% of Cr, 15.00% of Ni, 1.20% of Mn, 0.36% of Ti, 1.50% of Mo, 0.2% of Al, 0.40% of Si, 0.003% of B and 65.277% of Fe.
S2, vacuum induction melting: adding polysilicon twice, firstly, placing part of polysilicon, nickel plate, pure iron, molybdenum strip and chromium in a crucible of a vacuum induction furnace, vacuumizing the furnace until the vacuum degree is less than or equal to 5.0Pa, and refining for 15min at 1500 ℃; and adding carbon and aluminum, stopping power transmission after the carbon and aluminum are melted, introducing shielding gas argon, re-transmitting power, adding the rest polysilicon, manganese, ferroboron and titanium sponge at 1370 ℃, stirring, adjusting the temperature of molten steel to 1525 ℃, and pouring into a mould to obtain an alloy ingot casting primary body.
S3, vacuum arc consumable remelting: and (2) cutting the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2) by 60mm, and carrying out vacuum arc consumable remelting in a consumable furnace as a remelting electrode to obtain a consumable remelting ingot. And (3) performing head and tail cutting, surface peeling and cutting treatment after the cast ingot is cooled.
S4, forging: and (3) heating the consumable remelting cast ingot obtained in the step (S3) to 1200 ℃ for heat preservation for 2 hours, then carrying out 40% upsetting-drawing pre-deformation, then carrying out homogenization treatment at 1200 ℃ for 12 hours, and repeatedly carrying out upsetting for 2 times, wherein the final deformation of upsetting is 40%, thus obtaining the alloy forging rod with the diameter of 50 mm.
S5, rolling the pipe: processing the alloy forging rod obtained in the step S4 into a tube blank with the outer diameter of 42mm and the wall thickness of 4.5mm, and carrying out solution treatment at 1080 ℃ for 30min in an atmosphere protection furnace; then carrying out 12-pass cold rolling deformation, wherein the intermediate heat treatment temperature is 1080 ℃, the time is 20min, and the final heat treatment is carried out in an atmosphere protection roller type continuous heat treatment furnace, the treatment temperature is 1060 ℃ and the time is 12min; the deformation amount of the pre-deformation cold rolling is 20%, and the feeding amount is 1.5mm/min, so that the stainless steel ladle shell tube is obtained.
Example 3
A stainless steel ladle casing tube material for a lead-bismuth fast reactor fuel assembly, which comprises the following elements Fe, cr, ni, mn, ti, mo, al, C, si, B by mass percent: 0.04% of C, 15.00% of Cr, 14.00% of Ni, 1.00% of Mn, 0.20% of Ti, 1.30% of Mo, 0.10% of Al, 0.30% of Si, 0.004% of B and 68.056% of Fe. The total mass percentage of all impurity elements of the stainless steel shell and tube material is not higher than 0.03%; among the impurity elements, the mass percentage of P is not higher than 0.01%, the mass percentage of N is not higher than 0.003%, the mass percentage of S is not higher than 0.0015%, and the mass percentage of O is not higher than 0.0015%.
The preparation method of the stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 17%; the proportion of the raw materials meets the mass percentage of the elements: 0.04% of C, 15.00% of Cr, 14.00% of Ni, 1.00% of Mn, 0.20% of Ti, 1.30% of Mo, 0.10% of Al, 0.30% of Si, 0.004% of B and 68.056% of Fe.
S2, vacuum induction melting: adding polysilicon twice, firstly, placing part of polysilicon, nickel plate, pure iron, molybdenum strip and chromium in a crucible of a vacuum induction furnace, vacuumizing the furnace until the vacuum degree is less than or equal to 5.0Pa, and refining for 20min at 1300 ℃; and adding carbon and aluminum, stopping power transmission after the carbon and aluminum are melted, introducing shielding gas argon, re-transmitting power, adding the rest polysilicon, manganese, ferroboron and titanium sponge at 1350 ℃, stirring, adjusting the temperature of molten steel to 1500 ℃, and pouring into a mold to obtain an alloy ingot casting primary body.
S3, vacuum arc consumable remelting: and (2) cutting the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2) by 50mm, and carrying out vacuum arc consumable remelting in a consumable furnace as a remelting electrode to obtain a consumable remelting ingot. And (3) performing head and tail cutting, surface peeling and cutting treatment after the cast ingot is cooled.
S4, forging: and (3) heating the consumable remelting cast ingot obtained in the step (S3) to 1150 ℃, preserving heat for 2.5 hours, carrying out 20% upsetting-drawing pre-deformation, carrying out homogenization treatment at 1150 ℃ for 11.5 hours, and repeatedly upsetting for 3 times, wherein the final upsetting deformation is 30%, so as to obtain the alloy forging rod with the diameter of 45 mm.
S5, rolling the pipe: processing the alloy forging rod obtained in the step S4 into a tube blank with the outer diameter of 40mm and the wall thickness of 4mm, and carrying out solid solution treatment at 1050 ℃ in an atmosphere protection furnace for 40min; then performing 8-pass cold rolling deformation, wherein the intermediate heat treatment temperature is 1050 ℃, the time is 30min, and the final heat treatment is performed in an atmosphere protection roller type continuous heat treatment furnace, the treatment temperature is 1030 ℃, and the time is 15min; the deformation amount of the pre-deformation cold rolling is 15%, and the feeding amount is 1.0mm/min, so that the stainless steel ladle shell tube is obtained.
Example 4
A stainless steel ladle casing tube material for a lead-bismuth fast reactor fuel assembly, which comprises the following elements Fe, cr, ni, mn, ti, mo, al, C, si, B by mass percent: 0.08% of C, 16.00% of Cr, 16.00% of Ni, 1.10% of Mn, 0.48% of Ti, 1.40% of Mo, 0.30% of Al, 0.50% of Si, 0.004% of B and 64.136% of Fe. The total mass percentage of all impurity elements of the stainless steel shell and tube material is not higher than 0.03%; among the impurity elements, the mass percentage of P is not higher than 0.01%, the mass percentage of N is not higher than 0.003%, the mass percentage of S is not higher than 0.0015%, and the mass percentage of O is not higher than 0.0015%.
The preparation method of the stainless steel ladle shell tube material for the lead-bismuth fast reactor fuel assembly comprises the following steps:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 17%; the proportion of the raw materials meets the mass percentage of the elements: 0.08% of C, 16.00% of Cr, 16.00% of Ni, 1.10% of Mn, 0.48% of Ti, 1.40% of Mo, 0.30% of Al, 0.50% of Si, 0.004% of B and 64.136% of Fe.
S2, vacuum induction melting: adding polysilicon twice, firstly, placing part of polysilicon, nickel plate, pure iron, molybdenum strip and chromium in a crucible of a vacuum induction furnace, vacuumizing the furnace until the vacuum degree is less than or equal to 5.0Pa, and refining for 10min at 1700 ℃; and adding carbon and aluminum, stopping power transmission after the carbon and aluminum are melted, introducing shielding gas argon, re-transmitting power, adding the rest polysilicon, manganese, ferroboron and titanium sponge at 1400 ℃, stirring, adjusting the temperature of molten steel to 1550 ℃, and pouring into a mould to obtain an alloy ingot casting primary body.
S3, vacuum arc consumable remelting: and (2) cutting the shrinkage cavity part of the alloy ingot casting primary body obtained in the step (S2) by 80mm, and carrying out vacuum arc consumable remelting in a consumable furnace as a remelting electrode to obtain a consumable remelting ingot. And (3) performing head and tail cutting, surface peeling and cutting treatment after the cast ingot is cooled.
S4, forging: and (3) heating the consumable remelting cast ingot obtained in the step (S3) to 1180 ℃ and preserving heat for 1.5 hours, then carrying out 30% upsetting-drawing pre-deformation, then carrying out homogenization treatment at 1180 ℃ for 12 hours, and repeatedly carrying out upsetting for 5 times, wherein the final deformation of upsetting is 35%, thus obtaining the alloy forging rod with the diameter of 55 mm.
S5, rolling the pipe: processing the alloy forging rod obtained in the step S4 into a tube blank with the outer diameter of 50mm and the wall thickness of 5mm, and carrying out solution treatment at 1100 ℃ in an atmosphere protection furnace for 20min; then carrying out 15-pass cold rolling deformation, wherein the intermediate heat treatment temperature is 1100 ℃, the time is 10min, and the final heat treatment is carried out in an atmosphere protection roller type continuous heat treatment furnace, the treatment temperature is 1080 ℃, and the time is 8min; the deformation amount of the pre-deformation cold rolling is 25%, and the feeding amount is 2.0mm/min, so that the stainless steel ladle shell tube is obtained.
Comparison test:
comparing the performances of the 15Cr-15Ni series Ti-containing austenitic stainless steel (hereinafter referred to as 15-15 Ti) commonly used for lead-based fast reactor cladding tubes in the invention in example 1 and example 2, the chemical compositions of the 15-15Ti adopted in the invention are as follows: 16wt.% Cr, 15wt.% Ni, 1.5wt.% Mn, 0.36wt.% Ti, 2.1wt.% Mo, 0.40wt.% Si. 15-15Ti is mainly different from the stainless steel ladle tube material of the invention in that the Mn content is not reduced, the Al content is not required and the N content is not strictly controlled.
1. Component detection
Test instrument: oxygen-nitrogen-hydrogen analyzer, carbon-sulfur analyzer and optical microscope
The test steps are as follows: chemical composition detection was performed on consumable remelted ingots of example 1 and example 2, and microscopic observation was performed on alloy forged bars obtained by forging the consumable remelted ingots, the composition detection results are shown in table 1, and the microscopic observation results of the forged bars are shown in fig. 1 and 2. The O, N, H, C, S element is detected by an element analyzer, other elements are detected by a chemical method, the component detection is not usually carried out on the basic metal element, and the basic metal element of the consumable remelting ingot is Fe, so that the detection of Fe element is not needed.
2. Quality inspection
Test instrument: ultrasonic nondestructive flaw detector and optical microscope
The test steps are as follows: ultrasonic flaw detection and microscopic observation were performed on the stainless steel ladle pipes of example 1 and example 2, and microscopic observation results are shown in fig. 3 and 4.
3. Tensile test, high temperature endurance test
Test instrument: universal tensile testing machine
The test steps are as follows: stainless steel cladding tubes prepared in example 1, example 2 and 15-15Ti, respectively, were subjected to a high temperature tensile test at a temperature of 650 ℃ and a high temperature endurance test at a temperature of 1000 hours, and the test results are shown in Table 2.
4. Lead bismuth Corrosion test
Test instrument: optical microscope
The test steps are as follows: stainless steel cladding tubes prepared in example 1, example 2 and 15-15Ti respectively were subjected to static lead bismuth liquid metal corrosion at 600 ℃ for 500 hours, then observed under a microscope, and the test results are shown in fig. 5-7.
Table 1 results of the composition detection of consumable remelted ingots of example 1 and example 2
TABLE 2 comparison of the Properties of example 1, examples 2 and 15-15Ti
As shown in Table 1, the total content of all impurity elements in the consumable remelting cast ingot is lower than 0.03%, and the content is lower, which indicates that the content control of the impurity elements is good; the content of other elements is very close to the element proportion of the raw materials, which indicates that the components in the stainless steel ladle shell and tube material are well controlled. In addition, as can be seen from fig. 1 and 2, the alloy forging bar of the present invention has excellent deformed structure without the presence of banding carbide and macroscopic defects; the solidification segregation of the cast ingot is eliminated, and the grain size is more than 3 grades. In addition, the ultrasonic flaw detection quality detection result of the stainless steel cladding tube is qualified, and as can be seen from figures 3 and 4, the microstructure of the cladding tube is well controlled, the grain structure is uniform, and the grain size is 7-8 grades. Therefore, the stainless steel ladle shell tube material has uniform structure and excellent surface quality.
As shown in Table 2, the stainless steel ladle tube has good room temperature, high temperature tensile strength and tensile plasticity, and high temperature durability equivalent to that of stainless steel 15-15Ti, and the stainless steel ladle tube material has good room temperature and high temperature mechanical properties.
From fig. 5-7 it can be seen that the oxide thickness of the cladding tube of example 1 was 42 μm, the oxide thickness of the cladding tube of example 2 was 35 μm, and the oxide thickness of the 15-15Ti cladding tube was 83 μm after 500h static lead bismuth corrosion at 600 ℃. Therefore, the thickness of the generated oxide layer of the stainless steel ladle pipe material is smaller than that of similar austenitic stainless steel 15-15Ti after lead bismuth corrosion, and the stainless steel ladle pipe material has excellent lead bismuth liquid metal corrosion resistance.
In summary, the invention provides a stainless steel ladle shell tube material for a lead bismuth fast reactor fuel assembly, which improves the structural uniformity of alloy cast ingots, improves the oxidation resistance of the stainless steel ladle shell tube material and reduces inclusions in the material by reducing the Mn content, adjusting the Al content and strictly controlling the N content.
The invention provides a preparation method of a stainless steel ladle shell tube material for a lead-bismuth fast reactor fuel assembly, which can more accurately control the content of chemical elements in the stainless steel ladle shell tube material, better reduce the content of impurity elements and improve the tissue uniformity and cold and hot processing performance of the material. The forging is performed by adopting a method of multiple upsetting deformation and homogenization treatment, so that segregation of the cast ingot in the solidification process is eliminated, and an excellent deformation structure without strip structure and macroscopic defects is obtained. The stainless steel ladle shell tube material has good room temperature and high temperature mechanical properties and excellent lead-bismuth liquid metal corrosion resistance, and can better meet the material selection requirement of a lead-bismuth fast reactor fuel assembly.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.

Claims (9)

1. The stainless steel ladle casing pipe material for the lead-bismuth fast reactor fuel assembly is characterized by comprising the following elements Fe, cr, ni, mn, ti, mo, al, C, si, B in percentage by mass: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0.1% or less of Al or less than 0.3%, and the ratio of Ti to C by mass percent Ti/C is (4-6): 1; the balance being Fe;
the total mass percentage of all impurity elements of the stainless steel ladle shell and tube material is not higher than 0.03%; among the impurity elements, the mass percent of P is not higher than 0.01%, the mass percent of N is not higher than 0.003%, the mass percent of S is not higher than 0.0015%, and the mass percent of O is not higher than 0.0015%;
the stainless steel ladle shell tube material is prepared by the following preparation method:
s1, weighing: taking polycrystalline silicon, nickel plates, pure iron, molybdenum strips, metallic chromium, carbon, metallic aluminum, metallic manganese, ferroboron and sponge titanium as raw materials, wherein the mass percentage of boron element in the ferroboron is 15-20%; the proportion of the raw materials meets the mass percentage of the elements: 0.04% or less of C or less than 0.08%, 15.0% or less of Cr or less than 17.0%, 14.0% or less of Ni or less than 16.0%, 0.3% or less of Si or less than 0.5%, 1.0% or less of Mn or less than 1.2%, 0.2% or less of Ti or less than 0.5%, 1.3% or less of Mo or less than 1.5%, 0.003% or less of B or less than 0.004%, 0.1% or less of Al or less than 0.3%, and the ratio of Ti to C by mass percent Ti/C is (4-6): 1; the balance being Fe; the mass percentage of the polysilicon is 0.3-0.5%;
s2, vacuum induction melting: adding polysilicon twice, firstly, placing partial polysilicon, nickel plate, pure iron, molybdenum strip and metal chromium into a reaction container, vacuumizing and refining; adding carbon and metal aluminum, stopping power transmission after the carbon and the metal aluminum are melted, introducing protective gas, re-transmitting power, adding the rest polysilicon, metal manganese, ferroboron and sponge titanium at a first preset temperature, stirring, adjusting the temperature of molten steel to a second preset temperature, and pouring into a mold to obtain an alloy ingot casting primary body; the first preset temperature is 1350-1400 ℃; the second preset temperature is 1500-1550 ℃;
s3, vacuum arc consumable remelting: cutting off the shrinkage cavity part of the alloy ingot casting primary body obtained in the step S2, and carrying out vacuum arc consumable remelting to obtain a consumable remelting ingot;
s4, forging: upsetting-drawing and homogenizing the consumable remelting cast ingot obtained in the step S3 to obtain an alloy forging rod;
s5, rolling the pipe: and (3) processing the alloy forging rod obtained in the step (S4) into a tube blank, performing multi-pass cold rolling and heat treatment, and finally performing pre-deformation cold rolling to obtain the stainless steel ladle shell tube.
2. The stainless steel ladle tube material for the lead-bismuth fast reactor fuel assembly according to claim 1, wherein in the step S2, vacuum is pumped to a vacuum degree of less than or equal to 5.0Pa, and refining is carried out for 10-20min at 1300-1700 ℃.
3. The stainless steel ladle tube material for lead bismuth fast reactor fuel assemblies according to claim 1, wherein in the step S2, the shielding gas is argon.
4. The stainless steel ladle tube material for lead bismuth fast reactor fuel assemblies according to claim 1, wherein in the step S3, the shrinkage cavity is cut off by 50-80mm.
5. The stainless steel ladle tube material for the lead bismuth fast reactor fuel assembly according to claim 1, wherein in the step S4, 20-40% upsetting-drawing pre-deformation and homogenization treatment are performed, and then upsetting-drawing is performed for 2-5 times, wherein the final deformation is 30-40%; wherein the temperature of the homogenization treatment is 1150-1200 ℃, and the heat preservation time of the homogenization treatment is 11-12h.
6. The stainless steel ladle tube material for a lead bismuth fast reactor fuel assembly according to claim 1, wherein in the step S4, the diameter of the alloy forging rod is 45-55mm; in the step S5, the outer diameter of the tube blank is 40-50mm, and the wall thickness is 4-5mm.
7. The stainless steel ladle tube material for a lead bismuth fast reactor fuel assembly according to claim 1, wherein in the step S5, the tube blank is subjected to solution treatment before cold rolling, wherein the temperature of the solution treatment is 1050-1100 ℃, and the time of the solution treatment is 20-40min.
8. The stainless steel ladle tube material for the lead bismuth fast reactor fuel assembly according to claim 1, wherein in the step S5, the number of cold rolling passes is 8-15; the deformation amount of the pre-deformation cold rolling is 15-25%, and the feeding amount is 1-2mm/min.
9. The stainless steel ladle tube material for a lead bismuth fast reactor fuel assembly according to claim 1, wherein in the step S5, the heat treatment includes an intermediate heat treatment and a final heat treatment; wherein the temperature of the intermediate heat treatment is 1050-1100 ℃, and the time of the intermediate heat treatment is 10-30min; the temperature of the final heat treatment is 1030-1080 ℃, and the time of the final heat treatment is 8-15min.
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GB993613A (en) * 1963-11-22 1965-06-02 Sandvikens Jernverks Ab Alloy steels and articles made therefrom
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CN109355558A (en) * 2018-11-01 2019-02-19 中广核研究院有限公司 Austenitic stainless steel and preparation method thereof, application
AU2020102032A4 (en) * 2019-08-28 2020-10-08 Harbin Well Welding Co., Ltd. Deposited metal of stainless steel electrode for fast reactor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB993613A (en) * 1963-11-22 1965-06-02 Sandvikens Jernverks Ab Alloy steels and articles made therefrom
US3384476A (en) * 1963-11-22 1968-05-21 Sandvikens Jernverks Ab Alloy steel and method of making same
RU2009135567A (en) * 2009-09-24 2011-03-27 Открытое акционерное общество "Высокотехнологический научно-исследовательский институт неорганических материалов имени академика А. A PARTICULAR WALL PIPE FROM AUSTENITE BORN-CONTAINING STEEL FOR A SHELL OF A FUEL AND A METHOD FOR PRODUCING IT
CN109355558A (en) * 2018-11-01 2019-02-19 中广核研究院有限公司 Austenitic stainless steel and preparation method thereof, application
AU2020102032A4 (en) * 2019-08-28 2020-10-08 Harbin Well Welding Co., Ltd. Deposited metal of stainless steel electrode for fast reactor

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