CN103805918A - High-magnetic induction oriented silicon steel and production method thereof - Google Patents
High-magnetic induction oriented silicon steel and production method thereof Download PDFInfo
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Abstract
The invention provides high-magnetic induction oriented silicon steel and a production method thereof. The high-magnetic induction oriented silicon steel comprises the following chemical components in percentage by weight: 0.035-0.120% of C, 2.5-4.5% of Si, 0.05-0.20% of Mn, 0.005-0.050% of S, 0.015-0.035% of Als, 0.003-0.010% of N, 0.03-0.30% of Sn, 0.01-0.50% of Cu, less than or equal to 0.0100% of V, less than or equal to 0.0100% of Ti, more than one of Sb, Bi, Ni and Mo and the balance of Fe and inevitable impurities, wherein the percentage by weight of Sb, Bi, Nb and Mo is 0.0025-0.0250%; and (Sb/121.8+Bi/209.0+Nb/92.9+Mo / 95.9)/(Ti/47.9+V/50.9) is 0.1-15. According to the production method, inclusions separated out in a casting blank change in morphology by design of the steel components under the condition that no new equipment is additionally arranged, and the thick inclusions decline in the number; and compared with a conventional production method of the high-magnetic induction oriented silicon steel, the production method has the advantages that the heating temperature of the casting blank can be reduced by 100-150 DEG C, the finished product has stable magnetic property, and the typical magnetic induction B8 of the product is greater than or equal to 1.90T.
Description
Technical field
The present invention relates to oriented silicon steel and production method thereof, relate in particular 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 Si 2.0～4.5%, C 0.03～0.10%, Mn 0.03～0.2%, S 0.005～0.050%, the acid-soluble aluminium of Als() 0.02～0.05%, N 0.003～0.012%, some composition systems also contain 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) steel-making, through secondary refining and alloying, continuous casting becomes strand; Then strand is heated to approximately 1400 ℃ in special-purpose high temperature process furnace, and more than being incubated 45min, makes the abundant solid solution of favourable inclusion; Then carry out hot rolling, after laminar flow is cooling, batch, 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 taken off to the degree of finished product magnetic property that do not affect (generally should below 30ppm), and the annealing separating agent of coating take MgO as main component; Again carry out high temperature annealing, in high-temperature annealing process, steel plate generation secondary recrystallization, formation Magnesium Silicate q-agent bottom also complete purifying treatment (removing the element harmful to magnetic property such as S, N in steel), obtain the high magnetic induction grain-oriented silicon steel that orientation degree is high, iron loss is low; Finally by crossing coating insulating coating and the annealing that stretches, obtain the oriented silicon steel of commercial applications form.
Conventional production methods is take MnS+AlN as inhibitor.Inhibitor derives from inclusion intrinsic in strand, and these inclusiones form 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 ℃, 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, causes cold rolling process to produce difficulty, and lumber recovery is low, and cost is also high.
In order to reduce slab heating temperature, must in inhibitor, get rid of the effect of MnS or reduction MnS, and with AlN, Cu
2s etc. replace.This be because, AlN and Cu
2the solid solubility temperatures such as S are lower than MnS, are more suitable for realizing low-temperature heat.But when slab heating temperature is reduced to after certain temperature, can cause insufficient solid solution of inhibitor, be difficult to the stable high magnetic induction grain-oriented silicon steel that obtains.
The typical processing route that reduces slab heating temperature can be summarized as at present:
(1) AlN+ later stage nitridation process: add Trace Aluminum element in the time of steel-making, mainly for the production of high magnetic induction grain-oriented silicon steel.Its composition requires the massfraction <0.007% of S, carries out nitriding processing after decarburizing annealing.This technique principal feature is that steel band need be through the nitriding processing of 750 ℃ × 30sec after decarburizing annealing.In high temperature annealing temperature-rise period, form (A1, Si) N particle, before secondary recrystallization occurs, hinder first grain growth.After decarburizing annealing, the suitable dimension of first crystal grain is 18～30 μ m.This technique can be reduced to slab heating temperature below 1200 ℃, is that in current oriented silicon steel industrial production, strand heats the minimum temperature adopting.But it is high that this technique requires process parameters such as steel-making composition, first grain-size and nitriding homogeneity, and the difficulty of stable control magnetic property is large.In addition, after decarburization, nitriding has also increased the control difficulty of bottom.
(2) add the congenital inhibitor technique of Cu: with Cu
2s is as main inhibitor, Cu
2s realizes complete solid solution through 1250～1300 ℃ of heating.The small and dispersed Cu separating out in course of hot rolling
2s particle plays inhibitor effect, and in hot-rolled sheet, remaining thick MnS particle does not play restraining effect.But cannot stably manufactured high magnetic induction grain-oriented silicon steel.
In summary it can be seen, ripe high magnetic induction grain-oriented silicon steel production technique mainly contains two classes at present: high-temperature technology (take MnS+AlN as inhibitor) and low temperature process (AlN+ nitriding processing).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 in strand (AlN, MnS or Cu
xs) be difficult to control, cause subsequent anneal process window narrow, the difficulty of stable control magnetic property and bottom layer quality is large.
China Patent Publication No. CN1138107A discloses a kind of " 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 with respect to the rolling direction of this steel plate in 5 °, and (001) axle with respect to plate face vertical direction in 5 °; In this thick secondary recrystallization crystal grain or in crystal boundary, having diameter is the small grains of 0.05～2mm, and the relative angle of (001) axle of its (001) axle and thick subgrain is at 2～30 °.
Japanese patent application publication No. JP8232020A discloses a kind of " manufacture method of grain oriented magnetic steel disc ", it relates to a kind of manufacture of the siliconized plate of producing 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%, acid-soluble aluminium: 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 ℃, 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 newly added equipment not, by the design to steel grades, the inclusion morphology of separating out in strand is changed, the thick the amount of inclusions of size reduces, and compares the manufacture of traditional high magnetic induction grain-oriented silicon steel, can reduce by 100 ~ 150 ℃ of slab heating temperature, and final finished magnetic property is stable, 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 control the total amount of V, Ti, the inclusion morphology of separating out in strand is changed, the thick the amount of inclusions of size reduces, tiny, disperse the amount of inclusions increases, reduce slab heating temperature with this, thereby 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 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 form in steel casting process.Strand must at high temperature heat makes the abundant solid solution of these inclusiones, and the inclusion of solid solution is disperse educt in hot rolling process, adjusts inclusion morphology subsequently by normalizing annealing, and its small and dispersed is distributed.The fine foreign matter of separating out is as the needed effective inhibitor of secondary recrystallization, and also the grain-size to primary recrystallization and homogeneity important thereof, therefore have material impact to the magnetic property of final finished.
Conventionally, molten steel, in the process that is cooled to strand, can produce the thick inclusion of size, and thick inclusion is MnS+AlN complex inclusion by analysis, and referring to Fig. 1, its form and composition that provides a typical thick inclusion can illustrate above-mentioned viewpoint.According to Method of Energy Spectrum Analysis result, 1 place, position is mainly Mn, S, Ti element, and Al, N element are contained in 2,3,4,5,6,7,8,9,10 of positions.
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 be in heating of plate blank process fully solid solution, therefore for tradition directed silicon steel, needed 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 after hot rolling and normalizing annealing, still can keep thick form.A little less than thick inclusion restraint, on the one hand cause first grain-size inhomogeneous, a little less than inhibition ability when secondary recrystallization, this all can make secondary recrystallization imperfection on the other hand, and therefore final finished magnetic property is poor.
The present invention adds micro-Sb, Bi, Nb or Mo in steelmaking process, and controls the content of Ti, V, and the inclusion morphology of separating out in strand is changed, and the thick the amount of inclusions of size reduces, and the amount of inclusions tiny, disperse increases.
This is because trace element can preferentially form micro-carbon, nitrogen compound, has reduced the quantity of TiN, TiC or VN, makes in strand greatly to reduce take TiN, TiC or VN as the MnS+AlN complex inclusion quantity of core.TiN, TiC or VN can be used as the forming core core of MnS, preferentially separate out MnS, AlN becomes MnS+AlN complex inclusion take MnS as karyomorphism then, and this complex inclusion size is thick, be about 0.5 ~ 3.0 μ m, and the AlN inclusion size that small and dispersed is separated out is less than 400nm.As shown in Figure 1, its form and composition that provides a typical thick inclusion can illustrate above-mentioned viewpoint.
Need to further illustrate, be also very important about the ratio control between trace element.In the time that Sb, Bi, Nb, Mo are high containing quantity not sufficient or V, Ti content, without additive effect, in the time of Sb, Bi, Nb, Mo too high levels, Carbonitride Precipitation amount is many, and the tiny AlN amount of separating out is few, also can make magnetic property degenerate.Micronutrient levels is too high, also can make cold rolling poor processability.
The present invention adds micro-antimony (Sb), bismuth (Bi), niobium (Nb) or molybdenum (Mo) in steelmaking process, and controls the content of Ti, V, can make the thick the amount of inclusions of size in strand reduce, and the amount of inclusions tiny, disperse increases.Due to the easier solid solution of fine foreign matter, therefore can reduce the solid solubility temperature of strand.
Also it is pointed out that carbon, nitrogen compound that trace element forms can be used as auxiliary inhibitor, be conducive to the stable of magnetic property, referring to 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, 5 ~ 25 ℃ of the superheating temperature of molten steel, casting rate 0.5 ~ 2.0m/min;
2) strand heating
1200 ~ 1330 ℃ of Heating temperatures, heat-up time 150 ~ 600min;
3) hot rolling, conventional hot rolling;
4) normalizing annealing
Hot rolled coil is carried out to normalizing annealing, after normalizing annealing, carry out cooling, 10 ~ 100 ℃/sec of speed of cooling;
5) cold rolling
Be cold rolled to production board thickness, cold rolling draft >=85%;
6) decarburizing annealing
Heat-up rate, decarburizing atmosphere and decarburization dew point are set routinely, 800 ~ 900 ℃ of decarburization temperature, time 80 ~ 160sec;
7) MgO coating and high temperature annealing
The steel plate of above-mentioned decarburizing annealing is carried out MgO coating and in bell furnace or ring furnace, carries out conventional high temperature annealing;
8) insulating coating
Apply insulating coating on high temperature annealing plate surface, and obtain the high magnetic induction grain-oriented silicon steel of excellent magnetic through the smooth annealing of thermal stretch.
Further, in step 5) cold-rolled process, also comprise process annealing.
In addition, after described step 6) decarburizing annealing, carry out nitriding processing, infiltrate nitrogen content 50 ~ 260ppm.
In addition, if carry out nitriding processing, the Heating temperature of described strand can be 1050 ~ 1150 ℃.
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.Stablize pouring operation in order to control inclusion in casting blank form and to guarantee, while requiring cast, 5 ~ 25 ℃ of the superheating temperature of the interior molten steel of tundish are controlled the pouring speed of strand between 0.5 ~ 2.0m/min simultaneously.
Add after Sb, Bi, Nb, Mo, slab heating temperature can suitably reduce.In order to guarantee the fully solid solution of inclusion in strand, slab heating temperature is between 1200～1330 ℃.Can be controlled in 150 ~ 600min heat-up time.
Because core of the present invention is the inclusion size in refinement strand, therefore inventive point is equally applicable to the strand production of nitriding process low temperature process oriented silicon steel.Rear operation is carried out nitriding processing, and the Heating temperature of strand can further be reduced to below 1150 ℃.
Beneficial effect of the present invention:
The present invention, by adding trace element and control the content of corresponding impurity element in steelmaking process, changes the inclusion morphology of separating out in strand, and the thick the amount of inclusions of size reduces, and the amount of inclusions of small and dispersed increases.Compare traditional high magnetic induction grain-oriented silicon steel, can reduce by 100 ~ 150 ℃ of slab heating temperature, and final finished magnetic property is stable, 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 micro-strand.
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 has shown thick the amount of inclusions in the strand of the embodiment of the present invention and comparative example.Production method and finished product magnetic strength B that table 3 is high magnetic induction grain-oriented silicon steel embodiment of the present invention
8.
Embodiment 1
(1) smelting according to composition proportion as shown in table 1, is 5 ~ 15 ℃ by superheating temperature, and casting rate is that 1.3m/min casts, and obtains strand;
(2) strand is pressed to the strand heating cycle heating described in table 3;
(3) be hot-rolled down to the hot-rolled sheet of 2.3mm;
(4) normalizing annealing;
(5) be cold rolled to finished product thickness 0.30mm;
(6) decarburizing annealing, decarburization temperature is 810 ~ 880 ℃, decarburization time is 80 ~ 160s, and [C] content in steel plate is dropped to below 30ppm;
(7) on steel plate, applying after MgO coating is 100%H in atmosphere
2, temperature is the high temperature annealing carrying out under the condition of 1200 ℃ 20 hours;
(8) obtain high magnetic induction grain-oriented silicon steel after applying the smooth annealing of insulating coating and 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 has shown thick the amount of inclusions in the strand of embodiment 1-11 and comparative example 12-17.Adopt non-aqueous solution electrolysis extraction-electron microscopic observation method to analyze the amount of inclusions in strand.Observe the visual field of 10 2500 times, obtain averaging after 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 correspondences 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 approximately 100 ~ 150 ℃.Reducing under the condition of slab heating temperature, also can obtain the stable high magnetic induction grain-oriented silicon steel of magnetic property.In the time that composition meets requirement of the present invention, if carry out nitriding processing, even slab heating temperature be reduced to≤1125 ℃ time, also can obtain high magnetic induction oriented silicon steel.
Claims (5)
1. a high magnetic induction grain-oriented silicon steel, its composition 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 trace element Sb, Bi, Ni and Mo 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, 5 ~ 25 ℃ of the superheating temperature of molten steel, casting rate 0.5 ~ 2.0m/min;
2) strand heating
1200 ~ 1330 ℃ of Heating temperatures, heat-up time 150 ~ 600min;
3) hot rolling, conventional hot rolling;
4) normalizing annealing
Hot rolled coil is carried out to normalizing annealing, after normalizing annealing, carry out cooling, 10 ~ 100 ℃/sec of speed of cooling;
5) cold rolling
Be cold rolled to production board thickness, cold rolling draft >=85%;
6) decarburizing annealing
Heat-up rate, decarburizing atmosphere and decarburization dew point are set routinely, 800 ~ 900 ℃ of decarburization temperature, time 80 ~ 160sec;
7) MgO coating and high temperature annealing
The steel plate of above-mentioned decarburizing annealing is carried out MgO coating and in bell furnace or ring furnace, carries out conventional high temperature annealing;
8) insulating coating
Apply insulating coating on high temperature annealing plate surface, 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 comprises 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, after described step 6) decarburizing annealing, carries out nitriding processing, 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, 1050 ~ 1150 ℃ of the Heating temperatures of described strand.
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