WO2016045157A1 - 一种取向高硅钢的制备方法 - Google Patents

一种取向高硅钢的制备方法 Download PDF

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WO2016045157A1
WO2016045157A1 PCT/CN2014/088887 CN2014088887W WO2016045157A1 WO 2016045157 A1 WO2016045157 A1 WO 2016045157A1 CN 2014088887 W CN2014088887 W CN 2014088887W WO 2016045157 A1 WO2016045157 A1 WO 2016045157A1
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temperature
rolling
cold
rolled
silicon steel
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PCT/CN2014/088887
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English (en)
French (fr)
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王国栋
张元祥
王洋
卢翔
方烽
曹光明
李成刚
许云波
刘振宇
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东北大学
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Priority to EP14902512.4A priority Critical patent/EP3118336B1/en
Priority to US15/027,368 priority patent/US10032548B2/en
Priority to JP2016515529A priority patent/JP6208855B2/ja
Publication of WO2016045157A1 publication Critical patent/WO2016045157A1/zh

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
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    • H01F1/14766—Fe-Si based alloys
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    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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Definitions

  • the invention belongs to the technical field of metallurgy, and in particular relates to a preparation method of oriented high silicon steel.
  • High silicon steel generally refers to a Si-Fe alloy with a silicon content of 4.5 to 6.5%, but a 6.5% Si-Fe alloy has a magnetic permeability ⁇ s of approximately 0, and has high magnetic permeability, low coercivity, and low iron loss, especially The low frequency of high-frequency iron loss makes it an ideal soft magnetic alloy material; however, when the Si content is increased to 4.5% or more, the elongation of the alloy drops sharply, and the room temperature elongation of 6.5% of the Si-Fe alloy is almost 0.
  • High-silicon steel has become a hotspot in the research of magnetic materials in recent years.
  • the research direction focuses on the formation of ordered phase of non-oriented high-silicon steel and the reasons for explaining the brittleness of room temperature and the improvement measures. Europe, Russia and Japan have adjusted the alloy.
  • Oriented silicon steel obtains a single Goss texture by secondary recrystallization, has excellent magnetic properties with extremely high magnetic sensation and low iron loss along the rolling direction, and is mainly used for iron core of various transformers;
  • Si content of conventional oriented silicon steel is 2.8 ⁇ 3.4%, this Si content of Goss single crystal theoretical saturation magnetic induction Bs ⁇ 2.03T, B8 value can directly reflect the saturation magnetic induction strength of oriented silicon steel sheet, Hi-B (high magnetic induction) oriented silicon steel B 8 at 1.90 ⁇ 1.96T Between 0.936 ⁇ B 8 /B s ⁇ 0.966, it is the highest grade of oriented silicon steel.
  • Oriented high-silicon steel has a higher maximum magnetic permeability, higher resistivity, lower high-frequency iron loss, can be significantly reduced
  • the quality and volume of electrical components improve electrical efficiency.
  • 6.5% Si-Fe alloy saturated magnetic induction strength Bm1.80T
  • the preparation of oriented high-silicon steel also needs to solve a large number of process difficulties.
  • both oriented and non-oriented high-silicon steels need to solve the problem of matrix plasticity.
  • the conditions for suppressing the high-silicon steel to achieve perfect secondary recrystallization are also more stringent, so the following factors clearly affect the preparation of oriented high-silicon steel:
  • Si element can significantly improve the grain boundary migration ability of Fe-Si alloy and coarsen the grain, which causes the grain size of high Si steel slab to be very coarse, reaching the level of several tens of mm, which is very unfavorable for plasticity;
  • the necessary condition for satisfying the occurrence of secondary recrystallization is that the primary recrystallized grain growth of the strip is strongly inhibited, and the increase of the grain boundary migration rate after the cold rolling deformation of the high Si steel requires a stronger inhibitor;
  • the inhibitor may be a compound (such as an S compound and an N compound) or a simple substance (such as Cu, Sn, B, etc.), but the former requires high temperature solid solution and phase change precipitation control, and high temperature heating of the cast slab causes the crystal grain to be excessive. Coarsening, while high silicon steel is a single phase ferrite, there is no phase change window to control the fine precipitation of the N compound. However, elemental compounds are often used as auxiliary inhibitors, and the inhibitory power alone is insufficient, and it is easy to solid-solution strengthen the matrix and affect plasticity.
  • Oriented high-silicon steel was prepared by a conventional process, and only a small number of Japanese patents have been reported.
  • Sumitomo Metals No. 63-069917, 089622 patents obtained a 0.2-0.3 mm strip by hot-rolling-warm-cold rolling through a 50 mm thick slab.
  • the silicon infiltration method also has problems in the preparation of high silicon oriented silicon steel. It is mentioned that the diffusion annealing process after the non-oriented large amount of Si penetrates into the steel strip promotes grain growth, and the grain boundary migration in oriented silicon steel The reduction in the degree of orientation, or even the destruction of the original secondary recrystallized structure, ultimately failed to obtain good magnetic properties. There is no report on the magnetic sensation in the published research results.
  • the twin-roll strip casting technology uses a rotating two casting rolls as a crystallizer to directly inject liquid steel water into a molten pool composed of a casting roll and a side sealing plate.
  • the liquid steel directly solidifies into a thin strip having a thickness of 1 to 6 mm. It needs to go through continuous casting, heating, hot rolling and normalization.
  • the process characteristic is that the liquid metal undergoes pressure processing and plastic deformation while crystallizing and solidifying, and completes the whole process from liquid metal to solid strip in a short time, and the solidification speed can reach 10 2 to 10 4 ° C/s, which is greatly Refine the solidified grain size of high silicon steel.
  • thin strip continuous casting has unique advantages in the production of high-silicon Fe-Si alloys; in this respect, Sumitomo Metals of Japan has had related patent reports, and they have been strengthened by 1 to 2 mm thin strip continuous casting-cold rolling-high temperature annealing.
  • the Goss secondary recrystallized structure however, their understanding of thin strip continuous casting has limitations, the direct cold rolling of the cast strip is not high, and the inhibitor's ability to suppress is relatively weak, and high magnetic induction oriented high silicon steel is not obtained.
  • the present invention provides a preparation method of oriented high silicon steel, which is based on a system of texture-precipitation in the sub-rapid solidification process of high-silicon steel twin-roll strip casting. Understand and design the inhibitor program, through the casting belt grain solidification-growth behavior control and inhibitor element solid solution precipitation behavior design, realize the tissue-texture-precipitation flexible control, and obtain high magnetic induction oriented high silicon steel.
  • the preparation method of the oriented high silicon steel of the present invention is carried out as follows:
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1200 ⁇ 1250°C, the superheat degree is controlled to 20 ⁇ 50°C, and the molten steel enters the thin strip continuous casting machine through the tundish to form the casting belt. , the thickness is between 1.8 and 3.0 mm;
  • the hot-rolled strip is cooled to a temperature of 20 to 30 ° C / s to 550 ⁇ 600 ° C coiling, and then under low temperature hot rolling / warm rolling under nitrogen atmosphere, rolling temperature 760 ⁇ 5 ° C, finishing rolling
  • the temperature is 550-600 ° C, and the total reduction is 70-80%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then the multi-pass cold rolling is carried out at 100-200 ° C, the total reduction is 60-80%, and the aging treatment is carried out 2 to 3 times in the cold rolling process, and the aging treatment temperature is performed. It is 280-320 ° C, the time is 240-300 s, and each aging treatment is between the adjacent two passes of cold rolling to obtain a cold-rolled strip;
  • the cold-rolled strip is recrystallized and annealed at 850 ⁇ 10 °C for 120-180 s.
  • the re-crystallization annealing is carried out under a nitrogen-hydrogen mixed atmosphere, and the dew point of the mixed atmosphere is controlled at 30-60 ° C. Then coating the MgO coating and finally coiling to obtain a coated cold rolled strip;
  • the surface of the cold-rolled strip after purification and annealing is surface-cleaned to remove the scale, and then the insulating layer is coated, then flat-stretched and annealed at 800 ⁇ 10°C, and finally air-cooled to 650°C or less to obtain oriented high-silicon steel. .
  • the above oriented high silicon steel has a thickness of 0.10 to 0.25 mm.
  • the volume concentration of hydrogen in the nitrogen-hydrogen mixed atmosphere is 30%.
  • the molten steel enters the strip casting machine through the tundish, and a molten pool is formed in the crystallizer consisting of the rotating casting rolls and the side sealing plates and solidified.
  • Control method of inhibitor in matrix S and N in the inhibitor element are solid solution elements, and when N ⁇ 100ppm in the conventional process, it is easy to cause defects such as foaming, but the thin strip continuous casting process can significantly improve the solidification of N. Solubility; the amount of solid solution in the matrix is directly related to the supercooling of the molten steel during solidification. During the sub-rapid solidification process, the Si element increases and the solid-liquidus line decreases, so the solid solution dissolves more S and N elements due to the cooling rate. Faster (10 2 ⁇ 10 3 °C / s), so that the two are evenly distributed.
  • MnS and (Al, V, Nb) N series of second phase particles can strongly inhibit the growth behavior of primary grains during heating, in order to obtain uniform, developed and oriented
  • the accurate Goss grains provide a stable matrix, and after the secondary recrystallization is completed, the pure H 2 can be purified and annealed, and the S and N elements are discharged from the matrix, so that Mn, Al, V, and Nb exist only in a solid solution form.
  • (V, Nb) C is decomposed, and most of C elements are taken off to form (V, Nb).
  • N decomposes during high temperature annealing and acts as a nucleation point of AlN particles, and further promotes the precipitation of AlN particles. AlN cooperates with MnS as a composite inhibitor, and continues to maintain the matrix inhibition force so that secondary recrystallization occurs at a higher temperature, resulting in high orientation. Goss secondary grains to improve magnetic properties;
  • Hi-B oriented high silicon steel can be realized.
  • a second phase particle of 10 to 60 nm and uniform distribution is formed as an inhibitor in stages, which strongly hinders high silicon steel.
  • the initial recrystallization of the matrix progresses.
  • the high temperature annealing temperature increases, the accurate Goss grains in the matrix grow abnormally and develop into a perfect secondary recrystallized structure.
  • the iron loss value reaches or is close to the level reported in Japanese patents.
  • the comprehensive control ability of the inhibition force is improved, and it is convenient to prepare a high-profile silicon steel with a thin gauge of 0.10 to 0.25 mm, thereby obtaining a lower iron loss.
  • FIG. 1 is a schematic flow chart of a method for preparing an oriented high silicon steel according to the present invention
  • Figure 2 is a microscopic micrograph of the product of Example 3 of the present invention.
  • Example 3 is a macroscopic structural diagram of a cold rolled strip after recrystallization annealing in Example 3 of the present invention
  • Fig. 4 is a microscopic micrograph of a cast strip in Example 3 of the present invention; in the figure, MnS particles having a size of 20 to 200 nm are precipitated.
  • the thin strip continuous casting machine used in the embodiment of the present invention is a thin strip continuous casting machine disclosed in the patent CN103551532A.
  • the preparation method of the high silicon steel based on the strip casting technology is as shown in FIG. 1 : the molten steel is poured into the tundish through the ladle, and flows into the thin strip continuous casting machine through the cloth nozzle, in two rotations.
  • a molten pool is formed in a crystallizer consisting of a copper crystallization roll and a side seal plate, and the molten steel is solidified to form a cast strip; after one hot rolling, the coil is taken; the hot rolled strip is subjected to low temperature hot rolling and warm rolling under a protective atmosphere, followed by After pickling and cold rolling; after the cold rolling is completed, the initial recrystallization annealing and MgO are applied, and then the high temperature annealing process is performed; after the high temperature annealing, the steel coil is subjected to the insulating coating and the stretching and flattening, and the stretching is completed after the drawing is completed.
  • the observed microstructure in the examples of the present invention was performed by a Zeiss Ultra 55 type scanning electron microscope.
  • the purity of hydrogen used in the examples of the present invention was 99.9%.
  • the purity of the nitrogen gas used in the examples of the present invention was 99.9%.
  • the molten steel is smelted according to the set composition, and its composition contains C0.001%, Si6.6%, Mn0.2%, Al0.12%, V0.01%, Nb0.06%, S0.02%, N0. 020%, O0.0016%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1200 ° C, the superheat degree is controlled to 20 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 2.0 mm;
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1000 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1000 ° C, the final rolling temperature is 900 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1000 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1000 ° C, the final rolling temperature is 900 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1000 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1000 ° C, the final rolling temperature is 900 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled
  • the hot-rolled strip is cooled to 580 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 580 ° C.
  • the total reduction is 70%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 6 times at 100-200 ° C, the total reduction is 80%, and the aging treatment is performed twice in the cold rolling process, and the aging treatment temperature is 280 ° C for the time 300s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.10mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 °C for 120 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere to control the dew point of the mixed atmosphere at 30 ° C, and then coated with MgO coating. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1240 ° C at a rate of 30-40 ° C / h, and kept for 20 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.18 W/kg
  • the magnetic property P 10/400 is 6.75 W/kg
  • the magnetic induction B 8 is 1.74 T
  • B 8 /B S 0.961.
  • the molten steel is smelted according to the set composition, and its composition contains C0.003%, Si5.0%, Mn0.3%, Al0.05%, V0.04%, Nb0.03%, S0.03%, N0. 009%, O0.0018%, the balance is Fe and inevitable impurities;
  • Thin strip continuous casting process the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1250 ° C, the superheat degree is controlled to 50 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 2.3mm;
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 10%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 10%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 10%.
  • Hot rolled cast strip After casting and taking out the
  • the hot-rolled strip is cooled to 600 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 600 ° C.
  • the total reduction is 70%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 7 times at 100-200 ° C, the total reduction is 60%, and the aging treatment is carried out 3 times in the cold rolling process, and the aging treatment temperature is 320 ° C, the time is 240s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.25mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 180 s.
  • the cold rolled strip was in nitrogen hydrogen
  • the dew point of the mixed atmosphere is controlled at 40 ° C, then the MgO coating is applied, and finally coiled to obtain a cold rolled strip of the coating;
  • the volume concentration of hydrogen in the mixed atmosphere of nitrogen and hydrogen is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1220 ° C at a rate of 30-40 ° C / h, and kept for 30 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.62 W/kg
  • the magnetic property P 10/400 is 9.5 W/kg
  • the magnetic induction B 8 is 1.81 T
  • B 8 /B S 0.978.
  • the molten steel is smelted according to the set composition, and its composition contains C0.002%, Si6.5%, Mn0.23%, Al0.08%, V0.02%, Nb0.05%, S0.026%, N0. 018%, O0.0011%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1210 ° C, the superheat degree is controlled to 30 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 1.8mm;
  • Hot rolled cast strip After the casting is taken out of the roll, it is cooled to 1030 ° C at an inert gas atmosphere at a rate of 50 to 100 ° C / s, and then hot rolled, the rolling temperature is 1030 ° C, the final rolling temperature is 940 ° C, and the reduction is 13%. Hot rolled cast strip
  • the hot-rolled strip is cooled to 550 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 550 ° C.
  • the total reduction is 70%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 5 times at 100-200 ° C, the total reduction is 62%, and the aging treatment is carried out twice in the cold rolling process, and the aging treatment temperature is 320 ° C for the time 240s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.18mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 160 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere to control the dew point of the mixed atmosphere at 50 ° C, and then coated with MgO coating. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1230 ° C at a rate of 30-40 ° C / h, and kept for 24 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.22 W/kg
  • the magnetic property P 10/400 is 7.1 W/kg
  • the magnetic induction B 8 is 1.76 T
  • B 8 /B S 0.966.
  • the molten steel is smelted according to the set composition, and its composition contains C0.001%, Si5.8%, Mn0.29%, Al0.10%, V0.03%, Nb0.06%, S0.02%, N0. 015%, O0.0017%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1220 ° C, the superheat degree is controlled to 40 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 3.0mm;
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the
  • the hot-rolled strip is cooled to 570 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 570 ° C.
  • the total reduction is 80%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 6 times at 100-200 ° C, the total reduction is 70%, and the aging treatment is carried out 3 times in the cold rolling process, and the aging treatment temperature is 280 ° C, the time is 300s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.15mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 140 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere.
  • the dew point of the mixed atmosphere was controlled at 60 ° C, and then the MgO coating was applied. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1240 ° C at a rate of 30-40 ° C / h, and kept for 20 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.34 W/kg
  • the magnetic property P 10/400 is 7.4 W/kg
  • the magnetic induction B 8 is 1.77 T
  • B 8 /B S is 0.975.
  • the molten steel is smelted according to the set composition, and its composition contains C0.003%, Si5.2%, Mn0.27%, Al0.06%, V0.04%, Nb0.04%, S0.028%, N0. 014%, O0.0018%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1230 ° C, the superheat degree is controlled to 40 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 2.5mm;
  • Hot rolled cast strip After the casting is taken out of the roll, it is cooled to 1000 ° C at an inert gas atmosphere at a rate of 50 to 100 ° C / s, and then hot rolled, the rolling temperature is 1000 ° C, the final rolling temperature is 900 ° C, and the reduction is 12%. Hot rolled cast strip
  • the hot-rolled strip is cooled to 580 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 580 ° C.
  • the total reduction is 75%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 7 times at 100-200 ° C, the total reduction is 67%, and the aging treatment is carried out twice in the cold rolling process, and the aging treatment temperature is 300 ° C, the time is 280s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.18mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 180 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere to control the dew point of the mixed atmosphere at 30 ° C, and then coated with MgO coating. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1220 ° C at a rate of 30-40 ° C / h, and kept for 30 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.43 W/kg
  • the magnetic property P 10/400 is 8.2 W/kg
  • the magnetic induction B 8 is 1.76 T
  • B 8 /B S 0.965.
  • the molten steel is smelted according to the set composition, and its composition contains C0.002%, Si6.1%, Mn0.3%, Al0.07%, V0.01%, Nb0.05%, S0.026%, N0. 020%, O0.0012%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1250 ° C, the superheat degree is controlled to 50 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; the thickness is 2.8 mm;
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1030 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1030 ° C, the final rolling temperature is 940 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1030 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1030 ° C, the final rolling temperature is 940 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1030 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1030 ° C, the final rolling temperature is 940 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the
  • the hot-rolled strip is cooled to 560 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 560 ° C.
  • the total reduction is 75%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 5 times at 100-200 ° C, the total reduction is 80%, and the aging treatment is performed 3 times in the cold rolling process, and the aging treatment temperature is 300 ° C, the time is 300s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.12mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 160 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere to control the dew point of the mixed atmosphere at 40 ° C, and then coated with MgO coating. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1230 ° C at a rate of 30-40 ° C / h, and kept for 24 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.29 W/kg
  • the magnetic property P 10/400 is 7.5 W/kg
  • the magnetic induction B 8 is 1.74 T
  • B 8 /B S 0.973.
  • the molten steel is smelted according to the set composition, and its composition contains C0.001%, Si5.5%, Mn0.22%, Al0.11%, V0.02%, Nb0.05%, S0.03%, N0. 010%, O0.0018%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1200 ° C, the superheat degree is controlled to 20 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 3.0mm;
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the roll, it is cooled to 1050 ° C at an inert gas atmosphere at a rate of 50-100 ° C / s, and then hot-rolled, the rolling temperature is 1050 ° C, the final rolling temperature is 980 ° C, and the reduction is 15%.
  • Hot rolled cast strip After casting and taking out the
  • the hot-rolled strip is cooled to 600 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 600 ° C.
  • the total reduction is 70%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then cold rolling is performed 6 times at 100-200 ° C, the total reduction is 76%, and the aging treatment is performed twice in the cold rolling process, and the aging treatment temperature is 280 ° C for the time 280s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.18mm;
  • the cold-rolled strip was recrystallized and annealed at 850 ⁇ 10 ° C for 140 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere to control the dew point of the mixed atmosphere at 50 ° C, and then coated with MgO coating. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1240 ° C at a rate of 30-40 ° C / h, and kept for 20 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.49 W/kg
  • the magnetic property P 10/400 is 7.8 W/kg
  • the magnetic induction B 8 is 1.77 T
  • B 8 /B S 0.968.
  • the molten steel is smelted according to the set composition, and its composition contains C0.003%, Si5.8%, Mn0.29%, and Al0.06% by weight. V0.03%, Nb0.05%, S0.021%, N0.017%, O0.0016%, the balance is Fe and inevitable impurities;
  • the molten steel enters the tundish through the gate, the preheating temperature of the tundish is 1220 ° C, the superheat degree is controlled to 30 ° C, the molten steel enters the thin strip continuous casting machine through the tundish, and the rotating casting rolls and side sealing plates Forming a molten pool in the crystallizer and solidifying; thickness is 1.8mm;
  • Hot rolled cast strip After the casting is taken out of the roll, it is cooled to 1000 ° C at an inert gas atmosphere at a rate of 50 to 100 ° C / s, and then hot rolled, the rolling temperature is 1000 ° C, the final rolling temperature is 900 ° C, and the reduction is 10%. Hot rolled cast strip
  • the hot-rolled strip is cooled to 550 ° C at a rate of 20 to 30 ° C / s, and then subjected to low temperature hot rolling / warm rolling under a nitrogen atmosphere, the rolling temperature is 760 ⁇ 5 ° C, and the final rolling temperature is 550 ° C.
  • the total reduction is 70%, and the temperature is rolled;
  • the hot rolling is pickled to remove the scale, and then 7 times cold rolling is performed at 100-200 ° C, the total reduction is 70%, and the aging treatment is carried out 3 times in the cold rolling process, and the aging treatment temperature is 320 ° C, the time is 240s, each aging treatment is between two adjacent cold rolling, obtaining a cold-rolled strip with a thickness of 0.15mm;
  • the cold-rolled strip was recrystallized at 850 ⁇ 10 °C for 120 s.
  • the re-crystallization annealing was carried out under a nitrogen-hydrogen mixed atmosphere.
  • the dew point of the mixed atmosphere was controlled at 60 ° C, and then the MgO coating was applied. , finally coiling, obtaining a coated cold-rolled strip; the volume concentration of hydrogen in a nitrogen-hydrogen mixed atmosphere is 30%;
  • the cold-rolled strip of the coating is placed in a ring furnace at 400 ⁇ 10 ° C, and the temperature is raised to 1000 ⁇ 10 ° C at a rate of 30 to 40 ° C / h under the condition of hydrogen flow, and then 10 to 20 ° C / h.
  • the temperature is raised to 1130 ⁇ 10 ° C, and then heated to 1220 ° C at a rate of 30-40 ° C / h, and kept for 30 h for purification annealing;
  • the surface of the cold-rolled strip after purification and annealing is subjected to surface cleaning to remove the scale, and then the insulating layer is coated, and then subjected to flat tensile annealing at 800 ⁇ 10° C., and finally air-cooled to 650° C. or less to obtain oriented high-silicon steel, magnetic
  • the energy P 10/50 is 0.37 W/kg
  • the magnetic property P 10/400 is 7.2 W/kg
  • the magnetic induction B 8 is 1.75 T
  • B 8 /B S 0.970.

Abstract

一种取向高硅钢的制备方法，按以下步骤进行：（1）按设定成分冶炼钢水，其成分按重量百分比含C 0.001~0.003%，Si5.0~6.6%，Mn0.2~0.3%，Al0.05~0.12%，V0.01~0.04%，Nb0.03~0.06%，S0.02~0.03%，N0.009~0.020%，O≤0.0020%，余量为Fe及不可避免杂质；（2）薄带连铸过程后形成铸带；（3）在惰性气氛条件下进行热轧；（4）冷却至550~600℃卷取，在氮气气氛条件下进行低温热轧/温轧；（5）酸洗去除氧化皮，然后进行多道次冷轧；（6）再结晶退火，涂覆MgO涂层，最后卷取；（7）在氢气流通的条件下，进行净化退火；（8）去除氧化铁皮，涂覆绝缘层，平整拉伸退火，空冷卷取。

Description

一种取向高硅钢的制备方法 技术领域
本发明属于冶金技术领域，特别涉及一种取向高硅钢的制备方法。
背景技术
高硅钢一般指硅含量在4.5～6.5％的Si-Fe合金，但是6.5％Si-Fe合金由于其磁致伸缩λs近似为0，而且具有高导磁率，低矫顽力，低铁损尤其是高频铁损较低的特点，使其成为非常理想的软磁合金材料；但是当Si含量提高到4.5％以上时，合金延伸率急剧下降，6.5％的Si-Fe合金的室温延伸率几乎为0。
高硅钢成为近年来磁性材料研究的热点，研究的方向多集中在无取向高硅钢有序相形成规律和解释其室温脆性的原因以及改善措施这一方向上；欧洲、俄罗斯和日本都有通过调整合金成分，优化设计热轧-温轧-冷轧流程实现轧制6.5％Si无取向硅钢的报道；北京科技大学利用B等元素细化铸态组织，阻止DO3长程有序相形成从而提高板带低温塑性(CN1560309A)。在高硅钢的深入研究及工业化方向，日本也走在前列：他们综合研究了合金元素Ni、Al、Mn等对6.5％Si成型性能的改善；以及调控轧制过程对成型性的影响，提出低温热轧获得纤维织构以便于更低温度变形的思想(Takada Y,Journal of Applied Physics,1988,64,5367～5369)；更有学者提出薄带快淬的办法获得0.55mm甚至更薄的高硅微晶带解决脆性问题(Arai K.I,Journal of Applied Physics,1988,64,5373～5375)。
综合来看，这些通过成分和轧制变形得到6.5％Si电工钢的办法可以一定程度上解决无取向高硅钢轧制成型的难题，而薄带快淬法制备的微晶薄带宽度和厚度有限，几乎很难实现工业规模的生产；真正把6.5％Si无取向产品推向实用化的是日本钢管公司，他们采用化学气相沉积快速渗硅法(CVD)法和轧制法制成0.1～0.5mm规格6.5％Si-Fe合金(Haiji H.Journal of Magnetism and Magnetic Materials,1996,160,109～114)，称为“Super Ecore”，利用3％Si无取向电工钢成品进行渗硅处理，渗硅后采用高温热处理均匀化并促进晶粒长大，获得磁性能良好的6.5％Si无取向电工钢。
取向硅钢通过二次再结晶获得单一Goss织构，具有沿轧制方向具有极高的磁感和低铁损的优良磁性能，主要用于各种变压器的铁芯；常规取向硅钢Si含量2.8～3.4％，这个Si含量的Goss单晶理论饱和磁感Bs≈2.03T，B8值可以直观反映取向硅钢片的饱和磁感强度，Hi-B(高磁感)取向硅钢B8在1.90～1.96T之间，0.936≤B8/Bs≤0.966，是取向硅钢中最高等级的产品。
取向高硅钢具有更高的最大磁导率，更高的电阻率，更低的高频铁损值，能够显著降低 电器元件的质量和体积，提高电器效率，特别是6.5％Si-Fe合金(饱和磁感强度Bm1.80T)磁致伸缩几乎为0，能够显著降低高频变压器的噪音，具有极高的应用价值；但是取向高硅钢的制备也需要解决大量工艺难点，一方面，取向和无取向高硅钢都需要解决基体塑性问题。另一方面，满足发生高硅钢获得完善二次再结晶所需要的抑制剂条件也更加严格，所以下列因素显然影响了取向高硅钢的制备：
1)Si元素能够显著提高Fe-Si合金晶界迁移能力，粗化晶粒，这就造成高Si钢铸坯晶粒尺寸非常粗大，达到几十mm的级别，对于塑性非常不利；
2)满足二次再结晶发生的必要条件是带钢初次再结晶晶粒生长受到强烈抑制，而高Si钢冷轧变形后晶界迁移速率提高需要更强的抑制剂；
3)抑制剂可以是化合物(如S化物和N化物等)或者单质(如Cu、Sn、B等)，但是前者需要高温固溶和相变析出来控制，高温加热铸坯会造成晶粒过于粗化，而高硅钢是单相铁素体，没有相变窗口来控制N化物的细小析出。而单质化合物往往作为辅助抑制剂使用，单独使用抑制力不足，还容易固溶强化基体，影响塑性。
通过常规流程制备取向高硅钢，仅有少量日本专利做了一定的报道，住友金属昭63-069917、089622专利通过50mm厚的铸坯经过热轧-温轧-冷轧得到0.2～0.3mm板带，通过单一的MnS、AlN、TiC或者VC作为抑制剂，得到了6.5％Si取向硅钢，但是由于抑制剂的抑制力不足，二次再结晶取向度不高，B8/BS＝1.65T/1.80T＝0.916；而新日铁公司认识到抑制力不足的问题，通过渗氮的办法提高AlN的量，但是磁感B8仅提升到1.67T(平4-080321,224625)；显然，这种这两种方法并没有突破常规流程的制约。
另外，渗硅的办法在制备高硅取向硅钢方面也存在问题，前面提到在无取向大量Si深入钢带后的扩散退火过程会促进晶粒长大，在取向硅钢中这种晶界迁移会造成取向度的降低，甚至破坏原本完善的二次再结晶组织，最终无法得到良好的磁性能，目前公布的研究结果中也没有关于磁感的报道。
双辊薄带连铸技术，以转动的两个铸辊为结晶器，将液态钢水直接注入铸辊和侧封板组成的熔池内，由液态钢水直接凝固成形厚度为1～6mm薄带，可不需经过连铸、加热、热轧和常化等生产工序。其工艺特点是液态金属在结晶凝固的同时承受压力加工和塑性变形，在很短的时间内完成从液态金属到固态薄带的全部过程，凝固速度可达102～104℃/s，大大细化高硅钢凝固晶粒尺寸。因此，薄带连铸在生产高硅Fe-Si合金方面具有独特的优势；在这方面，日本住友金属曾有相关专利报道，他们通过1～2mm薄带连铸-冷轧-高温退火获得强的Goss二次再结晶组织；但是他们对于薄带连铸的认识存在局限性，铸带直接冷轧成材率不高， 而且抑制剂的抑制能力比较弱，没有得到高磁感取向高硅钢。
发明内容
针对现有取向高硅钢在制备方法上存在的上述问题，本发明提供一种取向高硅钢的制备方法，基于对高硅钢双辊薄带连铸亚快速凝固过程中组织-织构-析出的系统认识，设计抑制剂方案，通过铸带晶粒凝固-长大行为控制和抑制剂元素固溶析出行为设计，实现组织-织构-析出柔性控制，得到高磁感取向高硅钢。
本发明的取向高硅钢的制备方法按以下步骤进行：
1、按设定成分冶炼钢水，其成分按重量百分比含C0.001～0.003％，Si5.0～6.6％，Mn0.2～0.3％，Al0.05～0.12％，V0.01～0.04％，Nb0.03～0.06％，S0.02～0.03％，N0.009～0.020％，O≤0.0020％，余量为Fe及不可避免杂质；
2、薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1200～1250℃，控制过热度为20～50℃，钢水通过中间包进入薄带连铸机后形成铸带，厚度在1.8～3.0mm；
3、铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1000～1050℃，然后进行热轧，开轧温度1000～1050℃，终轧温度900～980℃，压下量10～15％，制成热轧铸带；
4、将热轧铸带以20～30℃/s的速率冷却至550～600℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度550～600℃，总压下量70～80％，制成温轧带；
5、将温轧带酸洗去除氧化皮，然后在100～200℃进行多道次冷轧，总压下量为60～80％，冷轧过程中进行2～3次时效处理，时效处理温度为280～320℃，时间为240～300s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带；
6、将冷轧带在850±10℃进行再结晶退火，时间为120～180s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在30～60℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；
7、将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1220～1240℃，保温20～30h进行净化退火；
8、将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢。
上述的取向高硅钢的厚度为0.10～0.25mm。
上述方法中，所述的氮气氢气混合气氛中氢气的体积浓度为30％。
上述方法中，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形。
上述的取向高硅钢的磁性能为：P10/50在0.18～0.62W/kg，P10/400在6.75～9.5W/kg，磁感B8在1.74～1.81T，B8/BS＝0.961～0.978。
本发明在国家自然科学基金项目(U1260204；51174059)资助下完成，创新性体现在以下几点：
1、将铸带中C元素量降低到30ppm以下的水平，消除C元素偏聚形成Fe3C后对塑性的不利影响，并且省去高温退火前的脱碳流程，大大简化初次再结晶工艺难度；
2、通过对Mn，S，Al、V、Nb尤其是N元素的固溶，强烈阻止DO3相的长程有序化对塑性的影响，而且间隙原子N能够显著增加晶内剪切变形提高基体塑性变形能力；
3、基体中抑制剂的控制方法：抑制剂元素中S、N是固溶元素，而且常规流程中N≥100ppm时，容易造成起泡等缺陷，但是薄带连铸流程可以明显提高N的固溶量；基体中固溶量与凝固时钢液过冷有直接关系，亚快速凝固过程中Si元素增加，固液相线降低，所以以固溶更多量的S和N元素，由于冷却速度较快(102～103℃/s)，使二者均匀分布。
4、钢液凝固过程中有部分20～200nm尺寸的MnS粒子析出，明显阻碍铸带凝固后的晶界迁移行为，大大细化了铸带晶粒，提高了高硅钢铸带的低温成型性能，这是薄带连铸过程独有的特点；
5、采用可分解的化合物作为抑制剂，例如MnS和(Al，V，Nb)N系列第二相粒子在升温过程中可以强烈抑制初次晶粒的长大行为，为获得均匀、发达且位向准确的Goss晶粒提供稳定基体，而且在二次再结晶完成后可以通过纯H2进行净化退火，将S、N元素排出基体，使Mn、Al，V，Nb仅仅以固溶的形式存在于基体中，避免类似TiN等化合物分解温度过高造成大量残留，也可以避免B等晶界偏聚元素在基体中的不均分布造成反相畴界能提高造成的矫顽力增加，从而降低磁化过程中矫顽力使得铁损降低；
6、复合抑制剂分阶段抑制策略：低温热轧和温轧阶段N元素和基体中残存的C元素形成(V，Nb)C和少量(V，Nb)N，抑制热轧过程中回复和再结晶，形成纤维组织提高基体塑性也细化晶粒，为二次再结晶提供稳定基体，初次再结晶过程中(V，Nb)C分解，C元素大部分被脱掉，形成(V，Nb)N，高温退火过程中分解并且作为AlN粒子形核质点，并且进一步促进AlN粒子的析出，AlN配合MnS作为复合抑制剂，继续保持基体抑制力使得二次再结晶发生在较高温度，产生高取向度Goss二次晶粒，提高磁性能；
7、Hi-B取向高硅钢得以实现，常规流程中3％Si取向硅钢通过抑制剂的设计可以提高 抑制力得到磁感B8值在1.90以上称为Hi-B取向硅钢，其磁感值与理论饱和磁感值的比值B8/Bs：1.90/2.03＝0.94，在另一方面，在初次再结晶组织中分阶段形成10～60nm且分布均匀的第二相粒子作为抑制剂，强烈阻碍高硅钢基体初次再结晶的进行，随着高温退火温度升高，基体中位向准确的Goss晶粒发生异常长大，发展成完善的二次再结晶组织，铁损值达到或接近日本专利报道水平，B8值达到1.74T以上，B8/BS＝1.74T/1.80T＝0.967，远超过日本专利报道磁感水平；
8、抑制力综合调控能力提高，便于制备薄规格0.10～0.25mm取向高硅钢，从而获得更低的铁损。
附图说明
图1为本发明的取向高硅钢的制备方法流程示意图；
图2为本发明实施例3中的产品的微观组织显微图；
图3为本发明实施例3中的冷轧带再结晶退火后的宏观组织图；
图4为本发明实施例3中的铸带的微观组织显微图；图中可见20～200nm尺寸的MnS粒子析出。
具体实施方式
本发明实施例中采用的薄带连铸机为专利CN103551532A公开的薄带连铸机。
本发明实施例中基于薄带连铸技术取向高硅钢的制备方法流程如图1所示：通过钢包冶炼钢水浇入中间包内，经过布流水口流入薄带连铸机，在两个旋转的铜结晶辊和侧封板组成的结晶器内形成熔池，钢水凝固后形成铸带；经过一道次热轧后进行卷取；热轧带在保护气氛下进行低温热轧和温轧，随后进行酸洗冷轧；冷轧完成后进行初次再结晶退火和涂MgO，然后进入高温退火过程；高温退火后，钢卷进行绝缘涂层和拉伸平整，拉伸平整完成后卷取。
本发明实施例中观测显微组织采用Zeiss Ultra55型扫描电镜。
本发明实施例中采用的氢气的纯度为99.9％。
本发明实施例中采用的氮气的纯度为99.9％。
实施例1
按设定成分冶炼钢水，其成分按重量百分比含C0.001％，Si6.6％，Mn0.2％，Al0.12％，V0.01％，Nb0.06％，S0.02％，N0.020％，O0.0016％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1200℃，控制过热度为20℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在2.0mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1000℃，然后进行热轧，开轧温度1000℃，终轧温度900℃，压下量15％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至580℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度580℃，总压下量70％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行6道次冷轧，总压下量为80％，冷轧过程中进行2次时效处理，时效处理温度为280℃，时间为300s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.10mm；
将冷轧带在850±10℃进行再结晶退火，时间为120s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在30℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1240℃，保温20h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.18W/kg，磁性能P10/400为6.75W/kg，磁感B8为1.74T，B8/BS＝0.961。
实施例2
按设定成分冶炼钢水，其成分按重量百分比含C0.003％，Si5.0％，Mn0.3％，Al0.05％，V0.04％，Nb0.03％，S0.03％，N0.009％，O0.0018％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1250℃，控制过热度为50℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在2.3mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1050℃，然后进行热轧，开轧温度1050℃，终轧温度980℃，压下量10％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至600℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度600℃，总压下量70％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行7道次冷轧，总压下量为60％，冷轧过程中进行3次时效处理，时效处理温度为320℃，时间为240s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.25mm；
将冷轧带在850±10℃进行再结晶退火，时间为180s，再结晶退火时冷轧带是在氮气氢 气混合气氛条件下进行，控制混合气氛的露点在40℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1220℃，保温30h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.62W/kg，磁性能P10/400为9.5W/kg，磁感B8为1.81T，B8/BS＝0.978。
实施例3
按设定成分冶炼钢水，其成分按重量百分比含C0.002％，Si6.5％，Mn0.23％，Al0.08％，V0.02％，Nb0.05％，S0.026％，N0.018％，O0.0011％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1210℃，控制过热度为30℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在1.8mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1030℃，然后进行热轧，开轧温度1030℃，终轧温度940℃，压下量13％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至550℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度550℃，总压下量70％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行5道次冷轧，总压下量为62％，冷轧过程中进行2次时效处理，时效处理温度为320℃，时间为240s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.18mm；
将冷轧带在850±10℃进行再结晶退火，时间为160s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在50℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1230℃，保温24h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.22W/kg，磁性能P10/400为7.1W/kg，磁感B8为1.76T，B8/BS＝0.966。
实施例4
按设定成分冶炼钢水，其成分按重量百分比含C0.001％，Si5.8％，Mn0.29％，Al0.10％，V0.03％，Nb0.06％，S0.02％，N0.015％，O0.0017％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1220℃，控制过热度为40℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在3.0mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1050℃，然后进行热轧，开轧温度1050℃，终轧温度980℃，压下量15％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至570℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度570℃，总压下量80％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行6道次冷轧，总压下量为70％，冷轧过程中进行3次时效处理，时效处理温度为280℃，时间为300s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.15mm；
将冷轧带在850±10℃进行再结晶退火，时间为140s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在60℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1240℃，保温20h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.34W/kg，磁性能P10/400为7.4W/kg，磁感B8为1.77T，B8/BS＝0.975。
实施例5
按设定成分冶炼钢水，其成分按重量百分比含C0.003％，Si5.2％，Mn0.27％，Al0.06％，V0.04％，Nb0.04％，S0.028％，N0.014％，O0.0018％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1230℃，控制过热度为40℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在2.5mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1000℃，然后进行热轧，开轧温度1000℃，终轧温度900℃，压下量12％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至580℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度580℃，总压下量75％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行7道次冷轧，总压下量为67％，冷轧过程中进行2次时效处理，时效处理温度为300℃，时间为280s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.18mm；
将冷轧带在850±10℃进行再结晶退火，时间为180s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在30℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1220℃，保温30h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.43W/kg，磁性能P10/400为8.2W/kg，磁感B8为1.76T，B8/BS＝0.965。
实施例6
按设定成分冶炼钢水，其成分按重量百分比含C0.002％，Si6.1％，Mn0.3％，Al0.07％，V0.01％，Nb0.05％，S0.026％，N0.020％，O0.0012％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1250℃，控制过热度为50℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在2.8mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1030℃，然后进行热轧，开轧温度1030℃，终轧温度940℃，压下量15％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至560℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度560℃，总压下量75％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行5道次冷轧，总压下量为80％，冷轧过程中进行3次时效处理，时效处理温度为300℃，时间为300s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.12mm；
将冷轧带在850±10℃进行再结晶退火，时间为160s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在40℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1230℃，保温24h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.29W/kg，磁性能P10/400为7.5W/kg，磁感B8为1.74T，B8/BS＝0.973。
实施例7
按设定成分冶炼钢水，其成分按重量百分比含C0.001％，Si5.5％，Mn0.22％，Al0.11％，V0.02％，Nb0.05％，S0.03％，N0.010％，O0.0018％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1200℃，控制过热度为20℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在3.0mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1050℃，然后进行热轧，开轧温度1050℃，终轧温度980℃，压下量15％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至600℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度600℃，总压下量70％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行6道次冷轧，总压下量为76％，冷轧过程中进行2次时效处理，时效处理温度为280℃，时间为280s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.18mm；
将冷轧带在850±10℃进行再结晶退火，时间为140s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在50℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1240℃，保温20h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.49W/kg，磁性能P10/400为7.8W/kg，磁感B8为1.77T，B8/BS＝0.968。
实施例8
按设定成分冶炼钢水，其成分按重量百分比含C0.003％，Si5.8％，Mn0.29％，Al0.06％， V0.03％，Nb0.05％，S0.021％，N0.017％，O0.0016％，余量为Fe及不可避免杂质；
薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1220℃，控制过热度为30℃，钢水通过中间包进入薄带连铸机，在旋转的铸辊与侧封板组成的结晶器内形成熔池并凝固成形；厚度在1.8mm；
铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1000℃，然后进行热轧，开轧温度1000℃，终轧温度900℃，压下量10％，制成热轧铸带；
将热轧铸带以20～30℃/s的速率冷却至550℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度550℃，总压下量70％，制成温轧带；
将温轧带酸洗去除氧化皮，然后在100～200℃进行7道次冷轧，总压下量为70％，冷轧过程中进行3次时效处理，时效处理温度为320℃，时间为240s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带，厚度为0.15mm；
将冷轧带在850±10℃进行再结晶退火，时间为120s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在60℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；氮气氢气混合气氛中氢气的体积浓度为30％；
将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1220℃，保温30h进行净化退火；
将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢，磁性能P10/50为0.37W/kg，磁性能P10/400为7.2W/kg，磁感B8为1.75T，B8/BS＝0.970。

Claims (3)

  1. 一种取向高硅钢的制备方法，其特征在于按以下步骤进行：
    (1)按设定成分冶炼钢水，其成分按重量百分比含C 0.001～0.003％，Si 5.0～6.6％，Mn0.2～0.3％，Al 0.05～0.12％，V 0.01～0.04％，Nb 0.03～0.06％，S 0.02～0.03％，N 0.009～0.020％，O≤0.0020％，余量为Fe及不可避免杂质；
    (2)薄带连铸过程：将钢水通过浇口进入中间包，中间包预热温度1200～1250℃，控制过热度为20～50℃，钢水通过中间包进入薄带连铸机后形成铸带，厚度在1.8～3.0mm；
    (3)铸带出辊后在惰性气氛条件下，以50～100℃/s的速率冷却至1000～1050℃，然后进行热轧，开轧温度1000～1050℃，终轧温度900～980℃，压下量10～15％，制成热轧铸带；
    (4)将热轧铸带以20～30℃/s的速率冷却至550～600℃卷取，然后在氮气气氛条件下，进行低温热轧/温轧，开轧温度760±5℃，终轧温度550～600℃，总压下量70～80％，制成温轧带；
    (5)将温轧带酸洗去除氧化皮，然后在100～200℃进行多道次冷轧，总压下量为60～80％，冷轧过程中进行2～3次时效处理，时效处理温度为280～320℃，时间为240～300s，每次时效处理是在相邻两道次冷轧之间，获得冷轧带；
    (6)将冷轧带在850±10℃进行再结晶退火，时间为120～180s，再结晶退火时冷轧带是在氮气氢气混合气氛条件下进行，控制混合气氛的露点在30～60℃，然后涂覆MgO涂层，最后卷取，获得涂层冷轧带；
    (7)将涂层冷轧带置于400±10℃的环形炉内，在氢气流通的条件下，先以30～40℃/h的速度升温至1000±10℃，然后以10～20℃/h的速度升温至1130±10℃，再以30～40℃/h的速度升温至1220～1240℃，保温20～30h进行净化退火；
    (8)将净化退火后的涂层冷轧带进行表面清理去除氧化铁皮，再涂覆绝缘层，然后在800±10℃进行平整拉伸退火，最后空冷至650℃以下卷取，获得取向高硅钢。
  2. 根据权利要求1所述的一种取向高硅钢的制备方法，其特征在于所述的取向高硅钢的厚度为0.10～0.25mm。
  3. 根据权利要求1所述的一种取向高硅钢的制备方法，其特征在于所述的取向高硅钢的磁性能为：P10/50在0.18～0.62W/kg，P10/400在6.75～9.5W/kg，磁感B8在1.74～1.81T，B8/BS＝0.961～0.978。
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