CN101348854B - Method for producing oriented electrical steel by low temperature heating - Google Patents

Method for producing oriented electrical steel by low temperature heating Download PDF

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CN101348854B
CN101348854B CN2008102220265A CN200810222026A CN101348854B CN 101348854 B CN101348854 B CN 101348854B CN 2008102220265 A CN2008102220265 A CN 2008102220265A CN 200810222026 A CN200810222026 A CN 200810222026A CN 101348854 B CN101348854 B CN 101348854B
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nitriding
annealing
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CN101348854A (en
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夏兆所
倪献娟
许学勇
周谊军
王全礼
潘丽梅
杜守志
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Shougang Group Co Ltd
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Shougang Corp
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Abstract

The invention relates to a method for producing oriented electrical steel through low-temperature heating, belonging to the oriented electrical steel technical field. The method comprises the following steps: a slab is heated at a temperature between 1,050 and 1,100 DEG C and then undergoes hot rolling, wherein the initial rolling temperature is between 900 and 1,100 DEG C and the finishing temperature is between 850 and 950 DEG C, and a hot-rolled plate with the thickness between 1.5 and 3.0 millimeters is obtained; secondly, the hot-rolled plate undergoes high-temperature coiling at a temperature of between 650 and 750 DEG C and then is hardened or undergoes heat preservation for 10 minutes to 2 hours; thirdly, the hot-rolled plate is rolled to the thickness of a finished product after undergoing primary cold rolling or secondary cold rolling with intermediate annealing, and the final total reduction rate is between 80 and 90 percent; and fourthly, the final finished product is obtained through decarburization annealing, nitriding treatment, coating of a MgO dusting agent and high-temperature annealing. The compositions in mass percentage of the slab are 0.005 to 0.08 percent of carbon, 2.5 to 6.5 percent of silicon, 0.015 to 0.04 percent of allylsulfanate, 0.001 to 0.4 percent of manganese, 0.01 to 1.0 percent of copper, less than or equal to 0.03 percent of sulfur, less than or equal to 0.02 percent of phosphor, 0.003 to 0.010 percent of nitrogen, and the balance being iron and unavoidable impurities. The method has the advantages of adoption of low slab heating temperature and reduction of the production energy consumption.

Description

A kind of production method of low-temperature heating oriented electrical steel
Technical field
The present invention relates to the oriented electrical steel production technical field, a kind of production method of low-temperature heating oriented electrical steel is provided especially.
Background technology
Grain-oriented electrical steel sheet as the core material of transformer, is the product of unique employing phenomenon of secondary recrystallization in Iron and Steel Production mainly.In order to obtain secondary recrystallization tissue preferably, the precipitate that requires to contain a large amount of small and disperseds in the steel is as inhibitor, as AlN, and MnS, MnSe etc. suppress growing up of primary recrystallization crystal grain in the high temperature annealing temperature-rise period.
Be in the production of oriented electrical steel of main inhibitor with AlN, for obtaining stable inhibitor, carry out normalizing usually after hot rolling, purpose is for separating out a large amount of tiny AlN, making hot-rolled sheet organize more all even recrystal grain more simultaneously.Usually the normalizing temperature is 1050-1150 ℃, Si in the steel under inferior temperature 3N 4With part A lN solid solution, the γ phase amount is many in this moment steel, nitrogen γ mutually in solid solubility than big 9 times in mutually at α, strict control begins chilling temperature and speed of cooling after the normalizing, because 10-50nm AlN separates out by γ-α phase transformation in process of cooling exactly.Water spray cooling after general air cooling arrives about 900 ℃.
At present in the production technique of the oriented electrical steel of development, in order further to reduce slab heating temperature, one class methods are by carry out the method acquisition inhibitor that nitriding is handled before high temperature annealing, so in slab heat-processed, do not require the complete solid solution of inhibitor forming element, thereby can take the lower slab heating temperature about 1200 ℃.
A kind of method that obtains oriented electrical steel is disclosed among the U.S. Patent No. 6488784B1 of company of Nippon Steel application.Chemical ingredients: C:0.003-0.08%, Si:2.0-5.5%, Als:0.01-0.04%, Mn:0.03-0.40%, N≤0.01%, S+Se≤0.03%, Sn≤0.2%, Cu≤0.4%.Slab heating temperature is 1100-1300 ℃, and steel plate is handled 900-1000 ℃ of nitriding after the decarburizing annealing.
A kind of method that obtains high magentic induction oriented electrical steel is disclosed in the U.S. Patent No. 4938807 of company of Nippon Steel application.Chemical ingredients: Si:1.5-4.8%, Als:0.012-0.05%, Mn≤0.45%, Ti:0.002-0.015%, N:0.001-0.012%, S/Se≤0.012, Ti/N0.06-0.6, Mn/ (S+Se) 〉=4.0.Slab heating temperature is 1200 ℃, through normalizing, adds MnN simultaneously in the MgO separant after the hot rolling, and the nitriding element of CrN etc. is finished nitriding in the temperature rise period and handled in final annealing.
A kind of method that has the oriented electrical steel of good magnetic performance and glassy membrane bottom by the nitriding process for producing is disclosed among the Japanese patent laid-open 5-112827 of company of Nippon Steel application.Chemical ingredients: C:0.025-0.075%, Si:2.5-4.5%, Als:0.01-0.06%, Mn:0.08-0.45%, S≤0.012%, N≤0.01%, P:0.015-0.045%.Slab heating temperature is 1200 ℃, does not make a practice of after the hot rolling, and steel plate carries out the nitriding processing at 500-900 ℃ after the decarburizing annealing.
In sum, the oriented electrical steel that low temperature slab heating technique is produced in the present patent documentation has much all been taked the nitriding processing, but in the composition design, and technical process especially aspect such as nitridation process all has separately characteristics.
Summary of the invention
The object of the invention is to provide a kind of production method of low-temperature heating oriented electrical steel, and energy consumption is reduced, and production efficiency improves.
Technical scheme of the present invention is: strand hot rolling after 1050-1100 ℃ of heating, start rolling temperature are 900-1100 ℃, and finishing temperature is 850-950 ℃, roll into the thick hot-rolled sheet of 1.5-3.0mm; Carry out high temperature at 650-750 ℃ and batch, batch back hardening or insulation 10min-2h; Then through once or the secondary cold-rolling of band process annealing to finished product thickness, its finally always draft be 80-90%; Again through decarburizing annealing, after handling, nitriding is coated with the MgO separant and high temperature annealing obtains final finished.
Characteristics are that high temperature batches replacement normalizing processing after having adopted hot rolling, and combine the preparation low-temperature oriented electrical steels with the nitriding processing in later stage.
Strand composition of the present invention is: 0.005-0.08%C, and 2.5-6.5%Si, 0.015-0.04%Als, 0.001-0.4%Mn, 0.01-1.0%Cu, S≤0.03%, P≤0.02%, 0.003-0.010%N, all the other are Fe and inevitable inclusion; Be mass percent.
Be main inhibitor with AlN among the present invention, so require to contain at least 0.015%Al and 0.003%N in the composition to guarantee to form required inhibitor.But Al is mingled with magnetic property is had a negative impact greater than being easy to generate thick AlN after 0.04%, and N influences surface quality greater than forming bubbling at surface of steel plate easily after 0.01%, and the size of wayward primary recrystallization crystal grain.Because handling, nitriding can introduce more nitrogen, can be so smelt in the composition nitrogen content less than 0.006%, thus having reduced the difficulty of smelting, promptly preferred N content is 0.003-0.006%.
Take the high temperature coiling technique after the hot rolling, coiling temperature is 650-750 ℃, and preferred temperature is 700-750 ℃.In the production of oriented electrical steel, the inhibitor such as AlN of separating out a large amount of small and disperseds before secondary recrystallization are the most key steps.Present once cold rolling method is produced in the oriented electrical steel and generally all take to carry out normalizing after hot rolling; make hot rolling microstructure more even on the one hand; the more important thing is deposition on the other hand and separate out the AlN inhibitor of a large amount of small and disperseds, thereby guarantee stable secondary recrystallization at cooling stages.The method that adopts high temperature to batch among the present invention, coiling temperature is 650-750 ℃, preferred temperature is 700-750 ℃, batches back hardening or insulation 10min-2h.Because slab heating temperature and hot rolling start rolling temperature are all lower, the deposition of AlN will take place at course of hot rolling, in the hardening process after high temperature batches or holding stage separate out the AlN of a large amount of small and disperseds, combine with follow-up nitriding processing, enough inhibition abilities are provided, guarantee that the stable of secondary recrystallization carries out, thereby simplified production technique, shortened process reduces cost.
Steel plate after the hot rolling through once or the secondary cold-rolling method of band process annealing be rolled down to finished product thickness, its final total draft is 80-90%; Steel plate after cold rolling carries out decarburizing annealing at 800-850 ℃ of insulation 3-6min, and furnace atmosphere is H 2And N 2Mixed gas, H wherein 2Content volume per-cent is 5-30%.
The temperature that nitriding is handled is 850-1000 ℃; Nitriding time is 20-100s, and the nitriding furnace atmosphere is NH 3, H 2And N 2Mixed gas, H wherein 2Content volume per-cent is 5-30%, NH 3Content volume per-cent is 1-15%, and surplus is N 2
According to the literature; the unsettled N that is introduced by nitriding easily and the Si combination inside the steel plate; form protective layer on the surface; stop N further deeply, have only by just can make in the slow intensification of high temperature annealing stage N to internal divergence more with Al in conjunction with the effect that forms AlN competence exertion inhibitor.United States Patent (USP) 4929286 and 4979996 has also been reported by nitriding and has been formed (Al, Si) N inhibitor, and non-traditional AlN inhibitor.As seen diffusibility and the distribution situation in steel band of N were the key factors that influences product performance during nitriding was handled.Adopt 850-1000 ℃ higher nitriding temperature among the present invention, increased infiltration and the diffusibility of N, N can be distributed in the entire belt steel more uniformly, thereby helped the formation of inhibitor.
Nitriding time causes the nitriding amount very few less than 20s easily, in the steel plate formation of inhibitor very few, the secondary recrystallization instability, magnetic property is relatively poor; Nitriding time greater than 100s after form protective membrane because nitriding process N concentrates on surface of steel plate easily, stop further carrying out of nitriding, the nitriding effect on the contrary can variation after the time lengthening, so nitriding time is 20-100s, the preferred time is 30-60s.
NH in the atmosphere 3Content was less than 1% o'clock, and the nitriding amount is too small, and magnetic property is relatively poor; NH 3Content was greater than 15% o'clock, and the nitriding amount increases not obvious, and bigger for the corrosion of nitriding equipment, and is bigger to the influence of glassy membrane bottom simultaneously, is unfavorable for the coating of back separant.So NH 3Content range is 1-15%, and preferred scope is 3-7%.
Handling the back in nitriding is main component coated with MgO and adds 2-5wt%TiO at surface of steel plate 2Separant after carry out high temperature annealing, heat up with the speed of 5-20 ℃/h 850-1100 ℃ of stage.
The present invention compares with the technology that domestic and international other low temperature nitriding process is produced oriented electrical steel; the temperature that has not only further reduced the slab heating is to 1050-1100 ℃; and the method that adopts 650-750 ℃ of high temperature to batch after hot rolling replaces traditional normalizing to handle; greatly reduce energy consumption, shortened Production Flow Chart.Nitriding after the decarburizing annealing is handled and enough inhibitor is provided for again the stable secondary recrystallization of formation, is a kind of more promising technology of producing low-temperature oriented electrical steels.
The invention has the advantages that, taked lower slab heating temperature, reduced production energy consumption.
Embodiment
Embodiment 1: with the steel-making of 25kg vacuum oven, chemical ingredients such as table 1, all the other are iron and unavoidable impurities.Strand hot rolling behind 1150 ℃ of heating 2.5h is batched insulation 30min in back to 2.2mm at 750 ℃.Once cold rolling is to 0.255mm, at H 2And N 2Mixed gas in carry out decarburizing annealing, technology is 835 ℃ * 5min.870 ℃ of nitriding 40s, atmosphere is NH 3, H 2And N 2Mixed gas, NH wherein 3Content volume per-cent is 6%, H 2Content volume per-cent is 25%, carries out high temperature annealing after the coating MgO separant, wherein heats up with 10 ℃/h speed 900-1100 ℃ of stage.Magnetic measurement results is as shown in table 2.
Table 1 experimental steel chemical ingredients unit: wt%
Embodiment C Si Als Mn Cu S N P
A 0.069 3.18 0.028 0.078 0.065 0.020 0.0055 ≤0.01
B 0.065 3.15 0.025 0.070 0.055 0.023 0.0050 ≤0.01
C 0.072 3.20 0.030 0.065 0.080 0.022 0.0058 ≤0.01
Table 2 experimental steel magnetic property result
Numbering P 17(w/kg) B 800(T)
Al 1.195 1.87
B1 1.201 1.86
C1 1.170 1.88
Embodiment 2: the hot rolling behind 1150 ℃ of heating 2.5h of the experimental steel among the embodiment 1, strand is batched the back hardening at 750 ℃ to 2.2mm, and cold rolling and decarburizing annealing condition is with embodiment 1.950 ℃ of nitriding 30s, atmosphere is NH 3, H 2And N 2Mixed gas, NH wherein 3Content volume per-cent is 5%, H 2Content volume per-cent is 25%, carries out high temperature annealing after the coating MgO separant, wherein heats up with 10 ℃/h speed 900-1100 ℃ of stage.Magnetic measurement results is as shown in table 3.
Table 3 experimental steel magnetic property result
Numbering P 17(w/kg) B 800(T)
A2 1.112 1.89
B2 1.150 1.87
C2 1.093 1.91
Embodiment 3: the experimental steel C among the embodiment 1, strand hot rolling behind 1150 ℃ of heating 2.5h is batched insulation 30min in back to 2.2mm at 700 ℃.Once cold rolling is to 0.255mm, at H 2And N 2Mixed gas in carry out decarburizing annealing, technology is 835 ℃ * 5min.900 ℃ of nitriding 10-80s, atmosphere is NH 3, H 2And N 2Mixed gas, NH wherein 3Content volume per-cent is 5%, H 2Content volume per-cent is 25%, carries out high temperature annealing after the coating MgO separant, wherein heats up with 10 ℃/h speed 900-1100 ℃ of stage.Magnetic measurement results is as shown in table 4.
Table 4 experimental steel magnetic property result
Numbering Nitriding time (s) P 17(w/kg) B 800(T)
C31 10 1.933 1.642
C32 40 1.162 1.89
C33 60 1.356 1.85
C34 80 1.602 1.78

Claims (4)

1. the production method of a low-temperature heating oriented electrical steel is characterized in that, strand hot rolling after 1050-1100 ℃ of heating, and start rolling temperature is 900-1100 ℃, finishing temperature is 850-950 ℃, rolls into the thick hot-rolled sheet of 1.5-3.0mm; Carry out high temperature at 650-750 ℃ and batch, batch back shrend or insulation 10min-2h; Then through once or the secondary cold-rolling of band process annealing to finished product thickness, its finally always draft be 80-90%; Again through decarburizing annealing, after handling, nitriding is coated with the MgO separant and high temperature annealing obtains final finished;
Described strand composition is: 0.005-0.08%C, and 2.5-6.5%Si, 0.015-0.04%Als, 0.001-0.4%Mn, 0.01-1.0%Cu, S≤0.03%, P≤0.02%, 0.003-0.010%N, all the other are Fe and inevitable inclusion; Be mass percent;
The nitriding temperature that described nitriding is handled is 850-1000 ℃; Nitriding time is 20-100s, and the nitriding furnace atmosphere is NH 3, H 2And N 2Mixed gas, H wherein 2Content volume per-cent is 5-30%, NH 3Content volume per-cent is 1-15%, and surplus is N 2
Described decarburizing annealing is that the steel plate after cold rolling carries out at 800-850 ℃ of insulation 3-6min; Furnace atmosphere is H 2And N 2Mixed gas, H wherein 2Content volume per-cent is 5-30%.
2. by the described method of claim 1, it is characterized in that nitriding time is 30-60s; NH 3Content volume per-cent is 3-7%.
3. by the described method of claim 1, it is characterized in that, add 2-5wt%TiO in the MgO separant 2
4. by the described method of claim 1, it is characterized in that described high temperature annealing is that the speed with 5-20 ℃/h heats up 850-1100 ℃ of stage.
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Publication number Priority date Publication date Assignee Title
CN101603148B (en) * 2009-07-28 2011-01-05 首钢总公司 Method for producing economic low-temperature heating oriented electrical steel
CN102041449B (en) * 2011-01-16 2012-05-30 首钢总公司 Method for improving electromagnetic performance of oriented electric steel by low-temperature plate blank heating process
CN102127716A (en) * 2011-01-16 2011-07-20 首钢总公司 Low-temperature heating oriented electrical steel with good surface coating and production method thereof
CN107630186A (en) * 2016-07-18 2018-01-26 鞍钢股份有限公司 A kind of method for improving electrical steel product surface insulation characteristic
CN106319174B (en) * 2016-09-23 2018-10-16 武汉钢铁有限公司 Improve the annealing separating agent of low temperature casting blank heating high magnetic induction grain-oriented silicon steel bottom layer quality
CN109112283A (en) * 2018-08-24 2019-01-01 武汉钢铁有限公司 The preparation method of low temperature high magnetic induction grain-oriented silicon steel

Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1231703A (en) * 1996-09-05 1999-10-13 阿奇亚斯佩丝阿里特尔尼公司 Process for the production of grain oriented electrical steel strip starting from thin slabs
CN1590567A (en) * 2003-08-27 2005-03-09 宝山钢铁股份有限公司 Production method of electrical steel plate for magnetic suspension long stator
CN1850430A (en) * 2006-05-18 2006-10-25 武汉科技大学 Thin slab process high magnetic induction oriented electrical steel sheet and its manufacturing method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1231703A (en) * 1996-09-05 1999-10-13 阿奇亚斯佩丝阿里特尔尼公司 Process for the production of grain oriented electrical steel strip starting from thin slabs
CN1590567A (en) * 2003-08-27 2005-03-09 宝山钢铁股份有限公司 Production method of electrical steel plate for magnetic suspension long stator
CN1850430A (en) * 2006-05-18 2006-10-25 武汉科技大学 Thin slab process high magnetic induction oriented electrical steel sheet and its manufacturing method

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Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing

Patentee after: Shougang Group Co. Ltd.

Address before: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing

Patentee before: Capital Iron & Steel General Company