CN103014285B - Manufacturing method of mirror surface oriented silicon steel with good magnetic performance and annealing parting agent - Google Patents
Manufacturing method of mirror surface oriented silicon steel with good magnetic performance and annealing parting agent Download PDFInfo
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- CN103014285B CN103014285B CN201110299949.2A CN201110299949A CN103014285B CN 103014285 B CN103014285 B CN 103014285B CN 201110299949 A CN201110299949 A CN 201110299949A CN 103014285 B CN103014285 B CN 103014285B
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Abstract
The invention discloses a manufacturing method of mirror surface oriented silicon steel with good magnetic performance and an annealing parting agent. The manufacturing method comprises the following steps of: 1) smelting; 2) hot rolling and normalizing; 3) cold rolling; 4) decarbonization and nitriding; and 5) parting agent coating and high-temperature annealing. The annealing parting agent comprises the following components in parts by mass: 65-96 parts of Al2O3 powder, 2-15 parts of silicate powder with a particle size of 0.1-100 microns, 1-10 parts of alkaline earth metal oxide and 1-10 parts of metal chloride. According to the invention, through the annealing parting agent consisting of Al2O3 powder, silicate powder, alkaline earth metal oxide and metal chloride, a glass film bottom layer is not formed on the surface of a steel plate in a high-temperature annealing process, and the steel can be effectively purified; and meanwhile, the embedded oxide on the near surface of a substrate is removed through the corrosion reaction of chloride so as to obtain a product with a smooth and clean surface and stable magnetic performance.
Description
Technical field
The present invention relates to oriented silicon steel manufacture method, particularly a kind of mirror surface-oriented silicon steel manufacture method and annealing separating agent with fine magnetic property.
Background technology
Oriented silicon steel, at H after hot rolling, normalizing and cold-rolling treatment
2-N
2carry out decarburizing annealing under atmosphere protection, eliminate rolling stress, form primary recrystallization, simultaneously logical moisture in stove, by carbon content control in steel band at below 30ppm, to prevent finished product generation magnetic aging.During decarburizing annealing, steel strip surface can be oxidized, and is formed with SiO
2and Fe
2siO
4be main zone of oxidation, disadvantageous effect is caused to further decarburization.In subsequent high temperature annealing process, the annealing separating agent generation chemical reaction that zone of oxidation and steel strip surface apply, generates with Mg
2siO
4be main glassy membrane bottom, this glassy membrane bottom can prevent when high temperature annealing steel band from boning and play the effect of purification steel.
Oriented silicon steel surface magnesium silicate glass film bottom has higher hardness, causes steel plate stamping piece performance poor, often only has several thousand times; And the embedded junction credit union of glassy membrane bottom and steel matrix hinders the motion of neticdomain wall, increase magnetic hysteresis loss.
In order to improve the punching performance of grain-oriented silicon-iron and improve magnetic property further, in prior art, develop the grain-oriented silicon-iron without glassy membrane bottom.
JFE company of Japan uses the Al do not reacted with surface of steel plate
2o
3deng as high temperature annealing separant, directly obtain the grain-oriented silicon-iron without glassy membrane bottom.This method will be eliminated the nearly oxide on surface of steel plate completely and be mingled with needs and strictly control decarburization dew point and make surface of steel plate not form ferriferous oxide, but this will certainly bring the problem such as decarburization, nitriding.
Armco company of the U.S. adds SiO in magnesium oxide
2as annealing separating agent, the loose Magnesium Silicate q-agent that secondary recrystallization annealing process light plate surface is formed is conducive to Annealing Protection gas and enters between steel plate layer and purify steel.But this method is often difficult to surperficial Magnesium Silicate q-agent to scrub off completely, the embedded oxide near for steel plate surface can not be eliminated completely, to reduction core loss limited efficiency.
NSC company of Japan adds muriate as annealing separating agent in magnesium oxide, adds a large amount of muriates and cause certain corrosion to surface of steel plate in secondary recrystallization annealing process, affect surperficial inhibitor, causes secondary recrystallization unstable.
Summary of the invention
The object of the present invention is to provide a kind of mirror surface-oriented silicon steel manufacture method and the annealing separating agent with fine magnetic property, by controlling decarburizing annealing condition, using Novel disk withdrawal fire screen from agent prescription, stable acquisition has excellent magnetic characteristics, the grain-oriented silicon-iron of any surface finish.
For achieving the above object, technical scheme of the present invention is:
The present invention is by using Al
2o
3silicate, alkaline earth metal oxide, basic metal, alkaline-earth metal or Mn, Zn muriatic one or more as annealing separating agent, high-temperature annealing process light plate surface is made not form glassy membrane bottom, and effectively can purify steel, utilize muriatic corrosion reaction to remove the embedded oxide on the nearly surface of substrate simultaneously, thus obtain any surface finish and magnetic property stable product.
Particularly, the mirror surface-oriented silicon steel manufacture method with fine magnetic property of the present invention, comprises the steps:
1) smelt
With converter or Electric furnace steel making, molten steel is after secondary refining and continuous casting, obtain blank plates of silicon steels, its composition by weight percent is: C:0.015 ~ 0.06%, Si:2.5 ~ 4.0%, acid-solubility Al:0.015 ~ 0.04%, Mn:0.06 ~ 0.45%, Cu:0.01 ~ 0.29%, S≤0.012%, N≤0.01%, and all the other are Fe and inevitable impurity.
2) hot rolling, normalizing
Heating of plate blank is to less than 1200 DEG C heating, and 1.5 ~ 3.0mm hot-rolled sheet is made in hot rolling; Carry out the normalizing annealing of 30 ~ 200s at 900 ~ 1150 DEG C, then carry out pickling.
3) cold rolling
With once or the above cold rolling process of secondary of band process annealing be rolled into the cold-reduced sheet of 0.20 ~ 0.35mm, final draft is greater than 80%, makes the cold-reduced sheet of 020 ~ 0.35mm;
4) decarburization, nitriding
Cold-reduced sheet N
2+ H
2carry out decarburizing annealing process in shielding gas, the carbon in steel plate is reduced to below 25ppm, formed with SiO at surface of steel plate simultaneously
2for the zone of oxidation of main component, Control for Oxygen Content 2.0g/m
2below; At the forward and backward of continuous decarburizing annealing or carry out continuous print Nitrizing Treatment by Control of Nitrogen Content at 150-350ppm simultaneously.
5) separant coating, high temperature annealing
At decarburization plate surface coated annealing separating agent, be nitrogen and hydrogen mixture in atmosphere after oven dry, 25% ~ 100%H
2, D.P. < 0 DEG C, temperature is carry out the insulation high temperature annealing of more than 15 hours under the condition of 1150 ~ 1250 DEG C, then through being coated with insulating coating and stretching and leveling annealing obtains the minute surface grain-oriented silicon-iron product of excellent magnetic.
The annealing separating agent that mirror surface-oriented silicon steel for having fine magnetic property of the present invention manufactures, its component content is: Al
2o
3powder, 65-96 part, silicate powder, 2-15 part, its particle diameter between 0.1-100 μm, alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part.
Further, silicate powder comprises Al4 (SiO
4)
3, CaSiO
3, Mg
2siO
4, Fe
2siO
4in more than one.
Metal chloride comprises alkali metal chloride LiCl, NaCl, KCl, RbCl, alkaline earth metal chloride BeCl
2, MgCl
2, CaCl
2, SrCl
2, BaCl
2in more than one.
Alkaline earth metal oxide to comprise in BeO, MgO, CaO, SrO, BaO more than one.
The main component Al of separant of the present invention
2o
3when high temperature annealing not with steel plate zone of oxidation and substrate generation chemical reaction, be beneficial to and form the oriented silicon steel of any surface finish.In high temperature annealing, the effect that impurity element diffusion admittance is provided is played with the silicate additive that certain particle diameter state exists, because the silicate of hydration status in temperature-rise period dewaters, therefore can cause a fixed gap, be beneficial to detrimental impurity in steel and spread in gaseous form.Due to Al
2o
3do not react with water, if silicate addition is less than 2%, or particle diameter is less than 0.1 μm, and during high temperature annealing, separant is too closely knit, to hinder elements such as harmful N, Se, the S of magnetic to external diffusion, cause the deterioration of finished product magnetic property.If silicate addition is greater than 15%, or particle diameter is greater than 100 μm, then can owing to releasing excess moisture, and cause the Additional oxidation of steel plate, later stage oxidizing reaction is made to be difficult to remove bottom completely, simultaneously particle diameter is crossed conference and is made too much chlorion go deep into zone of oxidation base portion, with metal generation chemical reaction and etched the matrix, is difficult to the mirror surface-oriented silicon steel obtaining any surface finish.So silicate addition should control between 2% ~ 15%, particle diameter should control between 0.1m ~ 100 μm.
Alkaline earth metal oxide additives has two effects.On the one hand, when River Bank Stability and water effect, form oxyhydroxide, oxyhydroxide decomposition temperature is higher than 580 DEG C, thus make surface of steel plate still have certain H+ to exist at relatively high temperatures, form acidic solution together with Cl-, this acidic solution can react with surface of steel plate oxide compound, thus removes the embedded oxide on zone of oxidation and nearly surface; On the other hand, the existence of alkaline earth metal oxide can increase the interfacial energy between oxide compound and matrix, thus makes inner oxygen to external diffusion, forms clearly more demarcated interface between, is conducive to the reaction of itself and HCl and forms smooth finish surface.If the addition of alkaline earth metal oxide is less than 1%, then amount of moisture is brought into very few, can not accomplish to remove oxide on surface and embedded oxide completely; If addition is greater than 10%, then can with metallic matrix generation corrosion reaction.Therefore, alkaline earth metal oxide additives addition is very few or too much all can affect the smooth finish of finished surface, and consider, its amount should control between 1% ~ 10%.
The metal chloride be brought in separant with certain compound form plays the effect of acid attack in high-temperature annealing process.Muriatic mass percent lower than 1%, then can not remove zone of oxidation and embedded oxide completely, can not obtain the finished product oriented silicon steel of any surface finish; Higher than 10%, then the corrosion of metallic matrix easily occurs, secondary recrystallization is affected and occurs magnetic property wild effect, simultaneously also can the smooth finish of injured surface.Answer this, muriatic addition should control between 1% ~ 10%.
By the present invention can obtain any surface finish and magnetic property stable without glassy membrane bottom grain-oriented silicon-iron product, there is excellent magnetic property and punching performance.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
With the steel-making of 500kg vacuum oven, slab chemical composition (wt%) is: 0.045%C, 3.25%Si, 0.006%S, 0.027%Als, 0.006%N, 0.15%Cu, 0.012%Mn all the other be Fe and inevitable impurity.Steel billet is rolled into the hot-rolled sheet that 2.6mm is thick after heating at 1150 DEG C.Hot-rolled sheet through 1150 DEG C of normalizing annealings after 1 minute, pickling the final thickness of slab 0.285mm of cold rolling one-tenth.Cold-reduced sheet carries out the decarburizing annealing process of 120 seconds at 835 DEG C, and surface oxygen content is 1.0 and 2.0g/m
2two levels; After Nitrizing Treatment, the nitrogen content of steel plate is 250ppm.Decarburizing annealing plate coating annealing separating agent, composition proportion, in table 1, carries out 1200 DEG C, the insulation high temperature annealing of 20 hours in dry nitrogen, hydrogen protective atmosphere after rolling; Through being coated with insulating coating and stretching and leveling annealing after uncoiling.
Table 1
| Explanation | Separant is filled a prescription |
| Embodiment 1 | Al 2O 396 parts of+Mg 2SiO 42 parts of (particle diameter 0.1 μm)+CaO, 1 part of+MgCl 21 part |
| Embodiment 2 | Al 2O 396 parts of+Mg 2SiO 42 parts of (particle diameter 100 μm)+CaO, 1 part of+MgCl 21 part |
| Embodiment 3 | Al 2O 365 parts of+Mg 2SiO 415 parts of (particle diameter 100 μm)+CaO, 10 parts of+MgCl 210 parts |
| Embodiment 4 | Al 2O 383 parts of+Mg 2SiO 415 parts of (particle diameter 10 μm)+CaO, 1 part of+MgCl 21 part |
| Embodiment 5 | Al 2O 374 parts of+Mg 2SiO 415 parts of (particle diameter 10 μm)+CaO, 10 parts of+MgCl 21 part |
| Embodiment 6 | Al 2O 365 parts of+Mg 2SiO 48 parts of (particle diameter 10 μm)+CaO, 5 parts of+MgCl 25 parts |
| Embodiment 7 | Al 2O 382 parts of+Mg 2SiO 48 parts of (particle diameter 10 μm)+CaO, 5 parts of+MgCl 25 parts |
| Embodiment 8 | Al 2O 375 parts of+Mg 2SiO 415 parts of (particle diameter 0.1 μm)+CaO, 5 parts of+NaCl 5 parts |
| Embodiment 9 | Al 2O 378 parts of+Mg 2SiO 42 parts of (particle diameter 10 μm)+CaO, 10 parts of+MgCl 210 parts |
| Embodiment 10 | Al 2O 370 parts of+Mg 2SiO 410 parts of (particle diameter 0.1 μm)+CaO, 10 parts of+SrCl 210 parts |
| Embodiment 11 | Al 2O 380 parts of+Fe 2SiO 410 parts of (particle diameter 0.1 μm)+CaO, 5 parts of+MgCl 25 parts |
| Embodiment 12 | Al 2O 389 parts of+Mg 2SiO 44 parts of (particle diameter 0.1 μm)+CaO, 4 parts of+MgCl 23 parts |
| Embodiment 13 | Al 2O 385 parts of+Mg 2SiO 48 parts of (particle diameter 0.1 μm)+CaO, 4 parts of+MgCl 23 parts |
| Embodiment 14 | Al 2O 385 parts of+Mg 2SiO 44 parts of (particle diameter 0.1 μm)+CaO, 8 parts of+MgCl 23 parts |
| Embodiment 15 | Al 2O 383 parts of+Mg 2SiO 46 parts of (particle diameter 0.1 μm)+CaO, 3 parts of+CaCl 28 parts |
| Embodiment 16 | Al 2O 383 parts of+Mg 2SiO 46 parts of (particle diameter 0.1 μm)+CaO, 3 parts of+KCl 8 parts |
| Embodiment 17 | Al 2O 386 parts of+Na 4SiO 44 parts of (particle diameter 0.1 μm)+SrO, 6 parts of+MgCl 24 parts |
| Comparative example 1 | MgO 100 parts of+SiO 235 parts |
| Comparative example 2 | MgO 100 parts of+CaCl 210 parts |
| Comparative example 3 | Al 2O 3100 parts |
Table 2
The glassy membrane bottom formed in tradition grain-oriented silicon-iron high-temperature annealing process has higher hardness, reduces the punching performance of siliconized plate, adds to cause mould man-hour and to a certain degree damage.Further, oxide compound in the base pinning structure hinders the motion of neticdomain wall, causes adverse influence to magnetic property.Bottomless layer grain-oriented silicon-iron significantly can improve the processing characteristics of siliconized plate, and magnetic property also can improve because of the disappearance of pinning structure further, thus obtains ultralow-iron-loss product.
Before the present invention, obtain the method for mirror surface-oriented silicon steel mainly with MgO and muriate or Al
2o
3be main, both can cause the instability of magnetic property, and the latter can not remove the embedded oxide formed in decarburizing annealing process.Method is also had to adopt at Al
2o
3add muriate equally in separant, but muriate itself needs to be aided with certain moisture could react with embedded oxide, simultaneously thus removed.
The introducing silicate of the invention and alkaline earth metal oxide, silicate adds the reliability of purification steel, alkaline earth metal oxide itself has water-soluble, the amount of moisture brought in high temperature annealing can be controlled easily, method is convenient, can stablize the mirror surface-oriented silicon steel product obtaining high-quality.Equipment used is the conventional production equipment of oriented silicon steel, has splendid practicality and generalization, thus has good promotion prospect.
Claims (2)
1. there is the mirror surface-oriented silicon steel manufacture method of fine magnetic property, comprise the steps:
1) smelt
With converter or Electric furnace steel making, molten steel is after secondary refining and continuous casting, obtain blank plates of silicon steels, its composition by weight percent is: C:0.015 ~ 0.06%, Si:2.5 ~ 4.0%, acid-solubility Al:0.015 ~ 0.04%, Mn:0.06 ~ 0.45%, Cu:0.01 ~ 0.29%, S≤0.012%, N≤0.01%, and all the other are Fe and inevitable impurity;
2) hot rolling, normalizing
Heating of plate blank is to less than 1200 DEG C heating, and 1.5 ~ 3.0mm hot-rolled sheet is made in hot rolling; Carry out the normalizing annealing of 30 ~ 200s at 900 ~ 1150 DEG C, then carry out pickling;
3) cold rolling
With once or the above cold rolling process of secondary of band process annealing be rolled into the cold-reduced sheet of 0.20 ~ 0.35mm, final draft is greater than 80%, makes the cold-reduced sheet of 0.20 ~ 0.35mm;
4) decarburization, nitriding
Cold-reduced sheet N
2+ H
2carry out decarburizing annealing process in shielding gas, the carbon in steel plate is reduced to below 25ppm, formed with SiO at surface of steel plate simultaneously
2for the zone of oxidation of main component, Control for Oxygen Content 2.0g/m
2below; At the forward and backward of continuous decarburizing annealing or carry out continuous print Nitrizing Treatment by Control of Nitrogen Content at 150-350ppm simultaneously;
5) separant coating, high temperature annealing
At decarburization plate surface coated annealing separating agent, annealing separating agent composition quality percentage ratio is: Al
2o
3powder, 65-96 part, silicate powder, 2-15 part, its particle diameter between 0.1-100 μm, alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part; Wherein, silicate powder comprises Al
4(SiO
4)
3, CaSiO
3, Mg
2siO
4, Fe
2siO
4in more than one; Metal chloride comprises alkali metal chloride LiCl, NaCl, KCl, RbCl, alkaline earth metal chloride BeCl
2, MgCl
2, CaCl
2, SrCl
2, BaCl
2in more than one; Alkaline earth metal oxide comprise in BeO, MgO, CaO, SrO, BaO more than one;
Be nitrogen and hydrogen mixture in atmosphere after oven dry, 25% ~ 100%H
2, D.P.<0 DEG C, temperature is carry out the insulation high temperature annealing of more than 15 hours under the condition of 1150 ~ 1250 DEG C, then through being coated with insulating coating and stretching and leveling annealing obtains the minute surface grain-oriented silicon-iron product of excellent magnetic.
2., for the annealing separating agent that the mirror surface-oriented silicon steel with fine magnetic property manufactures, by mass percent, its component content is: Al
2o
3powder, 65-96 part, silicate powder, 2-15 part, its particle diameter is between 0.1-100 μm, and alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part, wherein, silicate powder comprises Al
4(SiO
4)
3, CaSiO
3, Mg
2siO
4, Fe
2siO
4in more than one; Metal chloride comprises alkali metal chloride LiCl, NaCl, KCl, RbCl, alkaline earth metal chloride BeCl
2, MgCl
2, CaCl
2, SrCl
2, BaCl
2in more than one; Alkaline earth metal oxide comprise in BeO, MgO, CaO, SrO, BaO more than one.
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| CN103525999A (en) * | 2013-09-13 | 2014-01-22 | 任振州 | Preparation method of high-magnetic-induction oriented silicon steel sheet |
| CN103937941B (en) * | 2013-12-27 | 2016-01-20 | 上海实业振泰化工有限公司 | A kind of oriented silicon steel preparation method of extraordinary magnesium oxide boron additive material |
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| CN109112395B (en) * | 2018-08-10 | 2020-02-07 | 全球能源互联网研究院有限公司 | Non-bottom-layer oriented ultrathin strip base material and preparation method thereof |
| CN109306198A (en) * | 2018-08-22 | 2019-02-05 | 武汉钢铁有限公司 | For improving the masking liquid and preparation method thereof of high magnetic induction grain-oriented silicon steel magnesium silicate bottom layer quality |
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| CN110369500A (en) * | 2019-07-09 | 2019-10-25 | 鞍钢股份有限公司 | A kind of disconnected band control method of oriented silicon steel cold-rolled |
| CN110983004B (en) * | 2019-12-04 | 2021-07-02 | 新万鑫（福建）精密薄板有限公司 | Production process of bottom-layer-free ultrathin strip oriented silicon steel master strip |
| KR102390830B1 (en) | 2019-12-20 | 2022-04-25 | 주식회사 포스코 | Annealing separating agent composition for grain oriented electrical steel sheet, grain oriented electrical steel sheet, and method for manufacturing the same |
| 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 |
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| US4255205A (en) * | 1978-12-27 | 1981-03-10 | Kawasaki Steel Corporation | Method of producing grain-oriented silicon steel sheets having substantially no glass film |
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| US4255205A (en) * | 1978-12-27 | 1981-03-10 | Kawasaki Steel Corporation | Method of producing grain-oriented silicon steel sheets having substantially no glass film |
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