CN101358273B - Method for producing low-temperature oriented electrical steels - Google Patents
Method for producing low-temperature oriented electrical steels Download PDFInfo
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- CN101358273B CN101358273B CN2008102220104A CN200810222010A CN101358273B CN 101358273 B CN101358273 B CN 101358273B CN 2008102220104 A CN2008102220104 A CN 2008102220104A CN 200810222010 A CN200810222010 A CN 200810222010A CN 101358273 B CN101358273 B CN 101358273B
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Abstract
A production preparation method of low-temperature oriented electrical steel belongs to the technical field of oriented electrical steel. Casting blanks are heated at the temperature of 1050 DEG C to 1100 DEG C and goes through the nitriding process after decarurizing annealing; the nitriding temperature is from 850 DEG C to 1000 DEG C, the time of nitriding lasts for 20 seconds to 1000 seconds, and the atmosphere in a nitriding furnace is the mixture gas of NH3, H2 and N2; wherein, the NH3 content in volume is 1 percent to 15 percent. The method has the advantage that lower heating temperature of the casting blanks is adopted to reduce the energy consumption in production.
Description
Technical field
The present invention relates to the oriented electrical steel production technical field, a kind of production method of low-temperature oriented electrical steels is provided especially.
Background technology
The good magnetic property of grain-oriented electrical steel sheet comes from its Goss texture that forms by secondary recrystallization in final high-temperature annealing process.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.
The production method of traditional oriented electrical steel is in the high-temperature heater of special use slab to be heated to 1350-1400 ℃, makes inhibitor forming element Al, Mn; S; fully solid solution such as N is so that separate out second phase particle, the i.e. inhibitor that forms small and dispersed in subsequently hot rolling or normalizing process.The shortcoming of this production method is: (1) then can't guarantee to form enough and uniform inhibitor after the hot rolling if fail to meet the requirements of slab heating temperature, and secondary recrystallization will be unstable; (2) heat makes billet surface produce a large amount of iron scales, and high-temperature heater need often be cleared up and safeguard, has not only increased cost but also has reduced production efficiency; (3) to split phenomenon serious on the limit in the hot rolling, and lumber recovery is reduced; (4) heat itself has consumed a large amount of energy, has increased production cost.
In order to overcome the shortcoming of above-mentioned heat method, by constantly research and exploration, slab heating temperature is constantly reduced in the production by the whole bag of tricks.Wherein class methods are with the lower inhibitor of new solid solubility temperature, as Cu
2S, AlN etc. replace traditional inhibitor based on MnS.The common orientated electrical steel that Yi Xiete and Xin Lipeicike factory produce in the Russia, Cu in the composition, Mn content is higher and partly added Ni, and Cr etc. are with Cu
2S+AlN is main inhibitor, adopts 1250-1280 ℃ of low temperature slab addition, decarburization when secondary cold-rolling process annealing, low temperature recovery annealing behind the secondary cold-rolling.Thyssen also adopts Cu
2S+AlN is that main inhibitor has been reduced to 1260-1280 ℃ to slab heating temperature, and hot rolling is adopted the once cold rolling method and carried out cold rolling timeliness after 980-1080 ℃ of normalizing.
Another kind of method does not require the complete solid solution of inhibitor forming element in slab heat-processed, but obtains inhibitor by the method for carrying out the nitriding processing before high temperature annealing, thereby can further reduce slab heating temperature.
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: C0.025-0.075%, Si2.5-4.5%, Als0.01-0.06%, Mn0.08-0.45%, S≤0.012%, N≤0.01%, P0.015-0.045%, all the other are Fe and inevitable inclusion.Slab carries out hot rolling after 1200 ℃ of heating, with the once cold rolling method or there be twice of process annealing above cold-rolling practice to be rolled down to final thickness, steel plate carries out nitriding at 500-900 ℃ and handles after the decarburizing annealing, wherein NH
3Content is more than the 1000ppm, and protective atmosphere is H
2And N
2Mixed gas, carry out high temperature annealing then behind the separant coating.
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%, N0.001-0.012%, S/Se≤0.012, Ti/N 0.06-0.6, Mn/ (S+Se) 〉=4.0.Slab carries out hot rolling and normalizing after 1200 ℃ or following heating, be rolled down to final thickness through once cold rolling or at least twice above cold-rolling practice, applies at surface of steel plate after the decarburizing annealing to contain MgO, TiO
2, the separant of MnN or CrN etc. is finished nitriding in the temperature rise period in the time of final annealing and is handled.Perhaps apply common separant, but feed NH in the temperature rise period of final annealing
3Carrying out nitriding handles.
A kind of method that obtains high magentic induction oriented electrical steel is disclosed among the U.S. Patent No. 6741787B2 of Italy Te Ni company application.Chemical ingredients: C 0.015-0.075%, Si 2.5-4.5%, Mn 0.3-0.4%, Als 0.01-0.04%, S≤120ppm, N 0.003-0.013%, Ti≤50ppm, all the other are Fe and unavoidable impurities.Slab hot rolling after 1200-1320 ℃ of heating; carrying out the two-part normalizing at 1000-1150 ℃ and 800-950 ℃ handles; carry out primary recrystallization annealing and decarburization at 850-950 ℃ after being cold rolled to final thickness, carrying out nitriding at 850-1050 ℃ then and handle, atmosphere is NH
3, H
2And N
2Mixed gas NH wherein
3Content is the 1-35L/kg steel plate, last separant coating and high temperature annealing.
In sum, high temperature slab heating method is produced oriented electrical steel and is had the energy consumption height, and production efficiency is low, and shortcomings such as big are split on the hot rolling limit, and low temperature slab heating technique is that the focus of recent research also is the development in future direction.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 oriented electrical steels, and energy consumption is reduced, and production efficiency improves.
Strand carries out hot rolling among the present invention after heating; normalizing handle after once or the secondary cold-rolling of band process annealing to finished product thickness; again through decarburizing annealing, after handling, nitriding is coated with the MgO separant and high temperature annealing obtains final finished, and the committed step of each technical process is as follows:
1) hot rolling, strand are 1050-1100 ℃ of heating, and start rolling temperature is 900-1100 ℃, and finishing temperature is 850-950 ℃, and coiling temperature is 400-600 ℃, roll into the thick hot-rolled sheet of 1.5-3.0mm;
2) normalizing is handled, and hot-rolled sheet to 850-1050 ℃, is incubated the 60-150s postcooling at 1050-1150 ℃ of insulation 60-180s postcooling again;
3) cold rolling, use once or be with the secondary cold-rolling method of process annealing to be rolled down to finished product thickness, its final total draft is 80-90%;
4) decarburizing annealing, cold-rolled steel sheet is at 800-900 ℃ of insulation 3-6min, and furnace atmosphere is H
2And N
2Mixed gas, H wherein
2Content volume per-cent is 5-30%;
5) nitriding is handled, and nitriding temperature 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
6) separant coating and high temperature annealing are main component coated with MgO and add 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.
Described 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.
The preferred composition of oriented electrical steel among the present invention is: 0.005-0.08%C, 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%, 0.003-0.006%N, all the other are Fe and inevitable inclusion.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 reduced the difficulty of smelting.
Inhibitor mainly is to handle the back in nitriding to form among the present invention, so the slab heating phase does not just need higher Heating temperature to make the complete solid solution of inhibitor forming element, thereby can greatly reduce the requirement to process furnace 1050-1100 ℃ of heating, save energy is enhanced productivity.
After the technology that is more preferably on the aforementioned production method basis is hot rolling, be incubated the 120-180s postcooling to 850-950 ℃, be incubated the 90-150s postcooling again at 1100-1140 ℃.With 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%.Cold-rolled steel sheet is at 800-850 ℃ of insulation 4-6min, and furnace atmosphere is H
2And N
2Mixed gas, H wherein
2Content volume per-cent is 5-30%.
Steel band carries out nitriding processing, nitriding time 30-60s at 850-1000 ℃ after the decarburizing annealing; 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 3-7%.Last separant coating also carries out high temperature annealing.
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.Adopted 850-1000 ℃ higher nitriding temperature among the present invention, infiltration and the diffusibility of N have been increased, N can be distributed in the entire belt steel more uniformly, thereby help the formation of inhibitor, so can adopt more cryogenic heating cycle in the strand heating phase.
The invention based on the producing oriented electrical steel by low temperature slab heating of nitridation process is both at home and abroad analyzed, can find: the technology of Japanese Nippon Steel concentrates on after the decarburizing annealing in the secondary recrystallization process the steel plate nitriding, slab heating temperature is lower, below 1200 ℃, nitriding temperature is also lower, in especially concentrating on 700-900 ℃ of scope below 900 ℃.Slab heating temperature is higher in the technology of Italy Te Ni company, and between 1200-1320 ℃, nitriding temperature is also higher, between 900-1100 ℃.Posco is a technology mode of taking decarburization and nitriding to carry out simultaneously, and is main inhibitor with BN.The technology of domestic Baosteel is to carry out nitriding to handle before decarburizing annealing, to reduce the influence of surface film oxide to nitriding.
The invention has the advantages that production energy consumption further reduces, production efficiency improves; Do not need special high temperature bar plate heating stove, the potential benefit is big.
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.2.2mm is arrived in strand hot rolling behind 1100 ℃ of heating 2.5h.The normalizing condition is that 1120 ℃ of insulation 2.5min postcooling to 900 ℃ insulation 2min quench in 100 ℃ of water again.The band steel is rolled down to 0.255mm through once cold rolling, 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 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 2.
Table 1 experimental steel chemical ingredients unit: wt%
| Embodiment | C | Si | Als | Mn | Cu | S | N | P |
| A | 0.070 | 3.18 | 0.027 | 0.078 | 0.080 | 0.023 | 0.0054 | ≤0.01 |
| B | 0.075 | 3.10 | 0.030 | 0.082 | 0.060 | 0.027 | 0.0048 | ≤0.01 |
Table 2 experimental steel magnetic property result
| Numbering | P 17(w/kg) | B 800(T) |
| A1 | 1.138 | 1.89 |
| B1 | 1.155 | 1.87 |
Embodiment 2: hot rolling is to 2.2mm behind 1100 ℃ of heating 2.5h for the experimental steel among the embodiment 1, strand, and the normalizing condition is that 1120 ℃ of insulation 2.5min postcooling to 900 ℃ insulation 2min quench in 100 ℃ of water again.The band steel is rolled down to 0.255mm through once cold rolling, at H
2And N
2Mixed gas in carry out decarburizing annealing, technology is 835 ℃ * 5min.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 | 1.070 | 1.90 |
| B2 | 1.095 | 1.89 |
Embodiment 3: the experimental steel A among the embodiment 1, nitriding time are 10-80s, and all the other technologies are with among the embodiment 2.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) |
| A31 | 10 | 1.831 | 1.52 |
| A32 | 30 | 1.070 | 1.90 |
| A33 | 60 | 1.413 | 1.81 |
| A34 | 80 | 1.738 | 1.68 |
Embodiment 4: experimental steel B among the embodiment 1, NH during nitriding is handled
3Content volume per-cent is 2-9%, and all the other technologies are as shown in table 5 with embodiment 1. magnetic measurement results.
Table 5 experimental steel magnetic property result
| Numbering | NH 3(％) | P 17(w/kg) | B 800(T) |
| B41 | 2 | 1.729 | 1.63 |
| B42 | 5 | 1.155 | 1.87 |
| B43 | 9 | 1.512 | 1.78 |
Claims (1)
1. the production method of a low-temperature oriented electrical steels, it is characterized in that technology is: strand carries out hot rolling after heating, normalizing handle after once or the secondary cold-rolling of band process annealing to finished product thickness, again through decarburizing annealing, after handling, nitriding is coated with the MgO separant and high temperature annealing obtains final finished;
Wherein, nitriding temperature 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 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;
Described hot rolling be strand 1050-1100 ℃ of heating, start rolling temperature is 900-1100 ℃, finishing temperature is 850-950 ℃, coiling temperature is 400-600 ℃, rolls into the thick hot-rolled sheet of 1.5-3.0mm; Described normalizing is handled be hot-rolled sheet greater than 1050 to smaller or equal to 1150 ℃ of insulation 60-180s postcooling to 850-1050 ℃, be incubated the 60-150s postcooling again;
Described cold rolling be with 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%; Described decarburizing annealing is that cold-rolled steel sheet is incubated 3-6min at 800-900 ℃, and furnace atmosphere is H
2And N
2Mixed gas, H wherein
2Content volume per-cent is 5-30%;
Described high temperature annealing is to carry out high temperature annealing after surface of steel plate is coated with the MgO separant, and the speed 850-1100 ℃ of stage with 5-20 ℃/h heats up.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| PL2455497T3 (en) * | 2009-07-13 | 2019-07-31 | Nippon Steel & Sumitomo Metal Corporation | Manufacturing method of grain-oriented electrical steel sheet |
| BR112012001161B1 (en) * | 2009-07-17 | 2021-11-16 | Nippon Steel Corporation | METHOD OF PRODUCTION OF A GRAIN ORIENTED ELECTRIC STEEL SHEET |
| CN102127708A (en) * | 2011-01-16 | 2011-07-20 | 首钢总公司 | Method for producing oriented electrical steel by heating low-temperature slab |
| 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 |
| CN102337494B (en) * | 2011-09-26 | 2013-08-28 | 台州学院 | Method for processing wear-resisting corrosion-resisting nitriding layer on surface of Fe-Mn series stainless steel |
| CN107630133B (en) * | 2016-07-18 | 2019-06-28 | 鞍钢股份有限公司 | A kind of production method of the excellent high grade electrical steel product of frequency property |
| 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 |
| CN112522609B (en) * | 2020-11-18 | 2021-12-14 | 武汉钢铁有限公司 | High magnetic induction oriented silicon steel containing composite inhibitor and production method thereof |
| CN112941286B (en) * | 2021-01-29 | 2022-07-08 | 武汉钢铁有限公司 | High-magnetic-induction oriented silicon steel manufacturing method for improving effective nitrogen and bottom layer quality |
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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 |