CN103898411A - Liquid metal corrosion resistance martensite structural material for high temperature and preparation method of material - Google Patents
Liquid metal corrosion resistance martensite structural material for high temperature and preparation method of material Download PDFInfo
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Abstract
The invention discloses a liquid metal corrosion resistance martensite structural material for high temperature and a preparation method of the material, and belongs to the field of martensite structural materials for high temperature. The material comprises the following components in percentage by weight: 0.10-0.35 percent of C, 10.0-12.0 percent of Cr, 1.0-2.0 percent of W, less than or equal to 1.0 percent of Mn, 1.0-2.0 percent of Si, less than or equal to 0.45 percent of Ta and Nb, less than or equal to 0.3 percent of V and the balance of iron. According to the material, a chromium and silicon enriched dense oxide layer tightly bound with a matrix is formed on the surface of the matrix by adding silicon and chromium with high content, so that the oxidation resistance and the corrosion resistance of the matrix alloy to liquid metal can be improved, the content of theta ferrite is lower than 5% by controlling the contents of carbon, manganese and other elements, and a martensite structural material, which has excellent creeping performance, oxidation resistance and liquid metal corrosion resistance at high temperature, can be obtained. The martensite structural material is mainly applied to novel structural materials in the field of nuclear energy.
Description
Technical field
The invention belongs to high temperature martensitic structure Material Field, be specifically related to martensitic structure material having under a kind of high temperature good creep property, antioxidant property, resistance to liquid metal corrosion performance and preparation method thereof, be particularly related to a kind of high temperature martensitic structure of resistance to liquid metal corrosion material and preparation method, this structured material is mainly the new structural material that is applied to nuclear energy field.
Background technology
Along with the development of the essential industry such as nuclear power technology, atomic energy technology, liquid metal is used as nuclear reactor coolant because of its good heat conductivility, as fast neutron reactor, following nucleosynthesis first wall covering and Accelerator driven transmuting system etc.Liquid lead bismuth eutectic alloy is because it has low melting point (125 ℃), high boiling point (1670 ℃), good neutronics characteristic and good radioresistance injury reinforcing ability and heat conductivility, be not only the first-selected refrigerant of advanced nuclear reaction system design in the world, and be proposed the target as spallation neutron source.But the use of liquid lead bismuth will produce serious corrosion to the structured material of contact with it.Therefore need to have good over-all properties be good high-temperature behavior and good anti-oxidant, resistance to liquid metal corrosion performance to its structured material.
At present, in the cooling nuclear reaction system of liquid lead bismuth, have several candidate's advanced configuration material, as T91, HT9,316L and EP823 etc., wherein that the most outstanding is T91 and the Muscovite EP823 of the U.S..T91 is the high-temperature component high temperature steel for more the design of elevated steam conditions generating set is researched and developed, its heat resistance is good, creep tensile strength excellent performance, but because chromium content is 9%, corrosion experiments a large amount of in liquid metal show, T91 produces serious oxidation corrosion, can not meet the requirement of the anti-liquid metal corrosion performance under high temperature.EP823 is the structured material that Russia's exploitation is exclusively used in heavy metal reactor, its anti-liquid metal corrosion excellent performance, but its chromium equivalent is higher, for the delta ferrite duplex structure of martensite and 10%, its poor impact toughness, creep durability can be low, can not meet the requirement of creep-resistant property under hot conditions.Therefore the problem of materials of the following nuclear power system key position such as nucleosynthesis, advanced nuclear fission heap becomes an international difficult problem, and international nuclear power all has the structured material of good high temperature creep property, anti-irradiation and anti-liquid metal corrosion performance simultaneously in exploratory development.
Summary of the invention
The high temperature resistant martensitic structure of the resistance to liquid metal corrosion material that the object of the present invention is to provide a kind of high comprehensive performance, this material also has excellent high creep property simultaneously.
Design philosophy of the present invention is: abroad on the basis of martensitic structure material, by new Composition Design and a large amount of experiments, a kind of martensitic structure material with good resistance to liquid metal corrosion performance has been proposed, by design and optimization composition, adjust C and Mn content, make delta ferrite level in steel lower than 5%, obtain high tempering martensitic stucture, guarantee excellent toughness and the high temperature creep property of steel.
By adding chromium and the silicon of high level, generate fine and close rich chromium and the zone of oxidation of silicon, guarantee antioxidant property and the resistance to liquid metal corrosion performance of steel.
This structure iron microtexture is martensitic stucture, and martensitic stucture has good intensity mates with toughness plasticity, and at high temperature possesses and have good creep property.
Above Composition Design is the basis that material possesses good over-all properties, i.e. good high-temperature behavior, as high conventional mechanical property and creep property, good anti-oxidant and resistance to liquid metal corrosion performance.
Technical scheme of the present invention is:
A kind of martensitic structure of resistance to liquid metal corrosion material for high temperature, its Chemical Composition (weight percent) is: C:0.10 ~ 0.35%, Cr:10.0 ~ 12.0%, W:1.0 ~ 2.0%, Mn :≤1.0%, Si:1.0 ~ 2.0% is 0 when the content of Ta+Nb≤0.45%(Ta and Nb is different), V :≤0.3%, surplus is iron.
In described martensitic structure material: P < 0.007wt.%, S < 0.006wt.%, Cu < 0.01wt.%, Ti<0.010wt.%, Al<0.010wt.%, Co<0.005wt.%.
In described martensitic structure material structure, delta ferrite level is lower than 5%, and it generates the compact oxidation layer of rich chromium and silicon under the liquid metal corrosion environment of saturated oxygen concentration.
The preparation method of above-mentioned martensitic structure material, comprises the steps:
(1) in described ratio, each chemical composition is mixed, through smelting and cast acquisition high temperature steel steel ingot;
(2) steel ingot obtaining is forged in austenite one phase district: 1100 ~ 1200 ℃ of forging temperatures, forging ratio is 6 ~ 8, after forging, air cooling is to room temperature;
(3) steel ingot after forging carries out controlled rolling: first in recrystallization zone breaking down: breaking down temperature is 1050 ~ 1200 ℃; Then treat temperature in part recrystallization zone; Finally in the finish to gauge of non-recrystallization district: finishing temperature is 850～900 ℃; The control of rolling draught per pass is 20 ~ 25%, and total reduction control is 80 ~ 90%, rolls rear air cooling.
(4) thermal treatment process after controlled rolling: first air cooling after 1030 ~ 1100 ℃ of insulation 30 ~ 60min, then air cooling after 750 ~ 780 ℃ of insulation 90 ~ 120min.
In the present invention, constituent content range specification is as follows:
Carbon: carbon is austenite former, expands austenite phase region, dwindles ferrite phase region, can suppress the ferritic formation of high temperature in steel.Carbon and alloying elements cr, V, Ta etc. form M
23c
6type and MX type carbide, separate out at interfaces such as original austenite crystal prevention, laths circle, and pinning dislocation, obstruction interface movement, provide precipitation strength effect.But carbon is the easy element of diffusion, the easy alligatoring of carbide when too high levels and cause high temperature steel structure stability to reduce.Therefore carbon interpolation content is 0.10% ~ 0.35% in steel of the present invention.
Chromium: chromium is to improve one of the antioxidant property of steel and main interpolation element of resistance to liquid metal corrosion performance in high temperature steel.In oxidizing atmosphere, chromium is easily at the Surface Creation Cr of steel
2o
3, its content improves the antioxidant property that can improve steel, simultaneously fine and close Cr
2o
3layer can effectively hinder ion migration in steel and element dissolves in plumbous bismuth, thereby improves the anti-liquid metal corrosion performance of steel.But chromium too high levels makes easily to produce a large amount of high temperature ferrites in steel, therefore the control of chromium content is in the present invention: 10.0 ~ 12.0%.
Silicon: can promote SiO by increasing silicone content
2and FeSi
2o
4separate out, and the thickness of zone of oxidation is inversely proportional to the Si content that adds.Once fine and close SiO
2film forms, just can effectively hinder element to plumbous bismuth dissolve and plumbous bismuth to matrix permeability, thereby reduce rate of oxidation and erosion rate, raising solidity to corrosion.In high temperature steel, at least need 1.0% silicon effectively to resist the corrosion of liquid metal, and in the time that silicone content is greater than 2.0%, material can produce embrittlement phenomenon.Therefore in the present invention, silicone content control is 1.0 ~ 2.0%.
Tungsten: tungsten is the solution strengthening element in high temperature steel, tungsten can pass through to M
23c
6middle diffusion carrys out stable carbide size, thereby improves creep-resistant property.Because tungsten is the forming element of Laves phase in high temperature steel, the tungsten of too high amount can tertiary creep process in the separating out and alligatoring speed of Laves phase, the formation in tertiary creep cavity, solution strengthening effect reduces simultaneously, the creep property of steel reduces.The tungsten of too high amount also can promote the formation of delta ferrite in steel in addition, causes creep property to reduce.Therefore,, in the present invention, the content control of tungsten is 1.0 ~ 2.0%.
Manganese: manganese is austenite former and stable element, can significantly reduce the austenitic formation temperature A of steel
c1point and martensite formation temperature M
spoint, the hardening capacity of raising steel alloy, suppresses the formation of delta ferrite.But manganese content adds when too high, easily produces segregation in steel, be deformed into new austenite crystal, degrade performance to such an extent as to there is Local Phase.And manganese easily with steel in S form MnS and be mingled with, inclusion volume fraction increases the impelling strength of reduction steel.Therefore in steel of the present invention, the content of manganese interpolation control is less than 1.0%.
Ta, Nb: tantalum and niobium are carbide, form nano level precipitated phase as carbide, nitride and carbonitride with carbon in steel and nitrogen, improves the heat resistance of steel by precipitation and dispersion-strengthened.Its strong carbon solidification effect, can reduce M in addition
23c
6the alligatoring speed of type carbide, the creep property of raising high temperature steel.Increase with content, precipitated phase per-cent improves, but when too high levels, easily produces thick precipitated phase.Therefore in steel of the present invention, the content range control that tantalum niobium adds is Ta+Nb :≤0.45%.
V: vanadium is strong carbide forming element, forms nano level precipitated phase, pinning dislocation with carbon in steel and nitrogen.Gu carbon and organize the alloying elements such as Cr to cause slaking from matrix to diffusion in carbide, improves heat resistance.When V content is on the low side, be difficult for fully forming tiny carbide, do not have the effect of pinning dislocation, and content makes steel embrittlement when higher, therefore in steel of the present invention, the content control of vanadium is less than 0.30%.
S, P: be respectively main inclusions forming element and harmful element in steel.The crackle of the impact toughness of S on steel forms and expansion has totally unfavorable impact, damages the creep property of steel simultaneously.P sharply raises the ductile-brittle transition temperature of steel, has increased the cold shortness of steel.Therefore in steel of the present invention, S, P control very strict, control S < 0.005%, P < 0.007%.
In the present invention, heat treating regime is described as follows:
Normalizing temperature and soaking time thereof: the object of normalizing is the thick carbide in tissue when eliminating forging, rolling, at austenitizing state, its solid solution is entered to matrix, and in drawing process subsequently, M
23c
6and MX carbide can separate out at interfaces such as original austenite crystal prevention, laths circle, reach precipitation strength effect, obtain suitable grain size by adjusting normalizing temperature simultaneously.Steel of the present invention, in temperature, during lower than 1030 ℃ of normalizings, carbide does not fully dissolve, and can not fully play precipitating reinforcing effect.And when temperature is during higher than 1100 ℃, due to growing up fast of crystal grain, obtaining thick tissue, the impelling strength of steel declines rapidly.Therefore the present invention is chosen as 1030 ℃-1100 ℃ normalizing systems that keep 30-60min air cooling.
Tempering temperature and soaking time thereof: the object of tempering is for the effectively precipitation strength effect of performance carbide.Steel of the present invention is in the time that tempering temperature is too low, and as lower than 700 ℃, carbide can not be separated out fully.And in the time that tempering temperature is brought up to 800 ℃, precipitated phase slaking, the dislocation in steel is replied in a large number, and martensite dislocations strengthening effect reduces greatly, and the tensile strength of steel reduces.In order to obtain good comprehensive mechanical property, i.e. higher tensile strength and higher impelling strength, the tempering system of steel of the present invention is chosen as 740-780 ℃ of tempering 90-120min air cooling.
The invention has the beneficial effects as follows:
1, the present invention, by optimizing and revising the content of the element such as C, Mn, improves the hardening capacity of steel, and the formation that suppresses delta ferrite in steel remains on below 5% delta ferrite level, improves impelling strength and the high temperature creep property of high temperature steel.
2, the present invention adds high level Cr and Si form fine and close rich chromium and silicon oxide layer, improve antioxidant property and the resistance to liquid metal corrosion performance of steel.
3, steel high comprehensive performance of the present invention, can be used as the cooling nuclear reactor structure material of (600-850 ℃) liquid metal under hot conditions.
Accompanying drawing explanation
Fig. 1 is the microstructure schematic diagram of embodiment 1 in the present invention.
Fig. 2 is the antioxidant property of steel of the present invention and comparative example 1-2 steel under 700 ℃ of air atmosphere conditions.
Fig. 3 is antioxidant property under 800 ℃ of air atmosphere conditions.
Fig. 4 is 650 ℃ of high temperature endurance performances.
Fig. 5 is that in the present invention, embodiment 1 corrodes the cross-section morphology after 300h in the liquid lead bismuth alloy (Bi-45%Pb) of 600 ℃ of saturated oxygen concentration conditions.
Fig. 6 is that in the present invention, embodiment 2 corrodes the cross-section morphology after 300h in the liquid lead bismuth alloy (Bi-45%Pb) of 600 ℃ of saturated oxygen concentration conditions.
Fig. 7 is that in the present invention, embodiment 3 corrodes the cross-section morphology after 300h in the liquid lead bismuth alloy (Bi-45%Pb) of 600 ℃ of saturated oxygen concentration conditions.
Fig. 8 is that comparative example 1 corrodes the cross-section morphology after 300h in the liquid lead bismuth alloy (Bi-45%Pb) of 600 ℃ of saturated oxygen concentration conditions.
Embodiment
Following examples will be further described the present invention, but not thereby limiting the invention.Steel in embodiment becomes standard tensile, impact and enduring quality sample to test with the steel in comparative example through smelting, hot-work with thermal treatment post-treatment.Steel in embodiment 1-5 and comparative example 1-2 all adopts following method preparation, and step is as follows:
(1) in described ratio, each chemical composition is mixed, through smelting and cast acquisition high temperature steel steel ingot;
(2) steel ingot obtaining is forged in austenite one phase district: 1100 ~ 1200 ℃ of forging temperatures, forging ratio is 6 ~ 8, after forging, air cooling is to room temperature;
(3) steel ingot after forging carries out controlled rolling: first in recrystallization zone breaking down: breaking down temperature is 1050 ~ 1200 ℃; Then treat temperature in part recrystallization zone; Finally in the finish to gauge of non-recrystallization district: finishing temperature is 850 ~ 900 ℃; The control of rolling draught per pass is 20 ~ 25%, and total reduction control is 80 ~ 90%, rolls rear air cooling;
(4) thermal treatment process after controlled rolling: first air cooling after 1030 ~ 1100 ℃ of insulation 30 ~ 60min, then air cooling after 750 ~ 780 ℃ of insulation 90 ~ 120min.
Embodiment 1
In the present embodiment, the chemical composition of martensitic structure material is: C:0.25wt.%, Si:1.23wt.%, Cr:10.46wt.%, Mn:0.41wt.%, W:1.54wt.%, Ta:0.15wt.%, V:0.19wt.%, Nb:0.01wt.%, S<20(ppm), P:70(ppm), Cu<wt.0.01%, Al:65(ppm), Co:17(ppm), Ti:8(ppm), surplus is iron.
Embodiment 2
In the present embodiment, the chemical composition of martensitic structure material is: C:0.22wt.%, Si:1.56wt.%, Cr:10.73wt.%, Mn:0.67wt.%, W:1.41wt.%, Ta:0.19wt.%, V:0.21wt.%, Nb:0.01wt.%, S:50(ppm), P:70(ppm), Cu<wt.0.01%, Al:76(ppm), Co:24(ppm), Ti:6(ppm), surplus is iron.
Embodiment 3
In the present embodiment, the chemical composition of martensitic structure material is: C:0.32wt.%, Si:1.40wt.%, Cr:11.20wt.%, Mn:0.53wt.%, W:1.43wt.%, Ta:0.15wt.%, V:0.20wt.%, Ni:0.09wt.%, S<30(ppm), P:40(ppm), Cu < wt.0.01%, Al:53(ppm), Co:21(ppm), Ti:9(ppm), surplus is iron.
Embodiment 4
In the present embodiment, the chemical composition of martensitic structure material is: C:0.33wt.%, Si:1.37wt.%, Cr:11.90wt.%, Mn:0.31wt.%, W:1.53wt.%, Ta:0.41wt.%, V:0.39wt.%, Nb:0.01wt.%, S<20(ppm), P:60(ppm), Cu<wt.0.01%, Al:55(ppm), Co:23(ppm), Ti:14(ppm), surplus is iron.
In the present embodiment, the chemical composition of martensitic structure material is: C:0.20wt.%, Si:1.50wt.%, Cr:10.80wt.%, Mn:0.56wt.%, W:1.45wt.%, Ta:0.14wt.%, V:0.19wt.%, Nb:0.01wt.%, S:10(ppm), P:60(ppm), Cu<wt.0.01%, Al:80(ppm), Co:20(ppm), Ti:4(ppm), surplus is iron.
Comparative example 1
In the present embodiment, the chemical composition of martensitic structure material is: C:0.10wt.%, Si:0.30wt.%, Cr:8.21wt.%, Mn:0.40wt.%, V:0.20wt.%, Nb:0.08wt.%, Ni:0.08wt.%, Mo:0.96wt.%, S:10(ppm), P:120(ppm), surplus is iron.
Comparative example 2
In the present embodiment, the chemical composition of martensitic structure material is: C:0.20wt.%, Si:1.25wt.%, Cr:11.84wt.%, Mn:0.48wt.%, W:0.84wt.%, V:0.39wt.%, Nb:0.40wt.%, Ni:0.80wt.%, Mo:0.90wt.%, S:50(ppm), P:40(ppm), surplus is iron.
In above-described embodiment 1-5 and comparative example 1-2, mechanical properties and the impelling strength of steel are as shown in table 1, and the tensile strength in the time of 650 ℃ is as shown in table 2.
Table 1
Table 2
By table, 1-2 can find out, the present invention is by suitable increase chromium, carbon content and optimize other Composition Control delta ferrite levels lower than 5%, with respect to the steel in comparative example in improving room temperature and high temperature tensile properties, keep good impelling strength, in comparative example 2, steel is due to the delta ferrite that contains 10% left and right, its room temperature impact property is lower, is only 7 joules.
Fig. 1 is the microtexture of steel of the present invention, is martensitic stucture, and delta ferrite level is lower than 5%.
Fig. 2 is antioxidant property under 700 ℃ of air atmosphere conditions.Compared with steel in comparative example, steel of the present invention has obvious 700 ℃ of antioxidant property advantages.
Fig. 3 is antioxidant property under 800 ℃ of air atmosphere conditions.Compared with steel in comparative example, steel of the present invention has obvious 800 ℃ of antioxidant property advantages.
Fig. 4 is 650 ℃ of high temperature endurance performances.At stress during higher than 120MPa, embodiment 1,2,3 in the present invention has slightly high creep strength with respect to comparative example 2 steel, at stress during lower than 120MPa, in comparative example, steel creep strength significantly declines, there is flex point in curve, and embodiment steel still keeps good linear relationship, according to thermoisopleth extrapotation, in the creep rupture strength of low stress area steel of the present invention apparently higher than comparative steel.
Embodiment 1,2,3 and comparative example 1 that Fig. 5, Fig. 6, Fig. 7 and Fig. 8 are respectively in the present invention corrode the cross-section morphology after 300h in the liquid lead bismuth alloy (Bi-45%Pb) of 600 ℃ of saturated oxygen concentration conditions.The zone of oxidation of steel of the present invention and comparative steel is the infiltration of resistance to liquid metal all, but the oxide thickness in the embodiment of the present invention 1,2,3 is only for being respectively 24,22,24 μ m left and right, and in comparative example, the oxide thickness of steel is up to 49 μ m.What in the section element distribution results discovery steel of the present invention of oxide film, produce is the zone of oxidation of Fu Ge, Silicon-rich, and in comparative example, in steel oxidation layer, being mainly the oxide compound of iron, the zone of oxidation of Fu Ge and silicon has effectively improved the anti-oxidant and resistance to liquid metal corrosion ability of material.Result shows, steel of the present invention has more good resistance to liquid metal corrosion performance.
Claims (5)
1. the martensitic structure of a resistance to liquid metal corrosion material for high temperature, it is characterized in that: by weight percentage, its chemical composition is: C:0.10 ~ 0.35%, Cr:10.0 ~ 12.0%, W:1.0 ~ 2.0%, Mn :≤1.0%, Si:1.0 ~ 2.0%, Ta+Nb :≤0.45%, V :≤0.3%, surplus is iron.
2. the martensitic structure of resistance to liquid metal corrosion material for high temperature according to claim 1, it is characterized in that: in described martensitic structure material: P < 0.007wt.%, S < 0.005wt.%, Cu < 0.01wt.%, Ti<0.010wt.%, Al<0.010wt.%, Co<0.005wt.%.
3. the martensitic structure of resistance to liquid metal corrosion material for high temperature according to claim 1, is characterized in that: in described martensitic structure material structure, delta ferrite level is lower than 5%.
4. the martensitic structure of resistance to liquid metal corrosion material for high temperature according to claim 1, is characterized in that: described martensitic structure material generates the compact oxidation layer of rich chromium and silicon under the liquid metal corrosion environment of saturated oxygen concentration.
5. the preparation method with the martensitic structure of resistance to liquid metal corrosion material according to the arbitrary described high temperature of claim 1-4, is characterized in that: comprise the steps:
(1) in described ratio, each chemical composition is mixed, through smelting and cast acquisition high temperature steel steel ingot;
(2) steel ingot obtaining is forged in austenite one phase district: 1100 ~ 1200 ℃ of first forging temperatures, forging ratio is 6 ~ 8, after forging, air cooling is to room temperature;
(3) steel ingot after forging carries out controlled rolling: first in recrystallization zone breaking down: breaking down temperature is 1050 ~ 1200 ℃; Then treat temperature in part recrystallization zone; Finally in the finish to gauge of non-recrystallization district: finishing temperature is 850 ~ 900 ℃; The control of rolling draught per pass is 20 ~ 25%, and total reduction control is 80 ~ 90%, rolls rear air cooling;
(4) thermal treatment process after controlled rolling: first air cooling after 1030 ~ 1100 ℃ of insulation 30 ~ 60min, then air cooling after 750 ~ 780 ℃ of insulation 90 ~ 120min.
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Inventor after: Wang Zhiguang Inventor after: Dan Yiyin Inventor after: Yao Cunfeng Inventor after: Yan Wei Inventor after: Wei Kongfang Inventor after: Zhou Qiangguo Inventor after: Wang Wei Inventor after: Yang Ke Inventor before: Zhou Qiangguo Inventor before: Yan Wei Inventor before: Wang Wei Inventor before: Dan Yiyin Inventor before: Wang Zhiguang Inventor before: Yang Ke |
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Effective date of registration: 20181129 Address after: 730000 Nanchang Road, Lanzhou, Gansu 509 Co-patentee after: Institute of metal research, Chinese Academy of Sciences Patentee after: Modern Physics Inst., Chinese Academy of Sciences Address before: 110016 No. 72, Wenhua Road, Shenhe District, Liaoning, Shenyang Patentee before: Institute of metal research, Chinese Academy of Sciences |