CN102762752A - Manufacturing method for grain-oriented electromagnetic steel sheet - Google Patents
Manufacturing method for grain-oriented electromagnetic steel sheet Download PDFInfo
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- C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
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- C21D3/04—Decarburising
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- 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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- 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
- C21D8/1244—Modifying 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
- C21D8/1255—Modifying 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
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- 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
- C21D8/1244—Modifying 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
- C21D8/1272—Final recrystallisation annealing
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- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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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
Abstract
A hot-rolled steel sheet is produced by hot-rolling steel having a prescribed composition that includes 0.0020-0.010% Ti by weight and/or 0.010-0.50% copper by weight. An annealed steel sheet is produced by annealing the hot-rolled steel sheet. A cold-rolled steel sheet is produced by cold-rolling the annealed steel sheet. A decarburized annealed steel sheet is produced by decarburization annealing of the cold-rolled steel sheet at a temperature of 800-950 DEG C. A nitrided steel sheet is produced by nitriding the decarburized annealed steel sheet at a temperature of 700-850 DEG C. The nitrided steel sheet is finished by annealing.
Description
Technical field
The method of manufacture of the grain-oriented magnetic steel sheet that the present invention relates to have realized that the deviation (being scattered error, fluctuation) to magnetic properties suppresses.
Background technology
Grain-oriented magnetic steel sheet is that the azimuth elevation that contains Si, crystal grain accumulates in that { steel plate in 110}＜001＞orientation, it is used as the material of the Wound core etc. of static transformers such as X-former.The control of grain arrangement is to utilize the exaggerated grain growth phenomenon that is called as secondary recrystallization to carry out.
As the method for control secondary recrystallization, can enumerate out following two kinds of methods.A method is, makes the fine precipitate that is called as suppressor factor roughly fully after the solid solution under the temperature more than 1280 ℃ steel billet being heated, and carries out hot rolling, cold rolling and annealing etc., when hot rolling and annealing, fine precipitate separated out.Another method is, after being lower than under 1280 ℃ the temperature the steel billet heating, carries out hot rolling, cold rolling, decarburizing annealing, nitriding treatment and final annealing etc., when nitriding treatment, makes AlN as suppressor factor, (Al, Si) N etc. separates out.
, from recent years reduction CO
2The viewpoint of discharging is set out, the used time of decarburizing annealing in the manufacturing processed of requirement shortening grain-oriented magnetic steel sheet.Therefore, to using the low slab of C content to study.
But, be accompanied by the reduction of the C content of slab, behind the final annealing that carries out with the state that is wound into the coiled material shape, the deviation of the magnetic properties of different sites (magnetic properties deviation) becomes remarkable.
The prior art document
Patent documentation
Patent documentation 1: japanese kokai publication hei 3-122227 communique
Patent documentation 2: japanese kokai publication hei 11-323437 communique
Patent documentation 3: japanese kokai publication hei 6-256847 communique
Patent documentation 4: Japan special table 2001-515540 communique
Patent documentation 5: TOHKEMY 2000-199015 communique
Patent documentation 6: TOHKEMY 2007-254829 communique
Summary of the invention
The problem that invention will solve
The purpose of this invention is to provide a kind of method of manufacture that can suppress the grain-oriented magnetic steel sheet of magnetic properties deviation.
Be used to solve the means of problem
Understood that magnetic properties deviation behind above-mentioned such final annealing is below C content is 0.06 quality % and then be that 0.048 quality % is remarkable especially when following.The reason that produces the magnetic properties deviation behind the final annealing also do not confirm, even but can think that crystal grain can not grown equably yet sometimes in final annealing because before final annealing during visible equably crystal grain.In addition, as the reason that crystal grain can evenly not grown, can think because C content is low, thereby not carry out the phase transformation in the hot rolling fully, thereby the austenite phase transformation amount is little, it is unstable that hot rolling microstructure becomes.That is to say, can think not produce enough secondary recrystallizations, thereby not obtain good magnetic properties in the uneven part of hot rolling microstructure.
Present inventors based on experience so consider in order to make the grain growing homogenizing in the final annealing, whether can come to produce fully secondary recrystallization through forming effective precipitate.Thus, present inventors just the mensuration of the magnetic properties through in slab, adding the grain-oriented magnetic steel sheet that various elements obtain test repeatedly.As a result, present inventors find: for making the secondary recrystallization homogenizing, it is effective adding Ti and Cu.
The present invention is based on above-mentioned experience and accomplishes, and its main idea is following.
(1) a kind of method of manufacture of grain-oriented magnetic steel sheet is characterized in that, has following operation:
Steel is carried out hot rolling and obtain the operation of hot-rolled steel sheet; Said steel contains Si:2.5 quality %～4.0 quality %, C:0.01 quality %～0.060 quality %, Mn:0.05 quality %～0.20 quality %, acid-solubility Al:0.020 quality %～0.040 quality %, N:0.002 quality %～0.012 quality %, S:0.001 quality %～0.010 quality % and P:0.01 quality %～0.08 quality %; And further contain at least a kind that is selected among Ti:0.0020 quality %～0.010 quality % and the Cu:0.010 quality %～0.50 quality %, and remainder comprises Fe and unavoidable impurities;
Said hot-rolled steel sheet is annealed and obtain the operation of annealed sheet steel;
Carry out cold rolling to said annealed sheet steel and obtain the operation of cold-rolled steel sheet;
Under 800 ℃～950 ℃ temperature, said cold-rolled steel sheet carried out decarburizing annealing and obtain the operation of decarburizing annealing steel plate;
Then under 700 ℃～850 ℃, said decarburizing annealing steel plate carried out nitriding treatment and obtain the operation of nitriding treatment steel plate; And
Said nitriding treatment steel plate is carried out the operation of final annealing.
According to the method for manufacture of above-mentioned (1) described grain-oriented magnetic steel sheet, it is characterized in that (2) said steel is carried out hot rolling is after said steel is heated to the temperature below 1250 ℃, to carry out.
(3) according to the method for manufacture of above-mentioned (1) or (2) described grain-oriented magnetic steel sheet; It is characterized in that said steel further contains and is selected from least a among Cr:0.010 quality %～0.20 quality %, Sn:0.010 quality %～0.20 quality %, Sb:0.010 quality %～0.20 quality %, Ni:0.010 quality %～0.20 quality %, Se:0.005 quality %～0.02 quality %, Bi:0.005 quality %～0.02 quality %, Pb:0.005 quality %～0.02 quality %, B:0.005 quality %～0.02 quality %, V:0.005 quality %～0.02 quality %, Mo:0.005 quality %～0.02 quality % and the As:0.005 quality %～0.02 quality %.
According to the method for manufacture of each described grain-oriented magnetic steel sheet in above-mentioned (1)～(3), it is characterized in that (4) the Ti content of said steel is 0.0020 quality %～0.0080 quality %; The Cu content of said steel is 0.01 quality %～0.10 quality %; Be expressed as [Ti] at Ti content (quality %) with said steel, when the Cu content (quality %) of said steel is expressed as [Cu], the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up.
According to the method for manufacture of above-mentioned (4) described grain-oriented magnetic steel sheet, it is characterized in that (5) relation of " 10 * [Ti]+[Cu]≤0.07 " is set up.
The invention effect
According to the present invention, owing in steel, contain the Ti and/or the Cu of appropriate amount, and under suitable temperature, carry out decarburizing annealing and nitriding treatment, therefore can suppress the magnetic properties deviation.
Description of drawings
Fig. 1 is the figure of relation of the evaluation of expression Ti content and Cu content and magneticflux-density and deviation thereof.
Fig. 2 is the schema of method of manufacture of the grain-oriented magnetic steel sheet of expression embodiment of the present invention.
Embodiment
As stated, the present inventors just mensuration of the magnetic properties through in slab, adding the grain-oriented magnetic steel sheet that various elements obtain test repeatedly, and the result finds: for making the secondary recrystallization homogenizing, it is effective adding Ti and Cu.
In this experiment, for example use that C content is the silicon steel below the 0.06 quality % in the composition used in the manufacturing of the grain-oriented magnetic steel sheet utilize low temperature slab heating method.Then, in this carbon steel, contain Ti and Cu in all proportions, process the steel ingot of various compositions.And, under the temperature below 1250 ℃, steel ingot heated and carry out hot rolling, carry out cold rolling afterwards.And then, after cold rolling, carry out decarburizing annealing, carry out nitriding treatment and final annealing then.Then, measure the magneticflux-density B8 of resulting grain-oriented magnetic steel sheet, the deviation of the magneticflux-density B8 in the coiled material behind the investigation final annealing.Magneticflux-density B8 is the magneticflux-density that in grain-oriented magnetic steel sheet, produces when adding the magnetic field of 800A/m with 50Hz.
Its result finds: in steel ingot, contain under the situation of Cu of Ti and/or 0.010 quality %～0.50 quality % of 0.0020 quality %～0.010 quality %, the deviation of the magneticflux-density B8 in the coiled material behind the final annealing significantly reduces.
The result's who obtains through above-mentioned experiment shown in Fig. 1 a example.Though the details of experiment can after describe, zero mark among Fig. 1 representes that the MV of the magneticflux-density B8 of 5 veneer samples is that the above and peak of magneticflux-density B8 of 1.90T and the difference of Schwellenwert are below the 0.030T.In addition, among Fig. 1 ● the MV of representing the magneticflux-density B8 of at least 5 veneer samples is lower than the peak of 1.90T or magneticflux-density B8 and the difference of Schwellenwert surpasses 0.030T.Shown that by Fig. 1 when in steel ingot, containing the Cu of Ti and/or 0.010 quality %～0.50 quality % of 0.0020 quality %～0.010 quality %, the MV of magneticflux-density B8 is high, the deviation of magneticflux-density B8 is little.
Then, the method for manufacture to the grain-oriented magnetic steel sheet of embodiment of the present invention describes.Fig. 2 is the schema of method of manufacture of the grain-oriented magnetic steel sheet of expression embodiment of the present invention.
In this embodiment, at first, carry out the casting of the molten steel that grain-oriented magnetic steel sheet that regulation forms uses, make slab (step S1).Castmethod is not special to be limited.Molten steel for example contains Si:2.5 quality %～4.0 quality %, C:0.01 quality %～0.060 quality %, Mn:0.05 quality %～0.20 quality %, acid-solubility Al:0.020 quality %～0.040 quality %, N:0.002 quality %～0.012 quality %, S:0.001 quality %～0.010 quality % and P:0.01 quality %～0.08 quality %.Molten steel further contains at least a kind that is selected among Ti:0.0020 quality %～0.010 quality % and the Cu:0.010 quality %～0.50 quality %.That is to say, molten steel with the scope below the Ti:0.010 quality % and below the Cu:0.50 quality %, satisfy more than the Ti:0.0020 quality % at least or the side's more than the Cu:0.010 quality % mode contains a side or the both sides of Ti and Cu.The remainder of molten steel comprises Fe and unavoidable impurities.In addition, as unavoidable impurities, be also included within the manufacturing process of grain-oriented magnetic steel sheet and form suppressor factor, after utilizing the purifying of high temperature annealing, remain in the element in the grain-oriented magnetic steel sheet.
Here, the numerical definiteness reason to the composition of above-mentioned molten steel describes.
Si is unusual effective elements for the resistance that improves grain-oriented magnetic steel sheet, the eddy current losses that reduces a part that constitutes iron loss.If Si content is lower than 2.5 quality %, then can not fully suppress eddy current losses.On the other hand, if Si content surpasses 4.0 quality %, then processibility reduces.Therefore, Si content is defined as 2.5 quality %～4.0 quality %.
C is an effective elements for the tissue (primary recrystallization tissue) that control obtains through primary recrystallization.If C content is lower than 0.01 quality %, then can not fully obtain this effect.On the other hand, if C content surpasses 0.06 quality %, the required time lengthening of decarburizing annealing then, CO
2Quantity discharged increase.In addition, if decarburizing annealing is insufficient, then be difficult to the grain-oriented magnetic steel sheet that obtains having excellent magnetic characteristics.Therefore, C content is defined as 0.01 quality %～0.06 quality %.In addition, as stated, in the prior art, be under the situation below the 0.048 quality % at C content, the magnetic properties deviation behind the final annealing can be remarkable especially, so this embodiment is to be effective especially under the situation below the 0.048 quality % at C content.
Mn improves the ratio resistance of grain-oriented magnetic steel sheet and reduces iron loss.Mn also has the effect that prevents hot-rolled crackle.If Mn content is lower than 0.05 quality %, then can not fully obtain these effects.On the other hand, if Mn content surpasses 0.20 quality %, then the magneticflux-density of grain-oriented magnetic steel sheet reduces.Therefore, Mn content is defined as 0.05 quality %～0.20 quality %.
Acid-solubility Al is the important element that forms the AlN that plays a role as suppressor factor.If the content of acid-solubility Al is lower than 0.020 quality %, then can not form the AlN of q.s, thus the suppressor factor undercapacity.On the other hand, if the content of acid-solubility Al surpasses 0.040 quality %, thickization of AlN then, thereby suppressor factor strength degradation.Therefore, the content with acid-solubility Al is defined as 0.020 quality %～0.040 quality %.
N reacts with acid-solubility Al and forms the important element of AlN.Of the back, owing to be after cold rolling, to carry out nitriding treatment, therefore need do not contain a large amount of N in steel, but will make N content be lower than 0.002 quality % at grain-oriented magnetic steel sheet, need big load during steel-making sometimes.On the other hand, if N content surpasses 0.012 quality %, then when cold rolling, can in steel plate, produce the emptying aperture that is called as bubble.Therefore, N content is defined as 0.002 quality %～0.012 quality %.In order further to reduce bubble, preferred N content is below the 0.010 quality %.
S reacts with Mn and forms the important element of MnS precipitate.The MnS precipitate mainly exerts an influence to primary recrystallization, and the zonal change of the grain growing of the primary recrystallization that brings resulting from hot rolling is inhibited.If Mn content is lower than 0.001 quality %, then can not fully obtain this effect.On the other hand, if Mn content surpasses 0.010 quality %, then magnetic properties descends easily.Therefore, Mn content is defined as 0.001 quality %～0.010 quality %.In order further to improve magnetic properties, preferred Mn content is below the 0.009 quality %.
P improves the ratio resistance of grain-oriented magnetic steel sheet and reduces iron loss.If P content is lower than 0.01 quality %, then can not fully obtain this effect.On the other hand, if P content surpasses 0.08 quality %, the then cold rolling sometimes difficulty that becomes.Therefore, P content is defined as 0.01 quality %～0.08 quality %.
Ti and N react and form the TiN precipitate.In addition, Cu and S react and form the CuS precipitate.And, thereby having the growth of the crystal grain when making final annealing, these precipitates do not rely on the effect that ground, coiled material position homogenizing suppresses the magnetic properties deviation of grain-oriented magnetic steel sheet.Particularly, can think that the TiN precipitate can suppress the deviation of grain growing of the high-temperature zone of final annealing, thereby reduce the magnetic properties deviation of grain-oriented magnetic steel sheet.In addition, can think that the CuS precipitate can suppress the deviation of grain growing of the cold zone of decarburizing annealing or final annealing, thereby reduce the magnetic properties deviation of grain-oriented magnetic steel sheet.If Ti content is lower than 0.0020 quality % and Cu content is lower than 0.010 quality %, then can not fully obtain these effects.On the other hand,, form the TiN precipitate if Ti content surpasses 0.010 quality % then superfluously, also can be remaining behind final annealing.Equally,, form the CuS precipitate if Cu content surpasses 0.50 quality % then superfluously, also can be remaining behind final annealing.And, if these precipitates remain in the grain-oriented magnetic steel sheet, then be difficult to obtain high magnetic properties.Therefore, molten steel is with the scope below the Ti:0.010 quality % and below the Cu:0.50 quality %, to satisfy more than the Ti:0.0020 quality % at least or the side's more than the Cu:0.010 quality % mode contains a side or the both sides of Ti and Cu.That is to say that molten steel contains and is selected from least a among Ti:0.0020 quality %～0.010 quality % and the Cu:0.010 quality %～0.50 quality %.
In addition, the lower limit of Ti content is preferably 0.0020 quality %, and the upper limit of Ti content is preferably 0.0080 quality %.And the lower limit of Cu content is preferably 0.01 quality %, and the upper limit of Cu content is preferably 0.10 quality %.In addition, Ti content (quality %) is expressed as [Ti], when Cu content (quality %) is expressed as [Cu], more preferably the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up, the relation of preferred " 10 * [Ti]+[Cu]≤0.07 " is set up.
In addition, also can contain at least a in the following various element in the molten steel.
The character of the zone of oxidation that Cr and Sn form when improving decarburizing annealing is used the character of the glass epithelium that this zone of oxidation forms when also improving final annealing.That is to say that Cr and Sn improve magnetic properties through the stabilization that zone of oxidation and glass epithelium form, thereby suppress the magnetic properties deviation.But,, then become unstable during being formed with of glass epithelium if Cr content surpasses 0.20 quality %.In addition, if Sn content surpasses 0.20 quality %, then surface of steel plate be difficult to oxidized, insufficient during being formed with of glass epithelium.Therefore, Cr content and Sn content all are preferably below the 0.20 quality %.In addition, in order fully to obtain above-mentioned effect, Cr content and Sn content all are preferably more than the 0.01 quality %.In addition, Sn is the grain boundary segregation element, also has the effect that makes the secondary recrystallization stabilization.
In addition, also can contain Sb:0.010 quality %～0.20 quality %, Ni:0.010 quality %～0.20 quality %, Se:0.005 quality %～0.02 quality %, Bi:0.005 quality %～0.02 quality %, Pb:0.005 quality %～0.02 quality %, B:0.005 quality %～0.02 quality %, V:0.005 quality %～0.02 quality %, Mo:0.005 quality %～0.02 quality % and/or As:0.005 quality %～0.02 quality % in the molten steel.These elements all are the suppressor factor strengthening elements.
In this embodiment, after having made slab, slab is heated (step S2) from the molten steel of composition like this.The temperature of this heating preferably is defined as below 1250 ℃ from energy-conservation viewpoint.
Then, obtain hot-rolled steel sheet (step S3) through slab being carried out hot rolling.The thickness of hot-rolled steel sheet is not special to be limited, and for example is defined as 1.8mm～3.5mm.
Then,, hot-rolled steel sheet obtains annealed sheet steel (step S4) through being annealed.The annealed condition is not special to be limited, and for example under 750 ℃～1200 ℃ temperature, carries out 30 second～10 minute.Through this annealing, magnetic properties improves.
Then, through annealed sheet steel being carried out the cold rolling cold-rolled steel sheet (step S5) that obtains.Cold rolling can only carrying out 1 time is Yi Bian on one side also can carry out process annealing and carry out repeatedly cold rolling betwixt.30 second～10 minute are for example preferably carried out in process annealing under 750 ℃～1200 ℃ temperature.
In addition, if under the situation of not carrying out above-mentioned process annealing, carry out cold rollingly, then be difficult to obtain uniform characteristic sometimes.In addition, if Yi Bian, then obtain uniform characteristic easily, but magneticflux-density can reduce sometimes on one side carry out process annealing betwixt and carry out repeatedly cold rollingly.Therefore, the cold rolling number of times and the desired characteristic of the grain-oriented magnetic steel sheet that has or not preferred basis finally to obtain and the cost of process annealing decide.
In addition, in either case, all preferably final cold rolling draft is defined as 80%～95%.
After cold rolling,, obtain decarburizing annealing steel plate (step S6) through in 800 ℃～950 ℃ the moistening atmosphere that contains hydrogen and nitrogen, cold-rolled steel sheet being carried out decarburizing annealing.Remove the carbon in the steel plate through decarburizing annealing, produce primary recrystallization.If the temperature of decarburizing annealing is lower than 800 ℃, the crystal grain that then obtains through primary recrystallization (primary recrystallization crystal grain) is too small, can not fully show secondary recrystallization thereafter.On the other hand, if the temperature of decarburizing annealing surpasses 950 ℃, then primary recrystallization crystal grain is excessive, can not fully show secondary recrystallization thereafter.
Then, through the decarburizing annealing steel plate being carried out nitriding treatment, obtain nitriding treatment steel plate (step S7) 700 ℃～850 ℃ contain in the atmosphere of gas that hydrogen, nitrogen and ammonia etc. have the nitrogenize ability.Through nitriding treatment, the nitrogen content in the steel plate increases.If the temperature of nitriding treatment is lower than 700 ℃ or surpass 850 ℃, then nitrogen is difficult to be diffused into the inside of steel plate, can not fully show secondary recrystallization thereafter.
Then, on the surface of nitriding treatment steel plate, being coated with MgO with the water slurry shape is the annealing separation agent of principal constituent, and the nitriding treatment coiler plate is become the coiled material shape.Then, carry out step final annealing, obtain the final annealing steel plate (step S8) of coiled material shape through decarburization nitrogenize steel plate to the coiled material shape.Through final annealing, produce secondary recrystallization.
Then, carry out the uncoiling of final annealing steel plate and the removing of annealing separation agent of coiled material shape.Then, coating is the lining liquid of principal constituent with phosphagel phosphaljel and colloid silica on the surface of final annealing steel plate, forms insulation tunicle (step S9) through baking.
Can make grain-oriented magnetic steel sheet thus.
In addition, the steel as the hot rolling object is not limited to also can use so-called thin slab through casting the slab that molten steel obtains.In addition, when using thin slab, also may not carry out the slab heating below 1250 ℃.
Embodiment
Below, the experiment that present inventors are carried out describes.Condition in these experiments etc. is the example that adopts in order to confirm exploitativeness of the present invention and effect, and the present invention is not limited to these examples.
(the 1st experiment)
At first, use vacuum melting furnace to make to contain Si:3.2 quality %, C:0.055 quality %, Mn:0.10 quality %, acid-solubility Al:0.028 quality %, N:0.003 quality %, S:0.0060 quality % and P:0.030 quality % and further contain Ti and the Cu of amount shown in the table 1 and 15 kinds of steel ingots that remainder comprises Fe and unavoidable impurities.Then, under 1150 ℃, steel ingot carried out 1 hour annealing, carry out hot rolling then, obtain the hot-rolled steel sheet that thickness is 2.3mm.
Then, under 1100 ℃, hot-rolled steel sheet carried out the annealing in 120 seconds, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then annealed sheet steel is carried out cold rollingly, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, under 860 ℃, containing in the gas atmosphere of water vapour, hydrogen and nitrogen cold-rolled steel sheet carried out the decarburizing annealing in 100 seconds, obtain the decarburizing annealing steel plate.Then, under 770 ℃, containing in the gas atmosphere of hydrogen, nitrogen and ammonia the nitriding treatment that the decarburizing annealing steel plate was carried out 20 seconds, obtain the nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate, being coated with MgO with the water slurry shape is the annealing separation agent of principal constituent.Then, under 1200 ℃, carry out 20 hours final annealing, obtain the final annealing steel plate.Then, the final annealing steel plate is washed, size is used in the veneer magnetic-measurement that cuts into wide 60mm, long 300mm then.Then, coating is the lining liquid of principal constituent with phosphagel phosphaljel and colloid silica on the surface of final annealing steel plate, forms the insulation tunicle through baking.Like this, obtain the sample of grain-oriented magnetic steel sheet.
Then, measure the magneticflux-density B8 of the tropism of each side electro-magnetic steel plate.Magneticflux-density B8 is the magneticflux-density that in grain-oriented magnetic steel sheet, produces when adding the magnetic field of 800A/m with 50Hz as stated.In addition, each sample is measured the magneticflux-density B8 of 5 mensuration with the veneer sample.Then, each sample is obtained MV " average B8 ", mxm. " B8max " and Schwellenwert " B8min ".Also obtain poor " the Δ B8 " of mxm. " B8max " and Schwellenwert " B8min " in addition.Difference " Δ B8 " is the index of the amplitude of fluctuation of expression magnetic properties.Their result and Ti content and Cu content are shown in the table 1 in the lump.In addition, shown in Fig. 1 based on the evaluation result of MV " average B8 " and poor " Δ B8 ".As stated, zero mark among Fig. 1 representes that MV " average B8 " is more than the 1.90T and poor " Δ B8 " is below the 0.030T.In addition, among Fig. 1 ● expression MV " average B8 " is lower than 1.90T or poor " Δ B8 " above 0.030T.
Table 1
Like table 1 and shown in Figure 1, among Ti content and Cu content sample No.2～No.4, No.6～No.9 and the No.11～No.15 within the scope of the present invention, MV " average B8 " arrives more than the 1.90T greatly, poor " Δ B8 " is little below 0.030T.That is to say, obtained high magnetic properties, and the deviation of magnetic properties is little.
Particularly; Ti content (quality %) is expressed as [Ti], when Cu content (quality %) is expressed as [Cu]; In sample No.11, No.13 and No.15 that the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up, the MV " average B8 " and the balance of poor " Δ B8 " are good.Wherein, in the sample No.15 that the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up, the MV " average B8 " and the balance of poor " Δ B8 " are very good.
On the other hand, Ti content is lower than 0.0020 quality % and Cu content is lower than among the sample No.1 of 0.010 quality %, and poor " Δ B8 " is greatly to surpassing 0.030T.That is to say that the deviation of magnetic properties is big.In addition, the sample No.5 and the Cu content that surpass 0.010 quality % at Ti content surpass among the sample No.10 of 0.50 quality %, contain precipitate in a large number, have influence on final annealing, and MV " average B8 " is little of being lower than 1.90T as a result.That is to say, do not obtain sufficiently high magnetic properties.
(the 2nd experiment)
At first, use vacuum melting furnace to make to contain Si:3.2 quality %, C:0.051 quality %, Mn:0.09 quality %, acid-solubility Al:0.026 quality %, N:0.004 quality %, S:0.0053 quality %, P:0.027 quality %, Ti:0.0024 quality % and Cu:0.029 quality % and remainder to comprise the steel ingot of Fe and unavoidable impurities.Then, under 1150 ℃, steel ingot carried out 1 hour annealing, carry out hot rolling then, obtain the hot-rolled steel sheet that thickness is 2.4mm.
Then, under 1090 ℃, hot-rolled steel sheet carried out the annealing in 120 seconds, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then annealed sheet steel is carried out cold rollingly, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, cut out the steel plate of 8 annealing usefulness, in the temperature T 1 time of 790 ℃ shown in the table 2～960 ℃, containing in the gas atmosphere of water vapour, hydrogen and nitrogen steel plate is carried out the decarburizing annealing in 80 seconds, obtain the decarburizing annealing steel plate from cold-rolled steel sheet.Then, in the temperature T 2 times of 680 ℃ shown in the table 2～880 ℃, containing in the gas atmosphere of water vapour, hydrogen, nitrogen and ammonia the nitriding treatment that the decarburizing annealing steel plate was carried out 20 seconds, obtain the nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate, being coated with MgO with the water slurry shape is the annealing separation agent of principal constituent.Then, under 1200 ℃, carry out 20 hours final annealing, obtain the final annealing steel plate.Then, likewise carry out obtaining the sample of grain-oriented magnetic steel sheet with the 1st experiment from washing to the processing that the tunicle that insulate forms.
Then, likewise each sample is obtained MV " average B8 ", mxm. " B8max ", Schwellenwert " B8min " and poor " Δ B8 " with the 1st experiment.Their result and temperature T 1 and temperature T 2 are shown in the table 2 in the lump.
Table 2
As shown in table 2, in the temperature T 2 sample No.22～No.24 and No.27 within the scope of the present invention of the temperature T 1 of decarburizing annealing and nitriding treatment, MV " average B8 " arrive more than the 1.90T greatly, poor " Δ B8 " is little below 0.030T.That is to say, obtained high magnetic properties, and the deviation of magnetic properties is little.
On the other hand, in the temperature T 1 of decarburizing annealing was lower than 800 ℃ sample No.21, " average B8 " was little of being lower than 1.90T for MV.Temperature T 1 in decarburizing annealing surpasses among 950 ℃ the sample No.25, and poor " Δ B8 " to surpassing 0.030T, " average B8 " is little of being lower than 1.90T for MV greatly.In addition, in the temperature T 2 of nitriding treatment was lower than 700 ℃ sample No.26, " average B8 " was little of being lower than 1.90T for MV.Temperature T 2 at nitriding treatment surpasses among 850 ℃ the sample No.28, and poor " Δ B8 " to surpassing 0.030T, " average B8 " is little of being lower than 1.90T for MV greatly.
(the 3rd experiment)
At first, use vacuum melting furnace to make to contain Si:3.2 quality %, Mn:0.09 quality %, acid-solubility Al:0.026 quality %, N:0.004 quality %, S:0.0053 quality % and P:0.027 quality % and further contain Ti and the Cu of amount shown in the table 3 and 20 kinds of steel ingots that remainder comprises Fe and unavoidable impurities.Then, under 1150 ℃, steel ingot carried out 1 hour annealing, carry out hot rolling then, obtain the hot-rolled steel sheet that thickness is 2.4mm.
Then, under 1090 ℃, hot-rolled steel sheet carried out the annealing in 120 seconds, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then annealed sheet steel is carried out cold rollingly, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, cut out the steel plate of annealing usefulness from cold-rolled steel sheet, under 860 ℃, containing in the gas atmosphere of water vapour, hydrogen and nitrogen steel plate carried out the decarburizing annealing in 80 seconds, obtain the decarburizing annealing steel plate.Then, under 760 ℃, containing in the gas atmosphere of water vapour, hydrogen, nitrogen and ammonia the nitriding treatment that the decarburizing annealing steel plate was carried out 20 seconds, obtain the nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate, being coated with MgO with the water slurry shape is the annealing separation agent of principal constituent.Then, under 1200 ℃, carry out 20 hours final annealing, obtain the final annealing steel plate.Then, likewise carry out obtaining the sample of grain-oriented magnetic steel sheet with the 1st experiment from washing to the processing that the tunicle that insulate forms.
Then, likewise each sample is obtained MV " average B8 ", mxm. " B8max ", Schwellenwert " B8min " and poor " Δ B8 " with the 1st experiment.Their result and C content, Ti content and Cu content are shown in the table 3 in the lump.
Table 3
As shown in table 3; In C content, Ti content and Cu content sample No.32～No.34, No.37～No.39, No.42～No.44 and No.47～No.49 within the scope of the present invention, MV " average B8 " arrives more than the 1.90T greatly, poor " Δ B8 " is little below 0.025T.That is to say, obtained high magnetic properties, and the deviation of magnetic properties is little.Particularly under the little situation of C content, obtained good result.
In addition; At Ti content is that 0.0020 quality % ~ 0.080 quality %, Cu content are among the relation of 0.010 quality % ~ 0.10 quality % and " 20 * [Ti]+[Cu]≤0.18 " the sample No.32, No.33, No.37, No.38, No.42, No.43, No.47 and the No.48 that set up; The MV " average B8 " and the balance of poor " Δ B8 " are good; Wherein, In sample No.32, No.42 and No.47 that the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up, the MV " average B8 " and the balance of poor " Δ B8 " are very good.
On the other hand, Ti content is lower than 0.010 quality % and Cu content is lower than among sample No.31, No.36, No.41 and the No.46 of 0.50 quality %, and poor " Δ B8 " is greatly to surpassing 0.030T.Wherein, in the low sample No.31 of C content, No.36, " average B8 " is also little of being lower than 1.09T for MV.In addition, surpass 0.010 quality %, Cu content above among sample No.35, No.40, No.45 and the No.50 of 0.50 quality % at Ti content, " average B8 " is little of being lower than 1.90T for MV.
(the 4th experiment)
At first, use vacuum melting furnace to make to contain Si:3.2 quality %, C:0.048 quality %, Mn:0.08 quality %, acid-solubility Al:0.028 quality %, N:0.004 quality %, S:0.0061 quality %, P:0.033 quality %, Ti:0.0024 quality % and Cu:0.029 quality % and further contain Cr and the Sn of amount shown in the table 4 and 10 kinds of steel ingots that remainder comprises Fe and unavoidable impurities.Then, under 1100 ℃, steel ingot carried out 1 hour annealing, carry out hot rolling then, obtain the hot-rolled steel sheet that thickness is 2.3mm.
Then, under 1080 ℃, hot-rolled steel sheet carried out the annealing in 120 seconds, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then annealed sheet steel is carried out cold rollingly, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, under 870 ℃, containing in the gas atmosphere of water vapour, hydrogen and nitrogen cold-rolled steel sheet carried out the decarburizing annealing in 90 seconds, obtain the decarburizing annealing steel plate.Then, under 760 ℃, containing in the gas atmosphere of hydrogen, nitrogen and ammonia the nitriding treatment that the decarburizing annealing steel plate was carried out 20 seconds, obtain the nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate, being coated with MgO with the water slurry shape is the annealing separation agent of principal constituent.Then, under 1200 ℃, carry out 20 hours final annealing, obtain the final annealing steel plate.Then, likewise carry out obtaining the sample of grain-oriented magnetic steel sheet with the 1st experiment from washing to the processing that the tunicle that insulate forms.
Then, likewise each sample is obtained MV " average B8 ", mxm. " B8max ", Schwellenwert " B8min " and poor " Δ B8 " with the 1st experiment.Their result and Cr content and Sn content are shown in the table 4 in the lump.
Table 4
As shown in table 4, no matter in which of sample No.51～60, MV " average B8 " all arrive more than the 1.90T greatly, poor " Δ B8 " is all little below 0.030T.That is to say, obtained high magnetic properties, and the deviation of magnetic properties is little.Wherein, In the sample No.52 of the Sn of the Cr that contains 0.010 quality %～0.20 quality % and/or 0.010 quality %～0.20 quality %, No.53, No.55, No.56, No.58～No.60, MV " average B8 " arrive more than the 1.91T especially greatly, poor " Δ B8 " is especially little below 0.025T.
Utilize possibility on the industry
The present invention for example can be used for electro-magnetic steel plate manufacturing industry and electro-magnetic steel plate application industry.
Claims (12)
1. the method for manufacture of a grain-oriented magnetic steel sheet is characterized in that, has following operation:
Steel is carried out hot rolling and obtain the operation of hot-rolled steel sheet; Said steel contains Si:2.5 quality %～4.0 quality %, C:0.01 quality %～0.060 quality %, Mn:0.05 quality %～0.20 quality %, acid-solubility Al:0.020 quality %～0.040 quality %, N:0.002 quality %～0.012 quality %, S:0.001 quality %～0.010 quality % and P:0.01 quality %～0.08 quality %; And further contain at least a kind that is selected among Ti:0.0020 quality %～0.010 quality % and the Cu:0.010 quality %～0.50 quality %, and remainder comprises Fe and unavoidable impurities;
Said hot-rolled steel sheet is annealed and obtain the operation of annealed sheet steel;
Carry out cold rolling to said annealed sheet steel and obtain the operation of cold-rolled steel sheet;
Under 800 ℃～950 ℃ temperature, said cold-rolled steel sheet carried out decarburizing annealing and obtain the operation of decarburizing annealing steel plate;
Then under 700 ℃～850 ℃ temperature, said decarburizing annealing steel plate carried out nitriding treatment and obtain the operation of nitriding treatment steel plate; And
Said nitriding treatment steel plate is carried out the operation of final annealing.
2. the method for manufacture of grain-oriented magnetic steel sheet according to claim 1 is characterized in that, said steel is carried out hot rolling is after said steel is heated to the temperature below 1250 ℃, to carry out.
3. the method for manufacture of grain-oriented magnetic steel sheet according to claim 1; It is characterized in that said steel also further contains and is selected from least a among Cr:0.010 quality %～0.20 quality %, Sn:0.010 quality %～0.20 quality %, Sb:0.010 quality %～0.20 quality %, Ni:0.010 quality %～0.20 quality %, Se:0.005 quality %～0.02 quality %, Bi:0.005 quality %～0.02 quality %, Pb:0.005 quality %～0.02 quality %, B:0.005 quality %～0.02 quality %, V:0.005 quality %～0.02 quality %, Mo:0.005 quality %～0.02 quality % and the As:0.005 quality %～0.02 quality %.
4. the method for manufacture of grain-oriented magnetic steel sheet according to claim 2; It is characterized in that said steel also further contains and is selected from least a among Cr:0.010 quality %～0.20 quality %, Sn:0.010 quality %～0.20 quality %, Sb:0.010 quality %～0.20 quality %, Ni:0.010 quality %～0.20 quality %, Se:0.005 quality %～0.02 quality %, Bi:0.005 quality %～0.02 quality %, Pb:0.005 quality %～0.02 quality %, B:0.005 quality %～0.02 quality %, V:0.005 quality %～0.02 quality %, Mo:0.005 quality %～0.02 quality % and the As:0.005 quality %～0.02 quality %.
5. the method for manufacture of grain-oriented magnetic steel sheet according to claim 1 is characterized in that,
The Ti content of said steel is 0.0020 quality %～0.0080 quality %;
The Cu content of said steel is 0.01 quality %～0.10 quality %;
Be expressed as [Ti] at Ti content (quality %) with said steel, when the Cu content (quality %) of said steel is expressed as [Cu], the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up.
6. the method for manufacture of grain-oriented magnetic steel sheet according to claim 2 is characterized in that,
The Ti content of said steel is 0.0020 quality %～0.0080 quality %;
The Cu content of said steel is 0.01 quality %～0.10 quality %;
Be expressed as [Ti] at Ti content (quality %) with said steel, when the Cu content (quality %) of said steel is expressed as [Cu], the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up.
7. the method for manufacture of grain-oriented magnetic steel sheet according to claim 3 is characterized in that,
The Ti content of said steel is 0.0020 quality %～0.0080 quality %;
The Cu content of said steel is 0.01 quality %～0.10 quality %;
Be expressed as [Ti] at Ti content (quality %) with said steel, when the Cu content (quality %) of said steel is expressed as [Cu], the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up.
8. the method for manufacture of grain-oriented magnetic steel sheet according to claim 4 is characterized in that,
The Ti content of said steel is 0.0020 quality %～0.0080 quality %;
The Cu content of said steel is 0.01 quality %～0.10 quality %;
Be expressed as [Ti] at Ti content (quality %) with said steel, when the Cu content (quality %) of said steel is expressed as [Cu], the relation of " 20 * [Ti]+[Cu]≤0.18 " is set up.
9. the method for manufacture of grain-oriented magnetic steel sheet according to claim 5 is characterized in that, the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up.
10. the method for manufacture of grain-oriented magnetic steel sheet according to claim 6 is characterized in that, the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up.
11. the method for manufacture of grain-oriented magnetic steel sheet according to claim 7 is characterized in that, the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up.
12. the method for manufacture of grain-oriented magnetic steel sheet according to claim 8 is characterized in that, the relation of " 10 * [Ti]+[Cu]≤0.07 " is set up.
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- 2011-02-18 JP JP2011523633A patent/JP4943559B2/en active Active
- 2011-02-18 US US13/579,684 patent/US20120312423A1/en not_active Abandoned
- 2011-02-18 BR BR112012020741-5A patent/BR112012020741B1/en active IP Right Grant
- 2011-02-18 KR KR1020127024187A patent/KR20120118504A/en active Application Filing
- 2011-02-18 KR KR1020137026864A patent/KR101389248B1/en active IP Right Grant
- 2011-02-18 CN CN201180009920.4A patent/CN102762752B/en active Active
- 2011-02-18 PL PL11744742T patent/PL2537947T3/en unknown
- 2011-02-18 WO PCT/JP2011/053491 patent/WO2011102456A1/en active Application Filing
- 2011-02-18 EP EP11744742.5A patent/EP2537947B1/en active Active
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| JPH01301820A (en) * | 1988-02-03 | 1989-12-06 | Nippon Steel Corp | Production of grain oriented silicon steel sheet having high magnetic flux density |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103741031A (en) * | 2013-12-27 | 2014-04-23 | 钢铁研究总院 | Thin slab casting and rolling process-based vanadium-containing ordinary oriented silicon steel and manufacturing method thereof |
| CN103741031B (en) * | 2013-12-27 | 2016-01-20 | 钢铁研究总院 | CSP is containing vanadium common orientation silicon steel and manufacture method thereof |
| CN108026622A (en) * | 2015-09-28 | 2018-05-11 | 新日铁住金株式会社 | The hot rolled steel plate of grain-oriented magnetic steel sheet and grain-oriented magnetic steel sheet |
| CN108026622B (en) * | 2015-09-28 | 2020-06-23 | 日本制铁株式会社 | Grain-oriented electrical steel sheet and hot-rolled steel sheet for grain-oriented electrical steel sheet |
| CN111566250A (en) * | 2017-12-26 | 2020-08-21 | Posco公司 | Oriented electrical steel sheet and method for manufacturing the same |
| CN111566250B (en) * | 2017-12-26 | 2021-12-17 | Posco公司 | Oriented electrical steel sheet and method for manufacturing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2011102456A1 (en) | 2011-08-25 |
| CN102762752B (en) | 2016-04-13 |
| EP2537947A1 (en) | 2012-12-26 |
| PL2537947T3 (en) | 2019-05-31 |
| KR101389248B1 (en) | 2014-04-24 |
| JPWO2011102456A1 (en) | 2013-06-17 |
| KR20120118504A (en) | 2012-10-26 |
| EP2537947A4 (en) | 2017-07-26 |
| US20120312423A1 (en) | 2012-12-13 |
| JP4943559B2 (en) | 2012-05-30 |
| BR112012020741B1 (en) | 2022-07-19 |
| KR20130119516A (en) | 2013-10-31 |
| BR112012020741A2 (en) | 2016-08-23 |
| EP2537947B1 (en) | 2018-12-19 |
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