CN112646957A - Pretreatment method for improving lead and bismuth corrosion resistance of ferrite-martensite steel - Google Patents
Pretreatment method for improving lead and bismuth corrosion resistance of ferrite-martensite steel Download PDFInfo
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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Abstract
The invention discloses a pretreatment method for improving lead and bismuth corrosion resistance of ferrite-martensite steel, and belongs to the technical field of corrosion protection of nuclear materials. First, a ferrite-martensite steel is subjected to quenching and tempering heat treatment of quenching and tempering, followed by surface treatment to expose a metallic luster on the surface thereof, and the surface roughness is required to be less than 1 μm. Then, cold deformation treatment is carried out at room temperature, and the accumulated deformation amount is 10-40%. And finally, carrying out high-temperature oxidation treatment, wherein the oxidation temperature is 500-650 ℃, and the oxidation time is 5-50 h. The pretreatment method combining cold deformation and high-temperature oxidation can promote the generation of a compact oxide film on the surface of ferrite-martensite steel to improve the lead-bismuth corrosion resistance, and simultaneously, the deformation and the high-temperature oxidation system are reasonably controlled without damaging the mechanical property of the matrix. The method has the advantages of convenient operation, lower cost, no limitation of the size and the shape of the workpiece and convenient industrial popularization.
Description
Technical Field
The invention relates to the technical field of corrosion protection of nuclear materials, in particular to a pretreatment method for improving lead-bismuth corrosion resistance of ferrite-martensite steel.
Background
The lead-bismuth eutectic alloy has the advantages of weak neutron absorption and moderation capacity, low melting point, high boiling point, good chemical stability and the like, and is used as a coolant for a four-generation lead-bismuth cooling fast reactor, a coolant for an accelerator-driven subcritical system (ADS) and a spallation target candidate material. However, the high-temperature and flowing liquid lead-bismuth alloy can generate extremely strong corrosion action on the structural material, and cause damage to the safe operation of the reactor. How to improve the compatibility of the structural material and the liquid lead bismuth alloy becomes a problem to be solved urgently.
The 9-12% Cr ferrite-martensite steel has good thermal physical properties, excellent radiation swelling resistance and lower dissolution corrosion tendency in the liquid lead bismuth eutectic, and is taken as a preferred structural material of reactor core components in the fourth generation lead bismuth cooling fast reactor and ADS. The oxide layer generated on the surface has insufficient compactness, elements in a matrix easily penetrate through the oxide layer to cause accelerated oxidation corrosion, and the oxide layer with poor compactness is easy to damage and peel off, so that the oxidation corrosion behavior is accelerated. The faster oxidation corrosion rate directly affects the service life and safety of the ferrite-martensite steel in liquid lead bismuth. In order to solve the problems, researchers propose that the addition of Si can promote the formation of Si-rich oxide in an oxide layer and improve the corrosion resistance of liquid lead bismuth, but the excessive Si content can promote the formation of delta-ferrite and Laves phases and reduce the mechanical property. Although the effect of the addition of Al on the improvement of the oxide layer compactness is more remarkable, Al has a strong ferrite formation promoting effect, thereby limiting the amount of Al added. In addition, researchers also propose a method for refining grains to improve the corrosion resistance of the liquid lead bismuth, but after the liquid lead bismuth is in service at high temperature for a long time, the stability of a fine crystalline structure is gradually reduced, so that the mechanical property and the corrosion resistance of the lead bismuth are reduced. Therefore, how to improve the lead-bismuth corrosion resistance is an urgent problem to be solved on the premise of not damaging the mechanical properties of the ferrite-martensite steel.
Disclosure of Invention
Aiming at the technical problem of liquid lead bismuth corrosion resistance of ferrite-martensite steel, the invention aims to provide a pretreatment method for improving the liquid lead bismuth corrosion resistance of ferrite-martensite steel, wherein the pretreatment method combining cold deformation and high-temperature oxidation is adopted to promote the generation of a compact oxide film on the surface of the ferrite-martensite steel so as to resist the liquid lead bismuth corrosion, and meanwhile, the deformation and the high-temperature oxidation system are reasonably controlled without damaging the mechanical property of the steel.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a pretreatment method for improving lead-bismuth corrosion resistance of ferrite-martensite steel specifically comprises the following steps:
1) and (3) heat treatment: quenching and tempering heat treatment of quenching and tempering is carried out on the ferrite-martensite steel, wherein: and the quenching treatment is heat preservation at 950-1050 ℃ for 30-90 min, then water cooling, and the tempering treatment is heat preservation at 700-800 ℃ for 1-3 h, and then air cooling.
2) Surface treatment: and cleaning the surface of the material to completely remove surface oxide skin so as to expose the surface of the material with metallic luster, wherein the surface roughness is required to be less than 1 mu m.
3) Cold deformation: and performing cold deformation treatment at room temperature, wherein the accumulated deformation is 10-40%.
4) High-temperature oxidation: and carrying out oxidation treatment on the cold-deformed material, wherein the oxidation temperature is 500-650 ℃, and the oxidation time is 5-50 h.
Further, the ferrite-martensite steel is 9-12% Cr ferrite-martensite steel.
Further, the material product is one of a plate, a bar and a pipe.
Further, the surface treatment method in the step 2) is one of mechanical polishing and chemical polishing.
Further, the cold deformation in the step 3) is one of cold rolling, cold forging and cold extrusion.
Further, the optimal cold deformation amount in the step 3) is 10-30%.
Further, the atmosphere of the high-temperature oxidation treatment in the step 4) is air or an oxygen-controlled environment.
The design idea of the invention is as follows:
the cold deformation pretreatment is carried out on the ferrite-martensite steel, so that the vacancy concentration and the dislocation density in the material can be increased, the diffusion rate of alloy elements is remarkably improved, a uniform and compact oxide film is formed in the high-temperature oxidation treatment process, and the oxide film can effectively resist the corrosion of liquid lead and bismuth. Meanwhile, the microstructure such as martensite lath, grain size, carbide morphology and size and the like is not obviously changed by proper cold deformation, and the microstructure of the matrix is not degraded by a high-temperature oxidation system, so that the mechanical property is not damaged.
The invention has the following beneficial effects:
1. according to the invention, the compact oxide film with the thickness of 0.1-20 μm is formed on the surface of the ferrite-martensite steel, so that the lead bismuth corrosion resistance is obviously improved, and the corrosion speed of the ferrite-martensite steel pretreated by the method in liquid lead bismuth is obviously lower than that of an untreated sample.
2. The invention can improve the lead-bismuth corrosion resistance of the ferrite-martensite steel without damaging the mechanical property of the matrix.
3. The invention has convenient operation, is not limited by the size and the shape of the workpiece, and is convenient for industrialized popularization.
4. Compared with surface coating, aluminizing and other technological methods, the method has simpler process and lower cost.
Drawings
FIG. 1 is an SEM structure of 9Cr2WVTa ferrite-martensite steel before and after cold deformation pretreatment; wherein: (a) the structure is in a quenching and tempering heat treatment state; (b) 20% cold deformed pretreated tissue.
FIG. 2 shows the appearance of the surface oxide film of 20% cold-deformed 9Cr2WVTa ferrite-martensite steel after air oxidation at 600 ℃ for 20 h.
FIG. 3 shows the element content of the oxide film of 20% cold-deformed 9Cr2WVTa ferritic-martensitic steel after air oxidation at 600 ℃ for 20 hours.
FIG. 4 shows the cross-sectional morphology of a corrosion layer after 9Cr2WVTa ferrite-martensite steel is subjected to 20% cold deformation treatment and 600 ℃ air oxidation treatment for 20h and then placed in 550 ℃ saturated oxygen liquid lead bismuth for 500h
FIG. 5 is a cross-sectional view of a corrosion layer of 9Cr2WVTa ferrite-martensite steel without cold deformation and high-temperature oxidation treatment after being placed in a saturated oxygen liquid lead bismuth at 550 ℃ for 500 hours
FIG. 6 is a cross-sectional view of a corrosion layer of a 9Cr2WVTa ferrite-martensite steel subjected to pre-oxidation treatment at 600 ℃ for 20h after being placed in a saturated oxygen liquid lead bismuth at 550 ℃ for 500h
Detailed Description
In the following embodiments, 9Cr2WVTa ferritic-martensitic steel of 9% Cr is mainly used, but the present invention is also applicable to other 9 to 12% Cr ferritic-martensitic steels. Examples the present invention will be described more fully hereinafter so that those skilled in the art may better understand the invention and practice it.
Example 1
This example provides a 9Cr2WVTa ferritic-martensitic steel sheet with a chemical composition (wt.%): 0.11 percent of C, 8.86 percent of Cr, 1.62 percent of W, 0.24 percent of V, 0.11 percent of Ta, 0.45 percent of Mn, 0.05 percent of Si, 0.005 percent of S, 0.005 percent of P and the balance of Fe. The pretreatment process of the plate comprises the following steps:
1) and (3) heat treatment: quenching and tempering heat treatment of quenching and tempering is carried out on the ferrite-martensite steel plate, the quenching treatment is carried out after heat preservation for 60min at 1020 ℃, water cooling is carried out, the tempering treatment is carried out after heat preservation for 2h at 750 ℃, and air cooling is carried out.
2) Surface treatment: and (3) carrying out mechanical polishing treatment on the surface of the plate, completely removing surface oxide skin, and exposing the surface of the plate with metallic luster, wherein the surface roughness is required to be less than 1 mu m.
3) Cold deformation: cold rolling deformation treatment is carried out at room temperature, and the cold rolling deformation is 20%.
4) High-temperature oxidation: and (3) carrying out high-temperature oxidation treatment on the cold-rolled sheet in a box-type resistance furnace, wherein the oxidation temperature is 600 ℃, and the oxidation time is 20 hours.
FIG. 1(a) is a microstructure diagram after the quenching and tempering heat treatment, in which tempered martensite structures are formed and carbides are distributed at lath interfaces. The microstructure after 20% cold rolling deformation is shown in fig. 1(b), and it can be seen that the morphology and size of martensite laths and carbides are not changed by 20% cold rolling deformation. The surface appearance of the oxide film of the cold-rolled sheet after being pre-oxidized for 20 hours at 600 ℃ is shown in figure 2, a continuous oxide film is formed on the surface, and the oxide particles are fine. FIG. 3 shows the element distribution in the oxide film, and the thickness of the oxide film formed is about 200nm, and the contents of Fe, Cr, and Mn in the oxide film are 20%, 15%, and 11%, respectively. The sample pretreated by the method of the invention is placed in the saturated oxygen liquid lead bismuth at 550 ℃ for 500h, the cross section appearance of the corrosion layer is shown in figure 4, and the oxide film obtained after pretreatment effectively prevents the corrosion of the liquid lead bismuth, and the corrosion layer is not generated on the surface. After 500h of corrosion at 550 ℃, the hardness value of the matrix is 230HV, which is equivalent to the hardness value (228HV) of the initial quenched and tempered state. Therefore, after the ferrite-martensite steel is pretreated by the method, the lead and bismuth corrosion resistance is obviously improved, and the mechanical property of the matrix is not damaged.
Example 2
The same ferritic-martensitic steel sheet as in example 1 was used, and subjected to the same thermal refining treatment without pretreatment of cold deformation and high-temperature oxidation. The sample was placed in the same liquid lead-bismuth environment as in example 1, and the cross-sectional morphology of the corrosion layer is shown in fig. 5. It can be seen that the ferritic-martensitic steel surface formed a corrosion layer with a thickness of about 23 μm. It follows that ferritic-martensitic steels which have not been pretreated by the method according to the invention undergo significant oxidative corrosion.
Example 3
The same ferrite-martensite steel sheet as in example 1 was subjected to the same thermal refining treatment and high-temperature oxidation treatment, but no cold deformation pretreatment was performed before the oxidation treatment. The sample was placed in the same liquid lead-bismuth environment as in example 1, and the cross-sectional morphology of the corrosion layer is shown in fig. 6. It can be seen that the ferritic-martensitic steel surface formed a corrosion layer of about 9 μm thickness. It is seen that the ferritic-martensitic steel without being subjected to the cold deformation pretreatment cannot effectively resist corrosion by the liquid lead bismuth even if subjected to the high-temperature oxidation treatment.
Example 4
The same ferrite-martensite steel sheet as in example 1 was subjected to the same quenching and tempering heat treatment and high-temperature oxidation treatment, and the sheet was subjected to a cold deformation pretreatment of 60% before the oxidation treatment. The sample is placed in the same liquid lead bismuth environment as in example 1, the oxide film obtained by pretreatment effectively prevents the liquid lead bismuth from being corroded, and no corrosion layer is generated on the surface. After the corrosion is finished, the hardness value of the matrix is reduced to 180HV and is lower than the hardness value (228HV) of the initial quenched and tempered state. Therefore, if excessive cold deformation pretreatment is adopted, the mechanical property of the matrix is obviously deteriorated after long-term service at high temperature.
Example 5
The same ferrite-martensite steel sheet as in example 1 was subjected to the same thermal refining treatment and cold deformation treatment, and then the cold rolled steel sheet was subjected to 400 ℃ oxidation treatment for 20 hours. When the sample is placed in the same liquid lead-bismuth environment as in example 1, a continuous compact oxide film cannot be formed due to too low oxidation temperature, and obvious oxidation corrosion occurs to the ferrite-martensite steel.
Example 6
The same ferrite-martensite steel sheet as in example 1 was subjected to the same thermal refining treatment and cold deformation treatment, and the cold-rolled steel sheet was subjected to 700 ℃ oxidation treatment for 20 hours. When the sample is placed in the same liquid lead-bismuth environment as in example 1, the ferrite-martensite steel undergoes obvious oxidative corrosion due to loose oxide film formed on the surface due to the excessively high oxidation temperature.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. Besides the above embodiments, there may be variations of materials, cold deformation, high temperature oxidizing atmosphere, etc., and these equivalents should also be within the scope of protection.
Claims (8)
1. A pretreatment method for improving lead-bismuth corrosion resistance of ferrite-martensite steel is characterized by comprising the following steps: the method comprises the following steps of carrying out cold deformation and high-temperature oxidation pretreatment on ferrite-martensite steel to form a compact oxide film on the surface of the material, so as to improve the liquid lead bismuth corrosion resistance:
1) and (3) heat treatment: quenching and tempering heat treatment of quenching and tempering is carried out on the ferrite-martensite steel, and the process comprises the following steps: quenching treatment is carried out, specifically, heat preservation is carried out at 950-1050 ℃ for 30-90 min, and then water cooling is carried out; then carrying out tempering treatment, specifically, keeping the temperature of 700-800 ℃ for 1-3 h and then air cooling;
2) surface treatment: cleaning the surface of the material, completely removing surface oxide skin to expose metallic luster on the surface of the material, and requiring the surface roughness to be less than 1 mu m;
3) cold deformation: performing cold deformation treatment at room temperature, wherein the accumulated deformation is 10-40%;
4) high-temperature oxidation: and carrying out oxidation treatment on the cold-deformed material, wherein the oxidation temperature is 500-650 ℃, and the oxidation time is 5-50 h.
2. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the ferrite-martensite steel is 9-12% Cr ferrite-martensite steel.
3. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the material product is one of a plate, a bar or a pipe.
4. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the surface treatment method in the step 2) is one of mechanical polishing and chemical polishing.
5. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the cold deformation in the step 3) is one of cold rolling, cold forging and cold extrusion.
6. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the optimal cold deformation in the step 3) is 10-30%.
7. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: the high-temperature oxidation treatment atmosphere in the step 4) is air or oxygen-controlled environment.
8. The pretreatment method for improving the lead bismuth corrosion resistance of ferritic-martensitic steel as claimed in claim 1, wherein: after pretreatment, a compact oxide film with the thickness of 0.1-20 mu m is formed on the surface of the ferrite-martensite steel.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444999A (en) * | 2021-06-25 | 2021-09-28 | 中国科学院金属研究所 | Method for promoting generation of lead-bismuth corrosion resistant FeAl infiltration layer on surface of ferrite-martensite steel |
| CN113718193A (en) * | 2021-07-30 | 2021-11-30 | 西安交通大学 | Protective film for corrosion resistance of metal niobium at high temperature and preparation method thereof |
| CN114561614A (en) * | 2022-03-04 | 2022-05-31 | 西安交通大学 | Treatment method for improving corrosion resistance of steel material in lead or lead bismuth |
| CN115612926A (en) * | 2022-09-19 | 2023-01-17 | 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 |
| CN115838913A (en) * | 2022-12-06 | 2023-03-24 | 西安交通大学 | Method for improving high-temperature lead/lead bismuth corrosion resistance of material by coupling temperature control and irradiation effect |
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| CN113444999A (en) * | 2021-06-25 | 2021-09-28 | 中国科学院金属研究所 | Method for promoting generation of lead-bismuth corrosion resistant FeAl infiltration layer on surface of ferrite-martensite steel |
| CN113444999B (en) * | 2021-06-25 | 2022-05-06 | 中国科学院金属研究所 | Method for promoting generation of lead-bismuth corrosion resistant FeAl infiltration layer on surface of ferrite-martensite steel |
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| CN115612926B (en) * | 2022-09-19 | 2023-08-22 | 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 |
| CN115838913A (en) * | 2022-12-06 | 2023-03-24 | 西安交通大学 | Method for improving high-temperature lead/lead bismuth corrosion resistance of material by coupling temperature control and irradiation effect |
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