CN115505822B - Method for improving grain uniformity of oriented silicon steel and oriented silicon steel prepared by method - Google Patents

Method for improving grain uniformity of oriented silicon steel and oriented silicon steel prepared by method Download PDF

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CN115505822B
CN115505822B CN202211165827.9A CN202211165827A CN115505822B CN 115505822 B CN115505822 B CN 115505822B CN 202211165827 A CN202211165827 A CN 202211165827A CN 115505822 B CN115505822 B CN 115505822B
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silicon steel
annealing
temperature
oriented silicon
steel
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CN115505822A (en
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王�琦
王强明
王靖鸿
陈德顺
江健
孙高鹏
王佳伟
程笑天
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Anqing Xinpu Electric Equipment Co ltd
Wuxi Putian Iron Core Co Ltd
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Wuxi Putian Iron Core Co Ltd
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
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    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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    • C—CHEMISTRY; METALLURGY
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    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
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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
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium

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Abstract

The application discloses a method for improving grain uniformity of oriented silicon steel and the oriented silicon steel prepared by the method, and belongs to the technical field of oriented silicon steel manufacturing. The method of the application comprises the following steps: the molten iron is desulfurized, converted and refined to obtain molten steel; (2) continuously casting molten steel to obtain a continuous casting blank; (3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting blank to obtain a hot rolled plate; (4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate; (5) Coating a high-temperature annealing isolating agent, and drying and coiling to obtain a silicon steel coil; (6) carrying out high-temperature annealing in a chamber furnace; (7) And after high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally performing leveling stretching annealing to adjust the plate shape. The application controls the grain size of the whole coil of the oriented silicon steel by limiting the inner and outer diameter sizes of the oriented silicon steel coil, the annealing isolating agent and the high-temperature annealing process, eliminates fine grains and broken grains, improves the uniformity of the grains and reduces the iron loss.

Description

Method for improving grain uniformity of oriented silicon steel and oriented silicon steel prepared by method
Technical Field
The application relates to the technical field of oriented silicon steel manufacturing, in particular to a method for improving grain uniformity of oriented silicon steel and oriented silicon steel prepared by the method.
Background
The oriented silicon steel is a soft magnetic material with excellent performance, is mainly used as an iron core of a transformer, and is an important soft magnetic alloy indispensable in the power, electronic and military industries. At present, with the rapid development of various industries in China, the demand of China for electric power is also increasing. Because the coal resources in China are mainly distributed in the western region and the northern region, the water energy resources are mainly concentrated in the southwest region, the eastern region is deficient in primary energy resources, and the electricity load is relatively concentrated. The imbalance of energy resources and power load distribution determines the necessity of western electric east delivery. In the long-distance electric energy transmission process, a transformer is indispensable, and in the use process of the transformer, a certain amount of electric energy can be consumed by the iron core, and the property of the iron core that the iron core consumes electric energy per unit weight is called iron loss. The iron loss reduction has great significance for national energy conservation and emission reduction strategies.
Grain size of the oriented silicon steel is a main factor influencing iron loss of the iron core, and a high-temperature annealing process plays a critical role in growth of secondary recrystallized grains in the production process of the oriented silicon steel. The Gaussian grains in the oriented silicon steel can be abnormally grown to the size reaching the centimeter level in the procedure, but if the heating temperature and the heating time in the high-temperature annealing process are not required, a large number of ungrown grains exist in the silicon steel, so that the iron loss is increased sharply.
In production, because silicon steel is easy to adhere in the high-temperature annealing process, magnesium oxide and the like are adopted as high-temperature annealing isolating agents, so that the silicon steel is prevented from being in direct contact with the silicon steel. However, in the subsequent process of coating the insulating coating liquid, unreacted magnesium oxide is removed by water washing and acid washing, so that the high-temperature annealing isolation dosage used in the prior art is basically supersaturated, the diameter of the silicon steel coil after the magnesium oxide is coated can reach 1800mm, the inner diameter of the coil is 520mm, and the difference between the inner diameter and the outer diameter of the coil is 1280mm. The excessive difference of the diameters of the inner coil and the outer coil makes temperature conduction difficult, and a temperature field with high temperature of the inner coil and the outer coil and low temperature of the middle coil is formed. Too much magnesium oxide coating can also increase the diameter of the silicon steel coil, increase the heat conduction difficulty in the coil, and also cause uneven temperature of the silicon steel coil. The silicon steel temperature plays a vital role in abnormal growth of crystal grains, so that the temperature uniformity of a silicon steel coil needs to be improved, and the heat preservation time is ensured to be enough, so that the oriented silicon steel with qualified crystal grain size and good magnetic property can be produced. However, the current research on the grain size is more focused on the selection and the dosage of the inhibitor in the steel, the desired grain size is obtained through the selective growth effect of the inhibitor, and the uniformity of the grains of the whole coil is rarely solved from the temperature field in the furnace in the high-temperature annealing process.
Disclosure of Invention
The application provides a method for improving grain uniformity of oriented silicon steel and the oriented silicon steel prepared by the method, aiming at the defects of the prior art. The application controls the grain size of the whole coil of the oriented silicon steel by limiting the inner and outer diameter sizes of the oriented silicon steel coil, the annealing isolating agent and the high-temperature annealing process, eliminates fine grains and broken grains, improves the uniformity of the grains and reduces the iron loss.
The technical scheme of the application is as follows:
a method for improving grain uniformity of oriented silicon steel, comprising the steps of:
(1) The molten iron is desulfurized by a KR method, and is obtained by a converter and RH vacuum circulation degassing refining method;
(2) Continuously casting molten steel to obtain a continuous casting blank;
(3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting blank to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate;
(5) Coating a high-temperature annealing isolating agent, and drying and coiling to obtain a silicon steel coil;
(6) Carrying out high-temperature annealing of the chamber covering furnace;
(7) And after high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally performing leveling stretching annealing to adjust the plate shape.
Further, in the step (1), the molten steel comprises the following components in percentage by mass: c:0.03 to 0.06 percent of Si:2.90 to 3.25 percent of Mn:0.05 to 0.15 percent, P: less than or equal to 0.015 percent, S:0.003 to 0.006 percent of Al:0.025 to 0.050 percent, N: 0.008-0.011%, and the balance of iron and unavoidable impurities.
Further, in the step (5), the annealing separator comprises the following components in percentage by mass: magnesium oxide, titanium dioxide, sodium tetraborate; the magnesium oxide is spherical, the D50 particle size is smaller than 2 mu m, and the D50 particle size of the titanium dioxide is smaller than 0.5 mu m.
Further, in the step (5), the coating amount of the annealing separator is 8 to 10.0g/m 2 。
Further, in the step (5), the inner diameter d of the silicon steel coil 1 700mm, outside diameter d 2 1850-1900 mm.
Further, in the step (6), the air flow direction of the chamber furnace is from the outer ring to the inner ring of the silicon steel coil; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
Further, in the step (6), the specific process of the high-temperature annealing is as follows: heating to 680-700 ℃ in 3-4 h, preserving heat for t, heating to 880-900 ℃ in 10-13 ℃/h, preserving heat for 6-8 h, and heating to 1180-1210 ℃ in 10-12 ℃/h.
Further, the heat preservation time t satisfies the following relation:
a 0.5 +8lnb+1.2x<t<a 0.5 +6lnb+1.1x+1
wherein: t is the heat preservation time, h; a is d 2 -d 1 Mm; b is silicon steel thickness, mm; x is the coating quantity per unit area of the annealing separator, and g/m 2 。
Further, the silicon steel thickness refers to a target thickness of the prepared silicon steel, and the silicon steel thickness includes, but is not limited to, 0.23mm, 0.27mm.
An oriented silicon steel prepared by the method.
Further, the application of the oriented silicon steel in the transformer core.
The application can control the grain size of the whole steel coil to be normal, reduce the occurrence of abnormal grains and improve the uniformity of the grains by limiting the inner diameter and the outer diameter of the steel coil, the annealing isolating agent and the high-temperature annealing process.
The granularity of the annealing isolating agent is too large, the gap is large after coating, and the flatness is reduced; but the granularity is too little, can lead to the hydration rate too high, can produce a large amount of vapor at the high temperature annealing stage, in the coil of strip of high tension and compactly, vapor is difficult for discharging, not only can influence the reaction go on, can also influence the face for the watermark appears in the face, causes the colour difference, reduces pleasing to the eye degree. The application optimizes the high-temperature annealing isolating agent, reduces the granularity of magnesium oxide and titanium dioxide, and increases sodium tetraborate. The reduction of the granularity of magnesium oxide and titanium dioxide improves the stacking density after coating and reduces the air gap between the release agents. The smaller granularity is favorable for the rapid progress of the reaction, the increase of the bulk density and the thinning of the thickness of the high-temperature annealing isolating agent, and the sodium tetraborate is used as a reaction catalyst to accelerate the reaction. Under the condition, the reaction in the high-temperature annealing process is not affected, the air gap is thinned and reduced, the heat conduction efficiency is improved, the temperature uniformity of the steel plate is further improved, and a good environment is provided for the full and uniform growth of finished product grains.
The application changes the flow direction of the gas flow of the cover chamber furnace, the side cover and the furnace bottom of the cover chamber furnace are both provided with the resistance belt for heating, the heating area of the outer ring of the steel coil is large, the heating area of the outer ring of the steel coil is also large, the heat of the resistance belt of the side cover is taken out by adopting the heating mode of the inner ring in and the outer ring in, and the heat is fully conducted to the steel coil by adopting the flow mode of the cover chamber furnace gas flow in from the inner ring and the outer ring out to be changed into the mode of the outer ring in and out.
Because the temperature is not uniformly distributed and conducted in the axial direction and the radial direction of the steel coil, abnormal grains can occur in each abnormal temperature region of the steel coil, the application reduces the heat conduction thickness by greatly increasing the inner diameter and the outer diameter on the premise of unchanged coil weight by a method of greatly increasing the inner diameter and greatly increasing the outer diameter, the increase of the outer diameter does not exceed the inner cover, and the negative influence on the gas flow is avoided; the adjustment of the inner diameter and the outer diameter of the steel coil reduces the number of whole turns, reduces the interface generated by two different media of magnesium oxide-silicon steel, reduces the heat conduction difficulty, is beneficial to the improvement of the heat conduction efficiency, and improves the uniformity of the whole temperature of the steel coil.
According to the application, through limiting the heat preservation time, the secondary cold-rolled sheet fully recovers recrystallization, and the obtained primary recrystallization grains are fine, so that a good foundation is provided for the full and uniform growth of finished product grains.
The beneficial technical effects of the application are as follows:
(1) According to the application, the granularity of magnesium oxide and titanium dioxide is reduced by optimizing the high-temperature annealing isolating agent, the sodium tetraborate additive is added, and the generation of magnesium silicate glass films is promoted. The optimized high-temperature annealing isolating agent has good compactness and uniformity, low water content and few air gaps after coating, and enhances the heat conduction efficiency of the silicon steel coil.
(2) The application adopts the silicon steel coil with large coil diameter, and reduces the use of a high-temperature annealing isolating agent, thereby reducing the heat conduction thickness, shortening the heating time of the annealing stage and ensuring the smooth growth of secondary recrystallized grains; meanwhile, the annealing isolating agent is reduced, the heating time is shortened, and the energy and the generation cost are saved.
(3) The application adopts the mode of entering the outer ring and exiting the inner ring, so that heat can be fully conducted to the steel coil.
(4) According to the application, the heat preservation time is adjusted according to the difference between the inner and outer coils, the thickness of the silicon steel and the coating amount of the magnesium oxide in unit area, so that the growth of crystal grains is ensured to be complete, fine grains and broken grains are eliminated, and the grain distribution of the oriented silicon steel prepared by the application is uniform, the grain size in unit area is improved by 6-14 times, the iron loss is reduced by about 0.11W/kg, and the magnetic induction is improved by about 0.033T through the cooperative optimization of the process and the auxiliary agent in the preparation of the silicon steel.
Drawings
FIG. 1 is a graph showing the morphology of grains in a roll according to example 1 of the present application.
Fig. 2 is a morphology of the grains in the roll of comparative example 1.
Fig. 3 is a morphology of grains in the roll of comparative example 4.
Detailed Description
The present application will be described in detail below with reference to the drawings and examples.
Example 1
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the components of the refined molten steel are shown in table 1:
TABLE 1 molten steel refined in EXAMPLE 1
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 600 ℃ to obtain the silicon steel coil.
Wherein the annealing separator comprises the following components: thermally conductive magnesia, titania,Sodium tetraborate, wherein magnesium oxide is spherical, the granularity D50 is 1.742 mu m, the granularity D50 of titanium dioxide is 0.384 mu m as a pore filling agent, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 9.4g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1850mm.
(6) High-temperature annealing is carried out in a chamber covering furnace, and the gas flow of the chamber covering furnace is the flow of the outer ring inlet/outlet type atmosphere; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.5h to 680 ℃, and the heat preservation time t is 33h; then heating to 880 ℃ at the speed of 10 ℃/h, preserving heat for 6h, and heating to 1190 ℃ at the speed of 10 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method.
The grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the example 1, and the grain size is normal without fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 0.964W/kg, and the magnetic induction is 1.89T.
Example 2
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the components of the refined molten steel are shown in table 2:
TABLE 2 refined molten steel composition of EXAMPLE 2
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.27mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 620 ℃ to obtain a silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is spherical, the granularity D50 is 1.851 mu m, the granularity D50 of the titanium dioxide is 0.366 mu m as a pore filler, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 8.5g/m 2 Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1900mm.
(6) And (5) carrying out high-temperature annealing of the chamber furnace, wherein the gas flow of the chamber furnace is the outer ring inlet/outlet type atmosphere flow. The method comprises the steps of carrying out a first treatment on the surface of the The atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: heating to 700 ℃ for 4 hours, and keeping the temperature for 36 hours; then heating to 900 ℃ at a speed of 13 ℃/h, preserving heat for 8h, and heating to 1210 ℃ at a speed of 12 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method.
The grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the example 2, and the grain size is normal without fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 0.989W/kg, and the magnetic induction is 1.88T.
Example 3
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the components of the refined molten steel are shown in table 3:
TABLE 3 refined molten steel composition of EXAMPLE 3
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 620 ℃ to obtain a silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is spherical, the granularity D50 is 1.773 mu m, the granularity D50 of the titanium dioxide is 0.357 mu m as a pore filling agent, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 9.2g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1880mm.
(6) High-temperature annealing is carried out in a chamber covering furnace, and the gas flow of the chamber covering furnace is the flow of the outer ring inlet/outlet type atmosphere; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.8h, heating to 690 ℃, and keeping the temperature for 36h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape. The oriented silicon steel prepared by the method.
The grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the example 3, and the grain size is normal without fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 0.952W/kg, and the magnetic induction is 1.88T.
Comparative example 1
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the components of the refined molten steel are shown in table 4:
TABLE 4 Components of refined molten steel of comparative example 1
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(5) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(6) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 600 ℃ to obtain the silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is in a rod shape, the granularity D50 is 1.764 mu m, the granularity D50 of the titanium dioxide is 0.369 mu m as a pore filler, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 9.3g/m 2 . Inner diameter d of silicon steel coil 1 520mm, outer diameter d 2 1800mm. (6) And (5) carrying out high-temperature annealing of the chamber furnace, wherein the gas flow of the chamber furnace is the outer ring inlet/outlet type atmosphere flow. The method comprises the steps of carrying out a first treatment on the surface of the The atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.8h, heating to 690 ℃, and keeping the temperature for 37h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method.
The crystal grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the comparative example 1, and partial crystal grains are smaller and have fine crystals and broken crystals. The online iron loss of the silicon steel coil is 1.058W/kg, and the magnetic induction is 1.85T.
Comparative example 2
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the components of the refined molten steel are shown in table 5:
TABLE 5 Components of refined molten steel of comparative example 2
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 580 ℃ to obtain a silicon steel coil.
Wherein the annealing separator comprises the following components: the heat-conducting magnesium oxide, titanium dioxide and sodium tetraborate, wherein the granularity D50 of the magnesium oxide is 1.833 mu m, the granularity D50 of the titanium dioxide is 0.342 mu m as a pore filler, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 9.3g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1870mm.
(6) High-temperature annealing is carried out in a chamber covering furnace, and the gas flow of the chamber covering furnace is the flow of the outer ring inlet/outlet type atmosphere; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.5h, heating to 690 ℃, and keeping the temperature for 30h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method.
The crystal grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the comparative example 2, and partial crystal grains are smaller and have fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 1.069W/kg, and the magnetic induction is 1.84T.
Comparative example 3
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the compositions of the refined molten steel are shown in table 6:
TABLE 6 composition of refined molten steel of comparative example 3
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 660 ℃ to obtain the silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is rod-shaped, the granularity D50 is 1.821 mu m, the granularity D50 of the titanium dioxide is 0.356 mu m as a pore filling agent, and the proportion is water: magnesium oxide: titanium dioxide: sodium tetraborate = 900:100:10:0.5 The dosage of the high-temperature annealing isolating agent is 12.6g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1920mm. (6) High-temperature annealing is carried out in a chamber covering furnace, and the gas flow of the chamber covering furnace is the flow of the outer ring inlet/outlet type atmosphere; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.5h, heating to 690 ℃, and keeping the temperature for 40h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method.
The crystal grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the comparative example 3, and partial crystal grains are smaller and have fine crystals and broken crystals. The online iron loss of the silicon steel coil is 1.072W/kg, and the magnetic induction is 1.85T.
Comparative example 4
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the compositions of the refined molten steel are shown in table 7:
TABLE 7 refining of molten steel composition of comparative example 4
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.23mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 620 ℃ to obtain a silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is spherical, the granularity D50 is 3.284 mu m, the granularity D50 of the titanium dioxide is 0.648 mu m as a pore filling agent, and the proportion is water: magnesium oxide: titanium dioxide = 900:100:10 The dosage of the high-temperature annealing isolating agent is 9.5g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1860mm.
(6) And (5) carrying out high-temperature annealing of the chamber furnace, wherein the gas flow of the chamber furnace is the outer ring inlet/outlet type atmosphere flow. The method comprises the steps of carrying out a first treatment on the surface of the The atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.5h, heating to 690 ℃, and keeping the temperature for 34h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape.
The oriented silicon steel prepared by the method. The crystal grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the comparative example 4, and partial crystal grains are smaller and have fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 1.080W/kg, and the magnetic induction is 1.86T.
Comparative example 5
A method of improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Molten iron of a blast furnace is subjected to KR desulfurization, converter and RH refining, and refined molten steel is obtained;
(2) Continuously casting the molten steel by a continuous casting machine to obtain a continuous casting blank, wherein the compositions of the refined molten steel are shown in table 8:
TABLE 8 refining of molten steel composition of comparative example 5
(3) Carrying out high-temperature heat treatment on the continuous casting blank, and carrying out hot rolling to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate, and the thickness of silicon steel is 0.27mm;
(5) And coating an annealing isolating agent on the secondary cold-rolled sheet, and drying and coiling at 650 ℃ to obtain the silicon steel coil.
Wherein the annealing separator comprises the following components: the magnesium oxide is spherical, the granularity D50 is 1.764 mu m, the granularity D50 of the titanium dioxide is 0.648 mu m as a pore filling agent, and the proportion is water: magnesium oxide: titanium dioxide = 900:100:10 The dosage of the high-temperature annealing isolating agent is 9.5g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outside diameter d 2 1940mm.
(6) Carrying out high-temperature annealing of a cover chamber furnace, wherein the air flow of the cover chamber furnace is the air flow of the inner ring inlet and outlet type; the atmosphere of the chamber furnace is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and heating process is as follows: 3.5h, heating to 690 ℃, and keeping the temperature for 37h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the heat is preserved for 7h, and the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) And after high-temperature annealing, coating an insulating layer on the surface of the plate, and finally carrying out leveling stretching annealing to adjust the plate shape. The oriented silicon steel prepared by the method.
The crystal grain observation is carried out on the silicon steel sheet in the middle of the steel coil prepared in the comparative example 5, and partial crystal grains are smaller and have fine crystals and broken crystals. The on-line iron loss of the silicon steel coil is 1.032W/kg, and the magnetic induction is 1.85T.
Test example:
the iron loss and magnetic induction of the silicon steels prepared in examples 1 to 3 and comparative examples 1 to 5 were tested by the method for detecting magnetic induction and iron loss described in GB/T13789-2008 method for measuring magnetic properties of electrical steels (tapes) by monolithic tester, and the results are shown in Table 9.
Table 9 results of performance tests for examples 1 to 3 and comparative examples 1 to 5
Sequence number Core loss P 17/50 (W/kg) Magnetic induction B 800 (T)
Example 1 0.964 1.89
Example 2 0.989 1.88
Example 3 0.952 1.89
Comparative example 1 1.058 1.85
Comparative example 2 1.069 1.84
Comparative example 3 1.072 1.85
Comparative example 4 1.080 1.86
Comparative example 5 1.069 1.85
As is clear from Table 9, in examples 1 to 3 of the present application, since the heat conduction efficiency was improved, the heat conduction thickness was reduced, and the uniformity of the overall temperature of the steel coil was good, the uniformity of the crystal grains in the steel coil was high, and defects such as fine crystals and broken crystals were not found. In comparative example 1, because the difference between the inner and outer diameters is large, the heat conduction is slow, fine crystals and broken crystals appear, and the uniformity of crystal grains is poor; in comparative example 2, since the heat preservation time is insufficient, the crystal grains are not fully grown, fine crystal grains are not phagocytized, and the uniformity of the crystal grains is poor; in comparative example 3, the high-temperature annealing isolating agent is used in a large amount, so that the outer diameter is large, the heat conduction efficiency is poor, the temperature of a steel coil is uneven, fine crystals and broken crystals appear, and the uniformity of crystal grains is poor; in comparative example 4, because the magnesium oxide and titanium dioxide particles in the high-temperature annealing isolating agent are larger, the heat conduction efficiency is poor, the temperature uniformity is affected, fine crystals and broken crystals appear, and the uniformity of the crystal grains is poor; comparative example 5 is heavy overall, has a large outer diameter and a large heat conduction thickness, causes uneven temperature, and has fine crystals and broken crystals, and poor uniformity of crystal grains. From the detection results, it can be seen that, because of the improvement of the uniformity of the crystal grains, the iron loss and the magnetic induction performance of the oriented silicon steel produced in the embodiments 1 to 3 are obviously better than those of the comparative examples 1 to 5, the average iron loss is reduced by 0.101W/kg, the number of marks is increased by about 2, and the average magnetic induction is improved by 0.033T.
FIGS. 1-3 show the middle roll grain for example 1 and comparative examples 1 and 4. As can be seen from the graph, the grain size is uniform in example 1 (FIG. 1), and no obvious fine or broken grains are generated; in comparative example 1 (fig. 2), there were a large number of fine crystals, and necklace-like crushed crystals were present around the larger crystal grains; in comparative example 4 (fig. 3), a part of fine crystals were also present, and linear crushed crystals were also present. The grain uniformity in example 1 is much better than that of comparative examples 1 and 4.
And taking a silicon steel sheet with a certain size, washing off the surface coating by adopting hydrochloric acid under the condition of heating in a water bath, counting the crystal grains in the silicon steel sheet, and calculating to obtain the number of the crystal grains in unit area. The heat conductivity coefficient is tested according to GB/T3651-2008 method for measuring high temperature coefficient of Heat conductivity of metals. Grain size and monolithic thermal conductivity of the silicon steels prepared in examples 1 to 3 and comparative examples 1 to 5 of the present application are shown in Table 10.
Table 10 comparison of the test data for examples 1 to 3 and comparative examples 1 to 5
Sequence number Grain size (units/m) 2 ) Monolithic thermal conductivity (W/m K)
Example 1 749 24.18
Example 2 734 32.74
Example 3 827 26.52
Comparative example 1 9465 25.56
Comparative example 2 4568 23.48
Comparative example 3 6842 17.61
Comparative example 4 5168 21.37
Comparative example 5 7612 29.81
As can be seen from Table 10, the silicon steel prepared in the comparative example has a grain number several times that of the comparative example in a unit area, which contains a large amount of fine grains and crushed grains, and has poor grain uniformity. And the silicon steel sheet coated with the high-temperature annealing isolating agent is subjected to thermal conductivity detection, the smaller the consumption of the high-temperature annealing isolating agent is, the larger the corresponding thermal conductivity is, the better the thermal conductivity is, and the smaller the difference between the inner coil diameter and the outer coil diameter is combined, so that the temperature uniformity of the steel coil is better.
The above-described embodiments are exemplary only and not limiting. The scope of the present application should be indicated by the appended claims rather than by the foregoing description, and all changes and modifications that come within the meaning and range of equivalency of the claims are intended to be embraced therein.

Claims (3)

1. A method for improving grain uniformity of oriented silicon steel, the method comprising the steps of:
(1) Desulfurizing molten iron, converter and refining to obtain molten steel;
(2) Continuously casting molten steel to obtain a continuous casting blank;
(3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting blank to obtain a hot rolled plate;
(4) The hot-rolled plate is subjected to acid washing, primary cold rolling, decarburization annealing and secondary cold rolling to obtain a secondary cold-rolled plate;
(5) Coating a high-temperature annealing isolating agent, and drying and coiling to obtain a silicon steel coil;
(6) Carrying out high-temperature annealing of the chamber covering furnace;
(7) After high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally performing leveling stretching annealing to adjust the plate shape;
in the step (5), the annealing isolating agent comprises the following components in proportion: magnesium oxide: titanium dioxide: mass ratio of sodium tetraborate = 900:100:10:0.5; the D50 particle size of the magnesium oxide is smaller than 2 mu m, and the D50 particle size of the titanium dioxide is smaller than 0.5 mu m;
in the step (5), the coating amount of the annealing separator is 8-10.0 g/m 2 ；
In the step (5), the inner diameter d of the silicon steel coil 1 700mm, outside diameter d 2 1850 to 190 mm;
in the step (1), the molten steel comprises the following components in percentage by mass: c: 0.03-0.06%, si: 2.90-3.25%, mn: 0.05-0.15%, P: less than or equal to 0.015 percent, S: 0.003-0.006%, al:0.025 to 0.050%, N: 0.008-0.011%, the balance being iron and unavoidable impurities;
in the step (6), the specific process of the high-temperature annealing is as follows: heating to 680-700 ℃ for 3-4 hours, preserving heat for t, heating to 880-900 ℃ at 10-13 ℃/h, preserving heat for 6-8 hours, and heating to 1180-1210 ℃ at 10-12 ℃/h;
the heat preservation time t meets the following relation:
a 0.5 +8lnb+1.2x<t< a 0.5 +6lnb+1.1x+1
wherein: t is the heat preservation time, h; a is d 2 -d 1 Mm; b is silicon steel thickness, mm; x is the coating quantity per unit area of the annealing separator, and g/m 2 。
2. An oriented silicon steel produced by the method of claim 1.
3. Use of the oriented silicon steel of claim 2 in transformer cores.
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