CN108893580B - A kind of nitride strengthening ODS steel and preparation method thereof - Google Patents

A kind of nitride strengthening ODS steel and preparation method thereof Download PDF

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CN108893580B
CN108893580B CN201810748400.9A CN201810748400A CN108893580B CN 108893580 B CN108893580 B CN 108893580B CN 201810748400 A CN201810748400 A CN 201810748400A CN 108893580 B CN108893580 B CN 108893580B
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nitride
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严伟
李艳芬
单以银
石全强
杨柯
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Institute of Metal Research of CAS
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    • C21D2211/008—Martensite

Abstract

The invention belongs to high temperature resistant Flouride-resistani acid phesphatase metal material fields, and in particular to a kind of nitride strengthening ODS steel and preparation method thereof.By weight percentage, alloying component is as follows: C :≤0.03%, Si :≤0.5%, Mn:0.6~1.5%, Cr:8.0~15.0%, W :≤1.5%, Mo :≤1.5%, (W+Mo): 1.0~1.5%, Nb:0.02~0.06%, Ta:0.05~0.15%, (Nb+Ta): 0.10~0.15%, V:0.15~0.30%, 0.05%≤Y2O3≤ 0.5%, N:0.02~0.08%, Co :≤0.05%, Ni :≤0.01%, Al: < 0.01%, Ti: < 0.005%, Cu: < 0.01%, P < 0.010%, S < 0.005%, Fe surplus.By control carbon content 0.03% hereinafter, avoid the formation of high temperature it is long when service condition under the M that is easily roughened23C6Carbide, M are mainly Cr or Fe, and are only strengthened by nanoscale nitride and oxide synergy with thermal stability and Dispersed precipitate, thus to obtain excellent high temperature microstructure thermal stability and excellent anti-radiation performance.

Description

A kind of nitride strengthening ODS steel and preparation method thereof
Technical field
The invention belongs to high temperature resistant Flouride-resistani acid phesphatase metal material fields, and in particular to it is a kind of by nano nitride with it is nano oxidized The ferrite/martensite steel of object cooperative reinforcing, hereinafter referred to as nitride strengthening ODS steel (Oxide Dispersion Strengthened) and preparation method thereof.
Background technique
Positive Nuclear Power Development is one of grand strategy planning of China's energy development.However, the following forth generation fission-type reactor combustion Expect the exceedingly odious military service ring such as cladding materials and fusion reactor proliferation cladding structure material face Lingao temperature, strong neutron irradiation, corrosion Border fights strong neutron irradiation performance, mechanical behavior under high temperature, high-temperature oxidation resistance etc. and proposes high requirement, wherein resisting in strong Sub- irradiation behaviour and mechanical behavior under high temperature are two performance indicators of most critical.
Precipitated phase gets over small and dispersed, and thermal stability is higher, and the effect of performance is bigger.It is tiny, more with high stability Scattered precipitated phase can not only improve elevated temperature strength, moreover it is possible to capture irradiation defect, play the role of " trap ", to enhance anti-neutron spoke According to ability.Y2O3Particle is a kind of inertia rare earth oxide, and physicochemical properties are stablized, and has biggish neutron absorption cross-section； Even if being on active service when high temperature, long, under ambient stress, it still is able to stablize pinning dislocation motion, improves the high temperature microstructure heat of material Stability.When being subjected to large dosage of neutron irradiation, material internal occur (n, α) transmuting, generate have radioactive isotope and Helium atom, the nanometer Y of Dispersed precipitate in the base2O3Particle can prevent helium atom poly- as various irradiation defect traps such as helium Collection forms helium bubble, increases substantially anti-neutron irradiation performance.Therefore, oxide dispersion intensifying (ODS) steel has excellent high temperature Mechanical property and good resist strong neutron irradiation performance.
Currently, in fusion reactor in advanced iron structure material, Japan develops 9-12Cr series ODS steel, Europe development ODS-Eurofer97 steel, Chinese development CLAM-ODS steel, CLF-ODS steel etc..Compared with low activation steel (RAFM), accordingly add The ODS steel mechanical behavior under high temperature and anti-radiation performance of oxygenates are improved significantly.However, from it is at higher temperature, long when, irradiation Extreme service condition under see, there are still shortcomings when the ingredient and group of the above ODS steel are woven in initial designs: (1) such Contain carbon in the master alloy ingredient of ODS steel, will form a large amount of M23C6Carbide, the carbide still can be in subsequent high temperature Curing occurs when long under service condition to grow up.In addition, irradiation can also promote its curing；And coarse M23C6Carbide can induce Creep hole causes ductile-brittle transition temperature (DBTT) after creep rupture and irradiation to steeply rise；(2) W, Mo element are in high temperature Laves phase (Fe is formed during when long2W、Fe2Mo essential element), excessively high W, Mo constituent content will increase Laves phase and analyse Driving force out, under conditions of being aided with irradiation, coarsening rate is very big, not only reduces the solid solution strengthening effect of W, Mo element, slightly The Laves phase of change can also induce creep rupture, DBTT is caused to rise.
Patent document 1 (CN201110103010) is related to a kind of novel nitride strengthening martensite heat-resistant steel, wherein described The primary alloy constituent (weight percent) of martensite heat-resistant steel is Mn:0.8~1.5%；Cr:8.0~10.0%；W:≤ 1.5%；Mo :≤1.5%；And W+Mo:1.5~2.0%；Nb :≤0.06%；Ta :≤0.15%；And Nb+Ta:0.05~ 0.15%；V:0.1~0.3%；N:0.02~0.08%；Fe surplus；C :≤0.005%；Si :≤0.5%；S :≤0.005%； P :≤0.005%；Co :≤1.5%；O :≤0.0010%；Ni :≤0.01%；Al: < 0.01%；Ti: < 0.005%；Cu:< 0.01%.But alloy precipitation phase density is low, tissue thermostabilization is poor, is only used for 600 DEG C and following temperature, can not be 650 It is used under DEG C temperatures above.
Summary of the invention
The technical issues of proposing for background technique, it is an object of the invention to propose a kind of novel nitride strengthening ODS Steel and preparation method thereof is obtained excellent using the dispersed and tiny nitride with high thermal stability and oxide synergy invigoration effect The nitride strengthening ODS steel of good high temperature microstructure stability, by unique novel organization design, can obtain it is excellent it is anti-it is strong in Sub- irradiation behaviour and mechanical behavior under high temperature.
Technical scheme is as follows:
A kind of nitride strengthening ODS steel, by weight percentage, alloying component is as follows:
C :≤0.03%, Si :≤0.5%, Mn:0.6~1.5%, Cr:8.0~15.0%, W :≤1.5%, Mo :≤ 1.5%, (W+Mo): 1.0~1.5%, Nb:0.02~0.06%, Ta:0.05~0.15%, (Nb+Ta): 0.10~0.15%, V:0.15~0.30%, 0.05%≤Y2O3≤ 0.5%, N:0.02~0.08%, Co :≤0.05%, Ni :≤0.01%, Al: < 0.01%, Ti: < 0.005%, Cu: < 0.01%, P < 0.010%, S < 0.005%, Fe surplus；Existed by controlling carbon content 0.03% hereinafter, avoid the formation of high temperature it is long when service condition under the M that is easily roughened23C6Carbide, M are mainly Cr or Fe, and only by Strengthen with the nanoscale nitride and oxide synergy of thermal stability and Dispersed precipitate, thus to obtain excellent high temperature microstructure heat Stability and excellent anti-radiation performance.
The nitride strengthening ODS steel, tissue are ferrite or martensitic structure, the nanoscale nitrogen being distributed thereon The size of compound is between 10~50nm, and number density is 1021~1022The order of magnitude of a/cubic meter, and nano-oxide particles Size in 20nm hereinafter, number density is 1023The order of magnitude of a/cubic meter.
The preparation method of the nitride strengthening ODS steel, the preparation process of nitride strengthening ODS steel include: female conjunction Golden smelting → powder atomization → high-energy ball milling → powder jacket pumping → hot isostatic pressing curing molding → hot rolling → heat treatment, finally Tissue needed for obtaining；
By weight percentage, the master alloy ingredient of nitride strengthening ODS steel are as follows: C :≤0.005%；Si :≤0.5%； Mn:0.6~1.5%；Cr:8.0~15.0%；W :≤1.5%；Mo :≤1.5%；(W+Mo): 1.0~1.5%；Nb:0.02~ 0.06%；Ta:0.05~0.15%；(Nb+Ta): 0.10~0.15%；V:0.15~0.30%；N:0.02~0.08%；Co: ≤ 0.05%；Ni :≤0.01%；Al: < 0.01%；Ti: < 0.005%；Cu: < 0.01%；P < 0.010%, S < 0.005%；Fe Surplus；It writes a Chinese character in simplified form are as follows: Fe-0C- (8~15) Cr-1.25 (W+Mo) -0.20V-0.12 (Ta+Nb) -1.0Mn.
In described Fe-0C- (8~15) Cr-1.25 (W+Mo) -0.20V-0.12 (the Ta+Nb) -1.0Mn master alloy, Mn, Ta element is easy scaling loss element, ingredient need to be carried out by 90~93% recovery rates, and be added the alloying element in refining, when refining Between be 10~30min, during which stir 3~5 times.
The master alloy powder atomization requires as follows: granularity<40 μm, atomization pressure>3.5MPa, the degree of superheat>200 DEG C, protective atmosphere is the argon gas of 99.99% or more bulk purity.
In order to make the Y of 20~50nm of partial size2O3Nano particle even dispersion is distributed in master alloy powder, high-energy ball milling Process parameter control is as follows: milling atmosphere is the argon gas of 99.99% or more bulk purity, and ball material mass ratio is (5~10): 1, ball Consume time 40~60h, and revolving speed is 350~500r/min.
Reduce porosity to remove the gas of powder particle surface absorption, the air aspiration process of powder jacket is as follows: vacuum Degree is 10-1Pa, temperature are 400~500 DEG C, and the time is 3~5h.
The hot isostatic pressing cure process of the powder jacket is as follows: pressure is 120~150MPa, temperature 1000 ~1200 DEG C, the heat-insulation pressure keeping time is 3~5h.
In order to further increase the consistency and mechanical property of nitride strengthening ODS steel after curing molding, hot rolling technology control Make as follows: start rolling temperature is 1100~1200 DEG C, and finishing temperature is 900~950 DEG C, and rolling pass is 5~6 times.
The nitride strengthening ODS Heat-Treatment of Steel technology controlling and process is as follows: normalizing process parameter is 1050~1200 DEG C It is air-cooled to keep the temperature 60~90min, tempering process parameters are that 750~800 DEG C of 90~120min of heat preservation are air-cooled.
Design philosophy of the invention is:
Develop this technology key point first is that: the accurate control of C, N element in nitride strengthening ODS steel master alloy.Such as Shown in Fig. 1, M23C6The thermal stability of carbide and nitride difference is very big, at 600 DEG C, M23C6The curing speed of carbide is aobvious It writes and is higher than MX phase.Thus, carbon content must be controlled to 0.0050% hereinafter, in turn in nitrogen in nitride strengthening ODS steel master alloy Compound, which is strengthened, controls carbon content 0.03% hereinafter, just it is possible to prevente effectively from the formation of carbide in ODS steel.Why is C content It is limited to 0.03% extremely low level below, is because even can be given birth in steel when low-level of the carbon content 0.03% or more At the M of bulky grain23C6Carbide.Therefore, it is specified that C content is 0.0050% in the master alloy ingredient of nitride strengthening ODS steel Below.Secondly, N content needs to control in 0.02~0.08% level.On the one hand, it if N content is more than 0.08 or more, is easy Tiny nitride is consumed under the conditions of when high temperature is long and generates the faster Z phase of curing speed, ingredient substantially Cr (Nb, Ta, V) N；On the other hand, if N content is too low, the quantity that nitride is formed in steel is very little.Therefore, by previous experiments optimizing research, Nitrogen content must control in the range of 0.02~0.08% in nitride strengthening ODS steel master alloy.
Previous experiments can significantly improve holding for steel studies have shown that when using nitride strengthening martensite heat-resistant steel merely Long intensity, but since the number density of nitrogen in steel compound precipitated phase can only achieve 1021~1022The order of magnitude, thus while 600 DEG C/150MPa under conditions of obtain good creep rupture life of 14970h, but will occur to tie again after 650 DEG C of timeliness several hundred hours Crystalline substance, reason are the M of former pinning crystal boundary23C6Eliminate and Nitride Phase number density is inadequate.And at this time if contained by increasing nitrogen Amount can make the precipitation of Z phase improve to improve the number density of nitrogen in steel compound particle, damage the performance of material instead.Therefore, Nitride strengthening is individually added into be difficult to meet the intensity requirement under higher temperature.On the other hand, although passing through mechanical alloying It is 10 that method, which can obtain number density in ODS steel,23The nanoscale composition granule of the order of magnitude, but to obtain in ideal resist The number density of sub- irradiation behaviour, precipitated phase is the bigger the better, it is therefore desirable to reach 1024(this is that the number of phases is precipitated in current ODS steel to the order of magnitude The effort target of density).Therefore, other than nano-oxide particles, nano nitride is also needed in nitride strengthening ODS steel Cooperative reinforcing, to obtain optimal Radiation hardness.
It is well known that the half-life period of the artificial radioactivity nucleic of W, Ta is about several hundred days, but the artificial radioactivity of Mo, Nb The half-life period of nucleic is then up to 44 years, 20,000 years respectively.Overactivity elements Mo, Nb are replaced using low activation element W, Ta, it can be with Obtain the nitride strengthening ODS steel with low activation characteristic.Therefore, in present invention ingredient claimed, also comprising carrying out With the nitride strengthening ODS steel of low activation characteristic after composition adjustment.
Currently, also finding no the similar master alloy system with the present invention, this is also exactly main feature of the invention.This hair Bright novelty is the cooperative reinforcing of Nitride Oxide, i.e. nitrogen in steel compound and the synergistic effect of oxide particle.As before Described, the synergistic effect of precipitated phase can obtain more preferably technical effect than individually addition.
The invention has the advantages and beneficial effects that:
1, firstly, carbon content is extremely low in master alloy, 0.0050% hereinafter, so that in novel nitride strengthening ODS steel not It is formed in the M for being easy to be roughened under high temperature, radiation parameter23C6Carbide, to overcome its influence to high temperature mechanical property when long； Secondly, will form tiny nitride of taking measurements greatly in master alloy ingredient；Again, after mechanical alloying, in master alloy base Nanoscale composition granule is introduced in body, increases the number density of precipitated phase, is obtained and is assisted by the nitride and oxide of fine size With the novel nitride strengthening ODS steel strengthened.
2, the nitride strengthening ODS steel of present component, is primarily characterized in that: 1) extremely low (C:< of carbon content in steel 0.03%) M for being easy to cure under high temperature, is not formed in matrix23C6(M is mainly Cr, Fe) carbide；2) NbN in steel, The size of the nitride of TaN, VN high thermal stability is between 10~50nm, and number density (a/cubic meter) is 1021~1022Quantity Grade, and the size of nano-oxide particles in 20nm hereinafter, number density is 1023The order of magnitude；3) tri- kinds of elements of Co, W, Mo in steel Content is limited in lower level, to reduce the precipitation driving force of steel Laves phase under hot conditions when long.The ferrite of steel/ Martensitic matrix tissue is obtained by the strong pinning of nanoscale nitride and oxide with high thermal stability and Dispersed precipitate Excellent mechanical behavior under high temperature and anti-radiation performance under high temperature, strong irradiation service condition.
Detailed description of the invention:
Fig. 1 is M23C6The thermal stability of carbide and nitride compares.Wherein, (a) is that MX class is analysed under 1300 DEG C of high temperature Phase and M out23C6The curing speed of carbide (b) is MX class carbonitride and M under the conditions of when 600 DEG C of high temperature are long23C6Carbide Coarsening rate compare, abscissa exposure time represents time for exposure (h), ordinate mean diameter of Particies is represented average diameter of particles (nm), and gauge length is gauge length, and specimen head is sample end, P92creep specimens is creep sample.
Fig. 2 is Carbides Evolution of (9Cr-0.1C) the ODS steel at 700 DEG C after long-time aging.Wherein, (a) original state, (b) 1000h, (c) 5000h, (d) 10000h.
Fig. 3 is that phase morphology is precipitated in nitride to nitrogen content in master alloy in claimed range.Wherein, (a) embodiment 1 is female closes Gold, (b) 2 master alloy of embodiment, (c) 3 master alloy of embodiment, (d) 4 master alloy of embodiment.
Fig. 4 is that phase morphology is precipitated in nitride strengthening ODS steel corresponding with master alloy ingredient in Fig. 3.Wherein, (a)
Embodiment 1, (b) embodiment 2, (c) embodiment 3, (d) embodiment 4.
Morphology of Nitrides when Fig. 5 is N < 0.03% in master alloy.
The Z phase being precipitated after Morphology of Nitrides and long-time aging when Fig. 6 is N > 0.08% in master alloy.Wherein, (a) is nitrogenized Object precipitated phase, (b) Z phase.
Fig. 7 is the mechanical behavior under high temperature and structure stability of master alloy ingredient；Wherein, (a) mechanical curves, abscissa Time represents the time (h), and ordinate Stress represents stress (MPa)；(b) heat treatment state tissue；(c) 600 DEG C/150MPa, 14979h fracture；(d) precipitated phase in the lasting 3000h sample of 600 DEG C/150MPa；(e) 650 DEG C of enduring quality curves, abscissa Time represents the time (h), and ordinate Stress represents stress (MPa)；(f) perfect recrystallization occurs for 650 DEG C of timeliness 1000h.
Fig. 8 be 9Cr-ODS steel in crystal grain, nano-oxide pattern.Wherein, (a) grain morphology, it is (b) nano oxidized Object pattern, (c) grain size, nanoparticle size and number density.
Fig. 9 is the pattern of precipitated phase and the differentiation pattern at 700 DEG C after timeliness in novel nitride strengthening ODS steel.Its In, (a) original state, (b) 1000h, (c) 5000h, (d) 10000h.
Figure 10 is the hardness curve of novel nitride strengthening ODS steel after 700 DEG C of timeliness different times.
Specific embodiment:
In the specific implementation process, the present invention provides a kind of nitride strengthening ODS steel, alloying component (weight percent) Are as follows: C :≤0.03%, Si :≤0.5%, Mn:0.6~1.5%, Cr:8.0~15.0%, W :≤1.5%, Mo :≤1.5%, (W + Mo): 1.0~1.5%, Nb:0.02~0.06%, Ta:0.05~0.15%, (Nb+Ta): 0.10~0.15%, V:0.15~ 0.30%, 0.05%≤Y2O3≤ 0.5%, N:0.02~0.08%, Co :≤0.05%, Ni :≤0.01%, Al: < 0.01%, Ti: < 0.005%, Cu: < 0.01%, P < 0.010%, S < 0.005%, Fe surplus.By control carbon content in 0.03% (weight Percentage) hereinafter, avoid the formation of high temperature it is long when service condition under the M that is easily roughened23C6(M is mainly Cr, Fe) carbide, and only by Strengthen with the nanoscale nitride and oxide synergy of high thermal stability and Dispersed precipitate, thus to obtain excellent high temperature group Knit thermal stability and excellent anti-radiation performance.It organizes to be ferrite or martensitic structure, the nanoscale nitrogen being distributed thereon The size of compound is between 10~50nm, and number density (a/cubic meter) is 1021~1022The order of magnitude, and nano-oxide particles Size in 20nm hereinafter, number density is 1023The order of magnitude.
The preparation process of the nitride strengthening ODS steel, comprising: master alloy smelting → powder atomization → high-energy ball milling → powder Last jacket pumping → hot isostatic pressing curing molding → hot rolling → heat treatment, it is final to obtain required tissue.Nitride strengthening ODS steel Master alloy ingredient (weight percent) are as follows: C :≤0.005%；Si :≤0.5%；Mn:0.6~1.5%；Cr:8.0~ 15.0%；W :≤1.5%；Mo :≤1.5%；(W+Mo): 1.0~1.5%；Nb:0.02~0.06%；Ta:0.05~ 0.15%；(Nb+Ta): 0.10~0.15%；V:0.15~0.30%；N:0.02~0.08%；Co :≤0.05%；Ni:≤ 0.01%；Al: < 0.01%；Ti: < 0.005%；Cu: < 0.01%；P < 0.010%, S < 0.005%；Fe surplus；It can write a Chinese character in simplified form Are as follows: Fe-0C- (8-15) Cr-1.25 (W+Mo) -0.20V-0.12 (Ta+Nb) -1.0Mn.Using the method smelting of vacuum induction melting Refine super clean master alloy, using the high purity iron of Ultra-low carbon (content is in 0.002wt% or so), high-purity Cr, the pure V of dendrite, high-purity W, The high-purity raws such as Ta item carry out vacuum induction melting.Mn, Ta element are easy scaling loss element in master alloy, need to be by 90~93% Recovery rate carries out ingredient, and the alloying element is added in refining, and refining time is 10~30min, during which stirs 3~5 times.
The present invention is described in detail below by way of embodiments and comparative examples.
Embodiment 1:
In the present embodiment, nitride strengthening ODS steel, alloying component (weight percent) is C:0.03%, Si: 0.2%, Mn:1.0%, Cr:8.9%, W:1.43%, Nb:0.02%, Ta:0.10%, V:0.18%, Y2O3: 0.1%, N: 0.03%, Co:0.02%, Ni:0.005%, Al:0.005%, Ti:0.002%, Cu:0.005%, P:0.008%, S: 0.002%, Fe surplus.
The preparation process of the nitride strengthening ODS steel is as follows:
(1) master alloy is smelted, master alloy ingredient are as follows:
0.004C-8.9Cr-1.45W-0.19V-0.12Ta-0.02Nb-1.0Mn-0.032N, Mn, Ta element in master alloy For easy scaling loss element, ingredient need to be carried out by 90~93% recovery rates, and the alloying element is added in refining, and refining time is During which 20min is stirred 4 times；
(2) powder atomization, 35 μm of average particle size, atomization pressure 4.0MPa, 250 DEG C of the degree of superheat, protective atmosphere is body The argon gas of product purity 99.99%；
(3) high-energy ball milling, to make Y2O3Grain diameter 30nm and even dispersion is distributed in master alloy powder, high-energy ball milling Process parameter control is as follows: milling atmosphere be bulk purity 99.99% argon gas, ball material mass ratio be 8:1, Ball-milling Time 50h, Revolving speed is 400r/min；
(4) powder jacket is evacuated, and the gas for removal powder particle surface absorption reduces porosity, the pumping of powder jacket Technique is as follows: vacuum degree 10-1Pa, temperature are 450 DEG C, time 4h；
(5) hot isostatic pressing curing molding, pressure 130MPa, temperature are 1100 DEG C, and the heat-insulation pressure keeping time is 4h；
(6) hot rolling, start rolling temperature are 1150 DEG C, and finishing temperature is 920 DEG C, and rolling pass is 6 times；
(7) it is heat-treated, normalizing process parameter is that 1100 DEG C/80min/ is air-cooled, and tempering process parameters are 770 DEG C/100min/ It is air-cooled.
Embodiment 2:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, wherein master alloy ingredient are as follows:
0.003C-11Cr-1.5W-0.18V-0.14Ta-1.2Mn-0.05N。
In the present embodiment, nitride strengthening ODS steel, alloying component (weight percent) is C:0.015%, Si: 0.2%, Mn:1.0%, Cr:11%, W:1.5%, Ta:0.12%, V:0.18%, Y2O3: 0.15%, N:0.045%, Co: More than 0.03%, Ni:0.004%, Al:0.006%, Ti:0.002%, Cu:0.005%, P:0.005%, S:0.002%, Fe Amount.
Embodiment 3:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, wherein master alloy ingredient are as follows:
0.002C-12Cr-1.0W-0.4Mo-0.18V-0.13Ta-0.02Nb-0.6Mn-0.06N。
In the present embodiment, nitride strengthening ODS steel, alloying component (weight percent) is C:0.010%, Si: 0.3%, Mn:0.6%, Cr:12%, W:1.0%, Mo:0.4%, Nb:0.02%, Ta:0.12%, V:0.18%, Y2O3: 0.3%, N:0.056%, Co:0.01%, Ni:0.003%, Al:0.005%, Ti:0.001%, Cu:0.002%, P: 0.004%, S:0.003%, Fe surplus.
Embodiment 4:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, wherein master alloy ingredient are as follows:
0.005C-14Cr-1.2W-0.3Mo-0.22V-0.10Ta-0.04Nb-1.0Mn-0.075N。
In the present embodiment, nitride strengthening ODS steel, alloying component (weight percent) is C:0.008%, Si: 0.2%, Mn:0.8%, Cr:14%, W:1.2%, Mo:0.3%, Nb:0.042%, Ta:0.08%, V:0.20%, Y2O3: 0.5%, N:0.065%, Co:0.03%, Ni:0.002%, Al:0.005%, Ti:0.002%, Cu:0.003%, P: 0.005%, S:0.003%, Fe surplus.
The ODS steel of comparative example 1:9Cr-0.1C
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, alloying component are as follows: 0.10C-9.0Cr-2.0W-0.2V-0.27Y2O3。
Comparative example 2:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, wherein master alloy ingredient are as follows:
0.003C-8.8Cr-1.50W-0.18V-0.15Ta-0.8Mn-0.015N。
In this comparative example, nitride strengthening ODS steel, alloying component (weight percent) is C:0.02%, Si: 0.3%, Mn:0.8%, Cr:8.9%, W:1.50%, Ta:0.14%, V:0.16%, Y2O3: 0.3%, N:0.012%, Co: More than 0.04%, Ni:0.006%, Al:0.007%, Ti:0.002%, Cu:0.005%, P:0.004%, S:0.003%, Fe Amount.
Comparative example 3:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process, wherein master alloy ingredient are as follows:
0.005C-13Cr-1.46W-0.21V-0.14Ta-0.8Mn-0.085N。
In this comparative example, nitride strengthening ODS steel, alloying component (weight percent) is C:0.03%, Si: 0.1%, Mn:0.8%, Cr:13.2%, W:1.45%, Ta:0.12%, V:0.20%, Y2O3: 0.26%, N:0.086%, Co: More than 0.02%, Ni:0.004%, Al:0.006%, Ti:0.003%, Cu:0.004%, P:0.005%, S:0.004%, Fe Amount.
Comparative example 4:
Simple nitride strengthening is prepared using " master alloy smelting-hot rolling-heat treatment " preparation process same as Example 1 Steel, alloying component are as follows: 0.003C-8.9Cr-1.4W-0.20V-0.05Nb-0.8Mn-0.028N.
Comparative example 5:
Using same as Example 1, " master alloy smelting-powder atomization-high-energy ball milling-powder jacket pumping-heat etc. is quiet Cured molding-hot rolling-heat treatment " preparation process prepares ODS steel, alloying component are as follows: 0.01C-9Cr-1.5W-0.20V- 0.3Y2O3。
1 embodiment steel of table and comparative example steel mechanical property
As shown in Fig. 1 (a)-(b), from M23C6The thermal stability of carbide and nitride compares it can be seen that at 1300 DEG C Under high temperature, the curing speed of MX class carbide or nitride will be significantly less than M23C6Carbide is shown in Fig. 1 (a)；In addition, at 600 DEG C Under the conditions of when high temperature is long, the coarsening rate of MX class carbonitride will also be significantly less than M23C6Carbide is shown in Fig. 1 (b).
It, can be with from Carbides Evolution of (9Cr-0.1C) the ODS steel at 700 DEG C after long-time aging as shown in Fig. 2 (a)-(d) Find out, after running in conventional carbon containing ODS steel when high temperature is long, coarse M can be generated23C6Carbide damages the high temperature power of material Learn performance.
Fig. 3 (a), Fig. 3 (b), Fig. 3 (c), Fig. 3 (d) are respectively nitrogen content nitride in master alloy within the scope of component requirements Phase morphology is precipitated, wherein nitride precipitated phase is tiny；The number density of nitride precipitated phase is mentioned with the raising of nitrogen content Height, but the number density of nitride precipitated phase is all 1021~1022Magnitude.
Fig. 4 (a), Fig. 4 (b), Fig. 4 (c), Fig. 4 (d) are respectively Fig. 3 (a), Fig. 3 (b), Fig. 3 (c), the corresponding reality of Fig. 3 (d) Apply the pattern of precipitated phase in example 1~4.
9Cr-ODS steel of the comparative example 1 containing 0.1wt%C content long-time aging at 700 DEG C, through timeliness 5000h or more, M23C6Carbide begins to obviously grow up, as timeliness 10000h, M23C6The size maximum of Carbide Precipitation phase can achieve 1 μ m.Therefore carbon containing type ODS steel cannot overcome M23C6Carbide is easy the shortcomings that roughening.
N content is less than 0.02wt% in master alloy in comparative example 2, from figure 5 it can be seen that the obvious mistake of the density of precipitated phase It is low, therefore N content is not preferably less than 0.02wt% in master alloy.
Master alloy N > 0.080wt% in comparative example 3, the precipitation phase morphology of nitride is as shown in Fig. 6 (a), but 650 Nitride is easily formed Z phase during DEG C Long-term Aging 5000h, as shown in Fig. 6 (b).
Comparative example 4 is not add Y2O3The simple master alloy component steel 9CrWVNbN by nitride strengthening, although 600 There is excellent high temperature endurance performance (see Fig. 7 (a)) and good high temperature microstructure stability (see Fig. 7 (b), Fig. 7 (c)) at DEG C, And by up to 14979h it is long when creep tissue it is still stable.It can be seen that the tiny nitrogen of Dispersed precipitate in steel from Fig. 7 (d) Compound precipitated phase is the reason of 9CrWVNbN steel obtains good high temperature endurance performance at 600 DEG C to the static stabilization to tissue.
But when service temperature is from when being increased to 650 DEG C for 600 DEG C, Y is not added2O3It is simple by nitride strengthening mother close Golden ingredient 9CrWVNbN steel is organized just to recrystallize, intensity is rapid since precipitated phase number density is insufficient after lasting several hundred hours Decline and creep rupture occurs.As it can be seen that not adding Y2O3It is simple be not able to satisfy by the master alloy component steel of nitride strengthening it is higher At a temperature of requirement, need to introduce more disperse educt phases in steel matrix.
Comparative example 5 is only to add Y2O3The not 9Cr-ODS steel of nitrogenate.As shown in Fig. 8 (a)-(c), 9Cr-ODS steel Average grain size is about 1~2 μm, and nano particle size is about 3.5nm, number density 1023/m3.But also it is not achieved 1024/m3 The order of magnitude, therefore the precipitated phase for also needing more sizes tiny is to improve the ability of anti-neutron irradiation.
As shown in Fig. 9 (a)-(d), from precipitated phase in embodiment 2, precipitated phase is still after timeliness reaches 10000h at 700 DEG C It does not grow up, illustrates that it is steady to all have good heat for nanoscale nitride and nano-scale oxide in novel nitride strengthening ODS steel It is qualitative.
As shown in Figure 10, the hardness of novel nitride strengthening ODS steel can be seen that firmly after 700 DEG C of timeliness different times Degree does not change significantly, illustrates that novel nitride strengthening ODS steel has good stable mechanical property, this is good with it Structure stability is consistent.
Electronics, ion irradiation experiment are carried out to embodiment steel 1, comparative example 4 and comparative example 5, the results showed that, contain nitride It is less than with the void swelling of the embodiment steel 1 of nano-oxide particles and is only received by the comparative example steel 4 of nitride strengthening and containing only The comparative example steel 5 of rice oxide.
The above embodiments merely illustrate the technical concept and features of the present invention, and protection model of the invention can not be limited with this It encloses.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of nitride strengthening ODS steel, which is characterized in that by weight percentage, ingredient is as follows:
C :≤0.03%, Si :≤0.5%, Mn:0.6~1.5%, Cr:8.0~15.0%, W :≤1.5%, Mo :≤1.5%, (W+Mo): 1.0~1.5%, Nb:0.02~0.06%, Ta:0.05~0.15%, (Nb+Ta): 0.10~0.15%, V:0.15 ~0.30%, 0.05%≤Y2O3≤ 0.5%, N:0.02~0.08%, Co :≤0.05%, Ni :≤0.01%, Al: < 0.01%, Ti: < 0.005%, Cu: < 0.01%, P < 0.010%, S < 0.005%, Fe surplus；Existed by controlling carbon content 0.03% hereinafter, avoid the formation of high temperature it is long when service condition under the M that is easily roughened23C6Carbide, M are mainly Cr or Fe, and only by Strengthen with the nanoscale nitride and oxide synergy of thermal stability and Dispersed precipitate, thus to obtain excellent high temperature microstructure heat Stability and excellent anti-radiation performance.
2. nitride strengthening ODS steel according to claim 1, which is characterized in that it organizes to be ferrite or martensite group It knits, the size for the nanoscale nitride being distributed thereon is between 10~50nm, and number density is 1021~1022The number of a/cubic meter Magnitude, and the size of nano-oxide particles in 20nm hereinafter, number density is 1023The order of magnitude of a/cubic meter.
3. by the preparation method of nitride strengthening ODS steel described in one of claim 1~2, which is characterized in that the nitride is strong The preparation process for changing ODS steel includes: master alloy smelting → powder atomization → high-energy ball milling → powder jacket pumping → hot isostatic pressing Curing molding → hot rolling → heat treatment, it is final to obtain required tissue；
By weight percentage, the master alloy ingredient of nitride strengthening ODS steel are as follows: C :≤0.005%；Si :≤0.5%；Mn: 0.6~1.5%；Cr:8.0~15.0%；W :≤1.5%；Mo :≤1.5%；(W+Mo): 1.0~1.5%；Nb:0.02~ 0.06%；Ta:0.05~0.15%；(Nb+Ta): 0.10~0.15%；V:0.15~0.30%；N:0.02~0.08%；Co: ≤ 0.05%；Ni :≤0.01%；Al: < 0.01%；Ti: < 0.005%；Cu: < 0.01%；P < 0.010%, S < 0.005%；Fe Surplus；It writes a Chinese character in simplified form are as follows: Fe-0C- (8~15) Cr-1.25 (W+Mo) -0.20V-0.12 (Ta+Nb) -1.0Mn.
4. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that Fe-0C- (8~15) Cr- In 1.25 (W+Mo) -0.20V-0.12 (Ta+Nb) -1.0Mn master alloys, Mn, Ta element are easy scaling loss element, need to be by 90~93% Recovery rate carries out ingredient, and Mn, Ta element are added in refining, and refining time is 10~30min, during which stirs 3~5 times.
5. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that master alloy powder atomization is wanted Ask as follows: granularity<40 μm, atomization pressure>3.5MPa, the degree of superheat>200 DEG C, protective atmosphere be bulk purity 99.99% with On argon gas.
6. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that in order to make partial size 20~ The Y of 50nm2O3Nano particle even dispersion is distributed in master alloy powder, and high-energy-milling state modulator is as follows: milling atmosphere For the argon gas of 99.99% or more bulk purity, ball material mass ratio is (5~10): 1,40~60h of Ball-milling Time, revolving speed is 350~ 500r/min。
7. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that in order to remove powder particle The gas of adsorption reduces porosity, and the air aspiration process of powder jacket is as follows: vacuum degree 10-1Pa, temperature are 400~500 DEG C, the time is 3~5h.
8. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that heat of powder jacket etc. is quiet Cured moulding process is as follows: pressure is 120~150MPa, and temperature is 1000~1200 DEG C, and the heat-insulation pressure keeping time is 3~5h.
9. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that solid in order to further increase The consistency and mechanical property of nitride strengthening ODS steel after chemical conversion type, hot rolling technology control are as follows: start rolling temperature for 1100~ 1200 DEG C, finishing temperature is 900~950 DEG C, and rolling pass is 5~6 times.
10. the preparation method of nitride strengthening ODS steel according to claim 3, which is characterized in that nitride strengthening ODS Heat-Treatment of Steel technology controlling and process is as follows: normalizing process parameter is that 1050~1200 DEG C of 60~90min of heat preservation are air-cooled, tempering process ginseng Number is that 750~800 DEG C of 90~120min of heat preservation are air-cooled.
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