CN108838374A - The preparation method of Fe-based perovskite-like oxide silk - Google Patents
The preparation method of Fe-based perovskite-like oxide silk Download PDFInfo
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- CN108838374A CN108838374A CN201810851909.6A CN201810851909A CN108838374A CN 108838374 A CN108838374 A CN 108838374A CN 201810851909 A CN201810851909 A CN 201810851909A CN 108838374 A CN108838374 A CN 108838374A
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- temperature
- based perovskite
- wire rod
- annealing
- ingot casting
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000000137 annealing Methods 0.000 claims abstract description 26
- 238000010275 isothermal forging Methods 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 40
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 239000000956 alloy Substances 0.000 claims description 21
- 238000005266 casting Methods 0.000 claims description 21
- 229910045601 alloy Inorganic materials 0.000 claims description 19
- 229910052684 Cerium Inorganic materials 0.000 claims description 15
- 229910052746 lanthanum Inorganic materials 0.000 claims description 15
- 239000004615 ingredient Substances 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 230000006698 induction Effects 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 238000005275 alloying Methods 0.000 claims description 3
- 239000005030 aluminium foil Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000005098 hot rolling Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000003026 anti-oxygenic effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000007499 fusion processing Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B22D27/02—Use of electric or magnetic effects
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- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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- C21C7/06—Deoxidising, e.g. killing
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- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
- C21D8/065—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
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- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G3/00—Apparatus for cleaning or pickling metallic material
- C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
Abstract
This disclosure relates to which a kind of preparation method of Fe-based perovskite-like oxide silk, successively includes following key step：(a) discharge plasma is sintered；(b) it makes annealing treatment；(c) isothermal forging；(d) gren rod；(e) stress relief annealing；And (f) multi pass drawing, obtain Fe-based perovskite-like oxide silk.Disclosed method can improve Fe-based perovskite-like oxide silk internal structure quality, to improve its thermal shock resistance.
Description
Technical field
The disclosure belongs to metallurgical technology field more particularly to a kind of preparation method of Fe-based perovskite-like oxide silk.
Background technique
Electrothermal alloy is widely used in the fields such as electronics, chemical industry, machinery, is a kind of important alloy material.The material
It can be realized electric energy and heat energy conversion, reach heating purpose.Currently, Fe-based perovskite-like oxide is a kind of widely used electrothermal alloy
Material has many advantages, such as that high using temperature, resistivity is high, easy to process.
The preparation process of current Fe-based perovskite-like oxide mainly includes melting, deoxidation, Argon, hot rolling, annealing, rinsing step
Suddenly.Patent CN103938102B discloses a kind of preparation method of ferrum-chromium-aluminum system multi-element high-resistance electrothermal alloy, using fusing and
The preparation method that powder metallurgy combines can effectively avoid conventional smelting process prepare in due to fusing point between constituent element, density and
Quality proportioning differs greatly and the component segregation that generates, being uniformly distributed for each component is realized, in conjunction with subsequent homogenizing annealing, isothermal
The techniques such as forging, gren rod effectively improve alloy microstructure, improve mechanical property, use temperature and service life.This method
The product room temperature resistivity of preparation is up to 2.2 Ω mm2/ m, tensile strength is up to 1060MPa, and elongation percentage is up to 16%, anti-oxidant examination
It tests weight gain and is less than 2.6mg/cm2。
However, there are flaws for the Fe-based perovskite-like oxide internal structure of technical process manufacture, degree of grain refinement is inadequate,
Be unevenly distributed, and it is poor there are thermal shock resistance the problems such as.
Summary of the invention
Present disclose provides a kind of preparation method of Fe-based perovskite-like oxide silk, the Fe-based perovskite-like oxide yarn qualities of preparation
More preferably, crystal grain refinement, uniformly, have excellent thermal shock resistance.
The preparation method of a kind of Fe-based perovskite-like oxide silk that the disclosure provides includes：(1) ingredient：(2) Medium frequency induction is true
Empty furnace melting；(3) deoxidation；(4) Argon；(5) ingot casting；(6) it crushes；(7) discharge plasma is sintered；(8) it anneals；(9) isothermal
Forging；(10) gren rod；(11) stress relief annealing；(12) drawing.
Optionally, (1) presses following proportion scale ingredient：Cr：12-13%, Zr：5-8%, Ni：3-5%, Nb：3-5%,
Al:3-4%, Co：2-3%, Mo：2-3%, Si：1.3-1.6%, Ti：0.5-1%, Ce：0.1-0.3%, La：0.1-0.2%,
C：0.1-0.2%, B：0.001-0.01%, S：0.0001-0.0002%, P：0.0001-0.0002%, surplus are iron and miscellaneous
Matter；(2) melting processing, vacuum drying oven set of frequency 8K-10KHz are made in Medium frequency induction vacuum drying oven to above-mentioned ingredient；(3) deoxidation：
Aluminum deoxidation, the additional amount of aluminium are 1.5-2Kg/t, and deaeration time is greater than 20 minutes；(4) Argon, argon gas flow control is in 5-8L/
Min, argon blowing time 1-2min；(5) ingot casting, electromagnetic agitation ingot casting, frequency 25-30Hz, excitation current 450-500A；(6) it crushes,
Ingot casting is crushed, grinding, obtains alloy powder；(7) discharge plasma is sintered, and sintering temperature is 1350 DEG C -1400 DEG C, the time
For 8-9h；(8) homogenizing annealing：In vacuum heat treatment furnace, 20-25h is kept the temperature at 900-1000 DEG C；(9) isothermal forging passes through
Wire cutting mode is processed into cylinder ingots, carries out isothermal forging on a hydraulic press；(10) gren rod：Hot-rolled temperature：1400℃-
1425 DEG C, start rolling temperature：1425 DEG C, finishing temperature：1400℃；(11) stress relief annealing：In vacuum heat treatment furnace, annealing temperature
900-1000 DEG C of degree keeps the temperature 10h；(12) multi pass drawing is carried out after rinsing obtains Fe-based perovskite-like oxide silk.
Optionally, alloying component：Cr：12.9%, Zr：5.3%, C：0.01%, Si：1.05%, Ni：4%, Al：
3.4%, Co：2.6%, Mo：2.5%, Nb：3.2%, Ti：0.6%, Ce：0.15%, La：0.13%, B：0.006%, S：
0.0001%, P：0.0001%, surplus is iron and inevitable impurity.
Optionally, aluminium foil and boron powder package are placed in furnace bottom before melting.
Optionally, Ce and La 4 minutes addition smelting furnaces before coming out of the stove after vacuumize process, are sufficiently stirred.
Optionally, while Ce and La is added, 0.01% Tb is added.
Optionally, further include：900 DEG C of wire rod are preheated 20 minutes.
Optionally, further include：Alkali leaching processing, pickling processes, coating treatment are carried out to wire rod.
Optionally, when drawing, well-type electric furnace solution treatment, 1000-1200 DEG C of wire rod holding temperature, soaking time 2- are used
3 hours, hardening was cooling.
It can be used for making 2-6mm wire rod.
Optionally, when drawing, solution treatment, wire rod holding temperature 1000- are carried out using protective atmosphere continuous heat treating furnace
1200 DEG C, soaking time 2-3 hours, outside tube water was cold.
It can be used for making 0.2-2mm wire rod, the cold mode of outside tube water can be improved the wire rod service life.
Disclosed method improves the manufacture craft of Fe-based perovskite-like oxide silk, has the following advantages that：One, pass through friendship
Varying magnetic field plays the role of strong stirring, so that the condensation process of fusion process metal molten homogeneous and metal belt changes
Become, improves ingot quality, grain refinement effect is significant；Two, the content for having adjusted SI improves alloy thermal shock resistance, together
When, improve resistivity；Three, have the characteristics that impurity is low, toughness is strong, stretch-proof antioxygenic property is good；Four, high temperature hot rolling is filled
Divide the characteristic high using temperature using this alloy, effect of rolling is good.
Specific embodiment
A kind of preparation method of Fe-based perovskite-like oxide silk of the disclosure, the Fe-based perovskite-like oxide yarn quality of preparation is more
Good, crystal grain refinement, uniformly has excellent thermal shock resistance.A kind of preparation side for Fe-based perovskite-like oxide silk that the disclosure provides
Method, including：(1) ingredient：(2) Medium frequency induction vacuum drying oven melting；(3) deoxidation；(4) Argon；(5) ingot casting；(6) it crushes；(7) it discharges
Plasma sintering；(8) it anneals；(9) isothermal forging；(10) gren rod；(11) stress relief annealing；(12) drawing.
In an embodiment of the disclosure, (1) presses following proportion scale ingredient：Cr：12-13%, Zr：5-8%,
Ni：3-5%, Nb：3-5%, Al:3-4%, Co：2-3%, Mo：2-3%, Si：1.3-1.6%, Ti：0.5-1%, Ce：0.1-
0.3%, La：0.1-0.2%, C：0.1-0.2%, B：0.001-0.01%, S：0.0001-0.0002%, P：0.0001-
0.0002%, surplus is iron and impurity；(2) melting processing, vacuum drying oven frequency are made in Medium frequency induction vacuum drying oven to above-mentioned ingredient
8K-10KHz is set；(3) deoxidation：Aluminum deoxidation, the additional amount of aluminium are 1.5-2Kg/t, and deaeration time is greater than 20 minutes；(4) it blows
Argon, argon gas flow control is in 5-8L/min, argon blowing time 1-2min；(5) ingot casting, electromagnetic agitation ingot casting, frequency 25-30Hz, excitation
Electric current 450-500A；(6) it crushes, ingot casting is crushed, grinding, obtain alloy powder；(7) discharge plasma is sintered, sintering temperature
Degree is 1350 DEG C -1400 DEG C, time 8-9h；(8) homogenizing annealing：In vacuum heat treatment furnace, kept the temperature at 900-1000 DEG C
20-25h；(9) isothermal forging is processed into cylinder ingots by wire cutting mode, carries out isothermal forging on a hydraulic press；(10) hot rolling
Wire rod：Hot-rolled temperature：1400 DEG C -1425 DEG C, start rolling temperature：1425 DEG C, finishing temperature：1400℃；(11) stress relief annealing：?
In vacuum heat treatment furnace, 900-1000 DEG C of annealing temperature, 10h is kept the temperature；(12) multi pass drawing is carried out after rinsing obtains ferrum-chromium-aluminum
Lectrothermal alloy wire.
In another embodiment, alloying component：Cr：12.9%, Zr：5.3%, C：0.01%, Si：1.05%, Ni：
4%, Al：3.4%, Co：2.6%, Mo：2.5%, Nb：3.2%, Ti：0.6%, Ce：0.15%, La：0.13%, B：
0.006%, S：0.0001%, P：0.0001%, surplus is iron and inevitable impurity.
In any embodiment, aluminium foil and boron powder package are placed in furnace bottom before melting.
In any embodiment, Ce and La 4 minutes addition smelting furnaces before coming out of the stove after vacuumize process, are sufficiently stirred.
In any embodiment, while Ce and La is added, 0.01% Tb is added.
In any embodiment, further include：900 DEG C of wire rod are preheated 20 minutes.
In any embodiment, further include：Alkali leaching processing, pickling processes, coating treatment are carried out to wire rod.
In any embodiment, when drawing, using well-type electric furnace solution treatment, 1000-1200 DEG C of wire rod holding temperature,
Soaking time 2-3 hours, hardening was cooling.
The Fe-based perovskite-like oxide silk that any embodiment of the disclosure obtains, can be used for making 2-6mm wire rod.
In any embodiment, when drawing, protective atmosphere continuous heat treating furnace is used to carry out solution treatment, wire rod heat preservation
1000-1200 DEG C of temperature, soaking time 2-3 hours, outside tube water was cold.
It can be used for making 0.2-2mm wire rod, the cold mode of outside tube water can be improved the wire rod service life.
Method of disclosure improves the manufacture craft of Fe-based perovskite-like oxide silk, has the following advantages that：One, pass through alternation magnetic
, play the role of strong stirring, so that the condensation process of fusion process metal molten homogeneous and metal belt changes,
Ingot quality is improved, grain refinement effect is significant；Two, the content for having adjusted SI improves alloy thermal shock resistance, meanwhile,
Improve resistivity；Three, have the characteristics that impurity is low, toughness is strong, stretch-proof antioxygenic property is good；Four, high temperature hot rolling, sufficiently benefit
The characteristic for using temperature high with this alloy, effect of rolling are good.
Embodiment 1
The preparation method of Fe-based perovskite-like oxide silk provided in this embodiment includes：
(1) following proportion scale ingredient is pressed：Cr：12%, Zr：5%, Ni：3%, Nb：3%, Al:3%, Co：2%, Mo：
2%, Si：1.4%, Ti：0.5%, Ce：0.1%, La：0.1%, C：0.1%, B：0.001%, S：0.0001%, P：
0.0001%, surplus is iron and impurity；(2) melting processing, vacuum drying oven frequency are made in Medium frequency induction vacuum drying oven to above-mentioned ingredient
8KHz is set；(3) deoxidation：Aluminum deoxidation, the additional amount of aluminium are 1.5Kg/t, and deaeration time is greater than 20 minutes；(4) Argon, argon gas
Flow control is in 5L/min, argon blowing time 1min；(5) ingot casting, electromagnetic agitation ingot casting, frequency 25Hz, excitation current 450A；(6) powder
It is broken, ingot casting is crushed, grinding, obtains alloy powder；(7) discharge plasma is sintered, and sintering temperature is 1350 DEG C DEG C, and the time is
8-9h；(8) homogenizing annealing：In vacuum heat treatment furnace, 20-25h is kept the temperature at 900 DEG C；(9) isothermal forging passes through wire cutting
Mode is processed into cylinder ingots, carries out isothermal forging on a hydraulic press；(10) gren rod：Hot-rolled temperature：1400 DEG C, open rolling temperature
Degree：1425 DEG C, finishing temperature：1400℃；(11) stress relief annealing：In vacuum heat treatment furnace, 900 DEG C of annealing temperature, heat preservation
10h；(12) 900 DEG C of wire rod are preheated 20 minutes；(13) alkali leaching processing, pickling processes, coating treatment are carried out to wire rod；.(14)
Using well-type electric furnace solution treatment, 1000 DEG C of wire rod holding temperature, soaking time 2 hours, hardening was cooling.
Embodiment 2
The preparation method of Fe-based perovskite-like oxide silk provided in this embodiment includes：
(1) following proportion scale ingredient is pressed：Cr：13%, Zr：8%, Ni：5%, Nb：5%, Al:4%, Co：3%, Mo：
3%, Si：1.6%, Ti：1%, Ce：0.3%, La：0.2%, C：0.2%, B：0.01%, S：0.0002%, P：0.0002%,
Surplus is iron and impurity；(2) melting processing, vacuum drying oven set of frequency 10KHz are made in Medium frequency induction vacuum drying oven to above-mentioned ingredient；
(3) deoxidation：Aluminum deoxidation, the additional amount of aluminium are 2Kg/t, and deaeration time is greater than 20 minutes；(4) Argon, argon gas flow control is in 8L/
Min, argon blowing time 2min；(5) ingot casting, electromagnetic agitation ingot casting, frequency 30Hz, excitation current 500A；(6) it crushes, by ingot casting powder
Broken, grinding, obtains alloy powder；(7) discharge plasma is sintered, and sintering temperature is 1400 DEG C, time 8-9h；(8) uniformly
Annealing：In vacuum heat treatment furnace, 25h is kept the temperature at 1000 DEG C；(9) isothermal forging is processed into cylinder by wire cutting mode
Ingot carries out isothermal forging on a hydraulic press；(10) gren rod：Hot-rolled temperature：1350 DEG C -1425 DEG C, start rolling temperature：1425
DEG C, finishing temperature：1350℃；(11) stress relief annealing：In vacuum heat treatment furnace, 1000 DEG C of annealing temperature, 10h is kept the temperature；
(12) 900 DEG C of wire rod are preheated 20 minutes；(13) alkali leaching processing, pickling processes, coating treatment are carried out to wire rod；.(14) it uses
Well-type electric furnace solution treatment, 1000 DEG C of wire rod holding temperature, soaking time 2 hours, hardening was cooling.
Embodiment 3
The preparation method of Fe-based perovskite-like oxide silk provided in this embodiment includes：
(1) following proportion scale ingredient is pressed：Cr：12.5%, Zr：5.6%, Ni：3.4%, Nb：3.5%, Al:3.4%,
Co：2.3%, Mo：2.3%, Si：1.35%, Ti：0.57%, Ce：0.18%, La：0.15%, C：0.18%, B：0.008%,
S：0.00014%, P：0.00014%, surplus is iron and impurity；(2) melting is made in Medium frequency induction vacuum drying oven to above-mentioned ingredient
Processing, vacuum drying oven set of frequency 9KHz；(3) deoxidation：Aluminum deoxidation, the additional amount of aluminium are 1.8Kg/t, and deaeration time is greater than 20 points
Clock；(4) Argon, argon gas flow control is in 8L/min, argon blowing time 2min；(5) ingot casting, electromagnetic agitation ingot casting, frequency 30Hz, excitation
Electric current 500A；(6) it crushes, ingot casting is crushed, grinding, obtain alloy powder；(7) discharge plasma is sintered, and sintering temperature is
1400 DEG C, time 8-9h；(8) homogenizing annealing：In vacuum heat treatment furnace, 25h is kept the temperature at 1000 DEG C；(9) isothermal forging,
Cylinder ingots are processed by wire cutting mode, carry out isothermal forging on a hydraulic press；(10) gren rod：Hot-rolled temperature：1350
DEG C -1425 DEG C, start rolling temperature：1425 DEG C, finishing temperature：1350℃；(11) stress relief annealing：In vacuum heat treatment furnace, move back
1000 DEG C of fiery temperature keeps the temperature 10h；(12) 900 DEG C of wire rod are preheated 20 minutes；(13) to wire rod progress alkali leaching processing, pickling
Reason, coating treatment；.(14) solution treatment, wire rod holding temperature 1000-1200 are carried out using protective atmosphere continuous heat treating furnace
DEG C, soaking time 2-3 hours, outside tube water was cold.
By testing alloy wire provided in this embodiment, it is as follows to obtain data：1425 DEG C of maximum operating temperature,
Room temperature resistivity is up to 2.4 Ω mm2/ m, tensile strength is up to 1150MPa, and up to 19%, Oxidation Resistance Test weight gain is less than elongation percentage
2.4mg/cm2.Alloy wire made from embodiment is put into 1000 DEG C of atmosphere furnaces, 15min is kept the temperature, is then placed in anxious in cold water
Quickly cooling but, executes aforesaid operations 50 times repeatedly, it is found that the variation of above-mentioned test result between 0.2-0.8%, has stronger
Stability.The alloy wire that the embodiment of the present disclosure provides is better than the wire rod that the prior art can be prepared.
Disclosed method improves the manufacture craft of Fe-based perovskite-like oxide silk, has the following advantages that：One, pass through friendship
Varying magnetic field plays the role of strong stirring, so that the condensation process of fusion process metal molten homogeneous and metal belt changes
Become, improves ingot quality, grain refinement effect is significant；Two, the content for having adjusted SI improves alloy thermal shock resistance, together
When, improve resistivity；Three, have the characteristics that impurity is low, toughness is strong, stretch-proof antioxygenic property is good；Four, high temperature hot rolling is filled
Divide the characteristic high using temperature using this alloy, effect of rolling is good.
Obviously, those skilled in the art can carry out various modification and variations without departing from the essence of the disclosure to the disclosure
Mind and range.In this way, if these modifications and variations of the disclosure belong to the range of disclosure claim and its equivalent technologies
Within, then the disclosure is also intended to include these modifications and variations.
Claims (10)
1. a kind of preparation method of Fe-based perovskite-like oxide silk, which is characterized in that successively include the following steps：
(a) discharge plasma is sintered；
(b) it makes annealing treatment；
(c) isothermal forging；
(d) gren rod；
(e) stress relief annealing；And
(f) multi pass drawing obtains Fe-based perovskite-like oxide silk.
2. the method as described in claim 1, which is characterized in that include the following steps：
(1) ingredient：(2) Medium frequency induction vacuum drying oven melting；(3) deoxidation；(4) Argon；(5) ingot casting；(6) it crushes；(7) electric discharge etc. from
Daughter sintering；(8) it anneals；(9) isothermal forging；(10) gren rod；(11) stress relief annealing；(12) drawing.
3. the method as described in claim 1, which is characterized in that
(1) following proportion scale ingredient is pressed：Cr：12-13%, Zr：5-8%, Ni：3-5%, Nb：3-5%, Al:3-4%, Co：
2-3%, Mo：2-3%, Si：1.4-1.6%, Ti：0.5-1%, Ce：0.1-0.3%, La：0.1-0.2%, C：0.1-0.2%,
B：0.001-0.01%, S：0.0001-0.0002%, P：0.0001-0.0002%, surplus are iron and impurity；(2) match to above-mentioned
Material makees melting processing, vacuum drying oven set of frequency 8-10KHz in Medium frequency induction vacuum drying oven；(3) deoxidation：Aluminum deoxidation, aluminium add
Entering amount is 1.5-2Kg/t, and deaeration time is greater than 20 minutes；(4) Argon：Argon gas flow control is in 5-8L/min, argon blowing time 1-
2min；(5) ingot casting：Electromagnetic agitation ingot casting, frequency 25-30Hz, excitation current 450-500A；(6) it crushes：Ingot casting is crushed, is ground
Mill, obtains alloy powder；(7) discharge plasma is sintered：Sintering temperature is 1350-1400 DEG C, time 8-9h；(8) uniformly
Annealing：In vacuum heat treatment furnace, 20-25h is kept the temperature at 900-1000 DEG C；(9) isothermal forging：It is processed by wire cutting mode
At cylinder ingots, isothermal forging is carried out on a hydraulic press；(10) gren rod：Hot-rolled temperature：1400 DEG C -1425 DEG C, start rolling temperature：
1425 DEG C, finishing temperature：1400℃；(11) stress relief annealing：In vacuum heat treatment furnace, 900-1000 DEG C of annealing temperature, protect
Warm 10h；(12) multi pass drawing is carried out after rinsing obtains Fe-based perovskite-like oxide silk.
4. method as claimed in claim 3, which is characterized in that the alloying component prepared：Cr：12.9%, Zr：5.3%, C：
0.01%, Si：1.05%, Ni：4%, Al：3.4%, Co：2.6%, Mo：2.5%, Nb：3.2%, Ti：0.6%, Ce：
0.15%, La：0.13%, B：0.006%, S：0.0001%, P：0.0001%, surplus is iron and inevitable impurity.
5. method as claimed in claim 3, which is characterized in that aluminium foil and boron powder package are placed in furnace bottom before melting.
6. method as claimed in claim 5, which is characterized in that Ce and La 4 minutes addition smelting furnaces, vacuumize process before coming out of the stove
Afterwards, it is sufficiently stirred.
7. method as claimed in claim 6, which is characterized in that while Ce and La is added, 0.01% Tb is added.
8. method according to claim 2, which is characterized in that further include：900-1000 DEG C of wire rod is preheated 20 minutes, and
Alkali leaching processing, pickling processes, coating treatment are carried out to wire rod.
9. method according to claim 2, which is characterized in that when drawing, use well-type electric furnace solution treatment, wire rod heat preservation temperature
1000-1200 DEG C of degree, soaking time 2-3 hours, hardening was cooling.
10. method according to claim 2, which is characterized in that when drawing, consolidated using protective atmosphere continuous heat treating furnace
Molten processing, 1000-1200 DEG C of wire rod holding temperature, soaking time 2-3 hours, outside tube water was cold.
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