CN106756434A - Low activation ferrite/martensite steel and its smelting process of oxide dispersion intensifying - Google Patents

Low activation ferrite/martensite steel and its smelting process of oxide dispersion intensifying Download PDF

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CN106756434A
CN106756434A CN201611102765.1A CN201611102765A CN106756434A CN 106756434 A CN106756434 A CN 106756434A CN 201611102765 A CN201611102765 A CN 201611102765A CN 106756434 A CN106756434 A CN 106756434A
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purity
oxide dispersion
martensite steel
dispersion intensifying
smelting process
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CN106756434B (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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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/006Making ferrous alloys compositions used for making ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/18Electroslag remelting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/005Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/004Dispersions; Precipitations
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/005Ferrite
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/008Martensite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

A kind of low activation ferrite/martensite steel and its smelting process smelting process of oxide dispersion intensifying, belongs to special steel metallurgical technology field.The raw material for including and its mass percent are:Electrolysis 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%), balance of high-purity low-sulphur hematite iron.Its preparation method includes:Get the raw materials ready, vacuum induction melting, casting, forging and electroslag remelting process, ODS RAFM are obtained, with consistency it is high, composition is uniform, power consumption less, purity is high, smelting process is stable, meet large nuclear-power equipment needed for big specification ODS steel.

Description

Low activation ferrite/martensite steel and its smelting process of oxide dispersion intensifying
Technical field
The invention belongs to special steel metallurgical technology field, more particularly to a kind of low activation ferrite of oxide dispersion intensifying/ Martensite steel and its smelting process.
Background technology
The development of nuclear energy is to IX generations, and it is harsher that the working environment in reactor becomes, 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) has relatively low void swelling rate, thermal coefficient of expansion and higher heat-conductivity and good machine because of it Tool performance, is chosen as the first-selected structure candidate material of fusion reactor covering, and these materials have higher at 300~500 DEG C Thermal conductivity and anti-neutron irradiation damage ability.But its elevated temperature strength is not enough (operation maximum temperature is only capable of reaching 550 DEG C) and The shortcomings of easily producing helium crisp, significantly limit it in the key portion such as the wall of fusion reactor first and iv generation fission fast reactor involucrum The use of position.Due to the requirement of low activity, addible alloying element is limited, and the simple method by alloying is difficult significantly to carry Its performance high.
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 it is low activation ferrite/martensite steel (RAFM) matrix Middle addition Y2O3Prepare low activation ferrite/martensite steel (ODS-RAFM) of oxide dispersion intensifying.Nanometer precipitated phase is (rich in steel Y-Ti-O phases) there is strong pinning effect to dislocation, the elevated temperature strength and high temperature creep strength of material are remarkably improved, while Y2O3Room or He atoms that irradiation is produced can be captured, the damage that irradiation is caused is reduced.The standby key of ODS steels is will be tiny Oxide particle be dispersed in matrix, Chinese patent CN101328562A announce the low activation horse of oxide dispersion intensifying 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 uniformly mixing, thereafter The mechanical alloying under high-purity argon gas protection, isostatic pressed or hot pressed sintering densification shaping, then carry out hot extrusion or forging are rolled The machine-shapings such as system prepare required section bar.The alloy of preparation has the spies such as the excellent and low activation of anti-strong neutron irradiation, high-temperature behavior Point.The method that nitrogenous ODS nickel-less austenitics alloy is prepared 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%, balance of Fe mixing, loads horizontal planetary formula high energy Mechanical alloying is carried out in ball mill, sintering obtains nitrogenous ODS nickel-less austenitics alloy thereafter, can largely improve nothing Austenitic stainless steel service ability in high temperature environments.
The technique of above mechanical alloying prepares ODS steel, can to a certain extent improve the high-temperature behavior of alloy, but by It is more in the mechanical alloying equipment technological parameters that are different and need to controlling for using, cause the stabilization of current mechanical alloying technique Property and reappearance it is poor, be hardly formed unified operation standard and realize large-scale production.And the technique has intrinsic powder The problems such as easily pollution and oxidation and finished product packing are low, defect is more, it is difficult to preparing, cleanliness factor is identical, organize identical with performance Steel.Lack big machinery alloying and former simultaneously, make the industrial applications of ODS steel hindered.
The content of the invention
In order to solve the above problems, the present invention provides a kind of oxide dispersion intensifying low activation ferrite/martensite steel (ODS-RAFM) and its smelting process, by getting the raw materials ready, vacuum induction melting, cast, forging and electroslag smelting process, ODS- is obtained RAFM, with purity is high, smelting process stabilization, meet large nuclear-power equipment needed for big specification ODS steel.
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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%), balance of high-purity low-sulphur hematite iron.
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
Described iron scale, it is ensured that have enough oxygen contents in alloy.
The titanium sponge and rare-earth yttrium of addition, it is ensured that effective particle Y can be generated in molten steel2TiO5And/or Y2Ti2O7
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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, obtained Refractory metal melt;1~3min at timed intervals, successively to added in refractory metal melt 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 is 5~10Pa, and refining time is 50~60min;
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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, obtain cold But the ingot casting after, wherein, the cooling velocity of Slow cooling is controlled in 10~20 DEG C/min.
Step 4, forging
By the ingot casting after cooling, High temperature diffusion homogenizes 1~1.5h at 1100~1200 DEG C, and steel ingot is forged into Φ The rod iron of (45~60) cm;
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, under argon gas protection, refined using electro-slag re-melting method, oxygen is obtained The low activation ferrite/martensite steel of compound dispersion-strengtherning;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 described step 1, described rare-earth yttrium is using preceding removal surface oxide layer, it is therefore intended that, after preventing from adding Cause molten steel sticky.
In described step 2, the purpose of described vacuum refining is, it is ensured that refractory metal is melted and removed in alloy Gas.
In described step 2, the device of described vacuum melting is vaccum sensitive stove, and method is that material is placed in into vacuum sense Answer in the crucible of stove.
In described step 3, the purpose of described Slow cooling is to prevent crack due to thermal stress from occurring causing forge crack phenomenon Occur.
In described step 4, described forging, 1100~1200 DEG C of starting forging temperature, 900~1150 DEG C of final forging temperature.
In described step 5, the equipment of electroslag remelting is electroslag furnace.
In described step 5, in described 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 It is electrode diameter (cm).
In described step 5, the described 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 Individual/m3Micron order and 1019~1021Individual/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.
Low activation ferrite/martensite steel and its smelting process of a kind of oxide dispersion intensifying of the invention, compared to existing There is technology, its advantage is:
1. oxide dispersion intensifying of the invention is low activates ferrite/martensite steel, and raw material adds iron scale, it is ensured that There are enough oxygen contents in alloy, be 200~300 × 10-6
2. in smelting process of the invention, rare-earth yttrium is removed into surface oxide layer, effectively reduce the molten steel after melting and glue 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, it is ensured that Refractory metal melts, and eliminates the gas in alloy.
3. in smelting process of the invention, vacuum induction technique makes to generate a large amount of microns and the effective particle of nanoscale in steel (Y2TiO5Or Y2Ti2O7), micro-size particles retains the nanometer particle in steel in electroslag remelting process removal steel, it is ensured that tiny Oxide particle be dispersed in matrix, the low activation ferrite/martensite steel of the oxide dispersion intensifying of preparation has and causes The advantages of density is high, composition is uniform, power consumption is few.
Specific embodiment
Technical scheme is described further with reference to specific embodiment.
Embodiment 1
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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 Category tantalum (0.1%), vanadium metal (0.19%), titanium sponge (0.15%), high-purity rare-earth yttrium (0.3%), iron scale (1%), it is remaining It is high-purity low-sulphur hematite iron to measure;
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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 to added in refractory metal melt 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, obtain alloy and melt Body;Wherein, the technological parameter of vacuum refining is that vacuum is 8Pa, and refining time is 55min;
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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, forging
By the ingot casting after cooling, the High temperature diffusion homogenization 1h at 1200 DEG C, 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 Refining, is obtained the low activation ferrite/martensite steel of oxide dispersion intensifying;Wherein, the technological parameter of electroslag remelting is:Electroslag slag system It is ternary slag system:CaF2∶Al2O3∶Y2O3=7: 3: 0.15;The quantity of slag presses 0.25% control of electrode quality;Smelt electric current:I= 2000A;Smelt voltage:45V;Crystallizer leaving water temperature:38℃.
Embodiment 2
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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 It is high-purity low-sulphur hematite iron;
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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 to added in refractory metal melt 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, obtain alloy and melt Body;Wherein, the technological parameter of vacuum refining is that vacuum is 10Pa, and refining time is 60min;
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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, forging
By the ingot casting after cooling, the High temperature diffusion homogenization 1.5h at 1100 DEG C, 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 Refining, is obtained the low activation ferrite/martensite steel of oxide dispersion intensifying;Wherein, the technological parameter of electroslag remelting is:Electroslag slag system It is ternary slag system:CaF2∶Al2O3∶Y2O3=7: 3: 0.1;The quantity of slag presses 0.2% control of electrode quality;Smelt electric current:I= 2250A;Smelt voltage:50V;Crystallizer leaving water temperature:40℃.
Embodiment 3
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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 It is high-purity low-sulphur hematite iron;
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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 to added in refractory metal melt 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, obtain alloy and melt Body;Wherein, the technological parameter of vacuum refining is that vacuum is 5Pa, and refining time is 50min;
In described step 2, the purpose of described vacuum refining is, it is ensured that refractory metal is melted and removed in alloy Gas.
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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 described step 3, the purpose of described Slow cooling is to prevent crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, forging
By the ingot casting after cooling, the High temperature diffusion homogenization 1h at 1200 DEG C, 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 Refining, is obtained the low activation ferrite/martensite steel of oxide dispersion intensifying;Wherein, the technological parameter of electroslag remelting is:Electroslag slag system It is ternary slag system:CaF2∶Al2O3∶Y2O3=7: 3: 0.2;The quantity of slag presses 0.5% control of electrode quality;Smelt electric current:I= 2750A;Smelt voltage:40V;Crystallizer leaving water temperature:35℃.
Embodiment 4
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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 It is high-purity low-sulphur hematite iron;
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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 to added in refractory metal melt 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, obtain alloy and melt Body;Wherein, the technological parameter of vacuum refining is that vacuum is 6Pa, and refining time is 55min;
In described step 2, the purpose of described vacuum refining is, it is ensured that refractory metal is melted and removed in alloy Gas.
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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 described step 3, the purpose of described Slow cooling is to prevent crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, forging
By the ingot casting after cooling, the High temperature diffusion homogenization 1h at 1200 DEG C, 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 Refining, is obtained the low activation ferrite/martensite steel of oxide dispersion intensifying;Wherein, the technological parameter of electroslag remelting is:Electroslag slag system It is ternary slag system:CaF2∶Al2O3∶Y2O3=7: 3:0.2;The quantity of slag presses 0.5% control of electrode quality;Smelt electric current:I= 2750A;Smelt voltage:40V;Crystallizer leaving water temperature:35℃.
Embodiment 4
A kind of low activation ferrite/martensite steel of oxide dispersion intensifying, 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 It is high-purity low-sulphur hematite iron;
In described raw material, the composition and its mass percent requirement that high-purity low-sulphur hematite iron contains are as follows:S≤ 0.005%th, P≤0.01%, Al≤0.01%, Fe >=99.9%, balance of impurity, impurity≤0.08%.The conjunction of remaining raw material Golden purity >=99.9%.
A kind of smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying, comprises the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium Removal 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 to added in refractory metal melt 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, obtain alloy and melt Body;Wherein, the technological parameter of vacuum refining is that vacuum is 6Pa, and refining time is 55min;
In described step 2, the purpose of described vacuum refining is, it is ensured that refractory metal is melted and removed in alloy Gas.
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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 described step 3, the purpose of described Slow cooling is to prevent crack due to thermal stress from occurring causing forge crack phenomenon Occur.
Step 4, forging
By the ingot casting after cooling, the High temperature diffusion homogenization 1h at 1200 DEG C, 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 Refining, is obtained the low activation ferrite/martensite steel of oxide dispersion intensifying;Wherein, the technological parameter of electroslag remelting is:Electroslag slag system It is ternary slag system:CaF2∶Al2O3∶Y2O3=7: 3: 0.2;The quantity of slag presses 0.5% control of electrode quality;Smelt electric current:I= 2750A;Smelt voltage:40V;Crystallizer leaving water temperature:35℃.

Claims (8)

1. a kind of oxide dispersion intensifying is low activates ferrite/martensite steel, it is characterised in that the low work of the oxide dispersion intensifying Change ferrite/martensite steel, including raw material and its mass percent be:Electrolysis 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%), oxidation Iron sheet (1%), balance of high-purity low-sulphur hematite iron.
2. oxide dispersion intensifying as claimed in claim 1 is low activates ferrite/martensite steel, it is characterised in that described The composition 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%th, Fe >=99.9%, balance of impurity, impurity≤0.08%;Alloy purity >=99.9% of remaining described raw material.
3. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying described in claim 1, its feature exists In comprising the following steps:
Step 1, gets the raw materials ready
By the component proportion of the low activation ferrite/martensite steel of oxide dispersion intensifying, raw material is weighed, wherein, rare-earth yttrium removal 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, infusibility is obtained Metal bath;1~3min at timed intervals, successively to adding HIGH-PURITY SILICON, electrolytic manganese, vanadium metal, sponge in refractory metal melt Titanium, high-purity rare-earth yttrium carry out alloying, after high-purity rare-earth yttrium is added, then 5~10min of alloying, obtain alloy melt;Wherein, The technological parameter of vacuum refining is that vacuum is 5~10Pa, and refining time is 50~60min;
Step 3, casting
Under argon atmosphere, alloy melt is cast, obtained 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, forging
By the ingot casting after cooling, at 1100~1200 DEG C High temperature diffusion homogenize 1~1.5h, by steel ingot be forged to Φ (45~ 60) rod iron of cm;
Step 5, electroslag remelting
Using rod iron as the electrode of electroslag remelting, under argon gas protection, refined using electro-slag re-melting method, oxide is obtained The low activation ferrite/martensite steel of dispersion-strengtherning;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.
4. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying as claimed in claim 3, its feature exists In in described step 2, the device of described vacuum melting is vaccum sensitive stove, and method is that material is placed in into vaccum sensitive stove Crucible in.
5. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying as claimed in claim 3, its feature exists In, in described step 4, described forging, 1100~1200 DEG C of starting forging temperature, 900~1150 DEG C of final forging temperature.
6. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying as claimed in claim 3, its feature exists In in described step 5, the equipment of electroslag remelting is electroslag furnace.
7. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying as claimed in claim 3, its feature exists In, in described step 5, in described electro-slag re-melting method, smelting electric current: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), dElectrodeIt is electricity Polar diameter (cm).
8. the smelting process of the low activation ferrite/martensite steel of oxide dispersion intensifying as claimed in claim 3, its feature exists In in described step 5, the described quantity of slag is the 0.2~0.5% of electrode quality.
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