CN108474077B - Oriented electrical steel sheet and method for manufacturing the same - Google Patents

Oriented electrical steel sheet and method for manufacturing the same Download PDF

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CN108474077B
CN108474077B CN201680076266.1A CN201680076266A CN108474077B CN 108474077 B CN108474077 B CN 108474077B CN 201680076266 A CN201680076266 A CN 201680076266A CN 108474077 B CN108474077 B CN 108474077B
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annealing
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hot
steel sheet
electrical steel
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CN108474077A (en
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高炫昔
徐进旭
李相雨
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Posco Holdings Inc
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Posco Co Ltd
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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
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    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/54—Furnaces for treating strips or wire
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
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    • C21D2201/05—Grain orientation
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    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/008—Heat treatment of ferrous alloys containing Si
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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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    • 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
    • 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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    • 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
    • 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
    • C21D8/1266—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 between cold rolling steps
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    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic

Abstract

The grain-oriented electrical steel sheet according to an embodiment of the present invention includes, in wt%: 1.0 to 4.0%, C: 0.002% or less (0% excluded) and Bi: 0.001 to 0.1%, the balance comprising Fe and other unavoidable impurities.

Description

Oriented electrical steel sheet and method for manufacturing the same
Technical Field
The present invention relates to a grain-oriented electrical steel sheet and a method for manufacturing the same.
Background
The oriented electrical steel sheet is a soft magnetic material which is formed of grains oriented in a gaussian (Goss) orientation, which is also called a {110} <001> crystal orientation of the steel sheet, and has excellent magnetic properties in a rolling direction.
Such a grain-oriented electrical steel sheet is manufactured as follows: after heating the slab, it is usually rolled to a final thickness of 0.15 to 0.35mm by hot rolling, hot-rolled sheet annealing, cold rolling, and then subjected to high-temperature annealing for forming primary recrystallization annealing and secondary recrystallization.
In this case, it is known that the lower the temperature rise rate in the high-temperature annealing, the higher the aggregation degree of the secondary recrystallized gaussian orientation and the more excellent the magnetic properties. In general, in high-temperature annealing of grain-oriented electrical steel sheets, the temperature rise rate is 15 ℃ or less per hour, and it takes 2 to 3 days only for temperature rise and purification annealing for 40 hours or more is required, so that it can be said that the process consumes a lot of energy. In addition, since the conventional final high-temperature annealing process performs annealing in a Batch (Batch) form in a coil state, the following difficulties in the process occur. First, temperature deviation between the outer wrap portion and the inner wrap portion of the coil occurs due to heat treatment in the coil state, and the same heat treatment method cannot be applied to each portion, and magnetic deviation between the outer wrap portion and the inner wrap portion occurs. Second, in the process of coating MgO on the surface after decarburization annealing and forming an undercoat layer (Basecoating) in high temperature annealing, various surface defects occur, and thus the yield is lowered. Third, since the decarburization plate after the decarburization annealing is wound into a roll form, insulation coating is performed by performing planarization annealing again after high-temperature annealing, the production process is divided into three steps, and thus there is a problem that the yield is low.
Disclosure of Invention
Problems to be solved
An embodiment of the present invention provides a grain-oriented electrical steel sheet and a method for manufacturing the same.
Means for solving the problems
The grain-oriented electrical steel sheet according to an embodiment of the present invention includes, in wt%: 1.0 to 4.0%, C: 0.002% or less (0% excluded) and Bi: 0.001 to 0.1%, the balance comprising Fe and other unavoidable impurities.
Further, 0.05 wt% or less (0 wt% or less) of Mn, 0.01 wt% or less (0 wt% or less) of Al, 0.001 wt% or less (0 wt% or less) of S, and 0.001 wt% or less (0 wt% or less) of N may be contained.
P may be contained in an amount of 0.1 wt% or less (0 wt% is not included), Mo may be contained in an amount of 0.05 wt% or less (0 wt% is not included), Sn may be contained in an amount of 0.1 wt% or less (0 wt% is not included), and Sb may be contained in an amount of 0.05 wt% or less (0 wt% is not included).
The volume ratio of crystal grains having a crystal grain diameter of 20 to 500 μm may be 80% or more.
The volume ratio of the gaussian grains parallel to the plate surface of the steel sheet within an error range of 15 ° or less may be 80% or more.
A method of manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention includes: a step of heating a slab containing, in wt%, Si: 1.0 to 4.0% and C: 0.01 to 0.4%, the balance comprising Fe and other unavoidable impurities; a step of hot rolling the slab to produce a hot rolled sheet; a step of annealing the hot-rolled sheet; a step of cold-rolling the hot-rolled sheet after the annealing of the hot-rolled sheet to produce a cold-rolled sheet; a step of decarburization annealing of the cold-rolled sheet; and a step of performing a final annealing of the decarburization-annealed electrical steel sheet; after the step of annealing the hot-rolled sheet, the average grain diameter of the surface layer portion of the hot-rolled sheet may be 150 to 250 μm.
The slab may also contain 0.001 to 0.1 wt% Bi.
The slab may further include 0.05 wt% or less (excluding 0 wt%) of Mn, 0.01 wt% or less (excluding 0 wt%) of Al, 0.001 wt% or less (excluding 0 wt%) of S, and 0.001 wt% or less (excluding 0 wt%) of N.
P may be contained in an amount of 0.1 wt% or less (0 wt% is not included), Mo may be contained in an amount of 0.05 wt% or less (0 wt% is not included), Sn may be contained in an amount of 0.1 wt% or less (0 wt% is not included), and Sb may be contained in an amount of 0.05 wt% or less (0 wt% is not included).
In the step of heating the slab, heating may be performed at 1100 to 1350 ℃.
The step of annealing the hot rolled sheet may include a decarburization process.
The step of annealing the hot-rolled sheet may include a first step of annealing the hot-rolled sheet at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃, and a second step of annealing the hot-rolled sheet at a temperature of 1000 ℃ to 1200 ℃ and a dew point temperature of 0 ℃ or less.
The first step of annealing the hot rolled sheet may be performed for 10 to 300 seconds, and the second step of annealing the hot rolled sheet may be performed for 10 to 180 seconds.
The steps from the step of manufacturing the cold-rolled sheet to the above-described final annealing may be continuously performed.
The step of manufacturing the cold-rolled sheet and the step of the above decarburization annealing may be repeated 2 or more times.
The step of decarburization annealing may be annealed at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃.
The step of final annealing may include a first step of final annealing in which annealing is performed at 850 ℃ to 1000 ℃ and a dew point temperature of 70 ℃ or lower, and a step of final annealing at a temperature of 1000 ℃ to 1200 ℃ and containing 50 vol% or more of H2A final annealing second step carried out in the atmosphere of (3).
The first step of the final annealing may be performed for 10 to 180 seconds, and the second step of the final annealing may be performed for 10 to 600 seconds.
Effects of the invention
According to an embodiment of the present invention, a method for manufacturing a grain-oriented electrical steel sheet can be provided in which continuous annealing can be performed without performing Batch (Batch) type annealing in a coil state during final annealing.
In addition, the oriented electrical steel sheet having excellent magnetic properties can be produced only by the short-time final annealing.
In addition, a process of winding the cold-rolled steel sheet is not required.
In addition, a grain-oriented electrical steel sheet without using a grain growth inhibitor can be provided.
In addition, since the nitrogen immersion annealing can be omitted, the grain-oriented electrical steel sheet having excellent magnetic properties can be stably produced.
Drawings
FIG. 1 shows the result of analyzing the distribution of crystal grains after hot-rolled sheet annealing in example 2 was performed on a hot-rolled sheet containing 500ppm of Bi.
FIG. 2 shows the results of hot-rolled sheet annealing in example 2 in which a hot-rolled sheet containing no Bi was subjected to hot-rolled sheet annealing and the grain distribution was analyzed.
Detailed Description
The terms first, second, third and the like are used for describing various parts, components, regions, layers and/or sections, but are not limited thereto. These terms are only used to distinguish one element, component, region, layer or section from another element, component, region, layer or section. Thus, a first part, component, region, layer or section discussed below could be termed a second part, component, region, layer or section without departing from the scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms include plural forms as long as they do not mean a definite meaning contrary to the word in the sentence. The use of "comprising" in the specification is meant to specify the presence of stated features, regions, integers, steps, acts, elements and/or components, but does not preclude the presence or addition of other features, regions, integers, steps, acts, elements and/or components.
When a portion is referred to as being "on" or "over" another portion, it is directly on or over the other portion or there may be other portions between them. In contrast, when a portion is described as being "directly above" another portion, there is no other portion between them.
Although not otherwise defined, all terms used herein, including technical and scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art. Terms defined in commonly used dictionaries have meanings conforming to those of related art documents and the present disclosure, and are not to be interpreted as ideal or highly formulated meanings unless further interpreted and defined.
In addition, unless otherwise specified,% represents% by weight, and 1ppm is 0.0001% by weight.
Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the invention. However, the present invention may be realized in various forms and is not limited to the embodiments described herein.
In the conventional grain-oriented electrical steel sheet technology, precipitates such as AlN and MnS are used as grain growth inhibitors, and process conditions are very restricted because the distribution of the precipitates is strictly controlled in all the processes and the conditions for removing the precipitates remaining in the secondarily recrystallized steel sheet are very limited.
In contrast, in one embodiment of the present invention, precipitates such as AlN and MnS are not used as the grain growth inhibitor, and secondary recrystallization is not used. In one embodiment of the present invention, Bi is used to effectively grow grains in the surface layer portion in the annealing step of the hot-rolled sheet, thereby increasing the gaussian grain fraction and obtaining an electrical steel sheet having excellent magnetic properties.
The grain-oriented electrical steel sheet according to an embodiment of the present invention includes, in wt%: 1.0 to 4.0%, C: 0.002% or less (0% excluded) and Bi: 0.001 to 0.1%, the balance comprising Fe and other unavoidable impurities.
The components are specifically described below.
Silicon (Si) reduces magnetic anisotropy of an electrical steel sheet and increases resistivity to improve iron loss. When the Si content is less than 1.0 wt%, the iron loss is deteriorated, and when it exceeds 4.0 wt%, the brittleness is increased. Therefore, the Si content of the oriented electrical steel sheet after the slab and the final annealing step may be 1.0 wt% to 4.0 wt%.
In the case of carbon (C), in hot-rolled sheet annealing, cold-rolled sheet decarburization annealing, and final annealing, a process of moving C in the central portion to the surface layer portion is required in order to diffuse gaussian grains in the surface layer portion toward the central portion, and thus the content of C in the slab may be 0.01 to 0.4 wt%. After the finish annealing step of decarburization, the amount of carbon in the oriented electrical steel sheet may be 0.0020 wt% or less.
Bismuth (Bi) is a segregation element having high volatility, and has a feature of being volatilized at the surface when it is located in the surface layer portion to coarsen crystal grains in the surface layer portion, and on the contrary, has an effect of refining the crystal grains in the center portion of the steel. When less than 0.001 wt% is included, the effect may be slight. On the contrary, when the amount exceeds 0.1% by weight, the surface grain size is not uniform, so that it is preferable to add 0.001 to 0.1% by weight.
In one embodiment of the present invention, since precipitates such as AlN and MnS are not used as grain growth inhibitors, elements that must be used in general grain-oriented electrical steel sheets such as manganese (Mn), aluminum (Al), nitrogen (N), and sulfur (S) are controlled in an impurity range. That is, when Mn, Al, N, S, and the like are inevitably further contained, Mn of 0.05 wt% or less, Al of 0.01 wt% or less, S of 0.001 wt% or less, and N of 0.001 wt% or less may be further contained. More specifically, Al may be contained in an amount of 0.005 wt% or less.
Further, P may be contained in an amount of 0.1 wt% or less (not including 0 wt%), Mo in an amount of 0.05 wt% or less (not including 0 wt%), Sn in an amount of 0.1 wt% or less (not including 0 wt%), and Sb in an amount of 0.05 wt% or less (not including 0 wt%).
Phosphorus (P) is an atom that promotes the formation of gaussian grains, and when added excessively, cracks (Crack) are induced, possibly hindering grain growth. Specifically, P may be contained in an amount of 0.001 to 0.1 wt%.
Molybdenum (Mo) is an element that promotes the formation of gaussian grains of a hot-rolled sheet. Although decarburization is not hindered, crystal grain imbalance may occur when excessive addition is made. Specifically, Mo may be included in an amount of 0.001 to 0.05 wt%.
Tin (Sn) is an element which is present to form gaussian grains, and when it is excessively added, it interferes with decarburization due to surface segregation, and may interfere with crystal growth. Specifically, 0.001 to 0.1% by weight of Sn may be contained.
Antimony (Sb) is an element that promotes the formation of gaussian grains, and when added in excess, it may interfere with decarburization due to surface segregation, thereby interfering with crystal growth. Specifically, 0.001 to 0.05 wt% of Sb may be contained.
Further, as other inevitable impurities, components such as Ti, Mg, and Ca react with oxygen in steel to form oxides, which may hinder the domain movement of the final product as inclusions, and may cause deterioration of magnetic properties, and therefore, strong suppression is required. Therefore, when they are inevitably contained, the respective components may be controlled to 0.005% by weight or less.
In the electrical steel sheet, a volume ratio of crystal grains having a grain diameter of 20 to 500 μm may be 80% or more. When the volume ratio of crystal grains having a grain diameter of 20 to 500 μm is less than 80%, the magnetic properties may be lowered due to insufficient grain growth.
The volume ratio of the gaussian grains parallel to the plate surface of the steel sheet within an error range of 15 ° or less may be 80% or more. When the volume ratio of the gaussian crystal grains is less than 80%, sufficient magnetic properties may not be secured.
A method of manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention includes: a step of heating a slab containing, in wt%, Si: 1.0 to 4.0% and C: 0.01 to 0.4%, the balance comprising Fe and other unavoidable impurities; a step of hot rolling the slab to produce a hot rolled sheet; a step of annealing the hot-rolled sheet; a step of cold-rolling the hot-rolled sheet after the annealing of the hot-rolled sheet to produce a cold-rolled sheet; a step of decarburization annealing of the cold-rolled sheet; and a step of performing final annealing on the decarburized and annealed electrical steel sheet.
Next, the method for manufacturing the oriented electrical steel sheet will be described in detail for each step.
First, the slab is heated.
The composition of the slab is specifically described in the description of the composition of the electrical steel sheet, and therefore, a repetitive description thereof is omitted.
The slab heating temperature may be 1100 to 1350 c higher than the usual heating temperature. When the temperature is high during slab heating, the hot rolled structure becomes coarse, which has a problem of adversely affecting the magnetic properties. However, the method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention has a higher carbon content in the slab than conventional methods, and therefore, even if the slab heating temperature is high, the hot rolled structure does not coarsen, and heating at a higher temperature than usual is advantageous in hot rolling.
Then, the slab is hot-rolled to produce a hot-rolled sheet. The hot rolling temperature is not limited, and as an example, the hot rolling may be finished below 950 ℃.
Then, the hot-rolled sheet is subjected to hot-rolled sheet annealing. At this time, the hot rolled sheet annealing may include a decarburization process. Specifically, the decarburization annealing may be performed at a dew point temperature of 50 ℃ to 70 ℃ in a single-phase austenite region or a region where a composite phase of ferrite and austenite exists. At this time, the temperature range may be 850 ℃ to 1000 ℃. The atmosphere may be a mixed gas atmosphere of hydrogen and nitrogen. In addition, the decarburization amount in the decarburization annealing may be 0.0300% to 0.0600% by weight. More specifically, the step of annealing the hot-rolled sheet to include the decarburization process may include a first step of annealing the hot-rolled sheet at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃, and a second step of annealing the hot-rolled sheet at a temperature of 1000 ℃ to 1200 ℃ and a dew point temperature of 0 ℃ or less. More specifically, the first step of hot-rolled sheet annealing may be performed for 10 to 300 seconds, and the second step of hot-rolled sheet annealing may be performed for 10 to 180 seconds.
In the decarburization annealing, the size of the grains on the surface of the hot rolled plate grows roughly, but the grains inside the electrical steel sheet remain as a fine structure. After such decarburization annealing, the size of ferrite grains of the surface portion may be 150 μm to 250 μm. In this case, the average grain size of the surface layer portion is adjusted to the above range, so that the gaussian grain fraction of the finally manufactured oriented electrical steel sheet can be increased, and the magnetic properties of the oriented electrical steel sheet can be improved.
Then, the hot-rolled sheet after the hot-rolled sheet annealing is cold-rolled to produce a cold-rolled sheet. It is known that in a general process for manufacturing a high magnetic flux density oriented electrical steel sheet, it is effective to perform cold rolling 1 time at a high pressure reduction rate of approximately 90%. This is because an environment advantageous only to the grain growth of the gaussian grains in the primary recrystallized grains is created.
However, the method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention is advantageous in that the grain-oriented electrical steel sheet is formed such that the gaussian crystal grains in the surface layer portion generated by the decarburization annealing and the cold rolling are diffused into the inside, not by the amorphous grain growth of the gaussian crystal grains.
Therefore, in the case where cold rolling is performed at a reduction ratio of 50% to 70% at the time of cold rolling, a large amount of the gaussian distribution structure can be formed in the surface layer portion. In addition, it may be 55% to 65%.
Then, the cold-rolled sheet is subjected to decarburization annealing. The annealing may be performed at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃.
Further, if the cold rolling and decarburization annealing are performed 2 times or more, a large amount of gaussian distribution can be formed in the surface layer portion.
Then, the decarburization annealed electrical steel sheet is subjected to final annealing.
In the method for manufacturing a grain-oriented electrical steel sheet according to an embodiment of the present invention, unlike the conventional batch process (batch), the final annealing may be continuously performed after the cold rolling. That is, the steps from the step of manufacturing the cold-rolled sheet to the step of final annealing can be continuously performed. Therefore, the application of an annealing separator is not required.
The step of final annealing may include a first step of final annealing in which annealing is performed at 850 ℃ to 1000 ℃ and a dew point temperature of 70 ℃ or lower, and a step of final annealing at a temperature of 1000 ℃ to 1200 ℃ and containing 50 vol% or more of H2A final annealing second step carried out in the atmosphere of (3). More specifically, the second step of the final annealing may be performed in a process including 90 vol% or more of H2Is carried out in an atmosphere of (2).
As described above, in one embodiment of the present invention, Bi segregation may be used as the grain growth inhibitor, and AlN precipitates may not be used. Therefore, the burden of the purification annealing for decomposing and removing AlN and MnS can be reduced.
The present invention will be described in more detail below with reference to examples. However, such examples are merely illustrative of the present invention and the present invention is not limited thereto.
Example 1
Will contain, in weight%: 3.23%, C: a slab of 0.25% with the balance being Fe and inevitable impurities was heated at 1250 ℃ and then hot-rolled to a thickness of 1.6 mm. Then, the steel sheet was annealed at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 120 seconds, and then annealed at an annealing temperature of 1100 ℃ in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃ or lower for a time period shown in the following table 1, and then cooled and pickled, and cold rolled at a reduction of 60%.
The cold-rolled sheet was subjected to decarburization annealing at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 60 seconds, then to annealing at an annealing temperature of 1100 ℃ for 50 seconds in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃, and then to pickling after cooling, and cold-rolled at a reduction of 60%.
Thereafter, in the finish annealing, decarburization annealing was performed at 900 ℃ for 60 seconds in a mixed gas atmosphere of wet hydrogen and nitrogen (dew point temperature 60 ℃), and then, 100 vol% H at 1050 ℃ was performed2The heat treatment was performed in an atmosphere for 3 minutes. The annealing time at 1100 ℃ in the annealing of the hot-rolled sheet, the grain size of the surface layer portion after the annealing of the hot-rolled sheet, the gaussian grain fraction of the final electrical steel sheet, and the magnetic properties of the final electrical steel sheet were measured and are shown in table 1 below.
[ TABLE 1 ]
Figure BDA0001707175970000091
As shown in table 1, it is understood that the longer the annealing time when the dew point temperature is 0 ℃ or lower and the annealing temperature is 1100 ℃ at the time of annealing of the hot rolled sheet, the crystal grains of the surface layer portion grow and the gaussian fraction and the magnetic properties are excellent. However, if the annealing time is longer than an appropriate value, internal crystal grains grow, and the structure becomes nonuniform during decarburization annealing after cold rolling, which causes deterioration of the final magnetic properties.
Example 2
Will contain, in weight%: 3.22%, C: 0.245% and a slab containing Bi and the balance Fe and inevitable impurities shown in table 2 below was heated at 1250 ℃ and then hot-rolled to a thickness of 1.6mm, then annealed at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 120 seconds, then subjected to hot-rolled sheet annealing at an annealing temperature of 1100 ℃ for 30 seconds in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃ or less, cooled, acid-washed, and cold-rolled at a reduction of 60%.
The cold-rolled sheet was subjected to decarburization annealing at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 60 seconds, then to annealing at an annealing temperature of 1100 ℃ for 50 seconds in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃, and then to pickling after cooling, and cold-rolled at a reduction of 60%.
Thereafter, in the finish annealing, decarburization annealing was performed at 900 ℃ for 60 seconds in a mixed gas atmosphere of wet hydrogen and nitrogen (dew point temperature 60 ℃), and then, 100 vol% H at 1050 ℃ was performed2The heat treatment was carried out in an atmosphere for 3 minutes. The Bi content at the time of annealing of the hot-rolled sheet, the grain size of the surface layer portion after annealing of the hot-rolled sheet, the gaussian grain fraction of the final electrical steel sheet, and the magnetic properties of the final electrical steel sheet are shown in table 2 below.
[ TABLE 2 ]
Figure BDA0001707175970000101
As shown in table 2, it is found that Bi can be used as a grain growth inhibitor, the grain size of the surface layer portion can be appropriately adjusted after annealing of the hot-rolled sheet, and the gaussian fraction and the magnetic properties are excellent.
Example 3
Will contain, in weight%: 3.19%, C: 0.24%, Bi: a slab of 0.05% and the balance Fe and inevitable impurities was heated at 1250 ℃ and then hot-rolled to a thickness of 1.6mm, then annealed at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 120 seconds, then subjected to hot-rolled sheet annealing at an annealing temperature of 1100 ℃ in a mixed gas atmosphere of hydrogen and nitrogen having a dew point temperature of 0 ℃ or less for a time described in Table 3 below, cooled, then pickled, and cold-rolled at a reduction of 60%.
The cold-rolled sheet was subjected to decarburization annealing at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 60 seconds, then to annealing at an annealing temperature of 1100 ℃ for 50 seconds in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃, and then to pickling after cooling, and cold-rolled at a reduction of 60%.
Thereafter, in the finish annealing, decarburization annealing was performed at 900 ℃ for 60 seconds in a mixed gas atmosphere of wet hydrogen and nitrogen (dew point temperature 60 ℃), and then, 100 vol% H at 1050 ℃ was performed2The heat treatment was performed in an atmosphere for 3 minutes.The annealing time at 1100 ℃ in the annealing of the hot-rolled sheet, the grain size of the surface layer portion after the annealing of the hot-rolled sheet, the gaussian grain fraction of the final electrical steel sheet, and the magnetic properties of the final electrical steel sheet were measured and are shown in table 3 below.
[ TABLE 3 ]
Figure BDA0001707175970000111
As shown in table 3, it is understood that the longer the annealing time when the dew point temperature is 0 ℃ or lower and the annealing temperature is 1100 ℃ at the time of annealing of the hot rolled sheet, the crystal grains of the surface layer portion grow and the gaussian fraction and the magnetic properties are excellent. However, if the annealing time is longer than an appropriate value, internal crystal grains grow, and the structure becomes nonuniform during decarburization annealing after cold rolling, which causes deterioration of the final magnetic properties.
Example 4
Will contain, in weight%: 3.19%, C: 0.24%, Bi: 0.05% of a slab containing P, Sn, Sb, Mo, Al and Mn and the balance Fe and inevitable impurities shown in Table 4 below was heated at 1250 ℃ and then hot-rolled to a thickness of 1.6mm, then annealed at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 120 seconds, then annealed at an annealing temperature of 1100 ℃ in a hydrogen/nitrogen mixed gas atmosphere having a dew point temperature of 0 ℃ or lower for 120 seconds, cooled, then pickled, and cold-rolled at a reduction of 60%. The cold-rolled sheet was subjected to decarburization annealing at an annealing temperature of 870 ℃ and a dew point temperature of 60 ℃ for 60 seconds, then to annealing at an annealing temperature of 1100 ℃ for 50 seconds in a mixed gas atmosphere of hydrogen and nitrogen at a dew point temperature of 0 ℃, and then to pickling after cooling, and cold-rolled at a reduction of 60%. Thereafter, in the finish annealing, decarburization annealing was performed at 900 ℃ for 60 seconds in a mixed gas atmosphere of wet hydrogen and nitrogen (dew point temperature 60 ℃), and then, 100 vol% H at 1100 ℃2The heat treatment was performed in an atmosphere for 3 minutes. The surface grain size of the hot-rolled annealed sheet, the gaussian grain fraction of the final electrical steel sheet, and the magnetic properties of the final electrical steel sheet according to the respective compositions were measured and are shown in table 5 below.
[ TABLE 4 ]
Figure BDA0001707175970000121
[ TABLE 5 ]
Figure BDA0001707175970000122
As shown in tables 4 and 5, it was confirmed that the effect of improving the magnetic properties can be obtained when the composition further contains P, Sn, Sb, Mo, and the like in an appropriate range. In the case of Al and Mn, since their oxidation degree is high, when they are contained in a large amount, it is confirmed that crystal grains having orientation harmful to magnetic properties are formed, and the magnetic properties are adversely affected.
The present invention is not limited to the embodiments, and may be manufactured in various forms different from each other, and it will be understood by those skilled in the art that the present invention may be embodied in other specific forms without changing the technical idea or essential features of the present invention. The embodiments described above are therefore to be understood as illustrative in all respects and not restrictive.

Claims (15)

1. A grain-oriented electrical steel sheet, comprising, in wt%: 1.0 to 4.0%, C: 0.002% or less and not containing 0% and Bi: 0.001 to 0.1%, and the balance of Fe and other unavoidable impurities, wherein the volume ratio of crystal grains having a crystal grain diameter of 20 to 500 μm is 80% or more.
2. The oriented electrical steel sheet according to claim 1, further comprising 0.05 wt% or less and not comprising 0 wt% of Mn, 0.01 wt% or less and not comprising 0 wt% of Al, 0.001 wt% or less and not comprising 0 wt% of S, and 0.001 wt% or less and not comprising 0 wt% of N.
3. The oriented electrical steel sheet according to claim 1, further comprising 0.1 wt% or less and not comprising 0 wt% of P, 0.05 wt% or less and not comprising 0 wt% of Mo, 0.1 wt% or less and not comprising 0 wt% of Sn, and 0.05 wt% or less and not comprising 0 wt% of Sb.
4. The oriented electrical steel sheet according to claim 1, wherein a volume ratio of the gaussian grains parallel to a surface of the steel sheet within an error range of 15 ° or less is 80% or more.
5. A method for manufacturing a grain-oriented electrical steel sheet, comprising the steps of:
a step of heating a slab comprising, in weight%: 1.0 to 4.0% and C: 0.01 to 0.4%, the balance being Fe and other unavoidable impurities;
a step of hot rolling the slab to produce a hot rolled plate;
a step of hot-rolled sheet annealing the hot-rolled sheet;
a step of cold-rolling the hot-rolled sheet after the annealing of the hot-rolled sheet to produce a cold-rolled sheet;
a step of decarburization annealing the cold-rolled sheet; and
a step of subjecting the decarburized and annealed electrical steel sheet to final annealing,
wherein, after the step of annealing the hot-rolled sheet, the average grain diameter of the surface layer portion of the hot-rolled sheet is 150 to 250 μm,
wherein the step of final annealing includes a first step of final annealing in which annealing is performed at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 70 ℃ or lower, and a step of final annealing in which annealing is performed at a temperature of 1000 ℃ to 1200 ℃ and contains 50% by volume or more of H2A second step of final annealing carried out in an atmosphere of (a),
wherein the final annealing first step is performed for 10 to 180 seconds, and the final annealing second step is performed for 10 to 600 seconds.
6. The method of manufacturing a grain-oriented electrical steel sheet as set forth in claim 5, wherein the slab further comprises 0.001 to 0.1 wt% of Bi.
7. The method of manufacturing a grain-oriented electrical steel sheet according to claim 5, wherein the slab further comprises 0.05 wt% or less and not containing 0 wt% of Mn, 0.01 wt% or less and not containing 0 wt% of Al, 0.001 wt% or less and not containing 0 wt% of S, and 0.001 wt% or less and not containing 0 wt% of N.
8. The method of manufacturing a grain-oriented electrical steel sheet according to claim 5, wherein the slab further comprises 0.1 wt% or less and does not contain 0 wt% of P, 0.05 wt% or less and does not contain 0 wt% of Mo, 0.1 wt% or less and does not contain 0 wt% of Sn, and 0.05 wt% or less and does not contain 0 wt% of Sb.
9. The method of manufacturing a grain-oriented electrical steel sheet as claimed in claim 5, wherein the heating is performed at 1100 to 1350 ℃ in the step of heating the slab.
10. The method of manufacturing a grain-oriented electrical steel sheet as set forth in claim 5, wherein the step of annealing the hot-rolled sheet comprises a decarburization process.
11. The method of manufacturing a grain-oriented electrical steel sheet as claimed in claim 5, wherein the step of annealing the hot-rolled sheet comprises a first step of annealing the hot-rolled sheet at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃, and a second step of annealing the hot-rolled sheet at a temperature of 1000 ℃ to 1200 ℃ and a dew point temperature of 0 ℃ or less.
12. The method for manufacturing a grain-oriented electrical steel sheet as claimed in claim 11, wherein the first step of annealing the hot rolled sheet is performed for 10 to 300 seconds, and the second step of annealing the hot rolled sheet is performed for 10 to 180 seconds.
13. The method of manufacturing a grain-oriented electrical steel sheet as set forth in claim 5, wherein the steps from the step of manufacturing the cold-rolled sheet to the step of final annealing are continuously performed.
14. The method of manufacturing a grain-oriented electrical steel sheet as set forth in claim 5, wherein the step of manufacturing the cold-rolled sheet and the step of decarburization annealing are repeated 2 or more times.
15. The method of manufacturing a grain-oriented electrical steel sheet as set forth in claim 5, wherein the decarburization annealing is annealed at a temperature of 850 ℃ to 1000 ℃ and a dew point temperature of 50 ℃ to 70 ℃.
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