CN109554525B - Manufacturing method of mirror-surface oriented silicon steel - Google Patents
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Abstract
The invention discloses a method for manufacturing mirror surface oriented silicon steel, which comprises the following steps: smelting molten iron, adding one or more elements of Sb, Sn, P, Cu and Bi in the smelting process, and refining and pouring the molten steel to obtain a plate blank; heating the plate blank to 1320-1400 ℃, and then carrying out hot rolling on the plate blank to obtain a hot rolled plate; normalizing the hot rolled plate; cold rolling the hot rolled plate after normalizing treatment to prepare a cold rolled plate; performing decarburization annealing on the cold-rolled sheet, and reducing the carbon content in the cold-rolled sheet to below 30ppm while forming SiO on the surface of the cold-rolled sheet2The oxygen adhesion amount of the cold-rolled sheet is controlled to be less than 500ppm, and the reduction time is controlled to be more than 100 seconds; drying and annealing the cold-rolled sheet subjected to decarburization and annealing by using magnesium oxide as a separant; and raising the temperature of the cold-rolled sheet after drying and annealing to 1170-1250 ℃ at a preset temperature rise speed for high-temperature annealing.
Description
Technical Field
The invention relates to the technical field of steelmaking, in particular to a manufacturing method of mirror-surface oriented silicon steel.
Background
The oriented silicon steel is an energy-saving and consumption-reducing magnetic material essential in the power, electrician and telecommunication industries, and is mainly used for manufacturing various power transformers, distribution transformers and large-scale generator stators.
After the traditional oriented silicon steel is subjected to hot rolling, normalizing and cold rolling, the traditional oriented silicon steel is subjected to H2-N2-H2And (3) carrying out decarburization annealing under the protection of O atmosphere, and controlling the carbon content in the steel strip to be below 30ppm so as to prevent the finished plate from magnetic aging. Meanwhile, the decarburization annealing eliminates the rolling stress generated by cold rolling to form primary recrystallization. The surface of the steel strip is oxidized to form SiO during decarburization annealing2And Fe2SiO4The predominant oxide layer adversely affects further decarburization. In the high-temperature annealing process of the annular furnace in the post-process, the oxide layer and the annealing separant MgO coated on the surface of the steel strip are subjected to chemical reaction to generate Mg2SiO4(magnesium silicate) based glass substrates that prevent steel strip sticking during high temperature annealing.
The magnesium silicate bottom layer formed on the surface of the oriented silicon steel has high hardness, a die can be seriously abraded when the die is punched, and the punching burrs are high. Generally, the punching performance of the oriented silicon steel with the magnesium silicate bottom layer is only 3000-6000 times. The oriented silicon steel bottom layer structure consists of a surface continuous layer and a near-surface embedded discrete oxide, and the structure of the bottom layer has a pinning effect on a magnetic domain and blocks the magnetic domain from moving so as to increase the iron loss.
In order to improve the processing performance of the oriented silicon steel sheet and further improve the magnetic performance, the technology of mirror-surface oriented silicon steel without a magnesium silicate glass bottom layer is developed at home and abroad at present. The technology produces the magnesium-silicate-free bottom-layer mirror-oriented silicon steel mainly by changing the type of the annealing release agent or adding a part of alkaline earth metal chloride, oxide and the like into the conventional annealing release agent. The novel annealing separant has the defects of complex coating process, uneven coating and the like, and although the addition of a new additive into the conventional annealing separant can prevent the generation of a bottom layer or eliminate embedded oxides to obtain the mirror-surface-oriented silicon steel, the new additive in the annealing separant can influence the secondary recrystallization stability and the steel purification effect and influence the magnetic performance of a final finished product.
Disclosure of Invention
Aiming at the problems in the production of the prior mirror-surface oriented silicon steel, the invention adopts the conventional annealing separant MgO, avoids the problems of uneven coating, complex coating process and the like of the annealing separant, and does not add additives such as alkaline earth metal chloride, oxide and the like so as to avoid influencing the secondary recrystallization stability and the steel purification effect. One or more of Sb, Sn, P, Cu, Bi and the like are added in the smelting process, the oxygen adhesion amount and the reduction time on the surface of the steel plate in the decarburization annealing process are controlled, a conventional high-temperature annealing separant MgO is coated, and the mirror-surface oriented silicon steel with excellent magnetic performance and no magnesium silicate bottom layer can be stably obtained after high-temperature annealing.
The application provides a manufacturing method of mirror surface oriented silicon steel, which comprises the following steps:
smelting molten iron, adding one or more elements of Sb, Sn, P, Cu and Bi in the smelting process, and refining and pouring the molten steel to obtain a plate blank;
heating the plate blank to 1320-1400 ℃, and then carrying out hot rolling on the plate blank to obtain a hot rolled plate;
normalizing the hot rolled plate;
cold rolling the hot rolled plate after normalizing treatment to prepare a cold rolled plate;
performing decarburization annealing on the cold-rolled sheet, and reducing the carbon content in the cold-rolled sheet to below 30ppm while forming SiO on the surface of the cold-rolled sheet2The oxygen adhesion amount of the cold-rolled sheet is controlled to be less than 500ppm, and the reduction time is controlled to be more than 100 seconds;
drying and annealing the cold-rolled sheet subjected to decarburization and annealing by using magnesium oxide as a separant;
and raising the temperature of the cold-rolled sheet after drying and annealing to 1170-1250 ℃ at a preset temperature rise speed for high-temperature annealing.
Preferably, the smelting of the molten iron comprises:
and putting the molten iron into a converter or an electric furnace for smelting.
Preferably, when the slab is hot-rolled, the rough rolling finishing temperature is controlled to be not less than 1200 ℃, and the finish rolling starting temperature is controlled to be not less than 1000 ℃.
Preferably, when the hot rolled sheet is subjected to the normalizing treatment, the normalizing temperature is controlled to be 900 to 1200 ℃, and the normalizing time is controlled to be 1 to 3 minutes.
Preferably, before the cold rolling of the normalized hot-rolled sheet, the method further comprises:
and carrying out acid cleaning on the hot rolled plate subjected to the normalizing treatment.
Preferably, when the hot-rolled sheet subjected to the normalization treatment is cold-rolled, the cold-rolled sheet is rolled into a cold-rolled sheet of 0.20mm to 0.35mm by a cold-rolling method of one time or two or more times with intermediate annealing, and the final reduction is controlled to be 82% or more.
Preferably, when the cold-rolled sheet is decarburized and annealed, the protective gas used is H2、N2、H2And O.
Preferably, the step of raising the temperature of the cold-rolled sheet after drying and annealing to 1170-1250 ℃ at a preset temperature rise speed for high-temperature annealing comprises the following steps:
in a ring furnace or a bell-type furnace, raising the temperature to 1170-1250 ℃ at the temperature rise speed of 15-20 ℃/H, and carrying out high-temperature annealing on the cold-rolled sheet after drying and annealing, wherein the used protective gas is stripped from H during the high-temperature annealing2And N2The hydrogen content of the formed mixed gas is 25-100%.
Preferably, after the cold-rolled sheet after drying and annealing is heated to 1170-1250 ℃ at a preset temperature rise speed for high-temperature annealing, the method further comprises the following steps:
and (3) stretching and flattening annealing the steel strip discharged from the furnace, and controlling the temperature of the flattening annealing to be not more than 800 ℃.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
in the invention, one or more of Sb, Sn, P, Cu, Bi and other elements are added in the smelting process, and the elements inhibit the decarburization annealing processOxidizing and changing the structure of the oxide layer. Heating to 900-1100 deg.C by using conventional magnesia isolating agent, passing through MgO and SiO in surface oxide film2Chemically react to form Mg2SiO4The bottom layer (magnesium silicate or forsterite) can isolate the inhibitor from the protective atmosphere, and prevent the inhibitor from premature decomposition. Because the thickness of the generated magnesium silicate bottom layer is less than 1 mu m, elements such as Sb, Sn, P, Cu, Bi and the like are greatly enriched on the surface of the substrate and partially diffused and overflowed to the bottom layer along with the increase of the high-temperature annealing temperature in the later period, the thin magnesium silicate bottom layer formed in the earlier period is corroded and removed, and finally the mirror-surface oriented silicon steel product with stable and excellent magnetic performance and without the magnesium silicate bottom layer can be obtained.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow chart of a method for manufacturing mirror-oriented silicon steel according to an embodiment of the present application.
Detailed Description
Aiming at the problems in the production of the prior mirror-surface oriented silicon steel, the invention adopts the conventional annealing separant MgO, avoids the problems of uneven coating, complex coating process and the like of the annealing separant, and does not add additives such as alkaline earth metal chloride, oxide and the like so as to avoid influencing the secondary recrystallization stability and the steel purification effect. One or more of Sb, Sn, P, Cu, Bi and the like are added in the smelting process, the oxygen adhesion amount and the reduction time on the surface of the steel plate in the decarburization annealing process are controlled, a conventional high-temperature annealing separant MgO is coated, and the mirror-surface oriented silicon steel with excellent magnetic performance and no magnesium silicate bottom layer can be stably obtained after high-temperature annealing.
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
Example one
As shown in fig. 1, the present embodiment provides a method for manufacturing mirror-oriented silicon steel, including:
step S101: smelting molten iron, adding one or more elements of Sb (antimony), Sn (tin), P (phosphorus), Cu (copper) and Bi (bismuth) in the smelting process, and refining and pouring the molten steel to obtain a plate blank.
In the specific implementation process, when the molten iron is smelted, the molten iron can be put into a converter or an electric furnace for smelting, and the molten iron can be smelted through the converter or the electric furnace.
In the concrete implementation, when the slab is hot-rolled, the finish temperature of rough rolling is controlled to be not less than 1200 ℃ (for example, 1200 ℃, 1250 ℃, 1300 ℃, etc.), and the start temperature of finish rolling is controlled to be not less than 1000 ℃ (for example, 1000 ℃, 1050 ℃, 1100 ℃, etc.).
Step S102: and heating the plate blank to 1320-1400 ℃, and carrying out hot rolling on the plate blank to obtain a hot rolled plate.
Step S103: the hot rolled sheet is subjected to a normalizing treatment.
In the concrete implementation, when the hot rolled sheet is subjected to the normalizing treatment, the normalizing temperature is controlled to be 900 to 1200 ℃ (for example, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, etc.), the normalizing time is controlled to be 1 to 3 minutes (for example, 1 minute, 2 minutes, 3 minutes, etc.), and the pickling is further carried out after the normalizing treatment.
Step S104: and cold rolling the hot rolled plate after normalizing treatment to obtain the cold rolled plate.
In the specific implementation, when cold rolling is performed, a cold-rolled sheet of 0.20mm to 0.35mm is rolled by a single or double or more cold rolling method with intermediate annealing, and the final reduction is required to be 82% or more (for example, 82%, or 85%, or 90%, or the like).
Step S105: decarburization and annealing: subjecting a cold-rolled sheet to decarburization annealing at 900 to 1100 ℃ (for example, 900 ℃, 1000 ℃, 1100 ℃, etc.) to reduce the carbon content in the cold-rolled sheet to 30ppm or lessForming SiO on the surface of the cold-rolled sheet2(silicon dioxide) as the main component, controlling the oxygen adhesion amount of the cold-rolled plate to be less than 500ppm, and controlling the reduction time to be more than 100 seconds.
In the specific implementation process, when the decarburization annealing is carried out, the protective gas used is H2、N2H2O.
In the invention, one or more of Sb, Sn, P, Cu, Bi and other elements are added, and the elements are enriched on the surface of the steel plate in the decarburization annealing process, so that the oxidation reaction on the surface of the steel plate can be inhibited, and the SiO2 oxide layer structure on the surface of the decarburization annealed steel plate is changed. When the amount of oxygen adhered to the steel sheet after decarburization annealing is controlled to 500ppm or less, the reduction time after decarburization is prolonged to more than 100 seconds. The SiO2 oxide layer formed in the decarburization annealing process and the coated separant MgO form a loose magnesium silicate bottom layer with the thickness of less than 1 mu m at the early stage of high-temperature annealing, and the magnesium silicate bottom layer is removed under the action of Sb, Sn, P, Cu, Bi and other elements at the later stage of high-temperature annealing to obtain the mirror-surface oriented silicon steel without the magnesium silicate bottom layer.
Step S106: and (3) taking magnesium oxide as a separant, and carrying out drying annealing on the cold-rolled sheet subjected to decarburization annealing.
In the specific implementation process, a release agent with magnesium oxide as a main component can be coated according to a conventional process, and drying and annealing are carried out.
Step S107: and raising the temperature of the cold-rolled sheet after drying and annealing to 1170-1250 ℃ at a preset temperature rise speed for high-temperature annealing.
In the specific implementation process, the temperature of the cold-rolled sheet after drying annealing can be raised to 1170-1250 ℃ at a temperature rise speed of 15-20 ℃/H in a ring furnace or a bell-type furnace, wherein the protective gas used in the high-temperature annealing is lifted from H2And N2The hydrogen content of the formed mixed gas is 25-100%.
After step S107, the method further includes:
and (3) stretching and flattening annealing the steel strip discharged from the furnace, and controlling the temperature of the flattening annealing to be not more than 800 ℃.
The technical scheme in the embodiment of the application at least has the following technical effects or advantages:
in the invention, one or more of Sb, Sn, P, Cu, Bi and other elements are added in the smelting process, so that the elements inhibit oxidation and change the structure of an oxide layer in the decarburization annealing process. Heating to 900-1100 deg.C by using conventional magnesia isolating agent, passing through MgO and SiO in surface oxide film2Chemically react to form Mg2SiO4The bottom layer (magnesium silicate or forsterite) can isolate the inhibitor from the protective atmosphere, and prevent the inhibitor from premature decomposition. Because the thickness of the generated magnesium silicate bottom layer is less than 1 mu m, elements such as Sb, Sn, P, Cu, Bi and the like are greatly enriched on the surface of the substrate and partially diffused and overflowed to the bottom layer along with the increase of the high-temperature annealing temperature in the later period, the thin magnesium silicate bottom layer formed in the earlier period is corroded and removed, and finally the mirror-surface oriented silicon steel product with stable and excellent magnetic performance and without the magnesium silicate bottom layer can be obtained.
Example two
Smelting oriented silicon steel by using a converter, wherein the slab comprises the following chemical components in percentage by weight: 0.072% of C, 3.12% of Si, 0.077% of Mn, 0.022% of S, 0.008% of N, 0.145% of Sn, 0.035% of Cu, 0.0305% of Als, 0.025% of Cr, 0.016% of P, 0.022% of Sb, 0.0048% of Bi and the like, and the balance of Fe and inevitable impurities.
The slab was heated at 1370 ℃ and then hot-rolled into a hot-rolled sheet of 2.3mm thickness. The hot rolled sheet was annealed at 1125 ℃ for 1.5 minutes, pickled and cold rolled to a final thickness, and the cold rolled sheet was decarburized at 840 ℃ and the oxygen deposit amount on the surface of the decarburized sheet and the reduction time were as shown in Table 1. Directly coating a conventional magnesia separant without nitriding treatment, drying, and then entering a circular furnace for high-temperature annealing. Raising the temperature to 1190 ℃ at the heating rate of 17 ℃/h, and preserving the temperature for 25 hours, wherein the hydrogen content in the protective atmosphere is 75 percent. Drawing and flattening annealing at 800 ℃ after the material is taken out of the annular furnace.
As shown in Table 2, in Table 1, the alloy contents were constant for the decarburization conditions and the oxygen content of the examples.
TABLE 1
Among them, B800 and P17/50 are important magnetic performance indexes of the oriented silicon steel. B800 represents the magnetic induction of the oriented silicon steel. P17/50 represents the loss of oriented silicon steel at 50 Hz.
EXAMPLE III
Smelting oriented silicon steel by using a converter, wherein the plate blank comprises the following components in percentage by weight: c: 0.06% -0.10%, Si: 2.9% -3.3%, Mn: 0.05-0.10%, P: 0.01-0.055%, S: 0.01-0.03%, Als: 0.02-0.035%, N: 0.007-0.010%, Cr: 0.02% -0.4%, Sb: 0.005-0.065%, Sn: 0.02% -0.2%, Cu: 0.03% -0.10%, Bi: 0.001% -0.03%, etc., and the balance of Fe and inevitable impurities.
The slab was heated at 1370 ℃ and then hot-rolled into a hot-rolled sheet of 2.3mm thickness. The hot-rolled sheet was annealed for 1.5 minutes at 1125 ℃ in a normalizing process, pickled and cold rolled to final gauge. And (2) decarburization annealing is carried out on the cold-rolled sheet at 840 ℃, the reduction time after decarburization is 130 seconds, and the cold-rolled sheet is directly coated with a conventional magnesia separant without nitriding treatment and then enters a circular furnace for high-temperature annealing after being dried. Raising the temperature to 1190 ℃ at the heating rate of 17 ℃/h, and preserving the temperature for 25 hours, wherein the hydrogen content in the protective atmosphere is 75 percent. Drawing and flattening annealing at 800 ℃ after the material is taken out of the annular furnace.
As shown in Table 2, Table 2 shows examples in which the amount of alloy added in the smelting process was constant for decarburization and oxygen content.
TABLE 2
The above examples are merely preferred examples and are not intended to limit the embodiments of the present invention.
Magnesium silicate bottom layers formed on the surfaces of traditional oriented silicon steel are high in hardness, dies can be seriously abraded when the die is punched, and burrs of the punched die are high. Generally, the punching performance of the oriented silicon steel with the magnesium silicate bottom layer is only 3000-6000 times. The oriented silicon steel bottom layer structure consists of a surface continuous layer and a near-surface embedded discrete oxide, and the structure of the bottom layer has a pinning effect on a magnetic domain and blocks the magnetic domain from moving so as to increase the iron loss. The mirror surface oriented silicon steel can greatly improve the punching performance of the oriented silicon steel, the punching times can reach more than tens of thousands of times, the pinning structure is eliminated in the high-temperature annealing process, and a low-iron-loss product is easier to obtain theoretically.
Before the present invention, the method for obtaining mirror-oriented silicon steel mainly adds chloride to the conventional MgO isolating agent and uses a novel annealing isolating agent Al (in the background art)2O3(alumina) or SiO2Both of them can cause magnetic property fluctuation, and the novel annealing release agent has poor water solubility, complex coating process and difficult uniform coating.
The invention creatively adds one or more of Sb, Sn, P, Cu, Bi and other elements in a steel-making process, the elements inhibit the surface oxidation of the steel plate and change the structure of an oxide layer in the decarburization annealing process, and the oxygen adhesion amount on the surface of the steel plate is controlled to be less than 500ppm and the reduction time is controlled to be more than 100 seconds in the decarburization annealing process. In the high-temperature annealing stage, Sb, Sn, P, Cu, Bi and other elements are enriched on the surface of the substrate, diffused to the bottom layer and overflow to erode the magnesium silicate bottom layer so as to achieve the purpose of removing the bottom layer. The method is simple and easy to implement, and the mirror-surface oriented silicon steel product can be stably obtained. The equipment used in the field production is conventional production equipment of oriented silicon steel, and has good practicability and popularization, thereby having good popularization prospect.
One or more of Sb, Sn, P, Cu, Bi and other elements are added in the steel making process, and the subsequent process is according to the conventional production process, so that the process is simple and easy to control, and the cost is low.
Compared with the prior mirror-surface oriented silicon steel production, the inhibitor of the method is more stable, and the mirror-surface oriented silicon steel with stable magnetic performance can be more easily obtained.
The technical scheme in the embodiment of the application at least has the following technical effects or advantages:
in the invention, one or more of Sb, Sn, P, Cu, Bi and other elements are added in the smelting process, so that the elements inhibit oxidation and change the structure of an oxide layer in the decarburization annealing process. By conventional meansMgO isolating agent is heated to 900-1100 ℃ and passes through MgO and SiO in the surface oxide film2Chemically react to form Mg2SiO4The bottom layer (magnesium silicate or forsterite) can isolate the inhibitor from the protective atmosphere, and prevent the inhibitor from premature decomposition. Because the thickness of the generated magnesium silicate bottom layer is less than 1 mu m, elements such as Sb, Sn, P, Cu, Bi and the like are greatly enriched on the surface of the substrate and partially diffused and overflowed to the bottom layer along with the increase of the high-temperature annealing temperature in the later period, the thin magnesium silicate bottom layer formed in the earlier period is corroded and removed, and finally the mirror-surface oriented silicon steel product with stable and excellent magnetic performance and without the magnesium silicate bottom layer can be obtained.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. A method for manufacturing mirror-surface-oriented silicon steel, comprising:
smelting molten iron, adding Sb, Sn, P, Cu and Bi elements in the smelting process, and refining and pouring the molten steel to obtain a plate blank; the slab comprises the following components in percentage by weight: c: 0.06% -0.10%, Si: 2.9% -3.3%, Mn: 0.05-0.10%, P: 0.01-0.055%, S: 0.01-0.03%, Als: 0.02-0.035%, N: 0.007-0.010%, Cr: 0.02% -0.4%, Sb: 0.005-0.065%, Sn: 0.02% -0.2%, Cu: 0.03% -0.10%, Bi: 0.001 to 0.03 percent, and the balance of Fe and inevitable impurities;
heating the plate blank to 1320-1400 ℃, and then carrying out hot rolling on the plate blank, wherein the finishing temperature of rough rolling is controlled to be not lower than 1200 ℃, and the starting temperature of finish rolling is controlled to be not lower than 1000 ℃ to prepare a hot rolled plate;
normalizing and pickling the hot rolled plate, wherein the normalizing temperature is controlled to be 900-1200 ℃, and the normalizing time is controlled to be 1-3 minutes;
cold rolling the hot rolled plate after normalizing and pickling to obtain a cold rolled plate;
performing decarburization annealing on the cold-rolled sheet, controlling the annealing temperature to be 900-1100 ℃ during decarburization annealing, reducing the carbon content in the cold-rolled sheet to be below 30ppm, and simultaneously forming SiO on the surface of the cold-rolled sheet2The oxygen adhesion amount of the cold-rolled sheet is controlled to be less than 500ppm, and the reduction time is controlled to be more than 100 seconds;
drying and annealing the cold-rolled sheet subjected to decarburization and annealing by using magnesium oxide as a separant;
in a ring furnace or a bell-type furnace, raising the temperature of the cold-rolled sheet after drying and annealing to 1170-1250 ℃ at a temperature rise speed of 15-20 ℃/h for high-temperature annealing;
and stretching and flattening annealing the steel strip discharged from the furnace, and controlling the temperature of the flattening annealing to be not more than 800 ℃.
2. The method of claim 1, wherein said smelting molten iron comprises:
and putting the molten iron into a converter or an electric furnace for smelting.
3. The method according to claim 1, wherein the hot-rolled sheet after the normalization treatment is cold-rolled by a cold rolling method of one or more than two times with intermediate annealing to a cold-rolled sheet of 0.20mm to 0.35mm, and the final reduction is controlled to be 82% or more.
4. The method of claim 1, wherein the protective gas used in decarburization annealing of the cold-rolled sheet is H2、N2、H2And O.
5. The method of claim 1, wherein the protective gas used in the high temperature annealing is H2And N2The hydrogen content of the formed mixed gas is 25-100%.
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