CN116752042A - 一种具有自粘结性的高磁感取向硅钢极薄带的制备方法 - Google Patents
一种具有自粘结性的高磁感取向硅钢极薄带的制备方法 Download PDFInfo
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Abstract
一种具有自粘结性的高磁感取向硅钢极薄带的制备方法:母材选择;冷轧;退火;涂覆;待用。本发明不仅产品厚度在0.03~0.12mm,且使磁通密度B800为1.85~1.95T、损耗P1.5/400为7.50~16.50W/kg,T型剥离强度不低于0.50N/mm,并采用一次性冷轧,满足了电力电子行业设备中对于低损耗、高磁感中高频用极薄取向硅钢,及自粘接性能T型剥离强度不低于0.50N/mm需求。
Description
技术领域
本发明涉及一种取向硅钢的生产方法,具体属于一种具有自粘结性的高磁感取向硅钢极薄带的制备方法。
背景技术
取向硅钢极薄带是将传统的取向硅钢成品经过冷轧和退火而获得,主要用作高频变压器、大功率磁放大器、脉冲变压器、脉冲发电机、通讯的轭流圈、电感、储存和记忆元件,以及在振动和辐射条件下工作的变压器,在频率为400Hz~1000Hz范围显示出极低的铁损,被视为较高频率用的变压器铁芯材料。目前取向硅钢极薄带涂层主要为磷酸盐—铬酸盐绝缘涂层,其在去应力退火前后的绝缘性、附着性存在着一定的问题,同时取向硅钢极薄带在生产成本(如二次轧制导致成本偏高)、产品质量(磁感不能达到1.92T)等方面均存在一些问题。
中国专利申请号为CN201510239650.6的文献,公开了《一种厚度0.02mm超薄取向硅钢薄带的生产方法》,其工艺:(1)第一次冷轧:采用普通取向硅钢作为钢带原料,在室温下,保证一定的变形率范围下,进行第一次冷轧;(2)中间退火:在还原气氛下,进行中间退火,退火的温度为750℃~1150℃,形成再结晶组织;(3)第二次冷轧:在室温下,保证一定的变形率范围下,进行第二次冷轧,终轧厚度为0.02mm;(4)再结晶退火:在还原气氛下,进行再结晶退火,退火的温度为750℃~1150℃,形成再结晶组织;(5)涂覆:连续涂覆绝缘涂层,得到超薄取向硅钢薄带。该文献要进行两次轧制,导致生产成本提高。
中国专利申请号为CN201810126373.1的文献,公开了《一种超薄取向硅钢板材及其制备方法》:其工艺:(1)将无底层的板材经1~5道次冷轧得到厚度为0.01mm~0.1mm的冷轧板材;(2)将冷轧板材在H2气氛的连续退火炉中再结晶退火,得到退火的板材;(3)在退火的板材的表面涂覆厚度为0.1μm~2μm的涂层,得到超薄取向硅钢板材。该文献所制备的超薄取向硅钢板材厚度为0.01mm~0.1mm,带材损耗P1.5T/400Hz为9W/kg~16W/kg,磁通密度B8为1.75T~1.90T,能满足现有的电力、电子行业中电抗器、传感器等设备中对低损、高磁感中频软磁材料的需求。该文献B8为1.75T~1.90T较低,最高为1.90T,未能满足发展的电力、电子行业中电抗器、传感器等设备中对低损、高磁感中频软磁材料的需求。
中国专利申请号为申请号为CN201911126518.9的文献,公开了《一种具有自粘接性的取向硅钢及其制备方法》,其工艺:(1)炼钢,将Als含量控制在0.020%~0.035%,N含量控制在0.0050%~0.0100%,Mn含量控制在0.010%~1.00%,S含量控制在0.0030%~0.0300%,并在炼钢工序中加入少量P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种(P+Cu+Sn+Bi+Sb+Cr+As≤1.80%)作为辅助抑制剂;(2)经1100℃~1400℃低温或高温加热后的热轧;(3)热轧板1000℃~1150℃常化处理,经一次冷轧、脱碳退火、渗氮处理(热轧板坯≥1260℃加热时不渗氮)、涂氧化镁隔离涂层和高温退火后,获得0.15mm~0.50mm厚度的无硅酸镁底层取向硅钢,并涂敷含环氧树脂的有机自粘接绝缘涂层后,获得B800≥1.80T,P17≤1.60W/kg的成品性能,且T型剥离强度≥0.50N/mm的自粘接涂层取向硅钢成品。该文献所制备的取向硅钢成品厚度为0.15mm~0.50mm,为传统厚度规格的取向硅钢,使用性能为工频50Hz下磁性能。
发明内容
本发明在于克服现有技术存在的不足,提供一种不仅产品厚度在0.03~0.12mm,且使成品磁通密度B800为1.85~1.95T、损耗P1.5/400为7.50~
16.50W/kg,T型剥离强度不低于0.50N/mm,并采用一次性冷轧,满足了电力电子行业设备中对于低损耗、高磁感中高频用极薄取向硅钢,及自粘接性能T型剥离强度不低于0.50N/mm需求的高磁感取向硅钢极薄带的制备方法。
实现上述目的的措施:
一种具有自粘结性的高磁感取向硅钢极薄带的制备方法,其步骤:
1)母材
母材条件:
母材组分及重量百分比含量为:Si:2.80%~3.60%,Mn:0.01%~
1.00%,含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种的复合,且
满足(P+Cu+Sn+Bi+Sb+Cr+As)≤1.80%,其余为铁及不可避免的杂质;
母材性能:沿板宽全板面无硅酸镁底层,B800≥1.88T,P1.7/50≤1.45W/kg;
2)进行冷轧
采用常温冷轧;在冷轧累计压下率不低于65%下,经2~10道次可逆
式冷轧得到厚度为0.03mm~0.12mm的产品;
3)进行退火
退火气氛为干式H2与N2的混合气体或全H2;混合气体中H2的体积含量不低于50%,其余为N2;退火温度控制在750~1050℃,并在此温度下保温30~300S;
4)进行涂覆
a、在带材的表面涂覆有机水性绝缘涂料,并控制单面涂层厚度在0.05~2.00μm;
b、对涂层进行固化:固化温度控制在150~750℃,并在此保温下保温30~180S;
C、进行常规烘干,控制烘干后不挥发分含量在30~80%;
5)待用。
其在于:所述有机水性绝缘涂料的组成及重量百分比含量为:环氧树脂20.0~70.0%,潜伏型固化剂2.0~5.0%,其余为水。
优选地:所述固化温度控制在157~739℃,并在此保温下保温35~173S。
优选地::单面涂层厚度在0.05~1.93μm。
本发明中各原料及主要工艺的作用及机理
本发明之所以采用加入Si的母材,是由于Si能够提高电阻率,降低铁损。但是Si含量提高会导致加工脆性,因此,为保证加工性需控制Si的含量,Si含量在2.80%~3.60%之间;母材中Mn为有利析出MnS形成元素,而在1100℃~1200℃低温热轧工艺取向硅钢生产中,则以AlN为主要抑制剂,而Mn含量提高可降低涡流损耗,因此控制Mn含量在0.010%~1.00%;含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种,主要用作辅助抑制剂,且可降低涡流损耗,但含量不宜过高,因此控制(P+Cu+Sn+Bi+Sb+Cr+As)≤1.80%;母材沿板宽全板面无硅酸镁底层且板面干净、光洁,二次再结晶晶粒大小均匀,有利于再轧加工,提高加工效率,B800≥1.88T、P1.7/50≤1.45W/kg,母材磁性能优良有利于获得取向硅钢极薄带优良的成品性能。
本发明之所以采用一次轧制的常温冷轧工艺,经2~10道次可逆式冷轧得到冷轧带材,保证冷轧压下率>65%,冷轧成品带材厚度为0.03mm~0.12mm,以使降低冷轧工序制造成本,并保证获得取向硅钢极薄带优良的成品性能。
本发明之所以退火气氛为干式H2与N2的混合气体或全H2;混合气体中H2的体积含量不低于50%,其余为N2;退火温度控制在750~1050℃,并在此温度下保温30~180S,以使冷轧形变组织完成回复和再结晶,使基体中足够数量的[110](001)晶核(高斯晶核)长大,形成以高斯晶粒为主导的再结晶组织和织构,并尽量减少极薄带的表面氧化。
本发明之所以在带材表面涂覆单面厚度为0.05~2.00的有机水性绝缘涂料层,并控制涂层固化温度再150~750℃,固化保温时间再30~180S,在于以保证获得优良的极薄带成品附着性。
本发明与现有技术相比,本发明不仅产品厚度在0.03~0.12mm,且使磁通密度B800为1.85~1.95T、损耗P1.5/400为7.50~16.50W/kg,T型剥离强度不低于0.50N/mm,并采用一次性冷轧,满足了电力电子行业设备中对于低损耗、高磁感中高频用极薄取向硅钢,及自粘接性能T型剥离强度不低于0.50N/mm需求。
具体实施方式
下面对本发明予以详细描述:
表1为本发明各实施例及对比例的化学成分及退火工艺取值列表;
表2为本发明各实施例及对比例的涂液成分、固化工艺参数列表;
表3为本发明各实施例性及对比例性能检测情况列表。
本发明各实施例按照以下步骤生产
1)母材
母材条件:
母材组分及重量百分比含量为:Si:2.80%~3.60%,Mn:0.01%~
1.00%,含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种的复合,且
满足(P+Cu+Sn+Bi+Sb+Cr+As)≤1.80%,其余为铁及不可避免的杂质;
母材性能:沿板宽全板面无硅酸镁底层,B800≥1.88T,P1.7/50≤1.45W/kg;2)进行冷轧
采用常温冷轧;在冷轧累计压下率不低于65%下,经2~10道次可逆式冷轧得到厚度为0.03mm~0.12mm的产品;
3)进行退火
退火气氛为干式H2与N2的混合气体或全H2;混合气体中H2的体积含量不低于50%,其余为N2;退火温度控制在750~1050℃,并在此温度下保温30~300S;
4)进行涂覆
a、在带材的表面涂覆有机水性绝缘涂料,并控制单面涂层厚度在0.05~2.00μm;
b、对涂层进行固化:固化温度控制在150~750℃,并在此保温下保温30~180S;
C、进行常规烘干,控制烘干后不挥发分含量在30~80%;
5)待用。
表1本发明各实施例及对比例的取值列表(无硅酸镁底层取向硅钢母材相关要求、薄带退火工艺)
从表1可以看出,对比例Q1中无硅酸镁底层取向硅钢母材Si<2.80%,Mn<0.010%,Si、Mn含量偏低,母材磁感B800偏低,损耗P1.7/50偏高,导致极薄带损耗P1.5/400偏高,(P+Cu+Sn+Bi+Sb+Cr+As)>1.80%,导致热轧、冷轧加工难度加大,生产成本提高,退火温度<750℃,退火时间>300S,再结晶晶粒长大,导致极薄带成品性能整体下降,保护气氛中H2的体积含量<50%,再结晶发生不完全,导致极薄带成品性能整体下降;对比例Q2中母材Si<2.80%,Mn<0.010%,Si、Mn含量偏低,母材磁感B800偏低,母材损耗P1.7/50偏高,导致极薄带损耗P1.5/400偏高,(P+Cu+Sn+Bi+Sb+Cr+As)>1.80%,导致热轧、冷轧加工难度加大,生产成本提高,退火温度<750℃,退火时间>300S,再结晶晶粒长大,导致极薄带成品性能整体下降,保护气氛中H2的体积含量<50%,再结晶发生不完全,导致极薄带成品性能整体下降;对比例Q3中母材Si>3.60%,Mn>1.00%,(P+Cu+Sn+Bi+Sb+Cr+As)>1.80%,Si、Mn含量偏高,导致热轧、冷轧加工难度加大,生产成本提高,同时Mn>1.00%,母材性能整体下降,磁感B800偏低,损耗P1.7/50偏高,导致极薄带成品性能整体下降,退火温度>1050℃,退火时间<30S,再结晶晶粒长大,导致极薄带成品性能整体下降,保护气氛中H2的体积含量<50%,再结晶发生不完全,导致极薄带成品性能整体下降。
表2本发明各实施例及对比例的主要工艺参数列表(涂液成分、固化工艺)
说明:表2中有机水性绝缘涂料除所列物料外,其余均为水。
对比例Q1中环氧树脂<20.00%、潜伏型固化剂<2.00%,涂层经烘干后不挥发成分含量<30%,膜厚<0.05μm,固化温度<150℃,固化时间>180S,极薄带成品自粘接性下降;对比例Q2中环氧树脂<20.00%、潜伏型固化剂<2.00%,涂层经烘干后不挥发成分含量<30%,固化温度>750℃,固化时间<30S,极薄带成品自粘接性下降,膜厚>2.00μm,导致极薄带成品损耗P1.5/400升高,整体性能下降;对比例Q3中环氧树脂>70.00%、潜伏型固化剂>5.00%,涂层经烘干后不挥发成分含量>80%,固化温度>750℃,固化时间<30S,极薄带成品自粘接性下降,膜厚>2.00μm,导致极薄带成品损耗P1.5/400升高,整体性能下降。
表3本发明各实施例及对比例性能检测情况列表
对比例Q1中极薄带成品磁感B800<1.85T,损耗P1.5/400>16.50W/kg,成品T型剥离强度<0.50N/mm;对比例Q2中极薄带成品磁感B800<1.85T,损耗P1.5/400>16.50W/kg,成品T型剥离强度<0.50N/mm;对比例Q3极薄带成品磁感B800<1.85T,损耗P1.5/400>16.50W/kg,成品T型剥离强度<0.50N/mm。
本具体实施方式仅为最佳例举,并非对本发明技术方案的限制性实施。
Claims (4)
1.一种具有自粘结性的高磁感取向硅钢极薄带的制备方法,其步骤:
1)母材
母材条件:
母材组分及重量百分比含量为:Si:2.80%~3.60%,Mn:0.01%~1.00%,含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种的复合,且满足(P+Cu+Sn+Bi+Sb+Cr+As)≤1.80%,其余为铁及不可避免的杂质;
母材性能:沿板宽全板面无硅酸镁底层,B800≥1.88T,P1.7/50≤1.45W/kg;
2)进行冷轧
采用常温冷轧;在冷轧累计压下率不低于65%下,经2~10道次可逆式冷轧得到厚
度为0.03mm~0.12mm的产品;
3)进行退火
退火气氛为干式H2与N2的混合气体或全H2;混合气体中H2的体积含量不低于50%,其余为N2;退火温度控制在750~1050℃,并在此温度下保温30~300S;
4)进行涂覆
a、在带材的表面涂覆有机水性绝缘涂料,并控制单面涂层厚度在0.05~2.00μm;
b、对涂层进行固化:固化温度控制在150~750℃,并在此保温下保温30~180S;
C、进行常规烘干,控制烘干后不挥发分含量在30~80%;
5)待用。
2.如权利要求1所述的一种具有自粘结性的高磁感取向硅钢极薄带的制备方法,其特征在于:所述有机水性绝缘涂料的组成及重量百分比含量为:环氧树脂20.0~70.0%,潜伏型固化剂2.0~5.0%,其余为水。
3.如权利要求1所述的一种具有自粘结性的高磁感取向硅钢极薄带的制备方法,其特征在于:所述固化温度控制在157~739℃,并在此保温下保温35~173S。
4.如权利要求1所述的一种具有自粘结性的高磁感取向硅钢极薄带的制备方法,其特征在于:单面涂层厚度在0.05~1.93μm。
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