CN115044756A - Process method for improving adhesion of bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel - Google Patents

Process method for improving adhesion of bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel Download PDF

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CN115044756A
CN115044756A CN202210667644.0A CN202210667644A CN115044756A CN 115044756 A CN115044756 A CN 115044756A CN 202210667644 A CN202210667644 A CN 202210667644A CN 115044756 A CN115044756 A CN 115044756A
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annealing
temperature
plate
continuous casting
decarburization
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CN115044756B (en
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蔡子祥
闫成亮
王�琦
王强明
郝志奎
陈栋
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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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Abstract

The invention discloses a process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel, which comprises the following steps: (1) performing KR desulfurization, converter and RH refining on blast furnace molten iron, and continuously casting the refined molten steel by a continuous casting machine to obtain a continuous casting billet; (2) carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate; (3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate; (4) controlling the temperature, atmosphere and treatment time of the cold-rolled sheet, and performing decarburization annealing to obtain an annealed sheet; (5) coating a high-temperature annealing release agent on the annealing plate, and drying into coils; (6) carrying out high-temperature annealing; (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; according to the invention, the interface structure between the bottom layer and the iron substrate is adjusted by controlling the structure of the internal oxide layer of the Bi-containing steel, so that Bi escapes from the bottom layer at the early stage of the formation of the bottom layer or after the bottom layer is formed, thereby improving the bottom layer adhesiveness of the ultrahigh magnetic induction oriented silicon steel.

Description

Process method for improving adhesion of bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel
Technical Field
The invention relates to the technical field of oriented silicon steel manufacturing, in particular to a process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel.
Background
Oriented silicon steel is a soft magnetic material with excellent performance, is mainly used as an iron core of a transformer, and is an indispensable important soft magnetic alloy in the industries of electric power, electronics and military affairs. At present, with the rapid development of various industries in China, the electricity consumption in China is more and more, and the requirement on the transformer is higher and more. Oriented silicon steel is used as an important material in a transformer, and higher magnetic induction and lower iron loss are continuously pursued to improve the performance of the transformer. In 1994, the new-day iron banner factory firstly proposed that Bi is added into silicon steel, so that the magnetic induction can be obviously increased, and the iron loss can be reduced.
Bi is an element which is necessary to obtain the ultrahigh magnetic induction grain-oriented silicon steel, but once it is left in the matrix of the steel, the magnetic properties of the steel sheet are deteriorated. During or after the formation of the underlayer, Bi will escape from the steel in a gaseous or compound state. In the formation of the underlayer, when Bi forms a low-melting-point compound with the underlayer, the interface structure is easily smoothed, and adhesion of the underlayer is deteriorated.
Since part of Bi may be remained in the internal oxide having the pinning effect, the interface structure of the bottom layer is changed, and the area of the interface is increased. For general high magnetic induction oriented silicon steel products, the depth problem of the internal oxides is not considered, but the depth problem has great influence on ultrahigh magnetic induction oriented silicon steel. To ensure good high field core loss performance, it is important to ensure good adhesion of the underlayer, and to rationalize the structure between the underlayer and the iron substrate.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel. The interface structure between the bottom layer and the iron substrate is adjusted by controlling the structure of the internal oxidation layer of the Bi-containing steel, so that Bi escapes from the bottom layer at the early stage of the formation of the bottom layer or after the formation of the bottom layer is finished, and the adhesion of the bottom layer of the ultrahigh magnetic induction oriented silicon steel is improved.
The technical scheme of the invention is as follows:
a process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) performing KR desulfurization, converter and RH refining on blast furnace molten iron, and continuously casting the refined molten steel by a continuous casting machine to obtain a continuous casting billet;
the chemical components of the continuous casting slab comprise the following components in percentage by mass: c: 0.04 to 0.08, Si: 3.14 to 3.40, Mn: 0.06-0.12, S: 0.02 to 0.03, Als: 0.02-0.03, N: 0.006 to 0.010, Bi: 0.005 to 0.01, Sn: 0.01 to 0.06, and the balance of Fe and inevitable impurities.
(2) Carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) controlling the temperature, atmosphere and treatment time of the cold-rolled sheet, and performing decarburization annealing to obtain an annealed sheet; the carbon content in the annealed sheet is less than or equal to 30ppm, and the oxygen content is not more than 300 ppm.
The decarburization annealing temperature is 750-880 ℃, the dew point of the decarburization annealing is 55-80 ℃, and the oxidation degree PH is 2 O/PH 2 0.7 to 2.0, and the annealing time is 150 to 300 s.
Decarburization annealing in humidified H 2 And N 2 Under a mixed atmosphere of N 2 :H 2 The volume ratio is 1:4, heating is carried out at a heating rate of 100-200 ℃/s before 750 ℃, soaking is carried out for 1-20 s after the temperature reaches 750 ℃, and then decarburization annealing treatment is carried out.
(5) Coating a high-temperature annealing release agent on the annealing plate, and drying into coils; the single-side coating amount of the high-temperature annealing release agent is controlled to be 6-16 g/m 2 。
The preparation method of the high-temperature annealing separant comprises the following steps: firstly, adding TiO accounting for 10-20% of the total mass of magnesium oxide into water 2 And 5-10% of boric acid, stirring for 1h, adding a corresponding amount of MgO into the water, and continuously stirring for 1-3 h to obtain the magnesium oxide. The water content of the high-temperature annealing separant is 1.20-2.80%.
The single-side coating amount of the high-temperature annealing release agent satisfies the following relation:
2.5×(0.31e) 1/2 -15≤Y≤1.5×e 1/2 -10
wherein: y is the single-side magnesium oxide coating amount, g; and e is the oxygen content of the annealed sheet obtained by decarburization annealing, ppm.
(6) Carrying out high-temperature annealing in an annular furnace;
(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;
in the decarburization annealing process, the decarburization oxidation degree satisfies the following relationship:
2lna-24/b 1/2 -45/(c×d)-1.8≤X≤2.4lna-35/b 1/2 -58/(c×d)-0.8
wherein: x is the thickness of an oxide layer, and is mum; a is the Bi content, ppm; b is the temperature rise rate, DEG C/s; c is the decarburization dew point, DEG C; d is the decarburization oxidation degree.
The beneficial technical effects of the invention are as follows:
in the invention, Bi is released at the early stage of the formation of the bottom layer or after the formation of the bottom layer is finished, so that a low-melting-point compound cannot be formed, the interface of the bottom layer cannot be smoothened, the internal oxide has a pinning effect, and the adhesion of the bottom layer is good. According to the invention, the interface structure between the bottom layer and the iron matrix is adjusted by controlling the structure of the internal oxide layer of the Bi-containing steel, so that the adhesion of the bottom layer of the ultrahigh magnetic induction oriented silicon steel is improved.
According to the invention, the content of the reducing gas is regulated and controlled by controlling the nitrogen-hydrogen ratio in the decarburization line furnace, and the heating speed, soaking temperature and time in the furnace are regulated and controlled, so that the smooth formation of the surface oxide layer of the silicon steel at the initial stage of decarburization is ensured. The water vapor content in the furnace is regulated and controlled by controlling the dew point in the furnace, so that SiO formed on the surface of the silicon steel is ensured 2 The oxide layer is fine and uniform.
The invention ensures that the thickness of an oxide layer formed after decarburization annealing meets the formula by controlling the annealing temperature, the oxidation degree and the annealing time of the decarburization process: 2lna-24/b 1/2 -45/(c×d)-1.8≤X≤2.4lna-35/b 1/2 -58/(c x d) -0.8, so that the oxide layer is not too thick to affect the lamination factor and other properties, and the formation of the bottom layer is not affected by too thin.
The invention establishes a relation with the subsequent coating weight of magnesium oxide by detecting the oxygen content obtained by the decarburization coil, so that the formula is satisfied: 2.5X (0.31e) 1/2 -15≤Y≤1.5×e 1/2 10, proper amount of magnesium oxide and SiO in annealing release agent during high-temperature annealing 2 Generation of 2MgO + SiO 2 →Mg 2 SiO 4 The reaction can produce high quality bottom layer with good adhesion. The use of magnesium oxide is saved, and the production cost is reduced.
At present, the ultrahigh magnetic induction oriented silicon steel is difficult to generate an excellent bottom layer, so that the yield is low, the insulating property is poor, and the ultrahigh magnetic induction oriented silicon steel is not beneficial to being used in transformers and motors. On one hand, the yield of the ultrahigh magnetic induction oriented silicon steel is improved; on the other hand, the bottom layer adhesiveness of the ultrahigh magnetic induction oriented silicon steel is improved, and the yield of the product is reduced. The oriented silicon steel with ultrahigh magnetic induction can meet the use requirement of a high-capacity transformer.
Drawings
FIG. 1 shows the surface oxide layer morphology of example 8;
FIG. 2 shows the surface oxide layer morphology of comparative example 3;
FIG. 3 shows the cross-sectional oxide profile of example 8;
FIG. 4 shows the morphology of the cross-sectional oxide layer of comparative example 3.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.062%, Si: 3.26%, Mn: 0.09%, S: 0.026%, Al: 0.025%, N: 0.0082%, Bi: 0.0050%, Sn: 0.034%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere of N 2 :H 2 Is 1:4, is heated at a heating rate of 100 ℃/s before 750 ℃, is soaked for 5s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 750 ℃, the dew point of the decarburization annealing is 55 ℃, and the oxidation degree P is H2O /P H2 0.7, the annealing time is 150 s. The carbon content in the decarburized steel is 26ppm, the oxygen content is 211ppm, and an annealing plate is obtained;
(5) coating a high-temperature annealing release agent on the annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 10% of the total mass of magnesium oxide 2 And 5% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 1.24 percent, and the single-side coating amount of the release agent is controlled to be 6g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 2
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.065%, Si: 3.21%, Mn: 0.09%, S: 0.025%, Al: 0.024%, N: 0.0086%, Bi: 0.0060%, Sn: 0.036%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 135 ℃/s before 750 ℃, is soaked for 1s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 760 ℃, the dew point of the decarburization annealing is 58 ℃, and the oxidation degree P is H2O /P H2 0.8, the annealing time was 160 s. The carbon content in the decarburized steel is 25ppm, the oxygen content is 223ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 12% of the total mass of magnesium oxide 2 And 9% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 1.86 percent, and the single-side coating amount of the release agent is controlled to be 8g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 3
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.062%, Si: 3.20%, Mn: 0.08%, S: 0.027%, Al: 0.025%, N: 0.0087%, Bi: 0.0065%, Sn: 0.033%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 145 ℃/s before 750 ℃, is soaked for 12s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 780 ℃, the dew point of the decarburization annealing is 60 ℃, and the degree of oxidation P is H2O /P H2 0.9, the annealing time is 180 s. The carbon content in the decarburized steel is 24ppm, the oxygen content is 230ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 18% of the total mass of magnesium oxide 2 And 6% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 2.46 percent, and the single-side coating amount of the release agent is controlled to be 9g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 4
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.058%, Si: 3.21%, Mn: 0.09%, S: 0.026%, Al: 0.024%, N: 0.0082%, Bi: 0.0075%, Sn: 0.032%, and the balance of Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 160 ℃/s before 750 ℃, is soaked for 6s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 800 ℃, the dew point of the decarburization annealing is 65 ℃, and the oxidation degree P is H2O /P H2 The annealing time was 190s, 1.0. The carbon content in the decarburized steel is 23ppm, the oxygen content is 244ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 16% of the total mass of magnesium oxide 2 And 8% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 1.45 percent, and the single-side coating amount of the release agent is controlled to be 10g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 5
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.061%, Si: 3.22%, Mn: 0.09%, S: 0.029%, Al: 0.024%, N: 0.0088%, Bi: 0.0078%, Sn: 0.030%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 150 ℃/s before 750 ℃, is soaked for 15s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 830 ℃, the dew point of the decarburization annealing is 70 ℃, and the oxidation degree P is H2O /P H2 The annealing time was 200s, 1.2. The carbon content in the decarburized steel is 23ppm, the oxygen content is 257ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 15% of the total mass of magnesium oxide 2 And 7% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 1.73 percent, and the single-side coating amount of the release agent is controlled to be 12g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 6
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.058%, Si: 3.19%, Mn: 0.10%, S: 0.025%, Al: 0.023%, N: 0.0084%, Bi: 0.0085%, Sn: 0.032%, and the balance of Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 170 ℃/s before 750 ℃, is soaked for 20s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 850 ℃, the dew point of the decarburization annealing is 72 ℃, and the degree of oxidation P is H2O /P H2 The annealing time was 220s, 1.5. The carbon content in the decarburized steel is 22ppm, the oxygen content is 263ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 19% of the total mass of magnesium oxide 2 And 5.5% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 1.58 percent, and the single-side coating amount of the release agent is controlled to be 13g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 7
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.060%, Si: 3.22%, Mn: 0.09%, S: 0.026%, Al: 0.023%, N: 0.0088%, Bi: 0.0092%, Sn: 0.030%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 180 ℃/s before 750 ℃, is soaked for 8s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 870 ℃, the dew point of the decarburization annealing is 78 ℃, and the oxidation degree P is H2O /P H2 The annealing time was 280s, 1.8. The carbon content in the decarburized steel is 22ppm, the oxygen content is 274ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 13% of the total mass of magnesium oxide 2 And 8.5% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 1.86 percent, and the single-side coating amount of the release agent is controlled to be 14g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Example 8
A process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.063%, Si: 3.19%, Mn: 0.09%, S: 0.023%, Al: 0.025%, N: 0.0082%, Bi: 0.0100%, Sn: 0.032%, and the balance of Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 200 ℃/s before 750 ℃, is soaked for 10s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 880 ℃, the dew point of the decarburization annealing is 80 ℃, and the oxidation degree P is H2O /P H2 The annealing time was 300s, 2.0. The carbon content in the decarburized steel is 21ppm, the oxygen content is 289ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 20% of the total mass of magnesium oxide 2 And 10% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 2.37 percent, and the single-side coating amount of the release agent is controlled to be 15g/m 2 ；
(6) Annealing the annealing plate coated with the annealing release agent at high temperature in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Comparative example 1
A production method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.062%, Si: 3.18%, Mn: 0.10%, S: 0.025%, Al: 0.026%, N: 0.0084%, Bi: 0.0050%, Sn: 0.034%, the balance being Fe and unavoidable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:3, is heated at a heating rate of 90 ℃/s before 750 ℃, is soaked for 5s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 780 ℃, the dew point of the decarburization annealing is 55 ℃, and the degree of oxidation P is H2O /P H2 0.7, the annealing time is 150 s. The carbon content in the decarburized steel is 26ppm, the oxygen content is 206ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 10% of the total mass of magnesium oxide 2 And 5% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 2.08 percent, and the single-side coating amount of the release agent is controlled to be 6g/m 2 ；
(6) Carrying out high-temperature annealing on the silicon steel coated with the annealing separating agent in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flat stretching annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Comparative example 2
A production method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) blast furnace molten iron is subjected to KR desulfurization, converter and RH refining, and refined molten steel is continuously cast by a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.066%, Si: 3.18%, Mn: 0.09%, S: 0.026%, Al: 0.028%, N: 0.0087%, Bi: 0.0100%, Sn: 0.033% and the balance Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere of N 2 :H 2 Body ofHeating at a heating rate of 100 ℃/s before 750 ℃ at a volume ratio of 1:3, soaking for 0s after the temperature reaches 750 ℃, and then performing decarburization annealing treatment. The decarburization annealing temperature is 880 ℃, the dew point of the decarburization annealing is 75 ℃, and the oxidation degree P is H2O /P H2 0.7, the annealing time was 200 s. The carbon content in the decarburized steel is 25ppm, the oxygen content is 196ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 10% of the total mass of magnesium oxide 2 And 5% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 1.83 percent, and the single-side coating amount of the release agent is controlled to be 8g/m 2 ；
(6) Carrying out high-temperature annealing on the silicon steel coated with the annealing separating agent in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Comparative example 3
A production method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.064%, Si: 3.17%, Mn: 0.09%, S: 0.026%, Al: 0.025%, N: 0.0088%, Bi: 0.0060%, Sn: 0.031%, and the balance of Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:3, is heated at a heating rate of 150 ℃/s before 750 ℃, is soaked for 10s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 750 ℃,the dew point of decarburization annealing is 60 ℃, and the oxidation degree P is H2O /P H2 0.6, the annealing time is 160 s. The carbon content in the decarburized steel is 27ppm, the oxygen content is 201ppm, and an annealing plate is obtained;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 15% of the total mass of magnesium oxide 2 And 8% boric acid, water 8 times the mass of magnesium oxide. The water content of the magnesia release agent is 2.18 percent, and the single-side coating amount of the release agent is controlled to be 12g/m 2 ；
(6) Carrying out high-temperature annealing on the silicon steel coated with the annealing separating agent in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Comparative example 4
A production method for improving the adhesion of a bottom layer of Bi-containing ultrahigh-magnetic-induction oriented silicon steel comprises the following steps:
(1) KR desulfurization, converter and RH refining are carried out on blast furnace molten iron, and continuous casting is carried out on the refined molten steel through a continuous casting machine to obtain a continuous casting billet, wherein the continuous casting billet comprises the following chemical components in percentage by mass: c: 0.061%, Si: 3.19%, Mn: 0.09%, S: 0.027%, Al: 0.025%, N: 0.0085%, Bi: 0.0070%, Sn: 0.033% and the balance Fe and inevitable impurities;
(2) carrying out high-temperature heat treatment on the continuous casting billet at 1360 ℃, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) humidifying H of cold-rolled sheet 2 And N 2 Decarburization annealing is carried out in a mixed atmosphere, atmosphere N 2 :H 2 Is 1:4, is heated at a heating rate of 125 ℃/s before 750 ℃, is soaked for 5s after reaching 750 ℃, and then is subjected to decarburization annealing treatment. The decarburization annealing temperature is 800 ℃, the dew point of the decarburization annealing is 50 ℃, and the oxidation degree P is H2O /P H2 The annealing time was 170s, 1.0. The carbon content in the decarburized steel is 26ppm, and the oxygen content is 204ppm, obtaining an annealing plate;
(5) coating a treated high-temperature annealing release agent on an annealing plate, wherein the annealing release agent comprises the following components: magnesium oxide, TiO 16% of the total mass of magnesium oxide 2 And 7% boric acid, water mixed with 8 times of the mass of the magnesium oxide. The water content of the magnesia release agent is 2.12 percent, and the single-side coating amount of the release agent is controlled to be 14g/m 2 ；
(6) Carrying out high-temperature annealing on the silicon steel coated with the annealing separating agent in an annular furnace;
(7) and after high-temperature annealing, removing redundant MgO, coating an insulating layer on the surface of the plate, and finally performing flattening, stretching and annealing to adjust the plate shape. The thickness of the oxide layer and the finished product adhesion and magnetic properties are shown in Table 2.
Table 1 shows the specific process parameters of the above examples and comparative examples, and table 2 shows the results of the performance tests related to the corresponding examples and comparative examples.
TABLE 1
Figure BDA0003693460490000121
TABLE 2
Figure BDA0003693460490000122
Figure BDA0003693460490000131
The oxygen content in table 2 was measured using a LECO nitrogen oxygen analyzer; SiO 2 2 Observing the section of the decarburized coil silicon steel by adopting a scanning electron microscope according to the thickness of the oxidation layer, carrying out 5-position gauge length by using a self gauge length function of the scanning electron microscope, and calculating an arithmetic mean value of 5 results; the adhesion detection method refers to GB/T2522-2017 test method for insulation resistance and adhesion of coating of electrical steel strip (sheet); reference GB/T13789-
As can be seen from tables 1 and 2, the adhesion of the silicon steels produced in examples 1 to 8 of the present invention is significantly better than that of the silicon steels produced in comparative examples 1 to 4. Except that the adhesiveness is better than that of the comparative example, the magnetic induction intensity and the iron loss value of the silicon steel produced in the example are both better than those of the comparative example.
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 process method for improving the adhesion of a bottom layer of Bi-containing ultrahigh magnetic induction oriented silicon steel is characterized by comprising the following steps:
(1) performing KR desulfurization, converter and RH refining on blast furnace molten iron, and continuously casting the refined molten steel by a continuous casting machine to obtain a continuous casting billet;
(2) carrying out high-temperature heat treatment on the continuous casting billet, and carrying out hot rolling to obtain a hot rolled plate;
(3) the hot rolled plate is subjected to normalizing, acid cleaning and cold rolling to obtain a cold rolled plate;
(4) controlling the temperature, atmosphere and treatment time of the cold-rolled sheet, and performing decarburization annealing to obtain an annealed sheet;
(5) coating a high-temperature annealing release agent on the annealing plate, and drying into coils;
(6) carrying out high-temperature annealing;
(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;
in the decarburization annealing process, the decarburization oxidation degree satisfies the following relationship:
2lna-24/b 1/2 -45/(c×d)-1.8≤X≤2.4lna-35/b 1/2 -58/(c×d)-0.8
wherein: x is the thickness of an oxide layer, and is mum; a is the Bi content, ppm; b is the temperature rise rate, DEG C/s; c is the decarburization dew point, DEG C; d is the decarburization oxidation degree.
2. The process method as claimed in claim 1, wherein in the step (1), the chemical components of the continuous casting slab comprise the following components in percentage by mass: c: 0.04 to 0.08, Si: 3.14 to 3.40, Mn: 0.06-0.12, S: 0.02 to 0.03, Als: 0.02-0.03, N: 0.006 to 0.010, Bi: 0.005 to 0.01, Sn: 0.01 to 0.06, and the balance of Fe and inevitable impurities.
3. The process according to claim 1, wherein in the step (4), the decarburization annealing temperature is 750 to 880 ℃, the dew point of the decarburization annealing is 55 to 80 ℃, and the oxidation degree PH is 2 O/PH 2 0.7 to 2.0, and the annealing time is 150 to 300 s.
4. The process of claim 1, wherein in step (4), decarburization annealing is carried out on the humidified H 2 And N 2 Under a mixed atmosphere of N 2 :H 2 The volume ratio is 1:4, heating is carried out at a heating rate of 100-200 ℃/s before 750 ℃, soaking is carried out for 1-20 s after the temperature reaches 750 ℃, and then decarburization annealing treatment is carried out.
5. The process of claim 1, wherein in step (4), the carbon content of the annealed sheet is 30ppm or less and the oxygen content is not more than 300 ppm.
6. The process method as claimed in claim 1, wherein in the step (5), the preparation method of the high-temperature annealing release agent comprises the following steps: firstly, adding TiO accounting for 10-20% of the total mass of magnesium oxide into water 2 And 5-10% of boric acid, stirring for 1h, adding a corresponding amount of MgO into the water, and continuously stirring for 1-3 h to obtain the magnesium oxide.
7. The process method as claimed in claim 1, wherein in the step (5), the moisture content of the high-temperature annealing release agent is 1.20-2.80%.
8. The process of claim 1, wherein in step (5), the single-side coating amount of the high-temperature annealing separator satisfies the following relationship:
2.5×(0.31e) 1/2 -15≤Y≤1.5×e 1/2 -10
wherein: y is the single-side magnesium oxide coating amount, g; and e is the oxygen content of the annealed sheet obtained by decarburization annealing, ppm.
9. The process method as claimed in claim 8, wherein the single-side coating amount of the high-temperature annealing release agent is controlled to be 6-16 g/m 2 。
10. The process of claim 1, wherein in step (6), the high temperature annealing is performed in a ring furnace.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02305921A (en) * 1989-05-22 1990-12-19 Nippon Steel Corp Production of grain-oriented steel sheet having excellent magnetic characteristic
CN102758127A (en) * 2011-04-28 2012-10-31 宝山钢铁股份有限公司 Method for producing high magnetic induction orientation silicon steel with excellent magnetic performance and good bottom layer
DE102015114358A1 (en) * 2015-08-28 2017-03-02 Thyssenkrupp Electrical Steel Gmbh Method for producing a grain-oriented electrical strip and grain-oriented electrical strip
CN107779727A (en) * 2017-09-25 2018-03-09 北京首钢股份有限公司 A kind of production method of orientation silicon steel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02305921A (en) * 1989-05-22 1990-12-19 Nippon Steel Corp Production of grain-oriented steel sheet having excellent magnetic characteristic
CN102758127A (en) * 2011-04-28 2012-10-31 宝山钢铁股份有限公司 Method for producing high magnetic induction orientation silicon steel with excellent magnetic performance and good bottom layer
DE102015114358A1 (en) * 2015-08-28 2017-03-02 Thyssenkrupp Electrical Steel Gmbh Method for producing a grain-oriented electrical strip and grain-oriented electrical strip
CN107779727A (en) * 2017-09-25 2018-03-09 北京首钢股份有限公司 A kind of production method of orientation silicon steel

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