CN116752043A - 一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法 - Google Patents

一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法 Download PDF

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CN116752043A
CN116752043A CN202310731488.4A CN202310731488A CN116752043A CN 116752043 A CN116752043 A CN 116752043A CN 202310731488 A CN202310731488 A CN 202310731488A CN 116752043 A CN116752043 A CN 116752043A
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silicon steel
oriented silicon
coating
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杨佳欣
张宁国
申明辉
赵胜利
李国保
王雄奎
杜玉泉
骆新根
张敬
何伟
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Wuhan Iron and Steel Co Ltd
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Abstract

一种绝缘性能优良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，单面层间电阻值不低于100Ω.cm2，且仅采用一次冷轧，并满足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材料，及绝缘性能在单面层间电阻值不低于100Ω.cm2的需求。

Description

一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法
技术领域
本发明涉及一种取向硅钢的生产方法，具体属于一种绝缘性能优良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CN201911127354.1的文献，公开了《一种能提高涂层附着性能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，并涂敷含钛白粉等无机填充料的有机水性醇酸树脂绝缘涂层后，获得B800≥1.80T，P17≤1.60W/kg成品性能的特殊涂层取向硅钢成品。本申请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。
上述专利或涉及到加工中的二次轧制导致生产成本提高，或为传统厚度规格0.15mm～0.50mm的取向硅钢，或未进一步提高成品性能，因而不能满足电力电子行业中高频变压器、大功率磁放大器、脉冲变压器等对低损耗、高磁感的需求。
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，且使磁通密度B800为1.85～1.95T、损耗P1.5/400为7.50～16.50W/kg，单面层间电阻值不低于100Ω.cm2，且仅采用一次冷轧，并满足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材料，及绝缘性能在单面层间电阻值不低于100Ω.cm2的需求的绝缘性能优良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：
一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法，其步骤：
1)母材
母材成分Si＝2.80％～3.60％，Mn＝0.010％～1.00％，含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种，且满足(P+Cu+Sn+Bi+Sb+Cr+As)≤
1.80％，其余为铁和不可避免的杂质；
母材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、在带材的表面涂覆半有机水性醇酸树脂绝缘涂料，并控制单面涂层厚度在0.05～3.00μm；
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；并满足涂层经常规烘干后不挥发成分含量在30～80％；
5)待用。
其在于：所述半有机水性醇酸树脂绝缘涂料的组成及重量百分比含量为：醇酸树脂0.50～20％、氨基树脂0.50～20％、钛白粉0.50～30％、硫酸钡0.50～30％，其余为水。
优选地：固化温度控制在158～741℃，并在此保温下保温37～172S。
优选地单面涂层厚度在0.05～2.86μm。
本发明中各原料及主要工艺的作用及机理
本发明之所以选择在母材中加入Si的木材，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0.03～0.12mm，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。
本发明之所以在还原性气氛中进行成品退火，退火温度为750～1050℃，保温时间30～300S，保护气氛为干式H2与N2的混合气体，气氛中H2的体积含量为50～100％，以使冷轧形变组织完成回复和再结晶，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，并尽量减少极薄带带材的表面氧化。
本发明之所以在带材表面涂覆单面厚度为0.05～2.00的有机水溶性树脂绝缘涂料层，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绝缘性，即绝缘性能在单面层间电阻值不低于100Ω.cm。
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，单面层间电阻值不低于100Ω.cm2，且仅采用一次冷轧，并满足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材料，及绝缘性能在单面层间电阻值不低于100Ω.cm2的需求。
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
母材成分Si＝2.80％～3.60％，Mn＝0.010％～1.00％，含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种，且满足(P+Cu+Sn+Bi+Sb+Cr+As)≤
1.80％，其余为铁和不可避免的杂质；
母材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、在带材的表面涂覆半有机水性醇酸树脂绝缘涂料，并控制单面涂层厚度在0.05～3.00μm；
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；并满足涂层经常规烘干后不挥发成分含量在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中半有机水性醇酸树脂绝缘涂料除所列物料外，其余均为水。
对比例Q1中醇酸树脂＜0.50％、氨基树脂＜0.50％、钛白粉＜0.50％、硫酸钡＜0.50％，涂层经烘干后不挥发成分含量＜30％，极薄带成品层间电阻值下降，绝缘性能降低，膜厚＜0.05μm，固化温度＜150℃，固化时间＞180S，极薄带成品层间电阻值下降，绝缘性能降低；对比例Q2中醇酸树脂＜0.50％、氨基树脂＜0.50％、钛白粉＜0.50％、硫酸钡＜0.50％，涂层经烘干后不挥发成分含量＜30％，极薄带成品层间电阻值下降，绝缘性能降低，膜厚＞3.00μm，固化温度＞750℃，固化时间＜30S，极薄带成品层间电阻值下降，绝缘性能降低，膜厚＞3.00μm，导致极薄带成品损耗P1.5/400升高，整体性能下降；对比例Q3中醇酸树脂＜0.50％、氨基树脂＜0.50％、钛白粉＜0.50％、硫酸钡＜0.50％，涂层经烘干后不挥发成分含量＜30％，极薄带成品层间电阻值下降，绝缘性能降低，膜厚＞3.00μm，固化温度＞750℃，固化时间＜30S，极薄带成品层间电阻值下降，绝缘性能降低，膜厚＞3.00μm，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，单面层间电阻值＜100Ω.cm2；对比例Q2中极薄带成品磁感B800＜1.85T，损耗P1.5/400＞16.50W/kg，单面层间电阻值＜100Ω.cm2；对比例Q3中极薄带成品磁感B800＜1.85T，损耗P1.5/400＞16.50W/kg，单面层间电阻值＜100Ω.cm2。
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)

1.一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法，其步骤：
1)母材
母材成分Si＝2.80％～3.60％，Mn＝0.010％～1.00％，含P、Cu、Sn、Bi、Sb、Cr和As中的一种或几种，且满足(P+Cu+Sn+Bi+Sb+Cr+As)≤1.80％，其余为铁和不可避免的杂质；
母材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、在带材的表面涂覆半有机水性醇酸树脂绝缘涂料，并控制单面涂层厚度在0.05～3.00μm；
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；并满足涂层经常规烘干后不挥发成分含量在30～80％；
5)待用。
2.如权利要求1所述的一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法，其特征在于：所述半有机水性醇酸树脂绝缘涂料的组成及重量百分比含量为：醇酸树脂0.50～20％、氨基树脂0.50～20％、钛白粉0.50～30％、硫酸钡0.50～30％，其余为水。
3.如权利要求1所述的一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法，其特征在于：固化温度控制在158～741℃，并在此保温下保温37～172S。
4.如权利要求1所述的一种绝缘性能优良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0.05～2.86μm。
CN202310731488.4A 2023-06-20 2023-06-20 一种绝缘性能优良的高磁感取向硅钢极薄带的制备方法 Pending CN116752043A (zh)

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