CN102952931B - Glass-film-free oriented silicon steel manufacture method and annealing isolation agent - Google Patents
Glass-film-free oriented silicon steel manufacture method and annealing isolation agent Download PDFInfo
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- CN102952931B CN102952931B CN201110253467.3A CN201110253467A CN102952931B CN 102952931 B CN102952931 B CN 102952931B CN 201110253467 A CN201110253467 A CN 201110253467A CN 102952931 B CN102952931 B CN 102952931B
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Abstract
The invention discloses a glass-film-free oriented silicon steel manufacture method. The method comprises the following steps of: (1) smelting; (2) hot rolling and normalizing; (3) cold rolling; (4) decarburization and nitriding, wherein a cold-rolled sheet is subjected to decarburization annealing treatment in wet N2+H2 protective gas at 800 to 860 DEG C, and oxidation energy is controlled within 0.16 to 0.40; carbon in the steel sheet can be reduced to below 30ppm by the decarburization annealing treatment while an oxide layer mainly containing SiO2 is formed on the surface of the steel sheet, and the single-side oxygen content of the steel sheet is controlled to below 0.7g/m<2>; and continuous nitriding treatment is carried out on the steel sheet in ammonia-contained N2+H2 protective gas with oxidation energy of 0.05 to 0.15 to control the nitrogen content of the steel sheet within 180ppm to 280ppm; (5) application of an isolation agent; (6) high-temperature annealing and temperature rising and maintenance, wherein the steel sheet is heated to 1150 to 1250 DEG C in dry N2+H2 mixed atmosphere containing 50% to 90% of N2 and H2, is maintained at the 1150 to 1250 DEG C in pure hydrogen atmosphere for above 15 hours; and (7) coating of an insulation coating, stretching, leveling and annealing, thus obtaining the grain-oriented silicon steel product with an excellent magnetic property.
Description
Technical field
The present invention relates to oriented silicon steel manufacture method, particularly a kind of without glassy membrane oriented silicon steel manufacture method and annealing separating agent.
Background technology
During grain-oriented silicon-iron is produced, steel plate need be at wet H
2-N
2in protective atmosphere, carry out continuous decarburizing annealing processing.Object is that carbon in steel plate is dropped to below 30ppm, to prevent finished product generation magnetic aging.Form with SiO on decarburizing annealing process light plate surface
2and Fe
2siO
4be main zone of oxidation, in secondary recrystallization annealing process, react with the magnesium oxide generation solid-state diffusion of surface of steel plate coating: 2MgO+SiO
2→ Mg
2siO
4, form magnesium silicate glass film bottom.Magnesium silicate glass film bottom can prevent that steel plate from boning and playing the effect that purifies steel; Glassy membrane bottom and the tensile coating applying thereon insulate and tension force effect for final finished provides.
Grain-oriented silicon-iron surface magnesium silicate glass film bottom has high hardness, causes product punching poor performance.The nearly oxide on surface of the rough interfaces of glassy membrane bottom and matrix and steel plate is mingled with the movement of neticdomain wall is had to inhibition, is unfavorable for the further reduction of core loss.In order to improve grain-oriented silicon-iron punching performance, to reduce core loss, develop the grain-oriented silicon-iron without glassy membrane bottom.
Japanese Patent JP49096920 removes oriented silicon steel Surface glass films bottom by the method for pickling, but to wash glassy membrane bottom completely off and comprise oxide inclusion, need in strong acid, soak for a long time and wash approximately 10 μ m thickness table surface layers off, manufacturing cost high and the aspect such as medicine management and environmental pollution exist larger problem.
US Patent No. 3785882 adopts not the thick Al reacting with surface of steel plate oxide film
2o
3substitute MgO as annealing separating agent.In secondary recrystallization annealing process as the Al of annealing separating agent
2o
3do not react with surface of steel plate, can directly obtain without glassy membrane bottom product.But this method still can not be eliminated the nearly oxide on surface of steel plate completely and be mingled with.
US Patent No. 554719 is used MgO+SiO
2as annealing separating agent, form loose Magnesium Silicate q-agent on secondary recrystallization annealing process light plate surface, by scrubbing, surface porosity Magnesium Silicate q-agent is removed, obtain without glassy membrane bottom product.
Japanese Patent JP08269560A uses and adds muriatic magnesium oxide as annealing separating agent, passes through surface reaction: MCl
2+ Fe+ (1/2) O
2→ MO+FeCl
2individual, will form glassy membrane layer removing, obtain without glassy membrane bottom product.
US Patent No. 3785882 is used particle diameter for 100-400 order aluminum oxide is as annealing separating agent, is difficult to be coated in surface of steel plate by the mode of preparation slurry.In high-temperature annealing process, thick aluminum oxide easily causes the impression of surface of steel plate.
Chinese patent CN03802019.X is not forming ferriferous oxide (Fe
2siO
4, FeO etc.) atmospheric condition carrying out decarburizing annealing.Surface of steel plate forms fine and close SiO
2external oxidation layer, certainly will will cause decarburization difficulty.For the low temperature process that will form inhibitor by continuous nitriding mode the day after tomorrow, the zone of oxidation of surface compact also will cause nitriding extremely difficult.
US Patent No. 554719 is added 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 is often difficult to surperficial Magnesium Silicate q-agent to scrub off the product that obtains smooth finish surface completely, adopt this method the oxide inclusion on the nearly surface of steel plate can not be eliminated completely.
Japanese Patent JP08269560A adds muriate as annealing separating agent in magnesium oxide, adds a large amount of muriates, in secondary recrystallization annealing process, surface of steel plate is caused to 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 without glassy membrane oriented silicon steel manufacture method and annealing separating agent, overcome above-mentioned prior art deficiency, by controlling decarburizing annealing condition and high temperature annealing condition, use Novel disk withdrawal fire screen from agent prescription stable obtain have excellent magnetic characteristics, without the manufacture method of glassy membrane bottom grain-oriented silicon-iron.
For achieving the above object, technical scheme of the present invention is:
The present invention adds the aluminum oxide of low melting point oxide and/or magnesium oxide powder as high temperature annealing separant by use, and strictly control annealing process condition, directly obtain any surface finish and magnetic property stable product, thereby overcome the deficiency existing in foregoing invention.The liquid phase forming in separant in high-temperature annealing process can play sealing gland effect, suppress solid solution nitrogen and overflow from steel plate, thereby the stable and secondary recrystallization of protection inhibitor is perfect.The liquid phase forming also plays dissolves the effect of surface of steel plate oxide compound, thereby obtains the residual product of any surface finish oxide-free.
Particularly, of the present invention without glassy membrane oriented silicon steel manufacture method, it comprises the steps:
1) smelt
With converter or Electric furnace steel making, molten steel is after secondary refining and continuous casting, the composition weight percent that obtains blank plates of silicon steels is: C:0.015～0.06%, Si:2.5～4.0%, Als:0.015～0.04%, Mn:0.06～0.45%, S≤0.012%, N≤0.01%, and all the other are Fe and inevitable impurity;
2) hot rolling, normalizing
Below heating of plate blank to 1200 DEG C, 1.5～3.0mm hot-rolled sheet is made in hot rolling; Hot-rolled sheet carries out the normalizing annealing of 30～200s at 900～1150 DEG C, then carries out pickling;
3) cold rolling
Be rolled into the cold-reduced sheet of 0.20～0.50mm by once cold rolling method, final draft is greater than 80%;
4) decarburization, nitriding
Cold-reduced sheet is at 800～860 DEG C of wet N
2+ H
2in shielding gas, carry out decarburizing annealing processing, energy of oxidation p (H
2o)/p (H
2) be controlled at 0.16～0.40; By decarburizing annealing, the carbon in steel plate is reduced to below 30ppm, forms with SiO at surface of steel plate simultaneously
2for the zone of oxidation of main component, and by one side Control for Oxygen Content at 0.7g/m
2below; Then at the energy of oxidation p (H containing ammonia
2o)/p (H
2) be the N of 0.05-0.15
2+ H
2in shielding gas, carry out continuous nitriding processing, by Control of Nitrogen Content at 180-280ppm;
5) separant coating
Add the B of low melting point in decarburization plate surface-coated
2o
3, H
3bO
3, Na
2b
4o
7boron compound or Sb
2(SO
4)
3, Bi
2o
3, BiOCl aluminum oxide and/or magnesium oxide powder, consist of: the aluminum oxide of 100 parts of weight and/or magnesium oxide powder, the B of 0.5～5 part of weight
2o
3, H
3bO
3, Na
2b
4o
7boron compound or Sb
2(SO
4)
3, Bi
2o
3, BiOCl boron compound in more than one, the magnesium oxide citric acid used row CAA value of living is greater than 80s;
6) high temperature annealing
First heat up, the section that heats up atmosphere is dry nitrogen and hydrogen mixture atmosphere, and wherein nitrogen ratios is controlled at 50～90%, is warming up to 1150～1250 DEG C; Then insulation, 1150～1250 DEG C of holding temperatures, insulation atmosphere is pure hydrogen, soaking time is more than 15 hours;
7) painting insulating coating and stretching and leveling annealing obtain the grain-oriented silicon-iron product of excellent magnetic.
In step 4) in decarburization, nitriding process,
1. decarburizing annealing operation energy of oxidation p (H
2o)/p (H
2) determine the structure of zone of oxidation.Energy of oxidation p (H
2o)/p (H
2) lower than 0.15, form fine and close SiO
2zone of oxidation will cause decarburization difficulty (carbon content is high will be affected grain-size of decarburization plate and cause the finished product magnetic aging); Also affect nitriding efficiency, be difficult to infiltrate enough nitrogen (180～280ppm) at surface of steel plate simultaneously.Energy of oxidation p (H
2o)/p (H
2) higher than 0.40, the oxidation bed thickness of formation and loose; This will cause in high-temperature annealing process inhibitor unstable, and be difficult to completely clean to bottom or oxide removal, can not get any surface finish without bottom oriented silicon steel.
2. decarburizing annealing plate surface oxidation too high levels, is difficult to completely clean to bottom or oxide removal at high-temperature annealing process, can not get any surface finish without bottom oriented silicon steel.
3. with respect to dry gas atmosphere, in wet atmosphere, carry out nitriding and can significantly improve nitriding efficiency.
In the separant of the present invention's coating,
● aluminum oxide and/or magnesium oxide powder are coated in surface of steel plate and play main separant effect.Because can producing hydrolysis in the process of preparation slurry, MgO forms Mg (OH)
2, Mg in high-temperature annealing process (OH)
2the aqueous vapor that generation decomposition discharges can cause the further oxidation (this oxidation is disadvantageous to forming without low layer oriented silicon steel) of steel plate.Citric acid activity is an index that characterizes magnesium oxide hydrolysis, the high hydrolysis difficulty relatively that shows of citric acid activity value.
● B
2o
3, H
3bO
3, Na
2b
4o
7deng boron compound or Sb
2(SO
4)
3, Bi
2o
3, the low melting component such as BiOCl first forms liquid phase and can dissolve the oxide compound of surface of steel plate at high temperature, and to the corrosive nature of surface of steel plate can directly obtain surface be mirror-like without bottom oriented silicon steel; Also be conducive to the raising of magnetic property simultaneously.
In high-temperature annealing process of the present invention, improve the section N that heats up
2ratio can prevent from entering the nitrogen effusion of surface of steel plate in nitriding process, improves the stability of secondary recrystallization.
The present invention is without glassy membrane oriented silicon steel manufacture annealing separating agent, and it consists of: 100 parts of weight, aluminum oxide and/or magnesium oxide powder, 0.5～5 part of weight, B
2o
3, H
3bO
3, Na
2b
4o
7, Sb
2(SO
4)
3, Bi
2o
3, more than one in BiOCl.
Further, the active CAA value of described magnesium oxide citric acid is greater than 80s.
Beneficial effect of the present invention
In separant used in the present invention, add boron compound or the Sb of low melting point
2(SO
4)
3, Bi
2o
3, the liquid phase that forms in high-temperature annealing process such as BiOCl plays " sealing gland " effect, prevent that in steel plate, solid solution nitrogen is overflowed, thereby ensure that secondary recrystallization is perfect; Surface of steel plate form liquid phase can dissolve surface of steel plate oxide compound, thereby obtain smooth finish surface without bottom product.Can obtain any surface finish and the stable bottomless layer crystal grain oriented silicon steel of magnetic property by the present invention, there is excellent magnetic property and processing characteristics.
The invention has the advantages that:
1, decarburizing annealing energy of oxidation p (H
2o)/p (H
2) be controlled between 0.16-0.40, obtain thin and fine and close zone of oxidation and can ensure decarburization efficiency simultaneously.Carbon in steel plate is taken off to 30ppm, prevent magnetic aging and form suitable primary recrystallization grain-size.
2, because surface forms a certain amount of ferriferous oxide external oxidation layer, with respect to only forming fine and close SiO
2the situation nitriding efficiency of external oxidation layer significantly improves; Under wet atmospheric condition, nitriding has also significantly improved nitriding efficiency.The invention solves the technical problem that is difficult to nitriding without bottom orientation silicon steel process.
3, in separant, add boron compound or Sb
2(SO
4)
3, Bi
2o
3, BiOCl etc., the liquid phase forming in high-temperature annealing process play that " sealing gland " effect can prevent in steel plate that solid solution nitrogen is overflowed or atmosphere in nitrogen infiltrate in steel plate, thereby ensure the stable sufficient product of secondary recrystallization that obtains of inhibitor.Surface of steel plate form liquid phase can in high-temperature annealing process, eliminate surface of steel plate residual oxide completely, can obtain any surface finish without bottom product.
4, control a high temperature annealing intensification section nitrogen partial pressure, be conducive to the solid solution nitrogen in steel sheet, ensure improving of secondary recrystallization and stablizing of magnetic property.
Brief description of the drawings
Fig. 1 is that separant forms the schematic diagram on the impact of substrate solid solution nitrogen in high-temperature annealing process.
Fig. 2 is the schematic diagram of high temperature annealing intensification section a nitrogen content on substrate solid solution nitrogen impact in high-temperature annealing process.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
With 500kg vacuum oven steel-making, slab chemical composition (Wt%) is: all the other are Fe and inevitable impurity for 0.051%C, 3.25%Si, 0.006%S, 0.028%Als, 0.006%N, 0.011%Mn.Steel billet is rolled into the hot-rolled sheet that 2.5mm is thick after heating at 1150 DEG C.Hot-rolled sheet is through 1150 DEG C of normalizing annealings after 1 minute, and pickling is the final thickness of slab 0.225mm of cold rolling one-tenth also.Cold-reduced sheet is at energy of oxidation p (H
2o)/p (H
2) be 0.152 and temperature be the decarburizing annealing processing of carrying out under 835 DEG C of conditions 120 seconds; Then in the nitrogen hydrogen protective atmosphere of wet logical ammonia, carry out continuous nitriding processing.Decarburizing annealing plate coating annealing separating agent carries out 1200 DEG C, the insulation high temperature annealing of 20 hours in dry nitrogen hydrogen protective atmosphere after rolling, the section that heats up atmosphere is 75%N
2+ 25%H
2, high holding-zone switches to 100%H
2atmosphere; After uncoiling, anneal through being coated with insulating coating and stretching and leveling.
Finished product outward appearance and magnetic property are in table 2.
The standard of evaluating provides as follows:
With × represent that finished product surface oxygen content exceedes 0.2g/m
2, represent that with zero finished product surface oxygen content is no more than 0.2g/m
2, with × represent that finished product magnetic induction density, lower than 1.88T, represents that with △ finished product magnetic induction density is between 1.88-1.92T, represent that with zero finished product magnetic induction density is higher than 1.92T.
Table 2: separant formula is on Surface Quality and magnetic property impact
As shown in Figure 1, showing to add in aluminum oxide separant low melting component, to be conducive to substrate solid solution nitrogen stable.
Embodiment 2
With 500kg vacuum oven steel-making, slab chemical composition (Wt%) is: all the other are Fe and inevitable impurity for 0.051%C, 3.25%Si, 0.006%S, 0.028%Als, 0.006%N, 0.011%Mn.Steel billet is rolled into the hot-rolled sheet that 2.5mm is thick after heating at 1150 DEG C.Hot-rolled sheet is through 1150 DEG C of normalizing annealings after 1 minute, and pickling is the final thickness of slab 0.225mm of cold rolling one-tenth also.Cold-reduced sheet carries out the decarburizing annealing processing of 120 seconds under 835 DEG C of conditions; It is through nitriding processing that the nitrogen hydrogen of the logical ammonia then wetting is blended in energy of oxidation.The coating of decarburizing annealing plate consists of 80 parts of Al
2o
3+ 20 parts of MgO+2 part BiOCl annealing separating agents carry out 1200 DEG C, the insulation high temperature annealing of 20 hours in dry nitrogen, hydrogen protective atmosphere after rolling, the section that heats up atmosphere is nitrogen hydrogen mixeding gas, and high holding-zone switches to 100%H
2atmosphere; After uncoiling, anneal through being coated with insulating coating and stretching and leveling.
Table 3: decarburizing annealing energy of oxidation Surface Quality and magnetic property impact
As shown in Figure 2, it shows to increase a nitrogen content in high temperature annealing intensification section atmosphere and is conducive to the stable of substrate solid solution nitrogen.
Tradition grain-oriented silicon-iron Surface glass films bottom is mingled with the movement of neticdomain wall is had to inhibition with matrix rough interfaces and the nearly oxide on surface of steel plate, worsens magnetic property, is unfavorable for the further reduction of core loss; Surface inorganic matter glassy membrane bottom hardness is high, wearing and tearing processing mold.Obtain ultralow-iron-loss product without glassy membrane bottom grain-oriented silicon-iron can significantly improve magnetic property, and can improve the processing characteristics of product.At present without glassy membrane bottom grain-oriented silicon-iron technique still have that magnetic property is unstable, Magnesium Silicate q-agent bottom and nearly oxide on surface be mingled with and be difficult to remove completely and directly obtain the problems such as smooth finish surface high temperature annealing product.
Method of the present invention has solved the problems referred to above effectively, by optimize separant formula and control annealing conditions directly obtained any surface finish without glassy membrane bottom high temperature annealing finished product.Product magnetic property is stablized, can be obtained ultralow-iron-loss product, and processing characteristics is good.The present invention realizes technology and control is simple, the conventional production unit that equipment used is oriented silicon steel, thereby there is good popularizing application prospect.
Claims (2)
1. without a glassy membrane oriented silicon steel manufacture method, it comprises the steps:
1) smelt
With converter or Electric furnace steel making, molten steel is after secondary refining and continuous casting, the composition weight percent that obtains blank plates of silicon steels is: C:0.015～0.06%, Si:2.5～4.0%, Als:0.015～0.04%, Mn:0.06～0.45%, S≤0.012%, N≤0.01%, and all the other are Fe and inevitable impurity;
2) hot rolling, normalizing
Below heating of plate blank to 1200 DEG C, 1.5～3.0mm hot-rolled sheet is made in hot rolling; Hot-rolled sheet carries out the normalizing annealing of 30～200s at 900～1150 DEG C, then carries out pickling;
3) cold rolling
Be rolled into the cold-reduced sheet of 0.20～0.50mm by once cold rolling method, final draft is greater than 80%;
4) decarburization, nitriding
Cold-reduced sheet is at 800～860 DEG C of wet N
2+ H
2in shielding gas, carry out decarburizing annealing processing, energy of oxidation p (H
2o)/p (H
2) be controlled at 0.16～0.40; By decarburizing annealing, the carbon in steel plate is reduced to below 30ppm, forms with SiO at surface of steel plate simultaneously
2for the zone of oxidation of main component, and by one side Control for Oxygen Content at 0.7g/m
2below; Then at the energy of oxidation p (H containing ammonia
2o)/p (H
2) be 0.05～0.15 N
2+ H
2in shielding gas, carry out continuous nitriding processing, by Control of Nitrogen Content at 180～280ppm;
5) separant coating
The separant that adds low melting point in decarburization plate surface-coated, separant consists of: the aluminum oxide of 100 parts of weight and/or magnesium oxide powder, the B of 0.5～5 part of weight
2o
3, H
3bO
3, Na
2b
4o
7, Sb
2(SO
4)
3, Bi
2o
3, more than one in BiOCl;
6) high temperature annealing
First heat up, the section that heats up atmosphere is dry nitrogen and hydrogen mixture atmosphere, and wherein nitrogen ratios is controlled at 50～90%, is warming up to 1150～1250 DEG C; Then insulation, 1150～1250 DEG C of holding temperatures, insulation atmosphere is pure hydrogen, soaking time is more than 15 hours;
7) painting insulating coating and stretching and leveling annealing obtain the grain-oriented silicon-iron product of excellent magnetic.
2. as claimed in claim 1ly it is characterized in that without glassy membrane oriented silicon steel manufacture method, the active CAA value of magnesium oxide citric acid in described separant is greater than 80s.
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| 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 |
| CN104928567A (en) * | 2015-06-25 | 2015-09-23 | 宝山钢铁股份有限公司 | Grain-oriented silicon steel with good machining performance and production method thereof |
| CN105154646B (en) * | 2015-10-23 | 2018-06-08 | 武汉钢铁有限公司 | A kind of high magnetic induction grain-oriented silicon steel annealing separating agent and preparation method |
| CN107746929A (en) * | 2017-11-23 | 2018-03-02 | 武汉钢铁有限公司 | High magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced |
| CN108193032B (en) * | 2017-12-30 | 2019-11-15 | 新万鑫（福建）精密薄板有限公司 | A kind of magnesia annealing separating agent and coating processes improving orientation silicon steel surface quality |
| JP7269505B2 (en) * | 2019-01-16 | 2023-05-09 | 日本製鉄株式会社 | Manufacturing method of grain-oriented electrical steel sheet |
| US11946113B2 (en) * | 2019-01-16 | 2024-04-02 | Nippon Steel Corporation | Method for producing grain oriented electrical steel sheet |
| CN110643801A (en) * | 2019-10-31 | 2020-01-03 | 重庆望变电气（集团）股份有限公司 | High magnetic induction oriented steel treatment process |
| 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 |
| CN112646966B (en) * | 2020-12-17 | 2023-01-10 | 首钢智新迁安电磁材料有限公司 | Preparation method of non-bottom-layer oriented silicon steel and product thereof |
| CN112746150A (en) * | 2020-12-24 | 2021-05-04 | 吉林大学 | Method for improving oxidation resistance of iron-based automobile part |
| CN113211325B (en) * | 2021-05-07 | 2022-07-12 | 包头市威丰稀土电磁材料股份有限公司 | Method for preparing non-bottom-layer raw material of oriented silicon steel thin strip in physical sand blasting mode |
| CN115058682A (en) * | 2021-12-16 | 2022-09-16 | 刘鹏程 | Method for improving nitriding efficiency of high-magnetic induction oriented silicon steel |
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