CN103805918B - A kind of high magnetic induction grain-oriented silicon steel and production method thereof - Google Patents
A kind of high magnetic induction grain-oriented silicon steel and production method thereof Download PDFInfo
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Abstract
A kind of high magnetic induction grain-oriented silicon steel and production method thereof, does is its chemical component weight per-cent: C? 0.035 ~ 0.120%, Si? 2.5 ~ 4.5%, Mn? 0.05 ~ 0.20%, S? 0.005 ~ 0.050%, Als? 0.015 ~ 0.035%, N? 0.003 ~ 0.010%, Sn? 0.03 ~ 0.30%, Cu? 0.01 ~ 0.50%, V≤0.0100%, Ti≤0.0100%, in Sb, Bi, Ni and Mo more than one, Sb+Bi+Nb+Mo:0.0025 ~ 0.0250%; (Sb/121.8+Bi/209.0+Nb/92.9+Mo/95.9)/(Ti/47.9+V/50.9)=0.1 ~ 15; All the other are Fe and other inevitable impurity.The present invention is under the prerequisite of not newly added equipment, by the design to steel grades, the inclusion morphology of separating out in strand is changed, the amount of inclusions minimizing that size is thick, compare the manufacture of traditional high magnetic induction grain-oriented silicon steel, can reduce slab heating temperature 100 ~ 150 DEG C, and final finished magnetic property is stablized, its typical magnetic strength B8 >=1.90T.
Description
Technical field
The present invention relates to oriented silicon steel and production method thereof, particularly relate to a kind of high magnetic induction grain-oriented silicon steel and production method thereof.
Background technology
The basic chemical composition of tradition high magnetic induction grain-oriented silicon steel is Si2.0 ~ 4.5%, C0.03 ~ 0.10%, Mn0.03 ~ 0.2%, S0.005 ~ 0.050%, Als(dissolved aluminum) 0.02 ~ 0.05%, N0.003 ~ 0.012%, some component system are also containing one or more in the elements such as Cu, Mo, Sb, B, Bi.
The production method of tradition high magnetic induction grain-oriented silicon steel is: first use converter (or electric furnace) to make steel, through secondary refining and alloying, continuous casting becomes strand; Then strand is heated to about 1400 DEG C in special-purpose high temperature process furnace, and is incubated more than 45min, makes the abundant solid solution of favourable inclusion; Then carry out hot rolling, batch after section cooling, in Hot Rolled Plate Normalizing process, in silicon steel matrix, separate out the Second Phase Particles of small and dispersed, obtain effective inhibitor; Again hot-rolled sheet is cold rolled to decarburizing annealing after finished product thickness, [C] in steel plate is taken off the degree (generally should at below 30ppm) not affecting finished product magnetic property, and coating take MgO as the annealing separating agent of main component; Again carry out high temperature annealing, in high-temperature annealing process, steel plate generation secondary recrystallization, form Magnesium Silicate q-agent bottom and complete purifying treatment (element that S, N etc. in removing steel are harmful to magnetic property), obtaining the high magnetic induction grain-oriented silicon steel that orientation degree is high, iron loss is low; Eventually pass coating insulating coating and the annealing that stretches, obtain the oriented silicon steel of commercial applications form.
Conventional production methods take MnS+AlN as inhibitor.Inhibitor derives from inclusion intrinsic in strand, and these inclusiones are formed in steel casting process, and size is generally thick.In order to obtain stable magnetic property, must make the abundant solid solution of inhibitor such as thick MnS in strand, the highest need of Heating temperature reach 1400 DEG C, and this is the Limiting Level of traditional heating stove.In addition, because Heating temperature is high, strand scaling loss is large, process furnace needs frequent repairing, and utilization ratio is low.Meanwhile, energy consumption is high, and the limit of hot rolled coil is split greatly, and cause cold rolling process to produce difficulty, lumber recovery is low, and cost is also high.
In order to reduce slab heating temperature, the effect of MnS or reduction MnS must be got rid of in inhibitor, and with AlN, Cu
2s etc. replace.This is because, AlN and Cu
2the solid solubility temperatures such as S are lower than MnS, are more suitable for realizing low-temperature heat.But after slab heating temperature is reduced to certain temperature, insufficient solid solution of inhibitor can be caused, be difficult to stable acquisition high magnetic induction grain-oriented silicon steel.
The typical processing route reducing slab heating temperature can be summarized as at present:
(1) AlN+ later stage nitridation process: add Trace Aluminum element when making steel, mainly for the production of high magnetic induction grain-oriented silicon steel.The massfraction <0.007% of its component requirements S, carries out Nitrizing Treatment after decarburizing annealing.This technique principal feature is, after decarburizing annealing, steel band need through the Nitrizing Treatment of 750 DEG C × 30sec.Form (A1, Si) N particle in high temperature annealing temperature-rise period, before secondary recrystallization occurs, hinder first grain growth.After decarburizing annealing, the suitable dimension of first crystal grain is 18 ~ 30 μm.Slab heating temperature can be reduced to less than 1200 DEG C by this technique, is that in current oriented silicon steel industrial production, strand heats the minimum temperature adopted.But this technique requires high to steel-making composition, the first process parameter such as grain-size and nitriding homogeneity, and the difficulty of stability contorting magnetic property is large.In addition, after decarburization, nitriding too increases the control difficulty of bottom.
(2) the congenital inhibitor technique of Cu is added: with Cu
2s as major inhibitors, Cu
2s realizes complete solid solution through 1250 ~ 1300 DEG C of heating.The small and dispersed Cu separated out in course of hot rolling
2s particle plays inhibitor effect, and thick MnS particle remaining in hot-rolled sheet does not play restraining effect.But cannot stably manufactured high magnetic induction grain-oriented silicon steel.
In summary it can be seen, high magnetic induction grain-oriented silicon steel production technique ripe at present mainly contains two classes: high-temperature technology (taking MnS+AlN as inhibitor) and low temperature process (AlN+ Nitrizing Treatment).Wherein, the maximum deficiency of high-temperature technology is that slab heating temperature is too high, and production cost is high; The maximum deficiency of low temperature process is inclusion morphology (AlN, MnS or Cu in strand
xs) be difficult to control, cause subsequent annealing process window narrows, the difficulty of stability contorting magnetic property and bottom layer quality is large.
China Patent Publication No. CN1138107A discloses one " electro-magnetic steel plate of high flux density low iron loss grain orientation and manufacture method thereof ", it contains Si:2.5 ~ 4.0wt%, Al:0.005 ~ 0.06wt%, and among each crystal grain of this steel plate, by area occupation ratio, at least 95% is 5 ~ 50mm by diameter, and thick secondary recrystallization crystal grain forms, its (001) axle relative to the rolling direction of this steel plate within 5 °, and (001) axle relative to plate face vertical direction within 5 °; In this thick secondary recrystallization crystal grain or in crystal boundary, there is the small grains that diameter is 0.05 ~ 2mm, the relative angle of (001) axle of its (001) axle and thick subgrain is at 2 ~ 30 °.
Japanese patent application publication No. JP8232020A discloses one " manufacture method of grain oriented magnetic steel disc ", it relates to a kind of manufacture of producing the siliconized plate of cheap excellent magnetic, its step comprises cold continuous rolling and the annealing of specific roll speed, is adjusted to the total nitrogen content of specific ppm, then completes annealing.The weight percent proportioning of this steel disc is C:0.001 ~ 0.09%, silicon: 2 ~ 4.5%, dissolved aluminum: 0.01 ~ 0.08%, N:0.00010.004%, independent or total S and (or) selenium: 0.008 ~ 0.06%, copper: 0.01 ~ 1%, manganese: 0.01 ~ 0.5%, a small amount of Bi, P, Sn, Pb, B, V, niobium etc., surplus is Fe and other inevitable impurity.The cold continuous rolling rate of cold rolled silicon steel is 75 ~ 95%, and annealing temperature is 800 ~ 1000 DEG C, and annealing time is 1300 seconds, and total nitrogen content is 50 ~ 1000ppm.
Summary of the invention
The object of the present invention is to provide a kind of high magnetic induction grain-oriented silicon steel and production method thereof, under the prerequisite of not newly added equipment, by the design to steel grades, the inclusion morphology of separating out in strand is changed, the amount of inclusions minimizing that size is thick, compares the manufacture of traditional high magnetic induction grain-oriented silicon steel, can reduce slab heating temperature 100 ~ 150 DEG C, and final finished magnetic property is stablized, its typical magnetic strength B
8>=1.90T.
For achieving the above object, technical scheme of the present invention is:
The present invention adds micro-Sb, Bi, Nb, Mo, and the total amount of control V, Ti, the inclusion morphology of separating out in strand is changed, the amount of inclusions minimizing that size is thick, tiny, disperse the amount of inclusions increases, reduce slab heating temperature with this, thus obtain the good high magnetic induction grain-oriented silicon steel of Magnetic stability.
Particularly, a kind of high magnetic induction grain-oriented silicon steel of the present invention, its composition by weight percent is: C:0.035 ~ 0.120%, Si:2.5 ~ 4.5%, Mn:0.05 ~ 0.20%, S:0.005 ~ 0.050%, Als:0.015 ~ 0.035%, N:0.003 ~ 0.010%, Sn:0.03 ~ 0.30%, Cu:0.01 ~ 0.50%, V≤0.0100%, Ti≤0.0100%, in micro-Sb, Bi, Ni and Mo more than one, Sb+Bi+Nb+Mo:0.0025 ~ 0.0250%; Meet following formula: (Sb/121.8+Bi/209.0+Nb/92.9+Mo/95.9)/(Ti/47.9+V/50.9)=0.1 ~ 15 simultaneously; All the other are Fe and other inevitable impurity.
For tradition directed silicon steel, inhibitor derives from existing inclusion in slab, and these inclusiones are formed in steel casting process.Strand must at high temperature heat makes the abundant solid solution of these inclusiones, and inclusion disperse educt in hot rolling process of solid solution, adjusts inclusion morphology by normalizing annealing subsequently, its small and dispersed is distributed.The fine foreign matter of separating out, as the effective inhibitor required for secondary recrystallization, also to grain-size and the homogeneity important thereof of primary recrystallization, therefore has material impact to the magnetic property of final finished.
Usually, molten steel, in the process being cooled to strand, can produce the inclusion that size is thick, and thick inclusion is MnS+AlN complex inclusion by analysis, and see Fig. 1, it provides the form of a typical thick inclusion and composition can illustrate above-mentioned viewpoint.According to Method of Energy Spectrum Analysis result, position 1 place is mainly Mn, S, Ti element, and 2,3,4,5,6,7,8,9,10, position is containing Al, N element.
Compare the inclusion of small and dispersed, thick inclusion solid solubility temperature is high.In order to make the magnetic strength B8 >=1.88T of final finished, these thick inclusiones must abundant solid solution in heating of plate blank process, and therefore for tradition directed silicon steel, required slab heating temperature is high.
If tradition directed silicon steel strand is not through fully heating, thick inclusion is difficult to abundant solid solution, does not have the inclusion of solid solution still can keep thick form after hot rolling and normalizing annealing.Because thick inclusion restraint is weak, cause first grain-size uneven on the one hand, the rejection ability on the other hand during secondary recrystallization is weak, and this all can make secondary recrystallization imperfection, and therefore final finished magnetic property is poor.
The present invention adds Sb, Bi, Nb or Mo of trace in steelmaking process, and the content of control Ti, V, the inclusion morphology of separating out in strand is changed, the amount of inclusions minimizing that size is thick, the amount of inclusions that is tiny, disperse increases.
This is because trace element preferentially can form carbon, the nitrogen compound of trace element, decreases the quantity of TiN, TiC or VN, makes the MnS+AlN complex inclusion quantity being core with TiN, TiC or VN in strand greatly reduce.TiN, TiC or VN can as the forming core cores of MnS, preferential precipitation MnS, AlN is that karyomorphism becomes MnS+AlN complex inclusion with MnS then, and this complex inclusion size is thick, be about 0.5 ~ 3.0 μm, and the AlN inclusion size that small and dispersed is separated out is less than 400nm.As shown in Figure 1, it provides the form of a typical thick inclusion and composition can illustrate above-mentioned viewpoint.
Needing to further illustrate, is also very important about the ratio control between trace element.When Sb, Bi, Nb, Mo are containing quantity not sufficient or V, Ti content height, without additive effect, when Sb, Bi, Nb, Mo too high levels, Carbonitride Precipitation amount is many, and tiny AlN amount of precipitation is few, and magnetic property also can be made to degenerate.Micronutrient levels is too high, and cold-rolling workability also can be made to be deteriorated.
The present invention adds micro-antimony (Sb), bismuth (Bi), niobium (Nb) or molybdenum (Mo) in steelmaking process, and the content of control Ti, V, the amount of inclusions that in strand, size is thick can be made to reduce, and the amount of inclusions that is tiny, disperse increases.Due to the easier solid solution of fine foreign matter, the solid solubility temperature of strand therefore can be reduced.
Also it is pointed out that carbon, the nitrogen compound of trace element formation can be used as auxiliary inhibitor, be conducive to the stable of magnetic property, see Fig. 2.
The production method of high magnetic induction grain-oriented silicon steel of the present invention, it comprises the steps:
1) smelt and cast
Adopt converter or Electric furnace steel making, molten steel obtains strand after secondary refining and continuous casting, the superheating temperature of molten steel 5 ~ 25 DEG C, casting rate 0.5 ~ 2.0m/min;
2) strand heating
Heating temperature 1200 ~ 1330 DEG C, heat-up time 150 ~ 600min;
3) hot rolling, conventional hot rolling;
4) normalizing annealing
Normalizing annealing is carried out to hot rolled coil, cools after normalizing annealing, speed of cooling 10 ~ 100 DEG C/sec;
5) cold rolling
Be cold rolled to finished plate thickness, cold rolling draft >=85%;
6) decarburizing annealing
Heat-up rate, decarburizing atmosphere and decarburization dew point set routinely, decarburization temperature 800 ~ 900 DEG C, time 80 ~ 160sec;
7) MgO coating and high temperature annealing
MgO coating is carried out to the steel plate of above-mentioned decarburizing annealing and carry out conventional high temperature annealing in bell furnace or ring furnace;
8) insulating coating
At high temperature annealing plate surface application insulating coating, and obtain the high magnetic induction grain-oriented silicon steel of excellent magnetic through the smooth annealing of thermal stretch.
Further, also process annealing is comprised in step 5) cold-rolled process.
In addition, after described step 6) decarburizing annealing, carry out Nitrizing Treatment, infiltrate nitrogen content 50 ~ 260ppm.
In addition, if carry out Nitrizing Treatment, the Heating temperature of described strand can be 1050 ~ 1150 DEG C.
In manufacture method of the present invention:
The present invention adopts converter or Electric furnace steel making, and molten steel, after secondary refining and continuous casting, obtains strand.In order to control inclusion in casting blank form and ensure stablize pouring operation, when requiring to pour into a mould, the superheating temperature 5 ~ 25 DEG C of molten steel in tundish, controls the pouring speed of strand between 0.5 ~ 2.0m/min simultaneously.
After adding Sb, Bi, Nb, Mo, slab heating temperature can suitably reduce.In order to ensure that inclusion in strand can fully solid solution, slab heating temperature is between 1200 ~ 1330 DEG C.Heat-up time can control in 150 ~ 600min.
Due to the inclusion size that core of the present invention is in refinement strand, therefore inventive point is equally applicable to the strand production of nitriding process low temperature process oriented silicon steel.Rear operation carries out Nitrizing Treatment, then the Heating temperature of strand can be reduced to less than 1150 DEG C further.
Beneficial effect of the present invention:
The present invention passes through to add trace element in steelmaking process and the content controlling corresponding impurity element, and the inclusion morphology of separating out in strand is changed, the amount of inclusions minimizing that size is thick, and the amount of inclusions of small and dispersed increases.Compare traditional high magnetic induction grain-oriented silicon steel, slab heating temperature 100 ~ 150 DEG C can be reduced, and final finished magnetic property is stablized, its typical magnetic strength B
8>=1.90T.
Accompanying drawing explanation
Fig. 1 is form and the composition (× 30000 times) of thick inclusion in strand.
Fig. 2 is the relation between magnetic property and trace element.
Fig. 3 is the photo (× 300 times) of thick inclusion in the strand of embodiments of the invention 1.
Fig. 4 is the photo (× 300 times) that comparative example 12 does not add thick inclusion in the strand of trace element.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Table 1 is depicted as the composition of high magnetic induction grain-oriented silicon steel embodiment of the present invention.Table 2 shows thick the amount of inclusions in the strand of the embodiment of the present invention and comparative example.The production method that table 3 is high magnetic induction grain-oriented silicon steel embodiment of the present invention and finished product magnetic strength B
8.
Embodiment 1
(1) smelting according to composition proportion as shown in table 1, is 5 ~ 15 DEG C by superheating temperature, and casting rate is that 1.3m/min casts, and obtains strand;
(2) strand is pressed the strand heating cycle heating described in table 3;
(3) hot-rolled sheet of 2.3mm is hot-rolled down to;
(4) normalizing annealing;
(5) finished product thickness 0.30mm is cold rolled to;
(6) decarburizing annealing, decarburization temperature is 810 ~ 880 DEG C, and decarburization time is 80 ~ 160s, and [C] content in steel plate is dropped to below 30ppm;
(7) be 100%H in atmosphere apply MgO coating on steel plate after
2, temperature is the high temperature annealing carried out under the condition of 1200 DEG C 20 hours;
(8) high magnetic induction grain-oriented silicon steel is obtained after applying insulating coating and the smooth annealing of thermal stretch after uncoiling.
Table 1 unit: weight percent
Remarks: sequence number 1-11 is embodiment, and sequence number 12-17 is comparative example.
Table 2 shows thick the amount of inclusions in the strand of embodiment 1-11 and comparative example 12-17.Adopt the amount of inclusions in non-aqueous solution electrolysis extraction-electron microscopic observation method analysis strand.Observe the visual field of 10 2500 times, average after obtaining the thick the amount of inclusions in each visual field.
Table 2
| Sequence number | Thick the amount of inclusions in strand | Remarks |
| 1 | 1 | Corresponding diagram 3 |
| 2 | 2 | |
| 3 | 4 | |
| 4 | 1 | |
| 5 | 3 | |
| 6 | 4 | |
| 7 | 3 | |
| 8 | 2 | |
| 9 | 1 | |
| 10 | 2 | |
| 11 | 5 | |
| 12 | 24 | Corresponding diagram 4 |
| 13 | 19 | |
| 14 | 17 | |
| 15 | 16 | |
| 16 | 13 | |
| 17 | 21 |
Fig. 3 provides the photo (× 300 times) of thick inclusion in the strand of embodiment 1 correspondence in table 1.Fig. 4 provides the photo (× 300 times) of thick inclusion in the strand of comparative example 12 correspondence in table 1.
Table 3
From table 2, table 3, adopt technical scheme of the present invention, the thick the amount of inclusions in strand obviously reduces, and in strand, the abundant solid solubility temperature of inclusion reduces about 100 ~ 150 DEG C.Under the condition reducing slab heating temperature, also can obtain the stable high magnetic induction grain-oriented silicon steel of magnetic property.When composition meets application claims, if carry out Nitrizing Treatment, though slab heating temperature be reduced to≤1125 DEG C time, also can obtain high magnetic induction oriented silicon steel.
Claims (5)
1. a high magnetic induction grain-oriented silicon steel, its composition by weight percent is:
C：0.035~0.120%，
Si：2.5~4.5%，
Mn：0.05~0.20%，
S：0.005~0.050%，
Als：0.015~0.035%，
N：0.003~0.010%，
Sn：0.03~0.30%，
Cu：0.01~0.50%，
V：≤0.0100%，
Ti：≤0.0100%，
Trace element Sb, Bi, Ni and Mo in more than one, Sb+Bi+Nb+Mo:
0.0025 ~ 0.0250%; Meet following formula simultaneously:
（Sb/121.8+Bi/209.0+Nb/92.9+Mo/95.9）/（Ti/47.9+V/50.9）＝0.1~15；
All the other are Fe and other inevitable impurity.
2. the production method of high magnetic induction grain-oriented silicon steel as claimed in claim 1, it comprises the steps:
1) smelt, cast
Adopt converter or Electric furnace steel making, molten steel obtains strand after secondary refining and continuous casting, the superheating temperature of molten steel 5 ~ 25 DEG C, casting rate 0.5 ~ 2.0m/min;
2) strand heating
Heating temperature 1200 ~ 1330 DEG C, heat-up time 150 ~ 600min;
3) hot rolling, conventional hot rolling;
4) normalizing annealing
Normalizing annealing is carried out to hot rolled coil, cools after normalizing annealing, speed of cooling 10 ~ 100 DEG C/sec;
5) cold rolling
Be cold rolled to finished plate thickness, cold rolling draft >=85%;
6) decarburizing annealing
Heat-up rate, decarburizing atmosphere and decarburization dew point set routinely, decarburization temperature 800 ~ 900 DEG C, time 80 ~ 160sec;
7) MgO coating and high temperature annealing
MgO coating is carried out to the steel plate of above-mentioned decarburizing annealing and carry out conventional high temperature annealing in bell furnace or ring furnace;
8) insulating coating
At high temperature annealing plate surface application insulating coating, and obtain the high magnetic induction grain-oriented silicon steel of excellent magnetic through the smooth annealing of thermal stretch.
3. the production method of high magnetic induction grain-oriented silicon steel as claimed in claim 2, is characterized in that, also comprise process annealing in step 5) cold-rolled process.
4. the production method of high magnetic induction grain-oriented silicon steel as claimed in claim 2, is characterized in that, carry out Nitrizing Treatment after described step 6) decarburizing annealing, infiltrates nitrogen content 50 ~ 260ppm.
5. the production method of high magnetic induction grain-oriented silicon steel as claimed in claim 4, is characterized in that, the Heating temperature of described strand 1050 ~ 1150 DEG C.
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| KR101642281B1 (en) | 2014-11-27 | 2016-07-25 | 주식회사 포스코 | Oriented electrical steel sheet and method for manufacturing the same |
| CN104789862A (en) * | 2015-03-20 | 2015-07-22 | 宝山钢铁股份有限公司 | High-magnetic-induction low-iron-loss non-oriented electrical steel plate with good surface state and manufacturing method thereof |
| CN106399819B (en) * | 2016-06-16 | 2018-12-28 | 马鞍山钢铁股份有限公司 | A kind of orientation silicon steel and preparation method thereof |
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| CN108339851B (en) * | 2017-12-21 | 2019-08-09 | 东北大学 | A kind of cold rolling of oriented silicon steel strip in razor-thin and method for annealing |
| CN110318005B (en) * | 2018-03-30 | 2021-12-17 | 宝山钢铁股份有限公司 | High magnetic induction oriented silicon steel and manufacturing method thereof |
| CN112391512B (en) * | 2019-08-13 | 2022-03-18 | 宝山钢铁股份有限公司 | High magnetic induction oriented silicon steel and manufacturing method thereof |
| CN110791635A (en) * | 2019-09-30 | 2020-02-14 | 鞍钢股份有限公司 | Method for preparing high-magnetic-induction oriented silicon steel |
| CN114134422B (en) * | 2021-12-02 | 2022-09-20 | 武汉英杰寰宇贸易有限公司 | Soft magnetic steel with excellent lamellar tearing resistance and preparation method thereof |
| CN117363963A (en) * | 2022-06-30 | 2024-01-09 | 宝山钢铁股份有限公司 | Oriented silicon steel and manufacturing method thereof |
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