CN108431244A - Oriented electrical steel and its manufacturing method - Google Patents

Oriented electrical steel and its manufacturing method Download PDF

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Publication number
CN108431244A
CN108431244A CN201680075431.1A CN201680075431A CN108431244A CN 108431244 A CN108431244 A CN 108431244A CN 201680075431 A CN201680075431 A CN 201680075431A CN 108431244 A CN108431244 A CN 108431244A
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oriented electrical
steel plate
annealing
electrical steel
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CN108431244B (en
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韩奎锡
高炫昔
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Posco Holdings Inc
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Posco Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1272Final recrystallisation annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1261Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest following hot rolling
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1266Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest between cold rolling steps
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/004Very low carbon steels, i.e. having a carbon content of less than 0,01%
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2201/00Treatment for obtaining particular effects
    • C21D2201/05Grain orientation
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1255Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C2202/00Physical properties
    • C22C2202/02Magnetic

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Soft Magnetic Materials (AREA)
  • Manufacturing Of Steel Electrode Plates (AREA)

Abstract

The manufacturing method of the oriented electrical steel of one embodiment of the invention, includes the following steps:Slab is provided, slab % by weight includes:Si:More than 0 weight % and 4.0 weight % or less, C:0.001 weight % to 0.4 weight % and Mn:0.001 weight % to 2.0 weight %, surplus by Fe and other inevitably mixed impurity is constituted;Slab is reheated;Hot rolling is carried out to manufacture hot rolled steel plate to slab;Hot rolled plate annealing is carried out to hot rolled steel plate;First cold rolling is carried out to the hot rolled steel plate by hot rolled plate annealing;Decarburizing annealing is carried out to the steel plate Jing Guo cold rolling;Steel plate to completing decarburizing annealing carries out secondary cold-rolling;And final annealing is carried out to the steel plate for completing cold rolling, complete the thickness (D) that the steel plate of the final annealing existing magnetic domain size (2L) in crystal grain is less than steel plate.

Description

Oriented electrical steel and its manufacturing method
Technical field
This application involves a kind of oriented electrical steel and its manufacturing methods.
Background technology
Oriented electrical steel is the soft magnetic materials of the having excellent magnetic properties of rolling direction, and the material is by the knot with steel plate Crystalline substance is oriented to { 110 }<001>The crystal grain that is orientated of so-called Gauss (Goss) constitute.
This oriented electrical steel is manufactured by following steps:Hot rolling, hot rolled plate annealing are carried out after by heating of plate blank And cold rolling comes after being usually rolled into the final thickness of 0.15mm to 0.35mm, carries out primary recrystallization annealing, and in order to be formed Secondary recrystallization and carry out high annealing.
At this point, in high annealing, rate of temperature rise is slower, and the concentration class that the Gauss of secondary recrystallization is orientated is higher, and magnetism is got over It is excellent.In general, rate of temperature rise in the high annealing of oriented electrical steel be per hour 15 DEG C hereinafter, therefore only being needed in heating Couple of days, moreover, it is also necessary to purification annealing in 40 hours or more, it may be said that the process is the big process of energy expenditure.This Outside, current final high annealing process implements the annealing of (Batch) mode in batches, therefore the meeting in process under coil of strip state Generate following difficulty.The first, because being heat-treated under coil of strip state, it will produce temperature between the outer volume portion of coil of strip and curls inward portion Deviation is spent, therefore identical heat treatment mode cannot be applicable in each section, to generate magnetic biasing between volume portion and curls inward portion outside Difference.The second, MgO is coated on surface after decarburizing annealing, and will produce various during formation priming coat in high annealing Surface defect, therefore casting yield can be reduced.Third is moved back due to carrying out high temperature after being rolled into a roll the decarburization plate for completing decarburizing annealing Fire carries out insulation coating again later after planarized annealing, therefore production process is divided into three steps, generates asking for casting yield decline Topic.
Invention content
Technical problems to be solved
A kind of manufacturing method for being designed to provide oriented electrical steel of one embodiment of the invention and pass through this method The oriented electrical steel of manufacture.
Technical solution
The manufacturing method of the oriented electrical steel of one embodiment of the invention includes the following steps:Slab, the slab are provided % includes by weight:Si:More than 0 weight % and 4.0 weight % or less, C:0.001 weight % to 0.4 weight % and Mn:0.001 Weight % to 2.0 weight %, surplus by Fe and other inevitably mixed impurity is constituted;Slab is reheated;It is right Slab carries out hot rolling to manufacture hot rolled steel plate;Hot rolled plate annealing is carried out to hot rolled steel plate;To the hot-rolled steel by hot rolled plate annealing Plate carries out first cold rolling;Decarburizing annealing is carried out to the steel plate Jing Guo cold rolling;Steel plate to completing decarburizing annealing carries out secondary cold-rolling; And final annealing is carried out to the steel plate for completing cold rolling, it completes the steel plate of the final annealing existing magnetic domain size 2L in crystal grain and is less than Thickness D (the 2L of steel plate<D).
Slab may include being more than 0 weight % and 1 weight % Si below.
Slab can further include more than 0 weight % and 0.01 weight % Al below.
The relation reheating temperature of slab can be 1050 DEG C to 1350 DEG C.
Reduction ratio in the first cold rolling the step of and the step of secondary cold-rolling may respectively be 50% to 70%.
In the step of carrying out decarburizing annealing to the steel plate Jing Guo cold rolling and the steel plate for completing decarburizing annealing is carried out secondary cold The step of rolling can be repeated more than twice.
The step of decarburizing annealing, can be at a temperature of 800 DEG C to 1150 DEG C, the atmosphere of the hydrogen comprising 0 DEG C of dew-point temperature or more Middle implementation.
The step of final annealing, may include first step and second step, temperature of the first step at 850 DEG C to 1150 DEG C Under, implement in the atmosphere of 10 DEG C to 70 DEG C of dew-point temperature, at a temperature of 900 DEG C to 1200 DEG C, include 10 DEG C of dew-point temperature or less Hydrogen and nitrogen mixed-gas atmosphere in implement.
First step can be implemented 300 seconds hereinafter, second step can be implemented 60 seconds to 300 seconds.
The step of being carried out continuously final annealing after the cold rolling the step of.
Carbon amounts after the final annealing the step of in electric steel plate can be more than 0 weight % and 0.003 weight % or less.
In the steel plate for completing final annealing, from { 110 }<001>Being orientated has the volume point for the crystal grain being orientated within 15 degree Rate can be 50% or more.
The volume fraction for the crystal grain that grain size is 20 μm to 1000 μm in the steel plate for completing final annealing can be 50% or more.
The oriented electrical steel of one embodiment of the invention % by weight is counted:Si:More than 0 weight % and 4.0 weights % is measured hereinafter, C:More than 0 weight % and 0.003 weight % or less and Mn:0.001 weight % to 2.0 weight %, surplus by Fe and Inevitably mixed impurity is constituted for other, and existing magnetic domain size 2L is less than the thickness D of steel plate in crystal grain.
It may include being more than 0 weight % and 1.0 weight % Si below.
It can further include and be more than 0 weight % and 0.01 weight % Al below.
Existing magnetic domain size 2L can be 10 μm to 500 μm in crystal grain.
From { 110 }<001>It can be 50% or more that being orientated, which has the volume fraction for the crystal grain being orientated within 15 degree,.
The volume fraction for the crystal grain that grain size is 20 μm to 1000 μm can be 50% or more.
Advantageous effect
An embodiment according to the present invention is capable of providing when carrying out final annealing without implementing in batches under coil of strip state (Batch) annealing of form and the manufacturing method of the oriented electrical steel of continuous annealing can be implemented.
In addition, an embodiment according to the present invention, only can also produce oriented electrical steel with the annealing of short time.
In addition, an embodiment according to the present invention, is capable of providing the oriented electrical steel without using grain growth inhibitor Plate.
In addition, an embodiment according to the present invention, can omit nitriding annealing.
Description of the drawings
Fig. 1 is the microstructure for the oriented electrical steel for indicating to manufacture in embodiment 1 and the photo of magnetic domain.
Specific implementation mode
First, second and third equal term uses in order to illustrate a variety of parts, ingredient, region, layer and/or segmentation, But it is not limited to these.These terms be intended merely to by certain part, ingredient, region, layer or segmentation with other parts, ingredient, Region, layer or segmentation are distinguished and are used.Therefore, first part disclosed below, ingredient, region, layer or segmentation are not surpassing Go out in the range of the scope of the invention and is also described with second part, ingredient, region, layer or segmentation.
Technical term as used herein is intended merely to mention specific embodiment and provide, and is not for limiting this hair It is bright.Singulative as used herein also includes plural form in the case of no expression specific contrary.In specification The meaning of the "comprising" used has refined specific characteristic, field, integer, step, action, element and/or ingredient, rather than arranges Except the presence of other specific characteristics, field, integer, step, action, element, ingredient and/or group or additional.
When being related to the setting of certain part in the "upper" of another part or " top ", indicate the part directly in the another part The upper surface of or top formed, or both between may have other parts.On the other hand, it directly sets when being related to certain part It sets at " top " of another part, indicates that other parts are not present between the two.
Although not doing different definition, including all terms of technical term as used herein and scientific terminology have this hair The identical meaning of meaning that bright person of ordinary skill in the field is commonly understood by.Use defined in the dictionary generally used Language is added the meaning for being construed to be consistent with relevant technical literature and present disclosure, in the case that undefined, no It is interpreted preferably or very formal meaning.
In addition, unless otherwise specified, % indicates that weight %, 1ppm indicate 0.0001 weight %.
In the following, the embodiment that the present invention will be described in detail, so that those skilled in the art can be easy Implement.But the invention is not limited in embodiments described herein, can realize the present invention with diversified forms.
The required characteristic of oriented electrical steel of the core material for power conversion usually as transformer is high magnetic flux density With low iron loss characteristic.High magnetic flux density can not only improve power conversion efficiency, moreover it is possible to improve design magnetic flux density, therefore have It can be used less core material come the advantages of reducing transformer size.In addition, in power conversion process in oriented electrical steel certainly In the case of sending out the loss, that is, iron loss generated, have the advantages that the no-load loss of transformer can be reduced.
So far, the research of oriented electrical steel and the technological development overwhelming majority carry out to reduce iron loss.It is orientated The iron loss of electric steel plate is divided into magnetic hystersis loss (Hysteresis Loss), traditional eddy-current loss (Classical as follows Eddy Current Loss) and abnormal eddy-current loss (Anomalous Eddy Current Loss) this several major.
Magnetic hystersis loss is the loss of electric steel plate caused by the magnetization degree of oriented electrical steel itself, works as oriented electrical steel Do not have in plate the concentration class that impurity or defect and Gauss are orientated it is high when, loss is small.
Traditional eddy-current loss is damaged caused by the eddy current that generates of magnetic history light plate of oriented electrical steel itself Consumption makes every effort to damage to reduce to reduce the eddy current of steel plate to the maximum extent by carrying high Si content and reducing steel plate thickness so far Consumption.Another exception eddy-current loss is the magnetic domain (magnetic with the oriented electrical steel under the alternating current that transformer works Domain movement) and the relevant loss of rotation, with magnetic domain size (Magnetic domain size, 2L) smaller loss The characteristic of reduction.Research for improving abnormal eddy-current loss be relative to be previously used for improve magnetic hystersis loss and tradition vortex damage The research that the research of consumption carries out recently, the technology of exploitation have:By the way that laser irradiation on surface of steel plate, assigns surface of steel plate Local stress causes the method for temporary magnetic domain microminiaturization;And the bending of predetermined pattern is assigned to surface of steel plate to cause structure Magnetic domain changes, and thus causes the method for permanent magnetic domain microminiaturization.The method developed as another magnetic domain microminiaturization method The different coating substance of the coefficient of expansion to be coated on surface of steel plate, to be assigned because of expansion coefficient difference on surface of steel plate Caused by tension, thus cause magnetic domain microminiaturization.
The result of the research for reducing oriented electrical steel exception eddy-current loss is repeated in the present inventor, it was found that when It can reduce magnetic domain size when the grain size for reducing oriented electrical steel, and can greatly reduce oriented electrical steel therewith The whole iron loss of plate.
In general, magnetic domain size has the relationship of following formula (1) with grain size.
Magnetic domain size 2L ∝ (grain size)1/2 (1)
That is, the smaller then magnetic domain size of grain size is smaller, abnormal eddy-current loss reduces therewith.
It is reported that abnormal eddy-current loss has the relationship of following formula (2) with traditional eddy-current loss.
Wea=[1.63 × (2L/d) -1] × Wec (2)
In formula (2), Wea indicates that abnormal eddy-current loss, Wec indicate that traditional eddy-current loss, 2L indicate magnetic domain size, d tables Show steel plate thickness.
As shown in formula (2), it is assumed that when magnetic domain size reduces in the case that steel plate thickness is constant, abnormal eddy-current loss can also subtract It is small.
Can greatly it be subtracted according to the correlation (1) of grain size and magnetic domain size if reducing Gauss and being orientated grain size Small magnetic domain size can greatly reduce the iron loss of oriented electrical steel therewith.
To sum up, it in order to reduce the iron loss of oriented electrical steel, needs to obtain by forming Gauss orientation recrystal grain Excellent magnetization characteristic reduces traditional vortex to reduce magnetic hystersis loss by increasing Si contents and reducing steel plate thickness Loss is orientated grain size microminiaturization finally by by Gauss, magnetic domain size microminiaturization is reduced to abnormal eddy-current loss.In order to Reduce the overall losses of oriented electrical steel, preferably subtracts all magnetic hystersis losses, traditional eddy-current loss and abnormal eddy-current loss It is small, but according to circumstances, even if without the great improvement of magnetic hystersis loss or traditional eddy-current loss, it is big by the way that Gauss is orientated crystal grain It is small to minimize the oriented electrical steel that also manufactured only to greatly improve abnormal eddy-current loss and produce easy and having excellent magnetic properties.
The manufacturing method of the oriented electrical steel of one embodiment of the invention includes:Slab, slab % by weight are provided Including:Si:More than 0 weight % and 4.0 weight % or less, C:0.001 weight % to 0.4 weight % and Mn:0.001 weight % To 2.0 weight %, surplus by Fe and other inevitably mixed impurity is constituted;The slab is reheated;To institute It states slab and carries out hot rolling to manufacture hot rolled steel plate;Hot rolled plate annealing is carried out to the hot rolled steel plate;To being moved back by the hot rolled plate The hot rolled steel plate of fire carries out first cold rolling;Decarburizing annealing is carried out to the steel plate Jing Guo the cold rolling;To completing the decarburizing annealing Steel plate carry out secondary cold-rolling;And final annealing is carried out to the steel plate for completing the cold rolling.In addition to this, as needed, it is orientated The manufacturing method of electric steel plate can further comprise other steps.
In the following, being described in detail by step.
Slab is provided first, and slab % by weight includes:Si:More than 0 weight % and 4.0 weight % or less, C:0.001 Weight % to 0.4 weight % and Mn:0.001 weight % to 2.0 weight %, surplus is by Fe and other are inevitably mixed miscellaneous Texture at.
The reasons why limiting composition is as follows.
Silicon (Si) can reduce the magnetic anisotropy of oriented electrical steel, and increase specific resistance to improve iron loss.The present invention An embodiment be characterized in that, reduce the grain size of final products, substantially to reduce abnormal eddy-current loss, but more increase Si can more improve iron loss, therefore Si more than preferred addition specified amount.Therefore, can be added to Si can carry out the content of cold rolling Range i.e. 4 weight %.The problem of when Si contents are excessive, brittleness can be increased in cold rolling, cold rolling can not be carried out to will appear. More specifically, Si contents can be 1 weight % or less (except 0 weight %).
Carbon (C) is the element for promoting austenite phase transformation, is to homogenize the hot rolling microstructure of oriented electrical steel, in cold rolling Gauss is promoted to be orientated the formation of crystal grain to manufacture the important element of magnetic excellent oriented electrical steel.However, when finally producing When in product including C, magnetic ageing phenomenon can be caused, reduce magnetic characteristic, therefore C present in the electric steel plate finally manufactured should be 0.003 weight % or less.In order to promote phase transformation and Gauss to be orientated the recrystallization of crystal grain, the C added in slab by adding C It can just take effect when more than 0.001 weight %, it, can not because of non-uniform hot rolling microstructure under the content less than 0.001 weight % It is stably formed secondary recrystallization.However, when the content of the C added in slab is more than 0.4 weight %, in hot rolling because of Ovshinsky Body phase transformation and form small hot rolling microstructure, primary recrystallization crystal grain is small, coiling process or hot rolled plate after completing hot rolling In cooling procedure after annealing, coarse carbide may be formed, and form Fe at normal temperatures3C (cementite), easily leads to Non-uniform tissue.It is that 0.003 weight % is below in decarburization to C content moreover, in decarbonization process and final annealing process The problem of having annealing time increase in the process.Therefore, the C content in slab can be limited in 0.001 weight % to 0.4 weight Measure %.
Have the effect of increasing specific resistance to reduce iron loss in the same manner as manganese (Mn) and Si, same as C is to promote austenite phase Become, by the important element of the grain size microminiaturization of crystal grain in hot rolling and annealing operation.When the additive amount of this Mn is less than 0.001 weight When measuring %, sufficient phase transformation cannot be generated in the same manner as the effect of C, slab and hot rolling microstructure become thick, the crystalline substance of final products Grain grain size is not small enough, and the iron loss improvement brought by specific resistance increase is also very faint.Moreover, the additive amount as Mn is more than When 2.0 weight %, Fe is formed in surface of steel plate2SiO4Except can also form Mn oxide (Mn Oxide), in final annealing process In cannot be smoothed out decarburization.Therefore, the preferred additive amount of Mn is 0.001 weight % to 2.0 weight %.More specifically, Mn Additive amount be 0.01 weight % to 1.0 weight %.
In one embodiment of this invention, aluminium (Al) is considered inevitable impurity.That is, can be in slab and steel plate Al content is minimized.Specifically, when further including Al, range can be limited in 0.01 weight % or less.
Aforesaid ingredients be the present invention basic composition, even if in addition to this also have inevitably other alloying elements or Addition can improve other alloying elements of magnetic characteristic, cannot weaken the microminiaturization that feature of present invention is orientated crystal grain by Gauss To improve the effect of iron loss.
The method for manufacturing slab by the molten steel of aforementioned component can be Method of Partitioning, continuous metal cast process, sheet billet casting or strip casting.
Next, can be reheated to slab.Slab reheating temperature can be 1050 DEG C to 1350 DEG C.To slab into When row reheats, if temperature is low, rolling load increases;If temperature is high, it is likely that following problem occur:Form eutectic Point high-temperature oxide washs (washing) phenomenon to slab occur, and casting yield reduces, and also results in hot rolling microstructure in addition Coarsening carrys out harmful effect to magnetic recording tape.
Next, carrying out hot rolling to the slab for completing to reheat to manufacture hot rolled steel plate.When carrying out hot rolling, there can be Austria Family name's body carries out hot rolling within the temperature range of mutually existing, to manufacture hot rolled steel plate.In a low temperature of there is no austenite phase, not only Increase rolling load, the crystal grain microminiaturization effect by phase transformation can't be obtained.
Next, carrying out hot rolled plate annealing to hot rolled steel plate.It can be more than the temperature that can cause recrystallization and phase transformation At a temperature of to hot rolled plate carry out hot rolled plate annealing.Specifically, the low melting point oxide layer caused by high-temperature heating in order to prevent It generates, hot rolled plate annealing can be carried out at a temperature of 850 DEG C to 1150 DEG C.Atmosphere when hot rolled plate is annealed can be that can cause heat 0 DEG C or more the dew-point temperature and the atmosphere comprising hydrogen for rolling the decarburizing reaction of plate.
Next, carrying out first cold rolling to the hot rolled steel plate for completing hot rolled plate annealing.After implementing hot rolled plate annealing, Pickling can be carried out to steel plate and carries out cold rolling.Reduction ratio when cold rolling can be 50% to 70%.
Next, carrying out decarburizing annealing to the steel plate after cold rolling.Annealing for recrystallization is implemented to cold-rolled steel sheet, at this time In order to cause decarburizing reaction, at a temperature of 800 DEG C to 1150 DEG C, with 0 DEG C or more of dew-point temperature and include hydrogen Implement annealing in atmosphere.If temperature is too low, it is difficult to carry out decarburization;If temperature is excessively high, thicker oxide layer can be formed, instead may It can hinder decarburizing reaction.If dew-point temperature is too low, decarburizing reaction may be hindered.More specifically, dew-point temperature can be 10 DEG C To 70 DEG C.
Next, carrying out secondary cold-rolling to the steel plate for completing decarburizing annealing.Reduction ratio when cold rolling can be 50% to 70%. The step of decarburizing annealing is carried out to the steel plate after cold rolling and the step of carry out secondary cold-rolling to the steel plate for completing the decarburizing annealing It can repeatedly more than twice.As an example repeatedly twice when, can by first cold rolling step, decarburization annealing step, secondary cold-rolling step, The sequence of decarburization annealing step, three times cold rolling step and final annealing step carries out.At this point, in last one of cold rolling step until Implement cold rolling until as final product thickness, in order to cause decarburizing reaction in per pass decarbonization process, extremely at 800 DEG C At a temperature of 1150 DEG C, implement annealing in the atmosphere with 0 DEG C or more of dew-point temperature and comprising hydrogen.
Next, carrying out final annealing to the steel plate for completing cold rolling.
In the manufacturing method of the oriented electrical steel of one embodiment of the invention, not with previous (batch) in batches mode And then it continuously can implement final annealing by secondary cold-rolling with ground.
Final annealing step may include first step and second step, first step at a temperature of 850 DEG C to 1150 DEG C, Implement in the atmosphere that 10 DEG C to 70 DEG C of dew-point temperature, second step at a temperature of 900 DEG C to 1200 DEG C, include dew-point temperature 10 Implement in the mixed-gas atmosphere of DEG C hydrogen and nitrogen below.First step can be implemented 300 seconds hereinafter, second step can be implemented 60 seconds To 300 seconds.
Cold-reduced sheet before final annealing is in the 40 weight % to 60 because having carried out carbon amounts in decarburizing annealing at least slab The remaining state of silicon steel carbon amounts of weight %.Therefore, in the first step in final annealing, with the disengaging of carbon, on surface layer The crystal grain formed in part is internally spread.In the first step, can make carbon amounts in steel plate become 0.01 weight % with Under mode implement decarburization.
Later in the second step, the texture growing being orientated with Gauss spread in the first step.With it is previous because Abnormal particle growth and it is different the case where grain growth, in the manufacturing method of the oriented electrical steel of one embodiment of the invention Size of microcrystal can be within 1mm in goss texture.Therefore, compared with previous oriented electrical steel, one embodiment of the invention Oriented electrical steel can have the microstructure that crystal grain is constituted is orientated by the very small Gauss of size of microcrystal.
The carbon amounts completed in the electric steel plate of final annealing can be 0.003 weight % or less.
The oriented electrical steel of completion final annealing is dried after can coating insulating coating solution as needed.
In addition, in the final annealing of previous (Batch) in batches form, due to applying coated with the annealing that MgO is principal component Release agent, can have a MgO coatings, but the oriented electrical steel of one embodiment of the invention is due to can be in a continuous manner and overstepping one's bounds Batch mode carries out final annealing, therefore MgO coatings can be not present.
The Gauss that an embodiment through the invention generates is orientated (from { 110 }<001>The orientation being orientated within 15 degree) Crystal grain is showed more cold rolling and the decarburizing annealing then more increased tendency of crystal grain is repeated, and in the cold rolling carried out at least twice and is taken off After carbon annealing, the volume fraction for the crystal grain being orientated with Gauss in steel plate at least increases by 50% or more.
The grain size for the crystal grain that an embodiment through the invention generates is less than 5mm, the volume of 20 μm to 1000 μm of crystal grain It is 50% or more to divide rate.As a result, existing magnetic domain size is very small in crystal grain.The visible magnetic in previous oriented electrical steel Farmland size is bigger than conventional steel sheet thickness, but existing magnetic domain size in the crystal grain of the steel plate of embodiment manufacture through the invention 2L is less than steel plate thickness D.
The oriented electrical steel of one embodiment of the invention % by weight includes:Si:More than 0 weight % and 4.0 weight % Below, C:More than 0 weight % and 0.003 weight % or less and Mn:0.001 weight % to 2.0 weight %, surplus by Fe and its Inevitably mixed impurity is constituted for he, and existing magnetic domain size 2L is less than the thickness D of steel plate in crystal grain.
The composition of oriented electrical steel is identical as the composition of aforementioned slab, and model is formed in the manufacturing process of oriented electrical steel It encloses and does not have substantive variation, therefore omit repeated explanation.But, as previously described, because in decarburizing annealing and final annealing Decarburization is carried out in the process, therefore carbon content becomes 0.003 weight % or less.
The volume fraction for the crystal grain that the oriented electrical steel of one embodiment of the invention is orientated in steel plate with Gauss is extremely It reduces and adds 50% or more, therefore iron loss and magnetic flux density are excellent.In addition, in oriented electrical steel, grain size is 20 to 1000um Crystal grain account for 50% or more, the maximum value of size of microcrystal is less than 5mm, at this time in crystal grain existing magnetic domain size be less than steel plate Thickness.Because of this small domain structure, the abnormal eddy-current loss of the steel plate manufactured through the invention and pass through previous method The abnormal eddy-current loss of the oriented electrical steel of manufacture is compared to greatly reducing, to greatly improve whole iron loss.
More specifically, existing magnetic domain size 2L can be 10 μm to 500 μm in crystal grain.
In the following, present invention will be further described in detail through examples.But this embodiment is only intended to illustrate the present invention, this Invention is not limited to this.
Embodiment 1
Heating contains Si in terms of weight % at a temperature of 1100 DEG C:2.0 weight %, C:0.15% and Mn:0.05% simultaneously And after including the Fe of surplus and the slab of inevitable impurity, it is rolled into the thickness of 3mm, then at 1000 DEG C of annealing temperature Implement hot rolled plate to anneal and carry out cooling progress pickling later, implements to be cold-rolled to final thickness 0.27mm later.Implementing cold rolling When to final thickness, implement among cold rolling and cold rolling not comprising decarburizing annealing and direct cold rolling to final thickness method, And include the once above decarburizing annealing and the method for carrying out multistep cold rolling among cold rolling and cold rolling.Decarburizing annealing is 1000 Implement at a temperature of DEG C, in the moistening mixed-gas atmosphere (60 DEG C of dew-point temperature) of hydrogen and nitrogen.
When carrying out final annealing later, at a temperature of 1000 DEG C, the moistening mixed-gas atmosphere (dew-point temperature of hydrogen and nitrogen 60 DEG C) in implement annealing in two minutes after, at 1100 DEG C, the mixed gas gas of the hydrogen and nitrogen of dry (0 DEG C of dew-point temperature) Annealing in three minutes is implemented in atmosphere.
In the steel plate for completing final annealing process, compare the relationship point between rate and magnetic characteristic that Gauss is orientated crystal grain, And it is shown in table 1.
Wherein, point rate for crystal grain being orientated for Gauss is evaluated, and is measured from reason using conventional crystalline orientation measurement method { 110 } thought<001>Being orientated has the volume fraction of the crystal grain of the orientation of error within 15 degree.
Also, Ke Er microscopes are used, magnetic domain are observed in the state of demagnetizing to electric steel plate, to measure magnetic domain Mean size.
[table 1]
As shown in table 1, include occurring at least once during being cold-rolled to final thickness after implementing hot rolled plate annealing In the case of the intermediate annealing of decarburization, point rate that the Gauss in final products is orientated crystal grain can at least ensure 50% or more, energy Enough obtain small magnetic domain size.Divide rate and small magnetic domain size, final products that can obtain by this high Gauss orientation Obtain excellent magnetic flux density and low iron loss characteristic.
Embodiment 2
Slab is manufactured in the case of changing the Si contents in slab like that as shown in the following Table 2, the slab is with weight % Meter contains C:0.2% and Mn:0.05%, and include the Fe of surplus and inevitable impurity.Add at a temperature of 1150 DEG C 3mm thickness is rolled into after hot slab, then implement at 950 DEG C of annealing temperature hot rolled plate anneal and carry out it is cooling after implement it is sour It washes, and cold rolling is carried out with 60% reduction ratio.At a temperature of 900 DEG C, the mixed gas of the hydrogen and nitrogen of 60 DEG C of dew-point temperature Recrystallization and decarburizing annealing are implemented to the plate after cold rolling in atmosphere.Later, identical cold rolling twice is further repeated and takes off Carbon is annealed.Finally, after being cold-rolled to the steel plate thickness of 0.23mm, at a temperature of 950 DEG C, the hydrogen of 60 DEG C of dew-point temperature and nitrogen it is mixed The decarburizing annealing (first step) implemented in gas atmosphere 180 seconds is closed, later in the nitrogen atmosphere of 1000 DEG C of drying (0 DEG C of dew point) Implement heat treatment (second step) in 100 seconds.It is shown in table 2 special in the magnetic for changing the final annealing steel plate of Si contents Property.
[table 2]
As shown in table 2, when Si contents are 4 weight % or less, microcosmic group is ensured by multiple cold rolling and decarburizing annealing The final size of microcrystal knitted be 1000 μm hereinafter, ensure at this time magnetic domain size be less than steel plate thickness result can ensure it is excellent Iron loss.In the case where Si contents are more than 4 weight %, brittleness increases, and causes plate to rupture when carrying out cold rolling, it is difficult to be cold rolled to most Whole thickness, and fail realization decarburization during decarburizing annealing, show the size of microcrystal of very little and poor magnetic characteristic.
Embodiment 3
Heating contains Si in terms of weight % at a temperature of 1200 DEG C:3.0 weight %, C:0.25% and Mn:0.5% and Including after the slab of the Fe of surplus and inevitable impurity, it is rolled into the thickness of 2.5mm, then in 1100 DEG C of annealing temperature Under, implement hot rolled plate in the mixed-gas atmosphere of the hydrogen of 40 DEG C of dew-point temperature and nitrogen and anneal and carry out carrying out pickling after cooling down, it Once cold rolling is carried out with 65% reduction ratio afterwards.Then, at a temperature of 1050 DEG C, the hydrogen of 60 DEG C of dew-point temperature and nitrogen it is wet Moisten in mixed-gas atmosphere and decarburizing annealing is implemented to the plate after cold rolling.Later, secondary cold-rolling is implemented extremely to first decarburizing annealing plate Final annealing is carried out after final thickness 0.30mm.For final annealing, change the feelings of annealing temperature as shown in the following Table 3 Under condition, implement decarburizing annealing (first step) in the hydrogen of 65 DEG C of dew-point temperature and the moistening mixed-gas atmosphere of nitrogen, so that carbon contains Amount can become 0.003 weight % or less.Finally, and then decarburizing annealing, further heats up, at 1150 DEG C, 0 DEG C of dew point Implement final heat treatment (second) in dry nitrogen atmosphere.It is measured the size of microcrystal of the steel plate of final annealing, and is used Ke Er is measured microscopically magnetic domain size, and is shown in following table 3 after being compared with magnetic characteristic.
[table 3]
As shown in table 3, in the case where final annealing temperature (first step) is 850 to 1150 DEG C, in the final product, grain The ratio for the crystal grain that diameter is 20 to 1000 μm is 50% or more, and magnetic domain size is also shown smaller than steel plate thickness therewith, is shown Excellent iron loss characteristic.In the case where decarburization annealing temperature is less than 850 DEG C, the magnetic domain size showed is very small, but thinks It is 50% or less to cause the Gauss that the reason of whole magnetic characteristic difference is in crystal grain to be orientated point rate.On the contrary, in decarburization annealing temperature In the case of higher than 1150 DEG C, size of microcrystal is coarse, and magnetic domain size is more than steel plate thickness therewith, and iron loss is not improved.
The present invention is not limited to above-described embodiments, can be manufactured by different diversified forms.Technology belonging to the present invention is led The technical staff in domain will be understood that can be by other concrete forms on the basis of not changing technical thought of the invention or essential feature Implement the present invention.It is therefore to be understood that embodiment described above is schematical in all respects, rather than it is restrictive.

Claims (19)

1. a kind of manufacturing method of oriented electrical steel, includes the following steps:
Slab is provided, slab % by weight includes:Si:More than 0 weight % and 4.0 weight % or less, C:0.001 weight % To 0.4 weight % and Mn:0.001 weight % to 2.0 weight %, surplus is by Fe and other inevitably mixed impurity structures At;
The slab is reheated;
Hot rolling is carried out to manufacture hot rolled steel plate to the slab;
Hot rolled plate annealing is carried out to the hot rolled steel plate;
First cold rolling is carried out to the hot rolled steel plate by hot rolled plate annealing;
Decarburizing annealing is carried out to the steel plate Jing Guo the cold rolling;
Steel plate to completing the decarburizing annealing carries out secondary cold-rolling;And
Steel plate to completing the cold rolling carries out final annealing,
Complete the thickness (D) that the steel plate of the final annealing existing magnetic domain size (2L) in crystal grain is less than steel plate.
2. the manufacturing method of oriented electrical steel according to claim 1, wherein
The slab includes to be more than 0 weight % and 1 weight % Si below.
3. the manufacturing method of oriented electrical steel according to claim 1, wherein
The slab is further included more than 0 weight % and 0.01 weight % Al below.
4. the manufacturing method of oriented electrical steel according to claim 1, wherein
The relation reheating temperature of the slab is 1050 DEG C to 1350 DEG C.
5. the manufacturing method of oriented electrical steel according to claim 1, wherein
Reduction ratio in the first cold rolling the step of and the step of the secondary cold-rolling is respectively 50% to 70%.
6. the manufacturing method of oriented electrical steel according to claim 1, wherein
Two are carried out in the step of carrying out decarburizing annealing to the steel plate Jing Guo the cold rolling and to the steel plate for completing the decarburizing annealing The step of secondary cold rolling, is repeated more than twice.
7. the manufacturing method of oriented electrical steel according to claim 1, wherein
The step of decarburizing annealing, is at a temperature of 800 DEG C to 1150 DEG C, in the atmosphere of the hydrogen comprising 0 DEG C of dew-point temperature or more Implement.
8. the manufacturing method of oriented electrical steel according to claim 1, wherein
The step of final annealing includes first step and second step, temperature of the first step at 850 DEG C to 1150 DEG C Implement under degree, in the atmosphere of 10 DEG C to 70 DEG C of dew-point temperature, the second step at a temperature of 900 DEG C to 1200 DEG C, include Implement in the mixed-gas atmosphere of 10 DEG C of dew-point temperature hydrogen and nitrogen below.
9. the manufacturing method of oriented electrical steel according to claim 8, wherein
The first step is implemented 300 seconds hereinafter, the second step is implemented 60 seconds to 300 seconds.
10. the manufacturing method of oriented electrical steel according to claim 1, wherein
The step of final annealing being carried out continuously after the cold rolling the step of.
11. the manufacturing method of oriented electrical steel according to claim 1, wherein
Carbon amounts after the final annealing the step of in electric steel plate is more than 0 weight % and 0.003 weight % or less.
12. the manufacturing method of oriented electrical steel according to claim 1, wherein
In the steel plate for completing final annealing, from { 110 }<001>Being orientated the volume fraction with the crystal grain being orientated within 15 degree is 50% or more.
13. the manufacturing method of oriented electrical steel according to claim 1, wherein
The volume fraction for the crystal grain that grain size is 20 μm to 1000 μm in the steel plate for completing final annealing is 50% or more.
14. a kind of oriented electrical steel,
% by weight is counted:Si:More than 0 weight % and 4.0 weight % are hereinafter, C:More than 0 weight % and 0.003 weight % with Lower and Mn:0.001 weight % to 2.0 weight %, surplus by Fe and other inevitably mixed impurity is constituted,
Existing magnetic domain size (2L) is less than the thickness (D) of steel plate in crystal grain.
15. oriented electrical steel according to claim 14, wherein
Including more than 0 weight % and 1.0 weight % Si below.
16. oriented electrical steel according to claim 14, wherein
It further includes and is more than 0 weight % and 0.01 weight % Al below.
17. oriented electrical steel according to claim 14, wherein
Existing magnetic domain size (2L) is 10 μm to 500 μm in crystal grain.
18. oriented electrical steel according to claim 14, wherein
From { 110 }<001>It is 50% or more that being orientated, which has the volume fraction for the crystal grain being orientated within 15 degree,.
19. oriented electrical steel according to claim 14, wherein
The volume fraction for the crystal grain that grain size is 20 μm to 1000 μm is 50% or more.
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