CN113215374A - 一种无底层取向硅钢及其制备方法 - Google Patents

一种无底层取向硅钢及其制备方法 Download PDF

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CN113215374A
CN113215374A CN202110495129.4A CN202110495129A CN113215374A CN 113215374 A CN113215374 A CN 113215374A CN 202110495129 A CN202110495129 A CN 202110495129A CN 113215374 A CN113215374 A CN 113215374A
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刘宝志
张航
孙振东
刘瑞祥
张艳芳
李艳霞
贺海政
李源
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Baotou Weifeng Rare Earth Electromagnetic Material Co ltd
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Abstract

本发明公开了一种无底层取向硅钢的制备方法,包括以下步骤:S1、坯料预处理、S2、脱碳退火、S3、涂覆隔离剂、S4、高温退火、S5、拉伸热平整和S6、激光去除底层,所述激光去除底层的工艺参数为:激光400‑500W,重复频率100‑150kHz,振镜扫描速度6000‑7000mm/s。本发明利用激光刻痕的物理方法制备了无底层取向硅钢,代替了传统的用酸去除取向硅钢涂层或硅酸镁底层,制备的取向硅钢表面光亮,不含涂层或硅酸镁底层,同时通过退火补偿了激光制备过程中对钢带产生的塑性变形,制备的无底层取向硅钢,磁性能稳定。

Description

一种无底层取向硅钢及其制备方法
技术领域
本发明涉及软磁材料制备技术领域,尤其涉及一种无底层取向硅钢及其制备方法。
背景技术
传统取向硅钢工业生产中钢板经过H2-N2-H2O气氛中连续脱碳退火将基体中碳脱到0.0030%以下,并在钢板表面形成合适氧化层,然后表面涂布MgO隔离剂,在高温退火过程中MgO与钢板表面氧化层发生固态扩散反应:2MgO+SiO2→Mg2SiO4,形成Mg2SiO4玻璃膜底层。玻璃膜底层硬度高,导致取向硅钢的冲片性能差;底层与基体的粗糙界面对磁畴移动具有阻碍作用,不利于铁损降低。为了提高取向硅钢加工性能,并进一步降低铁芯损耗,开发了无底层取向硅钢。
无底层取向硅钢的炼钢、热轧、常化、冷轧等前序工艺与传统取向硅钢制造工艺相同,其他后续工艺包括两种方式。一种方式是通过强酸中长时间浸泡洗掉约0.01mm厚度,该工艺制造成本高,并在药剂管理和环境污染等方面存在较大问题。另一种方式为通过控制脱碳退火工艺,在钢板表面形成不含铁氧化物、再隔离剂涂布,仅高温退火后,不形成硅酸镁玻璃膜底层,制备得到无底层取向硅钢。
如,CN109112395A公开了一种无底层取向超薄带母材及其制备方法,母材原料组成为,C:0.035~0.075%,Si:2.8%~3.4%,Cu:0.20~0.45%,Sn:0.1~0.2%,Als:0.02%~0.03%,S:0.015~0.03%,Mn:0.04~0.08%,N:0.005~0.01%,Sb:0.03~0.09%,余量为Fe。制备方法包括:连铸、热轧、常化、酸洗、冷轧、脱碳退火、涂覆隔离层、高温退火和防潮处理步骤,该发明通过改进硅钢基板成分、隔离剂、热轧温度、脱碳和高温退火等工艺,获得表面无绝缘底层,该发明的制备方法可不经酸洗直接用于取向硅钢超薄带制备;用该母材制得的超薄带铁损和磁感性能优异,且制备成本低。
CN110983004A公开了一种无底层极薄带取向硅钢母带的生产工艺,步骤如下:对取向硅钢热轧原料带进行冷轧,脱碳退火、退火隔离剂涂覆、高温退火、热拉伸平整;其中退火隔离剂涂覆工艺包括:1)对取向硅钢表面进行清洗;2)回复退火处理,退火后冷却钢带;3)在钢带表面涂覆硅溶胶,采用钢带余热烘干;4)配置退火隔离剂涂液;5)将退火隔离剂溶液涂覆在钢带表面,烘干后卷取。该发明高温退火后可形成无硅酸镁绝缘底层的极薄带取向硅钢母带,后续可轻松将钢带表面的氧化镁粉去除,无需酸液进行清洗底层,生产成本低,安全环保。
上述现有技术制备过程中均不形成硅酸镁底层,但高温退火过程中,抑制剂不稳定,容易分解,导致二次再结晶不稳定,磁性能不稳定,成本昂贵,难以实现规模化生产。同时,当前无底层取向硅钢仍存在无底层取向硅钢的表面光洁化困难和无底层取向硅钢的成材率低等问题。因此,亟需开发一种无底层取向硅钢的制备方法。
发明内容
为了解决上述技术问题,本发明提供了一种无底层取向硅钢及其制备方法。
为了实现上述目的,本发明采用以下技术方案:
一种无底层取向硅钢的制备方法,包括以下步骤:S1、坯料预处理、S2、脱碳退火、S3、涂覆隔离剂、S4、高温退火、S5、拉伸热平整和S6、激光去除底层。
优选地,所述激光去除底层的工艺参数为:激光400-500W,重复频率100-150kHz,振镜扫描速度6000-7000mm/s。
优选地,所述制备方法中步骤S6激光去除底层后,还包括S7、去应力退火。
进一步优选地,所述去应力退火为:通保护气氛加热到600-800℃,保护气氛为体积比为1-3:1的氢气和氮气混合气,流量为3-10Nm3/h,退火保温时间1-10h。
优选地,所述制备方法中步骤S7去应力退火后,还包括步骤S8后处理。
进一步优选地,所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述再结晶退火为:在温度800-1000℃,保护气为氮气和氨分解气。
本发明还提供了上述制备方法制备的无底层取向硅钢。
本发明的有益效果为:
(1)本发明利用激光刻痕的物理办法制备了无底层取向硅钢薄带,代替了传统的用酸去除取向硅钢涂层或硅酸镁底层,制备的取向硅钢薄带表面光亮,不含涂层或硅酸镁底层。
(2)本发明通过退火补偿了激光制备过程中对钢带产生的塑性变形,同时,制备的无底层取向硅钢,磁性能稳定。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面对本发明的技术方案做进一步详述。
当实施例给出数值范围时,应理解,除非本发明另有说明,每个数值范围的两个端点以及两个端点之间任何一个数值均可选用。除非另外定义,本文中使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同意义。
如无特殊说明,本发明所采用的原料均为普通市售产品。
基础实施例
一种无底层取向硅钢的制备方法,包括以下步骤:
S1、坯料预处理;将厚度为2.0-2.8mm,宽为1000-1300mm的热轧坯料经酸洗去除表面氧化铁后轧制到0.5-0.7mm或成品厚度0.2-0.35mm;
S2、脱碳退火;将轧制后的坯料在温度800-900℃下,在氮气跟氨分解气保护条件下通入湿气,将钢中的碳含量降低到30ppm以下;
S3、涂覆隔离剂;所述隔离剂包括氧化镁和添加剂。
S4、高温退火:在温度为1150-1220℃和氨分解气的保护条件下,形成硅酸镁玻璃底层;
S5、拉伸热平整:将高温退火后的硅酸镁玻璃底层拉伸热平整完,得到厚度为0.2-0.35mm的取向硅钢;
S6、激光去除底层:工艺参数为:激光400-500W,重复频率100-150kHz,振镜扫描速度6000-7000mm/s;
S7、去应力退火:通保护气氛加热到600-800℃,保护气氛为体积比为1-3:1的氢气和氮气混合气,流量为3-10Nm3/h,退火保温时间1-10h;
S8、后处理:所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述二次冷轧为压制得到厚度为0.03-0.1mm,宽度为500-650mm的取向硅钢;
所述二次分切为将得到的取向硅钢切割成200-320mm宽的钢卷;
所述再结晶退火为:在温度800-1000℃,保护气为氮气和氨分解气。
实施例1
一种无底层取向硅钢的制备方法,包括以下步骤:
S1、坯料预处理;将厚度为2.4mm,宽为1200mm的热轧坯料经酸洗去除表面氧化铁后轧制到0.5-0.7mm;
S2、脱碳退火;将轧制后的坯料在温度为850℃和氮气与氨分解气保护条件下通入湿气,将钢中的碳含量降低到30ppm以下;
S3、涂覆隔离剂;所述隔离剂中质量百分比为95%的氧化镁和5%的硼酸盐;
S4、高温退火:在高温退火温度为1185℃,保护气为氨分解气的条件下,形成硅酸镁玻璃底层;
S5、拉伸热平整:将高温退火后的硅酸镁玻璃底层拉伸热平整完,得到厚度为0.3mm的取向硅钢;
S6、激光去除底层:工艺参数为:激光400W,重复频率100kHz,振镜扫描速度6000mm/s;
S7、去应力退火:通保护气加热到600℃,保护气为体积比为1:1的氢气和氮气混合气,流量为3Nm3/h,退火保温时间10h;
S8、后处理:所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述二次冷轧为压制得到厚度为0.08mm,宽度为600mm的取向硅钢薄带;
所述二次分切为将得到的取向硅钢薄带切割成300mm宽的钢卷;
所述再结晶退火为:温度800℃,保护气为氮气和氨分解气。
实施例2
一种无底层取向硅钢的制备方法,包括以下步骤:
S1、坯料预处理;将厚度为2.4mm,宽为1200mm的热轧坯料经酸洗去除表面氧化铁后轧制到0.5-0.7mm;
S2、脱碳退火;将轧制后的坯料在温度为850℃和氮气与氨分解气保护条件下通入湿气,将钢中的碳含量降低到30ppm以下;
S3、涂覆隔离剂;所述隔离剂中质量百分比为95%的氧化镁和5%的硼酸盐;
S4、高温退火:在高温退火温度为1185℃,保护气为氨分解气的条件下,形成硅酸镁玻璃底层;
S5、拉伸热平整:将高温退火后的硅酸镁玻璃底层拉伸热平整完,得到厚度为0.3mm的取向硅钢;
S6、激光去除底层:工艺参数为:激光500W,重复频率150kHz,振镜扫描速度7000mm/s;
S7、去应力退火:通保护气加热到800℃,保护气为体积比为3:1的氢气和氮气混合气,流量为10Nm3/h,退火保温时间1h;
S8、后处理:所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述二次冷轧为压制得到厚度为0.08mm,宽度为600mm的取向硅钢薄带;
所述二次分切为将得到的取向硅钢薄带切割成300mm宽的钢卷;
所述再结晶退火为:温度1000℃,保护气为氮气和氨分解气。
实施例3
一种无底层取向硅钢的制备方法,包括以下步骤:
S1、坯料预处理;将厚度为2.4mm,宽为1200mm的热轧坯料经酸洗去除表面氧化铁后轧制到0.5-0.7mm;
S2、脱碳退火;将轧制后的坯料在温度为850℃和氮气与氨分解气保护条件下通入湿气,将钢中的碳含量降低到30ppm以下;
S3、涂覆隔离剂;所述隔离剂中质量百分比为95%的氧化镁和5%的硼酸盐;
S4、高温退火:在高温退火温度为1185℃,保护气为氨分解气的条件下,形成硅酸镁玻璃底层;
S5、拉伸热平整:将高温退火后的硅酸镁玻璃底层拉伸热平整完,得到厚度为0.3mm的取向硅钢;
S6、激光去除底层:工艺参数为:激光470W,重复频率120Hz,振镜扫描速度6520s;
S7、去应力退火:通保护气加热到720℃,保护气为体积比为2:1的氢气和氮气混合气,流量为5Nm3/h,退火保温时间3h;
S8、后处理:所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述二次冷轧为压制得到厚度为0.08mm,宽度为600mm的取向硅钢薄带;
所述二次分切为将得到的取向硅钢薄带切割成300mm宽的钢卷;
所述再结晶退火为:温度880℃,保护气为氮气和氨分解气。
实施例4
一种无底层取向硅钢的制备方法,包括以下步骤:
S1、坯料预处理;将厚度为2.4mm,宽为1200mm的热轧坯料经酸洗去除表面氧化铁后轧制到0.5-0.7mm;
S2、脱碳退火;将轧制后的坯料在温度为850℃和氮气与氨分解气保护条件下通入湿气,将钢中的碳含量降低到30ppm以下;
S3、涂覆隔离剂;所述隔离剂中质量百分比为95%的氧化镁和5%的硼酸盐;
S4、高温退火:在高温退火温度为1185℃,保护气为氨分解气的条件下,形成硅酸镁玻璃底层;
S5、拉伸热平整:将高温退火后的硅酸镁玻璃底层拉伸热平整完,得到厚度为0.3mm的取向硅钢;
S6、激光去除底层:工艺参数为:激光440W,重复频率140kHz,振镜扫描速度6800mm/s;
S7、去应力退火:通保护气加热到650℃,保护气为体积比为1.5:1的氢气和氮气混合气,流量为8Nm3/h,退火保温时间5h;
S8、后处理:所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述二次冷轧为压制得到厚度为0.08mm,宽度为600mm的取向硅钢薄带;
所述二次分切为将得到的取向硅钢薄带切割成300mm宽的钢卷;
所述再结晶退火为:在温度920℃,保护气为氮气和氨分解气。
对比例1
本对比例与实施例3的区别在于,S6、激光去除底层:工艺参数为:激光550W,重复频率80kHz,振镜扫描速度5500mm/s;
S7、去应力退火:通保护气加热到820℃,保护气为体积比为1.5:1的氢气和氮气混合气,流量为12Nm3/h,退火保温时间5h。
对比例2
本对比例与实施例3的区别在于,S6、激光去除底层:工艺参数为:激光350W,重复频率180kHz,振镜扫描速度7500mm/s;
S7、去应力退火:通保护气加热到550℃,保护气为体积比为1.5:1的氢气和氮气混合气,流量为2Nm3/h,退火保温时间15h。
依据YB/T5224《中频用电工钢薄带》测量实施例1-4和对比例1-2制备的无底层取向硅钢薄带的磁性能,结果如表1所示。
表1无底层取向硅钢薄带的磁性能和表面状态
组别 损耗P1.5/400(W/Kg) 磁感B800(T)
实施例1 10.51 1.82
实施例2 10.32 1.84
实施例3 9.51 1.86
实施例4 10.05 1.85
对比例1 12.74 1.77
对比例2 12.59 1.76
综上所述,本发明利用激光刻痕的物理办法制备了无底层取向硅钢,代替了传统的用酸去除取向硅钢涂层或硅酸镁底层,制备的取向硅钢薄带表面光亮,不含涂层或硅酸镁底层。同时,通过退火补偿了激光制备过程中对钢带产生的塑性变形,制备的无底层取向硅钢,磁性能稳定。
以上是结合具体实施例对本发明进一步的描述,但这些实施例仅仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。

Claims (10)

1.一种无底层取向硅钢的制备方法,包括以下步骤:S1、坯料预处理、S2、脱碳退火、S3、涂覆隔离剂、S4、高温退火、S5、拉伸热平整,其特征在于,在步骤S5后还包括S6、激光去除底层;
所述激光去除底层的工艺参数;激光400-500W,重复频率100-150kHz,振镜扫描速度6000-7000mm/s。
2.根据权利要求1所述的制备方法,其特征在于,步骤S6激光去除底层后,还包括S7、去应力退火。
3.根据权利要求2所述的制备方法,其特征在于,所述去应力退火为:通保护气氛加热到600-800℃,保护气氛为体积比为1-3:1的氢气和氮气混合气,流量为3-10Nm3/h,退火保温时间1-10h。
4.根据权利要求1所述的制备方法,其特征在于,步骤S1中所述坯料为热轧坯料,所述热轧坯料的厚度为2.0-2.8mm,宽为1000-1300mm。
5.根据权利要求1所述的制备方法,其特征在于,步骤S1中所述坯料预处理为酸洗和冷轧。
6.根据权利要求5所述的制备方法,其特征在于,所述冷轧为将所述坯料轧制到厚度为0.5-0.7mm。
7.根据权利要求5所述的制备方法,其特征在于,所述冷轧为将所述坯料轧制到成品厚度0.2-0.35mm。
8.根据权利要求1所述的制备方法,其特征在于,所述步骤S7去应力退火后,还包括步骤S8后处理。
9.根据权利要求8所述的制备方法,其特征在于,所述后处理包括二次冷轧、二次分切、表面清洗、再结晶退火和剪切包装;
所述再结晶退火为:在温度800-1000℃,保护气为氮气和氨分解气。
10.根据权利要求1-9任一项所述的制备方法制备的无底层取向硅钢。
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