CN102762752B - The manufacture method of grain-oriented magnetic steel sheet - Google Patents
The manufacture method of grain-oriented magnetic steel sheet Download PDFInfo
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- C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
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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
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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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- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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- 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
The present invention relates to the manufacture method of grain-oriented magnetic steel sheet, wherein hot rolling carried out to the steel of the composition requirement containing Ti:0.0020 quality % ~ 0.010 quality % and/or Cu:0.010 quality % ~ 0.50 quality % and obtain hot-rolled steel sheet.Described hot-rolled steel sheet is annealed and obtains annealed sheet steel.Carry out cold rolling to described annealed sheet steel and obtain cold-rolled steel sheet.At the temperature of 800 DEG C ~ 950 DEG C, decarburizing annealing carried out to described cold-rolled steel sheet and obtain decarburization annealed steel sheet.Then at 700 DEG C ~ 850 DEG C, nitriding treatment carried out to described decarburization annealed steel sheet and obtain nitriding treatment steel plate.Final annealing is carried out to described nitriding treatment steel plate.
Description
Technical field
The present invention relates to the manufacture method achieving the grain-oriented magnetic steel sheet that the deviation (i.e. scattered error, fluctuation) to magnetic properties suppresses.
Background technology
Grain-oriented magnetic steel sheet is that the azimuth elevation containing Si, crystal grain is gathered in that { steel plate in 110} < 001 > orientation, it is used as the material of the Wound core of the static transformers such as transformer etc.The control of grain arrangement utilizes the exaggerated grain growth phenomenon being called as secondary recrystallization to carry out.
As the method controlling secondary recrystallization, following two kinds of methods can be listed.A method is, heats and the nano-precipitation roughly completely after solid solution that makes to be called as inhibitor at the temperature more than 1280 DEG C to steel billet, carries out hot rolling, cold rolling and annealing etc., when hot rolling and annealing, nano-precipitation is separated out.Another method is, at lower than the temperature of 1280 DEG C by heating steel billet after, carry out hot rolling, cold rolling, decarburizing annealing, nitriding treatment and final annealing etc., make the precipitation such as AlN, (Al, Si) N as inhibitor when nitriding treatment.
, from reduction CO in recent years
2the viewpoint of discharge is set out, and requires the time that the decarburizing annealing in the manufacturing processed of shortening grain-oriented magnetic steel sheet is used.Therefore, to using the low slab of C content to be studied.
But along with the reduction of the C content of slab, after the final annealing carried out with the state being wound into coiled material shape, the deviation (magnetic properties deviation) of the magnetic properties of different sites becomes remarkable.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 3-122227 publication
Patent documentation 2: Japanese Unexamined Patent Publication 11-323437 publication
Patent documentation 3: Japanese Unexamined Patent Publication 6-256847 publication
Patent documentation 4: Japanese Unexamined Patent Application Publication 2001-515540 publication
Patent documentation 5: Japanese Unexamined Patent Publication 2000-199015 publication
Patent documentation 6: Japanese Unexamined Patent Publication 2007-254829 publication
Summary of the invention
The problem that invention will solve
The object of this invention is to provide a kind of manufacture method that can suppress the grain-oriented magnetic steel sheet of magnetic properties deviation.
For solving the means of problem
Understood the magnetic properties deviation after above-mentioned such final annealing C content be below 0.06 quality % so that be below 0.048 quality % time remarkable especially.The reason producing the magnetic properties deviation after final annealing is not also determined, even if but can think because before final annealing equably visible crystal grain time, in final annealing, crystal grain also can not grow equably sometimes.In addition, can not the reason of homoepitaxial as crystal grain, can think, because C content is low, thus do not carry out the phase transformation in hot rolling fully, thus austenite phase transformation amount to be little, hot rolling microstructure becomes unstable.That is, can think and not produce enough secondary recrystallizations in the part that hot rolling microstructure is uneven, thus not obtain good magnetic properties.
The present inventors consider based on experience so, in order to make the grain growing homogenizing in final annealing, whether produce secondary recrystallization fully by forming effective precipitate.Thus, the present inventors test repeatedly with regard to the mensuration of the magnetic properties by adding the grain-oriented magnetic steel sheet that various element obtains in slab.As a result, the present inventors find: for making secondary recrystallization homogenizing, and it is effective for adding Ti and Cu.
The present invention completes based on above-mentioned experience, and its main idea is as follows.
(1) manufacture method for grain-oriented magnetic steel sheet, is characterized in that, has following operation:
Hot rolling is carried out to steel and obtains the operation of hot-rolled steel sheet, described 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 containing at least a kind that is selected from Ti:0.0020 quality % ~ 0.010 quality % and Cu:0.010 quality % ~ 0.50 quality %, and remainder comprises Fe and inevitable impurity,
Described hot-rolled steel sheet is annealed and obtains the operation of annealed sheet steel;
Carry out cold rolling to described annealed sheet steel and obtain the operation of cold-rolled steel sheet;
At the temperature of 800 DEG C ~ 950 DEG C, decarburizing annealing carried out to described cold-rolled steel sheet and obtain the operation of decarburization annealed steel sheet;
Then at 700 DEG C ~ 850 DEG C, nitriding treatment carried out to described decarburization annealed steel sheet and obtain the operation of nitriding treatment steel plate; And
Described nitriding treatment steel plate is carried out to the operation of final annealing.
(2) manufacture method of the grain-oriented magnetic steel sheet according to above-mentioned (1), is characterized in that, described to carry out hot rolling to steel be carry out after described steel being heated to the temperature of less than 1250 DEG C.
(3) manufacture method of the grain-oriented magnetic steel sheet according to above-mentioned (1) or (2), it is characterized in that, described steel is further containing being selected from 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 %, at least one in Mo:0.005 quality % ~ 0.02 quality % and As:0.005 quality % ~ 0.02 quality %.
(4) manufacture method of the grain-oriented magnetic steel sheet according to any one of above-mentioned (1) ~ (3), is characterized in that, the Ti content of described steel is 0.0020 quality % ~ 0.0080 quality %; The Cu content of described steel is 0.01 quality % ~ 0.10 quality %; When the Ti content (quality %) of described steel being expressed as [Ti], the Cu content (quality %) of described steel being expressed as [Cu], the relation of " 20 × [Ti]+[Cu]≤0.18 " is set up.
(5) manufacture method of the grain-oriented magnetic steel sheet according to above-mentioned (4), is characterized in that, the relation of " 10 × [Ti]+[Cu]≤0.07 " is set up.
Invention effect
According to the present invention, due to Ti and/or Cu containing appropriate amount in steel, and carry out decarburizing annealing and nitriding treatment at a proper temperature, therefore, it is possible to suppress magnetic properties deviation.
Accompanying drawing explanation
Fig. 1 is the figure of the relation of the evaluation representing Ti content and Cu content and magneticflux-density and deviation thereof.
Fig. 2 is the schema of the manufacture method of the grain-oriented magnetic steel sheet representing embodiments of the present invention.
Embodiment
As mentioned above, the present inventors test repeatedly with regard to the mensuration of the magnetic properties by adding the grain-oriented magnetic steel sheet that various element obtains in slab, found that: for making secondary recrystallization homogenizing, and it is effective for adding Ti and Cu.
In this experiment, such as use utilizes C content in composition used in the manufacture of the grain-oriented magnetic steel sheet of low temperature slab heating method to be the silicon steel of below 0.06 quality %.Then, in all proportions containing Ti and Cu in this silicon steel, the steel ingot of various composition is made.Further, at the temperature below 1250 DEG C, heating is carried out to carry out hot rolling to steel ingot, carry out cold rolling afterwards.And then, after cold rolling, carry out decarburizing annealing, then carry out nitriding treatment and final annealing.Then, measure the magneticflux-density B8 of the grain-oriented magnetic steel sheet obtained, the deviation of the magneticflux-density B8 in the coiled material after investigation final annealing.Magneticflux-density B8 is with the magneticflux-density produced in grain-oriented magnetic steel sheet during the magnetic field of the additional 800A/m of 50Hz.
It found that: when Cu containing the Ti of 0.0020 quality % ~ 0.010 quality % and/or 0.010 quality % ~ 0.50 quality % in steel ingot, the deviation of the magneticflux-density B8 in the coiled material after final annealing significantly reduces.
An example of the result obtained by above-mentioned experiment shown in Fig. 1.Although the details of experiment can after be described, the mean value of the magneticflux-density B8 of zero mark expression 5 pieces of veneer samples in Fig. 1 is more than 1.90T and the difference of the maximum value of magneticflux-density B8 and Schwellenwert is below 0.030T.In addition, in Fig. 1 ● represent the mean value of the magneticflux-density B8 of at least 5 pieces of veneer samples lower than the maximum value of 1.90T or magneticflux-density B8 and the difference of Schwellenwert more than 0.030T.Shown by Fig. 1, during Cu containing the Ti of 0.0020 quality % ~ 0.010 quality % and/or 0.010 quality % ~ 0.50 quality % in steel ingot, the mean value of magneticflux-density B8 is high, and the deviation of magneticflux-density B8 is little.
Then, the manufacture method of the grain-oriented magnetic steel sheet of embodiments of the present invention is described.Fig. 2 is the schema of the manufacture method of the grain-oriented magnetic steel sheet representing embodiments of the present invention.
In the present embodiment, first, carry out the casting of the molten steel of the grain-oriented magnetic steel sheet of composition requirement, make slab (step S1).Castmethod is not particularly limited.Molten steel is such as containing 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 is further containing at least a kind that is selected from Ti:0.0020 quality % ~ 0.010 quality % and Cu:0.010 quality % ~ 0.50 quality %.That is, molten steel contains one or both of Ti and Cu with the scope of below Ti:0.010 quality % and Cu:0.50 below quality %, the mode that at least meets a side of more than Ti:0.0020 quality % or Cu:0.010 more than quality %.The remainder of molten steel comprises Fe and inevitable impurity.In addition, as inevitable impurity, be also included within the manufacturing process of grain-oriented magnetic steel sheet and form inhibitor, the element remained in after utilizing the purifying of high temperature annealing in grain-oriented magnetic steel sheet.
Here, the numerical definiteness reason of the composition of above-mentioned molten steel is described.
Si is very effective element for the eddy current losses of the resistance of raising grain-oriented magnetic steel sheet, a part for reduction formation iron loss.If Si content is lower than 2.5 quality %, then fully can not suppress eddy current losses.On the other hand, if Si content is more than 4.0 quality %, then processibility reduces.Therefore, Si content is defined as 2.5 quality % ~ 4.0 quality %.
C is effective element for the tissue (primary recrystallization tissue) controlling to be obtained by 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 is more than 0.06 quality %, then the time lengthening needed for decarburizing annealing, CO
2quantity discharged increase.In addition, if decarburizing annealing is insufficient, then the grain-oriented magnetic steel sheet obtaining having excellent magnetic characteristics is difficult to.Therefore, C content is defined as 0.01 quality % ~ 0.06 quality %.In addition, as mentioned above, in the prior art, when C content is below 0.048 quality %, the magnetic properties deviation after final annealing can be remarkable especially, and therefore present embodiment is effective especially when C content is below 0.048 quality %.
Mn improves the ratio resistance of grain-oriented magnetic steel sheet and reduces iron loss.Mn also has the effect preventing 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 is more than 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 forming the AlN played a role as inhibitor.If the content of acid-solubility Al is lower than 0.020 quality %, then can not form the AlN of q.s, thus inhibitor undercapacity.On the other hand, if the content of acid-solubility Al is more than 0.040 quality %, then AlN coarsening, thus inhibitor strength degradation.Therefore, the content of 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.As described later, owing to being carry out nitriding treatment after cold rolling, therefore not needing containing a large amount of N in steel for directional electromagnetic steel plate, but N content will be made lower than 0.002 quality %, during steel-making, sometimes need large load.On the other hand, if N content is more than 0.012 quality %, then can produce the emptying aperture being called as bubble in steel plate when cold rolling.Therefore, N content is defined as 0.002 quality % ~ 0.012 quality %.In order to reduce bubble further, preferred N content is below 0.010 quality %.
S reacts with Mn and forms the important element of MnS precipitate.MnS precipitate mainly has an impact to primary recrystallization, and to resulting from, the zonal variation of grain growing of hot rolling and the primary recrystallization brought 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 is more than 0.010 quality %, then magnetic properties easily declines.Therefore, Mn content is defined as 0.001 quality % ~ 0.010 quality %.In order to improve magnetic properties further, preferred Mn content is below 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 is more than 0.08 quality %, then sometimes cold rolling become difficulty.Therefore, P content is defined as 0.01 quality % ~ 0.08 quality %.
Ti and N reacts and forms TiN precipitate.In addition, Cu and S reacts and forms CuS precipitate.And the growth of the crystal grain that these precipitates have when making final annealing does not rely on coiled material position ground homogenizing thus suppresses the effect of the magnetic properties deviation of grain-oriented magnetic steel sheet.Particularly, can think that TiN precipitate can suppress the deviation of the grain growing of the high-temperature zone of final annealing, thus reduce the magnetic properties deviation of grain-oriented magnetic steel sheet.In addition, can think that CuS precipitate can suppress the deviation of the grain growing of the cold zone of decarburizing annealing or final annealing, thus reduce the magnetic properties deviation of grain-oriented magnetic steel sheet.If Ti content lower than 0.0020 quality % and Cu content lower than 0.010 quality %, then can not fully obtain these effects.On the other hand, if Ti content is more than 0.010 quality %, form TiN precipitate then superfluously, after the final anneal also can be remaining.Equally, if Cu content is more than 0.50 quality %, form CuS precipitate then superfluously, after the final anneal also can be remaining.And, if these precipitates remain in grain-oriented magnetic steel sheet, be then difficult to obtain high magnetic properties.Therefore, molten steel with the scope of below Ti:0.010 quality % and Cu:0.50 below quality %, to contain one or both of Ti and Cu in the mode of the side at least meeting more than Ti:0.0020 quality % or Cu:0.010 more than quality %.That is, molten steel contains at least one be selected from Ti:0.0020 quality % ~ 0.010 quality % and 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 %.Further, 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, when Ti content (quality %) being expressed as [Ti], Cu content (quality %) being expressed as [Cu], preferably the relation of " 20 × [Ti]+[Cu]≤0.18 " is set up, and more preferably the relation of " 10 × [Ti]+[Cu]≤0.07 " is set up.
In addition, also can containing at least one in following various element in molten steel.
The character of the zone of oxidation that Cr and Sn is formed when improving decarburizing annealing, the character of the glass epithelium using this zone of oxidation to be formed when also improving final annealing.That is, the stabilization that Cr and Sn is formed by zone of oxidation and glass epithelium and improve magnetic properties, thus suppress magnetic properties deviation.But, if Cr content is more than 0.20 quality %, then become unstable during being formed of glass epithelium.In addition, if Sn content is more than 0.20 quality %, then surface of steel plate is difficult to oxidized, insufficient during being formed of glass epithelium.Therefore, Cr content and Sn content are all preferably below 0.20 quality %.In addition, in order to fully obtain above-mentioned effect, Cr content and Sn content are all preferably more than 0.01 quality %.In addition, Sn is grain boundary segregation element, also has the effect making secondary recrystallization stabilization.
In addition, also 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 % can be contained in molten steel.These elements are all inhibitor strengthening elements.
In the present embodiment, after having made slab from the molten steel so formed, slab has been heated (step S2).The temperature of this heating, from the view point of energy-conservation, is preferably defined as less than 1250 DEG C.
Then, hot-rolled steel sheet (step S3) is obtained by carrying out hot rolling to slab.The thickness of hot-rolled steel sheet is not particularly limited, such as, be defined as 1.8mm ~ 3.5mm.
Then, annealed sheet steel (step S4) is obtained by annealing to hot-rolled steel sheet.Annealing condition be not particularly limited, such as carry out at the temperature of 750 DEG C ~ 1200 DEG C 30 second ~ 10 minutes.By this annealing, magnetic properties improves.
Then, cold-rolled steel sheet (step S5) is obtained by carrying out cold rolling to annealed sheet steel.Cold rollingly only 1 time can be carried out, also process annealing can be carried out betwixt while carry out repeatedly cold rolling.Process annealing such as preferred carry out at the temperature of 750 DEG C ~ 1200 DEG C 30 second ~ 10 minutes.
In addition, if carry out cold rolling when not carrying out above-mentioned process annealing, then be sometimes difficult to obtain uniform characteristic.In addition, if carry out process annealing betwixt while carry out repeatedly cold rolling, then easily obtain uniform characteristic, but magneticflux-density can reduce sometimes.Therefore, cold rolling number of times and the presence or absence of process annealing preferably decide according to the characteristic required by grain-oriented magnetic steel sheet finally obtained and cost.
In addition, in either case, all preferred finally cold rolling draft is defined as 80% ~ 95%.
After cold rolling, by carrying out decarburizing annealing 800 DEG C ~ 950 DEG C contain in the moistening atmosphere of hydrogen and nitrogen to cold-rolled steel sheet, obtain decarburization annealed steel sheet (step S6).By the carbon in decarburizing annealing removing steel plate, produce primary recrystallization.If the temperature of decarburizing annealing is lower than 800 DEG C, then the crystal grain (primary recrystallization crystal grain) obtained by primary recrystallization is too small, fully can not show secondary recrystallization thereafter.On the other hand, if the temperature of decarburizing annealing is more than 950 DEG C, then primary recrystallization crystal grain is excessive, fully can not show secondary recrystallization thereafter.
Then, by carrying out nitriding treatment 700 DEG C ~ 850 DEG C have in the atmosphere of the gas of nitrogenize ability containing hydrogen, nitrogen and ammonia etc. to decarburization annealed steel sheet, nitriding treatment steel plate (step S7) is obtained.By nitriding treatment, the nitrogen content in steel plate increases.If the temperature of nitriding treatment is lower than 700 DEG C or more than 850 DEG C, then nitrogen is difficult to the inside being diffused into steel plate, fully can not show secondary recrystallization thereafter.
Then, the surface of nitriding treatment steel plate is the annealing separation agent of principal constituent with MgO with the coating of water slurry shape, nitriding treatment coiler plate is become coiled material shape.Then, by carrying out step final annealing to the decarburization nitrogenize steel plate of coiled material shape, the final annealing steel plate (step S8) of coiled material shape is obtained.By final annealing, produce secondary recrystallization.
Then, the uncoiling of final annealing steel plate and the removing of annealing separation agent of coiled material shape is carried out.Then, the coating liquid that the surface of final annealing steel plate to be coated with aluminum phosphate and colloid silica be principal constituent, forms insulation tunicle (step S9) by baking.
Thus can manufacturer tropism's electro-magnetic steel plate.
In addition, the steel as hot rolling object is not limited to the slab obtained by casting molten steel, also can use so-called thin slab.In addition, when using thin slab, the heating of plate blank of less than 1250 DEG C may not also be carried out.
Embodiment
Below, the experiment that the present inventors carry out is described.Condition etc. in these experiments is that the present invention is not limited to these examples in order to confirm the example that exploitativeness of the present invention and effect adopt.
(the 1st experiment)
First, vacuum melting furnace is used to make containing 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 containing Ti and Cu of the amount of Table 1 and remainder comprises 15 kinds of steel ingots of Fe and inevitable impurity.Then, steel ingot is carried out to the annealing of 1 hour at 1150 DEG C, then carry out hot rolling, obtain the hot-rolled steel sheet that thickness is 2.3mm.
Then, hot-rolled steel sheet is carried out to the annealing in 120 seconds at 1100 DEG C, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then carry out cold rolling to annealed sheet steel, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, at 860 DEG C, cold-rolled steel sheet is carried out to the decarburizing annealing in 100 seconds in the gas atmosphere containing water vapour, hydrogen and nitrogen, obtain decarburization annealed steel sheet.Then, at 770 DEG C, decarburization annealed steel sheet is carried out to the nitriding treatment in 20 seconds in the gas atmosphere containing hydrogen, nitrogen and ammonia, obtain nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate with the annealing separation agent that the coating of water slurry shape take MgO as principal constituent.Then, at 1200 DEG C, carry out the final annealing of 20 hours, obtain final annealing steel plate.Then, final annealing steel plate is washed, then cut into the veneer magnetic-measurement size of wide 60mm, long 300mm.Then, the coating liquid that the surface of final annealing steel plate to be coated with aluminum phosphate and colloid silica be principal constituent, forms insulation tunicle by baking.Like this, the sample of grain-oriented magnetic steel sheet is obtained.
Then, the magneticflux-density B8 of each side tropism electro-magnetic steel plate is measured.Magneticflux-density B8 is described above, is with the magneticflux-density produced in grain-oriented magnetic steel sheet during the magnetic field of the additional 800A/m of 50Hz.In addition, to the magneticflux-density B8 of each Specimen Determination 5 pieces of mensuration veneer samples.Then, mean value " average B8 ", maximum " B8max " and Schwellenwert " B8min " are obtained to each sample.Also obtain the difference " Δ B8 " of maximum " B8max " and Schwellenwert " B8min " in addition.Difference " Δ B8 " is the index of the amplitude of fluctuation representing magnetic properties.Their result and Ti content and Cu content are shown in table 1 in the lump.In addition, shown in Fig. 1 based on the evaluation result of mean value " average B8 " and poor " Δ B8 ".As mentioned above, zero mark expression mean value " average B8 " in Fig. 1 is for more than 1.90T and poor " Δ B8 " is below 0.030T.In addition, in Fig. 1 ● represent mean value " average B8 " lower than 1.90T or poor " Δ B8 " more than 0.030T.
Table 1
As shown in table 1 and Fig. 1, in Ti content and Cu content sample No.2 ~ No.4, No.6 ~ No.9 and No.11 ~ No.15 within the scope of the present invention, mean value " average B8 " is greatly little of below 0.030T to more than 1.90T, poor " Δ B8 ".That is, obtain high magnetic properties, and the deviation of magnetic properties is little.
Particularly, when Ti content (quality %) being expressed as [Ti], Cu content (quality %) being 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 balance of mean value " average B8 " and poor " Δ B8 " is good.Wherein, in the sample No.15 that the relation of " 10 × [Ti]+[Cu]≤0.07 " is set up, the balance of mean value " average B8 " and poor " Δ B8 " is very good.
On the other hand, Ti content lower than 0.0020 quality % and Cu content lower than in the sample No.1 of 0.010 quality %, poor " Δ B8 " is greatly to more than 0.030T.That is, the deviation of magnetic properties is large.In addition, at Ti content more than the sample No.5 of 0.010 quality % and Cu content more than in the sample No.10 of 0.50 quality %, in a large number containing precipitate, have influence on final annealing, result mean value " average B8 " is little of lower than 1.90T.That is, sufficiently high magnetic properties is not obtained.
(the 2nd experiment)
First, vacuum melting furnace is used to make the steel ingot comprising Fe and inevitable impurity containing 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.Then, steel ingot is carried out to the annealing of 1 hour at 1150 DEG C, then carry out hot rolling, obtain the hot-rolled steel sheet that thickness is 2.4mm.
Then, hot-rolled steel sheet is carried out to the annealing in 120 seconds at 1090 DEG C, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then carry out cold rolling to annealed sheet steel, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, cut out the steel plates of 8 pieces of annealing from cold-rolled steel sheet, under the temperature T1 of 790 DEG C shown in table 2 ~ 960 DEG C, steel plate is carried out to the decarburizing annealing in 80 seconds in the gas atmosphere containing water vapour, hydrogen and nitrogen, obtain decarburization annealed steel sheet.Then, under the temperature T2 of 680 DEG C shown in table 2 ~ 880 DEG C, decarburization annealed steel sheet is carried out to the nitriding treatment in 20 seconds in the gas atmosphere containing water vapour, hydrogen, nitrogen and ammonia, obtain nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate with the annealing separation agent that the coating of water slurry shape take MgO as principal constituent.Then, at 1200 DEG C, carry out the final annealing of 20 hours, obtain final annealing steel plate.Then, carry out, from the process of washing to the tunicle that insulate and being formed, obtaining the sample of grain-oriented magnetic steel sheet in the same manner as the 1st tests.
Then, in the same manner as the 1st tests, mean value " average B8 ", maximum " B8max ", Schwellenwert " B8min " and poor " Δ B8 " are obtained to each sample.Their result and temperature T1 and temperature T2 are shown in table 2 in the lump.
Table 2
As shown in table 2, in the temperature T2 sample No.22 ~ No.24 within the scope of the present invention and No.27 of the temperature T1 of decarburizing annealing and nitriding treatment, mean value " average B8 " is little of below 0.030T to more than 1.90T, poor " Δ B8 " greatly.That is, obtain high magnetic properties, and the deviation of magnetic properties is little.
On the other hand, at the temperature T1 of decarburizing annealing lower than in the sample No.21 of 800 DEG C, mean value " average B8 " is little of lower than 1.90T.In sample No.25 more than 950 DEG C of the temperature T1 of decarburizing annealing, poor " Δ B8 ", greatly to more than 0.030T, mean value " average B8 " is little of lower than 1.90T.In addition, at the temperature T2 of nitriding treatment lower than in the sample No.26 of 700 DEG C, mean value " average B8 " is little of lower than 1.90T.In sample No.28 more than 850 DEG C of the temperature T2 of nitriding treatment, poor " Δ B8 ", greatly to more than 0.030T, mean value " average B8 " is little of lower than 1.90T.
(the 3rd experiment)
First, vacuum melting furnace is used to make containing 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 containing Ti and Cu of the amount of Table 3 and remainder comprises 20 kinds of steel ingots of Fe and inevitable impurity.Then, steel ingot is carried out to the annealing of 1 hour at 1150 DEG C, then carry out hot rolling, obtain the hot-rolled steel sheet that thickness is 2.4mm.
Then, hot-rolled steel sheet is carried out to the annealing in 120 seconds at 1090 DEG C, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then carry out cold rolling to annealed sheet steel, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, cut out the steel plate of annealing from cold-rolled steel sheet, at 860 DEG C, steel plate is carried out to the decarburizing annealing in 80 seconds in the gas atmosphere containing water vapour, hydrogen and nitrogen, obtain decarburization annealed steel sheet.Then, at 760 DEG C, decarburization annealed steel sheet is carried out to the nitriding treatment in 20 seconds in the gas atmosphere containing water vapour, hydrogen, nitrogen and ammonia, obtain nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate with the annealing separation agent that the coating of water slurry shape take MgO as principal constituent.Then, at 1200 DEG C, carry out the final annealing of 20 hours, obtain final annealing steel plate.Then, carry out, from the process of washing to the tunicle that insulate and being formed, obtaining the sample of grain-oriented magnetic steel sheet in the same manner as the 1st tests.
Then, in the same manner as the 1st tests, mean value " average B8 ", maximum " B8max ", Schwellenwert " B8min " and poor " Δ B8 " are obtained to each sample.Their result and C content, Ti content and Cu content are shown in 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, mean value " average B8 " is little of below 0.025T to more than 1.90T, poor " Δ B8 " greatly.That is, obtain high magnetic properties, and the deviation of magnetic properties is little.Particularly when C content is little, obtain good result.
In addition, Ti content be 0.0020 quality % ~ 0.080 quality %, Cu content be 0.010 quality % ~ 0.10 quality % and the relation of " 20 × [Ti]+[Cu]≤0.18 " set up sample No.32, No.33, No.37, No.38, No.42, No.43, No.47 and No.48 in, the balance of mean value " average B8 " and poor " Δ B8 " is good, wherein, in sample No.32, No.42 and No.47 that the relation of " 10 × [Ti]+[Cu]≤0.07 " is set up, the balance of mean value " average B8 " and poor " Δ B8 " is very good.
On the other hand, Ti content lower than 0.0020 quality % and Cu content lower than in sample No.31, No.36, No.41 and No.46 of 0.010 quality %, poor " Δ B8 " is greatly to more than 0.030T.Wherein, in sample No.31, No.36 that C content is low, mean value " average B8 " is also little to be arrived lower than 1.09T.In addition, at Ti content more than 0.010 quality %, Cu content more than in sample No.35, No.40, No.45 and No.50 of 0.50 quality %, mean value " average B8 " is little of lower than 1.90T.
(the 4th experiment)
First, vacuum melting furnace is used to make containing 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 containing Cr and Sn of the amount of Table 4 and remainder comprises 10 kinds of steel ingots of Fe and inevitable impurity.Then, steel ingot is carried out to the annealing of 1 hour at 1100 DEG C, then carry out hot rolling, obtain the hot-rolled steel sheet that thickness is 2.3mm.
Then, hot-rolled steel sheet is carried out to the annealing in 120 seconds at 1080 DEG C, obtain annealed sheet steel.Then, carry out the pickling of annealed sheet steel, then carry out cold rolling to annealed sheet steel, obtain the cold-rolled steel sheet that thickness is 0.23mm.Then, at 870 DEG C, cold-rolled steel sheet is carried out to the decarburizing annealing in 90 seconds in the gas atmosphere containing water vapour, hydrogen and nitrogen, obtain decarburization annealed steel sheet.Then, at 760 DEG C, decarburization annealed steel sheet is carried out to the nitriding treatment in 20 seconds in the gas atmosphere containing hydrogen, nitrogen and ammonia, obtain nitriding treatment steel plate.
Then, on the surface of nitriding treatment steel plate with the annealing separation agent that the coating of water slurry shape take MgO as principal constituent.Then, at 1200 DEG C, carry out the final annealing of 20 hours, obtain final annealing steel plate.Then, carry out, from the process of washing to the tunicle that insulate and being formed, obtaining the sample of grain-oriented magnetic steel sheet in the same manner as the 1st tests.
Then, in the same manner as the 1st tests, mean value " average B8 ", maximum " B8max ", Schwellenwert " B8min " and poor " Δ B8 " are obtained to each sample.Their result and Cr content and Sn content are shown in table 4 in the lump.
Table 4
As shown in table 4, no matter sample No.51 ~ 60 which in, mean value " average B8 " is all large all little of below 0.030T to more than 1.90T, poor " Δ B8 ".That is, obtain high magnetic properties, and the deviation of magnetic properties is little.Wherein, containing in sample No.52, No.53, No.55, No.56, No.58 ~ No.60 of the Cr of 0.010 quality % ~ 0.20 quality % and/or the Sn of 0.010 quality % ~ 0.20 quality %, mean value " average B8 " is large especially little of below 0.025T especially to more than 1.91T, poor " Δ B8 ".
Industry utilizes possibility
The present invention such as can be used for electro-magnetic steel plate manufacturing industry and electro-magnetic steel plate application industry.
Claims (3)
1. a manufacture method for grain-oriented magnetic steel sheet, is characterized in that, has following operation:
Carry out hot rolling to steel and obtain the operation of hot-rolled steel sheet, described steel contains Si:2.5 quality % ~ 4.0 quality %, C:0.01 quality % ~ 0.057 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 containing Ti:0.0033 quality % ~ 0.010 quality % and Cu:0.010 quality % ~ 0.50 quality %, also further containing being selected from 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 %, at least one in Mo:0.005 quality % ~ 0.02 quality % and As:0.005 quality % ~ 0.02 quality %, and remainder is made up of Fe and inevitable impurity,
Described hot-rolled steel sheet is annealed and obtains the operation of annealed sheet steel;
Carry out cold rolling to described annealed sheet steel and obtain the operation of cold-rolled steel sheet;
At the temperature of 800 DEG C ~ 950 DEG C, decarburizing annealing carried out to described cold-rolled steel sheet and obtain the operation of decarburization annealed steel sheet;
Then at the temperature of 700 DEG C ~ 850 DEG C, nitriding treatment carried out to described decarburization annealed steel sheet and obtain the operation of nitriding treatment steel plate; And
The surface of described nitriding treatment steel plate is the annealing separation agent of principal constituent with MgO with the coating of water slurry shape, nitriding treatment coiler plate is become coiled material shape, then carries out the operation of step final annealing,
Wherein, when the Ti content (quality %) of described steel being expressed as [Ti], the Cu content (quality %) of described steel being expressed as [Cu], the relation of " 10 × [Ti]+[Cu]≤0.07 " is set up,
It is described that to carry out hot rolling to steel be carry out after described steel being heated to the temperature of less than 1150 DEG C.
2. the manufacture method of grain-oriented magnetic steel sheet according to claim 1, is characterized in that, the Ti content of described steel is 0.0033 quality % ~ 0.0080 quality %;
The Cu content of described steel is 0.01 quality % ~ 0.10 quality %.
3. the manufacture method of grain-oriented magnetic steel sheet according to claim 1, is characterized in that, the C content of described steel is 0.01 quality % ~ 0.048 quality %.
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| 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 |
| WO2016035345A1 (en) | 2014-09-04 | 2016-03-10 | Ｊｆｅスチール株式会社 | Method for manufacturing directional magnetic steel sheet, and nitriding treatment equipment |
| PL3358031T3 (en) * | 2015-09-28 | 2020-12-28 | Nippon Steel Corporation | Grain-oriented electrical steel sheet and hot-rolled steel sheet for grain-oriented electrical steel sheet |
| KR101676630B1 (en) * | 2015-11-10 | 2016-11-16 | 주식회사 포스코 | Oriented electrical steel sheet and method for manufacturing the same |
| EP3653754A4 (en) * | 2017-07-13 | 2020-11-11 | Nippon Steel Corporation | Oriented electromagnetic steel plate |
| JP6954351B2 (en) * | 2017-07-13 | 2021-10-27 | 日本製鉄株式会社 | Directional electrical steel sheet |
| JP6946847B2 (en) * | 2017-08-17 | 2021-10-13 | 日本製鉄株式会社 | Manufacturing method of grain-oriented electrical steel sheet |
| JP6946846B2 (en) * | 2017-08-17 | 2021-10-13 | 日本製鉄株式会社 | Manufacturing method of grain-oriented electrical steel sheet |
| KR102099866B1 (en) * | 2017-12-26 | 2020-04-10 | 주식회사 포스코 | Grain oriented electrical steel sheet method for manufacturing the same |
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