CN104294155A - Ultra-low carbon oriented silicon steel and preparation method thereof - Google Patents
Ultra-low carbon oriented silicon steel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses ultra-low carbon oriented silicon steel and a preparation method thereof. The ultra-low carbon oriented silicon steel comprises the following components in percentage by mass: 0.002%-0.005% of C, 2.8%-4.0% of Si, 0.07%-0.3% of Mn, 0.02%-0.1% of Al, no more than 0.5% of Cu, 0.01%-0.03% of S, 0.004%-0.02% of N, no more than 0.005% of O, and the balance of Fe and inevitable impurities, wherein the magnetic property P17/50 is 0.8-1.1W/kg, and the magnetic induction B8 is 1.85-1.94T. The preparation method comprises the following steps: (1) smelting molten steel, introducing the molten steel into a tundish and carrying out roll-casting to form a casting strip; (2) carrying out hot rolling; (3) carrying out laminar cooling, pickling, and carrying out two-stage cold rolling; and (4) heating to 1200+/-10 DEG C under the protective condition of nitrogen, then carrying out heat preservation under the condition of pure dry nitrogen, carrying out high-temperature annealing, and cooling to 400+/-10 DEG C along with the furnace, and carrying out air cooling. According to the method disclosed by the invention, the content of C is controlled to be lower than 50ppm; the entire process is controlled to be single-phase ferrite matrix; the molding property of the casting strip is improved; fine and uniform primary recrystallization tissues are obtained; and the product has good property.
Description
Technical field
The invention belongs to metallurgical technology field, particularly a kind of Ultra-low carbon oriented silicon steel and preparation method thereof.
Background technology
Oriented silicon steel has the fine magnetic property of high magnetic strength, low iron loss along rolling direction, is mainly used in the iron core of various transformer, is indispensable important non-retentive alloy in power electronics and war industry.Tradition directed silicon steel complicated process of preparation is tediously long mainly to be comprised: smelting-continuous casting-strand heat-hot rolling-normalizing-cold rolling-decarburizing annealing-high temperature annealing etc.; in order to ensure that perfect secondary recrystallization occurs oriented electrical steel, strand heat, course of hot rolling Comprehensive Control and normalizing process become requisite process node.Strand needs 1350 ~ 1400 DEG C of insulations to dissolve the precipitates such as thick MnS and AlN that formed in casting process and small and dispersed precipitation in subsequent hot rolled and normalizing operation, and so high Heating temperature can cause a series of shortcomings such as energy dissipation, lumber recovery is low, equipment loss is large; Control hot rolling and normalizing also improve technology difficulty and complexity.
Twin-roll thin strip continuous casting technology fundamentally changes traditional Thin Strip Steel production method, can not need through production processes such as continuous casting, heating, hot rolling and normalizing, but with two casting rolls of rotating for crystallizer, directly injected by liquid molten steel in the molten bath of casting roll and side seal board composition, going out thickness by liquid molten steel direct production is 1 ~ 6mm strip; Its process characteristic is that liquid metal bears press working and viscous deformation crystallization and freezing while, and complete all processes from liquid metal to solid-state strip in a short period of time, setting rate can reach 10
2~ 10
4dEG C/s; Therefore, thin strap continuous casting is producing the advantage in Fe-Si alloy with uniqueness; Particularly, utilize the feature of twin-roll thin strip continuous casting Sub realizable fuzzy matrix, the precipitation of second phase particles in oriented silicon steel Cast Strip and behavior of growing up can be suppressed, realize the Flexible Control of inhibitor.
Nippon patent (flat 2-258149,1990) principal character is that casting-milling technology parameter and cold-rolling process are on the impact of magnetic property of oriented silicon steel; Italy Te Erni house journal US6964711 add its feature of a time hot rolling technology with the impact of hot rolling technology on magnetic property; U.S.'s Armco house journal US6739384 principal character is cooling twice speed and the cold rolling draft of one-phase the impact of magnetic property.In order to refinement hot rolling microstructure in old process; solid solution AlN precipitate in normalizing process; need to add 0.03 ~ 0.05%C when smelting; the austenite of 20 ~ 30% is formed in hot rolling and normalizing temperature range; after cold rolling process; carry out decarburizing annealing again, to ensure iron loss lower in finished product oriented silicon steel.And mention the component system obviously also inheriting old process about the component system in casting oriented silicon steel patent above; But current method all has flow process complicated, cost is high, and the dissatisfactory shortcoming of performance.
Summary of the invention
For the problems referred to above that existing oriented silicon steel exists in preparation method and aspect of performance; the invention provides a kind of Ultra-low carbon oriented silicon steel and preparation method thereof; by Ultra-low carbon Composition Design; while omission continuous casting, hot rolling and normalizing operation; further omission decarburizing annealing operation; avoided the formation of coarse precipitates by control solidi fication and cooling twice path, obtain the high magnetic strength of Thin Specs, the directional silicon steel of low iron loss.
The composition of Ultra-low carbon oriented silicon steel of the present invention is by mass percentage containing C 0.002 ~ 0.005%, Si 2.8 ~ 4.0%, Mn 0.07 ~ 0.3%, Al 0.02 ~ 0.1%, Cu≤0.5%, S 0.01 ~ 0.03%, N 0.004 ~ 0.02%, O≤0.005%, surplus is Fe and inevitable impurity.
The magnetic property P of above-mentioned Ultra-low carbon oriented silicon steel
17/50be 0.8 ~ 1.1W/kg, magnetic strength B
8be 1.85 ~ 1.94T.
The thickness of above-mentioned Ultra-low carbon oriented silicon steel is at 0.11 ~ 0.35mm.
The preparation method of Ultra-low carbon oriented silicon steel of the present invention carries out according to the following steps:
1, by set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes Cast Strip; The superheating temperature controlling molten steel in strip casting process is 20 ~ 50 DEG C;
2, hot rolling is carried out in Cast Strip, start rolling temperature is 980 ~ 1030 DEG C, and finishing temperature is 880 ~ 950 DEG C, and total reduction, 10 ~ 15%, obtains hot-rolled strip;
3, by hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 60 ~ 70%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 850 ~ 1050 DEG C, and annealing time is 3 ~ 5min; Then it is cold rolling to carry out the two-stage, and draft is 50 ~ 90%, makes cold rolling strap;
4, under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h, then under 1200 ± 10 DEG C of conditions; under pure dry hydrogen condition, be incubated at least 20h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C; air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel.
Described pure dry hydrogen condition refers to that dew point is lower than the hydrogen circulation condition of-30 DEG C.
The thickness of the cold rolling strap in aforesaid method is at 0.11 ~ 0.35mm.
The thickness of above-mentioned Cast Strip is at Cast Strip thickness 2.0 ~ 3.0mm.
The present invention is at project of national nature science fund project (U1260204; 51174059) complete under subsidizing, the principle of Composition Design is:
Carbon controls below 0.005%; In order to form a certain amount of austenite in conventional manufacturing procedures, produce dynamic recrystallization refinement hot rolling microstructure, and better solid solution inhibitor element needs the carbon adding 0.03 ~ 0.05% when smelting during normalizing, on the other hand, for ensureing that the performance need of finished product directional silicon steel carries out decarburizing annealing in subsequent handling; Under thin strap continuous casting condition, solidification of molten steel speed, because in the delta ferrite that first formed, the solid solution capacity of C element is considerably less, cause C element local segregation, the effect of all even thinning microstructure can not be played, reduce the processability of Cast Strip on the contrary, add Sub realizable fuzzy matrix and can suppress the precipitation of precipitate and behavior of growing up, therefore can in smelting process, C content be controlled at below 50ppm, improve Cast Strip plasticity, and omit decarburizing annealing technique;
Silicone content is 2.8 ~ 4.0%; Silicon is most important alloying element in directional silicon steel, can significantly improve resistivity, reduces the eddy losses in silicon steel, promotes secondary recrystallization, improves orientation degree thus improves magnetic property; But Si content, for the reason controlling the Ovshinsky scale of construction, is limited in less than 3.4% by old process; Thin strap continuous casting flow process has then thoroughly been broken away from austenitizing and has been contained quantitative limitation to Si, therefore in oriented silicon steel composition, Si content can be brought up to 4.0%;
The content of Mn, S, Al and N respectively 0.07 ~ 0.3%, 0.01 ~ 0.03%, 0.02 ~ 0.1% and 0.004 ~ 0.02%N; In oriented silicon steel, MnS and AlN is the most frequently used inhibitor, can significantly hinder growing up of primary recrystallization crystal grain, promotes the generation of secondary recrystallization; Conventional manufacturing procedures is due to the restriction by slab heating temperature, there is the upper limit in the content of the inhibitor component of strand solid solution, and under thin strap continuous casting condition, Cast Strip can the more inhibitor components of solid solution, and its content all exceedes the restriction of old process to inhibitor constituent content.
Method of the present invention controls C content lower than 50ppm in smelting molten steel process, and controlling whole process is single-phase ferrite matrix, and improve Cast Strip processability, without the need to normalizing and decarburizing annealing technique, solid solution more suppresses element; A large amount of atom N solid solution makes easily shearing strain to occur in the cold-rolled process of Cast Strip, increases nucleation site, thus obtains the primary recrystallization tissue of fine uniform, and grain-size is 10 ~ 15 μm; Further, in primary recrystallization, goss texture originates from the shear zone of cold-reduced sheet, and through-thickness is more evenly distributed, and is conducive to improving secondary recrystallization orientation degree; Adding of a large amount of inhibitor element can significantly improve rejection ability, makes product have good performance.
Accompanying drawing explanation
Fig. 1 be in the embodiment of the present invention preparation method's schematic flow sheet of Ultra-low carbon oriented silicon steel;
Fig. 2 is the metallographic microstructure figure of the Cast Strip in the embodiment of the present invention 1;
Fig. 3 is the transmission micro-organization chart of hot-rolled strip after Cast Strip in the embodiment of the present invention 2, hot-rolled strip and annealing; Wherein (a) is Cast Strip, and (b) is hot-rolled strip, and (c) is the hot-rolled strip after process annealing;
Fig. 4 is the macrostructure figure after the cold rolling strap high temperature annealing in the embodiment of the present invention 2.
Embodiment
The equipment observing microstructure adopt in the embodiment of the present invention is Zeiss Ultra 55 type scanning electron microscope.
The equipment observing transmission microstructure adopt in the embodiment of the present invention is Tecnai F20 transmission electron microscope.
Strip caster in the embodiment of the present invention is strip caster disclosed in patent CN103551532A.
The purity of the hydrogen adopted in the embodiment of the present invention is 99.9%.
Preparation method's flow process based on strip continuous casting technology Ultra-low carbon directional silicon steel of the present invention is as shown in Figure 1: pour in tundish by ladle by the molten steel smelted, flow into by two copper crystallization rolls rotated and the molten bath that forms of side seal board again, molten steel is become strip by the casting roll casting rotated, batch after hot rolling and section cooling, iron scale is removed in pickling; Directly by one-phase rolled by cold rolling machine, carry out process annealing through continuous annealing furnace, continue through two-stage rolled by cold rolling machine to finished product thickness, carry out high temperature annealing finally by high-temperature annealing furnace.
Hydraulic pressure during section cooling in the embodiment of the present invention is 0.1 ~ 0.2MPa.
Embodiment 1
By set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes the Cast Strip of thickness 2.05mm; The superheating temperature controlling molten steel in strip casting process is 20 DEG C; Cast Strip metallographic microstructure as shown in Figure 2;
Hot rolling is carried out in Cast Strip, and start rolling temperature is 980 DEG C, and finishing temperature is 880 DEG C, and total reduction, 15%, obtains hot-rolled strip;
By hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 60%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 850 DEG C, and annealing time is 5min; Then it is cold rolling to carry out the two-stage, and draft is 50%, makes cold rolling strap, and thickness is at 0.35mm;
Under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; Then, under 1200 ± 10 DEG C of conditions, under pure dry hydrogen (dew point is lower than-30 DEG C) condition, be incubated 22h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C, and air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel, composition is by mass percentage containing C 0.002%, Si 4.0%, Mn 0.3%, Al 0.02%, S 0.023%, N 0.004%, O 0.004%, surplus is Fe and inevitable impurity, magnetic property P
17/50for 0.8W/kg, magnetic strength B
8for 1.85T, microstructure as shown in Figure 2.
Embodiment 2
By set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes the Cast Strip of thickness 2.31mm; The superheating temperature controlling molten steel in strip casting process is 30 DEG C;
Hot rolling is carried out in Cast Strip, and start rolling temperature is 1030 DEG C, and finishing temperature is 950 DEG C, and total reduction, 10%, obtains hot-rolled strip; By hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 70%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 1050 DEG C, and annealing time is 3min; Then it is cold rolling to carry out the two-stage, and draft is 57%, makes cold rolling strap, and thickness is at 0.27mm;
Under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; Then, under 1200 ± 10 DEG C of conditions, under pure dry hydrogen (dew point is lower than-30 DEG C) condition, be incubated 20h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C, and air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel, composition is by mass percentage containing C 0.003%, Si 3.7%, Mn 0.24%, Al 0.04%, S 0.018%, N 0.0094%, O 0.005%, surplus is Fe and inevitable impurity, magnetic property P
17/50for 0.9W/kg, magnetic strength B
8for 1.90T;
Cast Strip transmission microstructure is as shown in Fig. 3 (a), and as shown in Figure 3 (b), the hot-rolled strip transmission microstructure after process annealing as shown in Figure 3 (c) for hot-rolled strip transmission microstructure.
Embodiment 3
By set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes the Cast Strip of thickness 2.41mm; The superheating temperature controlling molten steel in strip casting process is 40 DEG C;
Hot rolling is carried out in Cast Strip, and start rolling temperature is 1000 DEG C, and finishing temperature is 900 DEG C, and total reduction, 11%, obtains hot-rolled strip;
By hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 65%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 950 DEG C, and annealing time is 4min; Then it is cold rolling to carry out the two-stage, and draft is 80%, makes cold rolling strap, and thickness is at 0.15mm;
Under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; Then, under 1200 ± 10 DEG C of conditions, under pure dry hydrogen (dew point is lower than-30 DEG C) condition, be incubated 22h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C, and air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel, composition is by mass percentage containing C 0.004%, Si 2.8%, Mn 0.19%, Al 0.05%, S 0.015%, N 0.008%, O 0.003%, surplus is Fe and inevitable impurity, magnetic property P
17/50for 1.1W/kg, magnetic strength B
8for 1.94T.
Embodiment 4
By set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes the Cast Strip of thickness 2.73mm; The superheating temperature controlling molten steel in strip casting process is 50 DEG C;
Hot rolling is carried out in Cast Strip, and start rolling temperature is 1010 DEG C, and finishing temperature is 920 DEG C, and total reduction, 13%, obtains hot-rolled strip;
By hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 60%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 900 DEG C, and annealing time is 5min; Then it is cold rolling to carry out the two-stage, and draft is 81%, makes cold rolling strap, and thickness is at 0.18mm;
Under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; Then, under 1200 ± 10 DEG C of conditions, under pure dry hydrogen (dew point is lower than-30 DEG C) condition, be incubated 24h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C, and air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel, composition is by mass percentage containing C 0.005%, Si 3.2%, Mn 0.11%, Al 0.09%, S 0.018%, N 0.008%, O 0.003%, surplus is Fe and inevitable impurity, magnetic property P
17/50for 1.1W/kg, magnetic strength B
8for 1.94T.
Embodiment 5
By set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes the Cast Strip of thickness 3.0mm; The superheating temperature controlling molten steel in strip casting process is 30 DEG C;
Hot rolling is carried out in Cast Strip, and start rolling temperature is 980 DEG C, and finishing temperature is 880 DEG C, and total reduction, 10%, obtains hot-rolled strip;
By hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 60%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 1000 DEG C, and annealing time is 3min; Then it is cold rolling to carry out the two-stage, and draft is 90%, makes cold rolling strap, and thickness is at 0.11mm;
Under nitrogen protection condition, cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; Then, under 1200 ± 10 DEG C of conditions, under pure dry hydrogen (dew point is lower than-30 DEG C) condition, be incubated 20h, carry out high temperature annealing, last furnace cooling is to 400 ± 10 DEG C, and air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel, composition is by mass percentage containing C 0.002%, Si 3.5%, Mn 0.07%, Al 0.1%, Cu 0.05%, S 0.02%, N 0.01%, O 0.002%, surplus is Fe and inevitable impurity, magnetic property P
17/50for 1.0W/kg, magnetic strength B
8for 1.85T.
Claims (5)
1. a Ultra-low carbon oriented silicon steel, is characterized in that composition by mass percentage containing C 0.002 ~ 0.005%, Si 2.8 ~ 4.0%, Mn 0.07 ~ 0.3%, Al 0.02 ~ 0.1%, Cu≤0.5%, S 0.01 ~ 0.03%, N 0.004 ~ 0.02%, O≤0.005%, surplus is Fe and inevitable impurity.
2. Ultra-low carbon oriented silicon steel according to claim 1, is characterized in that the magnetic property P of this oriented silicon steel
17/50be 0.8 ~ 1.1W/kg, magnetic strength B
8be 1.85 ~ 1.94T.
3. Ultra-low carbon oriented silicon steel according to claim 1, is characterized in that the thickness of this oriented silicon steel is at 0.11 ~ 0.35mm.
4. a preparation method for Ultra-low carbon oriented silicon steel according to claim 1, is characterized in that carrying out according to the following steps:
(1) by set component smelting molten steel, then entered the tundish of preheating by cast gate, now tundish preheating temperature is 1200 ~ 1250 DEG C, and molten steel enters in strip caster by tundish, and casting becomes Cast Strip; The superheating temperature controlling molten steel in strip casting process is 20 ~ 50 DEG C;
(2) hot rolling is carried out in Cast Strip, start rolling temperature is 980 ~ 1030 DEG C, and finishing temperature is 880 ~ 950 DEG C, and total reduction, 10 ~ 15%, obtains hot-rolled strip;
(3) by hot-rolled strip section cooling, then iron scale is removed in pickling, then it is cold rolling to carry out two benches; The cold rolling draft of one-phase is 60 ~ 70%, the cold rolling laggard interline annealing of one-phase, and annealing temperature is 850 ~ 1050 DEG C, and annealing time is 3 ~ 5min; Then it is cold rolling to carry out the two-stage, and draft is 50 ~ 90%, makes cold rolling strap;
(4) under nitrogen protection condition; cold rolling strap is warming up to 1200 ± 10 DEG C with the speed of 10 ~ 30 DEG C/h; then under 1200 ± 10 DEG C of conditions; under pure dry hydrogen condition, be incubated at least 20h carry out high temperature annealing; last furnace cooling is to 400 ± 10 DEG C; air cooling, to normal temperature, obtains Ultra-low carbon oriented silicon steel.
5. the preparation method of Ultra-low carbon oriented silicon steel according to claim 4, is characterized in that the thickness of described Cast Strip is at Cast Strip thickness 2.0 ~ 3.0mm.
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CN107164692A (en) * | 2017-06-01 | 2017-09-15 | 东北大学 | A kind of method of the quick secondary recrystallization of orientation silicon steel based on thin band continuous casting technique |
CN108339851A (en) * | 2017-12-21 | 2018-07-31 | 东北大学 | A kind of cold rolling of oriented silicon steel strip in razor-thin and method for annealing |
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CN114134423A (en) * | 2021-12-02 | 2022-03-04 | 东北大学 | Ultrashort-flow rare earth oriented silicon steel and preparation method thereof |
CN114134421A (en) * | 2021-12-02 | 2022-03-04 | 东北大学 | Ultra-low-carbon yttrium-containing oriented silicon steel and preparation method thereof |
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