CN115404324B - 一种电子器件用超薄不锈钢带及其制备方法 - Google Patents

一种电子器件用超薄不锈钢带及其制备方法 Download PDF

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CN115404324B
CN115404324B CN202210891406.8A CN202210891406A CN115404324B CN 115404324 B CN115404324 B CN 115404324B CN 202210891406 A CN202210891406 A CN 202210891406A CN 115404324 B CN115404324 B CN 115404324B
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stainless steel
rolling
temperature
parts
steel strip
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CN115404324A (zh
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贲海峰
单朝晖
王勇
瞿锋
赵毅
季倪伟
杨少旭
徐鑫玉
郁烨华
蒋益彰
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Jiangsu Yongjin Metal Technology Co ltd
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Abstract

本发明公开了一种电子器件用超薄不锈钢带及其制备方法。制备方法包括以下步骤:步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧,得到厚度为1±0.2mm的不锈钢带A;步骤2:将不锈钢带A进行一次退火、二次退火、酸洗,得到不锈钢带B;步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧,得到厚度为0.1~0.2mm的不锈钢带C;步骤4:将不锈钢C进行表面渗氮、电解抛光,得到不锈钢带D;步骤5:将不锈钢带D进行淬火、三次退火,得到不锈钢带E;步骤6:将不锈钢带E置于平整机中,平整,得到超薄不锈钢带。

Description

一种电子器件用超薄不锈钢带及其制备方法
技术领域
本发明涉及不锈钢带技术领域,具体为一种电子器件用超薄不锈钢带及其制备方法。
背景技术
近年来,超薄不锈钢带是将不锈钢带经过辊压机多次轧制,得到的厚度≤0.3mm的带材;现有工艺中,通常采用热轧或冷轧进行轧制;相较于热轧过程中在变形、稳定性、抗疲劳等方面效果较差,轧制过程不稳定,薄度受限等问题。冷轧不锈钢带具有成型速度快、涂层损伤低等优点,可以制备超薄不锈钢带。
现有冷轧超薄不锈钢带中,存在机械性能不稳定、表面粗糙度不均匀等问题,轧制过程中易产生氢脆,影响产品质量,降低良品率。另一方面,超薄不锈钢带表面硬度低,耐磨性、耐腐蚀性不佳。如果通过表面涂层化,会使得不锈钢带厚度增加,影响其应用范围。
综上,解决上述问题,制备一种电子器件用超薄不锈钢带及其制备方法。
发明内容
本发明的目的在于提供一种电子器件用超薄不锈钢带及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种电子器件用超薄不锈钢带的制备方法,包括以下步骤:
步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧,得到厚度为1±0.2mm的不锈钢带A;
步骤2:将不锈钢带A进行一次退火、二次退火、酸洗,得到不锈钢带B;
步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧,得到厚度为0.1~0.2mm的不锈钢带C;
步骤4:将不锈钢C进行表面渗氮、电解抛光,得到不锈钢带D;
步骤5:将不锈钢带D进行淬火、三次退火,得到不锈钢带E;
步骤6:将不锈钢带E置于平整机中,平整,得到超薄不锈钢带。
较为优化地,步骤1中,一次冷轧过程中,轧制剂A的喷射速度为300~360L/min,温度为40~50℃;轧制力为4000~4500KN,轧制张力为200~300KN,轧制速率为350~450m/min;步骤3中,二次冷轧过程中,轧制剂B的喷射速度为260~300L/min,温度为30~40℃;轧制力为3000~3500KN,轧制张力为100~200KN,轧制速率为250~300m/min。
较为优化地,所述轧制剂A的原料包括以下组分:按重量计,50~60份5号白油、20~30份棕榈油、5~8份1-辛基-3-甲基咪唑六氟磷酸盐、5~10份月桂醇聚氧乙烯醚、5~10份茶多酚棕榈酸酯、5~6份复合二硫化钼。
较为优化地,所述轧制剂B的原料包括以下组分:按重量分数计,1~1.5份复合二硫化钼、0.5~1份二氧化硅、3~5份离子液体、2~3份甘油、92~94份去离子水。
较为优化地,所述二硫化钼复合物的制备方法为:将二硫化钼分散在去离子水中,加入硝酸铈、硝酸镍搅拌均匀,加入氨水调节pH=10.8~11.2,搅拌均匀,得到混合液;将混合液在180~200℃水热反应12小时,洗涤干燥;在氮气氛围下,设置温度为200~300℃煅烧2~3小时,得到复合二硫化钼;所述离子液体的制备方法为:将乙醇胺与琥珀酸依次加入反应瓶中,混合均匀;氮气氛围下,设置微波功率为300W,反应温度为60~65℃,反应30~35分钟;洗涤干燥,得到离子液体。
较为优化地,步骤2中,一次退火过程中,气氛氛围为含氧量为5%的氧气-氮气混合气,温度为1050~1150℃,退火速度70~80m/min;二次退火过程中,气体氛围为氢气含量为5%的氢气-氮气混合气,温度为700~800℃,退火时间为4~6分钟。
较为优化地,酸洗过程中,在电解液为180~200g/L的亚硫酸钠、20~40g/L的抗坏血酸的混合溶液中,设置温度为70~80℃,电压为35V处理5~7分钟,转移至含有45~55g/L的硫酸、20~25g/L的氢氟酸、10~15g/L柠檬酸的混酸溶液中,设置温度为55~65℃处理5~8分钟。
较为优化地,步骤4中,表面渗氮过程中,气体氛围为氨气,温度为400~600℃,渗氮时间为6~8小时;电解抛光过程为:5~6wt%硫酸铵水溶液中,设置温度为75~80℃,电压为200~250V抛光1~2分钟。
较为优化地,步骤5中,淬火过程中,在磁场强度为5~10T下,以液氮为淬火介质冷却4~6分钟;三次退火过程中,气体氛围为氮气,流量为120~160L/min,温度为1000~1200℃,退火速度70~80m/min;步骤6中,平整过程中,轧制力为1500~2000KN,轧制速率为150~200m/min,延伸率为1~2%。
较为优化地,一种电子器件用超薄不锈钢带的制备方法制备得到的超薄不锈钢带。
本技术方案中,通过在一次冷轧过程中使用油系轧制剂,在二次冷轧过程使用水系轧制剂;协同增强冷轧后不锈钢带的机械稳定性;同时通过冷轧、酸洗、抛光等多个步骤的协同,均匀化表面粗糙度。通过渗氮处理强化表面强度,增加耐磨性和耐腐蚀性。从而有效提高超薄不锈钢带的质量和良品率。
(1)方案中使用轧制剂A(油系轧制剂)、轧制剂B(水系轧制)辅助两次轧制过程,形成良好的润滑膜,有效抑制不锈钢带轧制过程中的机械不稳定性和氢脆现象。其中轧制A相较于轧制剂B粘度更高,因此,油系轧制剂A一次冷轧后表面粗糙度较高,约为0.5~0.6μm;然后通过低粘度的水系轧制剂B二次冷轧后,表面粗糙度降至0.06~0.08μm;两者协同,在保持机械稳定性的前提下,使得不锈钢带具有良好粗糙度表面。同时,两种抑制剂的辅助协同,有效降低了轧制力,降低了能耗。
其中,两种轧制剂中均含有二硫化钼复合物作为减膜剂,相较于直接使用二硫化钼,表面负载有氧化铈氧化镍纳米粒子的复合物,不仅利于片层二硫化钼和粒子氧化铈、氧化镍的分散性,同时,两者间存在界面相互作用(滑动摩擦),更有助于减磨,抑制微裂纹产生。同时,冷轧退火后残留在表面的二硫化钼复合物可以有效存在渗氮过程(二硫化钼复合物具有催化作用,可以氨气分解,从而促进渗氮)。
其中,轧制剂B中,为了在不增加甘油含量的基础增加一定粘度,使得轧制剂B可以在钢界面形成良好的润滑膜,因此在其中另外加入了二氧化硅和离子液体(离子液体是由二乙醇胺和琥珀酸制备得到的,既可以有效分散无机粒子、增加粘度,又可以增加防腐性能),协同有效减磨的基础上,抑制水系轧制剂的腐蚀性,抑制氢脆,从而保证不锈钢带的力学性能。
(2)方案中,通过在一次轧制后一次退火后进行二次退火有效除去表面碳,抑制碳腐蚀,抑制氢脆。
利用退火后表面残留的无机颗粒(硫化钼复合物和二氧化硅)促进表面渗氮,形成耐磨性好、耐腐蚀性佳的表面。并在气体氛围下表面渗碳后,使用电解抛光,进一步表面钝化,降低表面粗糙度至0.02±0.01μm左右。同时,电解抛光中使用的是的硫酸铵溶液,可以作为氮源,促进渗氮层厚度,提高表面性能。另一方面,由于最终需要平整化,表面渗氮后,表面硬度增加,易使得平整化过程中产生微裂纹,从而降低超薄不锈钢带的耐腐蚀性和机械性能,降低成品率。因此方案中,使用磁性淬火,使得表面渗氮层具有一定韧性,从而抑制平整化过程中的缺陷。
综上,通过多步协同工艺过程,提高超薄不锈钢带冷轧过程中机械稳定性、粗糙度均匀化,以及增加表面耐腐蚀性和耐磨性。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
以下实施例中,所述不锈钢带为304不锈钢带;
实施例中,退火后冷却段气体氛围为氢气,氢气露点控制在-50℃,氧含量控制小于50ppm;急冷区分机转速为2000rpm,冷却温度为150℃;缓冷区为自然冷却,温度为50℃。
所述复合二硫化钼的制备方法为:称取质量比为1:1.5:3的硝酸铈、硝酸镍、二硫化钼;将二硫化钼分散在去离子水中,得到2mg/mL的分散液,加入硝酸铈、硝酸镍搅拌均匀,加入氨水调节pH=11.0,搅拌均匀,得到混合液;将混合液在180℃水热反应12小时,洗涤干燥;将其在氮气氛围下,设置温度为200~300℃煅烧2小时,得到复合二硫化钼。
所述离子液的制备方法为:按照摩尔比为1:1称取乙醇胺与琥珀酸,将两种物质依次加入反应瓶中,混合均匀;氮气氛围下,设置微波功率为300W,反应温度为60℃反应30分钟;丙酮洗涤、干燥,得到离子液体。
实施例1:
步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧:轧制剂A的喷射速度为350L/min,温度为45℃;轧制力为4200KN,轧制张力为250KN,轧制速率为400m/min;得到不锈钢带A;
步骤2:将不锈钢带A进行一次退火:气氛氛围为含氧量为5%的氧气-氮气混合气,温度为1100℃,退火速度75m/min;进行二次退火:气体氛围为氢气含量为5%的氢气-氮气混合气,温度为750℃,退火时间为5分钟;进行酸洗:在电解液为190g/L的亚硫酸钠、30g/L的抗坏血酸的混合溶液中,设置温度为75℃,电压为35V处理6分钟,转移至含有50g/L的硫酸、20g/L的氢氟酸、15g/L柠檬酸的混酸溶液中,设置温度为60℃处理6分钟;得到不锈钢带B;
步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧:轧制剂B的喷射速度为280L/min,温度为40℃;轧制力为3200KN,轧制张力为150KN,轧制速率为280m/min,得到不锈钢带C;
步骤4:将不锈钢C进行表面渗氮:气体氛围为氨气,温度为450℃,渗氮时间为8小时;进行电解抛光:将其作为阳极,5wt%硫酸铵水溶液中,设置温度为80℃,电压为200V抛光2分钟,得到不锈钢带D;
步骤5:将不锈钢带D进行淬火:在磁场强度为8T下,以液氮为淬火介质中冷却5分钟;进行三次退火:气体氛围为氮气,流量为150L/min,温度为1100℃,退火速度85m/min;得到不锈钢带E;
步骤6:将不锈钢带E置于平整机中,平整:轧制力为1800KN,轧制速率为180m/min,延伸率为1%;得到超薄不锈钢带。
本技术方案中,所述轧制剂A的原料包括以下组分:按重量计,55份5号白油、25份棕榈油、6份1-辛基-3-甲基咪唑六氟磷酸盐、10份月桂醇聚氧乙烯醚、8份茶多酚棕榈酸酯、5份复合二硫化钼。
所述轧制剂B的原料包括以下组分:按重量分数计,1.5份复合二硫化钼、0.5份二氧化硅、4.5份离子液体、2.5份甘油、93份去离子水。
实施例2:
步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧:轧制剂A的喷射速度为300L/min,温度为50℃;轧制力为4500KN,轧制张力为300KN,轧制速率为450m/min;得到不锈钢带A;
步骤2:将不锈钢带A进行一次退火:气氛氛围为含氧量为5%的氧气-氮气混合气,温度为1050℃,退火速度70m/min;进行二次退火:气体氛围为氢气含量为5%的氢气-氮气混合气,温度为700℃,退火时间为6分钟;进行酸洗:在电解液为180g/L的亚硫酸钠、40g/L的抗坏血酸的混合溶液中,设置温度为70℃,电压为35V处理7分钟,转移至含有55g/L的硫酸、20g/L的氢氟酸、15g/L柠檬酸的混酸溶液中,设置温度为55℃处理8分钟;得到不锈钢带B;
步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧:轧制剂B的喷射速度为260L/min,温度为40℃;轧制力为3500KN,轧制张力为200KN,轧制速率为300m/min,得到不锈钢带C;
步骤4:将不锈钢C进行表面渗氮:气体氛围为氨气,温度为400℃,渗氮时间为8小时;进行电解抛光:将其作为阳极,5wt%硫酸铵水溶液中,设置温度为80℃,电压为200V抛光2分钟,得到不锈钢带D;
步骤5:将不锈钢带D进行淬火:在磁场强度为5T下,以液氮为淬火介质中冷却4分钟;进行三次退火:气体氛围为氮气,流量为160L/min,温度为1000℃,退火速度700m/min;得到不锈钢带E;
步骤6:将不锈钢带E置于平整机中,平整:轧制力为2000KN,轧制速率为200m/min,延伸率为2%;得到超薄不锈钢带。
本技术方案中,所述轧制剂A的原料包括以下组分:按重量计,50份5号白油、30份棕榈油、8份1-辛基-3-甲基咪唑六氟磷酸盐、10份月桂醇聚氧乙烯醚、5份茶多酚棕榈酸酯、6份复合二硫化钼。
所述轧制剂B的原料包括以下组分:按重量分数计,1份复合二硫化钼、1份二氧化硅、3份离子液体、3份甘油、92份去离子水。
实施例3:
步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧:轧制剂A的喷射速度为360L/min,温度为40℃;轧制力为4000KN,轧制张力为200KN,轧制速率为350m/min;得到不锈钢带A;
步骤2:将不锈钢带A进行一次退火:气氛氛围为含氧量为5%的氧气-氮气混合气,温度为1150℃,退火速度80m/min;进行二次退火:气体氛围为氢气含量为5%的氢气-氮气混合气,温度为800℃,退火时间为4分钟;进行酸洗:在电解液为200g/L的亚硫酸钠、20g/L的抗坏血酸的混合溶液中,设置温度为80℃,电压为35V处理5分钟,转移至含有45g/L的硫酸、25g/L的氢氟酸、10g/L柠檬酸的混酸溶液中,设置温度为65℃处理5分钟;得到不锈钢带B;
步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧:轧制剂B的喷射速度为300L/min,温度为30℃;轧制力为3000KN,轧制张力为100KN,轧制速率为250m/min,得到不锈钢带C;
步骤4:将不锈钢C进行表面渗氮:气体氛围为氨气,温度为600℃,渗氮时间为6小时;进行电解抛光:将其作为阳极,6wt%硫酸铵水溶液中,设置温度为75℃,电压为250V抛光1分钟,得到不锈钢带D;
步骤5:将不锈钢带D进行淬火:在磁场强度为10T下,以液氮为淬火介质中冷却6分钟;进行三次退火:气体氛围为氮气,流量为120L/min,温度为1200℃,退火速度80m/min;得到不锈钢带E;
步骤6:将不锈钢带E置于平整机中,平整:轧制力为1500KN,轧制速率为150m/min,延伸率为1%;得到超薄不锈钢带。
本技术方案中,所述轧制剂A的原料包括以下组分:按重量计,60份5号白油、20份棕榈油、5份1-辛基-3-甲基咪唑六氟磷酸盐、5份月桂醇聚氧乙烯醚、10份茶多酚棕榈酸酯、5份复合二硫化钼。
所述轧制剂B的原料包括以下组分:按重量分数计,1.5份复合二硫化钼、0.5份二氧化硅、5份离子液体、2份甘油、94份去离子水。
对比例1:两次冷轧过程均使用轧制剂A;其余与实施例1相同。
对比例2:两次冷轧过程均使用轧制剂B;其余与实施例1相同。
对比例3:轧制剂B中使用1-辛基-3-甲基咪唑六氟磷酸盐替代离子液体;其余与实施例1相同。
对比例4:使用二硫化钼替代复合二硫化钼;其余与实施例1相同。
对比例5:不进行二次退火;其余与实施例1相同。
对比例6:不进行电解抛光过程;其余与实施例1相同。
对比例7:不进行淬火过程;其余与实施例1相同。
实验:将实施例和对比例中制备得到的超薄不锈钢带进行相关性能检测。参照标准方法GB/T228.1进行力学性能测试;参照GB/T4239进行硬度测试,载荷为200g;参照ASTM-B117-2011盐雾实验,5wt%氯化钠溶液,温度为35℃,试验时间为720小时;计算得到腐蚀率。
实施例 屈服强度MPa 硬度HV 腐蚀率g/cm2.h
实施例1 371 168 0.196
实施例2 366 164 0.201
实施例3 362 163 0.204
对比例1 340 149 0.321
对比例2 344 152 0.367
对比例3 351 159 0.213
对比例4 358 154 0.301
对比例5 360 163 0.340
对比例6 354 160 0.207
对比例7 362 165 0.512
结论:由实施例1~3中的数据表明:所制备得到的超薄不锈钢带具有优异的力学性能,良好的表面硬度和优异的耐腐蚀性。对比例1~ 2的数据表明:单一使用一种轧制剂使得性能下降,两种轧制剂之间存在协同作用。对比例3~4中表明:离子液体形成了更好的耐腐蚀的界面膜层,有效提高了钢带机械性能的稳定性;复合二硫化钼相较于二硫化钼具有更好的减磨性和分散性,促使形成了更好的界面膜层,利于冷轧。对比例5表明:不进行二次退火,使得酸洗过程后存在碳腐蚀性,降低了超薄不锈钢带的性能。对比例6中,由于未进行电解抛光,使得渗氮层性能降低,从而使得耐腐蚀性和硬度降低。对比例7中,由于未进行淬火过程,使得平整过程中存在微裂纹,使得耐腐蚀性能下降。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (7)

1.一种电子器件用超薄不锈钢带的制备方法,其特征在于:包括以下步骤:
步骤1:将3±0.2mm的不锈钢带置于二十辊轧机中,在轧制剂A的辅助下进行一次冷轧,得到厚度为1±0.2mm的不锈钢带A;
步骤2:将不锈钢带A进行一次退火、二次退火、酸洗,得到不锈钢带B;
步骤3:将不锈钢带B置于二十辊轧机中,在轧制剂B的辅助下进行二次冷轧,得到厚度为0.1~0.2mm的不锈钢带C;
步骤4:将不锈钢C进行表面渗氮;设置电解抛光过程为:5~6wt%硫酸铵水溶液中,设置温度为75~80℃,电压为200~250V抛光1~2分钟,得到不锈钢带D;
步骤5:将不锈钢带D进行在磁场强度为5~10T下,以液氮为淬火介质冷却4~6分钟,三次退火,得到不锈钢带E;
步骤6:将不锈钢带E置于平整机中,平整,得到超薄不锈钢带;
所述轧制剂A的原料包括以下组分:按重量计,50~60份5号白油、20~30份棕榈油、5~8份1-辛基-3-甲基咪唑六氟磷酸盐、5~10份月桂醇聚氧乙烯醚、5~10份茶多酚棕榈酸酯、5~6份复合二硫化钼;
所述轧制剂B的原料包括以下组分:按重量分数计,1~1.5份复合二硫化钼、0.5~1份二氧化硅、3~5份离子液体、2~3份甘油、92~94份去离子水;
所述复合二硫化钼的制备方法为:将二硫化钼分散在去离子水中,加入硝酸铈、硝酸镍搅拌均匀,加入氨水调节pH=10.8~11.2,搅拌均匀,得到混合液;将混合液在180~200℃水热反应12小时,洗涤干燥;在氮气氛围下,设置温度为200~300℃煅烧2~3小时,得到复合二硫化钼;所述离子液的制备方法为:将乙醇胺与琥珀酸依次加入反应瓶中,混合均匀;氮气氛围下,设置微波功率为300W,反应温度为60~65℃,反应30~35分钟;洗涤干燥,得到离子液体。
2.根据权利要求1中所述的一种电子器件用超薄不锈钢带的制备方法,其特征在于:步骤1中,一次冷轧过程中,轧制剂A的喷射速度为300~360L/min,温度为40~50℃;轧制力为4000~4500KN,轧制张力为200~300KN,轧制速率为350~450m/min;步骤3中,二次冷轧过程中,轧制剂B的喷射速度为260~300L/min,温度为30~40℃;轧制力为3000~3500KN,轧制张力为100~200KN,轧制速率为250~300m/min。
3.根据权利要求1中所述的一种电子器件用超薄不锈钢带的制备方法,其特征在于:步骤2中,一次退火过程中,气氛氛围为含氧量为5%的氧气-氮气混合气,温度为1050~1150℃,退火速度70~80m/min;二次退火过程中,气体氛围为氢气含量为5%的氢气-氮气混合气,温度为700~800℃,退火时间为4~6分钟。
4.根据权利要求1中所述的一种电子器件用超薄不锈钢带的制备方法,其特征在于:步骤2中,酸洗过程中,在电解液为180~200g/L的亚硫酸钠、20~40g/L的抗坏血酸的混合溶液中,设置温度为70~80℃,电压为35V处理5~7分钟,转移至含有45~55g/L的硫酸、20~25g/L的氢氟酸、10~15g/L柠檬酸的混酸溶液中,设置温度为55~65℃处理5~8分钟。
5.根据权利要求1中所述的一种电子器件用超薄不锈钢带的制备方法,其特征在于:步骤4中,表面渗氮过程中,气体氛围为氨气,温度为400~600℃,渗氮时间为6~8小时。
6.根据权利要求1中所述的一种电子器件用超薄不锈钢带的制备方法,其特征在于:步骤5中,三次退火过程中,气体氛围为氮气,流量为120~160L/min,温度为1000~1200℃,退火速度70~80m/min;步骤6中,平整过程中,轧制力为1500~2000KN,轧制速率为150~200m/min,延伸率为1~2%。
7.根据权利要求1~6任一项所述的一种电子器件用超薄不锈钢带的制备方法制备得到的超薄不锈钢带。
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