CN113528952A - High-silicon high-chromium ferrite/martensite heat-resistant steel resistant to liquid lead or lead bismuth corrosion and preparation method thereof - Google Patents
High-silicon high-chromium ferrite/martensite heat-resistant steel resistant to liquid lead or lead bismuth corrosion and preparation method thereof Download PDFInfo
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- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C21D2211/008—Martensite
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Abstract
The invention discloses high-silicon high-chromium ferrite/martensite heat-resistant steel resistant to liquid lead or lead bismuth corrosion and a preparation method thereof, belonging to the technical field of production and manufacturing of heat-resistant metal materials for nuclei. The heat-resistant steel comprises the following chemical components: c is more than or equal to 0.14 percent and less than or equal to 0.22 percent, Si is more than or equal to 0.8 percent and less than or equal to 1.6 percent, Mn is more than or equal to 0.5 percent and less than or equal to 0.9 percent, Cr is more than or equal to 10.5 percent and less than or equal to 12.5 percent, Ni is more than or equal to 0.5 percent and less than or equal to 0.9 percent, Mo is more than or equal to 0.5 percent and less than or equal to 1.0 percent, W is more than or equal to 0.5 percent and less than or equal to 1.0 percent, Nb is more than or equal to 0.05 percent and less than or equal to 0.5 percent, V is more than or equal to 0.05 percent and less than or equal to 0.6 percent, Ce is less than or equal to 0.06 percent, B is less than or equal to 0.015 percent, N is less than or equal to 0.05 percent, and the balance is iron. The preparation process is smelting → homogenizing → hot working → cold working → heat treatment. According to the invention, Si is added, the corrosion resistance of the material to liquid lead (lead bismuth) is improved based on the internal oxidation principle, and the material has good mechanical properties at room temperature and high temperature.
Description
Technical Field
The invention belongs to the technical field of nuclear heat-resistant, irradiation-resistant and corrosion-resistant structural materials, and particularly relates to liquid lead or lead bismuth corrosion-resistant high-silicon high-chromium ferrite/martensite heat-resistant steel and a preparation method thereof.
Background
The lead (lead bismuth) fast reactor is a fast neutron reactor which adopts liquid lead or lead bismuth alloy as a coolant, and is one of six types of four-generation reactors which are mainly developed internationally. When liquid lead or lead-bismuth alloy is used as a coolant, the liquid lead or lead-bismuth alloy has poor compatibility with common structural materials, particularly austenitic stainless steel can generate severe Ni dissolution corrosion, and in addition, austenitic steel with an FCC structure can generate severe radiation swelling under fast reactor strong radiation. Therefore, ferrite/martensite heat-resistant steel with chromium content of 9-12 wt.% becomes an important candidate material for parts such as cladding tubes, outer sleeves, heat exchange tubes and the like. The improvement of the high-temperature strength and the lead-bismuth corrosion resistance of the material becomes an important research and development target of the structural material for the lead or lead-bismuth cooling reactor.
In order to improve the lead-bismuth corrosion resistance of ferrite/martensite, two main technical schemes are provided. One is an internal oxidation method and one is a surface coating method. The main principle of the endogenous oxidation method is that a certain amount of Si or Al is added into the alloy, and the oxygen content in liquid lead (lead bismuth) is controlled, so that a stable and uniform oxide protective film is generated on the surface of the alloy. The surface coating method is to directly coat a protective film on the surface of the alloy steel. Compared with the surface coating method, the alloy designed by the internal oxidation method can automatically repair the damaged part under the condition that the surface oxide film is damaged or falls off, has higher safety and reliability, and is a solution method which is easier to realize industrial production. The invention provides the high-silicon high-chromium ferrite/martensite heat-resistant steel for improving the corrosion resistance of the material to liquid lead (lead bismuth) based on the Si internal oxidation method.
Disclosure of Invention
Aiming at the using environment of the liquid lead-bismuth coolant of the fourth generation lead-cooled fast reactor, the invention provides the high-silicon high-chromium ferrite/martensite heat-resistant steel resisting the corrosion of liquid lead or lead-bismuth and the preparation method thereof, and the high-silicon high-chromium ferrite/martensite heat-resistant steel has good high-temperature mechanical property while the corrosion resistance of the material to the liquid lead or lead-bismuth is improved.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the liquid lead or lead bismuth corrosion resistant high-silicon high-chromium ferrite/martensite heat-resistant steel comprises the following chemical components in percentage by weight: 0.14-0.22% of C, 0.8-1.6% of Si, 0.5-0.9% of Mn, 10.5-12.5% of Cr, 0.5-0.9% of Ni, 0.5-1.0% of Mo, 0.5-1.0% of W, 0.05-0.5% of Nb, 0.05-0.6% of V, less than or equal to 0.06% of Ce, less than or equal to 0.015% of B, less than or equal to 0.05% of N, and the balance of iron and other inevitable residual elements.
In the chemical components of the heat-resistant steel, the residual elements are controlled as follows according to weight percentage: less than or equal to 0.015 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.006 percent of O and less than or equal to 0.0002 percent of H.
In the chemical components of the heat-resistant steel, the C + N content is 0.15-0.22 wt.%, the Mo + W content is 1.0-1.7 wt.%, the Nb + V content is 0.3-0.8 wt.%, and the Ni + Mn content is more than or equal to 1.1 wt.%.
The preparation method of the high-silicon high-chromium ferrite/martensite heat-resistant steel resisting liquid lead or lead bismuth corrosion comprises the following steps:
1) smelting and ingot casting: the smelting equipment is a vacuum induction furnace, or the smelting equipment is a vacuum induction furnace and an electroslag remelting furnace, or the smelting equipment is a vacuum induction furnace and a vacuum consumable electrode furnace.
2) Homogenizing: homogenizing the cast ingot, wherein the homogenizing heat preservation interval is 1000-1200 ℃, and the heat preservation time is 3-25 h; the homogenization treatment aims to homogenize the components in the steel and adjust the content of delta-ferrite.
3) Hot processing; carrying out hot processing on the sample subjected to homogenization treatment in the step (2), wherein the hot processing can adopt a forging process alone or a combined process of forging and rolling; wherein: the heat preservation temperature is 1000-1180 ℃ in the forging or rolling process, and the heat preservation time is more than or equal to 40 min; the forging ratio in the forging process is more than or equal to 3, and the rolling ratio in the rolling process is more than or equal to 2.
4) Cold processing: the pipe or sheet product is prepared by adopting a cold rolling process, wherein in the cold rolling process, the single-pass cold deformation is less than or equal to 40 percent, and the intermediate annealing heat preservation temperature is 680-780 ℃.
5) Carrying out heat treatment on the sample processed in the step 3) or the step 4): the heat treatment system is as follows: (a) normalizing: the heat preservation temperature is 940-1100 ℃, and the heat preservation time is 10 min-2 h; (b) tempering: the heat preservation temperature is 670-790 ℃, and the heat preservation time is 25 min-4 h.
The microstructure of the ferrite/martensite heat-resistant steel after heat treatment is mainly martensite, and the content of delta ferrite is less than or equal to 16 percent.
The performance of the ferrite/martensite heat-resistant steel after heat treatment is as follows: the yield strength of the material at room temperature is more than 580MPa, the tensile strength is more than 700MPa, and the elongation is more than 16 percent; the yield strength at the high temperature of 650 ℃ is more than 140MPa, the tensile strength is more than 220MPa, and the elongation is more than 17%.
The design idea of the invention is as follows:
according to the invention, a certain content of Si element is added into ferrite/martensite heat-resistant steel with the Cr content of more than 10%, and a compact oxide film is formed based on an internal oxidation method, so that the liquid lead (lead bismuth) resistance of the material is improved. Meanwhile, in order to balance the delta-ferrite structure, the invention puts forward control requirements on the sum of partial elements (C + N, Mo + W, Nb + V, Ni + Mn), designs corresponding hot working and heat treatment methods, and finally obtains the structure with the delta-ferrite content less than 16%. In addition, in order to ensure the high-temperature mechanical property of the material, the content of elements formed by precipitation strengthening phases such as C, Mo, W, Nb, V, B, N and the like is optimally designed.
The invention has the advantages and beneficial effects that:
1. according to the invention, Si in a specific range is added into high Cr ferrite/martensite heat-resistant steel, so that the corrosion resistance of the material to liquid lead (lead bismuth) is improved, and the corrosion rate of the material in liquid lead bismuth at 550 ℃ is lower than that of HT-9 steel.
2. The invention can obtain microstructures with different delta-ferrite contents by regulating and controlling the content of partial elements and the hot working process, and can obtain the performances of yield strength of more than 580MPa at room temperature, tensile strength of more than 700MPa, elongation of more than 16%, yield strength of more than 140MPa at high temperature of 650 ℃, tensile strength of more than 220MPa and elongation of more than 17% when the content of the delta-ferrite is less than 16%.
3. The preparation method of the alloy is simple, easy to operate and convenient for industrial production.
Drawings
FIG. 1 is a metallographic photograph of the rolled high-silicon high-chromium ferritic/martensitic heat-resistant steel showing resistance to corrosion by liquid lead (lead bismuth) in example 1.
FIG. 2 is a photograph of the cross-sectional shape of the corrosion layer of the high silicon high chromium ferritic/martensitic heat resistant steel resistant to liquid lead (lead bismuth) corrosion of example 1 after corrosion for 500 hours in liquid lead bismuth at a saturated oxygen concentration of 550 ℃.
FIG. 3 is a photograph of the cross-sectional morphology of the corrosion layer of the HT-9 steel of comparative example 1 after corrosion in liquid lead bismuth with a saturated oxygen concentration at 550 ℃ for 500 h.
Detailed Description
The following examples further illustrate a high silicon high chromium ferritic/martensitic heat resistant steel resistant to liquid lead (lead bismuth) corrosion and a method of making the same, but are not intended to limit the invention thereto.
Example 1:
a50 kg vacuum induction furnace is adopted for smelting, and the chemical components (wt.%):
c: 0.17%, Si: 1.2%, Mn: 0.7%, Cr: 11.0%, Ni: 0.7%, Mo: 0.8%, W: 0.7%, Nb: 0.3%, V: 0.3 percent, Ce is less than or equal to 0.05 percent, B: 0.005%, N: 0.02%, O: 0.003%; the balance being iron.
Example 2:
a25 kg vacuum induction furnace is adopted for smelting, and the chemical components (wt.%):
c: 0.18%, Si: 1.2%, Mn: 0.7%, Cr: 10.8%, Ni: 0.8%, Mo: 0.8%, W: 0.6%, Nb: 0.3%, V: 0.3 percent, Ce is less than or equal to 0.05 percent, B: 0.003%, N: 0.04%, O: 0.003%; the balance being iron.
Comparative example 1:
a50 kg vacuum induction furnace is adopted for smelting, and the chemical components (wt.%):
c: 0.21%, Si: 0.42%, Mn: 0.61%, Cr: 12.0%, Ni: 0.6%, Mo: 1.0%, W: 0.54%, V: 0.29%, B: 0.0037%, N: 0.03%, O: 0.0007 percent; the balance being iron.
The preparation processes adopted in the examples and comparative examples are as follows:
1) smelting and ingot casting: the smelting equipment is a vacuum induction furnace.
2) The homogenization process comprises the following steps: keeping the temperature at 1100 ℃ for 10 h;
3) the forging process comprises the following steps: keeping the temperature at 1100 ℃ for 1h, forging the steel plate into a plate blank with the thickness of 35mm, wherein the forging ratio is more than 3;
4: the rolling process comprises the following steps: keeping the temperature at 1100 ℃ for 40min, and rolling the plate into a plate with the thickness of 13mm by a two-roller mill;
the heat treatment processes used in examples 1 and 2 are as follows: normalizing at 1050 deg.C for 45 min; the tempering heat preservation temperature is 720 ℃, and the heat preservation time is 2.5 h.
The heat treatment process used in comparative example 1 was as follows: normalizing at 1050 deg.C for 45 min; the tempering heat preservation temperature is 760 ℃, and the heat preservation time is 1.5 h.
FIG. 1 is a metallographic structure of a rolled steel sheet after tempering in example 1, and it can be seen from the metallographic structure that the structure is mainly martensite and further contains about 12% of delta-ferrite.
After the immersion etching of the lead bismuth in the saturated oxygen static state at 550 ℃ for 500h, the etching interface is shown in FIG. 2, and the thickness of the etching layer is about 20 μm. In contrast, in the comparative example HT-9, after the immersion corrosion of the saturated oxygen static lead bismuth at 550 ℃ for 500h, the corrosion interface is as shown in FIG. 3, and the thickness of the corrosion layer is about 29 μm. The comparison of the two shows that the lead-bismuth corrosion resistance of the alloy is superior to that of HT-9 steel.
The tensile properties were measured and the properties are shown in Table 1. The yield at room temperature of the examples is more than 730MPa, the tensile strength is more than 900MPa, and the elongation is more than 18 percent, while the yield at 650 ℃ is more than 200MPa, the tensile strength is more than 299MPa, and the elongation is more than 37 percent. Has good toughness.
Table 1: examples tensile Properties
Claims (7)
1. A high-silicon high-chromium ferrite/martensite heat-resistant steel resisting liquid lead or lead bismuth corrosion is characterized in that: the heat-resistant steel comprises the following chemical components in percentage by weight: 0.14-0.22% of C, 0.8-1.6% of Si, 0.5-0.9% of Mn, 10.5-12.5% of Cr, 0.5-0.9% of Ni, 0.5-1.0% of Mo, 0.5-1.0% of W, 0.05-0.5% of Nb, 0.05-0.6% of V, less than or equal to 0.06% of Ce, less than or equal to 0.015% of B, less than or equal to 0.05% of N, and the balance of iron and other inevitable residual elements.
2. The high silicon high chromium ferritic/martensitic heat resistant steel resistant to liquid lead or lead bismuth corrosion of claim 1 wherein: in the chemical components of the heat-resistant steel, the residual elements are controlled as follows according to weight percentage: less than or equal to 0.015 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.006 percent of O and less than or equal to 0.0002 percent of H.
3. The high silicon high chromium ferritic/martensitic heat resistant steel resistant to liquid lead or lead bismuth corrosion of claim 1 wherein: in the chemical components of the heat-resistant steel, the C + N content is 0.15-0.22 wt.%, the Mo + W content is 1.0-1.7 wt.%, the Nb + V content is 0.3-0.8 wt.%, and the Ni + Mn content is more than or equal to 1.1 wt.%.
4. The method for preparing high-silicon high-chromium ferritic/martensitic heat-resistant steel resistant to liquid lead or lead bismuth corrosion according to claim 1, characterized in that: the microstructure of the ferrite/martensite heat-resistant steel (after heat treatment) is mainly martensite, and the content of delta ferrite is less than or equal to 16 percent.
5. The method for preparing high-silicon high-chromium ferritic/martensitic heat-resistant steel resistant to liquid lead or lead bismuth corrosion according to claim 1, characterized in that: properties of the ferrite/martensite heat-resistant steel (after heat treatment): the yield strength of the material at room temperature is more than 580MPa, the tensile strength is more than 700MPa, and the elongation is more than 16 percent; the yield strength at the high temperature of 650 ℃ is more than 140MPa, the tensile strength is more than 220MPa, and the elongation is more than 17%.
6. A method of producing a high silicon high chromium ferritic/martensitic heat resistant steel resistant to corrosion by liquid lead or lead bismuth according to any one of claims 1 to 3 characterised in that: the method comprises the following steps:
1) smelting and ingot casting: the smelting equipment is a vacuum induction furnace, or the smelting equipment is a vacuum induction furnace and an electroslag remelting furnace, or the smelting equipment is a vacuum induction furnace and a vacuum consumable electrode furnace.
2) Homogenizing: homogenizing the cast ingot, wherein the homogenizing heat preservation interval is 1000-1200 ℃, and the heat preservation time is 3-25 h;
3) hot processing: carrying out hot processing on the sample subjected to homogenization treatment in the step (2), wherein the hot processing adopts forging treatment, or the hot processing adopts a combined process of forging and rolling; wherein: the heat preservation temperature is 1000-1180 ℃ in the forging or rolling process, and the heat preservation time is more than or equal to 40 min; the forging ratio in the forging process is more than or equal to 3, and the rolling ratio in the rolling process is more than or equal to 2.
4) Cold processing: the pipe or sheet product is prepared by adopting a cold rolling process, wherein in the cold rolling process, the single-pass cold deformation is less than or equal to 40 percent, and the intermediate annealing heat preservation temperature is 680-780 ℃.
5) And (3) carrying out heat treatment on the sample processed in the step (3) or the step (4).
7. The method for preparing high-silicon high-chromium ferritic/martensitic heat-resistant steel resistant to liquid lead or lead bismuth corrosion according to claim 6, characterized in that: in the step (5), the heat treatment system comprises the following steps:
(a) normalizing: the heat preservation temperature is 940-1100 ℃, and the heat preservation time is 10 min-2 h;
(b) tempering: the heat preservation temperature is 670-790 ℃, and the heat preservation time is 25 min-4 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115354227A (en) * | 2022-08-22 | 2022-11-18 | 中国核动力研究设计院 | Ferrite martensitic steel for reactor fuel cladding material and heat treatment process thereof |
| CN115478220A (en) * | 2022-09-19 | 2022-12-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof |
| CN115491600A (en) * | 2022-09-19 | 2022-12-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof |
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| CN115354227A (en) * | 2022-08-22 | 2022-11-18 | 中国核动力研究设计院 | Ferrite martensitic steel for reactor fuel cladding material and heat treatment process thereof |
| CN115478220A (en) * | 2022-09-19 | 2022-12-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof |
| CN115491600A (en) * | 2022-09-19 | 2022-12-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Ferrite/martensite heat-resistant steel for lead-bismuth pile and preparation method thereof |
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