CN109618429A - 一种耐温在200-250℃的金属箔发热片的制备方法 - Google Patents
一种耐温在200-250℃的金属箔发热片的制备方法 Download PDFInfo
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Abstract
本发明公开了一种耐温在200‑250℃的金属箔发热片的制备方法,其是通过金属箔的表面复合一层带粘性的聚酰亚胺薄膜而得。其中带粘性的聚酰亚胺薄膜是在热固性聚酰亚胺薄膜表面涂覆一层热熔性的聚酰胺酸液体而得,热熔性的聚酰胺酸液体的制备是先将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化;本发明通过在金属箔的表面复合一层带粘性的聚酰亚胺薄膜而使得的耐温达到200‑250℃。
Description
技术领域
本发明涉及一种金属箔发热片,特别是一种耐温在200-250℃的金属箔发热片的制备方法。
背景技术
金属箔发热片传统上使用聚酰亚胺薄膜涂有机硅压敏胶、环氧树脂热熔胶,FEP树脂涂覆等材料加以绝缘,但是有机硅压敏胶耐温只有180℃,环氧树脂耐温只有150℃, FEP耐温只有200℃,这里的耐温都是指长期耐温。很明显,上述这些涂覆在聚酰亚胺薄膜上的物质最大耐温都无法超过200℃,因此限制了这种蚀刻金属波发热片应用环境。
发明内容
本发明的目的是为了解决上述现有技术的不足而提供一种耐温在200-250℃的金属箔发热片的制备方法。
为了实现上述目的,本发明所设计的一种耐温在200-250℃的金属箔发热片的制备方法,包括以下步骤:
步骤一、制备热固性聚酰亚胺薄膜,先将二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米粉末,最后再分批加入二酐到反应釜中,搅拌,最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP,再脱泡流延成膜即可得到热固性聚酰亚胺薄膜;其中改性纳米粉末按重量份包括20-30份四氟化硅、10-15份氧化铝、30-40份氧化硅、1-5份氧化钛、0.1-0.3份氧化铪;
步骤二、制备带粘性的聚酰亚胺薄膜,在上述得到的热固性聚酰亚胺薄膜上涂上一层热熔性的聚酰胺酸液体,涂层厚度在3-7微米,具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化,其中烘箱的梯次温度为80-380℃,传送带的速度2-15米/min;
步骤三、制备金属箔发热片,先将金属箔与带粘性的聚酰亚胺薄膜热压复合,然后对金属箔进行蚀刻,已经蚀刻一面的金属箔再与带粘性的聚酰亚胺薄膜热压复合,最后连接出两个正负极即可得到金属箔发热片,其中热压复合时的热压温度为300-350℃,压力大于6kgf/平方厘米,保温时间为3-10分钟。
所述烘箱的梯次温度具体为
从80℃加热至100℃,保温30-60min,
加热升温至160℃,保温15-30min,
加热升温至200℃,保温15-30min,
加热升温至250℃,保温30-60min,
加热升温至300℃,保温15-30min,
加热升温至380℃,保温5-15min。
所述二酐为均苯四甲酸二酐(PMDA)、3,3',4,4'-联苯四羧酸二酐(BPDA)、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐(BPADA)、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种;
所述二胺为4,4-二氨基二苯醚(ODA)、对苯二胺(PPD)、4,4-二氨基二苯基甲烷(MDA)、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)(TFMB)、4,4-二氨基苯砜(4,4-DDS)、1,4-双(4-氨基-2-三氟甲基苯氧基)苯(6FAPB)中的一种或几种;
所述的极性溶剂是二甲基乙酰胺(DMAC)、N-甲基吡咯烷酮(NMP)、二甲基甲酰胺(DMF)中的一种或几种。
本发明得到的一种耐温在200-250℃的金属箔发热片的制备方法,其通过在金属箔的表面复合一层带粘性的聚酰亚胺薄膜而使得的耐温达到200-250℃。
具体实施方式
下面结合实施例对本发明进一步说明。
实施例1:
本实施例提供的一种耐温在200-250℃的金属箔发热片的制备方法,包括以下步骤:
步骤一、制备热固性聚酰亚胺薄膜,先将二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米粉末,最后再分批加入二酐到反应釜中,搅拌,最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP,再脱泡流延成膜即可得到热固性聚酰亚胺薄膜;其中改性纳米粉末按重量份包括20份四氟化硅、10份氧化铝、30份氧化硅、1份氧化钛、0.1份氧化铪;
步骤二、制备带粘性的聚酰亚胺薄膜,在上述得到的热固性聚酰亚胺薄膜上涂上一层热熔性的聚酰胺酸液体,涂层厚度在3-7微米,具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化,其中烘箱的梯次温度为80-380℃,传送带的速度2-15米/min;
步骤三、制备金属箔发热片,先将金属箔与带粘性的聚酰亚胺薄膜热压复合,然后对金属箔进行蚀刻,已经蚀刻一面的金属箔再与带粘性的聚酰亚胺薄膜热压复合,最后连接出两个正负极即可得到金属箔发热片,其中热压复合时的热压温度为300-350℃,压力大于6kgf/平方厘米,保温时间为3-10分钟。
所述烘箱的梯次温度具体为
从80℃加热至100℃,保温30-60min,
加热升温至160℃,保温15-30min,
加热升温至200℃,保温15-30min,
加热升温至250℃,保温30-60min,
加热升温至300℃,保温15-30min,
加热升温至380℃,保温5-15min。
所述二酐为均苯四甲酸二酐(PMDA)、3,3',4,4'-联苯四羧酸二酐(BPDA)、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐(BPADA)、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种;
所述二胺为4,4-二氨基二苯醚(ODA)、对苯二胺(PPD)、4,4-二氨基二苯基甲烷(MDA)、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)(TFMB)、4,4-二氨基苯砜(4,4-DDS)、1,4-双(4-氨基-2-三氟甲基苯氧基)苯(6FAPB)中的一种或几种;
所述的极性溶剂是二甲基乙酰胺(DMAC)、N-甲基吡咯烷酮(NMP)、二甲基甲酰胺(DMF)中的一种或几种。
实施例2:
本实施例提供的一种耐温在200-250℃的金属箔发热片的制备方法,包括以下步骤:
步骤一、制备热固性聚酰亚胺薄膜,先将二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米粉末,最后再分批加入二酐到反应釜中,搅拌,最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP,再脱泡流延成膜即可得到热固性聚酰亚胺薄膜;其中改性纳米粉末按重量份包括30份四氟化硅、15份氧化铝、40份氧化硅、5份氧化钛、0.3份氧化铪;
步骤二、制备带粘性的聚酰亚胺薄膜,在上述得到的热固性聚酰亚胺薄膜上涂上一层热熔性的聚酰胺酸液体,涂层厚度在3-7微米,具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化,其中烘箱的梯次温度为80-380℃,传送带的速度2-15米/min;
步骤三、制备金属箔发热片,先将金属箔与带粘性的聚酰亚胺薄膜热压复合,然后对金属箔进行蚀刻,已经蚀刻一面的金属箔再与带粘性的聚酰亚胺薄膜热压复合,最后连接出两个正负极即可得到金属箔发热片,其中热压复合时的热压温度为300-350℃,压力大于6kgf/平方厘米,保温时间为3-10分钟。
实施例3:
本实施例提供的一种耐温在200-250℃的金属箔发热片的制备方法,包括以下步骤:
步骤一、制备热固性聚酰亚胺薄膜,先将二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米粉末,最后再分批加入二酐到反应釜中,搅拌,最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP,再脱泡流延成膜即可得到热固性聚酰亚胺薄膜;其中改性纳米粉末按重量份包括25份四氟化硅、12份氧化铝、35份氧化硅、3份氧化钛、0.2份氧化铪;
步骤二、制备带粘性的聚酰亚胺薄膜,在上述得到的热固性聚酰亚胺薄膜上涂上一层热熔性的聚酰胺酸液体,涂层厚度在3-7微米,具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化,其中烘箱的梯次温度为80-380℃,传送带的速度2-15米/min;
步骤三、制备金属箔发热片,先将金属箔与带粘性的聚酰亚胺薄膜热压复合,然后对金属箔进行蚀刻,已经蚀刻一面的金属箔再与带粘性的聚酰亚胺薄膜热压复合,最后连接出两个正负极即可得到金属箔发热片,其中热压复合时的热压温度为300-350℃,压力大于6kgf/平方厘米,保温时间为3-10分钟。
Claims (3)
1.一种耐温在200-250℃的金属箔发热片的制备方法,其特征在于:包括以下步骤:
步骤一、制备热固性聚酰亚胺薄膜,先将二胺放入反应釜中,并用极性溶剂溶解,然后放入改性纳米粉末,最后再分批加入二酐到反应釜中,搅拌,最后加入极性溶剂调节控制最后反应生成物的粘度达到90000±5000 cP,再脱泡流延成膜即可得到热固性聚酰亚胺薄膜;其中改性纳米粉末按重量份包括20-30份四氟化硅、10-15份氧化铝、30-40份氧化硅、1-5份氧化钛、0.1-0.3份氧化铪;
步骤二、制备带粘性的聚酰亚胺薄膜,在上述得到的热固性聚酰亚胺薄膜上涂上一层热熔性的聚酰胺酸液体,涂层厚度在3-7微米,具体步骤是将通过二酐与二胺在极性溶剂下缩聚而得的聚酰胺酸溶液稀释涂到热固性聚酰亚胺薄膜上面,接着放置到设置有烘箱的传送带上,完成聚酰胺酸的彻底亚胺化,其中烘箱的梯次温度为80-380℃,传送带的速度2-15米/min;
步骤三、制备金属箔发热片,先将金属箔与带粘性的聚酰亚胺薄膜热压复合,然后对金属箔进行蚀刻,已经蚀刻一面的金属箔再与带粘性的聚酰亚胺薄膜热压复合,最后连接出两个正负极即可得到金属箔发热片,其中热压复合时的热压温度为300-350℃,压力大于6kgf/平方厘米,保温时间为3-10分钟。
2.根据权利要求1所述的一种耐温在200-250℃的金属箔发热片的制备方法,其特征在于:所述二酐为均苯四甲酸二酐(PMDA)、3,3',4,4'-联苯四羧酸二酐(BPDA)、3,3',4,4'-二苯酮四酸二酐(BTDA)、4,4'-联苯醚二酐(ODPA)、双酚A二酐(BPADA)、4,4'-(六氟异丙烯)二酞酸酐(6FPA)中的一种或几种;
所述二胺为4,4-二氨基二苯醚(ODA)、对苯二胺(PPD)、4,4-二氨基二苯基甲烷(MDA)、2,2'-双(三氟甲基)-4,4'-二氨基联苯(TFMB)(TFMB)、4,4-二氨基苯砜(4,4-DDS)、1,4-双(4-氨基-2-三氟甲基苯氧基)苯(6FAPB)中的一种或几种;
所述的极性溶剂是二甲基乙酰胺(DMAC)、N-甲基吡咯烷酮(NMP)、二甲基甲酰胺(DMF)中的一种或几种。
3.根据权利要求1所述的一种耐温在200-250℃的金属箔发热片的制备方法,其特征在于:
所述烘箱的梯次温度具体为
从80℃加热至100℃,保温30-60min,
加热升温至160℃,保温15-30min,
加热升温至200℃,保温15-30min,
加热升温至250℃,保温30-60min,
加热升温至300℃,保温15-30min,
加热升温至380℃,保温5-15min。
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