CN113913680A - Gd-containing duplex stainless steel with excellent neutron absorption performance and preparation method thereof - Google Patents
Gd-containing duplex stainless steel with excellent neutron absorption performance and preparation method thereof Download PDFInfo
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C21D2211/001—Austenite
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Abstract
The invention discloses Gd-containing duplex stainless steel with excellent neutron absorption performance and a preparation method thereof, and belongs to the technical field of duplex stainless steel. The stainless steel comprises the following components in percentage by mass: c: 0.02-0.06 wt.%; cr: 23.00-26.00 wt.%; ni: 4.00-8.00 wt.%; si: 1.00 wt.% or less; rare earth Gd: 0.50-3.00 wt.%; mn: 1.00-2.00 wt.%; mo: 1.00-2.00 wt.%; al < 0.10 wt.%; o < 0.002 wt.%; n < 0.02 wt.%; s < 0.002 wt.%; p < 0.010 wt.%; the balance of Fe. The Gd-containing duplex stainless steel has excellent comprehensive shielding performance for neutrons and gamma rays, hot-working crack resistance and good mechanical property, can be directly used as a structural member for designing and manufacturing neutron shielding products, and can realize functional structure integrated design.
Description
Technical Field
The invention relates to the technical field of nuclear radiation shielding protection, in particular to Gd-containing duplex stainless steel with excellent neutron absorption performance and a preparation method thereof.
Background
Along with the rapid development of nuclear power in China, increasing spent fuel and radioactive waste are serious problems in China, and about 2 ten thousand tons is expected to be generated in the end of 2030. The spent fuel and radioactive waste have strong neutron radiation in addition to strong alpha, beta and gamma rays, so that the transport container reaches 6 times or 20 times of the spent fuel from each ton of spent fuel and radioactive waste transported to a storage or post-treatment plant by a nuclear power plant, the efficiency is low, even if the storage and transport containers mostly depend on import and are insufficient in quantity, and on the other hand, the urgency of spent fuel treatment is further aggravated by the shortage of post-treatment capacity. Therefore, the research and development of the neutron absorption material with good neutron absorption performance and integrated functional structure design is the key of weight reduction and capacity expansion of the spent fuel container.
At present, the neutron absorption materials used abroad mainly comprise boron-containing cast steel, B4C-Al composite materials, lead-boron-polyethylene composite materials, cadmium-containing neutron absorption materials and the like. The boron-containing cast steel has low boron content, the processability of the boron-containing cast steel is sharply reduced along with the increase of the boron content, and the organic polymer is difficult to resist high temperature and easy to age under the irradiation condition, so B is selected at home and abroad4More C/Al composite materials exist. The American AAR company, the METAMIC company and the like are reported to produce B4C/Al material products such as Boral, tamic and the like by a powder metallurgy method and put into use in a spent fuel storage pool. The preparation method has already achieved initial achievements in the aspects of material preparation process, mechanical property research, corrosion influence, neutron absorption performance and the like in units such as China institute of engineering and physics, Jiangsu Syngnathus science and technology GmbH. But B4The C-Al plate can not be directly used in water environment, and is generally applied to the outer surface of a spent fuel storage cylinder firstly and then applied to the B4Welding a layer of stainless steel to the C-Al plate to weld B4Isolation of C-Al from water environmentOn, the spent fuel storage cylinder can not be fully covered by 360 degrees due to structural limitation4C-Al plate. Therefore, further reinforcement and perfection are needed from the structural and neutron shielding aspects. Moreover, B-containing neutron shielding materials have some common technical problems that natural B has limited neutron absorbing capacity and needs to be added with 10B or added with a large amount of B by powder metallurgy4C can meet the neutron absorption function, so that the manufacturing cost is greatly improved. In addition, in order to meet the neutron absorption performance, the great addition of the B content can cause fatal damage to the processing performance and the mechanical property of the material, and the application of the functional/structural integrated neutron shielding material of the high-B-content material is restricted.
In contrast, Gd is more advantageous than B. 157Gd has a neutron absorption cross section of 255000B, which is approximately 66 times the neutron absorption cross section of 10B. The equivalent thermal neutron absorption cross section of natural Gd is 49163B, which is 64 times that of natural B. It follows that the amount of Gd added to the alloy is relatively low to achieve the same neutron absorption capacity, e.g. 0.5 wt.% Gd is equivalent to a shielding effect of 2 wt.% B in steel. Besides the advantage of a large neutron absorption cross section, Gd-containing alloys have the following advantages: (1) gd is easy to add, only Gd metal is directly adopted for alloying during alloy smelting, the operation is convenient, a powder metallurgy mode is not needed, and the manufacturing cost is lower. (2) The Gd addition does not have adverse effect on the room-temperature mechanical properties of the alloy. Under the room temperature environment, the tensile strength of the duplex stainless steel hot rolled plate containing 1 wt.% Gd can reach 700.2MPa, the yield strength reaches 552.3MPa, the elongation is 38.08%, and the requirement of a structural material is met. (3) Gd does not generate He after absorbing neutrons, so that the material is irradiated to swell and helium is brittle, and meanwhile, the Gd has a certain shielding effect on gamma rays. (4) Under the condition of water, the Gd-containing phase in the alloy can not be dissolved as fast as chromium boride, and the alloy has better corrosion resistance. Therefore, the Gd-containing alloy is a novel ideal function/structure integrated neutron shielding material following the B-containing material.
Therefore, aiming at the requirements of the functional/structural integrated neutron shielding material, the Gd-containing duplex stainless steel with excellent neutron absorption performance is obtained by adjusting the content and the proportion of each element in the duplex stainless steel alloy through reasonable component design and assisting with the processes of heat treatment and the like.
Disclosure of Invention
Aiming at the urgent need of spent fuel treatment on a neutron absorption material with an integrated functional structure, the invention aims to provide Gd-containing duplex stainless steel with excellent neutron absorption performance and a preparation method thereof. The Gd-containing duplex stainless steel can meet the neutron absorption and radioactive ray shielding functions during spent fuel treatment, has good hot working performance and low processing cost through the optimization of alloy elements, and meets the integrated design requirement of a functional structure.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the Gd-containing duplex stainless steel with excellent neutron absorption performance comprises the following chemical components in percentage by weight:
c: 0.02-0.06 wt.%; cr: 23.00-26.00 wt.%; ni: 4.00-8.00 wt.%; si ≤ 1.00 wt.%; rare earth Gd: 0.50-3.00 wt.%; mn: 1.00-2.00 wt.%; mo: 1.00-2.00 wt.%; al < 0.10 wt.%; the balance of Fe.
In the chemical composition of the stainless steel, C is preferably 0.02-0.04 wt.%, Cr is preferably 23.00-25.00 wt.%, Ni is preferably 5.00-8.00 wt.%, and rare earth Gd is preferably 0.50-2.50 wt.%.
Controlling the contents of impurity elements in the stainless steel as follows: o < 0.002 wt.%; n < 0.02 wt.%; s < 0.002 wt.%; p < 0.010 wt.%.
The stainless steel consists of austenite and ferrite, and the volume ratio of the austenite phase to the ferrite phase is about 1: 1.
the chemical composition design mechanism of the duplex stainless steel is as follows:
the austenitic stainless steel contains C, Cr, Ni, Si, Gd, Mn, Mo, Al, N, and a small amount of impurity elements P, S, O. C, Cr, Ni, Si, Mn and Mo are alloyed, and importantly rare earth Gd is added for microalloying, so that the hot working performance of the material is improved, and the hot working process is optimized by adjusting the contents of Cr and Ni.
The element C being austenitizedThe element can obviously improve the proportion of an austenite phase to meet the condition that the proportion of the austenite phase to a ferrite phase is 1: 1, in the presence of a catalyst. And C can obviously improve the tensile strength of the duplex stainless steel by forming a gap solid solution. For Gd-containing duplex stainless steel, Cr is easy to precipitate at grain boundary in the hot working process due to the existence of higher Cr element23C6Carbide causes the matrix near the grain boundary to be poor in Cr, thereby reducing the intergranular corrosion resistance of the matrix. Therefore, the carbon content in the duplex stainless steel is properly reduced, and the C content is controlled as follows: 0.020-0.060 wt.%.
Cr is an element which strongly forms and stabilizes the ferrite phase, and its main role is to improve the corrosion resistance on the one hand and to secure the proportion of the ferrite phase in the structure on the other hand. The Cr content is controlled to be 23.00-26.00 wt.% in the invention.
Ni is a main forming element of an austenite phase, and mainly functions to enlarge an austenite phase region, form and stabilize the austenite phase, so as to satisfy a condition that a ratio of the austenite phase to a ferrite phase is 1: 1, in the presence of a catalyst. The Ni content is controlled to be 4.00-8.00 wt% in the invention.
The rare earth element Gd mainly plays a role in neutron absorption, but the adding time must be well mastered, and the rare earth element Gd is added when oxygen in molten steel is basically removed to be less than 0.001 wt%, so that the formation of rare earth oxide can be obviously reduced. Meanwhile, rare earth Gd can react with Ni element to precipitate two Gd-containing phases, one is a Gd-rich precipitated phase, and the Gd content is about 40%; one is a Gd-poor precipitated phase with a Gd content of about 12%, while the Gd-poor precipitated phase is more likely to coordinate deformation of the substrate at high temperatures and is less likely to crack the substrate during thermal deformation. And because rare earth Gd consumes Ni element in the matrix to generate precipitated phase, ferrite forming elements such as Cr, Mo, Si and the like in the matrix are enriched, the ratio of Ni equivalent to Cr equivalent in the alloy is changed, the ferrite content is increased, and the austenite phase content is reduced. The addition of 4.00 wt.% Gd to the alloy results in a complete transformation of the austenite phase to the ferrite phase in the duplex stainless steel and a single phase ferritic steel. Therefore, to ensure that the ratio of ferrite to austenite phases is 1: 1, the contents of Cr and Mo elements need to be properly reduced. Compared with the high-alloy duplex stainless steel with the same nickel content, the Gd-containing duplex stainless steel saves the addition of Cr and Mo elements and reduces the cost. In conclusion, the content of rare earth Gd in the invention is controlled to be 0.50-3.00 wt.%.
The Mo element is a ferrite element and is mainly used for improving the pitting corrosion resistance, the crevice corrosion resistance and other properties of the steel. In the invention, the Mo content is controlled to be 0.50-2.00 wt.%.
The Mn element is also an element for stabilizing austenite, and is mainly used for stabilizing an austenite structure and ensuring the stability of the proportion of an austenite phase. In the present invention, the Mn content is controlled to 0.50 to 1.50 wt.%.
Al is a strong deoxidizing element and also a strong ferrite forming element. Is mainly used for removing O before Gd is alloyed, so that the O content is reduced to the lowest level, and rare earth oxide is avoided being formed. However, when the Al content is high, Al inclusions can be formed in the alloy, and the high-temperature strength and toughness of the alloy can be reduced, and the Al content is controlled to be less than or equal to 0.10 wt%.
N is an intense austenite forming and stabilizing element, the range of an austenite phase region in a phase diagram is expanded strongly, and the content of N is controlled to be less than or equal to 0.02wt percent in the invention.
O is considered as a harmful impurity in duplex stainless steel and forms rare earth oxides with the added rare earth Gd very easily. Rare earth Gd is added into the alloy to play a certain role in deoxidation, but attention is paid to the removal of rare earth oxide, if the rare earth oxide is excessive, the hot working performance of the alloy is damaged, and therefore, the O content is controlled to be less than 0.002 wt.%.
The invention provides a preparation method of Gd-containing duplex stainless steel with excellent neutron absorption performance, which comprises the following specific steps:
pure metal raw materials of Fe, Cr, Ni, Mo, Mn and part of C are mixed by a vacuum induction furnace and then placed in a crucible for vacuumizing and power-feeding smelting. The carbon deoxidation efficiency and the nitrogen efficiency are enhanced by depending on a higher vacuum environment and a low melting rate during the smelting, and the residual C, Al is added after the molten steel is completely melted and refined.
The refining is to keep the temperature of the molten steel at 1500 ℃ for not less than 10 minutes so as to effectively reduce the content of impurities such as oxygen, sulfur, nitrogen and the like in the molten steel.
After refining, 0.04-0.08MPa of argon is introduced into the induction furnace, and Si and Mn are added to further reduce the content of oxygen and sulfur.
Then keeping the temperature for 10-30 minutes, adding Gd to fully melt, and casting into steel ingots by temperature regulation.
And forging and forming the smelted steel ingot, putting the steel ingot into a heating furnace in the forging process, heating to 950-fold sand 1100 ℃ at the heating speed of 100-150 ℃/h, preserving heat for 2-4 hours, then discharging from the furnace and starting forging, wherein the open forging temperature is not lower than 950 ℃ and not higher than 1060 ℃, the finish forging temperature is 850-fold sand 950 ℃, cooling in air after forging, and polishing to remove the oxide skin of the stainless steel forging blank.
Compared with the prior art, the invention has the following beneficial effects:
1. the Gd-containing duplex stainless steel has excellent neutron absorption performance and gamma ray shielding function, simultaneously has good mechanical property, can be prepared into spent fuel storage and transportation, post-treatment equipment, parts and the like, and has the function of functional structure integration.
2. The novel Gd-containing duplex stainless steel has high comprehensive performance and low cost. Compared with austenitic stainless steel, the mechanical property is high, and the corrosion resistance is good. Compared with nickel-based Gd-containing alloy, the alloy has lower cost and extremely high economical efficiency.
Drawings
FIG. 1 is a forged structure of a duplex stainless steel according to examples 1 to 3.
FIG. 2 is a graph of room temperature tensile properties of the duplex stainless steels of examples 1-3.
FIG. 3 is the room temperature elongation of the duplex stainless steels of examples 1-3.
FIG. 4 is a graph of the room temperature impact properties of the duplex stainless steels of examples 1-3.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
The chemical compositions of stainless steels in examples 1-3 and comparative examples 1-3 are shown in Table 1.
TABLE 1 Gd-containing duplex stainless steel alloy compositions of examples and comparative examples
The stainless steels of examples 1-3 and comparative examples 1-3 were prepared as follows:
pure metal raw materials of Fe, Cr, Ni, Mo, Mn and part of C are mixed by a vacuum induction furnace and then placed in a crucible for vacuumizing and power-feeding smelting. The carbon deoxidation efficiency and the nitrogen efficiency are enhanced by depending on a higher vacuum environment and a low melting rate during the smelting, and the residual C, Al is added after the molten steel is completely melted and refined. The refining temperature is 1500 ℃, and the heat preservation time is 30 minutes. And (3) introducing argon gas of 0.06MPa into the induction furnace after refining, and adding Si and Mn to further reduce the oxygen and sulfur contents. Then keeping the temperature for 15 minutes, adding Gd to fully melt, and casting into steel ingots by temperature regulation.
And forging and forming the smelted steel ingot, putting the steel ingot into a heating furnace in the forging process, heating to 1060 ℃ at a heating speed of 100 ℃/h, preserving heat for 2-4 hours, then starting forging, cooling in air to obtain a stainless steel forging blank, and polishing to remove oxide skin, wherein the open forging temperature is not lower than 950 ℃ and not higher than 1060 ℃, and the finish forging temperature is 900 ℃.
The forging of stainless steels in examples 1 to 3 and comparative examples 1 to 3 is shown in Table 2.
TABLE 2 forging conditions of Gd-containing duplex stainless steels of examples and comparative examples
FIG. 1 is a forged structure of the stainless steels prepared in examples 1 to 3, the stainless steels being composed of austenite and ferrite in a volume ratio of austenite phase to ferrite phase of about 1: 1.
then, a tensile sample of the standard M10 is prepared on a forged rod, and room temperature tensile property analysis is carried out, as shown in figure 2, the mechanical properties of the Gd-containing duplex stainless steel in examples 1-3 all meet the mechanical property requirement of 304B7 in the ASTM-887B-containing stainless steel standard, and the requirements of the functional structure integrated material are met.
FIG. 3 shows the elongation at room temperature of the duplex stainless steels of examples 1 to 3, and it can be seen that the elongation of examples 1, 2 and 3 is 30%, 40% and 18%, respectively.
FIG. 4 is a graph of the room temperature impact properties of the duplex stainless steels of examples 1-3, and the room temperature impact energy of example 2 is as high as 70J.
Claims (8)
1. Gd-containing duplex stainless steel with excellent neutron absorption performance is characterized in that: the stainless steel comprises the following chemical components in percentage by weight:
c: 0.02-0.06 wt.%; cr: 23.00-26.00 wt.%; ni: 4.00-8.00 wt.%; si ≤ 1.00 wt.%; rare earth Gd: 0.50-3.00 wt.%; mn: 1.00-2.00 wt.%; mo: 1.00-2.00 wt.%; al < 0.10 wt.%; the balance of Fe.
2. The Gd-containing duplex stainless steel having excellent neutron absorption according to claim 1, wherein: in the chemical components of the stainless steel, C: 0.02-0.04 wt.%, Cr: 23.00-25.00 wt.%, Ni: 5.00-8.00 wt.%, rare earth Gd: 0.50-2.50 wt.%.
3. Gd-containing duplex stainless steel with good neutron absorption properties according to claim 1 or 2, characterised in that: controlling the contents of impurity elements in the stainless steel as follows: o < 0.002 wt.%; n < 0.02 wt.%; s < 0.002 wt.%; p < 0.010 wt.%.
4. Gd-containing duplex stainless steel with good neutron absorption properties according to claim 1 or 2, characterised in that: the stainless steel consists of austenite and ferrite, and the volume ratio of the austenite phase to the ferrite phase is about 1: 1.
5. the method for preparing a Gd-containing duplex stainless steel having excellent neutron absorption according to claim 1, wherein: the method comprises the following steps:
(1) smelting a Gd-containing duplex stainless steel ingot by vacuum induction;
(2) carrying out homogenization treatment on the Gd-containing duplex stainless steel ingot;
(3) and forging the homogenized Gd-containing duplex stainless steel sample.
6. The method for manufacturing a Gd-containing duplex stainless steel having excellent neutron absorption according to claim 4, wherein: in the step (1), a vacuum induction smelting method is adopted to smelt steel ingots, and in the smelting process, O must be controlled to be less than 0.001 wt.% before Gd alloy is added.
7. The method for manufacturing a Gd-containing duplex stainless steel having excellent neutron absorption according to claim 4, wherein: in the step (2), the Gd-containing duplex stainless steel ingot is subjected to homogenization treatment, the homogenization treatment temperature is 950-.
8. The method for manufacturing a Gd-containing duplex stainless steel having excellent neutron absorption according to claim 4, wherein: in the step (3), the forging temperature is controlled at 900-.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0844312A1 (en) * | 1995-08-09 | 1998-05-27 | Sumitomo Metal Industries, Ltd. | Stainless steels excellent in thermal neutron absorption |
KR101637509B1 (en) * | 2014-12-31 | 2016-07-08 | 한국생산기술연구원 | Method of manufacturing ferrous alloy having gadolinium |
CN107974542A (en) * | 2017-10-24 | 2018-05-01 | 昆明理工大学 | A kind of grain refining preparation method of nickel-saving type two phase stainless steel |
KR20190027668A (en) * | 2017-09-07 | 2019-03-15 | 한국생산기술연구원 | Neutron absorber and a fabrication method thereof |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0844312A1 (en) * | 1995-08-09 | 1998-05-27 | Sumitomo Metal Industries, Ltd. | Stainless steels excellent in thermal neutron absorption |
KR101637509B1 (en) * | 2014-12-31 | 2016-07-08 | 한국생산기술연구원 | Method of manufacturing ferrous alloy having gadolinium |
KR20190027668A (en) * | 2017-09-07 | 2019-03-15 | 한국생산기술연구원 | Neutron absorber and a fabrication method thereof |
CN107974542A (en) * | 2017-10-24 | 2018-05-01 | 昆明理工大学 | A kind of grain refining preparation method of nickel-saving type two phase stainless steel |
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