CN108251753A - A kind of high-magnetostriction coefficient Fe-Ga base strips and preparation method thereof - Google Patents
A kind of high-magnetostriction coefficient Fe-Ga base strips and preparation method thereof Download PDFInfo
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- CN108251753A CN108251753A CN201810126561.4A CN201810126561A CN108251753A CN 108251753 A CN108251753 A CN 108251753A CN 201810126561 A CN201810126561 A CN 201810126561A CN 108251753 A CN108251753 A CN 108251753A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000000137 annealing Methods 0.000 claims abstract description 136
- 238000005096 rolling process Methods 0.000 claims abstract description 102
- 238000001953 recrystallisation Methods 0.000 claims abstract description 88
- 238000005097 cold rolling Methods 0.000 claims abstract description 76
- 238000010438 heat treatment Methods 0.000 claims abstract description 52
- 238000005121 nitriding Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000009749 continuous casting Methods 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 23
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- 238000005554 pickling Methods 0.000 claims description 48
- 238000005098 hot rolling Methods 0.000 claims description 47
- 238000001816 cooling Methods 0.000 claims description 40
- 238000011282 treatment Methods 0.000 claims description 25
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- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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Abstract
The present invention relates to a kind of high-magnetostriction coefficient Fe Ga base strips and preparation method thereof.The present invention can simply and efficiently carry out large-scale production using the slab of molding, sheet billet continuous casting, sheet blank continuous casting and thin strap continuous casting using traditional rolling and annealing process;The inhibitor system of the intrinsic inhibitor+nitriding of low temperature is established, tiny Cu is precipitated in control heat treatment and rolling mill practice2S, Nb (C, N) and V (C, N) or its miscible precipitate are as main intrinsic inhibitor, when intrinsic restraint deficiency, it supplements to form the nitride such as AIN or BN using nitriding before secondary recrystallization annealing, realizes restraint flexible control;Finely regulating Cold-rolling Parameters ensure that primary recrystallization obtains the tissue of fine uniform and advantageous texture, realize the coordination matching of tissue, texture and inhibitor before secondary recrystallization, are improved and sharp Goss ({ 110 }<001>) texture secondary recrystallization.Fe Ga bases strip finished product magnetostriction coefficient (3/2) λ s of the present invention are up to 220~370ppm.
Description
Technical field
The invention belongs to technical field of magnetic materials, more particularly to a kind of high-magnetostriction coefficient Fe-Ga bases strip and its
Preparation method.
Background technology
Magnetostriction materials refer to that its length changes under magnetic fields and generate displacement acting or under alternating magnetic field
Cyclic extension occurs and generates vibration or sound wave with shortening, so as to convert electromagnetic energy into the intellectual material of mechanical energy or acoustic energy.It
Sonar underwater acoustic transducer, electroacoustic transducer, marine exploration and exploitation, Micro-displacement Driving, vibration damping and vibrationproof, intelligent mechanism with from
The high-technology fields such as dynamicization are widely used, and are important energy and information transition material.
Magnetostriction materials mainly include rare earth ultra-magnetostriction material Tb-Dy-Fe and traditional magnetostriction materials Fe-
Ni, Fe-Al etc..Although Tb-Dy-Fe, due to intrinsic brittleness and expensive price, limits it with very big magneto-strain value
Use scope.There is magnetostriction coefficient is small, energy density is low etc. in Fe-Ni, Fe-Al etc..
Fe-Ga (Galfenol) alloys are because with magnetostriction coefficient is larger, tensile strength is high, saturation magnetic field is small, magnetic conductance
The features such as rate is high, price is low, becomes the magnetostriction materials for having both big magnetostriction coefficient and excellent mechanical property.
Fe-Ga alloys Magnetostriction is in notable anisotropy,<100>Direction magnetostriction coefficient is maximum, i.e. monocrystalline λ 100
=271ppm.(S Guruswamy,N Srisukhumbowornchai,A E Clark,J B Restorff,and M Wun-
Fogle.Strong ductile and low-field-magnetostrictive alloys based on Fe-
Ga.Scripta.mater.,2000,43:239-244;N Srisukhumbowornchai and S Guruswamy.Large
magnetostriction in directionally solidified FeGa and FeGaAl
alloys.J.Appl.Phys.,2001,90(11):5680-5688).Since Fe-Ga alloy monocrystallines manufacturing cost is high and high
Using being also easy to produce serious eddy-current loss under the conditions of frequency, thus the high efficiency based on rolling need to be developed, low cost prepare η (<100>//
RD) the method for texture Fe-Ga polycrystalline alloy strip.Rolling, which prepares excellent magnetic, to be stretched the key technologies of Fe-Ga strips and is to stablize
Forming and secondary recrystallization texture controlling.
2007, S M Na et al. reported rolling Fe81.3Ga18.7A small amount of B and S are added in alloy, is obtained approximate vertical
Square texture ({ 001 }<100>) or approximation Goss ({ 110 }<100>) texture, highest magnetostriction coefficient for 220ppm (S M Na,
A B Flatau.Secondary recrystallization crystallographic texture and
magnetostriction in rolled Fe-Ga based alloys.J.Appl.Phys.,2007,101:09N518)。
2011, S M Na et al. also reported added 1at%NbC in Fe-Ga is rolled, containing 0.5%H2Pass through height in the Ar gas of S
Temperature processing and surface can induce and obtain strong Goss ({ 110 }<001>) texture, magnetostriction coefficient reaches 292ppm (S M
Na,A B Flatau.Single grain growth and large magnetostriction in secondarily
recrystallized Fe-Ga thin sheet with sharp Goss(011)[100]
orientation.Scripta.Mater.,2012,66:307-310).Yuan Chao in 2015 et al. reports solidifying in rolling orientation
Solid Fe-Ga in add 0.1at%NbC, in the slow temperature-rise period of strip is rolled by S come realize surface can induce obtain it is strong
Goss texture, magnetostriction coefficient reach 245ppm (Chao Yuan, Jiheng Li, Wen lan Zhang, Xiao qian
Bao,Xuexu Gao.Sharp Goss orientation and large magnetostriction in the rolled
columnar-grained Fe–Ga alloys.J.Magn.Magn.Mater.,2015,374:459-462)。
United States Patent (USP) US2009/0039714A1 adds Al, Be and more than 1mol.%NbC, packet in Fe-Ga alloys
It is anti-oxidation to cover hot rolling, by hot rolling, two step warm-rollings and subsequent heat treatment, obtains the Fe-Ga strips with η texture.Chinese patent
CN101465406A, B, Cr, Nb, VC, TiC, MnS, the AlN of addition atomic ratio more than 0.5% and a small amount of S, Sn, Sb element,
Rely on the H of low content (volume ratio 0.001-0.008%)2S or O2In higher than 900 DEG C of long heat treatments, obtain Goss or
Cubic texture Fe-Ga thin plates.Chinese patent CN103014594A adds a small amount of Al, Nb, C, B as inhibitor formation element, adopts
Element is induced by the use of S as secondary recrystallization, by secondary recrystallization heat treatment and reducing atmosphere high-temperature heat treatment, is had
The magnetostriction strip of strong Goss texture.
Research or patent above with respect to Fe-Ga magnetostriction alloy thin slices, inhibitor control and secondary recrystallization process
It mismatches, largely needs introducing surface segregation that Goss crystal grain is promoted to improve secondary recrystallization.The introducing of surface segregation, one
Aspect cost increases, equipment precision requirement is high, on the other hand must 1200 DEG C or higher temperature annealing acquisition improve it is secondary again
Crystallization and elimination S elements cause Ga volatilizations serious the adverse effect of magnetic property.Although Chinese patent CN 104711475A, lead to
It crosses 5%~15%mol%Al of addition and nitriding twice is carried out after hot rolling and cold rolling, to remove the dependence to surface segregation,
But higher Al content reduces magnetostriction coefficient and twice nitriding complex procedures.Relatively low another of the studies above Magnetostriction
One main cause is that the secondary recrystallization degree of orientation is relatively low, and regulates and controls the coordination before secondary recrystallization between tissue, texture and inhibitor
Matching is the key that improve the secondary recrystallization degree of orientation.
In conclusion develop the high-magnetostriction coefficient Fe-Ga bases that a kind of production efficiency is high, at low cost and performance is stablized
Alloy thin band preparation method is current urgent problem.
Invention content
For the above problem existing for existing Fe-Ga alloy preparation techniques, the present invention proposes a kind of high-magnetostriction system
The preparation method of number Fe-Ga base strips, mentality of designing are as follows:
1) using the slab of molding, sheet billet continuous casting, sheet blank continuous casting and thin strap continuous casting, traditional rolling and annealing are utilized
Simply and efficiently prepared by scale for technological process;
2) inhibitor system of the intrinsic inhibitor+nitriding of low temperature is established, control heat treatment and rolling mill practice are precipitated tiny
Cu2S, AIN, Nb (C, N) and V (C, N) or its miscible precipitate are as main intrinsic inhibitor;When intrinsic restraint deficiency
When, it supplements to form nitride using nitriding before secondary recrystallization annealing, is improved by selectivity induction and texture is sharp
Secondary recrystallization tissue;
3) finely regulating rolling parameter with ensure primary recrystallization obtain fine uniform tissue and suitable texture.
From the angle for coordinating collocation between optimizing tissue, texture and inhibitor, sharp secondary recrystallization Goss texture is obtained,
Improve the magnetic hysteresis telescopicing performance of Fe-Ga based alloy strips.
Technical scheme is as follows:
High-magnetostriction coefficient Fe-Ga base strips, ingredient are by weight percentage:Ga:15~32%, C:0.001~
0.12%, Al:0.005~0.08%, Nb:0.03~0.75%, surplus is Fe and other inevitable impurity.
Further, the high-magnetostriction coefficient Fe-Ga base strips, ingredient also contain by weight percentage:Cu:
≤ 0.5%, S:0.008~0.035%, Mn:0.01~0.3%.
Further, the high-magnetostriction coefficient Fe-Ga base strips, ingredient also contain by weight percentage:Sn:
0.02~0.1%, Sb:0.01~0.03.%, V:0.01~0.1%, Mo:0.01~3.0%, Tb:0.05~0.6%, N:
0.006~0.02% or B:It is one or more in 0.005~0.05%.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1:It smelts
By the set component of strip, cast after being smelted at a temperature of 1440~1600 DEG C;
Step 2:Hot rolling
(1) by blank heating to 1000~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 900~1250 DEG C of start rolling temperature, finishing temperature 600~1050
DEG C, 4~8 passage of hot rolling, hot rolling total reduction 50~99%, the hot rolled plate of acquisition 1~4mm thickness after cooling;
Step 3:Pickling and cold rolling
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, obtains the thin strip cold of 0.10~1.0mm thickness;
Step 4:Decarburizing annealing
By thin strip cold in wet N2+H2Mixed atmosphere in, carry out decarburizing annealing, annealing temperature be 800~1000 DEG C, move back
The fiery time is 2~30min, N2Shared volume ratio is 20~75%;
Step 5:Secondary recrystallization is annealed
The annealed sheet that will be obtained after decarburizing annealing, inert atmosphere or inertia reduction mixed atmosphere under the conditions of carry out it is secondary again
Recrystallization annealing temperature processing, obtains high-magnetostriction coefficient Fe-Ga base strips.
Further, it casts in step 1, after the smelting and molding, sheet billet continuous casting, sheet blank continuous casting and strip can be used
Any one process in continuous casting is realized.
Further, in the step 3 (1), pickling is carried out again after carrying out normalizing annealing processing to hot rolled plate, normalizing is moved back
Fiery temperature be 700~1100 DEG C, the normalizing annealing time be 2~120min, rapid cooling after normalizing.
Further, including following two rollings, any one rolling can be used in the cold rolling described in step 3 (2)
Carry out cold rolling:
Rolling:Warm cold rolling is first carried out, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, Ran Houjin
The relatively low warm cold rolling of trip temperature, rolling temperature are room temperature~600 DEG C, and reduction ratio is 10~92%;
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, then
The rapid cooling after 800~1100 DEG C of 5~120min that anneal, second of warm cold rolling relatively low for temperature, rolling temperature is room temperature~600
DEG C, reduction ratio is 50~92%.
Further, the secondary recrystallization annealing described in step 5, including the following two kinds pattern:
Pattern one:Annealed sheet is heated to 1000~1200 DEG C from 600~900 DEG C and keeps the temperature 0.5~10h, heating process
Using continuous warming or the multisection type containing moderate soak is annealed
Pattern two:Annealed sheet is subjected to 15~600min cycle annealings at 900~1200 DEG C.
Further, inert atmosphere refers to nitrogen atmosphere or argon gas atmosphere in step 5;The inertia reduction mixed atmosphere
Refer to the mixed atmosphere of inert gas and hydrogen.
Further, the secondary recrystallization annealing described in step 5, stove is can be used after the completion of secondary recrystallization annealing
Any one mode cools down in cold, air-cooled or quenching.
The preparation method of second of high-magnetostriction coefficient Fe-Ga base strip, includes the following steps:
Step 1:It smelts
By the set component of strip, cast after being smelted at a temperature of 1440~1600 DEG C;
Step 2:Hot rolling
(1) by blank heating to 1000~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 900~1250 DEG C of start rolling temperature, finishing temperature 600~1050
DEG C, 4~8 passage of hot rolling, hot rolling total reduction 50~99%, the hot rolled plate of acquisition 1~4mm thickness after cooling;
Step 3:Pickling and cold rolling
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, obtains the thin strip cold of 0.10~1.0mm thickness;
Step 4:Decarburizing annealing
By thin strip cold in wet N2+H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature is 800~1000 DEG C, annealing
Time is 2~30min, N2Shared volume ratio is 20~75%;
Step 5:Nitrizing Treatment
By strip in dry NH3+N2+H2Mixed atmosphere in carry out Nitrizing Treatment;
Step 6:Secondary recrystallization is annealed
The annealed sheet that decarburizing annealing is obtained under the conditions of inert atmosphere or inertia reduction mixed atmosphere secondary tie again
Crystalline substance annealing, obtains high-magnetostriction coefficient Fe-Ga base strips.
Further, in step 1, after the smelting casting molding, sheet billet continuous casting, sheet blank continuous casting and thin can be used
It is realized with any one process in continuous casting.
Further, in the step 3 (1), pickling is carried out again after carrying out normalizing annealing processing to hot rolled plate, normalizing is moved back
Fiery temperature be 700~1100 DEG C, the normalizing annealing time be 2~120min, rapid cooling after normalizing.
Further, including following two rollings, any one rolling can be used in the cold rolling described in step 3 (2)
Carry out cold rolling:
Rolling:Warm cold rolling is first carried out, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, Ran Houjin
The warm cold rolling of row lower temperature, rolling temperature are room temperature~600 DEG C, and reduction ratio is 10~92%;
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, then
The rapid cooling after 800~1100 DEG C of 5~120min that anneal, second of warm cold rolling relatively low for temperature, rolling temperature is room temperature~600
DEG C, reduction ratio is 50~92%.
Further, the Nitrizing Treatment process described in step 5;The NH3+N2+H2In mixed atmosphere, H2Shared body
Product is than being 50~80%, NH3Shared volume ratio is 5~30%, and nitriding temperature is 600~1050 DEG C, and the time is 10~500s, is oozed
Nitrogen quantity is 30~800ppm.
Further, the secondary recrystallization annealing described in step 6, including the following two kinds pattern:
Pattern one:Annealed sheet is heated to 1000~1200 DEG C from 600~900 DEG C and keeps the temperature 0.5~10h, heating process
Using continuous warming or the multisection type containing moderate soak is annealed
Pattern two:Annealed sheet is subjected to 15~600min cycle annealings at 900~1200 DEG C.
Further, inert atmosphere refers to nitrogen atmosphere or argon gas atmosphere in step 6;The inertia reduction mixed atmosphere
Refer to the mixed atmosphere of inert gas and hydrogen, mixed proportion is arbitrary proportion.
Further, the secondary recrystallization annealing described in step 6, stove is can be used after the completion of secondary recrystallization annealing
Any one mode cools down in cold, air-cooled or quenching.
Further, the step 5 Nitrizing Treatment can move back before decarburizing annealing, after decarburizing annealing or with decarburization
Fire is synchronous to carry out
The principle of the present invention is as follows:
In high-magnetostriction coefficient Fe-Ga base strips, the weight percent content of C and N are respectively 0.001~0.12% He
0.006~0.02%, Nb (C, N), V (C, N), Fe can be formed3C, the precipitated phases such as AlN inhibit primary recrystallization crystal grain, cold rolling
Process can also promote formation of shear bands, increase Goss grain nucleations position, and a certain amount of C also helps to improve Fe-Ga in addition
The magnetostriction coefficient of alloy.
Al weight percent contents 0.005~0.08%.During the restraint deficiency of intrinsic inhibitor, in Nitrizing Treatment process
In, Al inhibits matrix grain by reacting generation AIN precipitated phases with N, as inhibitor in the heating later stage slowly.Al content is less than
0.005% supplement restraint is insufficient, and excessively high also unfavorable to Magnetostriction more than 0.08% restraint.
The weight percent content of Cu and S is respectively≤0.5% and 0.008~0.035%.In hot rolling and then heat treatment
Process forms Cu2S inhibits matrix grain as intrinsic inhibitor in slow temperature-rise period.Their solid solubility temperatures are very low, are conducive to
Reduce slab heating temperature.
The weight percent content of B is 0.005~0.05%.Modeling is improved by crystal grain thinning and raising crystal boundary binding force
Property, BN can also be formed and strengthen restraint.
The weight percent content of Mn is 0.01~0.3%.Mn plays desulfidation and formation MnS Pinning crystal grain is long
Greatly.
The weight percent content of Nb and V is respectively 0.03~0.75% and 0.01~0.1%.By thinning microstructure and carry
High crystal boundary binding force improves plasticity, also crystal grain can be inhibited to grow up by being dissolved and being formed Nb (C, N), V (C, N).
The weight percent content of Sn and Sb is respectively 0.01~0.1% and 0.01~0.03%.As cyrystal boundary segregation member
Element can assist enhancing restraint.
The weight percent content of Mo is 0.01~3.0%.Help to improve plasticity and homogenization primary recrystallization crystal grain;
Mo can also be enriched in surface when being heated at high temperature slab prevents grain boundary oxidation, enhances ductility.
The weight percent content of Tb is 0.05~0.6%.Its precipitated phase can assist pinning crystal boundary to move, and can also pass through
It generates distortion of lattice and influences phase transformation to promote magnetostriction coefficient.
The preparation method of high-magnetostriction coefficient Fe-Ga base strips of the present invention, when using molding, sheet billet continuous casting and sheet billet
During the technique of continuous casting, make coarse Cu in 1000 DEG C or more heat preservations before hot rolling2S, Nb (C, N) and V (C, N) etc. be completely or partially
Solid solution, then in a large amount of tiny precipitate of hot rolling and follow-up heat treatment process deformation-induced precipitation, so as to improve intrinsic inhibitor
Intensity.
The preparation method of high-magnetostriction coefficient Fe-Ga base strips of the present invention when using the technique of thin strap continuous casting, utilizes
The characteristics of thin strap continuous casting Sub realizable fuzzy matrix, (setting rate was up to 102~104DEG C/s), more inhibitor groups can be dissolved in Cast Strip
Point, realize restraint flexible control.
Cold-rolled process uses different rolling temperature and reduction ratio, obtains and advantageous ties again from regulation and control deformation micro-structure angle
Brilliant texture and tissue signature especially regulate and control the quantity and the angle of deviation of primary recrystallization Goss nucleus, to improve secondary recrystallization
Accuracy.The addition of the elements such as Nb and V is to Recrystallization nucleation and grows up and has larger impact, is conducive to obtain the first of fine uniform
Recrystallized structure and advantageous primary recrystallization texture.Different inhibitor systems and content are formed, need to match it is different just
Secondary recrystallized structure and texture could realize perfect secondary recrystallization.Therefore, it is necessary to regulate and control Cold-rolling Parameters realization tissue, knit
The coordination collocation of structure and restraint.
The purpose of nitridation process of the present invention is to form the nitride such as AlN or BN before secondary recrystallization to supplement to inhibit
Power, high-temperature annealing process effectively can inhibit matrix grain to grow, and are conducive to accurate Goss crystal grain and sent out in suitable temperature range
Secondary recrystallization is improved in life, obtains excellent Magnetostriction.When the control of intrinsic inhibitor is met the requirements, it is convenient to omit ooze
Nitrogen treatment process, but appropriate nitriding is conducive to final finished with superior Magnetostriction.
Secondary recrystallization annealing process of the present invention regulates and controls annealing schedule, heating rate and annealing atmosphere, it is therefore intended that makes
Restraint decline matches with accurate Goss abnormal growths process, this extremely closes control secondary recrystallization sophistication and the degree of orientation
It is important.
High-magnetostriction coefficient Fe-Ga base strips of the present invention and preparation method thereof, compared with prior art, advantageous effect
For:
1st, using molding, sheet billet continuous casting, sheet blank continuous casting and thin strap continuous casting, traditional rolling and annealing process stream are utilized
Journey prepares to stability and high efficiency the big magnetic hysteresis coefficient of dilatation Fe-Ga alloy thin bands with sharp Goss secondary recrystallizations texture, improves
Production efficiency reduces production cost.
2nd, it using intrinsic inhibitor or another plus acquisition type inhibitor design, is precipitated by heat treatment and rolling mill practice tiny
Cu2S, AIN, Nb (C, N) and V (C, N) or its miscible precipitate are as main intrinsic inhibitor.When intrinsic restraint deficiency
When, nitridation process is adjusted in due course forms the nitride such as AIN or BN supplement restraint, with reference to regulation and control secondary recrystallization annealing atmosphere,
Realize restraint flexible control.Coordinate matched angle from optimization inhibitor, tissue and texture, given birth to using the selection of Goss crystal grain
Long advantage is improved and is orientated sharp secondary recrystallization;
3rd, finely regulating Cold-rolling Parameters, primary recrystallization obtain the tissue and favorable texture of fine uniform, and raising is secondary again
The degree of orientation of crystal grain, so as to promote Fe-Ga alloy magnetic hysteresis coefficient of dilatation.
4th, stable formation and texture controlling are realized by reasonable control composition and technological parameter, finally obtains 0.1~1.0mm
Thick Fe-Ga strip finished products, magnetostriction coefficient (3/2) λ s are up to 220~370ppm.
In conclusion the method that a kind of rolling of the present invention prepares high-magnetostriction coefficient Fe-Ga base strips, in inhibitor
It controls and its is matched down with the coordination of tissue, texture, realize that rolling high efficiency and low cost prepare high-orientation Fe-Ga based alloys
Strip has broad application prospects.
Description of the drawings
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or it will show below
There is attached drawing needed in technology description to be briefly described.It should be evident that the accompanying drawings in the following description is only this
Section Example described in application.
Fig. 1 is the preparation method flow diagram of the high-magnetostriction coefficient Fe-Ga base strips of the present invention;
Fig. 2 passes through secondary recrystallization for the 4th group of high-magnetostriction coefficient Fe-Ga bases strip in the table 2 of the embodiment of the present invention 2
The ODF of sample is permanent after annealingSectional view;
Fig. 3 is the microstructure after high-magnetostriction coefficient Fe-Ga base strip sample decarburizing annealings in the embodiment of the present invention 6
Figure, wherein, horizontal direction be RD directions, vertical direction TD directions.
Fig. 4 (a) is that the 3rd group of high-magnetostriction coefficient Fe-Ga base strip is moved back by secondary recrystallization in the embodiment of the present invention 8
Macroscopic organization chart after fire;
Fig. 4 (b) is that the 4th group of high-magnetostriction coefficient Fe-Ga base strip is moved back by secondary recrystallization in the embodiment of the present invention 8
Macroscopic organization chart after fire.
Specific embodiment
Technical scheme of the present invention is further described in detail with reference to example.
Embodiment 1
High-magnetostriction coefficient Fe-Ga base strips, constituent contain by weight percentage:C:0.03%, Al:
0.03%, Nb:0.25%, Cu:0.5%%, Mn:0.08%, S:0.02%, Sn:0.06%, Mo:0.5%, surplus for Fe and
Other inevitable impurity, Ga contents are different as shown in table 1.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip in table 1, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, it is thick to obtain 2.5mm for 1150~1200 DEG C of start rolling temperature after cooling
Hot rolled plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) hot rolled plate after pickling is subjected to cold rolling, the thin strip cold of 0.25mm thickness is obtained using secondary rolling,
In:
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is 400~800 DEG C, reduction ratio 40%, then 950
Rapid cooling after DEG C annealing 40min, the second warm cold rolling relatively low for temperature, rolling temperature is 300 DEG C, reduction ratio 83%;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 850 DEG C, annealing time 4min;
Step 5, Nitrizing Treatment:
It is 10%NH in dry volume ratio by strip3+ 20%N2+ 70%H2Nitrizing Treatment, nitriding are carried out in mixed atmosphere
Temperature is 900 DEG C, and nitriding amount is 160ppm;
Step 6, secondary recrystallization is annealed:
By annealed sheet under inert atmosphere conditions, 950 DEG C are heated to from 800 DEG C of speed with 20 DEG C/h and keep the temperature 2h, so
1150 DEG C are heated to the speed of 15 DEG C/h keep the temperature 4h afterwards, it is air-cooled to obtain high-magnetostriction coefficient Fe-Ga base strips, measure difference
The results are shown in Table 1 by magnetostriction coefficient (3/2) λ s of high-magnetostriction coefficient Fe-Ga base strips made from Ga contents.
The magnetostriction coefficient contrast table of 1 difference of table high-magnetostriction coefficient Fe-Ga base strips made from Ga contents
Serial number | Ga contents (weight percent %) | Secondary recrystallization completeness (%) | (3/2)λs(ppm) |
1 | 15.0 | 100 | 220 |
2 | 17.2 | 100 | 280 |
3 | 21.8 | 100 | 310 |
4 | 22.6 | 100 | 355 |
5 | 23.5 | 100 | 342 |
6 | 27.1 | 100 | 295 |
7 | 32.0 | 100 | 330 |
As it can be seen from table 1 when secondary recrystallization develop it is perfect, Ga contents become influence magnetic hysteresis telescopicing performance it is crucial because
One of element, result is consistent with influence of the Ga contents to monocrystalline magnetostriction coefficient, absolutely proves and is precisely controlled Ga contents to Fe-
The importance of Ga alloy magnetic hysteresis telescopicing performances.
Embodiment 2
High-magnetostriction coefficient Fe-Ga base strips, constituent and weight percent content are Ga:22.3%, it is other
Constituent is as shown in table 2, and surplus is Fe and other inevitable impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip in table 2, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1250 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, it is thick to obtain 2.3mm for 1100~1200 DEG C of start rolling temperature after cooling
Hot rolled plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) hot rolled plate after pickling is subjected to cold rolling, the thin strip cold of 0.2mm thickness is obtained using secondary rolling, wherein:
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is 400~800 DEG C, reduction ratio 56%, then 900
Rapid cooling after DEG C annealing 30min, the second warm cold rolling relatively low for temperature, rolling temperature is 200 DEG C, reduction ratio 80%;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 875 DEG C, annealing time 5min;
Step 5, Nitrizing Treatment:
It is 15%NH in dry volume ratio by strip3+ 15%N2+ 70%H2Nitrizing Treatment, nitriding are carried out in mixed atmosphere
Temperature is 800 DEG C, and nitriding amount is 180ppm;
Step 6, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 1200 DEG C are heated to simultaneously from 800 DEG C of speed with 20 DEG C/h
2h is kept the temperature, quenching obtains high-magnetostriction coefficient Fe-Ga base strips, measures the high-magnetostriction coefficient of heterogeneity and content
The results are shown in Table 2 by magnetostriction coefficient (3/2) λ s of Fe-Ga base strips.
The ODF of the 4th group of high-magnetostriction coefficient Fe-Ga bases strip sample after secondary recrystallization is annealed is permanent in table 2
Section, as shown in Figure 2.
The Magnetostriction contrast table of the high-magnetostriction coefficient Fe-Ga base strips of the different constituents of table 2 and content
Single sharp Goss texture is obtained after secondary recrystallization as can be seen from Figure 2, therefore magnetostriction coefficient reaches
To 327ppm, the control level for illustrating secondary recrystallization texture is the key that determine one of Fe-Ga alloy magnetostriction performances.
The 10th~12 group in table 2 is contrast experiment, from Table 2, it can be seen that when Fe-Ga alloy thin band constituent weights
Amount degree is in the scope of the invention (serial number 1~9), and inhibitor Effective Regulation is realized with nitriding by controlling to be precipitated,
Promote secondary more perfect in crystallization, raising magnetic hysteresis telescopicing performance.Conversely, when Fe-Ga alloy thin band constituent weight percents
Than content beyond the scope of the invention (contrast experiment 10~12), then restraint intensity is too strong or too weak, it is difficult to obtain ideal
Secondary recrystallization, Magnetostriction are relatively low.
Embodiment 3
High-magnetostriction coefficient Fe-Ga base strips, constituent contain by weight percentage:Ga:20.4%, C:
0.05%, Nb:0.1%, Cu:0.2%%, Mn:0.08%, S:0.015%, Mo:0.05%, Tb:0.3, surplus is Fe and its
Its inevitable impurity, Al content are different as shown in table 3.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip in table 3, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) slab after heating and thermal insulation is subjected to hot rolling, 1150 DEG C of start rolling temperature obtains 4mm thickness hot rolled plates after cooling;
Step 3, pickling and cold rolling:
(1) hot rolling is subjected to pickling to remove oxide;
(2) by hot rolled plate after 1050 DEG C of normalizing annealings rapid cooling, annealing time 5min, then using a rolling,
Rolling temperature is 400 DEG C, and reduction ratio 75% obtains the thin strip cold of 1.0mm thickness;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 20%N2+ 80%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 830 DEG C, annealing time 8min;
Step 5, Nitrizing Treatment:
It is 20%NH in dry volume ratio by strip3+ 20%N2+ 70%H2Nitrizing Treatment, nitriding are carried out in mixed atmosphere
Temperature is 700 DEG C, nitriding time 120s, and nitriding amount is 300ppm;
Step 6, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 850 DEG C are heated to from 600 DEG C of speed with 50 DEG C/h, so
1000 DEG C are heated to the speed of 20 DEG C/h afterwards, is then heated to 1200 DEG C with the speed of 15 DEG C/h, quenching obtains high mangneto and stretches
Contracting coefficient Fe-Ga base strips measure the magnetostriction coefficient of the high-magnetostriction coefficient Fe-Ga base strips of different Al contents
(3/2) the results are shown in Table 3 by λ s.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different Al contents of table 3
Serial number | Al content (weight percent %) | Secondary recrystallization completeness (%) | (3/2)λs(ppm) |
1 | 0.005 | 100 | 290 |
2 | 0.02 | 100 | 295 |
3 | 0.03 | 100 | 320 |
4 | 0.05 | 100 | 325 |
5 | 0.065 | 100 | 310 |
6 | 0.08 | 100 | 290 |
Contrast experiment 7 | 0.2 | 40% | 195 |
The 7th group in table 3 is contrast experiment, from table 3 it can be seen that when Al content is in the scope of the invention (serial number 1~
6), secondary recrystallization is completed preferable, and Magnetostriction is excellent;It is secondary when Al content is beyond the scope of the invention (contrast experiment 7)
Recrystallizing completeness reduces, therefore Magnetostriction is relatively low.
Embodiment 4
High-magnetostriction coefficient Fe-Ga base strips, constituent contain by weight percentage:Ga:31.5%, C:
0.06%, Al:0.01%, surplus is that Fe and other inevitable impurity, Nb contents are different as shown in table 4.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip in table 4, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1250 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, it is thick to obtain 1.8mm for 1150~1200 DEG C of start rolling temperature after cooling
Hot rolled plate;
Step 4, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) by hot rolled plate, rapid cooling, annealing time 8min are advanced using a rolling after 1000 DEG C of normalizing annealings
Row temperature cold rolling, rolling temperature are 700 DEG C, then reduction ratio 44% carries out the warm cold rolling of lower temperature, rolling temperature 200
DEG C, reduction ratio 85% obtains the thin strip cold of 0.15mm thickness;
Step 5, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 850 DEG C, annealing time 4min;
Step 6, secondary recrystallization is annealed:
By annealed sheet under inert atmosphere conditions, 1000 DEG C are heated to from 900 DEG C of speed with 30 DEG C/h and keep the temperature 4h, so
1100 DEG C being heated to the speed of 10 DEG C/h afterwards and keeping the temperature 5h, furnace cooling obtains high-magnetostriction coefficient Fe-Ga base strips, measures not
With magnetostriction coefficient (3/2) λ s of high-magnetostriction coefficient Fe-Ga base strips of Nb contents, the results are shown in Table 4.
The magnetostriction coefficient contrast table of 4 difference of table high-magnetostriction coefficient Fe-Ga base strips made from Nb contents
Classification | Nb contents (weight percent %) | Secondary recrystallization completeness (%) | (3/2)λs(ppm) |
Contrast experiment 1 | 0.01 | 25 | 170 |
2 | 0.03 | 100 | 285 |
3 | 0.1 | 100 | 292 |
4 | 0.28 | 100 | 345 |
5 | 0.42 | 100 | 314 |
6 | 0.56 | 100 | 310 |
7 | 0.74 | 100 | 292 |
Contrast experiment 8 | 1.52 | 15 | 156 |
The 1st group and the 8th group in table 4 is contrast experiment, as can be seen from Table 4 when Nb contents are in the scope of the invention
(serial number 2~7) can realize that restraint, tissue and texture coordinate collocation, obtain sharp and improve Goss secondary recrystallizations and knit
Structure, Magnetostriction are excellent;When Nb contents are beyond the scope of the invention (contrast experiment 1 and 8), secondary recrystallization completeness drop
It is low, therefore Magnetostriction is relatively low.
Embodiment 5
High-magnetostriction coefficient Fe-Ga base strips, ingredient contain by weight percentage:Ga:17%, C:0.03%, Al:
0.048%, Nb:0.45%, Cu:0.5%%, Mn:0.08%, S:0.02%, Sn:0.06%, Mo:0.5%, surplus for Fe and
Other inevitable impurity, B content are different as shown in table 5.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip in table 5, cast after being smelted at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1250 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1150~1200 DEG C of start rolling temperature obtains 2mm thickness after cooling
Hot rolled plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) hot rolled plate after pickling is subjected to cold rolling, the thin strip cold of 0.2mm thickness is obtained using secondary rolling, wherein:
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is 400~800 DEG C, reduction ratio 60%, Ran Hou
Rapid cooling after 1000 DEG C of annealing 10min, second of warm cold rolling relatively low for temperature, rolling temperature is 600 DEG C, reduction ratio 75%;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 30%N2+ 70%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 900 DEG C, annealing time 15min;
Step 5, secondary recrystallization is annealed:
By annealed sheet, under the conditions of inertia restores mixed atmosphere, 900 DEG C are heated to from 800 DEG C of speed with 120 DEG C/h,
Then 1200 DEG C are heated to the speed of 60 DEG C/h and keep the temperature 2h, it is air-cooled to obtain high-magnetostriction coefficient Fe-Ga base strips, it measures
The results are shown in Table 5 by magnetostriction coefficient (3/2) λ s of the high-magnetostriction coefficient Fe-Ga base strips of different B contents.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different B contents of table 5
Serial number | B content (weight percent %) | Secondary recrystallization completeness (%) | (3/2)λs(ppm) |
1 | 0.005 | 100 | 228 |
2 | 0.015 | 100 | 240 |
3 | 0.03 | 100 | 256 |
4 | 0.04 | 100 | 247 |
5 | 0.05 | 100 | 243 |
Contrast experiment 6 | 0.5 | 10 | 120 |
The 6th group in table 5 is contrast experiment, as can be seen from Table 5 when B content is in the scope of the invention (serial number 1~
5), secondary recrystallization is completed preferable, and Magnetostriction is excellent;It is secondary when B content is beyond the scope of the invention (contrast experiment 6)
Recrystallizing completeness reduces, and Magnetostriction is relatively low.
Embodiment 6
High-magnetostriction coefficient Fe-Ga base strips, constituent contain by weight percentage:Ga:23.5%, C:
0.025%, Nb:0.054%, Al:0.035%, Cu:0.1%%, Mn:0.05%, S:0.02%, Sn:0.06%, V:
0.05%, surplus is Fe and other inevitable impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1190 DEG C of start rolling temperature obtains 2mm thickness hot rolled plates after cooling;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate being used into a rolling, first carries out warm cold rolling, rolling temperature is 500 DEG C, reduction ratio 40%,
Then the warm cold rolling of lower temperature is carried out, rolling temperature is 100 DEG C, and reduction ratio 70% obtains the thin strip cold of 0.35mm thickness;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 20%N2+ 80%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It it is 870 DEG C, annealing time 5min, Fig. 3 sees in the micro-organization chart of the base strip sample after decarburizing annealing;
Step 5, Nitrizing Treatment:
It is 25%NH in dry volume ratio by strip3+ 20%N2+ 55%H2Nitrizing Treatment, nitriding are carried out in mixed atmosphere
Temperature is 870 DEG C, and nitriding amount is different as shown in table 6;
Step 6, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 950 DEG C are heated to from 850 DEG C of speed with 30 DEG C/h, so
1150 DEG C being heated to the speed of 20 DEG C/h afterwards and keeping the temperature 6h, quenching obtains high-magnetostriction coefficient Fe-Ga base strips.It measures and oozes
The result of magnetostriction coefficient (3/2) λ s of high-magnetostriction coefficient Fe-Ga base strips made from nitriding amount difference in nitrogen processing
As shown in table 6.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different nitriding amounts of table 6
Serial number | Nitriding amount (ppm) | (3/2)λs(ppm) |
1 | 30 | 265 |
2 | 100 | 302 |
3 | 160 | 345 |
4 | 380 | 320 |
5 | 560 | 356 |
6 | 800 | 290 |
Contrast experiment 7 | 1000 | 80 |
From figure 3, it can be seen that obtaining uniform primary recrystallization tissue after decarburizing annealing, be conducive to secondary recrystallization
It completes.
As can be seen from Table 6, when nitriding amount is too low (serial number 1~6), it is inadequate that supplement forms restraint, secondary recrystallization
Not perfect, Magnetostriction is relatively low;When nitriding amount is too high (contrast experiment 7), supplement restraint is unfavorable for by force very much secondary tying again
Crystalline substance causes Magnetostriction relatively low.
Embodiment 7
High-magnetostriction coefficient Fe-Ga base strips, constituent contain by weight percentage:Ga:22.0%, C:
0.05%, Al:0.03%, Nb:0.25%, Sn:0.05%, V:0.1, Mo:0.1%, surplus for Fe and it is other inevitably
Impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted at 1420~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1180 DEG C of start rolling temperature obtains 3mm thickness hot rolled plates after cooling;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) hot rolled plate after pickling is subjected to cold rolling, is for the first time warm cold rolling, rolling temperature is using secondary rolling
400~800 DEG C, then reduction ratio 66% carries out rapid cooling after intermediate annealing, second of warm cold rolling relatively low for temperature, rolling
Temperature is 200~600 DEG C, and reduction ratio 80%, intermediate anneal temperature is different as shown in table 7, obtains the cold rolling of 0.2mm thickness
Strip;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 850 DEG C, annealing time 8min:
Step 5, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 1200 DEG C are heated to simultaneously from 800 DEG C of speed with 30 DEG C/h
2h is kept the temperature, quenching obtains high-magnetostriction coefficient Fe-Ga base strips.
Secondary rolling intermediate anneal temperature is different, the magnetostriction of high-magnetostriction coefficient Fe-Ga base strips obtained
The results are shown in Table 7 by coefficient (3/2) λ s.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from 7 different annealing temperature of table
Serial number | Intermediate anneal temperature | The intermediate annealing time | (3/2)λs(ppm) |
1 | 800 | 30 | 285 |
2 | 900 | 10 | 290 |
3 | 900 | 30 | 300 |
4 | 950 | 30 | 320 |
5 | 1050 | 10 | 340 |
Contrast experiment 6 | 1150 | 10 | 180 |
The 6th group in table 7 is contrast experiment, as can be seen from Table 7 when intermediate annealing schedule is in the scope of the invention
(serial number 1~5), can obtain excellent Magnetostriction;When intermediate annealing schedule is beyond the scope of the invention (contrast experiment 6),
Magnetostriction is relatively low.
Embodiment 8
High-magnetostriction coefficient Fe-Ga base strips, ingredient contain by weight percentage:Ga:19%, C:0.03%, Nb:
0.15%, Al:0.01%, Sn:0.06%, V:0.1%, B:0.02%, Tb:0.2%, surplus for Fe and it is other inevitably
Impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1200 DEG C of start rolling temperature obtains 2.2mm thickness hot rolled plates after cooling;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) by after pickling hot rolled plate carry out cold rolling, using secondary rolling obtain 0.45mm, 0.35mm, 0.25mm,
The thin strip cold of 0.15mm, 0.1mm thickness, secondary rolling:It is for the first time warm cold rolling, rolling temperature is 400~800 DEG C, pressure
Rate is 55%, then the rapid cooling after 1025 DEG C of 30min that anneal, second of warm cold rolling relatively low for temperature, rolling temperature 500
DEG C, reduction ratio is different as shown in table 8;
Step 4, Nitrizing Treatment:
It is 5%NH in dry volume ratio by thin strip cold3+ 20%N2+ 75%H2Nitrizing Treatment is carried out in mixed atmosphere, is oozed
Nitrogen temperature is 950 DEG C, nitriding time 40s, and nitriding amount is 280ppm;
Step 5, decarburizing annealing:
It is 25%N in wet volume ratio by the strip after Nitrizing Treatment2+ 75%H2Mixed atmosphere in carry out decarburization move back
Fire, annealing temperature are 850 DEG C, annealing time 5min;
Step 6, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 1025 DEG C are heated to from 800 DEG C of speed with 20 DEG C/h, so
1100 DEG C are heated to the speed of 15 DEG C/h afterwards, be then heated to 1200 DEG C with the speed of 120 DEG C/h and keeps the temperature 2h, quenching obtains
High-magnetostriction coefficient Fe-Ga base strips.
Reduction ratio is different in secondary second of cold-rolled process of rolling, high-magnetostriction coefficient Fe-Ga base strips obtained
Magnetostriction coefficient (3/2) λ s the results are shown in Table 8.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different reduction ratios of table 8
Serial number | Finished product thickness (mm) | Secondary cold-rolling reduction ratio (%) | (3/2)λs(ppm) |
1 | 0.45 | 55 | 280 |
2 | 0.35 | 65 | 325 |
3 | 0.25 | 75 | 345 |
4 | 0.15 | 85 | 350 |
5 | 0.1 | 90 | 290 |
Macroscopic organization chart of the 3rd group of Fe-Ga base strip sample after secondary recrystallization is annealed is shown in Fig. 4 (a) in table 8, the 4th
Macroscopic organization chart of the group Fe-Ga base strip samples after secondary recrystallization is annealed is shown in Fig. 4 (b);High temperature moves back as can be seen from Figure 4
The perfect subgrain of Centimeter Level is obtained after fire, magnetic hysteresis telescopicing performance is excellent, further illustrates secondary recrystallization control to magnetic
The importance of stagnant telescopicing performance.Secondary cold-rolling reduction ratio can obtain excellent magnetic hysteresis within the scope of the present invention as can be seen from Table 8
Telescopicing performance.
Embodiment 9
High-magnetostriction coefficient Fe-Ga base strips, ingredient contain by weight percentage:Ga:24.6%, C:0.07%, Nb:
0.38%, Al:0.045%, Cu:0.1%%, Mn:0.05%, S:0.01%, V:0.08%, surplus is Fe and other can not keep away
The impurity exempted from.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1200 DEG C of start rolling temperature obtains the hot rolling of 2.0mm thickness after cooling
Plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) by hot rolled plate after 1025 DEG C of normalizing annealings rapid cooling, annealing time 5min, then using a rolling,
The thin strip cold of 0.35mm thickness is obtained, wherein:
Rolling:Warm cold rolling is first carried out, rolling temperature is 700 DEG C, then reduction ratio 58% carries out lower temperature
Warm cold rolling, rolling temperature be 200 DEG C, reduction ratio 77%;
Step 4, decarburizing annealing and Nitrizing Treatment:
By thin strip cold wet volume ratio be 15%NH3+ 20%N2+ 65%H2Mixed atmosphere in be carried out at the same time decarburization
Annealing and Nitrizing Treatment, annealing temperature are 870 DEG C, annealing time 2min, and nitriding amount is 286ppm;
Step 5, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, it is heated to from 800 DEG C with different heating rates as shown in table 9
1200 DEG C and 4h is kept the temperature, furnace cooling obtains high-magnetostriction coefficient Fe-Ga base strips, measures its magnetostriction coefficient (3/2) λ s knots
Fruit is as shown in table 9.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different heating rates of table 9
Classification | Heating rate (DEG C/h) | (3/2)λs(ppm) |
1 | 10 | 295 |
2 | 25 | 305 |
3 | 50 | 312 |
4 | 70 | 289 |
5 | 120 | 260 |
Contrast experiment 6 | 200 | 189 |
The 6th group in table 9 is contrast experiment, as can be seen from Table 9 when heating rate is in (serial number in the scope of the invention
1~5) excellent Magnetostriction can, be obtained;When heating rate is beyond the scope of the invention (contrast experiment 6), magnetostriction
It can be relatively low.
Embodiment 10
High-magnetostriction coefficient Fe-Ga base strips, ingredient contain by weight percentage:Ga:23.2%, C:0.065%,
Nb:0.59%, Al:0.005%, Cu:0.05%%, Mn:0.05%, S:0.01%, Sn:0.04%, surplus is Fe and other
Inevitable impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1180 DEG C of start rolling temperature obtains the hot rolling of 2.3mm thickness after cooling
Plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, is for the first time warm cold rolling, rolling temperature is using secondary rolling
400~800 DEG C, reduction ratio 60%, then the rapid cooling after 950 DEG C of 20min that anneal, is the relatively low warm cold rolling of temperature for the second time,
Rolling temperature is 300 DEG C, and reduction ratio 78% obtains the thin strip cold of 0.2mm thickness;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 850 DEG C, annealing time 5min:
Step 5, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, cycle annealing is carried out using different annealing temperature and time,
Quenching obtains high-magnetostriction coefficient Fe-Ga base strips, and measuring its magnetostriction coefficient (3/2) λ s, the results are shown in Table 10.
The magnetostriction coefficient pair of high-magnetostriction coefficient Fe-Ga base strips made from 10 different annealing temperatures of table, that is, time
Compare table
Serial number | Annealing temperature (DEG C) | Annealing time (min) | (3/2)λs(ppm) |
1 | 900 | 280 | 301 |
2 | 950 | 240 | 310 |
3 | 1000 | 30 | 260 |
4 | 1000 | 600 | 308 |
5 | 1100 | 15 | 275 |
6 | 1200 | 30 | 240 |
Contrast experiment 7 | 1300 | 120 | 155 |
It can be seen that secondary recrystallization annealing is carried out using constant temperature system, when annealing temperature and time system are in table 10
In the scope of the invention (serial number 1~5), excellent Magnetostriction can be obtained;When annealing schedule is beyond the scope of the invention (comparison
7), Magnetostriction is relatively low for experiment.
Embodiment 11
High-magnetostriction coefficient Fe-Ga base strips, ingredient contain by weight percentage:Ga:31%, C:0.04%, Nb:
0.28%, Al:0.025%, Sn:0.06%, V:0.1%, Mo:0.2%, Tb:0.2%, surplus is Fe and other inevitable
Impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, it smelts:
By the set component of strip, cast after being smelted respectively at 1440~1600 DEG C;
Step 2, hot rolling:
(1) by blank heating to 1100~1280 DEG C of heat preservations;
(2) blank after heating and thermal insulation is subjected to hot rolling, 1150 DEG C of start rolling temperature obtains the hot rolling of 2.5mm thickness after cooling
Plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, is for the first time warm cold rolling, rolling temperature is using secondary rolling
400~800 DEG C, reduction ratio 68%, then the rapid cooling after 1000 DEG C of 15min that anneal, is the relatively low warm cold rolling of temperature for the second time,
Rolling temperature is 300 DEG C, and reduction ratio 81% obtains the thin strip cold of 0.15mm thickness;
Step 4, decarburizing annealing:
By thin strip cold wet volume ratio be 25%N2+ 75%H2Mixed atmosphere in carry out decarburizing annealing, annealing temperature
It is 830 DEG C, annealing time 5min:
Step 5, Nitrizing Treatment:
It is 15%NH in dry volume ratio by strip3+ 20%N2+ 65%H2Nitrizing Treatment, nitriding are carried out in mixed atmosphere
Temperature is 850 DEG C, nitriding time 180s, and nitriding amount is 400ppm;
Step 6, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 600min are kept the temperature at 1000 DEG C, respectively furnace cooling, air-cooled and quench
Fire obtains high-magnetostriction coefficient Fe-Ga base strips, and it is as shown in table 11 to measure its magnetostriction coefficient (3/2) λ s result.
The magnetostriction coefficient contrast table of high-magnetostriction coefficient Fe-Ga base strips made from the different types of cooling of table 11
Classification | The type of cooling | (3/2)λs(ppm) |
1 | Furnace cooling | 330 |
2 | It is air-cooled | 345 |
3 | Quenching | 370 |
In table 11 it can be seen that after secondary recrystallization annealing, compared to furnace cooling and air-cooled, can using the type of cooling of quenching
To obtain higher magnetic hysteresis telescopicing performance.
Embodiment 12
High-magnetostriction coefficient Fe-Ga base strips, constituent and weight percent content are Ga:22.3%, it is other
Constituent is as shown in table 12, and surplus is Fe and other inevitable impurity.
The preparation method of above-mentioned high-magnetostriction coefficient Fe-Ga base strips, includes the following steps:
Step 1, ingot casting:
By the set component of strip in table 12, obtained after being smelted respectively at 1440~1600 DEG C using strip casting machine
2.8mm thickness Cast Strip;
Step 2, hot rolling:
(1) Cast Strip is heated to 1000~1280 DEG C of heat preservations;
(2) Cast Strip after heating and thermal insulation is subjected to hot rolling, 1025 DEG C of start rolling temperature obtains the hot rolling of 2.3mm thickness after cooling
Plate;
Step 3, pickling and cold rolling:
(1) hot rolled plate is subjected to pickling;
(2) hot rolled plate after pickling is subjected to cold rolling, the thin strip cold of 0.23mm thickness is obtained using secondary rolling,
In:
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is 400~800 DEG C, reduction ratio 56%, then 900
Rapid cooling after DEG C annealing 5min, the second warm cold rolling relatively low for temperature, rolling temperature is 20 DEG C, reduction ratio 77%;
Step 4, decarburizing annealing:
By thin strip cold in wet 25%N2+ 75%H2Mixed atmosphere in, carry out decarburizing annealing, annealing temperature 830
DEG C, annealing time 4min;
Step 5, secondary recrystallization is annealed:
By annealed sheet under the conditions of inertia restores mixed atmosphere, 1200 DEG C are heated to simultaneously from 800 DEG C of speed with 20 DEG C/h
Keep the temperature 2h, water quenching obtains high-magnetostriction coefficient Fe-Ga base strips, measure using heterogeneity in the case of thin strap continuous casting blank and
The result of magnetostriction coefficient (3/2) λ s of the high-magnetostriction coefficient Fe-Ga base strips of content is as shown in table 12
The Magnetostriction contrast table of the high-magnetostriction coefficient Fe-Ga base strips of the different constituents of table 12 and content
As can be seen from Table 12, use thin strap continuous casting mode can with flexible control inhibitor, realize improve it is secondary again
Crystallization, magnetic hysteresis telescopicing performance are higher.
The existing preparation method one side complex process about high-magnetostriction coefficient Fe-Ga alloys, it is such as solidifying using orientation
Gu coated rolling;Another aspect inhibitor controls and secondary recrystallization process mismatches, so most of introducing surface is inclined
On the one hand analysis can induce advantage and the accuracy for the growth selection for improving Goss by surface, on the other hand be formed by surface layer
More Nb and the precipitate of S delay the recession of surface layer inhibitor further surface layer grain to be hindered to grow up.Surface segregation draws
Enter that there are cost is higher, equipment precision requirement is high, it is difficult to the problems such as industrializing.
A kind of preparation method of high-magnetostriction coefficient Fe-Ga base strips proposed by the present invention, efficiently solves above-mentioned ask
Topic.The novel inhibitors System Design of the intrinsic inhibitor+nitriding of low temperature is established, control heat treatment and rolling mill practice are precipitated tiny
Cu2S, Nb (C, N) and V (C, N) or miscible precipitate therein are as main intrinsic inhibitor;When intrinsic restraint deficiency
When, it supplements to form nitride using nitriding.Restraint flexibility control is realized especially with the advantage of thin strap continuous casting Sub realizable fuzzy matrix
System eliminates the dependence of surface energy.
The coordination that tissue, texture and inhibitor are realized by reasonable control composition, rolling mill practice and annealing process is taken
Match, it is final improved and sharp η (<100>//RD) texture secondary recrystallization crystal grain, improve magnetic hysteresis coefficient of dilatation.
At present, domestic and international market is to having both the Fe-Ga alloys demand of big magnetostriction coefficient and excellent mechanical property very
Urgently, the present invention using traditional rolling and is moved back using the slab of molding, sheet billet continuous casting, sheet blank continuous casting and thin strap continuous casting
What ignition technique flow can be simple and efficient mass produce, and magnetic hysteresis telescopicing performance is better than existing report, thus with very
Good popularizing application prospect.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (13)
1. high-magnetostriction coefficient Fe-Ga base strips, which is characterized in that its ingredient is by weight percentage:Ga:15~32%,
C:0.001~0.12%, Al:0.005~0.08%, Nb:0.03~0.75%, surplus for Fe and it is other inevitably it is miscellaneous
Matter.
2. high-magnetostriction coefficient Fe-Ga base strips according to claim 1, which is characterized in that the high mangneto is stretched
Contracting coefficient Fe-Ga base strips, ingredient also contain by weight percentage:Cu:≤ 0.5%, S:0.008~0.035%, Mn:
0.01~0.3%.
3. high-magnetostriction coefficient Fe-Ga base strips according to claim 1 or 2, which is characterized in that the high mangneto
Coefficient of dilatation Fe-Ga base strips, ingredient also contain by weight percentage:Sn:0.02~0.1%, Sb:0.01~0.03%,
V:0.01~0.1%, Mo:0.01~3.0%, Tb:0.05~0.6%, N:0.006~0.02% or B:0.005~0.05%
In it is one or more.
4. the preparation method of the high-magnetostriction coefficient Fe-Ga base strips described in claim 1-3 any one, feature exist
In including the following steps:
Step 1:It smelts
By the set component of strip, cast after being smelted at a temperature of 1440~1600 DEG C;
Step 2:Hot rolling
(1) by blank heating to 1000~1280 DEG C of heat preservations;
(2) by the blank after heating and thermal insulation, hot rolling is carried out, 900~1250 DEG C of start rolling temperature, 600~1050 DEG C of finishing temperature is cold
But the hot rolled plate of 1~4mm thickness is obtained afterwards;
Step 3:Pickling and cold rolling
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, obtains the thin strip cold of 0.10~1.0mm thickness;
Step 4:Decarburizing annealing
By thin strip cold in wet N2+H2In mixed atmosphere, decarburizing annealing is carried out, annealing temperature is 800~1000 DEG C, during annealing
Between be 2~30min, N2Shared volume ratio is 20~75%;
Step 5:Secondary recrystallization is annealed
The annealed sheet that decarburizing annealing is obtained, progress secondary recrystallization moves back under the conditions of inert atmosphere or inertia reduction mixed atmosphere
Fire processing, obtains high-magnetostriction coefficient Fe-Ga base strips.
5. the preparation method of the high-magnetostriction coefficient Fe-Ga base strips described in claim 1-3 any one, feature exist
In including the following steps:
Step 1:It smelts
By the set component of strip, cast after being smelted at a temperature of 1440~1600 DEG C;
Step 2:Hot rolling
(1) by blank heating to 1000~1280 DEG C of heat preservations;
(2) by the slab after heating and thermal insulation, hot rolling is carried out, 900~1250 DEG C of start rolling temperature, 600~1050 DEG C of finishing temperature is cold
But the hot rolled plate of 1~4mm thickness is obtained afterwards;
Step 3:Pickling and cold rolling
(1) hot rolled plate is subjected to pickling to remove oxide;
(2) hot rolled plate after pickling is subjected to cold rolling, obtains the thin strip cold of 0.10~1.0mm thickness;
Step 4:Decarburizing annealing
By thin strip cold, in wet N2+H2In mixed atmosphere, decarburizing annealing is carried out, annealing temperature is 800~1000 DEG C, during annealing
Between be 2~30min, N2Shared volume ratio is 20~75%.;
Step 5:Nitrizing Treatment
By strip, in dry NH3+N2+H2Nitrizing Treatment is carried out in mixed atmosphere;
Step 6:Secondary recrystallization is annealed
The annealed sheet that decarburizing annealing is obtained, progress secondary recrystallization moves back under the conditions of inert atmosphere or inertia reduction mixed atmosphere
Fire processing, obtains high-magnetostriction coefficient Fe-Ga base strips.
6. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that institute
It casts after the smelting stated, any one process in molding, sheet billet continuous casting, sheet blank continuous casting and thin strap continuous casting can be used
It realizes.
7. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that institute
The pickling stated is to carry out pickling again after normalizing annealing processing is carried out to hot rolled plate, and normalizing annealing temperature is 700~1100 DEG C, often
The annealing time be 2~120min, rapid cooling after normalizing.
8. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that institute
The cold rolling stated including following two rollings, can be used any one rolling and carry out cold rolling:
Rolling:First carry out warm cold rolling, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, then carry out compared with
The warm cold rolling of low temperature, rolling temperature are room temperature~600 DEG C, and reduction ratio is 10~92%;
Secondary rolling:It is for the first time warm cold rolling, rolling temperature is room temperature~800 DEG C, and reduction ratio is 30~95%, Ran Hou
Rapid cooling after 800~1100 DEG C of 5~120min of annealing, second of warm cold rolling relatively low for temperature, rolling temperature is room temperature~600
DEG C, reduction ratio is 50~92%.
9. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that institute
The secondary recrystallization annealing stated including the following two kinds pattern, can be used any one pattern and carry out secondary recrystallization annealing
Processing:
Pattern one:Annealed sheet is heated to 1000~1200 DEG C from 600~900 DEG C and keeps the temperature 0.5~10h, heating process uses
Continuous warming or the multisection type annealing containing moderate soak.
Pattern two:Annealed sheet is subjected to 15~600min cycle annealings at 900~1200 DEG C.
10. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that
The secondary recrystallization annealing carries out under the conditions of inert atmosphere or inertia reduction mixed atmosphere, and the inert atmosphere is
Refer to nitrogen atmosphere or argon gas atmosphere;The inertia reduction mixed atmosphere refers to the mixed atmosphere of inert gas and hydrogen.
11. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 4 or 5, which is characterized in that
The secondary recrystallization annealing can be used any one in furnace cooling, air-cooled or quenching after the completion of secondary recrystallization annealing
Kind mode cools down.
12. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 5, which is characterized in that described
Step 5 Nitrizing Treatment NH3+N2+H2In mixed atmosphere, H2Shared volume ratio is 50~80%, NH3Shared volume ratio for 5~
30%, nitriding temperature is 600~1050 DEG C, and the time is 10~500s, and nitriding amount is 30~800ppm.
13. the preparation method of high-magnetostriction coefficient Fe-Ga base strips according to claim 5, which is characterized in that described
Nitrizing Treatment can before decarburizing annealing, after decarburizing annealing or it is synchronous with decarburizing annealing carry out.
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CN114231852A (en) * | 2021-11-26 | 2022-03-25 | 沈阳工业大学 | Magnetostrictive thin strip material, preparation method and application |
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CN110257613A (en) * | 2019-07-05 | 2019-09-20 | 武汉钢铁有限公司 | Improve the method for low temperature high magnetic induction grain-oriented silicon steel magnetic property |
CN114231852A (en) * | 2021-11-26 | 2022-03-25 | 沈阳工业大学 | Magnetostrictive thin strip material, preparation method and application |
CN114231852B (en) * | 2021-11-26 | 2022-10-11 | 沈阳工业大学 | Magnetostrictive thin strip material, preparation method and application |
CN115522029A (en) * | 2021-11-26 | 2022-12-27 | 沈阳工业大学 | Magneto-electric power generation device, and preparation method and test method of giant magnetostrictive Fe-Ga sheet material assembled with magneto-electric power generation device |
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CN114480982A (en) * | 2022-01-12 | 2022-05-13 | 沈阳工业大学 | Low-cost high magnetostriction coefficient Fe-Al based thin strip and preparation method thereof |
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