CN104726760B - Method for manufacturing the oriented electrical steel sheet - Google Patents
Method for manufacturing the oriented electrical steel sheet Download PDFInfo
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- CN104726760B CN104726760B CN201410806720.7A CN201410806720A CN104726760B CN 104726760 B CN104726760 B CN 104726760B CN 201410806720 A CN201410806720 A CN 201410806720A CN 104726760 B CN104726760 B CN 104726760B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/16—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of sheets
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Abstract
The method for manufacturing the oriented electrical steel sheet according to one embodiment of the present invention comprises the steps of providing an electrical steel sheet slab; re-heating the slab; hot-rolling the slab into a hot-rolled steel sheet; cold-rolling the hot-rolled steel sheet into a cold-rolled steel sheet; performing primary recrystallization annealing on the cold-rolled steel sheet; and performing secondary recrystallization annealing on the electrical steel sheet after primary recrystallization annealing, wherein the secondary recrystallization annealing is performed in a state with an electric field applied.
Description
Technical field
The present invention relates to the manufacture method and oriented electrical steel of a kind of oriented electrical steel.
Background technology
Oriented electrical steel is a kind of very excellent soft magnetic material of magnetic property on steel plate rolling direction, because orientation
Electric steel plate forms so-called goss texture, and all crystal grains of wherein steel plate surface are oriented to { 110 } face, and in the rolling direction
Crystal orientation is parallel to 001 ＞ axles of ＜.
Generally, magnetic property represents magnetic flux density and iron loss, crystal grain is orientated according to 001 ＞ of { 110 } ＜ and is correctly arranged with regard to energy
Obtain high magnetic flux density.
001 ＞ of its { 110 } of the excellent oriented electrical steel of magnetic property ＜ orientations goss texture (Goss texture) should
It is highly developed along steel plate rolling direction, in order to form this set texture, need to by the secondary recrystallization of abnormal grain growth come
Form Gauss orientation crystal grain.
To form this goss texture, various process conditions should very accurate, be strictly controlled, as in the steel-making stage
Slab when component control, hot rolling is reheated and hot rolling technology controlling factors, hot rolled plate are annealed, primary recrystallization is annealed, secondary
Recrystallization annealing etc..
Oriented electrical steel is by slab reheating, hot rolling, hot rolled plate annealing, once cold rolling or including intermediate annealing
Secondary cold-rolling, primary recrystallization, secondary recrystallization technique to be manufacturing.
Secondary recrystallization annealing process is divided into the temperature rise period of the secondary recrystallization to form Gauss (Goss) crystal grain and improvement
Purification annealing (purification annealing) stage of iron loss.
In the temperature rise period, in order to allow the secondary recrystallization to form Gauss (Goss) crystal grain stably to occur, to be less than or wait
1050 DEG C～1100 DEG C of secondary recrystallization started temperature is warming up in the slow speed of 40 DEG C/hr.
Formed Gauss (Goss) crystal grain secondary recrystallization terminate after, due to precipitate formation element N and S it is not complete
It is complete to remove, there are many island crystal grain (island during precipitate, and secondary recrystallization Gauss crystal grain can be re-formed during cooling
Grain), iron loss is caused to increase.
Therefore, at a temperature of more than 1100 DEG C that secondary recrystallization terminates, implement the long-time purification of more than 30 hours
Annealing, to remove the island crystal grain in N, S and secondary recrystallization crystal grain of residual, and then improves iron loss.
The purification annealing process that the long heat treatment of more than 30 hours is carried out at a temperature of more than 1100 DEG C is to ensure that
The necessary technique of low iron loss, but the productivity ratio of oriented electrical steel can be caused to decline, and maintain high temperature consume many energy.
The content of the invention
It is an object of the invention to provide a kind of oriented electrical steel and its manufacture method.
The manufacture method of the oriented electrical steel of one embodiment of the invention, including：
Electric steel plate slab is provided, the electric steel plate slab is in terms of percentage by weight (%) comprising 2.0～6.5%
Si, balance of Fe and other inevitable impurity；
The slab is reheated；
The slab is rolled into into hot rolled steel plate；
The hot rolled steel plate is cold rolled to into cold-rolled steel sheet；
Primary recrystallization annealing is carried out to the cold-rolled steel sheet；And
Secondary recrystallization annealing is carried out to the electric steel plate after primary recrystallization annealing；
Wherein, the secondary recrystallization annealing is carried out in the state of electric field is applied.
The secondary recrystallization annealing includes temperature rise period and purification annealing stage, and the purification annealing can apply electric field
In the state of carry out.
The big I of the electric field is 1kV/cm～3kV/cm.
For the annealing atmosphere of secondary recrystallization annealing, hot place can be carried out using the mixed gas of hydrogen and nitrogen in the temperature rise period
Reason, can carry out all heat-treated using hydrogen in purification annealing stage.
The temperature rise period is to be warming up to 1050 DEG C～1100 DEG C of stage, can be with the liter less than or equal to 40 DEG C/hr
Warm speed heats up, and can more than 1100 DEG C at a temperature of carry out purification annealing.
The manufacture method of the oriented electrical steel, can also include：After the rolling hot-rolling steel plate, to hot rolled plate
Annealed, hot rolled plate annealing can more than 900 DEG C at a temperature of carry out.
Once cold rolling or more than twice cold rolling including intermediate annealing are carried out in the rolling cold-rolled steel sheet, and
The temperature that steel plate can be carried out in cold-rolled process maintains more than 100 DEG C of warm-rolling.
The manufacture method of the oriented electrical steel, may also include：After the rolling cold-rolled steel sheet, to cold-rolled steel sheet
Carry out decarburizing annealing and nitridation annealing, and it is described cold-rolled steel sheet is carried out decarburizing annealing and nitridation annealing when, can carry out simultaneously
Decarburizing annealing and nitridation annealing.
The nitrogen quantity that the decarburizing annealing and nitridation annealing are formed in may proceed to steel plate is 100～300ppm.
The slab in terms of percentage by weight (%) can include 2.0～6.5% Si, 0.015～0.04% Al,
Less than 0.20% Mn (do not include 0%), less than 0.01% N, 0.01～0.10% C, less than 0.01% S (do not include
0%), balance of Fe and other inevitable impurity.
The oriented electrical steel of one embodiment of the invention is manufactured by the following method, and electric steel plate slab is carried out again
Heating, be rolled into hot rolled steel plate, the slab by weight percentage comprising 2.0～6.5% Si, balance of Fe and other
Inevitably then the hot rolled steel plate is cold rolled to cold-rolled steel sheet, carries out primary recrystallization to the cold-rolled steel sheet by impurity
Annealing, then secondary recrystallization annealing is carried out to the electric steel plate after primary recrystallization annealing, the secondary recrystallization annealing
Carry out in the state of electric field is applied, N, S content remained in electric steel plate is respectively below 10ppm.
The secondary recrystallization annealing includes temperature rise period and purification annealing stage, enters in the state of the electric field is applied
The row purification annealing, then N, S content for remaining in electric steel plate can be below 10ppm respectively.
When the size of the electric field is 1kV/cm～3kV/cm, residual N, the S content in electric steel plate can be 10ppm respectively
Below.
The manufacture method of the oriented electrical steel of one embodiment of the invention shortens the purification annealing in secondary recrystallization technique
Time, so as to improve productivity ratio.
And, shorten purification annealing time and can reduce the energy produced needed for electric steel plate, so as to improve business efficiency.
In addition, purification can increase the atomic diffusion rates inside electric steel plate when annealing, after purification annealing, the N of residual,
Island crystal grain (island grain) in S and Gauss (GOSS) secondary recrystallization crystal grain less than conventional electric steel plate, therefore
The electric steel plate more excellent than conventional electric steel plate magnetic property can be provided.
Specific embodiment
Referring to the drawings and the following example for describing in detail, it is possible to be expressly understood advantages of the present invention, feature and
The method for realizing these advantages and feature.However, the present invention can be implemented in a variety of different ways, it is not limited to following enforcement
Example.The purpose for providing the following example is that the fully open present invention is so that those skilled in the art has to the content of the invention
One comprehensively understands, and protection scope of the present invention should be defined by claims.The identical accompanying drawing mark in description in the whole text
Note represents identical element.
The manufacture method of the oriented electrical steel of one embodiment of the invention, including：Electric steel plate slab is provided；To the plate
Base is reheated；The slab is rolled into into hot rolled steel plate；The hot rolled steel plate is cold rolled to into cold-rolled steel sheet；To described cold rolling
Steel plate carries out primary recrystallization annealing；And secondary recrystallization annealing is carried out to the electric steel plate after primary recrystallization annealing,
Wherein, the secondary recrystallization annealing is carried out in the state of electric field is applied.
The electric field level can be 1kV/cm～3kV/cm.
The secondary recrystallization annealing includes temperature rise period and purification annealing stage, and the purification annealing can apply electric field
In the state of carry out.
For the annealing atmosphere of secondary recrystallization annealing, the temperature rise period can enter under the mixed-gas atmosphere of hydrogen and nitrogen
Row heat treatment, purification annealing stage can carry out all heat-treated in a hydrogen atmosphere.
The temperature rise period is to be warming up to 1050 DEG C～1100 DEG C of stage, can be with the liter less than or equal to 40 DEG C/hr
Warm speed heats up, and can more than 1100 DEG C at a temperature of carry out purification annealing.
In the manufacturing process of oriented electrical steel, in order to secondary recrystallization can stably occur under high temperature, as crystal grain
Growth inhibitor uses precipitate, more than the precipitate decomposition temperature at a temperature of secondary recrystallization can occur.
But, after secondary recrystallization annealing, if precipitate formation element N and S are remained in electric steel plate, meeting during cooling
Re-form precipitate and hinder magnetic domain movement, so as to cause iron loss to increase.Secondary recrystallization due to forming Gauss (Goss) crystal grain
Occur at a very rapid rate, therefore after secondary recrystallization terminates, in Gauss (Goss) crystal grain, can there are many island crystal grain
(island grain), and this island crystal grain may interfere with the movement of magnetic domain, cause iron loss to increase.
Therefore, it is the oriented electrical steel that manufactures low iron loss, after secondary recrystallization, it is necessary to implement long at high temperature
The purification annealing process of time heat treatment.
If increasing the diffusion velocity of atom, the N remained after will promoting to form secondary recrystallization and S diffusions, and then can
Shorten the time for removing N and S, can also promote Fe diffusions in mother metal, and then the time for removing island crystal grain can be shortened.
There are many free electrons in metal material, using electrode from it is outside apply electric field when, surface can powered and polarity
With outer electrode conversely, electric potential difference is produced between surface and center.Therefore, electro-chemical potential (electro-chemical can be produced
Potential difference), in metal, the hole mobility of opposite band negative polarity can increase.The increase of hole mobility finally makes ferrum
Atomic diffusion rates increase.
Therefore, the purification annealing stage in secondary recrystallization annealing, if carrying out hot place in the state of electric field is applied
Reason, the N remained after will promoting to form secondary recrystallization and S diffusions, and then the time for removing N and S can be shortened, also promote mother
The Fe diffusions of material, and then the time for removing island crystal grain can be shortened.
And, if purification annealing is carried out in the state of electric field is applied, can more effectively remove N, S than prior art.
Therefore, according to one embodiment of the invention, the oriented electrical steel after secondary recrystallization annealing will can be remained in electric steel plate
N and S contents controlled in below 10ppm respectively.
In order to have uniform recrystallization microtextured and fine precipitate distribution before cold rolling, can be with described
After rolling hot-rolling steel plate, hot rolled plate is annealed, hot rolled plate annealing can more than 900 DEG C at a temperature of carry out.
Additionally, carrying out once cold rolling or more than twice cold including intermediate annealing in the rolling cold-rolled steel sheet
Roll, and the warm-rolling that steel billet temperature maintains more than 100 DEG C can be carried out in cold-rolled process.
And, the primary recrystallization annealing carried out after the rolling cold-rolled steel sheet can carry out nitrogen after decarburizing annealing
Annealing can carry out decarburizing annealing and nitridation annealing simultaneously.
The nitrogen quantity that the decarburizing annealing and nitridation annealing are formed in may proceed to steel plate is 100～300ppm.Nitrogen quantity is less than
During 100ppm, nitrogen possibly cannot normally form inhibitor, when nitrogen quantity is more than 300ppm, in secondary recrystallization annealing process, remove
Denitrification may need the excessive time.
The slab includes 2.0～6.5% Si, balance of Fe and other inevitable impurity.And, the slab
Can also include 0.015～0.04% Al, less than 0.20% Mn (do not include 0%), less than 0.01% N, 0.01～
0.10% C, less than 0.01% S (not including 0%).
The reasons why to limiting the components system, illustrates.
[Si:2.0～6.5 weight %]
Solvents of the Si as electric steel plate, plays a part of to increase resistivity of material reduction iron loss (core loss).
When Si contents are less than 2.0 weight %, resistivity reduces eddy-current loss and increases, and causes iron loss characteristic to deteriorate.And,
In high annealing, undergo phase transition between ferrite and austenite, not only secondary recrystallization becomes unstable, and gather texture
Can also be badly damaged.
When Si contents are more than 6.5 weight %, the mechanical equivalent of light fragility of electric steel plate increases and toughness reduction, causes the operation of rolling
Middle plate splits incidence rate increase, and the formation of secondary recrystallization becomes unstable.
[Al:0.005～0.04 weight %]
Al except the AlN of micro- precipitation when hot rolling and hot rolled plate are annealed, also with the nitrogen that imported by ammonia during cold rolling after annealing from
The nitride shape of (Al, Si, Mn) N and AlN types that son is combined and formed with Al, Si, Mn for existing with solid solution condition in steel
Formula is present, so as to play a part of powerful grain growth inhibitor.
When Al is less than 0.005 weight %, the quantity and volume for being formed is at a fairly low level, therefore can not expect to fill
The inhibitor effect for dividing.
When Al is more than 0.040 weight %, thick nitride is formed, grain growth restraint can be reduced.
[Mn:Below 0.20 weight %]
Mn increases resistivity and reduces eddy-current loss, so as to have the effect for reducing overall iron loss, and with Si and passes through nitrogen
Change the precipitate for processing that the nitrogen for importing is reacted and formed (Al, Si, Mn) N, so as to suppress the growth of primary recrystallization crystal grain,
To there is secondary recrystallization.
When Mn is more than 0.20 weight %, surface of steel plate is except Fe2SiO4Outside can also form substantial amounts of (Fe, Mn) and Mn
Oxide, and then base coating is formed in hindering high annealing, cause poor surface quality, and cause ferrum in high annealing
Phase transformation between ferritic and austenite, thus gather texture can be badly damaged, magnetic property is greatly deteriorated.Therefore, Mn contents are limited to
Below 0.20 weight %.
[N:Below 0.01 weight %]
N is to form the element of AlN with Al reactions.In process for making, when N is more than 0.01 weight %, then in hot rolling
During afterwards, as nitrogen diffusion can cause surface defect, and excessive nitride is formed under slab state and is reduced
Rolling property, causes subsequent technique to become complicated, cost increase.
And, when the annealing process after cold rolling carries out the nitrogen treatment using ammonia, be to be formed (Al, Si, Mn) N and
The nitride such as AlN can further make necessary N solid solutions again.
[C:0.01～0.10 weight %]
C, as the element for causing phase transformation between ferrite and austenite, is to improve the fragility bad electrical sheet of rolling property by force
Element necessary to the rolling of plate.However, when C remains in final products, the carbide meeting formed because of magnetic aging effect
Magnetic property is made to be deteriorated.
When C content is less than 0.01 weight %, then as the phase transformation between ferrite and austenite can not normally play work
With slab and the inequality of hot rolling microtextured can be caused to homogenize.
And, when more than 0.10 weight %, then sufficient decarburization effect, Er Qieyin can not be obtained in decarburizing annealing technique
Phase transition phenomena secondary recrystallization set texture can be damaged, and cause the magnetic property degradation phenomena that magnetic aging causes.
[S:Below 0.010 weight %]
S is reacted and the important element of formation MnS with Mn.
When S contents are more than 0.01 weight %, the precipitate of MnS can suppress the growth of crystal grain, Er Qiezhu in being formed in slab
Slab central part can be segregated to when making, it is difficult to which the microtextured of subsequent technique is controlled.
Hereinafter, the present invention is further described by embodiment.
[embodiment 1]
Slab in terms of weight % comprising 3.18% Si, 0.056% C, 0.11% Mn, 0.0052% S,
0.0051% N, 0.028% Al, balance of Fe and other inevitable impurity.In 1150 DEG C of slab reheating temperature
Under, by the heating of plate blank 180 minutes, hot rolling was then carried out to be rolled into hot rolled plate of the thickness as 2.3mm.The hot rolled plate is heated
To after more than 1100 DEG C, kept for 90 seconds at 910 DEG C, and quickly cooled down in water, carried out with the thickness of 0.30mm after pickling cold
Roll.Cold-reduced sheet is kept for 180 seconds in the hydrogen of the humidity that temperature is 870 DEG C, nitrogen and ammonia gas mixture bromhidrosis atmosphere, and while
Decarburization and nitridation annealing are carried out, makes nitrogen content become 200ppm.Secondary recrystallization anneal when being warming up to 1200 DEG C 25% nitrogen+
Carry out under the mixed atmosphere of 75% hydrogen, and purification annealing is carried out at 1200 DEG C.
To confirm to carry out the effect for applying electric field when purification is annealed, in the state of applying electric field in electrode making alive, inspection
Survey and changed according to the iron loss of purification annealing time.
As shown in table 1, when purification annealing is carried out, when electric field of the applying size for 2kV/cm, purification annealing time is just
Can shorten.According to the general purification annealing heat-treats for not applying electric field, after annealing 30 hours, iron loss is 0.95W/k (contrast materials
9) carry out, but after applying an electric field purification anneal when, annealing 18 hours after, iron loss be 0.89W/kg (invention material 6), iron loss
It is extremely outstanding.
[embodiment 2]
Slab in terms of the percentage by weight (%) comprising 3.16% Si, 0.053% C, 0.98% Mn, 0.0052%
S, 0.0049% N, 0.028% acid-solubility Al, balance of Fe and other inevitable impurity.Temperature is reheated in slab
At 1150 DEG C of degree, by the heating of plate blank 180 minutes, hot rolling is then carried out to be rolled into hot rolled plate of the thickness as 2.3mm.By the heat
Roll after plate is heated to more than 1100 DEG C, kept for 90 seconds at 910 DEG C, and quickly cooled down in water, with the thickness of 0.30mm after pickling
Degree carries out cold rolling.Cold-reduced sheet is kept into 180 in the hydrogen of the humidity that temperature is 870 DEG C, nitrogen and ammonia gas mixture bromhidrosis atmosphere
Second, and while carry out decarburization and nitridation annealing, make nitrogen content be 200ppm.Secondary recrystallization is annealed when being warming up to 1200 DEG C
Carry out under the mixed atmosphere of+75% hydrogen of 25% nitrogen, and purification annealing is carried out at 1200 DEG C.
By confirming in the impact for carrying out the direction of an electric field applied when purification is annealed, in the shape for applying both positive and negative polarity electrode voltage
Purification annealing is carried out under state, iron loss is then detected.
[table 2]
As shown in table 2, when purification annealing is carried out, in the case of purification annealing time identical, apply the ferrum of external electrical field
Damage less.Even if changing the polarity of outer electrode, apply negative or positive electrode voltage and come conversion field direction, its effect difference is not yet
Greatly, and whether the applying of electric field has considerable influence to improving iron loss.
More than, embodiments of the invention are illustrated, however, it will be understood by those skilled in the art that not changing skill
In the case of art thought or essential feature, the present invention otherwise can be implemented.
Therefore, above-described embodiment is exemplary and nonrestrictive.Protection scope of the present invention should be with claim
Book is defined rather than described above, the shape for having altered or changing derived from the implication, scope and such equivalents by claims
Formula, all falls within protection scope of the present invention.
Claims (4)
1. a kind of manufacture method of oriented electrical steel, including：
Electric steel plate slab is provided, the electric steel plate slab is in terms of percentage by weight % comprising 2.0～6.5% Si, surplus
For Fe and other inevitable impurity；
The slab is reheated；
The slab is rolled into into hot rolled steel plate；
The hot rolled steel plate is cold rolled to into cold-rolled steel sheet；
Primary recrystallization annealing is carried out to the cold-rolled steel sheet；And
Secondary recrystallization annealing is carried out to the electric steel plate after primary recrystallization annealing；
Wherein, the secondary recrystallization annealing includes temperature rise period and purification annealing stage, and the purification annealing is applying electric field
In the state of carry out.
2. the manufacture method of oriented electrical steel according to claim 1, wherein,
The size of the electric field is 1kV/cm～3kV/cm.
3. the manufacture method of oriented electrical steel according to claim 2, also includes：
After the rolling hot-rolling steel plate, more than 900 DEG C at a temperature of, hot rolled plate is annealed.
4. the manufacture method of the oriented electrical steel according to any one of claims 1 to 3, wherein,
The slab also comprising 0.015～0.04% Al, the Mn more than 0% and less than or equal to 0.20%, less than 0.01%
N, 0.01～0.10% C, the S more than 0% and less than or equal to 0.01%.
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| KR102177523B1 (en) | 2015-12-22 | 2020-11-11 | 주식회사 포스코 | Grain orientied electrical steel sheet and method for manufacturing the same |
| KR102133909B1 (en) * | 2018-12-19 | 2020-07-14 | 주식회사 포스코 | Grain oriented electrical steel sheet and method for manufacturing the same |
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| JPS61181116A (en) * | 1985-02-07 | 1986-08-13 | Toshiba Corp | Manufacture of rolled iron core |
| JPH08143974A (en) * | 1994-11-28 | 1996-06-04 | Kawasaki Steel Corp | Production of grain-oriented silicon steel sheet |
| KR100241005B1 (en) * | 1995-12-23 | 2000-03-02 | 이구택 | The manufacturing method of oriented electric steel sheet with only one cold rolling processed |
| KR100521571B1 (en) * | 2003-04-18 | 2005-10-17 | 현대자동차주식회사 | Method of manufacturing Al-Mg-Si alloy sheet with excellent formability |
| KR101223115B1 (en) * | 2010-12-23 | 2013-01-17 | 주식회사 포스코 | Grain-oriented electrical steel sheet with extremely low iron loss and method for manufacturing the same |
| CN102127622B (en) * | 2011-01-18 | 2012-12-26 | 北京科技大学 | Method for improving magnetic characteristics of orientated silicon steel by heat treatment of pulse electric field |
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