CN106756434B - Oxide dispersion intensifying low activation ferrite/martensite steel and its smelting process - Google Patents

Oxide dispersion intensifying low activation ferrite/martensite steel and its smelting process Download PDF

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CN106756434B
CN106756434B CN201611102765.1A CN201611102765A CN106756434B CN 106756434 B CN106756434 B CN 106756434B CN 201611102765 A CN201611102765 A CN 201611102765A CN 106756434 B CN106756434 B CN 106756434B
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purity
oxide dispersion
low activation
martensite steel
smelting process
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CN106756434A (en
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战东平
邱国兴
蔡南
刘越
葛启桢
杨永坤
刘志明
孟沈童
姜周华
李长生
张慧书
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/006—Making ferrous alloys compositions used for making ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/18—Electroslag remelting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/004—Dispersions; Precipitations
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/005—Ferrite
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

A kind of oxide dispersion intensifying low activation ferrite/martensite steel and its smelting process smelting process, belong to special steel metallurgical technology field.The raw material for including and its mass percent are：It is electrolysed chromium (8.9~9.1%), electrolytic manganese (0.4~0.5%), HIGH-PURITY SILICON (0.05~0.08%), high purity graphite (0.08~0.12%), tungsten (1.4~1.6%), metal tantalum (0.1%), vanadium metal (0.18~0.22%), titanium sponge (0.1~0.25%), high-purity rare-earth yttrium (0.2~0.5%), iron scale (1%), surplus is high-purity low-sulphur hematite iron.Preparation method includes：ODS RAFM are made in stock, vacuum induction melting, casting, forging and electroslag remelting process, with consistency high, ingredient uniformly, energy consumption less, purity is high, smelting process is stable, meets big specification ODS steel needed for large nuclear-power equipment.

Description

Oxide dispersion intensifying low activation ferrite/martensite steel and its smelting process
Technical field
The invention belongs to special steel metallurgical technology field, more particularly to a kind of oxide dispersion intensifying low activation ferrite/ Martensite steel and its smelting process.
Background technology
In Section IX generation, has been arrived in the development of nuclear energy, and working environment in reactor becomes harsher, material especially the One wall/cladding materials is the critical problem for realizing forth generation nuclear reactor " efficiently, safety, economy " operation.Low activation iron element Body/martensite steel (RAFM) is because it is with lower void swelling rate, coefficient of thermal expansion and higher heat-conductivity and good machine Tool performance, is chosen as the preferred structure candidate material of fusion reactor covering, these materials have higher at 300~500 DEG C Thermal conductivity and anti-neutron irradiation damage ability.But its elevated temperature strength is insufficient (operation maximum temperature is only capable of reaching 550 DEG C) and The shortcomings of helium is crisp is easy tod produce, significantly limits it in the key portion such as the first wall of fusion reactor and Section IV generation fission fast reactor involucrum The use of position.Due to the requirement of low activity, addible alloying element is limited, is difficult merely substantially to carry by the method for alloying Its high performance.
Oxide dispersion intensifying (ODS) is considered as the effective technology for improving materials'use temperature range, to improve RAFM The elevated temperature strength of steel, in recent years countries in the world scientist begin one's study in low activation ferrite/martensite steel (RAFM) matrix Middle addition Y2O3Prepare oxide dispersion intensifying low activation ferrite/martensite steel (ODS-RAFM).Nanometer precipitated phase is (rich in steel Y-Ti-O phases) there is strong pinning effect to dislocation, it is remarkably improved the elevated temperature strength and high temperature creep strength of material, simultaneously Y2O3The vacancy or He atoms that irradiation generates can be captured, is damaged caused by reducing irradiation.The standby key of ODS steels is will be tiny Oxide particle be dispersed in matrix, the oxide dispersion intensifying low activation horse that Chinese patent CN101328562A is announced Family name's body Steel material and preparation method thereof is by CLAM comminuted steel shots, Y2O3Powder and Ti powder are placed in degasification in sealing container after evenly mixing, thereafter The mechanical alloying under high-purity argon gas protection, isostatic pressed or hot pressed sintering densification molding, then carry out hot extrusion or forging are rolled The machine-shapings such as system prepare required proximate matter.The alloy of preparation, which has, resists strong neutron irradiation, high-temperature behavior excellent and low activation etc. is special Point.The method for preparing nitrogenous ODS nickel-less austenitics alloy with mechanical alloying method that Chinese patent CN102828097A is announced, with The simple metal element powders and nanometer Y of Fe, Cr, Mn, W, Ti, Al2O3Powder presses Cr：17~20%, Mn：18~22%, W：1.5 ~2.5%, Al：2~4%, Ti：0.5~1.0%, Y2O3：0.3-0.6%, surplus mix for Fe, are packed into horizontal planetary formula high energy Mechanical alloying is carried out in ball mill, sintering thereafter obtains nitrogenous ODS nickel-less austenitics alloy, can largely improve nothing Austenitic stainless steel service ability in a high temperauture environment.
The technique of the above mechanical alloying prepares ODS steel, can improve the high-temperature behavior of alloy to a certain extent, but by It is more in the mechanical alloying equipment difference of use and the technological parameter that need to control, cause the stabilization of current mechanical alloying technique Property and reproducibility it is poor, be hardly formed unified operation standard and realize large-scale production.And there is intrinsic powder for the technique It is easy to pollute with oxidation and the problems such as finished product compactness is low, defect is more, it is difficult to prepare, cleanliness factor is identical, tissue is identical with performance Steel.Lack big machinery alloying and former simultaneously, keeps the industrial applications of ODS steel hindered.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of oxide dispersion intensifying low activation ferrite/martensite steel (ODS-RAFM) and its ODS- is made by stock, vacuum induction melting, cast, forging and electroslag smelting process in smelting process RAFM is high with purity, smelting process is stable, meets big specification ODS steel needed for large nuclear-power equipment.
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (8.9~9.1%), electrolytic manganese (0.4~0.5%), HIGH-PURITY SILICON (0.05~0.08%), high purity graphite (0.08~ 0.12%), tungsten (1.4~1.6%), metal tantalum (0.1%), vanadium metal (0.18~0.22%), titanium sponge (0.1~ 0.25%), high-purity rare-earth yttrium (0.2~0.5%), iron scale (1%), surplus are high-purity low-sulphur hematite iron.
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
The iron scale, ensure that has enough oxygen contents in alloy.
The titanium sponge and rare-earth yttrium of addition, ensure that can generate effective particle Y in molten steel2TiO5And/or Y2Ti2O7。
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are mixed, vacuum refining is carried out, obtains Refractory metal melt；1~3min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, vanadium metal, Titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then 5~10min of alloying, obtain alloy melt；Its In, the technological parameter of vacuum refining is that vacuum degree is 5~10Pa, and refining time is 50~60min；
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 50 ~60 DEG C；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 190~210 DEG C, is air-cooled to room temperature, obtained cold But the ingot casting after, wherein the cooling velocity of Slow cooling is controlled in 10~20 DEG C/min.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1~1.5h at 1100~1200 DEG C, and steel ingot is forged to Φ The rod iron of (45~60) cm；
Step 5, electroslag remelting
It using rod iron as the electrode of electroslag remelting, under protection of argon gas, is refined using electro-slag re-melting method, oxygen is made Compound dispersion-strengtherning low activation ferrite/martensite steel；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system is ternary slag System：CaF2∶Al2O3∶Y2O3=7: 3: (0.1~0.2)；Crystallizer leaving water temperature：35~40 DEG C.
In the step 1, the rare-earth yttrium is using preceding removal surface oxide layer, it is therefore intended that, after preventing addition Cause molten steel sticky.
In the step 2, the purpose of the vacuum refining is, ensures in refractory metal fusing and removal alloy Gas.
In the step 2, the device of the vacuum melting is vaccum sensitive stove, and method is that material is placed in vacuum sense It answers in the crucible of stove.
In the step 3, the purpose of the Slow cooling is, prevents crack due to thermal stress from occurring causing forge crack phenomenon Occur.
In the step 4, the forging, 1100~1200 DEG C of starting forging temperature, 900~1150 DEG C of final forging temperature.
In the step 5, the equipment of electroslag remelting is electroslag furnace.
In the step 5, in the electro-slag re-melting method, electric current is smelted：2000~2750A；Smelt voltage：40~ 50V；Wherein, electric current I=S (55/d are smeltedElectrode+ 0.05), I is electric current, and S is the cross sectional area (mm of consutrode2), dElectrode For electrode diameter (cm).
In the step 5, the quantity of slag is the 0.2~0.5% of electrode quality.
In smelting process, the purpose of vacuum induction melting is that 10 are generated in steel using DIRECT ALLOYING technique12~1013 A/m3Micron order and 1019~1021A/m3Nanoscale Y-Ti-O phase particles, the purpose of electroslag remelting is micron order in removal steel Y-Ti-O phases make to remain nanoscale Y-Ti-O phases in steel.
A kind of oxide dispersion intensifying low activation ferrite/martensite steel and its smelting process of the present invention, compared to existing There are the technology, advantage to be：
1. the oxide dispersion intensifying low activation ferrite/martensite steel of the present invention, iron scale is added in raw material, ensure that There are enough oxygen contents in alloy, is 200~300 × 10-6；
2. in the smelting process of the present invention, rare-earth yttrium is removed into surface oxide layer, it is viscous to effectively reduce the molten steel after melting Degree；Vacuum melting technique adds the segmentation smelting technology of other raw material meltings using the raw material elder generation melting being unlikely to be burnt, and ensures Refractory metal melts, and eliminates the gas in alloy.
3. in the smelting process of the present invention, vacuum induction technique makes to generate a large amount of microns and the effective particle of nanoscale in steel (Y2TiO5Or Y2Ti2O7), electroslag remelting process removes the nanometer particle in micro-size particles reservation steel in steel, ensure that tiny Oxide particle be dispersed in matrix, the oxide dispersion intensifying low activation ferrite/martensite steel of preparation, which has, to be caused The advantages that density is high, ingredient is uniform, energy consumption is few.
Specific implementation mode
Technical scheme of the present invention is described further with reference to specific embodiment.
Embodiment 1
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (8.9%), electrolytic manganese (0.48%), HIGH-PURITY SILICON (0.06%), high purity graphite (0.11%), tungsten (1.45%), gold Belong to tantalum (0.1%), vanadium metal (0.19%), titanium sponge (0.15%), high-purity rare-earth yttrium (0.3%), iron scale (1%), it is remaining Amount is high-purity low-sulphur hematite iron；
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are placed in vaccum sensitive stove crucible, very Sky refining, obtains refractory metal melt；2min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, Vanadium metal, titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then alloying 5min, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is vacuum degree 8Pa, refining time 55min；
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 55 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 200 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 15 DEG C/min.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1h at 1200 DEG C, and starting forging temperature is 1250 DEG C, final forging temperature 1150 DEG C, steel ingot is forged to the rod iron of Φ 45cm；
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, in electroslag furnace, under argon gas protection, essence is carried out using electro-slag re-melting method Oxide dispersion intensifying low activation ferrite/martensite steel is made in refining；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system For ternary slag system：CaF2∶Al2O3∶Y2O3=7: 3: 0.15；The quantity of slag is controlled by the 0.25% of electrode quality；Smelt electric current：I= 2000A；Smelt voltage：45V；Crystallizer leaving water temperature：38℃.
Embodiment 2
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (8.9%), electrolytic manganese (0.5%), HIGH-PURITY SILICON (0.08%), high purity graphite (0.12%), tungsten (1.6%), metal Tantalum (0.1%), vanadium metal (0.18%), titanium sponge (0.25%), high-purity rare-earth yttrium (0.25%), iron scale (1%), surplus For high-purity low-sulphur hematite iron；
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are placed in vaccum sensitive stove crucible, very Sky refining, obtains refractory metal melt；1min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, Vanadium metal, titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then alloying 10min, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is vacuum degree 10Pa, refining time 60min；
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 60 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 190 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 20 DEG C/min.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1.5h at 1100 DEG C, and starting forging temperature is 1150 DEG C, final forging temperature It is 900 DEG C, steel ingot is forged to the rod iron of Φ 50cm；
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, in electroslag furnace, under argon gas protection, essence is carried out using electro-slag re-melting method Oxide dispersion intensifying low activation ferrite/martensite steel is made in refining；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system For ternary slag system：CaF2∶Al2O3∶Y2O3=7: 3: 0.1；The quantity of slag is controlled by the 0.2% of electrode quality；Smelt electric current：I= 2250A；Smelt voltage：50V；Crystallizer leaving water temperature：40℃.
Embodiment 3
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (9.1%), electrolytic manganese (0.5%), HIGH-PURITY SILICON (0.08%), high purity graphite (0.08%), tungsten (1.4%), metal Tantalum (0.1%), vanadium metal (0.22%), titanium sponge (0.20%), high-purity rare-earth yttrium (0.40%), iron scale (1%), surplus For high-purity low-sulphur hematite iron；
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are placed in vaccum sensitive stove crucible, very Sky refining, obtains refractory metal melt；3min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, Vanadium metal, titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then alloying 7min, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is vacuum degree 5Pa, refining time 50min；
In the step 2, the purpose of the vacuum refining is, ensures in refractory metal fusing and removal alloy Gas.
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 50 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 210 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 10 DEG C/min.
In the step 3, the purpose of the Slow cooling is, prevents crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1h at 1200 DEG C, and starting forging temperature is 1150 DEG C, final forging temperature 90 DEG C, steel ingot is forged to the rod iron of Φ 45cm；
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, in electroslag furnace, under argon gas protection, essence is carried out using electro-slag re-melting method Oxide dispersion intensifying low activation ferrite/martensite steel is made in refining；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system For ternary slag system：CaF2∶Al2O3∶Y2O3=7: 3: 0.2；The quantity of slag is controlled by the 0.5% of electrode quality；Smelt electric current：I= 2750A；Smelt voltage：40V；Crystallizer leaving water temperature：35℃.
Embodiment 4
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (9.1%), electrolytic manganese (0.4%), HIGH-PURITY SILICON (0.05%), high purity graphite (0.08%), tungsten (1.4%), metal Tantalum (0.1%), vanadium metal (0.22%), titanium sponge (0.10%), high-purity rare-earth yttrium (0.20%), iron scale (1%), surplus For high-purity low-sulphur hematite iron；
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are placed in vaccum sensitive stove crucible, very Sky refining, obtains refractory metal melt；2min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, Vanadium metal, titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then alloying 7min, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is vacuum degree 6Pa, refining time 55min；
In the step 2, the purpose of the vacuum refining is, ensures in refractory metal fusing and removal alloy Gas.
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 55 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 200 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 15 DEG C/min.
In the step 3, the purpose of the Slow cooling is, prevents crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1h at 1200 DEG C, and starting forging temperature is 1150 DEG C, final forging temperature 90 DEG C, steel ingot is forged to the rod iron of Φ 45cm；
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, in electroslag furnace, under argon gas protection, essence is carried out using electro-slag re-melting method Oxide dispersion intensifying low activation ferrite/martensite steel is made in refining；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system For ternary slag system：CaF2∶Al2O3∶Y2O3=7: 3：0.2；The quantity of slag is controlled by the 0.5% of electrode quality；Smelt electric current：I= 2750A；Smelt voltage：40V；Crystallizer leaving water temperature：35℃.
Embodiment 4
A kind of oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electricity Xie Ge (9.1%), electrolytic manganese (0.4%), HIGH-PURITY SILICON (0.05%), high purity graphite (0.08%), tungsten (1.4%), metal Tantalum (0.1%), vanadium metal (0.22%), titanium sponge (0.25%), high-purity rare-earth yttrium (0.50%), iron scale (1%), surplus For high-purity low-sulphur hematite iron；
In the raw material, ingredient and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows：S≤ 0.005%, P≤0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, includes the following steps：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium Remove surface oxide layer；
Step 2, vacuum induction melting
Crome metal, tungsten, metal tantalum, graphitic carbon, iron scale and high purity iron are placed in vaccum sensitive stove crucible, very Sky refining, obtains refractory metal melt；2min at timed intervals, successively into refractory metal melt be added HIGH-PURITY SILICON, electrolytic manganese, Vanadium metal, titanium sponge, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then alloying 7min, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is vacuum degree 6Pa, refining time 55min；
In the step 2, the purpose of the vacuum refining is, ensures in refractory metal fusing and removal alloy Gas.
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 55 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 200 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 15 DEG C/min.
In the step 3, the purpose of the Slow cooling is, prevents crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1h at 1200 DEG C, and starting forging temperature is 1150 DEG C, final forging temperature 90 DEG C, steel ingot is forged to the rod iron of Φ 45cm；
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, in electroslag furnace, under argon gas protection, essence is carried out using electro-slag re-melting method Oxide dispersion intensifying low activation ferrite/martensite steel is made in refining；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system For ternary slag system：CaF2∶Al2O3∶Y2O3=7: 3: 0.2；The quantity of slag is controlled by the 0.5% of electrode quality；Smelt electric current：I= 2750A；Smelt voltage：40V；Crystallizer leaving water temperature：35℃.

Claims (5)

1. a kind of smelting process of oxide dispersion intensifying low activation ferrite/martensite steel, which is characterized in that including following step Suddenly：
Step 1, it stocks up
By the component proportion of oxide dispersion intensifying low activation ferrite/martensite steel, raw material is weighed, wherein rare-earth yttrium removes Surface oxide layer；
The oxide dispersion intensifying low activation ferrite/martensite steel, including raw material and its mass percent be：Electrolysis It is 0.4 ~ 0.5%, HIGH-PURITY SILICON be 0.05 ~ 0.08%, high purity graphite is 0.08 ~ 0.12%, tungsten that chromium, which is 8.9 ~ 9.1%, electrolytic manganese, Be 0.18 ~ 0.22% for 1.4 ~ 1.6%, metal tantalum 0.1%, vanadium metal, titanium sponge be 0.1 ~ 0.25%, high-purity rare-earth yttrium be 0.2 ~ 0.5%, iron scale 1%, surplus are high-purity low-sulphur hematite iron；
The ingredient and its mass percent that the high-purity low-sulphur hematite iron contains require as follows：S≤0.005%、P≤ 0.01%, Al≤0.01%, Fe >=99.9%, surplus are impurity, impurity≤0.08%；
Step 2, vacuum induction melting
Electrolysis chromium, tungsten, metal tantalum, high purity graphite, iron scale and high-purity low-sulphur hematite iron are mixed, vacuum fine is carried out Refining, obtains refractory metal melt；HIGH-PURITY SILICON, electrolytic manganese, gold is added in 1 ~ 3min at timed intervals into refractory metal melt successively Belong to vanadium, titanium sponge, high-purity rare-earth yttrium and carries out alloying, after high-purity rare-earth yttrium is added, then 5 ~ 10min of alloying, it is molten to obtain alloy Body；Wherein, the technological parameter of vacuum refining is that vacuum degree is 5 ~ 10Pa, and refining time is 50 ~ 60min；
Step 3, it casts
Under argon atmosphere, alloy melt is cast, obtains ingot casting, wherein cast degree of superheat control is 50 ~ 60 ℃；
After the completion of casting, ingot casting is placed in holding furnace after slowly cooling to 190 ~ 210 DEG C, room temperature is air-cooled to, after being cooled down Ingot casting, wherein the cooling velocity of Slow cooling is controlled in 10 ~ 20 DEG C/min；
Step 4, it forges
By ingot casting after cooling, High temperature diffusion homogenizes 1 ~ 1.5h at 1100 ~ 1200 DEG C, and steel ingot is forged to Φ (45 ~ 60) The rod iron of cm；
Step 5, electroslag remelting
It using rod iron as the electrode of electroslag remelting, under protection of argon gas, is refined using electro-slag re-melting method, oxide is made Dispersion-strengtherning low activation ferrite/martensite steel；Wherein, the technological parameter of electroslag remelting is：Electroslag slag system is ternary slag system： CaF2：Al2O3：Y2O3=7：3：(0.1~0.2)；Crystallizer leaving water temperature：35~40℃.
2. the smelting process of oxide dispersion intensifying low activation ferrite/martensite steel as described in claim 1, feature exist In in the step 2, the device of the vacuum induction melting is vaccum sensitive stove, and method is that material is placed in vacuum sense It answers in the crucible of stove.
3. the smelting process of oxide dispersion intensifying low activation ferrite/martensite steel as described in claim 1, feature exist In, in the step 4, the forging, 1100 ~ 1200 DEG C of starting forging temperature, 900 ~ 1150 DEG C of final forging temperature.
4. the smelting process of oxide dispersion intensifying low activation ferrite/martensite steel as described in claim 1, feature exist In in the step 5, the equipment of electroslag remelting is electroslag furnace.
5. the smelting process of oxide dispersion intensifying low activation ferrite/martensite steel as described in claim 1, feature exist In, in the step 5, in the electro-slag re-melting method, smelting electric current：2000~2750A；Smelt voltage：40~50V；Its In, smelt electric current I=S (55/dElectrode+ 0.05), I is electric current, and S is the cross sectional area of consutrode, unit mm2, dElectrodeFor Electrode diameter, unit cm.
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