高磁性能冷轧无取向硅钢薄带的研制
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摘要
本文通过添加有利元素、热轧板常化、调整冷轧和退火工艺等方法成功研制出高磁性能的0.2mm厚冷轧无取向硅钢薄带产品,产品性能(B50≥1.66T、P1.0/400≤11W/kg)达到了新日铁同类牌号(20HTH1200)的标准,处于世界先进水平,满足了国内部分用户对该类产品的需求。论文分析和探讨了热轧板常化、冷轧和退火工艺、元素晶界偏聚等因素对无取向硅钢薄带磁性能、晶粒尺寸、织构、析出物等方面的影响。
研究结果表明,常化使得热轧板组织更均匀,能够明显降低无取向硅钢薄带的铁损,但对磁感应强度无明显影响。随着常化温度的升高成品晶粒尺寸增大且更加均匀,但过高温度的常化会使成品晶粒尺寸偏大同时均匀性变差,常化温度选择在900～950℃比较适宜。随着常化温度的升高,成品钢带中{100}面织构和(110)[001]织构等有利织构比例逐渐增高,同时{111}面不利织构组分的比例在逐渐的降低。
在对冷轧工艺的研究中发现,采用一次冷轧工艺由于压下率过大,成品钢带中{111}面不利织构组分的比例较高,铁损偏高,磁性能不理想。采用二次冷轧工艺时,较低和较高的第二次冷轧压下率生产出的成品钢带中{111}面不利织构组分的比例都比较高,第二次冷轧压下率控制在55-70%比较适宜,能够获得铁损较低同时磁感应强度较高的无取向硅钢薄带产品。
Sn元素的添加对于降低无取向硅钢薄带的铁损有明显的效果,但也会在一定程度上降低磁感应强度,对二者的影响与Sn的添加量有关。添加0.05%Sn对铁损和磁感应强度无明显影响；当Sn的添加量为0.1%时,铁损明显下降,同时磁感应强度也有一定程度的降低；当Sn的添加量为0.15%时,磁感应强度与添加量为0.1%时相比变化不大,但铁损有所增高。随着Sn含量的增高,成品钢带中{111}面织构的比例逐渐降低,晶粒尺寸也明显减小。Sn沿晶界偏聚降低了晶界能,使得{111}面织构在原始晶界处的形核和晶粒长大过程受到了抑制,从而降低了成品钢带中{111}面织构的比例。在对Sn元素晶界偏聚的研究过程中发现,Sn在晶界上的偏聚量并不均匀,不同样品晶界处Sn的平均偏聚量也不同。经过统计,700℃保温后的常化板中Sn的平均偏聚量最高,成品板中平均偏聚量其次,常化板中的平均偏聚量最低。随着Sn添加量的增加,晶界处Sn的平均偏聚量逐渐增加。
实验在常化板中观察到了在晶界处钉扎的TiN析出物,TiN等析出物很难在最终退火过程中去除,会对成品钢带的磁畴移动产生不利影响,在钢的冶炼过程中,应尽量降低Ti的含量。在热轧板和常化板中都观察到了MnS析出物,热轧板中的MnS尺寸较小、数量较多,常化板中的MnS析出物尺寸较大、数量较少。高温常化使得热轧板中原本细小弥散分布的MnS粗化,发生Ostwald长大。MnS析出物数量减少且尺寸增大,这对于最终退火时再结晶晶粒长大过程有利,同时也减小了成品钢带中畴壁移动时的阻碍,对提高成品钢带磁性能有利。
In this dissertation, through adding favourable element, hot band normalizing, changing manufacturing parameter of cold rolling and annealing, thin non-oriented electrical steel sheets (thickness of 0.2mm) with high magnetic properties have been manufactured successfully. The magnetic properties of these products have achieved the level of 20HTH1200, the same grade product of NSC, and satisfied requirements in China. The effects of hot band normalizing, cold rolling and annealing process, grain boundary segregation on magnetic properties, grain size, texture, precipitation have been analyzed and discussed.
The experimental results showed that normalizing could make the structure of hot band more uniform and reduce the core loss obviously, but it had little effect on the magnetic induction. As the normalizing temperature increased the grain size of final product was larger and became more even, but the grain became overlarge and uneven if normalized at overhigh temperature. The best normalizing temperature was between 900℃and 950℃. The proportion of{100}texture and (110)[001] texture increased and the proportion of{111} texture decreased when increasing the normalizing temperature.
The research on cold rolling process showed that because of the overhigh reduction the proportion of{111} texture in final product was very high and the magnetic properties were bad when using single-stage cold rolling process. When using two-stage cold rolling process, the proportion of{111} texture was also high with the overhigh or overlow second cold rolling reduction. The best magnetic properties were obtained when the second cold rolling reduction was between 55% and 70%.
The addition of Tin could reduce the core loss and it also make the magnetic induction reduce, the effects were related to the content of Tin. There was little effect on the core loss and magnetic induction when the content of Tin was 0.05%. When the content was increased to 0.1% the core loss and magnetic induction reduced obviously. When the content reached 0.15% the magnetic induction had little change compared with adding 0.1% Tin, but the core loss increased a little. As the content of Tin increase the proportion of{111} texture in final product decrease obviously as well as the grain size. Because the grain boundary segregation of Tin could reduce the grain boundary energy the nucleation and grain growth of{111} nucleus at the original grain boundary were restrained. We found that the distribution of Tin at the grain boundary was no equal and was proportional to the content of Tin. Different specimens had different average contents of Tin at at the grain boundary, the normalized band after annealing at 700℃for 5 hours was the highest, the final product was the medial and the normalized band was the lowest.
TiN precipitate pin at the grain boundary in the final product was observed. The TiN precipitate could block the movement of magnetic domain, which was bad to the magnetic properties. So it's better for the magnetic properties to reduce the content of Ti in electrical steels as much as possible. There were MnS precipitates with different quantity and size in hot band and normalized band. The quantity of MnS precipitates in hot band was higher than normalized band, the size of MnS precipitate in normalized band was larger. Normalizing can make small MnS precipitates in hot band congregate and enlarge, it is benefit for the grain growth in final annealing process and the movement of domain-wall in final product.
研究结果表明,常化使得热轧板组织更均匀,能够明显降低无取向硅钢薄带的铁损,但对磁感应强度无明显影响。随着常化温度的升高成品晶粒尺寸增大且更加均匀,但过高温度的常化会使成品晶粒尺寸偏大同时均匀性变差,常化温度选择在900～950℃比较适宜。随着常化温度的升高,成品钢带中{100}面织构和(110)[001]织构等有利织构比例逐渐增高,同时{111}面不利织构组分的比例在逐渐的降低。
在对冷轧工艺的研究中发现,采用一次冷轧工艺由于压下率过大,成品钢带中{111}面不利织构组分的比例较高,铁损偏高,磁性能不理想。采用二次冷轧工艺时,较低和较高的第二次冷轧压下率生产出的成品钢带中{111}面不利织构组分的比例都比较高,第二次冷轧压下率控制在55-70%比较适宜,能够获得铁损较低同时磁感应强度较高的无取向硅钢薄带产品。
Sn元素的添加对于降低无取向硅钢薄带的铁损有明显的效果,但也会在一定程度上降低磁感应强度,对二者的影响与Sn的添加量有关。添加0.05%Sn对铁损和磁感应强度无明显影响；当Sn的添加量为0.1%时,铁损明显下降,同时磁感应强度也有一定程度的降低；当Sn的添加量为0.15%时,磁感应强度与添加量为0.1%时相比变化不大,但铁损有所增高。随着Sn含量的增高,成品钢带中{111}面织构的比例逐渐降低,晶粒尺寸也明显减小。Sn沿晶界偏聚降低了晶界能,使得{111}面织构在原始晶界处的形核和晶粒长大过程受到了抑制,从而降低了成品钢带中{111}面织构的比例。在对Sn元素晶界偏聚的研究过程中发现,Sn在晶界上的偏聚量并不均匀,不同样品晶界处Sn的平均偏聚量也不同。经过统计,700℃保温后的常化板中Sn的平均偏聚量最高,成品板中平均偏聚量其次,常化板中的平均偏聚量最低。随着Sn添加量的增加,晶界处Sn的平均偏聚量逐渐增加。
实验在常化板中观察到了在晶界处钉扎的TiN析出物,TiN等析出物很难在最终退火过程中去除,会对成品钢带的磁畴移动产生不利影响,在钢的冶炼过程中,应尽量降低Ti的含量。在热轧板和常化板中都观察到了MnS析出物,热轧板中的MnS尺寸较小、数量较多,常化板中的MnS析出物尺寸较大、数量较少。高温常化使得热轧板中原本细小弥散分布的MnS粗化,发生Ostwald长大。MnS析出物数量减少且尺寸增大,这对于最终退火时再结晶晶粒长大过程有利,同时也减小了成品钢带中畴壁移动时的阻碍,对提高成品钢带磁性能有利。
In this dissertation, through adding favourable element, hot band normalizing, changing manufacturing parameter of cold rolling and annealing, thin non-oriented electrical steel sheets (thickness of 0.2mm) with high magnetic properties have been manufactured successfully. The magnetic properties of these products have achieved the level of 20HTH1200, the same grade product of NSC, and satisfied requirements in China. The effects of hot band normalizing, cold rolling and annealing process, grain boundary segregation on magnetic properties, grain size, texture, precipitation have been analyzed and discussed.
The experimental results showed that normalizing could make the structure of hot band more uniform and reduce the core loss obviously, but it had little effect on the magnetic induction. As the normalizing temperature increased the grain size of final product was larger and became more even, but the grain became overlarge and uneven if normalized at overhigh temperature. The best normalizing temperature was between 900℃and 950℃. The proportion of{100}texture and (110)[001] texture increased and the proportion of{111} texture decreased when increasing the normalizing temperature.
The research on cold rolling process showed that because of the overhigh reduction the proportion of{111} texture in final product was very high and the magnetic properties were bad when using single-stage cold rolling process. When using two-stage cold rolling process, the proportion of{111} texture was also high with the overhigh or overlow second cold rolling reduction. The best magnetic properties were obtained when the second cold rolling reduction was between 55% and 70%.
The addition of Tin could reduce the core loss and it also make the magnetic induction reduce, the effects were related to the content of Tin. There was little effect on the core loss and magnetic induction when the content of Tin was 0.05%. When the content was increased to 0.1% the core loss and magnetic induction reduced obviously. When the content reached 0.15% the magnetic induction had little change compared with adding 0.1% Tin, but the core loss increased a little. As the content of Tin increase the proportion of{111} texture in final product decrease obviously as well as the grain size. Because the grain boundary segregation of Tin could reduce the grain boundary energy the nucleation and grain growth of{111} nucleus at the original grain boundary were restrained. We found that the distribution of Tin at the grain boundary was no equal and was proportional to the content of Tin. Different specimens had different average contents of Tin at at the grain boundary, the normalized band after annealing at 700℃for 5 hours was the highest, the final product was the medial and the normalized band was the lowest.
TiN precipitate pin at the grain boundary in the final product was observed. The TiN precipitate could block the movement of magnetic domain, which was bad to the magnetic properties. So it's better for the magnetic properties to reduce the content of Ti in electrical steels as much as possible. There were MnS precipitates with different quantity and size in hot band and normalized band. The quantity of MnS precipitates in hot band was higher than normalized band, the size of MnS precipitate in normalized band was larger. Normalizing can make small MnS precipitates in hot band congregate and enlarge, it is benefit for the grain growth in final annealing process and the movement of domain-wall in final product.
引文
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