CN103014285A - 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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- CN103014285A CN103014285A CN2011102999492A CN201110299949A CN103014285A CN 103014285 A CN103014285 A CN 103014285A CN 2011102999492 A CN2011102999492 A CN 2011102999492A CN 201110299949 A CN201110299949 A CN 201110299949A CN 103014285 A CN103014285 A CN 103014285A
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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 the 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 will be at H after process hot rolling, normalizing and cold-rolling treatment
2-N
2Carry out decarburizing annealing under the atmosphere protection, eliminate rolling stress, form primary recrystallization, logical moisture in the stove simultaneously, with carbon content control in the steel band below 30ppm, to prevent finished product generation magnetic aging.Oxidation can occur in steel strip surface during decarburizing annealing, forms with SiO
2And Fe
2SiO
4Be main zone of oxidation, further decarburization is caused disadvantageous effect.In follow-up 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 the steel band bonding and play the effect that purifies steel when high temperature annealing.
Oriented silicon steel surface magnesium silicate glass film bottom has higher hardness, causes the steel plate stamping piece performance relatively 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, increases magnetic hysteresis loss.
For punching performance and the further magnetic property that improves that improves grain-oriented silicon-iron, develop the grain-oriented silicon-iron without the glassy membrane bottom in the prior art.
Japan JFE company uses not the Al with the surface of steel plate reaction
2O
3Deng as the high temperature annealing separant, directly obtain the grain-oriented silicon-iron without the glassy membrane bottom.This method will be eliminated the nearly oxide on surface of steel plate fully and be mingled with the strict control of needs decarburization dew point and make surface of steel plate not form ferriferous oxide, but this will certainly bring the problems such as decarburization, nitriding.
U.S. Armco company adds SiO in magnesium oxide
2As annealing separating agent, the loose Magnesium Silicate q-agent that secondary recrystallization annealing process light plate surface forms is conducive to Annealing Protection gas and enters steel plate interlayer purification steel.But this method often is difficult to surperficial Magnesium Silicate q-agent is scrubbed off fully, the embedded oxide on the nearly surface of steel plate can not be eliminated fully, and is limited to reducing the core loss effect.
Japan NSC company adds muriate as annealing separating agent in magnesium oxide, add a large amount of muriates and in the secondary recrystallization annealing process surface of steel plate is caused certain corrosion, affects 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 annealing separating agent with fine magnetic property, from agent prescription, stable acquisition has excellent magnetic characteristics, the grain-oriented silicon-iron of any surface finish by control decarburizing annealing condition, use Novel disk withdrawal fire screen.
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, make high-temperature annealing process light plate surface not form the glassy membrane bottom, and can effectively purify steel, utilize simultaneously muriatic corrosion reaction to remove the embedded oxide on the nearly surface of substrate, thereby 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) smelts
With converter or Electric furnace steel making, molten steel is behind secondary refining and continuous casting, obtain blank plates of silicon steels, its composition 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%, all the other are Fe and inevitable impurity.
2) hot rolling, normalizing
Heating below the heating of plate blank to 1200 ℃, 1.5～3.0mm hot-rolled sheet is made in hot rolling; 900～1150 ℃ of normalizing annealings of carrying out 30～200s, then carry out pickling.
3) cold rolling
With once or be rolled into the cold-reduced sheet of 0.20～0.35mm with the above cold rolling process of the secondary of process annealing, final draft is made the cold-reduced sheet of 020～0.35mm greater than 80%;
4) decarburization, nitriding
Cold-reduced sheet N
2+ H
2Carry out decarburizing annealing in the shielding gas and process, the carbon in the steel plate is reduced to below the 25ppm, form with SiO at surface of steel plate simultaneously
2Be 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 simultaneously continuous nitriding and process Control of Nitrogen Content at 150-350ppm.
5) separant coating, high temperature annealing
At decarburization plate surface coated annealing separating agent, oven dry is nitrogen and hydrogen mixture in atmosphere afterwards, 25%～100%H
2, D.P.＜0 ℃, temperature is the high temperature annealing that is incubated under 1150～1250 ℃ the condition more than 15 hours, obtains the minute surface grain-oriented silicon-iron product of excellent magnetic through being coated with the annealing of insulating coating and stretching and leveling again.
The annealing separating agent that mirror surface-oriented silicon steel be used to having fine magnetic property of the present invention is made, its component content is: Al
2O
3Powder, 65-96 part, silicate powder, 2-15 part, its particle diameter between 0.1-100 μ m, 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 comprises among BeO, MgO, CaO, SrO, the 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 the oriented silicon steel that forms any surface finish.The silicate additive that exists with certain particle diameter state plays the effect that the impurity element diffusion admittance is provided in high temperature annealing, because the silicate of hydration status dehydration in the temperature-rise period, therefore can cause a fixed gap, be beneficial to that detrimental impurity spreads with gas form in the steel.Because Al
2O
3Do not give birth to reaction with steeping in water for reconstitution, if the silicate addition is less than 2%, or particle diameter is less than 0.1 μ m, and separant is too closely knit during high temperature annealing, can hinder elements such as magnetic harmful N, Se, S to external diffusion, causes the deteriorated of finished product magnetic property.If the silicate addition is greater than 15%, or particle diameter is greater than 100 μ m, then can be owing to emitting excess moisture, and cause the additional oxidation of steel plate, make the later stage oxidizing reaction be difficult to remove fully bottom, simultaneously particle diameter is crossed conference and is made too much chlorion go deep into the zone of oxidation base portion, and the etched the matrix with metal generation chemical reaction is difficult to obtain the mirror surface-oriented silicon steel of any surface finish.So the silicate addition should be controlled between 2%～15%, particle diameter should be controlled between 0.1m～100 μ m.
Alkaline earth metal oxide additives has two effects.On the one hand, when slurries are prepared and the water effect, form oxyhydroxide, the oxyhydroxide decomposition temperature is higher than 580 ℃, thereby make surface of steel plate under comparatively high temps, still have certain H+ to exist, form acidic solution with Cl-, this acidic solution can react with the surface of steel plate oxide compound, thereby 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 the matrix, thereby makes inner oxygen to external diffusion, and between forms clearly more demarcated interface, 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 fewly, can not accomplish to remove fully oxide on surface and embedded oxide; If addition greater than 10%, then can react with the metallic matrix corrosion.Therefore, the very few or too much smooth finish that all can affect finished surface of alkaline earth metal oxide additives addition considers, and its amount should be controlled between 1%～10%.
Be brought into metal chloride in the separant plays acid attack in high-temperature annealing process effect with certain compound form.Muriatic mass percent is lower than 1%, then can not remove zone of oxidation and embedded oxide fully, can not obtain the finished product oriented silicon steel of any surface finish; Be higher than 10%, the corrosion of metallic matrix then easily occurs, secondary recrystallization is affected and the magnetic property wild effect occurs, smooth finish that simultaneously also can injured surface.Answer this, muriatic addition should be controlled 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, have excellent magnetic property and punching performance.
Embodiment
The present invention will be further described below in conjunction with embodiment.
With 500kg vacuum oven steel-making, slab chemical composition (wt%) is: all the other are Fe and inevitable impurity 0.045%C, 3.25%Si, 0.006%S, 0.027%Als, 0.006%N, 0.15%Cu, 0.012%Mn.Steel billet is rolled into the thick hot-rolled sheet of 2.6mm after 1150 ℃ of lower heating.After 1 minute, pickling is the final thickness of slab 0.285mm of cold rolling one-tenth also through 1150 ℃ of normalizing annealings for hot-rolled sheet.Cold-reduced sheet is processed 835 ℃ of decarburizing annealings of carrying out 120 seconds, and surface oxygen content is 1.0 and 2.0g/m
2Two levels; After nitriding was processed, the nitrogen content of steel plate was 250ppm.Decarburizing annealing plate coating annealing separating agent, composition proportion sees Table 1, carries out 1200 ℃, 20 hours high temperature annealing of insulation after the rolling in the nitrogen of doing, hydrogen protective atmosphere; Anneal through being coated with insulating coating and stretching and leveling after the uncoiling.
Table 1
| Explanation | The separant prescription |
| Embodiment 1 | Al 2O 396 parts+Mg 2SiO 42 parts of (particle diameter 0.1 μ m)+1 part+MgCl of CaO 21 part |
| Embodiment 2 | Al 2O 396 parts+Mg 2SiO 42 parts of (particle diameter 100 μ m)+1 part+MgCl of CaO 21 part |
| Embodiment 3 | Al 2O 365 parts+Mg 2SiO 415 parts of (particle diameter 100 μ m)+10 parts+MgCl of CaO 210 parts |
| Embodiment 4 | Al 2O 383 parts+Mg 2SiO 415 parts of (particle diameter 10 μ m)+1 part+MgCl of CaO 21 part |
| Embodiment 5 | Al 2O 374 parts+Mg 2SiO 415 parts of (particle diameter 10 μ m)+10 parts+MgCl of CaO 21 part |
| Embodiment 6 | Al 2O 365 parts+Mg 2SiO 48 parts of (particle diameter 10 μ m)+5 parts+MgCl of CaO 25 parts |
| Embodiment 7 | Al 2O 382 parts+Mg 2SiO 48 parts of (particle diameter 10 μ m)+5 parts+MgCl of CaO 25 parts |
| Embodiment 8 | Al 2O 375 parts+Mg 2SiO 45 parts of 15 parts of (particle diameter 0.1 μ m)+5 parts+NaCl of CaO |
| Embodiment 9 | Al 2O 378 parts+Mg 2SiO 42 parts of (particle diameter 10 μ m)+10 parts+MgCl of CaO 210 parts |
| Embodiment 10 | Al 2O 370 parts+Mg 2SiO 410 parts of (particle diameter 0.1 μ m)+10 parts+SrCl of CaO 210 parts |
| Embodiment 11 | Al 2O 380 parts+Fe 2SiO 410 parts of (particle diameter 0.1 μ m)+5 parts+MgCl of CaO 25 parts |
| Embodiment 12 | Al 2O 389 parts+Mg 2SiO 44 parts of (particle diameter 0.1 μ m)+4 parts+MgCl of CaO 23 parts |
| Embodiment 13 | Al 2O 385 parts+Mg 2SiO 48 parts of (particle diameter 0.1 μ m)+4 parts+MgCl of CaO 23 parts |
| Embodiment 14 | Al 2O 385 parts+Mg 2SiO 44 parts of (particle diameter 0.1 μ m)+8 parts+MgCl of CaO 23 parts |
| Embodiment 15 | Al 2O 383 parts+Mg 2SiO 46 parts of (particle diameter 0.1 μ m)+3 parts+CaCl of CaO 28 parts |
| Embodiment 16 | Al 2O 383 parts+Mg 2SiO 48 parts of 6 parts of (particle diameter 0.1 μ m)+3 parts+KCl of CaO |
| Embodiment 17 | Al 2O 386 parts+Na 4SiO 44 parts of (particle diameter 0.1 μ m)+6 parts+MgCl of SrO 24 parts |
| Comparative example 1 | 100 parts+SiO of MgO 235 parts |
| Comparative example 2 | 100 parts+CaCl of MgO 210 parts |
| Comparative example 3 | Al 2O 3100 parts |
Table 2
The glassy membrane bottom that forms in the tradition grain-oriented silicon-iron high-temperature annealing process has higher hardness, reduces the punching performance of siliconized plate, adds can cause to a certain degree damage to mould man-hour.And oxide compound pinning structure in matrix has hindered the motion of neticdomain wall, and magnetic property is caused adverse influence.Bottomless layer crystal grain oriented silicon steel can significantly improve the processing characteristics of siliconized plate, and magnetic property also can further improve because of the disappearance of pinning structure, thereby obtains the 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 unstable of magnetic property, and the latter can not remove the embedded oxide that forms in the decarburizing annealing process.Also have method to adopt at Al
2O
3The same muriate that adds could react with embedded oxide but muriate itself need to be aided with certain moisture, thereby simultaneously it be removed in the separant.
Introducing silicate and the alkaline earth metal oxide of the invention, silicate has increased the reliability that purifies steel, alkaline earth metal oxide itself has water-soluble, can control at an easy rate the amount of moisture of bringing in the high temperature annealing, method is convenient, can stablize the mirror surface-oriented silicon steel product that obtains high-quality.Equipment used is the conventional production unit of oriented silicon steel, has splendid practicality and generalization, thereby has good promotion prospect.
Claims (9)
1. have the mirror surface-oriented silicon steel manufacture method of fine magnetic property, comprise the steps:
1) smelts
With converter or Electric furnace steel making, molten steel is behind secondary refining and continuous casting, obtain blank plates of silicon steels, its composition 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 below the heating of plate blank to 1200 ℃, 1.5～3.0mm hot-rolled sheet is made in hot rolling; 900～1150 ℃ of normalizing annealings of carrying out 30～200s, then carry out pickling;
3) cold rolling
With once or be rolled into the cold-reduced sheet of 0.20～0.35mm with the above cold rolling process of the secondary of process annealing, final draft is made the cold-reduced sheet of 0.20～0.35mm greater than 80%;
4) decarburization, nitriding
Cold-reduced sheet N
2+ H
2Carry out decarburizing annealing in the shielding gas and process, the carbon in the steel plate is reduced to below the 25ppm, form with SiO at surface of steel plate simultaneously
2Be 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 simultaneously continuous nitriding and process Control of Nitrogen Content at 150-350ppm;
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 μ m, alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part; Oven dry is nitrogen and hydrogen mixture in atmosphere afterwards, 25%～100%H
2, D.P.＜0 ℃, temperature is the high temperature annealing that is incubated under 1150～1250 ℃ the condition more than 15 hours, obtains the minute surface grain-oriented silicon-iron product of excellent magnetic through being coated with the annealing of insulating coating and stretching and leveling again.
2. the mirror surface-oriented silicon steel manufacture method with fine magnetic property as claimed in claim 1 is characterized in that, the decarburizing annealing surface of steel plate forms with SiO
2Be the zone of oxidation of main component, Control for Oxygen Content is at 2.0g/m
2Below.
3. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 1 is characterized in that, silicate powder comprises Al4 (SiO
4)
3, CaSiO
3, Mg
2SiO
4, Fe
2SiO
4In more than one.
4. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 1 is characterized in that, 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.
5. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 1 is characterized in that, alkaline earth metal oxide comprises more than one among BeO, MgO, CaO, SrO, the BaO.
6. the annealing separating agent of making for the mirror surface-oriented silicon steel with fine magnetic property is pressed mass percent, and its component content is: Al
2O
3Powder, 65-96 part, silicate powder, 2-15 part, its particle diameter between 0.1-100 μ m, alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part.
7. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 6 is characterized in that, silicate powder comprises Al4 (SiO
4)
3, CaSiO
3, Mg
2SiO
4, Fe
2SiO
4In more than one.
8. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 6 is characterized in that, 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.
9. the annealing separating agent of the mirror surface-oriented silicon steel manufacturing be used to having fine magnetic property as claimed in claim 6 is characterized in that, alkaline earth metal oxide comprises more than one among BeO, MgO, CaO, SrO, the BaO.
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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 |
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| CN107002158B (en) * | 2014-11-26 | 2019-06-18 | Posco公司 | The manufacturing method of oriented electrical steel annealing separator composition and the oriented electrical steel using it |
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| US11773462B2 (en) | 2016-12-22 | 2023-10-03 | Posco Co., Ltd | Annealing separator composition for grain-oriented electrical steel sheet, grain-oriented electrical steel sheet, and method for producing grain-oriented electrical steel sheet |
| US11830533B2 (en) | 2018-03-30 | 2023-11-28 | Sony Corporation | Method of producing magnetic powder and method of producing magnetic recording medium |
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| CN103014285B (en) | 2015-04-01 |
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