CN115505822A - 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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CN115505822A
CN115505822A CN202211165827.9A CN202211165827A CN115505822A CN 115505822 A CN115505822 A CN 115505822A CN 202211165827 A CN202211165827 A CN 202211165827A CN 115505822 A CN115505822 A CN 115505822A
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silicon steel
annealing
temperature
oriented silicon
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CN115505822B (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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    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
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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
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    • C—CHEMISTRY; METALLURGY
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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
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    • 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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    • 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
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract

The invention 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 comprises the following steps: (1) molten iron is desulfurized, converted and refined to obtain molten steel; (2) continuously casting molten steel to obtain a continuous casting billet; (3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting billet to obtain a hot rolled plate; (4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate; (5) Coating a high-temperature annealing release agent, and drying and coiling to obtain a silicon steel coil; (6) carrying out high-temperature annealing in a hood chamber furnace; (7) And after high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally, carrying out flattening, stretching and annealing to adjust the plate shape. The invention controls the grain size of the whole oriented silicon steel coil by limiting the internal and external diameter sizes of the oriented silicon steel coil, the annealing separant 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 invention relates to the technical field of oriented silicon steel manufacturing, in particular to a method for improving grain uniformity of oriented silicon steel and the 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 domestic and various industries, the demand of China on electric power is increasing. Because the coal resources of China are mainly distributed in the west and north regions, the water energy resources are mainly concentrated in the southwest region, and the primary energy resources in the eastern region are deficient and the electric loads are relatively concentrated. The imbalance between the energy resource and the distribution of the power load determines the necessity of the west-east power transmission. In the process of long-distance electric energy transmission, a transformer is indispensable, in the use process of the transformer, a certain electric energy can be consumed by an iron core, and the property of the electric energy consumed by the iron core per unit weight is called iron loss. The iron loss reduction has great significance to the national strategy of energy conservation and emission reduction.
The grain size of the oriented silicon steel is a main factor influencing the iron loss of the iron core, and the high-temperature annealing process in the production process of the oriented silicon steel plays a crucial role in the growth of secondary recrystallized grains. Gauss grains in the oriented silicon steel abnormally grow to reach the centimeter level in the process, but if the heating temperature and the heating time in the high-temperature annealing process do not meet the requirements, a large number of non-grown grains exist in the silicon steel, so that the iron loss is increased rapidly.
In production, because the silicon steel is easy to bond in the high-temperature annealing process, magnesium oxide and the like are used as high-temperature annealing separants to avoid direct contact between the silicon steel and the silicon steel. However, in the subsequent process of coating the insulating coating liquid, unreacted magnesium oxide can be removed by water washing and acid washing, so that the high-temperature annealing isolating agent used in the prior art is basically supersaturated to be used, the diameter of the general coil can reach 1800mm after the magnesium oxide is coated on the silicon steel coil, 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 overlarge difference between the inner and outer roll diameters makes the temperature conduction difficult, and forms a temperature field with high temperature of the inner and outer rolls and low temperature of the middle roll. Too much magnesium oxide will also increase the diameter of the coil, increase the difficulty of heat conduction in the coil, and also cause non-uniform temperature of the coil. The temperature of the silicon steel plays a vital role in abnormal growth of crystal grains, so that the temperature uniformity of the 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 performance can be produced. However, the research on the grain size at present focuses more on the selection and the dosage of the inhibitor in the steel, the desired grain size is obtained through the selective growth of the inhibitor, and the grain uniformity of the whole coil is rarely solved from the temperature field in the furnace in the high-temperature annealing process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for improving grain uniformity of oriented silicon steel and the oriented silicon steel prepared by the method. The invention controls the grain size of the whole oriented silicon steel coil by limiting the internal and external diameter sizes of the oriented silicon steel coil, the annealing separant 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 invention is as follows:
a method for improving grain uniformity of oriented silicon steel comprises the following steps:
(1) Molten iron is desulfurized by a KR method, and molten steel is obtained by a converter and an RH vacuum circulation degassing refining method;
(2) Continuously casting molten steel to obtain a continuous casting billet;
(3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting billet to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate;
(5) Coating a high-temperature annealing release agent, and drying and coiling to obtain a silicon steel coil;
(6) Performing high-temperature annealing in a hood chamber furnace;
(7) And after high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally, carrying out flattening, stretching and annealing to adjust the plate shape.
Further, in the step (1), the molten steel contains the following components by mass percent: c:0.03 to 0.06%, si:2.90 to 3.25%, mn:0.05 to 0.15%, P: less than or equal to 0.015%, S:0.003 to 0.006%, al:0.025 to 0.050%, N:0.008 to 0.011 percent, and the balance of iron and inevitable impurities.
Further, in the step (5), the annealing release agent comprises the following components in percentage by mass: magnesium oxide, titanium dioxide, sodium tetraborate; the magnesium oxide is spherical, the D50 particle size is less than 2 mu m, and the D50 particle size of the titanium dioxide is less than 0.5 mu m.
Further, in the step (5), the coating amount of the annealing release agent is 8-10.0 g/m 2 。
Further, in the step (5), the silicon steel coil is internally providedDiameter d 1 700mm, outer diameter d 2 Is 1850-1900 mm.
Further, in the step (6), the gas flow direction of the cover chamber furnace is from the outer ring to the inner ring of the silicon steel coil; the atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
Further, in the step (6), the specific process of the high-temperature annealing is as follows: firstly heating to 680-700 ℃ within 3-4 h, preserving heat for t, then heating to 880-900 ℃ at the speed of 10-13 ℃/h, preserving heat for 6-8 h, and then heating to 1180-1210 ℃ at the speed of 10-12 ℃/h.
Further, the heat preservation time t satisfies the following relational expression:
a 0.5 +8lnb+1.2x<t<a 0.5 +6lnb+1.1x+1
in the formula: t is the holding time h; a is d 2 -d 1 Mm; b is the thickness of silicon steel, mm; x is the coating amount per unit area of the annealing release agent, g/m 2 。
Further, the silicon steel thickness refers to a target thickness of the prepared silicon steel, and includes, but is not limited to, 0.23mm, 0.27mm.
An oriented silicon steel prepared by the method.
Further, the oriented silicon steel is applied to the iron core of the transformer.
The invention can control the grain size of the whole steel coil to be normal, reduce the occurrence of grain abnormality and improve the uniformity of the grain by limiting the inner and outer diameter sizes of the steel coil, the annealing separant and the high-temperature annealing process.
The granularity of the annealing release agent is too large, the gap is large after coating, and the flatness is reduced; the granularity is too small, the hydration rate is too high, a large amount of water vapor can be generated in the high-temperature annealing stage, the water vapor is not easy to discharge in a high-tension and compact steel coil, the reaction can be influenced, the plate surface can be influenced, the watermark appears on the plate surface, the chromatic aberration is caused, and the attractiveness is reduced. The invention optimizes the high-temperature annealing separant, reduces the granularity of magnesium oxide and titanium dioxide, and increases sodium tetraborate. The reduction of the granularity of the magnesium oxide and the titanium dioxide improves the bulk density after coating and reduces air gaps in the middle of the separant. The smaller granularity is beneficial to the rapid reaction, the stacking density is increased, the thickness of the high-temperature annealing separant is favorably reduced, 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 influenced, the air gap is reduced and reduced, the heat conduction efficiency is improved, the heat conductivity is improved, the uniformity of the temperature of the steel plate is further improved, and a good environment is provided for full and uniform growth of finished product crystal grains.
The invention changes the flow direction of furnace gas flow in the cover chamber, the side cover and the furnace bottom of the furnace in the cover chamber are heated by resistance belts, the heating area of the outer ring of the steel coil is large, the heating area is also large, and the heating mode of inner ring in and outer ring out is adopted, so that the heat of the resistance belt of the side cover is not completely transferred to the steel coil by the gas and is taken out.
The invention starts from a circumference formula, and on the premise of unchanging coil weight, the heat conduction thickness is reduced by a method of increasing the inner diameter by a larger amplitude and increasing the outer diameter by a smaller amplitude, and the increase of the outer diameter thickness does not exceed the inner cover and does not generate negative influence on gas flow; the adjustment of the inner diameter and the outer diameter of the steel coil leads the integral number of turns to be reduced, the interface generated by two different media of magnesium oxide and silicon steel is reduced, the heat conduction difficulty can be reduced, the improvement of the heat conduction efficiency is facilitated, and the integral temperature uniformity of the steel coil is improved.
According to the invention, the secondary cold-rolled sheet is fully recovered and recrystallized by limiting the heat preservation time, and the obtained primary recrystallized grains are fine, so that a good foundation is provided for fully and uniformly growing the finished product grains.
The beneficial technical effects of the invention are as follows:
(1) According to the invention, the granularity of magnesium oxide and titanium dioxide is reduced by optimizing the high-temperature annealing separant, and the generation of a magnesium silicate glass film is promoted by adding the sodium tetraborate additive. The optimized high-temperature annealing separant 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 invention adopts the silicon steel coil with large coil diameter and reduces the use of the high-temperature annealing release agent, thereby reducing the heat conduction thickness, shortening the temperature rise time in the annealing stage and ensuring the smooth growth of secondary recrystallized grains; meanwhile, the annealing release agent is reduced, the heating time is shortened, and the energy and the production cost are saved.
(3) The invention adopts the mode of outer ring feeding and inner ring discharging, so that the heat can be fully conducted to the steel coil.
(4) According to the method, 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 magnesium oxide in unit area, the growth of crystal grains is completely ensured, fine grains and broken grains are eliminated, through the cooperative optimization of the process and the auxiliary agent in the preparation of the silicon steel, the grain distribution of the oriented silicon steel prepared by the method is uniform, the size of the crystal grains 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.
Drawings
FIG. 1 is a graph of the grain morphology in the coil of example 1 of the present invention.
Fig. 2 is the grain morphology in the volume of comparative example 1.
Fig. 3 is the grain morphology in the roll of comparative example 4.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
A method of improving grain uniformity in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) Continuously casting molten steel by a continuous casting machine to obtain a continuous casting billet, wherein the components of the refined molten steel are shown in table 1:
table 1 molten steel composition of example 1 refining
Figure BDA0003861938350000041
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying and coiling at 600 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: the heat-conducting magnesium oxide, titanium dioxide and sodium tetraborate, wherein the magnesium oxide is spherical, the granularity D50 is 1.742 mu m, the granularity D50 of the titanium dioxide is 0.384 mu m, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are used as pore fillers, and the mixture ratio is that water: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 9.4g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 Is 1850mm.
(6) Performing high-temperature annealing in a cover chamber furnace, wherein the airflow of the cover chamber furnace flows in an outer ring-in and inner ring-out type atmosphere; the atmosphere of the hood chamber furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rising process comprises the following steps: heating to 680 ℃ within 3.5h, and keeping the temperature t for 33h; then the temperature is raised to 880 ℃ at the speed of 10 ℃/h, the temperature is kept for 6h, and then the temperature is raised to 1190 ℃ at the speed of 10 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An 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 embodiment 1, the grain size is normal, and no fine grains or broken grains exist. The online 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron, and refining to obtain refined molten steel;
(2) Continuously casting molten steel by a continuous casting machine to obtain a continuous casting billet, wherein the components of the refined molten steel are shown in table 2:
table 2 example 2 molten steel composition of refining
Figure BDA0003861938350000051
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.27mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying at 620 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent 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, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are taken as pore fillers, and the proportion is as follows: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 8.5g/m 2 Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 Is 1900mm.
(6) And (4) carrying out high-temperature annealing in a cover chamber furnace, wherein the airflow of the cover chamber furnace flows in an outer ring-in and inner ring-out type atmosphere. (ii) a The atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rising process comprises the following steps: heating to 700 ℃ for 4h, and keeping the temperature for 36h; then the temperature is raised to 900 ℃ at the speed of 13 ℃/h, the temperature is preserved for 8h, and then the temperature is raised to 1210 ℃ at the speed of 12 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An 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 embodiment 2, the grain size is normal, and no fine grains or broken grains exist. The online 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 3:
TABLE 3 molten steel composition of example 3 refining
Figure BDA0003861938350000061
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying at 620 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: the heat-conducting magnesium oxide, titanium dioxide and sodium tetraborate, wherein 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, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are used as pore fillers, and the mixture ratio is water: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 9.2g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 Is 1880mm.
(6) Carrying out high-temperature annealing in a cover chamber furnace, wherein the air flow of the cover chamber furnace is in outer ring-in and inner ring-out type atmosphere flow; the atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rise process comprises the following steps: heating to 690 ℃ within 3.8h, and keeping the temperature for 36h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. An 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 embodiment 3, the grain size is normal, and no fine grains or broken grains exist. 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 4:
TABLE 4 molten steel composition refined in comparative example 1
Figure BDA0003861938350000071
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(5) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(6) And coating an annealing release agent on the secondary cold-rolled sheet, and drying and coiling at 600 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: the magnesium oxide is rod-shaped, the granularity D50 is 1.764 mu m, the granularity D50 of the titanium dioxide is 0.369 mu m, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are taken as pore fillers, and the proportion of the magnesium oxide to the titanium dioxide is as follows: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 9.3g/m 2 . Inner diameter d of silicon steel coil 1 520mm, outer diameter d 2 Is 1800mm. (6) And carrying out high-temperature annealing in a cover chamber furnace, wherein the air flow of the cover chamber furnace is in outer ring-in and inner ring-out type atmosphere flow. (ii) a The atmosphere of the hood chamber furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rise process comprises the following steps: heating to 690 ℃ within 3.8h, and keeping the temperature t for 37h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An oriented silicon steel prepared by the method.
And (3) observing the crystal grains of the silicon steel sheet in the middle of the steel coil prepared in the comparative example 1, wherein part of the crystal grains are small and fine crystals and broken crystals exist. 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 5:
TABLE 5 molten steel composition refined in comparative example 2
Figure BDA0003861938350000081
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying and coiling at 580 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent 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 titanium dioxide particles are spherical, the granularity D50 is 0.342 mu m, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are used as pore fillers, and the mixture ratio is that water: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 9.3g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 1870mm.
(6) Carrying out high-temperature annealing in a cover chamber furnace, wherein the air flow of the cover chamber furnace is in outer ring-in and inner ring-out type atmosphere flow; the atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rising process comprises the following steps: heating to 690 ℃ in 3.5h, and keeping the temperature for 30h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An oriented silicon steel prepared by the method.
And (3) observing the crystal grains of the silicon steel sheet in the middle of the steel coil prepared in the comparative example 2, wherein part of the crystal grains are small and fine grains and crushed grains exist. The online 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 6:
TABLE 6 molten steel composition refined in comparative example 3
Figure BDA0003861938350000091
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying and coiling at 660 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: the heat-conducting magnesium oxide, titanium dioxide and sodium tetraborate, wherein 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, and the magnesium oxide, the titanium dioxide and the sodium tetraborate are used as pore fillers, and the mixture ratio is that water: magnesium oxide: titanium dioxide: sodium tetraborate =900:100:10:0.5 (mass ratio), the dosage of the high-temperature annealing release agent is 12.6g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 Is 1920mm. (6) Performing high-temperature annealing in a cover chamber furnace, wherein the airflow of the cover chamber furnace flows in an outer ring-in and inner ring-out type atmosphere; of furnace with mantle chamberThe atmosphere is a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rising process comprises the following steps: heating to 690 ℃ within 3.5h, and keeping the temperature t for 40h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An oriented silicon steel prepared by the method.
And (3) observing the crystal grains of the silicon steel sheet in the middle of the steel coil prepared in the comparative example 3, wherein part of the crystal grains are small and fine crystals and broken crystals exist. 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 7:
TABLE 7 composition of molten steel refined in comparative example 4
Figure BDA0003861938350000101
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.23mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying at 620 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: the magnesium oxide and the titanium dioxide are in a spherical shape, the granularity D50 of the magnesium oxide is 3.284 mu m, the granularity D50 of the titanium dioxide is 0.648 mu m, and the magnesium oxide and the titanium dioxide are taken as pore fillers, and the mixture ratio is as follows: magnesium oxide: titanium dioxide =900:100:10 (mass ratio), the dosage of the high-temperature annealing release agent is 9.5g/m 2 . Inner of silicon steel coilDiameter d 1 700mm, outer diameter d 2 1860mm.
(6) And carrying out high-temperature annealing in a cover chamber furnace, wherein the air flow of the cover chamber furnace is in outer ring-in and inner ring-out type atmosphere flow. (ii) a The atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rise process comprises the following steps: heating to 690 ℃ within 3.5h, and keeping the temperature t for 34h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape.
An oriented silicon steel prepared by the method. And (3) observing the crystal grains of the silicon steel sheet in the middle of the steel coil prepared in the comparative example 4, wherein part of the crystal grains are small and fine crystals and broken crystals exist. The online 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 in oriented silicon steel, the method comprising the steps of:
(1) Performing KR desulfurization, converter and RH refining on blast furnace molten iron, and refining to obtain refined molten steel;
(2) The molten steel was continuously cast by a continuous casting machine to obtain a continuous cast slab, wherein the composition of the refined molten steel is shown in table 8:
TABLE 8 composition of molten steel refined in comparative example 5
Figure BDA0003861938350000102
(3) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate, wherein the thickness of the silicon steel is 0.27mm;
(5) And coating an annealing release agent on the secondary cold-rolled sheet, and drying and coiling at 650 ℃ to obtain the silicon steel coil.
Wherein the annealing release agent comprises the following components: thermal conductive magnesium oxide and titanium dioxide, wherein the magnesium oxide is spherical, the granularity D50 is 1.764 mu m, and the granularity D50 of the titanium dioxide is 0.648 mu mm is used as a pore filler, and the mixture ratio is water: magnesium oxide: titanium dioxide =900:100:10 (mass ratio), the dosage of the high-temperature annealing release agent is 9.5g/m 2 . Inner diameter d of silicon steel coil 1 700mm, outer diameter d 2 Is 1940mm.
(6) Carrying out high-temperature annealing in a hood chamber furnace, wherein the gas flow in the hood chamber flows in an atmosphere with an inner ring entering and an outer ring exiting; the atmosphere of the mantle furnace was a mixed atmosphere of hydrogen and nitrogen.
The high-temperature annealing and temperature rise process comprises the following steps: heating to 690 ℃ within 3.5h, and keeping the temperature t for 37h; then the temperature is raised to 890 ℃ at the speed of 11 ℃/h, the temperature is preserved for 7h, and then the temperature is raised to 1200 ℃ at the speed of 11 ℃/h.
(7) After high-temperature annealing, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. An oriented silicon steel prepared by the method.
And (3) observing the crystal grains of the silicon steel sheet in the middle of the steel coil prepared in the comparative example 5, wherein part of the crystal grains are small and fine crystals and broken crystals exist. The online iron loss of the silicon steel coil is 1.032W/kg, and the magnetic induction is 1.85T.
Test example:
the iron loss and the magnetic induction of the silicon steels prepared in examples 1 to 3 and comparative examples 1 to 5 were measured by the method for detecting the magnetic induction and the iron loss described in GB/T13789-2008 "method for measuring magnetic properties of electrical steel (strip) using a single-piece tester", and the results are shown in table 9.
TABLE 9 results of performance test of examples 1 to 3 and comparative examples 1 to 5
Serial number Iron 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 can be seen from table 9, in the embodiments 1 to 3 of the present invention, since the heat conduction efficiency is improved, the heat conduction thickness is reduced, and the overall temperature uniformity of the steel coil is good, the uniformity of the crystal grains in the steel coil is high, and the defects of fine grains, broken grains, and the like are not found. Comparative example 1 has poor uniformity of crystal grains due to large difference between the diameters of the inner and outer coils, slow heat conduction, and occurrence of fine crystals and crushed crystals; comparative example 2 because the holding time is insufficient, the crystal grains are not completely grown, fine crystal grains are not phagocytized, and the uniformity of the crystal grains is poor; comparative example 3 because the high temperature annealing release agent dosage is large, the outer diameter is large, the heat conduction efficiency is poor, the steel coil temperature is not uniform, fine grains and broken grains occur, and the grain uniformity is poor; comparative example 4 because the high temperature annealing separant has larger magnesium oxide and titanium dioxide particles, the heat conduction efficiency is poor, the temperature uniformity is influenced, fine grains and crushed grains occur, and the grain uniformity is poor; comparative example 5 has a heavy overall, a large outer diameter, a large heat conduction thickness, resulting in uneven temperature, occurrence of fine grains, crushed grains, and poor uniformity of grains. It can also be seen from the detection results that, because of the improvement of the uniformity of the crystal grains, the oriented silicon steel produced in the embodiments 1 to 3 of the invention has significantly better loss and magnetic induction performance than the comparative examples 1 to 5, the iron loss is averagely reduced by 0.101W/kg, the number of the iron loss is improved by about 2, and the magnetic induction is averagely improved by 0.033T.
FIGS. 1 to 3 show the condition of the crystal grains in the middle of the coil in example 1 and comparative examples 1 and 4. As can be seen, the crystal grains in example 1 (FIG. 1) are uniform in size and have no obvious fine crystals or broken crystals; in comparative example 1 (fig. 2), a large amount of fine crystals were present, and necklace-like crushed crystals were present around the larger crystal grains; in comparative example 4 (FIG. 3), there were also partial fine crystals and linear crushed crystals. The grain uniformity in example 1 is much better than in comparative examples 1, 4.
Taking a silicon steel sheet with a certain size, washing off the surface coating by hydrochloric acid under the water bath heating condition, counting the number of grains in the silicon steel sheet, and calculating to obtain the number of the grains in unit area. The heat conductivity coefficient is tested according to GB/T3651-2008 'measuring method for metal high temperature heat conductivity coefficient'. The grain sizes and the single-piece heat transfer coefficients of the silicon steels prepared in examples 1 to 3 according to the present invention and comparative examples 1 to 5 are shown in table 10.
TABLE 10 comparison of the test data of examples 1 to 3 and comparative examples 1 to 5
Serial number Grain size (pieces/m) 2 ) Monolithic Heat conduction coefficient (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, it can be seen from the grain sizes that the number of grains of the silicon steel prepared in the comparative example is several times that of the silicon steel prepared in the example, a large amount of fine grains and crushed grains are included, and the uniformity of the grains is poor. The silicon steel sheet coated with the high-temperature annealing release agent is subjected to heat conduction coefficient detection, the amount of the high-temperature annealing release agent is less, the corresponding heat conduction coefficient is larger, the heat conductivity is better, the inner and outer coil diameter difference is smaller in combination, and the temperature uniformity of a steel coil is better.
The above embodiments are exemplary only and not limiting. The scope of the present invention is defined by the appended claims rather than 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 (10)

1. A method of improving grain uniformity in oriented silicon steel, the method comprising the steps of:
(1) Molten iron is desulfurized, converted and refined to obtain molten steel;
(2) Continuously casting molten steel to obtain a continuous casting billet;
(3) Carrying out high-temperature heat treatment and hot rolling on the continuous casting billet to obtain a hot rolled plate;
(4) Carrying out acid pickling, primary cold rolling, decarburization annealing and secondary cold rolling on the hot rolled plate to obtain a secondary cold rolled plate;
(5) Coating a high-temperature annealing release agent, and drying and coiling to obtain a silicon steel coil;
(6) Carrying out high-temperature annealing in a hood chamber furnace;
(7) And after high-temperature annealing, coating an insulating layer on the surface of the steel plate, and finally performing smooth stretching annealing to adjust the plate shape.
2. The method according to claim 1, wherein in the step (1), the molten steel contains the following components by mass percent: c:0.03 to 0.06%, si:2.90 to 3.25%, mn:0.05 to 0.15%, P: less than or equal to 0.015%, S:0.003 to 0.006%, al:0.025 to 0.050%, N:0.008 to 0.011 percent, and the balance of iron and inevitable impurities.
3. The method according to claim 1, wherein in the step (5), the annealing separator comprises the following components in percentage by mass: magnesium oxide, titanium dioxide, sodium tetraborate; the D50 particle size of the magnesium oxide is less than 2 μm, and the D50 particle size of the titanium dioxide is less than 0.5 μm.
4. The method according to claim 1, wherein the annealing separator is coated in an amount of 8 to 10.0g/m in the step (5) 2 。
5. The method according to claim 1, wherein in the step (5), the inner diameter d of the silicon steel coil 1 700mm, outer diameter d 2 Is 1850-1900 mm.
6. The method of claim 1, wherein in step (6), the direction of the gas flow in the enclosure furnace is from the outer coil to the inner coil of the silicon steel coil.
7. The method according to claim 1, wherein in the step (6), the specific process of the high-temperature annealing is as follows: firstly heating to 680-700 ℃ within 3-4 h, preserving heat for t, then heating to 880-900 ℃ at the speed of 10-13 ℃/h, preserving heat for 6-8 h, and then heating to 1180-1210 ℃ at the speed of 10-12 ℃/h.
8. The method according to claim 7, wherein the incubation time t satisfies the following relation:
a 0.5 +8lnb+1.2x<t<a 0.5 +6lnb+1.1x+1
in the formula: t is the holding time h; a is d 2 -d 1 Mm; b is the thickness of silicon steel, mm; x is the coating amount per unit area of the annealing release agent, g/m 2 。
9. An oriented silicon steel prepared by the method of claims 1-8.
10. Use of the oriented silicon steel of claim 9 in a transformer core.
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