CN106825587A - A kind of method for preparing oxide dispersion intensifying ferrous alloy - Google Patents
A kind of method for preparing oxide dispersion intensifying ferrous alloy Download PDFInfo
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Abstract
A kind of method for preparing oxide dispersion intensifying ferrous alloy, belongs to field of metal dispersion reinforcement technology.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 carried out crushing in the disintegrating machine with protective atmosphere and obtains intermediate alloy powder, 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 after high temperature insostatic pressing (HIP) and heat treatment by just obtaining final oxide dispersion intensifying ferrous alloy.The present invention effectively reduces the content of oxygen and nonmetal inclusion in ingot casting using the smelting technology of duplex, and the intermediate alloy of alloying prevents the oxidation of Mn elements, and can shorten Ball-milling Time, reducing energy consumption.The oxide dispersion intensifying ferrous alloy of preparation is by L21Type Ni2AlMn intermetallic compounds and dispersed oxide mutually common reinforcing, strengthen effect is significant.
Description
Technical field
The invention belongs to field of metal dispersion reinforcement technology, specifically provide one kind and intermediate alloy is prepared using foundry alloy method
Powder, and then it is strong to obtain dispersed oxide that intermediate alloy powder, matrix powder and oxide powder are carried out into mechanical alloying
The method for changing iron(-)base powder.
Background technology
γ of the Alfer with similar nickel-base alloy strengthened jointly by intermetallic compound and nano-oxide/
The two-phase structure of γ ', is expected to improve the temperature in use limit and mechanical behavior under high temperature of conventional ferrite heat-resisting alloy, in high temperature
There is important application prospect in structural material field.Nano-oxide particles have excellent heat endurance and chemical stability,
At a temperature of alloy melting point, nano-oxide still can play inhibition to the motion of dislocation, be strong dispersed oxide
Most important hardening constituent in alloy.(Ni, Fe) Al intermetallic compound phases (β ' phases) are that the 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 is up to 1638 DEG C, with higher
Intensity and hardness.Meanwhile, closely, lattice misfit is small for the lattice parameter of β ' and ferrite matrix (β), and this makes β ' mutually and β
Coherence orientation relationship is easily formed between matrix, this creates condition for the homogeneous nucleation and disperse shape of β ' phases are separated out.In alloy
Middle addition Mn elements can change the phase structure of intermetallic compound, intermetallic compound is 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 thing is better than single-phase NiAl phases.Try to reduce excessive oxygen content, it is that control is separated out to shorten Ball-milling Time, reducing energy consumption
The key of phase structure and raising 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 easily in ma process aoxidize, not only make participation shape
Into Ni2The Mn elements of AlMn intermetallic compounds are reduced, it is impossible to reach the purpose of effectively control intermetallic compound composition.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 increases impurity oxygen content, causes the roughening of dispersed oxide phase.Above-mentioned two factor is all straight
The structure and heat endurance for being related to intermetallic compound and oxide are connect, the lifting of reinforcing effect is limited.
The content of the invention
It is an object of the invention to provide a kind of method for preparing oxide dispersion intensifying ferrous alloy.Prepared by the method
Oxide dispersion intensifying ferrous alloy is by L21Type Ni2AlMn intermetallic compounds and dispersed oxide mutually common reinforcing, using two
The superposition for planting the reinforcing effect of precipitated phase improves the mechanical behavior under high temperature of material.
The present invention obtains intermediate alloy ingot casting using the technique using vacuum melting+electroslag melting duplex.In electroslag melting
During, consutrode is slowly melted by resistance, is mingled with to create by the parameter such as shape, depth, viscosity for adjusting slag bath
The condition that thing floats, the money consumption electric shock baton drop after dissolving reacts and is purified with slag charge through the slag material layer of melting,
And recrystallized in the bottom of crystallizer, obtain low-sulfur, dense structure, uniform, pure intermediate alloy ingot casting.Intermediate alloy is cast
Ingot carries out broken obtaining intermediate alloy powder, intermediate alloy powder and matrix powder and oxygen in the disintegrating machine 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 loads steel capsule, degassing, soldering and sealing treatment, hot canned forging consolidation shaping is carried out, and be heat-treated, obtain final oxygen
Compound dispersion strengthening iron-base alloy.The preparation technology flow of oxide dispersion intensifying ferrous alloy is as shown in figure 1, concrete technology is walked
Suddenly have：
1st, 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 alcohol dries 30-90min in treatment at 60 DEG C in an oven after cleaning.
2nd, the vacuum induction melting+electroslag melting of intermediate alloy：Intermediate alloy will be prepared into by the raw material of pretreatment, 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 composition of thing 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 are used in fusion process, and power is increased after furnace charge is melting down, bath temperature is increased
To 1600-1700 DEG C, 25-35min is incubated, lowers the temperature afterwards, be filled with argon gas, molten steel poured and builds up intermediate alloy ingot casting；Vacuum sense
Answering the ingot casting of melting carries out inert atmosphere electroslag melting.The composition of electroslag remelting slag charge is：15-20%CaO, 15-20%Al2O3,
1-5%TiO2, 1-5%MgO, 3-10%CeO, surplus CaF2.Poured into crystallizer after slag charge is heated into molten condition, be powered
After playing electric arc, adjustment remelting voltage is 35-65V, electric current 3000-8000A；Consutrode is slowly melted by resistance, gold after dissolving
Category drop reacts and is purified with slag charge through the slag material layer of melting, 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
It is 20ppm.
3rd, intermediate alloy ingot casting is crushed：By intermediate alloy ingot casting surface scale removal, one kind with cooling system with
The high-speed disc of protective atmosphere is crushed in galling crushing device.Powder after crushing is screened, intermediate alloy powder is obtained.
4th, mechanical alloying：Machine is carried out after parent metal powder, intermediate alloy powder and nano-oxide particles are mixed
Tool alloying, parent metal powder is Fe powder, and nano-oxide is Y2O3.Alloying component proportioning is first according to be weighed, and
In mixed-powder in addition addition 0.3~0.5wt.% stearic acid 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 is 30-35h, obtains mechanical alloying powder.
5th, 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 high temperature insostatic pressing (HIP), and hip temperature is 950~1150 DEG C, and pressure is 100~
200MPa, soaking time is 1~3h；Obtain close to fully dense oxide dispersion intensifying ferrous alloy.
6th, it is heat-treated：High temperature insostatic pressing (HIP) oxide dispersion intensifying ferrous alloy carries out two benches heat treatment, and solid solution is carried out first
Treatment, then carries out Ageing Treatment.Solid solution temperature is 800~1200 DEG C, air cooling after 2~4h of insulation.Aging temperature
It is 500~800 DEG C, air cooling after 2~120h of insulation.Composition is finally given for 5Ni-1Al-3Mn-0.3Y2O3- 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, it is possible to shorten Ball-milling Time, reducing energy consumption.The long-time ball milling that reduces of Ball-milling Time introduces what is be mingled with
Risk.Intermediate alloy powder has larger distortion of lattice, and sintering activity is high.Ni in alloy2AlMn intermetallic compounds and more
The particle diameter of dephasing is all very tiny, and is evenly distributed, and invigoration effect is notable.
Brief description of the drawings
Fig. 1 is process chart of the invention
Specific embodiment
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, alcohol dries 90min in treatment at 60 DEG C in an oven after cleaning.Intermediate alloy carries out melting in vaccum sensitive stove,
CaO ceramic crucibles are used in fusion process, and power is increased after furnace charge is melting down, bath temperature is risen to 1600 DEG C, insulation
30min, lowers the temperature, is filled with argon gas afterwards, molten steel is poured and builds up intermediate alloy ingot casting；The ingot casting of vacuum induction melting carries out indifferent gas
Atmosphere electroslag melting.The composition of electroslag remelting slag charge is：20%CaO, 15%Al2O3, 1%TiO2, 1%MgO, 3%CeO, surplus
CaF2.Poured into crystallizer after slag charge is heated into molten condition, be powered after electric arc, adjustment remelting voltage is 35-65V, electricity
Stream 3000-8000A, obtains pure 7.73Ni-1.55Al-4.64Mn-0.46Ti- surplus Fe intermediate alloy ingot castings.Close centre
The oxygen content of golden ingot casting is 100ppm, and sulfur content is 20ppm.By the removal of intermediate alloy ingot casting surface scale, carried in one kind
Cooling system is crushed in galling crushing device with the high-speed disc of protective atmosphere.Powder after crushing is screened, is obtained with
Between alloy powder.By the nanometer Y of 35wt.%Fe powder, the intermediate alloy powder of 64.7wt.% and 0.3wt.%2O3Powder mixes
After carry out mechanical alloying, be first according to alloying component proportioning weighed, and in mixed-powder in addition addition 0.3~
0.5wt.% stearic acid is used 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 is 30-35h, obtains mechanical conjunction
Aurification powder.Mechanical alloying carries out vacuum seal using mild steel as jacket, and jacket carries out high temperature insostatic pressing (HIP), high temperature insostatic pressing (HIP) temperature
It is 950 DEG C to spend, and pressure is 200MPa, and soaking time is 2h；Obtain 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, empty after insulation 2h
It is cold.Aging temperature is 550 DEG C, air cooling after insulation 100h.Composition is finally given for 5Ni-1Al-3Mn-0.3Y2O3-0.3Ti-
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, and pretreatment time is 30min, and alcohol is cleaned
Afterwards in an oven in treatment drying 60min at 70 DEG C；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, bath temperature is risen to 1600 DEG C, 30min is incubated, cooling afterwards,
Argon gas is filled with, molten steel is poured and is built up intermediate alloy ingot casting；The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag
The composition of remelting slag charge is：20%CaO, 15%Al2O3, 3%TiO2, 3%MgO, 5%CeO, surplus CaF2.Slag charge is heated to
Poured into crystallizer after molten condition, be powered after electric arc, 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 is 20ppm.By the removal of intermediate alloy ingot casting surface scale, in one kind with cooling system and protection gas
The high-speed disc of atmosphere is crushed in galling crushing device.Powder after crushing is screened, band intermediate alloy powder is obtained.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.Alloying component proportioning is first according to be weighed, and addition 0.3~0.5wt.% stearic acid conducts in addition 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 is 340~500 revs/min, and Ball-milling Time is 30-35h, obtains mechanical alloying powder.Mechanical alloying is adopted
Vacuum seal is carried out as jacket with mild steel, jacket carries out high temperature insostatic pressing (HIP), and hip temperature is 1000 DEG C, and pressure is
150MPa, soaking time is 2h；Obtain close to fully dense oxide dispersion intensifying ferrous alloy.High temperature insostatic pressing (HIP) dispersed oxide
Reinforced iron-base alloy carries out solid solution and Ageing Treatment.Solid solution temperature is 1000 DEG C, air cooling after insulation 3h.Aging temperature
It is 600 DEG C, air cooling after insulation 80h.Composition is finally given for 5Ni-1Al-3Mn-0.3Y2O3The 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, and pretreatment time is 30min, and alcohol is cleaned
Afterwards in an oven in treatment drying 45min at 75 DEG C；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, bath temperature is risen to 160 DEG C, 30min is incubated, cooling afterwards,
Argon gas is filled with, molten steel is poured and is built up intermediate alloy ingot casting；The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag
The composition of remelting slag charge is：15%CaO, 15%Al2O3, 5%TiO2, 5%MgO, 8%CeO, surplus CaF2.Slag charge is heated to
Poured into crystallizer after molten condition, be powered after electric arc, 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 is 20ppm.By the removal of intermediate alloy ingot casting surface scale, in one kind with cooling system and protection gas
The high-speed disc of atmosphere is crushed in galling crushing device.Powder after crushing is screened, band intermediate alloy powder is obtained.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.Alloying component proportioning is first according to be weighed, and addition 0.3~0.5wt.% stearic acid conducts in addition 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 is 340~500 revs/min, and Ball-milling Time is 30-35h, obtains mechanical alloying powder.Mechanical alloying is adopted
Vacuum seal is carried out as jacket with mild steel, jacket carries out high temperature insostatic pressing (HIP), and hip temperature is 1100 DEG C, and pressure is
130MPa, soaking time is 3h；Obtain close to fully dense oxide dispersion intensifying ferrous alloy.High temperature insostatic pressing (HIP) dispersed oxide
Reinforced iron-base alloy carries out solid solution and Ageing Treatment.Solid solution temperature is 1100 DEG C, air cooling after insulation 4h.Aging temperature
It is 700 DEG C, air cooling after insulation 60h.Composition is finally given for 5Ni-1Al-3Mn-0.3Y2O3The 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, and pretreatment time is 30min, and alcohol is cleaned
Afterwards in an oven in treatment drying 30min at 80 DEG C；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, bath temperature is risen to 1600 DEG C, 30min is incubated, cooling afterwards,
Argon gas is filled with, molten steel is poured and is built up intermediate alloy ingot casting；The ingot casting of vacuum induction melting carries out inert atmosphere electroslag melting.Electroslag
The composition of remelting slag charge is：20%CaO, 15%Al2O3, 5%TiO2, 5%MgO, 10%CeO surplus CaF2.Slag charge is heated to
Poured into crystallizer after molten condition, be powered after electric arc, 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 is 20ppm.By the removal of intermediate alloy ingot casting surface scale, in one kind with cooling system and protection gas
The high-speed disc of atmosphere is crushed in galling crushing device.Powder after crushing is screened, band intermediate alloy powder is obtained.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.Alloying component proportioning is first according to be weighed, and addition 0.3~0.5wt.% stearic acid conducts in addition 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 is 340~500 revs/min, and Ball-milling Time is 30-35h, obtains mechanical alloying powder.Mechanical alloying is adopted
Vacuum seal is carried out as jacket with mild steel, jacket carries out high temperature insostatic pressing (HIP), and hip temperature is 1150 DEG C, and pressure is
100MPa, soaking time is 3h；Obtain close to fully dense oxide dispersion intensifying ferrous alloy.High temperature insostatic pressing (HIP) dispersed oxide
Reinforced iron-base alloy carries out solid solution and Ageing Treatment.Solid solution temperature is 1200 DEG C, air cooling after insulation 4h.Aging temperature
It is 800 DEG C, air cooling after insulation 24h.Composition is finally given for 5Ni-1Al-3Mn-0.3Y2O3The oxide of -0.3Ti- surpluses Fe is more
Dissipate reinforced iron-base alloy.
Claims (5)
1. a kind of method for preparing oxide dispersion intensifying iron(-)base powder, it is characterised in that：
Step one, 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 5% aqueous hydrochloric acid solution, removes oxide on surface, and pretreatment time is 25-35min, alcohol
In an oven in treatment drying 30-90min at 60 DEG C after cleaning；The mass ratio and desirable oxidation of each alloying element in intermediate alloy
The mass ratio of each element is consistent in thing dispersion strengthening iron-base alloy；
Step 2, will by pretreatment raw material be prepared into intermediate alloy, the composition of target oxide dispersion strengthening iron-base alloy
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 risen to 1600-1700 DEG C, be incubated 25-
35min, lowers the temperature, is filled with argon gas afterwards, 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 composition of electroslag remelting slag charge is：15-20%CaO, 15-20%Al2O3, 1-5%TiO2, 1-5%MgO, 3-
10%CeO, surplus CaF2；Poured into crystallizer after slag charge is heated into molten condition, be powered after electric arc, adjust remelting voltage
It is 35-65V, electric current 3000-8000A；Consutrode is slowly melted by resistance, slag charge of the molten drop after fusing through melting
Layer reacts and is purified with slag charge, 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, and sulfur content is 20ppm；
Step 3, by intermediate alloy ingot casting surface scale removal, in a kind of high-speed disc with cooling system Yu protective atmosphere
Crushed in worn-off crushing device.Powder after crushing is screened, band intermediate alloy powder is obtained；
Step 4, will parent metal powder, intermediate alloy powder and nano-oxide particles mix after carry out mechanical alloying,
Parent metal powder is Fe powder, oxide Y2O3；Alloying component proportioning is first according to be weighed, and in mixed-powder in addition
Addition 0.3~0.5wt.% stearic acid 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 after premixing is uniform in 99.999% high-purity argon gas or hydrogen atmosphere, drum's speed of rotation is 340~500
Rev/min, Ball-milling Time is 30-35h, obtains mechanical alloying powder；
Step 5, mechanical alloying powder is densified using heat and other static pressuring processes, with mild steel to mechanical alloying powder
Last jacket, then carries out high temperature insostatic pressing (HIP), obtains close to fully dense oxide dispersion intensifying ferrous alloy；
Step 6, high temperature insostatic pressing (HIP) oxide dispersion intensifying ferrous alloy carry out two benches heat treatment, solution treatment are carried out first, so
After carry out air cooling after Ageing Treatment, finally give composition for 5Ni-1Al-3Mn-0.3Y2O3The oxide of -0.3Ti- surpluses Fe is more
Dissipate reinforced iron-base alloy.
2. a kind of method for preparing oxide dispersion intensifying iron(-)base powder as claimed in claim 1, it is characterised in that step
The composition of the target oxide dispersion strengthening iron-base alloy described in rapid is：5Ni-1Al-3Mn-0.3Y2O3- 0.3Ti- surpluses
Fe。
3. a kind of method for preparing oxide dispersion intensifying iron(-)base powder as claimed 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.
4. a kind of method for preparing oxide dispersion intensifying iron(-)base powder as claimed in claim 1, it is characterised in that step
Solid solution temperature described in rapid six is 800~1200 DEG C, air cooling after 2~4h of insulation；Aging temperature is 500~800
DEG C, it is incubated 2~120h.
5. a kind of method for preparing oxide dispersion intensifying iron(-)base powder as claimed in claim 1, it is characterised in that step
The oxygen content of the intermediate alloy ingot casting described in rapid two is 100ppm, and sulfur content is 20ppm.
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Cited By (9)
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| CN109605759A (en) * | 2018-12-06 | 2019-04-12 | 广州市神火科技有限公司 | A kind of efficient earphone electrode welding |
| CN110396603A (en) * | 2019-07-18 | 2019-11-01 | 西安交通大学 | A kind of remelting method of ferroaluminium |
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| WO2020019401A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Multi-scale and multi-phase dispersion strengthened iron-based alloy, and preparation and representation method therefor |
| WO2020019402A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Oxide dispersion-strengthened iron-based alloy powder and characterization method therefor |
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| CN111893337A (en) * | 2020-07-01 | 2020-11-06 | 中国科学院金属研究所 | Preparation method of high-temperature alloy |
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| CN113444962A (en) * | 2021-06-10 | 2021-09-28 | 湘潭大学 | Method for preparing multi-nano-phase reinforced iron-based alloy |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948970A (en) * | 2010-10-13 | 2011-01-19 | 北京科技大学 | Mechanical alloying method for preparing strengthened dispersion alloy of nickel-based oxide |
| CN101979691A (en) * | 2010-10-13 | 2011-02-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened cobalt-based super alloy |
| CN102127712A (en) * | 2011-02-22 | 2011-07-20 | 中南大学 | Micro alloyed oxide dispersion-strengthening ferrite steel and preparation method |
| CN103233182A (en) * | 2013-06-07 | 2013-08-07 | 北京科技大学 | Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy |
| CN104532097A (en) * | 2014-12-25 | 2015-04-22 | 钢铁研究总院 | High-strength high-corrosion-resistant nickel-based high-temperature alloy and solution and aging heat treatment method thereof |
| US20150252458A1 (en) * | 2014-03-05 | 2015-09-10 | Korea Atomic Energy Research Institute | Ferritic/martensitic oxide dispersion strengthened steel with enhanced creep resistance and method of manufacturing the same |
-
2016
- 2016-12-05 CN CN201611100574.1A patent/CN106825587B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948970A (en) * | 2010-10-13 | 2011-01-19 | 北京科技大学 | Mechanical alloying method for preparing strengthened dispersion alloy of nickel-based oxide |
| CN101979691A (en) * | 2010-10-13 | 2011-02-23 | 北京科技大学 | Method for preparing oxide dispersion strengthened cobalt-based super alloy |
| CN102127712A (en) * | 2011-02-22 | 2011-07-20 | 中南大学 | Micro alloyed oxide dispersion-strengthening ferrite steel and preparation method |
| CN103233182A (en) * | 2013-06-07 | 2013-08-07 | 北京科技大学 | Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy |
| US20150252458A1 (en) * | 2014-03-05 | 2015-09-10 | Korea Atomic Energy Research Institute | Ferritic/martensitic oxide dispersion strengthened steel with enhanced creep resistance and method of manufacturing the same |
| CN104532097A (en) * | 2014-12-25 | 2015-04-22 | 钢铁研究总院 | High-strength high-corrosion-resistant nickel-based high-temperature alloy and solution and aging heat treatment method thereof |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11639542B2 (en) | 2018-07-27 | 2023-05-02 | Central South University | Multi-scale and multi-phase dispersion strengthened iron-based alloy, and preparation and characterization methods thereof |
| US11584979B2 (en) | 2018-07-27 | 2023-02-21 | Central South University | Oxide dispersion-strengthened iron-based alloy powder and characterization method thereof |
| WO2020019401A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Multi-scale and multi-phase dispersion strengthened iron-based alloy, and preparation and representation method therefor |
| WO2020019402A1 (en) * | 2018-07-27 | 2020-01-30 | 中南大学 | Oxide dispersion-strengthened iron-based alloy powder and characterization method therefor |
| CN109605759A (en) * | 2018-12-06 | 2019-04-12 | 广州市神火科技有限公司 | A kind of efficient earphone electrode welding |
| CN110396603B (en) * | 2019-07-18 | 2020-10-27 | 西安交通大学 | Remelting method of iron-aluminum alloy |
| CN110396603A (en) * | 2019-07-18 | 2019-11-01 | 西安交通大学 | A kind of remelting method of ferroaluminium |
| CN110607487A (en) * | 2019-10-09 | 2019-12-24 | 北京钢研高纳科技股份有限公司 | ODS-Fe3Al alloy, alloy product and preparation method thereof |
| CN111230098A (en) * | 2020-03-18 | 2020-06-05 | 北京大学 | Metal-based nano composite powder material, preparation method and application thereof |
| CN111230098B (en) * | 2020-03-18 | 2021-07-13 | 北京大学 | Metal-based nano composite powder material, preparation method and application thereof |
| CN111893337A (en) * | 2020-07-01 | 2020-11-06 | 中国科学院金属研究所 | Preparation method of high-temperature alloy |
| CN111893337B (en) * | 2020-07-01 | 2022-02-11 | 中国科学院金属研究所 | Preparation method of high-temperature alloy |
| CN112064011A (en) * | 2020-08-27 | 2020-12-11 | 北京科技大学 | Method for preparing multi-nano-phase reinforced ferrite alloy with complex shape |
| CN112064011B (en) * | 2020-08-27 | 2021-06-29 | 北京科技大学 | Method for preparing multi-nano-phase reinforced ferrite alloy with complex shape |
| CN113444962A (en) * | 2021-06-10 | 2021-09-28 | 湘潭大学 | Method for preparing multi-nano-phase reinforced iron-based alloy |
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