CN106825587B - A method of preparing oxide dispersion intensifying ferrous alloy - Google Patents

A method of preparing oxide dispersion intensifying ferrous alloy Download PDF

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CN106825587B
CN106825587B CN201611100574.1A CN201611100574A CN106825587B CN 106825587 B CN106825587 B CN 106825587B CN 201611100574 A CN201611100574 A CN 201611100574A CN 106825587 B CN106825587 B CN 106825587B
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章林
刘烨
单化杰
王道宽
陈晓玮
曲选辉
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University of Science and Technology Beijing USTB
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    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

A method of oxide dispersion intensifying ferrous alloy is prepared, field of metal dispersion reinforcement technology is belonged to.Using iron block, Fe Mn alloys and Ni Al alloys as raw material; pure intermediate alloy ingot casting is obtained by the technique of vacuum melting+electroslag melting duplex; intermediate alloy ingot casting is crushed to obtain intermediate alloy powder in the crusher with protective atmosphere, and intermediate alloy powder obtains oxide dispersion intensifying iron(-)base powder after carrying out high-energy ball milling with matrix powder and oxide powder.Oxide dispersion intensifying iron(-)base powder just obtains final oxide dispersion intensifying ferrous alloy after hot isostatic pressing and heat treatment.The present invention effectively reduces the content of oxygen and nonmetal inclusion in ingot casting, and the intermediate alloy of alloying prevents the oxidation of Mn elements, and can shorten Ball-milling Time, reduces energy consumption.The oxide dispersion intensifying ferrous alloy of preparation is by L21Type Ni2AlMn intermetallic compounds and dispersed oxide mutually common reinforcing.

Description

A method of preparing oxide dispersion intensifying ferrous alloy
Technical field
The invention belongs to field of metal dispersion reinforcement technology, specifically provides and a kind of intermediate alloy is prepared using master alloy method Powder, so the progress mechanical alloying of intermediate alloy powder, matrix powder and oxide powder is strong to obtain dispersed oxide Change the method for iron(-)base powder.
Background technology
By intermetallic compound and Alfer that nano-oxide is strengthened jointly have the γ of similar nickel-base alloy/ The two-phase structure of γ ' is expected to that the temperature in use limit of conventional ferrite heat-resisting alloy and mechanical behavior under high temperature can be improved, in high temperature There is important application prospect in structural material field.Nano-oxide particles have excellent thermal stability and chemical stability, At a temperature of alloy melting point, nano-oxide still can play inhibition to the movement of dislocation, be that dispersed oxide is strong Most important hardening constituent in alloy.(Ni, Fe) Al intermetallic compound phases (β ' phases) are that one kind in ferrous alloy is effective Hardening constituent, it is a kind of long-range order B2The intermetallic compound of structure (CsCl types), fusing point are up to 1638 DEG C, have higher Intensity and hardness.Meanwhile β ' is mutually very close with the lattice constant of ferrite matrix (β), lattice misfit is small, this makes β ' mutually and β It is easy to form coherence orientation relationship between matrix, this creates condition for homogeneous nucleation and disperse the shape precipitation of β ' phases.In alloy Middle addition Mn elements can change the phase structure of intermetallic compound, and intermetallic compound is made to be changed into L2 by NiAl types1Type Ni2AlMn intermetallic compounds, Mn elements can preferentially occupy Al lattices, reduce the strain energy of forming core, make intermetallic compound Number density increase an order of magnitude, and influence of the hardening constituent to ferrous alloy ductility is little.Ni2AlMn intermetallics The reinforcing effect of object is better than single-phase NiAl phases.Try to reduce excessive oxygen content, it is that control is precipitated to shorten Ball-milling Time, reduce energy consumption Phase structure and the key for improving material comprehensive mechanical property.
L2 is being prepared using conventional mechanical alloying technique1Type Ni2AlMn intermetallic compounds and oxide are strengthened jointly Oxide dispersion intensifying ferrous alloy when, Ti and Mn elements are easy to aoxidize in ma process, not only make participation shape At Ni2The Mn elements of AlMn intermetallic compounds are reduced, and cannot achieve the purpose that effectively to control intermetallic compound ingredient.When long Between the mechanical behavior under high temperature that can reduce being mingled with of being readily incorporated of ball milling and the nonmetal inclusion (Al-Mg-O) in raw material material. Meanwhile the oxidation of Ti and Mn elements makes impurity oxygen content increase, and leads to the roughening of dispersed oxide phase.Above-mentioned two factor is all straight The structure and thermal stability for being related to intermetallic compound and oxide are connect, the promotion for strengthening effect is limited.
Invention content
The purpose of the present invention is to provide a kind of methods preparing oxide dispersion intensifying ferrous alloy.Prepared by this method Oxide dispersion intensifying ferrous alloy is by L21Type Ni2AlMn intermetallic compounds and dispersed oxide mutually common reinforcing, utilize two The superposition of the reinforcing effect of kind precipitated phase improves the mechanical behavior under high temperature of material.
The present invention is utilized obtains intermediate alloy ingot casting using the technique of vacuum melting+electroslag melting duplex.In electroslag melting During, consutrode is slowly melted by resistance, is mingled with to create by parameters such as shape, depth, the viscosity of adjusting slag bath The condition that object floats, the money consumption electric shock baton drop after dissolving pass through the slag material layer of melting to react and purified with slag charge, And recrystallized in the bottom of crystallizer, obtain low-sulfur, dense structure, uniform, pure intermediate alloy ingot casting.Intermediate alloy is cast Ingot is crushed to obtain intermediate alloy powder, intermediate alloy powder and matrix powder and oxygen in the crusher with protective atmosphere Compound powder obtains oxide dispersion intensifying iron(-)base powder after carrying out high-energy ball milling.Oxide dispersion intensifying fe-based alloy powder After end is packed into steel capsule, degassing, soldering and sealing processing, hot canned forging consolidation molding is carried out, and be heat-treated, obtain final oxygen Compound dispersion strengthening iron-base alloy.The preparation process flow of oxide dispersion intensifying ferrous alloy is as shown in Figure 1, concrete technology walks Suddenly have:
1, pretreatment of raw material:Using iron block, Fe-Mn alloys, Ni-Al alloys and Fe-Ti alloys as raw material, various raw materials Purity be all higher than 99.9%.Raw metal is pre-processed in 5% aqueous hydrochloric acid solution, removes oxide on surface, pretreatment Time is 25-35min, and 30-90min is dried in processing at 60 DEG C in an oven after alcohol is cleaned.
2, vacuum induction melting+electroslag melting of intermediate alloy:It will be prepared into intermediate alloy by pretreated raw material, in Between in alloy the content of matrix element Fe be 20~40wt.%, remaining is Ni, Al, Ti and Mn alloying element, and intermediate alloy In each alloying element mass ratio it is consistent with the mass ratio of each element in target oxide dispersion strengthening iron-base alloy, desirable oxidation The ingredient of object dispersion strengthening iron-base alloy is:5Ni-1Al-3Mn-0.3Y2O3- 0.3Ti- surpluses Fe.Intermediate alloy is in vacuum induction Melting is carried out in stove, CaO ceramic crucibles is used in fusion process, and increase power after furnace charge is melting down, bath temperature is made to increase To 1600-1700 DEG C, 25-35min is kept the temperature, cools down later, be filled with argon gas, molten steel is cast into intermediate alloy ingot casting;Vacuum sense The ingot casting of melting is answered to carry out inert atmosphere electroslag melting.The ingredient of electroslag remelting slag charge is:15-20%CaO, 15-20%Al2O3, 1-5%TiO2, 1-5%MgO, 3-10%CeO, surplus CaF2.It pours into crystallizer, is powered after slag charge is heated to molten condition After playing electric arc, adjustment remelting voltage is 35-65V, electric current 3000-8000A;Consutrode is slowly melted by resistance, gold after dissolving Belonging to drop passes through the slag material layer of melting to react and purified with slag charge, and is recrystallized in the bottom of crystallizer, obtains Dense structure, uniform, pure electroslag remelting intermediate alloy ingot casting.The oxygen content of intermediate alloy ingot casting is 100ppm, sulfur content For 20ppm.
3, intermediate alloy ingot casting is broken:By intermediate alloy ingot casting surface oxide skin remove, one kind with cooling system with The high-speed disc of protective atmosphere galls to be crushed in crushing device.Broken powder is screened, intermediate alloy powder is obtained.
4, mechanical alloying:Machine is carried out after parent metal powder, intermediate alloy powder and nano-oxide particles are mixed Tool alloying, parent metal powder are Fe powder, nano-oxide Y2O3.It is weighed first, in accordance with alloying component proportioning, and In addition 0.3~0.5wt.% stearic acid is added in mixed-powder as process control agent, to avoid powder in Process During High Energy Ball Milling Caking.By (99.999%) carries out high-energy ball milling, ball milling in high-purity argon gas or hydrogen atmosphere after the premixing uniformly of above-mentioned powder Machine rotating speed is 340~500 revs/min, and Ball-milling Time 30-35h obtains mechanical alloying powder.
5, sintering densification:Mechanical alloying powder is densified using heat and other static pressuring processes, with mild steel to machine Tool alloying powder jacket, then carries out hot isostatic pressing, and hip temperature is 950~1150 DEG C, and pressure is 100~ 200MPa, soaking time are 1~3h;It obtains close to fully dense oxide dispersion intensifying ferrous alloy.
6, it is heat-treated:Hot isostatic pressing oxide dispersion intensifying ferrous alloy carries out two benches heat treatment, is dissolved first Processing, then carries out ageing treatment.Solid solution temperature is 800~1200 DEG C, air-cooled after 2~4h of heat preservation.Aging temperature It is 500~800 DEG C, it is air-cooled after 2~120h of heat preservation.It is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3- 0.3Ti- surpluses Fe Oxide dispersion intensifying ferrous alloy.
It is an advantage of the invention that on the basis of traditional iron-based ODS alloys, nanocrystalline intermetallics (β ' phases) are introduced, The technique that vacuum induction melting and electroslag melting are combined can effectively reduce the oxygen content of ingot casting and the content of nonmetal inclusion, The intermediate alloy of alloying prevents the oxidation of Mn elements.Due to using pre-alloyed intermediate alloy powder, conjunction can be shortened The time of aurification, therefore Ball-milling Time can be shortened, reduce energy consumption.Ball-milling Time reduces what the introducing of long-time ball milling was mingled with Risk.Intermediate alloy powder has larger distortion of lattice, sintering activity high.Ni in alloy2AlMn intermetallic compounds and more The grain size of dephasing is all very tiny, and is evenly distributed, and invigoration effect is notable.
Description of the drawings
Fig. 1 is the process flow chart of the present invention
Specific implementation mode
Embodiment 1:35wt.%Fe powder++ 0.3wt.% nanometers of intermediate alloy powder Y2O3Powder prepares 5Ni-1Al-3Mn- 0.3Y2O3- 0.3Ti- surplus Fe oxide dispersion intensifying ferrous alloys
Using iron block, Fe-Mn alloys, Ni-Al alloys and Fe-Ti alloys as raw material, the purity of various raw materials is all higher than 99.9%.Raw metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, and pretreatment time is 30min, 90min is dried in processing at 60 DEG C in an oven after alcohol is cleaned.Intermediate alloy carries out melting in vaccum sensitive stove, CaO ceramic crucibles are used in fusion process, and increase power after furnace charge is melting down, so that bath temperature is risen to 1600 DEG C, heat preservation 30min cools down, is filled with argon gas later, and molten steel is cast into intermediate alloy ingot casting;The ingot casting of vacuum induction melting carries out indifferent gas Atmosphere electroslag melting.The ingredient of electroslag remelting slag charge is:20%CaO, 15%Al2O3, 1%TiO2, 1%MgO, 3%CeO, surplus CaF2.It pours into crystallizer, has been powered after electric arc after slag charge is heated to molten condition, adjustment remelting voltage is 35-65V, electricity 3000-8000A is flowed, pure 7.73Ni-1.55Al-4.64Mn-0.46Ti- surplus Fe intermediate alloy ingot castings are obtained.It closes centre The oxygen content of golden ingot casting is 100ppm, sulfur content 20ppm.Intermediate alloy ingot casting surface oxide skin is removed, is carried in one kind The high-speed disc of cooling system and protective atmosphere galls to be crushed in crushing device.Broken powder is screened, is obtained in band Between alloy powder.By 35wt.%Fe powder, the nanometer Y of the intermediate alloy powder of 64.7wt.% and 0.3wt.%2O3Powder mixes After carry out mechanical alloying, weighed first, in accordance with alloying component proportioning, and in addition add in mixed-powder 0.3~ 0.5wt.% stearic acid is as process control agent.After above-mentioned powder is pre-mixed uniformly in high-purity argon gas or hydrogen atmosphere (99.999%) high-energy ball milling is carried out, drum's speed of rotation is 340~500 revs/min, and Ball-milling Time 30-35h obtains mechanical conjunction Aurification powder.Mechanical alloying carries out vacuum seal using mild steel as jacket, and jacket carries out hot isostatic pressing, hot isostatic pressing temperature Degree is 950 DEG C, pressure 200MPa, soaking time 2h;It obtains close to fully dense oxide dispersion intensifying ferrous alloy.Heat Isostatic pressed oxide dispersion intensifying ferrous alloy carries out solid solution and ageing treatment.Solid solution temperature is 900 DEG C, keeps the temperature sky after 2h It is cold.Aging temperature is 550 DEG C, air-cooled after heat preservation 100h.It is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3-0.3Ti- The oxide dispersion intensifying ferrous alloy of surplus Fe.
Embodiment 2:40wt.%Fe powder++ 0.3wt.% nanometers of intermediate alloy powder Y2O3Powder prepares 5Ni-1Al-3Mn- 0.3Y2O3- 0.3Ti- surplus Fe oxide dispersion intensifying ferrous alloys
Using iron block, Fe-Mn alloys and Ni-Al alloys as raw material, the purity of various raw materials is all higher than 99.9%.Metal Raw material is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, pretreatment time 30min, and alcohol is cleaned 60min is dried in processing at 70 DEG C in an oven afterwards;Intermediate alloy carries out melting in vaccum sensitive stove, is used in fusion process CaO ceramic crucibles, and power is increased after furnace charge is melting down, so that bath temperature is risen to 1600 DEG C, keeps the temperature 30min, cooling later, It is filled with argon gas, molten steel is cast into intermediate alloy ingot casting;The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag The ingredient of remelting slag charge is:20%CaO, 15%Al2O3, 3%TiO2, 3%MgO, 5%CeO, surplus CaF2.Slag charge is heated to It pours into crystallizer, has been powered after electric arc after molten condition, adjustment remelting voltage is 35-65V, electric current 3000-8000A, is obtained Pure 8.38Ni-1.68Al-5.02Mn-0.5Ti- surplus Fe intermediate alloy ingot castings.The oxygen content of intermediate alloy ingot casting is 100ppm, sulfur content 20ppm.Intermediate alloy ingot casting surface oxide skin is removed, in one kind with cooling system and protection gas The high-speed disc of atmosphere galls to be crushed in crushing device.Broken powder is screened, band intermediate alloy powder is obtained.It will The nanometer Y of 40wt.%Fe powder, the intermediate alloy powder of 59.7wt.% and 0.3wt.%2O3Mechanical alloy is carried out after powder mixing Change.It is weighed first, in accordance with alloying component proportioning, and in addition adds 0.3~0.5wt.% stearic acid conducts in mixed-powder Process control agent.By (99.999%) carries out high energy ball in high-purity argon gas or hydrogen atmosphere after the premixing uniformly of above-mentioned powder Mill, drum's speed of rotation are 340~500 revs/min, and Ball-milling Time 30-35h obtains mechanical alloying powder.Mechanical alloying is adopted Mild steel is used to carry out vacuum seal as jacket, jacket carries out hot isostatic pressing, and hip temperature is 1000 DEG C, and pressure is 150MPa, soaking time 2h;It obtains close to fully dense oxide dispersion intensifying ferrous alloy.Hot isostatic pressing dispersed oxide Reinforced iron-base alloy carries out solid solution and ageing treatment.Solid solution temperature is 1000 DEG C, air-cooled after heat preservation 3h.Aging temperature It is 600 DEG C, it is air-cooled after heat preservation 80h.It is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3The oxide of -0.3Ti- surpluses Fe is more Dissipate reinforced iron-base alloy.
Embodiment 3:50wt.%Fe powder++ 0.3wt.% nanometers of intermediate alloy powder Y2O3Powder prepares 5Ni-1Al-3Mn- 0.3Y2O3- 0.3Ti- surplus Fe oxide dispersion intensifying ferrous alloys
Using iron block, Fe-Mn alloys and Ni-Al alloys as raw material, the purity of various raw materials is all higher than 99.9%.Metal Raw material is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, pretreatment time 30min, and alcohol is cleaned 45min is dried in processing at 75 DEG C in an oven afterwards;Intermediate alloy carries out melting in vaccum sensitive stove, is used in fusion process CaO ceramic crucibles, and power is increased after furnace charge is melting down, so that bath temperature is risen to 160 DEG C, keeps the temperature 30min, cooling later, It is filled with argon gas, molten steel is cast into intermediate alloy ingot casting;The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag The ingredient of remelting slag charge is:15%CaO, 15%Al2O3, 5%TiO2, 5%MgO, 8%CeO, surplus CaF2.Slag charge is heated to It pours into crystallizer, has been powered after electric arc after molten condition, adjustment remelting voltage is 35-65V, electric current 3000-8000A, is obtained Pure 10.06Ni-2.01Al-6.04Mn-0.6Ti- surplus Fe intermediate alloy ingot castings.The oxygen content of intermediate alloy ingot casting is 100ppm, sulfur content 20ppm.Intermediate alloy ingot casting surface oxide skin is removed, in one kind with cooling system and protection gas The high-speed disc of atmosphere galls to be crushed in crushing device.Broken powder is screened, band intermediate alloy powder is obtained.It will The nanometer Y of 50wt.%Fe powder, the intermediate alloy powder of 49.7wt.% and 0.3wt.%2O3Mechanical alloy is carried out after powder mixing Change.It is weighed first, in accordance with alloying component proportioning, and in addition adds 0.3~0.5wt.% stearic acid conducts in mixed-powder Process control agent.By (99.999%) carries out high energy ball in high-purity argon gas or hydrogen atmosphere after the premixing uniformly of above-mentioned powder Mill, drum's speed of rotation are 340~500 revs/min, and Ball-milling Time 30-35h obtains mechanical alloying powder.Mechanical alloying is adopted Mild steel is used to carry out vacuum seal as jacket, jacket carries out hot isostatic pressing, and hip temperature is 1100 DEG C, and pressure is 130MPa, soaking time 3h;It obtains close to fully dense oxide dispersion intensifying ferrous alloy.Hot isostatic pressing dispersed oxide Reinforced iron-base alloy carries out solid solution and ageing treatment.Solid solution temperature is 1100 DEG C, air-cooled after heat preservation 4h.Aging temperature It is 700 DEG C, it is air-cooled after heat preservation 60h.It is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3The oxide of -0.3Ti- surpluses Fe is more Dissipate reinforced iron-base alloy.
Embodiment 4:60wt.%Fe powder++ 0.3wt.% nanometers of intermediate alloy powder Y2O3Powder prepares 5Ni-1Al-3Mn- 0.3Y2O3- 0.3Ti- surplus Fe oxide dispersion intensifying ferrous alloys
Using iron block, Fe-Mn alloys and Ni-Al alloys as raw material, the purity of various raw materials is all higher than 99.9%.Metal Raw material is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removes oxide on surface, pretreatment time 30min, and alcohol is cleaned 30min is dried in processing at 80 DEG C in an oven afterwards;Intermediate alloy carries out melting in vaccum sensitive stove, is used in fusion process CaO ceramic crucibles, and power is increased after furnace charge is melting down, so that bath temperature is risen to 1600 DEG C, keeps the temperature 30min, cooling later, It is filled with argon gas, molten steel is cast into intermediate alloy ingot casting;The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag The ingredient of remelting slag charge is:20%CaO, 15%Al2O3, 5%TiO2, 5%MgO, 10%CeO surpluses CaF2.Slag charge is heated to It pours into crystallizer, has been powered after electric arc after molten condition, adjustment remelting voltage is 35-65V, electric current 3000-8000A, is obtained Pure 12.6Ni-2.52Al-7.56Mn-0.76Ti- surplus Fe intermediate alloy ingot castings.The oxygen content of intermediate alloy ingot casting is 100ppm, sulfur content 20ppm.Intermediate alloy ingot casting surface oxide skin is removed, in one kind with cooling system and protection gas The high-speed disc of atmosphere galls to be crushed in crushing device.Broken powder is screened, band intermediate alloy powder is obtained.It will The nanometer Y of 50wt.%Fe powder, the intermediate alloy powder of 49.7wt.% and 0.3wt.%2O3Mechanical alloy is carried out after powder mixing Change.It is weighed first, in accordance with alloying component proportioning, and in addition adds 0.3~0.5wt.% stearic acid conducts in mixed-powder Process control agent.By (99.999%) carries out high energy ball in high-purity argon gas or hydrogen atmosphere after the premixing uniformly of above-mentioned powder Mill, drum's speed of rotation are 340~500 revs/min, and Ball-milling Time 30-35h obtains mechanical alloying powder.Mechanical alloying is adopted Mild steel is used to carry out vacuum seal as jacket, jacket carries out hot isostatic pressing, and hip temperature is 1150 DEG C, and pressure is 100MPa, soaking time 3h;It obtains close to fully dense oxide dispersion intensifying ferrous alloy.Hot isostatic pressing dispersed oxide Reinforced iron-base alloy carries out solid solution and ageing treatment.Solid solution temperature is 1200 DEG C, air-cooled after heat preservation 4h.Aging temperature It is 800 DEG C, it is air-cooled after heat preservation for 24 hours.It is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3The oxide of -0.3Ti- surpluses Fe is more Dissipate reinforced iron-base alloy.

Claims (3)

1. a kind of method preparing oxide dispersion intensifying iron(-)base powder, it is characterised in that:
Step 1: using iron block, Fe-Mn alloys and Ni-Al alloys as raw material, the purity of various raw materials is all higher than 99.9%; Raw metal is pre-processed in 5vol.% aqueous hydrochloric acid solutions, removal oxide on surface, pretreatment time 25-35min, 30-90min is dried in processing at 60 DEG C in an oven after alcohol is cleaned;The mass ratio and target of each alloying element in intermediate alloy The mass ratio of each element is consistent in oxide dispersion intensifying ferrous alloy;
Step 2: intermediate alloy, the ingredient of target oxide dispersion strengthening iron-base alloy will be prepared by pretreated raw material For:5Ni-1Al-3Mn-0.3Y2O3- 0.3Ti- surpluses Fe;Intermediate alloy carries out melting in vaccum sensitive stove, in fusion process Using CaO ceramic crucibles, and power is increased after furnace charge is melting down, bath temperature is made to rise to 1600-1700 DEG C, keep the temperature 25- 35min cools down, is filled with argon gas later, and molten steel is poured into intermediate alloy ingot casting;The ingot casting of vacuum induction melting carries out indifferent gas Atmosphere electroslag melting;The ingredient of electroslag remelting slag charge is:15-20%CaO, 15-20%Al2O3, 1-5%TiO2, 1-5%MgO, 3- 10%CeO, surplus CaF2;It pours into crystallizer, has been powered after electric arc after slag charge is heated to molten condition, adjust remelting voltage For 35-65V, electric current 3000-8000A;Consutrode is slowly melted by resistance, and the molten drop after fusing passes through the slag charge of melting Layer reacts with slag charge and is purified, and is recrystallized in crystalliser feet, obtains dense structure, uniform, pure electricity Slag remelting intermediate alloy ingot casting;The oxygen content of intermediate alloy ingot casting is 100ppm, sulfur content 20ppm;
Step 3: intermediate alloy ingot casting surface oxide skin is removed, in a kind of high-speed disc with cooling system and protective atmosphere It galls and is crushed in crushing device;Broken powder is screened, intermediate alloy powder is obtained;
Step 4: mechanical alloying is carried out after parent metal powder, intermediate alloy powder and nano-oxide particles are mixed, Parent metal powder is Fe powder, oxide Y2O3;It is weighed first, in accordance with alloying component proportioning, and another in mixed-powder Outer addition 0.3~0.5wt.% stearic acid is as process control agent, to avoid powder agglomates in Process During High Energy Ball Milling;By above-mentioned powder High-energy ball milling is carried out in 99.999% high-purity argon gas or hydrogen atmosphere after the premixing uniformly of end, drum's speed of rotation is 340~ 500 revs/min, Ball-milling Time 30-35h obtains mechanical alloying powder;
Step 5: being densified to mechanical alloying powder using heat and other static pressuring processes, with mild steel to mechanical alloying powder Then last jacket carries out hot isostatic pressing, obtain close to fully dense oxide dispersion intensifying ferrous alloy;
Step 6: hot isostatic pressing oxide dispersion intensifying ferrous alloy carries out two benches heat treatment, solution treatment is carried out first, so Air-cooled after progress ageing treatment afterwards, it is 5Ni-1Al-3Mn-0.3Y to finally obtain ingredient2O3The oxide of -0.3Ti- surpluses Fe is more Dissipate reinforced iron-base alloy.
2. a kind of method preparing oxide dispersion intensifying iron(-)base powder as described in claim 1, it is characterised in that step Hip temperature described in rapid five is 950~1150 DEG C, and pressure is 100~200MPa, and soaking time is 1~3h.
3. a kind of method preparing oxide dispersion intensifying iron(-)base powder as described in claim 1, it is characterised in that step Solid solution temperature described in rapid six is 800~1200 DEG C, air-cooled after 2~4h of heat preservation;Aging temperature is 500~800 DEG C, keep the temperature 2~120h.
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