CN106148659A - A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel - Google Patents

A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel Download PDF

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CN106148659A
CN106148659A CN201510184625.2A CN201510184625A CN106148659A CN 106148659 A CN106148659 A CN 106148659A CN 201510184625 A CN201510184625 A CN 201510184625A CN 106148659 A CN106148659 A CN 106148659A
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low activation
martensite steel
activation ferrite
fine grained
ferrite
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陈胜虎
戎利建
闫德胜
姜海昌
王本贤
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The invention discloses the preparation technology of a kind of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel, belong to low activation ferrite/martensite rings territory.The present invention rotates swaging deformation technique by introducing, both the purpose of crystallite dimension refinement had been achieved, refine again carbide size and improve the even distribution of carbide, the dislocation pile up that deformation causes is eliminated afterwards, it is achieved the preparation of high-strength plasticity low activation ferrite/martensite steel by annealing.The dispersion-strengthened action of this technology utilization Ultra-fine Grained and tiny carbide improves the intensity of material, and utilization simultaneously is uniformly distributed carbide and causes the improvement of strain hardening capacity to improve the plasticity of material.The strong plasticity of the Ultra-fine Grained low activation ferrite/martensite steel of the present invention is significantly improved, and can be that Nuclear Power Industry prepares novel high-strength plasticity low activation ferrite/martensite steel.

Description

A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel
Technical field:
The present invention relates to low activation ferrite/martensite rings territory, specifically a kind of high-strength plasticity Ultra-fine Grained is low The preparation technology of activation ferrite/martensite steel.
Background technology:
Low activation ferrite/martensite steel has excellent thermophysical property and ripe technical foundation, is generally recognized For being the main candidate material of following nuclear reactor construction.Low activation ferrite/martensite steel is due to its Service Environment For strong radiation environment, long-term irradiation can cause the embrittlement of ferrite/martensite steel, therefore have influence on the mechanicalness of steel Energy and fracture behaviour.Recent studies have found that, compared with traditional coarse grain material, nanometer and submicron material have Preferably anti-radiation performance, shows good application prospect in Nuclear Power Industry.
At present, by severe plastic deformation, crystal grain is refined to nanometer or sub-micrometer scale, densification can be prepared Block nanometer/submicrometer structure material, thus of great interest.But, nanometer prepared by these methods / submicron material because of the shortcomings such as plasticity deterioration, complicated process of preparation, overall dimensions be limited are difficult to industrialization should With.Therefore, in relatively large body material, how to obtain nanometer or submicrometer structure, and how to obtain have good The nanometer of good obdurability coupling or submicron material are the problems needing to solve.
Summary of the invention:
It is an object of the invention to provide a kind of block body ultrafine grain low activation ferrite/martensite preparing large-size The method of steel, utilizes and rotates swaging deformation and make annealing treatment the method combined, by crystallite dimension and carbide Refinement, and improve carbide even distribution, improve the strong of low activation ferrite/martensite steel simultaneously Degree and plasticity, overcome the shortcoming that super fine crystal material plasticity deteriorates.
To achieve these goals, technical scheme is as follows:
A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel, including melting, forging, Heat treatment, rotate swaging deformation and annealing, specifically include following steps:
1) by after raw material melting ingot casting, solution treatment, forging and heat treatment are carried out successively, described heat treated Cheng Wei: the sample after forging is carried out Quenching Treatment at 1000~1150 DEG C, is incubated 0.5~2h, take out shrend; Then, carry out temper at 700~800 DEG C, be incubated 1~3h, take out air cooling to room temperature;
2) swaging deformation is rotated: by step 2) sample after heat treatment is processed into cylindric, at accurate swager On carry out shunting time controllable deforming, every time deformation amount controlling is 5%~20%, and total deformation is 80%~95%;
3) annealing: the sample after rotating swaging deformation makes annealing treatment at 650~750 DEG C, insulation 10~30min, take out air cooling to room temperature.
Above-mentioned steps 1) in, described fusion process is according to the change of low activation ferrite/martensite steel by raw material Study and point carry out dispensing, load CaO crucible, use vacuum induction melting ingot casting;By weight percentage, institute The chemical composition stating low activation ferrite/martensite steel is: carbon: 0.08~0.14%, chromium: 8.5~9.5%, tungsten: 1.5~2.0%, vanadium: 0.2~0.3%, tantalum: 0.05~0.15%, manganese: 0.4~0.6%, silicon: 0~0.3%, surplus is Ferrum and inevitable impurity.
Above-mentioned steps 1) in, described solution treatment process is: ingot casting is heated to 1050~1150 DEG C and is incubated 1~3h;Described forging process is: is placed on swager by gained sample after solution treatment and forges, then Air cooling is to room temperature, and cogging forging temperature is 1050~1150 DEG C, and final forging temperature is more than 900 DEG C.
The high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel that the present invention is prepared according to above-mentioned technique, its crystal grain Size range is 100~400nm, and carbide is uniformly distributed in matrix, and carbide size scope is 10~80nm.
Elongation percentage >=28.0% of described low activation ferrite/martensite steel, yield strength >=590MPa, tension is strong Degree >=760MPa.
The design philosophy of the present invention is:
The present invention rotates swaging deformation technique by introducing, and had both achieved the purpose of crystallite dimension refinement, and had refined again Carbide size and improve the even distribution of carbide, eliminates deformation by annealing afterwards and causes Dislocation pile up, it is achieved the preparation of high-strength plasticity low activation ferrite/martensite steel.Utilize Ultra-fine Grained and tiny carbon The dispersion-strengthened action of compound improves the intensity of material, and utilization is uniformly distributed carbide and causes strain hardening capacity Improvement improve the plasticity of material.
Present invention have the advantage that
1, invention significantly improves the mechanical property of low activation ferrite/martensite steel.Utilize and rotate forging and stamping change The method that shape and annealing combine prepares the equally distributed ultrafine-grained (UFG) microstructure of tiny carbide so that material Intensity and plasticity be improved significantly, while plasticity preferably (elongation percentage is more than 28.0%), have relatively High intensity (, at more than 590MPa, tensile strength is up to more than 760MPa for yield strength).
2, the present invention uses rotation swaging deformation and the group technology of annealing, and preparation method is simple.By control Processing parameters processed and heat treating regime, can prepare the Ultra-fine Grained low activation ferrite/geneva of high-strength plasticity Body steel.
Accompanying drawing illustrates:
Fig. 1 is the microstructure picture of low activation ferrite/martensite steel before present invention process processes;Wherein, (a) Crystallite dimension and distribution of carbides (scanning electron microscopic observation 8000 ×);Carbide (transmission electron microscope between (b) lath Observe 38000 ×).
Fig. 2 is low activation ferrite/martensite steel microstructure picture after processing through present invention process;Its In, (a) distribution of carbides (scanning electron microscopic observation 8000 ×);(b) crystallite dimension and distribution of carbides (transmission Electron microscopic observation 80000 ×).
Fig. 3 is the engineering stress-strain before and after processing through present invention process of the low activation ferrite/martensite steel Curve.
Detailed description of the invention:
Embodiment 1
Using ingot iron, crome metal, tungsten, vanadium, smooth and manganese is raw material, prepares by mass fraction (wt.%) The chemical composition of alloy is: C:0.11%, Cr:8.86%, W:1.62%, V:0.24%, Ta:0.11%, Mn: 0.45%, Si:0.05%, surplus is the alloy of Fe.
Concrete production craft step is as follows:
1) melting: the raw material of preparation is loaded CaO crucible, melting in vaccum sensitive stove, and is cast into casting Ingot, after ingot casting solidifies completely, die sinking is taken out;
2) solution treatment: ingot casting is heated to 1100 DEG C and carries out solution treatment, be incubated 2h;
3) forging: by step 2) sample be placed on rapidly on swager and forge, then air cooling is to room temperature, Cogging forging temperature about 1050 DEG C, final forging temperature is more than 900 DEG C;After cogging forging, excise rising head, finally It is forged into the thick sheet material of 30mm;
4) heat treatment: the alloy after forging is carried out Quenching Treatment at 1050 DEG C, is incubated 1h, takes out rapid water Quench;Then, carry out temper at 750 DEG C, be incubated 2h, take out air cooling to room temperature;
5) rotate swaging deformation: by step 4) alloy be processed into the cylindric sample of a diameter of 20mm, Carrying out shunting time controllable deforming on accurate swager, every time deformation amount controlling is 10%, and total deformation is 90%, Wherein, deflection=(deforming sectional area after starting section is amassed-deformed)/deformation starting section is amassed;
6) annealing: the alloy after rotating swaging deformation makes annealing treatment at 700 DEG C, is incubated 30min, Take out air cooling to room temperature.
Fig. 2 is the micro-organization chart of low activation ferrite/martensite steel after present invention process processes, from figure 2 (a) is it can be seen that tiny carbide is uniformly distributed in the base;The crystallite dimension of alloy is understood more by Fig. 2 (b) Uniformly, crystallite dimension is 200~300nm, and carbide size is 50~70nm, and is uniformly distributed in the base. And without present invention process process alloy microscopic structure (in addition to rotating swaging deformation and annealing treating process, its Remaining all techniques are all identical with case study on implementation 1 with parameter) see Fig. 1, from Fig. 1 (a) it can be seen that its crystal grain chi Very little be about 30 μm, for 100 times of ultra-fine grained ferrite/martensite steel, and carbide be mainly distributed on crystal boundary and Between martensite lath;The size being understood bar-shaped carbide by Fig. 1 (b) is: long axis direction is about 200nm, short axle Direction is about 100nm, much larger than the carbide size of ultra-fine grained ferrite/martensite steel.This significant crystal grain The Dispersed precipitate of refinement and tiny carbide makes the mechanical property of ultra-fine grained ferrite/martensite steel obtain Significantly improve.Before and after present invention process processes, the engineering stress strain curve of ferrite/martensite steel is such as Shown in Fig. 3, it can be seen that the mechanical property of the ultra-fine grained ferrite/martensite steel after the present invention processes is: At the yield strength of 606MPa, the tensile strength of 783MPa and the elongation percentage of 28.0%, relatively present invention process Before reason, the mechanical property of ferrite/martensite steel is greatly improved.
Embodiment 2
Using ingot iron, crome metal, tungsten, vanadium, smooth and manganese is raw material, prepares by mass fraction (wt.%) The chemical composition of alloy is: C:0.12%, Cr:8.79%, W:1.78%, V:0.24%, Ta:0.09%, Mn:0.52%, Si:0.22%, surplus is the alloy of Fe.
Concrete production craft step is as follows:
1) melting: the raw material of preparation is loaded CaO crucible, melting in vaccum sensitive stove, and is cast into casting Ingot, after ingot casting solidifies completely, die sinking is taken out;
2) solution treatment: ingot casting is heated to 1100 DEG C and carries out solution treatment, be incubated 2h;
3) forging: by step 2) sample be placed on rapidly on swager and forge, then air cooling is to room temperature, Cogging forging temperature about 1050 DEG C, final forging temperature is more than 900 DEG C;After cogging forging, excise rising head, finally It is forged into the thick sheet material of 32mm;
4) heat treatment: the alloy after forging is carried out Quenching Treatment at 1030 DEG C, is incubated 1h, takes out rapid water Quench;Then, carry out temper at 740 DEG C, be incubated 2h, take out air cooling to room temperature;
5) rotate swaging deformation: by step 4) sheet fabrication become the cylindric sample of a diameter of 22mm, Carrying out shunting time controllable deforming on accurate swager, every time deformation amount controlling is 6%, and total deformation is 93%; Wherein, deflection=(deforming sectional area after starting section is amassed-deformed)/deformation starting section is amassed;
6) annealing: the alloy after rotating swaging deformation makes annealing treatment at 720 DEG C, is incubated 20min, Take out air cooling to room temperature.
The microscopic structure of the ultra-fine grained ferrite/martensite steel obtained under these process conditions and phase in case study on implementation 1 With, crystallite dimension does not changes significantly, about 200~about 300nm, and carbide size is about 50~70nm, And be uniformly distributed in the base.Ultra-fine grained ferrite/martensite steel bending at the mechanical property of room temperature: 598MPa Take intensity, the tensile strength of 760MPa and the elongation percentage of 28.5%, the front ferrite of relatively present invention process process/ The mechanical property of martensite steel is greatly improved.
The present invention uses rotation swaging deformation and the group technology of annealing, not only prepares the block of large-size Body Ultra-fine Grained low activation ferrite/martensite steel, meets material simultaneously and has the requirement of high-strength plasticity, preparation Ultra-fine Grained low activation ferrite/martensite steel has the mechanical property of excellence.

Claims (7)

1. the preparation technology of a high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel, it is characterised in that: should Preparation technology comprises the steps:
1) by after raw material melting ingot casting, solution treatment, forging and heat treatment are carried out successively, described heat treated Cheng Wei: the sample after forging is carried out Quenching Treatment at 1000~1150 DEG C, is incubated 0.5~2h, take out shrend; Then, carry out temper at 700~800 DEG C, be incubated 1~3h, take out air cooling to room temperature;
2) swaging deformation is rotated: by step 2) sample after heat treatment is processed into cylindric, at accurate swager On carry out shunting time controllable deforming, every time deformation amount controlling is 5%~20%, and total deformation is 80%~95%;
3) annealing: the sample after rotating swaging deformation makes annealing treatment at 650~750 DEG C, insulation 10~30min, take out air cooling to room temperature.
2. according to the preparation work of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 Skill, it is characterised in that: step 1) in, described fusion process is that raw material loads CaO crucible in proportion, Use vacuum induction melting ingot casting.
3. according to the preparation of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 or 2 Technique, it is characterised in that: step 1) in, raw material is according to the chemical composition of low activation ferrite/martensite steel Carry out dispensing;By weight percentage, the chemical composition of described low activation ferrite/martensite steel is: carbon: 0.08~0.14%, chromium: 8.5~9.5%, tungsten: 1.5~2.0%, vanadium: 0.2~0.3%, tantalum: 0.05~0.15%, manganese: 0.4~0.6 %, silicon: 0~0.3%, surplus is ferrum and inevitable impurity.
4. according to the preparation work of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 Skill, it is characterised in that: step 1) in, described solution treatment is ingot casting to be heated to 1050~1150 DEG C and protects Temperature 1~3h.
5. according to the preparation work of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 Skill, it is characterised in that: step 1) in, described forging process is: be placed on by gained sample after solution treatment Forging on swager, then air cooling is to room temperature, and cogging forging temperature is 1050~1150 DEG C, final forging temperature More than 900 DEG C.
6. according to the preparation work of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 Skill, it is characterised in that: through step 3) crystallite dimension of gained low activation ferrite/martensite steel after annealing Scope is 100~400nm, and carbide is uniformly distributed in matrix, and carbide size scope is 10~80nm.
7. according to the preparation work of the high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel described in claim 1 Skill, it is characterised in that: elongation percentage >=28.0% of described low activation ferrite/martensite steel, yield strength >= 590MPa, tensile strength >=760MPa.
CN201510184625.2A 2015-04-17 2015-04-17 A kind of preparation technology of high-strength plasticity Ultra-fine Grained low activation ferrite/martensite steel Pending CN106148659A (en)

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CN106119492A (en) * 2016-08-24 2016-11-16 中国科学院合肥物质科学研究院 A kind of hot-working method of fusion reactor commercial scale low activation martensitic steel sheet material
CN107699810A (en) * 2017-09-30 2018-02-16 中国科学院合肥物质科学研究院 A kind of low activatable structural material and its design method based on various factors coupling
CN107881368A (en) * 2017-11-23 2018-04-06 宁波升鸿机械设备有限公司 A kind of blower fan
CN108754079A (en) * 2018-06-13 2018-11-06 武汉科技大学 It is a kind of to promote the heat treatment method that nano-carbide is precipitated in steel containing W alloy
CN111549294A (en) * 2020-05-25 2020-08-18 中国科学院金属研究所 High-strength Fe-Cr-Zr-W-Mo-B ferrite alloy resistant to liquid lead and bismuth corrosion and preparation method thereof
WO2021147271A1 (en) * 2020-01-23 2021-07-29 清华大学 Interphase-precipitation-enhanced low-activation ferritic steel and preparation method therefor
CN113235014A (en) * 2021-05-06 2021-08-10 中国科学院合肥物质科学研究院 High-performance silicon-containing ferrite/martensite steel
CN114686664A (en) * 2022-02-28 2022-07-01 东北大学 Composite preparation method of high-strength D6A fine-grained steel

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106119492A (en) * 2016-08-24 2016-11-16 中国科学院合肥物质科学研究院 A kind of hot-working method of fusion reactor commercial scale low activation martensitic steel sheet material
CN106119492B (en) * 2016-08-24 2017-11-07 中国科学院合肥物质科学研究院 A kind of hot-working method of fusion reactor commercial scale low activation martensitic steel sheet material
CN107699810A (en) * 2017-09-30 2018-02-16 中国科学院合肥物质科学研究院 A kind of low activatable structural material and its design method based on various factors coupling
CN107699810B (en) * 2017-09-30 2020-01-10 中国科学院合肥物质科学研究院 Low-activation structural material based on multi-factor coupling and design method thereof
CN107881368A (en) * 2017-11-23 2018-04-06 宁波升鸿机械设备有限公司 A kind of blower fan
CN108754079A (en) * 2018-06-13 2018-11-06 武汉科技大学 It is a kind of to promote the heat treatment method that nano-carbide is precipitated in steel containing W alloy
WO2021147271A1 (en) * 2020-01-23 2021-07-29 清华大学 Interphase-precipitation-enhanced low-activation ferritic steel and preparation method therefor
CN111549294A (en) * 2020-05-25 2020-08-18 中国科学院金属研究所 High-strength Fe-Cr-Zr-W-Mo-B ferrite alloy resistant to liquid lead and bismuth corrosion and preparation method thereof
CN113235014A (en) * 2021-05-06 2021-08-10 中国科学院合肥物质科学研究院 High-performance silicon-containing ferrite/martensite steel
CN114686664A (en) * 2022-02-28 2022-07-01 东北大学 Composite preparation method of high-strength D6A fine-grained steel
CN114686664B (en) * 2022-02-28 2023-03-07 东北大学 Composite preparation method of high-strength D6A fine-grained steel

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Application publication date: 20161123