CN100389222C - Production method for improving electromagnetic performance and bottom layer quality of copper containing orientation silicium steel - Google Patents
Production method for improving electromagnetic performance and bottom layer quality of copper containing orientation silicium steel Download PDFInfo
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- CN100389222C CN100389222C CNB2005100200032A CN200510020003A CN100389222C CN 100389222 C CN100389222 C CN 100389222C CN B2005100200032 A CNB2005100200032 A CN B2005100200032A CN 200510020003 A CN200510020003 A CN 200510020003A CN 100389222 C CN100389222 C CN 100389222C
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Abstract
The present invention discloses a production method for improving electromagnetic properties and bottom quality of coppery oriented silicon steel plates. The present invention solves the problems of poor magnetic properties as well as poor and unstable bottom quality of the existing oriented silicon steel technology which mainly uses aluminium nitride and copper as inhibitors. The technical measure comprises the production method for improving electromagnetic properties and bottom quality of coppery oriented silicon steel plates. The present invention comprises the steps that primary cold rolling of silicon steel plates with the thickness from 1.8 to 2.8mm is carried out after the silicon steel plates are pickled, and the thickness of the rolled silicon steel plates is from 0.50 to 0.70mm; the intermediate complete decarburizing annealing is carried out, and the oxygen content of the silicon steel plates are from 300 to 750 ppm; the secondary cold rolling is carried out, and the silicon steel plates are rolled to the end thickness; the recovery annealing of the silicon steel plates is carried out at the temperature of 400 to 595 DEG C in nitrogen hydrogen atmosphere, the voltage ratio of which is smaller than 0.61; annealing isolating agents which comprise magnesia as main components are coated; the annealing is carried out at the temperature below 1200 DEG C; the stretching levelling annealing is carried out after the uncoiling, and insulating coatings are coated at the same time.
Description
Technical field
The present invention relates to the production method of silicon steel sheet, especially belong to the production method that raising oriented silicon steel bearing copper plate electromagnetic performance and bottom layer quality, employing contain middle gross decarburization annealing and twice cold-rolling practice.
Background technology
60 to late nineteen seventies, adopt aluminium nitride and copper as inhibitor, and after the oriented silicon steel with low hot rolling operation slab heating temperature is developed, because what it adopted is twice cold-rolling practice of gross decarburization annealed in the middle of containing, promptly hot-rolled sheet is being carried out twice cold rolling pilot process, once be referred to as the thermal treatment of process annealing, when process annealing, the carbon amount in the steel plate is reduced to (gross decarburization annealing in the middle of being referred to as) below the 30ppm, be cold rolled to for the second time directly to be coated with the magnesium oxide annealing separating agent or after low temperature recovery annealing, to be coated with the magnesium oxide annealing separating agent behind the finished product thickness and carry out high temperature annealing and subsequent disposal, but the bottom layer quality of finished product is difficult to improve always.
Comparatively sophisticated at present general directional silicon steel (is the CGO steel; mainly with MnS as inhibitor) or the high magnetic induction grain-oriented silicon steel plate (be the Hi-B steel; mainly with MnS+AlN as inhibitor) means that obtain good bottom be by with cold-rolling of steel plate to finished product thickness; decarburizing annealing or surface treatment that employing is implemented under the protective atmosphere at comparatively high temps (being generally 820～870 ℃) are annealed, and can obtain good SiO on the surface of steel plate
2Layer finally obtains good Magnesium Silicate q-agent bottom at surface of steel plate behind high temperature annealing.Can obtain good finished surface insulation layer effect after being coated with insulating coating on this basis.But hot rolling heating need carried out more than 1360 ℃, causes like this that equipment damages easily under hot conditions, and fault is more, and the energy consumption height yields poorly, the high deficiency of production cost.
Because finished product Magnesium Silicate q-agent bottom layer quality is bad, to cause the finished product insulating coating of poor quality, this make on the one hand insulating coating to the tension force effect of steel plate because of can not get bringing into play the raising that has influence on finished product magnetic, the electromagnetic core that also can cause on the other hand making with this siliconized plate increases because of siliconized plate layer insulation weak effect makes its loss.Therefore, for many years, the researchist has carried out number of research projects to obtain good, the uniform product of insulating coating of finished surface bottom layer quality both at home and abroad.Russia's document (с т а л ь, 2001.5 P57～59) has been mentioned such as methods such as adopting high aquation rate magnesium oxide, the middle decarburizing annealing technology of adjustment and interpolation magnesium oxide additive and has been improved methods such as bottom layer quality.These methods can make moderate progress to the bottom layer quality of finished product to a certain extent, but still have more problem:
Usually, general oriented silicon steel (CGO) or high magnetic induction grain-oriented silicon steel (Hi-B) through decarburizing annealing or surface treatment annealing, can form one deck than the close SiO of Jun Yun Er Cause under near the wet type nitrogen nitrogen atmosphere 840 ℃ after being cold rolled to finished product thickness
2, the Magnesium Silicate q-agent bottom is in about 950～1100 ℃ of temperature ranges of high temperature annealing stage, by the SiO of surface of steel plate
2With the formation that reacts of MgO separant, therefore, the quality of formed bottom layer quality depends on that to a great extent the Magnesium Silicate q-agent bottom forms the SiO on front spring surface
2Whether the quality that layer forms is good.Steel plate is implemented this decarburizing annealing of nitrogen nitrogen atmosphere or surface treatment annealing about 840 ℃ before coating magnesium oxide separant be to help forming good SiO most
2The method of layer.
Yet, for the hot rolling low temperature slab hot type oriented silicon steel of mainly producing as inhibitor, twice cold-rolling practice of employing with aluminium nitride+copper, what process annealing was implemented is middle gross decarburization annealing, promptly in the process annealing process, the carbon amount in the cold-reduced sheet of interior thickness is taken off below the 30ppm; After for the second time cold rolling, steel plate is without annealing or promptly carrying out low-temperature annealing below 600 ℃ far below 840 ℃, and (generally below 600 ℃, if improve annealing temperature finished product magnetic is worsened) is coated with the magnesium oxide separant and carries out high temperature annealing.In this kind production method, the annealing temperature that is coated with the preceding finished product thickness cold-reduced sheet of MgO owing to steel plate is low, the bottom layer quality that is difficult to obtain.Therefore, in order to obtain good bottom layer quality, generally be from middle annealing stage, magnesium oxide separant itself, high temperature annealing stage or their aspects such as combination, take variety of way to try hard to make surface of steel plate good SiO of formation before the Magnesium Silicate q-agent bottom generates
2Layer, yet, in fact be difficult to make steel plate before the Magnesium Silicate q-agent bottom forms, to form good SiO in these operations at surface of steel plate
2Layer.In middle decarburizing annealing operation, though take process means might make the surface of steel plate after the process annealing obtain good SiO
2Layer, but through after for the second time cold rolling, the SiO of surface of steel plate
2Layer quality is destroyed, as with this as the Magnesium Silicate q-agent bottom condition that generates in back operation, no matter be its SiO
2The thickness of layer still is that the close degree of Qi Cause all is difficult to meet the demands.If adopt the high magnesium oxide separant of water ratio or take such as methods such as the composition that changes protective atmosphere, dew points in the high temperature annealing stage, because what adopt during high temperature annealing is coil annealing, surface of steel plate SiO
2Formation will be subjected to the homogeneity of plate shape, magnesian glue spread and water ratio thereof, the homogeneity of each position temperature of coil of strip, in fact the influence of coiling tension or the like factor will form good SiO at surface of steel plate before the Magnesium Silicate q-agent bottom forms
2Layer is very difficult.Therefore, these methods are difficult to fundamentally improve bottom layer quality, and the bad tension force effect that also can influence insulating coating of bottom layer quality can't be brought into play the improvement effect of tension force coating to magnetic property.
The oriented silicon steel bearing copper that it is contained Cr+Ni is disclosed in the EP0709470A1 patent, with the steel plate after for the second time cold rolling 600～750 ℃ of temperature, at intrinsic standoff ratio (P
H2O/ P
H2) be to carry out two minutes with interior anneal in 0.62～0.88 the atmosphere, to improve silicon steel sheet surface SiO
2Layer quality, but still exist because of steel plate annealing temperature and higher magnetic and the bottom layer quality problem of unstable that makes common orientation silicon steel (CGO) or high magnetic induction grain-oriented silicon steel plate of intrinsic standoff ratio after for the second time cold rolling.
Summary of the invention
The objective of the invention is at the above-mentioned main deficiency that exists in the technology as the oriented silicon steel of inhibitor with aluminium nitride and copper, provide a kind of can making to contain the raising oriented silicon steel bearing copper electromagnetic performance that the directional silicon steel bottom layer quality is good and stable, magnetic is good, method is simple of twice cold-rolling process production of middle gross decarburization annealed and the production method of bottom layer quality as inhibitor, employing with aluminium nitride and copper.
Realize the technology contents of above-mentioned purpose:
Improve the production method of oriented silicon steel bearing copper electromagnetic performance and bottom layer quality, its step:
1) with component and weight percent be: 0.015～0.050%C, 2.5～4.0%Si, 0.10～0.30%Mn, 0.010～0.035%Als, 0.0070～0.0120%N, 0.30～0.60%Cu and≤0.015%S, surplus for Fe and inevitable elemental composition, thickness be the silicon steel sheet of 1.8～2.8mm, it is cold rolling to carry out the first time after the pickling, and being rolled to thickness is 0.50～0.70mm;
2) P in 810～880 ℃ of temperature, wet type nitrogen nitrogen atmosphere and annealing furnace
H20/ P
H2Be to carry out centre gross decarburization annealing under 0.20～0.50 condition, the carbon content of blank plates of silicon steels is dropped to below the 30ppm, Control for Oxygen Content is in 300～750ppm scope;
3) it is cold rolling to carry out the second time, is rolled to the finished product desired thickness;
4) at 400～595 ℃, P
H2O/ P
H2Less than carrying out 5 minutes with interior recovery annealing under 0.61 the nitrogen nitrogen atmosphere condition;
5) coating is the annealing separating agent of main component with magnesium oxide;
6) under the condition that is lower than 1200 ℃ of temperature, anneal;
7) carry out stretching and leveling annealing after the uncoiling, be coated with insulating coating simultaneously.
It is that Control for Oxygen Content is in 350～700ppm scope;
It is that Control for Oxygen Content is in 400～600ppm scope;
It is that Control for Oxygen Content is in 450～580ppm scope;
It is the P when recovery annealing
H1O/ P
H2Be controlled at 0.55;
It is the P when recovery annealing
H2O/ P
H2Be controlled at less than 0.45;
P when it is recovery annealing
H2O/ P
H2Be controlled at less than 0.35;
The following describes the qualification reason and the mechanism of the relevant technology of the present invention in process annealing and recovery annealing:
About Control for Oxygen Content: in 300～750ppm scope, is that oxygen level height then its degree of oxidation is high more because steel plate in middle decarburizing annealing process, can make the surface produce oxidation inevitably with the Control for Oxygen Content of surface of steel plate after the process annealing.Two oxidising processs generally can take place in the decarburizing annealing stage in steel plate, it at first is near the silicon generation oxidation the surface of steel plate, can produce the desiliconization phenomenon when oxidation is serious, be that oxidation formation FeO takes place Fe then, degree of oxidation is high more, and the FeO layer is thick more, and the surface desiliconization takes place or generate thick FeO layer all can hinder in the back operation and form good Magnesium Silicate q-agent bottom, therefore, the oxygen level upper limit with surface of steel plate after the process annealing is limited to 750ppm.If oxygen level is lower than 300ppm, in fact can't reach the purpose of gross decarburization, so the oxygen level lower limit is limited to 300ppm.
About for the second time cold rolling back the finished product thickness cold-reduced sheet is carried out low temperature recovery annealing and technology qualification reason thereof.
The qualification reason of low temperature recovery annealing temperature: by discovering; with aluminium nitride and copper oriented silicon steel as inhibitor; when twice cold-rolling practice of gross decarburization annealing (carbon is taken off below the 30ppm) produced in the middle of employing contained; after for the second time being cold-rolled to finished product thickness; the low temperature recovery annealing that steel plate is carried out in the wet type protective atmosphere under certain conditions helps improving the bottom layer quality of finished product, thereby obtains good insulating coating characteristic.When the recovery annealing temperature is higher than 595 ℃, though more help surface of steel plate SiO
2The control of layer and the improvement of plate shape, but the magnetic of finished product is worsened; And when being lower than 400 ℃, the SiO that generates of surface of steel plate on the one hand
2Quantity not sufficient also can have influence on the coating effect of MgO coating on the other hand.Therefore, the low temperature recovery annealing temperature is limited to 400～595 ℃.
During low temperature recovery annealing, the intrinsic standoff ratio (P of protective atmosphere
H2O/ P
H2) the qualification reason.Through scrutinizing silicon steel sheet in wet type
The situation that the oxide compound of surface of steel plate generates during protective atmosphere annealing, and rule of thumb, think when steel plate is annealed that when intrinsic standoff ratio was low, surface of steel plate can at first form SiO under wet type atmosphere
2, along with the raising of intrinsic standoff ratio, surface of steel plate will generate Fe then
2SiO
4, this forms the Magnesium Silicate q-agent bottom during to high temperature annealing is favourable.When the intrinsic standoff ratio of atmosphere was higher than 0.61, the FeO component in the surface of steel plate zone of oxidation began to increase, and causes generating Fe
3O
4, the bottom layer quality of finished product reduces after making, and is unfavorable for finally obtaining the good insulation performance coating.Therefore, when low temperature recovery is annealed, with the intrinsic standoff ratio (P of protective atmosphere
H2O/ P
H2) be limited to below 0.61.
The invention has the advantages that on the basis of the surface of steel plate degree of oxidation after the decarburizing annealing in the middle of suitably controlling, when the steel plate after for the second time cold rolling is carried out low temperature recovery annealing, intrinsic standoff ratio by control low-temperature annealing atmosphere can obtain good bottom layer quality, improves magnetic.And have characteristics simple to operate.
Embodiment
With component and weight percent be: 0.034%C, 3.10%Si, 0.20%Mn, 0.0040%S, 0.015%Als, 0.0086%N, 0.49%Cu, all the other are the directional silicon steel slab that is hot-rolled down to 2.50mm thickness of Fe and inevitable impurity, carry out the first time cold rolling be rolled to 0.63mm after, in the wet type nitrogen nitrogen atmosphere of temperature that the present invention sets and intrinsic standoff ratio (all seeing tabulation), implement process annealing, the carbon in the steel plate is taken off below the 30ppm; Be cold-rolled to for the second time finished product thickness 0.27mm; In the nitrogen nitrogen atmosphere of temperature of setting and different intrinsic standoff ratio (all seeing Table row), implement low temperature recovery annealing; Coating is the annealing separating agent of main component with MgO; Being rolled into the back anneals under less than 1200 ℃ temperature; Carry out stretching and leveling annealing after the uncoiling, be coated with insulating coating simultaneously, the finished product magnetic and the coating performance that obtain are seen tabulation.Also listed the intrinsic standoff ratio of the oxygen level in the steel plate and recovery annealing atmosphere after the process annealing in the table.By following tabulation as seen, magnetic property and the insulating coating by the product of the inventive method manufacturing all is better than comparative example.
Table
Claims (7)
1. improve the production method of oriented silicon steel bearing copper electromagnetic performance and bottom layer quality, its step:
1) with component and weight percent be: 0.015～0.050%C, 2.5～4.0%Si, 0.10～0.30%Mn, 0.010～0.035%Als, 0.0070～0.0120%N, 0.30～0.60%Cu and≤0.015%S, surplus for Fe and inevitable elemental composition, thickness be the silicon steel sheet of 1.8～2.8mm, it is cold rolling to carry out the first time after the pickling, and being rolled to thickness is 0.50～0.70mm;
2) P in 810～880 ℃ of temperature, wet type nitrogen nitrogen atmosphere and annealing furnace
H2O/ P
H2Be to carry out centre gross decarburization annealing under 0.20～0.50 condition, the carbon content of silicon steel sheet is dropped to below the 30ppm, Control for Oxygen Content is in 300～750ppm scope;
3) it is cold rolling to carry out the second time, is rolled to the finished product desired thickness;
4) at 400～595 ℃, P
H2O/ P
H2Less than carrying out 5 minutes with interior recovery annealing under 0.61 the nitrogen nitrogen atmosphere condition;
5) coating is the annealing separating agent of main component with magnesium oxide;
6) anneal being lower than under 1200 ℃ of temperature;
7) carry out stretching and leveling annealing after the uncoiling, be coated with insulating coating simultaneously.
2. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality is characterized in that Control for Oxygen Content is in 350～700ppm scope.
3. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality is characterized in that Control for Oxygen Content is in 400～600ppm scope.
4. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality is characterized in that Control for Oxygen Content is in 450～580ppm scope.
5. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality is characterized in that P when recovery annealing
H2O/ P
H2Be controlled at less than 0.55.
6. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality is characterized in that P when recovery annealing
H2O/ P
H2Be controlled at less than 0.45.
7. the production method of raising oriented silicon steel bearing copper electromagnetic performance according to claim 1 and bottom layer quality, P when it is characterized in that recovery annealing
H2O/ P
H2Be controlled at less than 0.35.
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| CNB2005100200032A CN100389222C (en) | 2005-12-13 | 2005-12-13 | Production method for improving electromagnetic performance and bottom layer quality of copper containing orientation silicium steel |
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Families Citing this family (12)
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| CN101545072B (en) | 2008-03-25 | 2012-07-04 | 宝山钢铁股份有限公司 | Method for producing oriented silicon steel having high electromagnetic performance |
| CN101643881B (en) * | 2008-08-08 | 2011-05-11 | 宝山钢铁股份有限公司 | Method for producing silicon steel with orientedgrain including copper |
| EP2537946B1 (en) * | 2010-02-18 | 2019-08-07 | Nippon Steel Corporation | Method for manufacturing grain-oriented electrical steel sheet |
| CN102534363B (en) * | 2010-12-17 | 2015-10-07 | 鞍钢股份有限公司 | A kind of common orientation silicon steel manufacture method of energy-saving high efficiency |
| CN102492893A (en) * | 2011-12-26 | 2012-06-13 | 武汉钢铁(集团)公司 | General oriented silicon steel produced by continuous casting and rolling of sheet billet and its manufacture method |
| CN103695620B (en) * | 2013-12-16 | 2016-01-06 | 武汉钢铁(集团)公司 | The production method of the oriented silicon steel that a kind of bottom layer quality is excellent |
| CN106480305A (en) * | 2015-08-24 | 2017-03-08 | 鞍钢股份有限公司 | A kind of production method improving cold rolling electric decarburization efficiency |
| CN106480281A (en) * | 2015-08-24 | 2017-03-08 | 鞍钢股份有限公司 | A kind of production method of high magentic induction oriented electrical sheet |
| CN105420597B (en) * | 2015-11-26 | 2017-11-21 | 武汉钢铁有限公司 | A kind of production method of cupric low temperature high magnetic induction grain-oriented silicon steel |
| CN106086865B (en) * | 2016-06-16 | 2019-08-02 | 新万鑫（福建）精密薄板有限公司 | A kind of magnesia coating processes improving orientation silicon steel bottom |
| CN106755790A (en) * | 2016-11-15 | 2017-05-31 | 上海大学 | A kind of utilization magnetic field recovery annealing improves the process of silicon steel performance |
| CN114150126A (en) * | 2021-12-02 | 2022-03-08 | 湖南华菱涟源钢铁有限公司 | Copper-containing general oriented silicon steel and preparation method thereof |
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