CN113501985B - 一种低介电常数聚酰亚胺薄膜的制备方法 - Google Patents
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Abstract
本发明公开了一种低介电常数聚酰亚胺薄膜的制备方法,通过将芳香二胺与聚四氟乙烯分散液混合后,与脂肪族二酐进行聚合、亚胺化制备得到;所述聚四氟乙烯分散液包括聚四氟乙烯微粉、全氟烷基乙氧基硅烷、油性溶剂。本发明制备得到的聚酰亚胺薄膜具有较低的介电常数和介电损耗,能够适用于挠性印制电路板在高频下的传输要求。
Description
技术领域
本发明属于高分子材料领域,尤其涉及一种低介电常数聚酰亚胺薄膜的制备方法。
背景技术
随着电子信息产业的飞速发展,作为电子元器件之间相互连接的载体,印制电路板已成为整个电子信息产业的关键基础。伴随着电子产品的传输高频化和高速数字化,在印制电路板的介质层中传输信号时,不可避免的会发生信号传输速度减慢、信号传输时间延迟、传播衰减等现象,印制电路板中的绝缘介质材料的介电常数不仅影响信号的传输速度,还很大程度上影响信号的损耗。因此,有效的降低印制电路板中绝缘介质材料的介电常数是提高微电子器件传输速度和效率最有效以及最直接的手段。
在高分子材料中,聚酰亚胺凭借着优异的综合性能,被广泛用于挠性印制电路板。然而,传统的芳香聚酰亚胺的介电常数一般高于3.0,同时具有较高的介电损耗,无法满足电路板的信号传输高频化的要求。因此,需要对传统的芳香聚酰亚胺进行改性,以获得较低介电常数、低介电损耗的高性能聚酰亚胺。
发明内容
基于上述技术问题,本发明提供了一种低介电常数聚酰亚胺薄膜的制备方法,所得到的聚酰亚胺薄膜具有较低的介电常数,能够适用于挠性印制电路板在高频下的传输要求。
本发明技术方案具体如下:
本发明提供了一种低介电常数聚酰亚胺薄膜的制备方法,通过将芳香二胺与聚四氟乙烯分散液混合后,与脂肪族二酐进行聚合、亚胺化制备得到;所述聚四氟乙烯分散液包括聚四氟乙烯微粉、全氟烷基乙氧基硅烷、油性溶剂。
本发明所述芳香二胺溶于非质子极性溶剂后与聚四氟乙烯分散液进行混合;对于本发明所述非质子极性溶剂无特别限定,可以选自二甲基甲酰胺、N-甲基吡咯烷酮、二甲基亚砜等。
对于所述聚四氟乙烯分散液的制备方法不作具体限定,本领域技术人员可以根据常规手段制备得到。比如,包括但不限于以下方法:将全氟烷基乙氧基硅烷加入油性溶剂中,搅拌混合后加入聚四氟乙烯微粉,进一步搅拌,过滤,即得。
优选地,所述聚四氟乙烯分散液中,聚四氟乙烯微粉占聚四氟乙烯分散液重量的40-60%。
优选地,所述聚四氟乙烯分散液中,聚四氟乙烯微粉与全氟烷基乙氧基硅烷的重量比为60-80:5-15。
优选地,所述聚四氟乙烯微粉的平均粒径为0.05-10μm;优选为0.05-0.5μm。
优选地,所述全氟烷基乙氧基硅烷为十三氟辛基三乙氧基硅烷。
优选地,所述油性溶剂为酮类溶剂。
优选地,所述聚四氟乙烯微粉的重量与所述芳香二胺和脂肪族二酐的总重量的比为0.5-2:1。
优选地,所述脂肪族二酐选自1,2,3,4-环戊四羧酸二酐或双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐。
对于本发明所用的芳香二胺无特别限定,可以是一种,也可以是不同二胺的组合。所述芳香二胺的具体例子包括但不限于:对苯二胺、2,4,6-三甲基-1,3-苯二胺、4,4’-二氨基二苯醚、1,4-双(4-氨基苯氧基)苯等。
对于本发明所述亚胺化制备聚酰亚胺薄膜的方法不作具体限定,可以采用本领域常规的亚胺化方法,如热亚化法或化学亚胺化法。
有益效果:
本发明提供了一种低介电常数聚酰亚胺薄膜的制备方法,以脂肪族二酐与芳香二胺为聚合单体,并通过特定方式在聚酰亚胺中引入聚四氟乙烯微粉,由此得到的聚酰亚胺薄膜具有较低的介电常数和介电损耗。
具体地,本发明所述聚四氟乙烯微粉是以聚四氟乙烯分散液的形式加入到芳香二胺中。通过聚酰四氟乙烯分散液组成、组分配比、加入量等多方面的调控,使得聚四氟乙烯微粉能够更好的分散于聚酰亚胺基体中,有效避免了聚四氟乙烯微粉的团聚,有利于其性能的发挥。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明,但是应该明确提出这些实施例用于举例说明,但是不解释为限制本发明的范围。
实施例1
配制聚四氟乙烯分散液:将十三氟辛基三乙氧基硅烷加入丙酮中,搅拌混合,然后加入粒径为0.1μm的聚四氟乙烯微粉,进一步搅拌,过滤,即得;所述聚四氟乙烯分散液中,聚四氟乙烯微粉的占比为55%;聚四氟乙烯微粉与十三氟辛基三乙氧基硅烷的重量比为70:10。
低介电常数的聚酰亚胺薄膜的制备方法:
在氮气氛围下,将4,4’-二氨基二苯醚加入N-甲基吡咯烷酮中,搅拌至溶解,然后与上述制备得到的聚四氟乙烯分散液混合,搅拌30min至混合均匀。然后加入1,2,3,4-环戊四羧酸二酐,室温下搅拌反应12h,得混合聚酰胺酸溶液;
其中,4,4’-二氨基二苯醚与1,2,3,4-环戊四羧酸二酐的摩尔比为1:1;所述聚四氟乙烯微粉与4,4’-二氨基二苯醚和1,2,3,4-环戊四羧酸二酐重量之和的比为1:1;
将混合聚酰胺酸溶液在洁净的玻璃上流延成膜,在160℃热风去溶剂,降至室温;然后将玻璃置于可控升温速率的真空烘箱中程序升温:在110℃,干燥1h;升温至200℃,干燥1h;继续升温至320℃,干燥1h,自然冷却,待烘箱温度降至室温,在水中剥离,得到厚度约20μm的聚酰亚胺薄膜。
实施例2
配制聚四氟乙烯分散液:将十三氟辛基三乙氧基硅烷加入环己酮中,搅拌混合,然后加入粒径为0.5μm的聚四氟乙烯微粉,进一步搅拌,过滤,即得;所述聚四氟乙烯分散液中,聚四氟乙烯微粉的占比为40%;聚四氟乙烯微粉与十三氟辛基三乙氧基硅烷的重量比为60:5。
低介电常数的聚酰亚胺薄膜的制备方法:
在氮气氛围下,将1,4-双(4-氨基苯氧基)苯加入N-甲基吡咯烷酮中,搅拌至溶解,然后与上述制备得到的聚四氟乙烯分散液混合,搅拌20min至混合均匀。然后加入双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐,室温下搅拌反应10h,得混合聚酰胺酸溶液;
其中,1,4-双(4-氨基苯氧基)苯与双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐的摩尔比为1:1.05;所述聚四氟乙烯微粉与1,4-双(4-氨基苯氧基)苯和均双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐重量之和的比为2:1;
将混合聚酰胺酸溶液在洁净的玻璃上流延成膜,在150℃热风去溶剂,降至室温;然后将玻璃置于可控升温速率的真空烘箱中程序升温:在100℃,干燥1.5h;升温至200℃,干燥0.5h;继续升温至300℃,干燥1h,自然冷却,待烘箱温度降至室温,在水中剥离,得到厚度约20μm的聚酰亚胺薄膜。
实施例3
配制聚四氟乙烯分散液:将十三氟辛基三乙氧基硅烷加入丙酮中,搅拌混合,然后加入粒径为5μm的聚四氟乙烯微粉,进一步搅拌,过滤,即得;所述聚四氟乙烯分散液中,聚四氟乙烯微粉的占比为60%;聚四氟乙烯微粉与十三氟辛基三乙氧基硅烷的重量比为80:15。
低介电常数的聚酰亚胺薄膜的制备方法:
在氮气氛围下,将2,4,6-三甲基-1,3-苯二胺加入N-甲基吡咯烷酮中,搅拌至溶解,然后与上述制备得到的聚四氟乙烯分散液混合,搅拌30min至混合均匀。然后加入1,2,3,4-环戊四羧酸二酐,室温下搅拌反应12h,得混合聚酰胺酸溶液;
其中,2,4,6-三甲基-1,3-苯二胺与1,2,3,4-环戊四羧酸二酐的摩尔比为0.995:1;所述聚四氟乙烯微粉与2,4,6-三甲基-1,3-苯二胺和1,2,3,4-环戊四羧酸二酐重量之和的比为1:1;
将混合聚酰胺酸溶液在洁净的玻璃上流延成膜,在160℃热风去溶剂,降至室温;然后将玻璃置于可控升温速率的真空烘箱中程序升温:在110℃,干燥1h;升温至200℃,干燥1h;继续升温至320℃,干燥1h,自然冷却,待烘箱温度降至室温,在水中剥离,得到厚度约20μm的聚酰亚胺薄膜。
对比例1
聚酰亚胺薄膜的制备方法:
在氮气氛围下,将粒径为0.1μm的聚四氟乙烯微粉和4,4’-二氨基二苯醚加入N-甲基吡咯烷酮中,搅拌30min。然后加入1,2,3,4-环戊四羧酸二酐,室温下搅拌反应12h,得混合聚酰胺酸溶液;
其中,4,4’-二氨基二苯醚与1,2,3,4-环戊四羧酸二酐的摩尔比为1:1;所述聚四氟乙烯微粉与4,4’-二氨基二苯醚和1,2,3,4-环戊四羧酸二酐重量之和的比为1:1;
将混合聚酰胺酸溶液在洁净的玻璃上流延成膜,在160℃热风去溶剂,降至室温;然后将玻璃置于可控升温速率的真空烘箱中程序升温:在110℃,干燥1h;升温至200℃,干燥1h;继续升温至320℃,干燥1h,自然冷却,待烘箱温度降至室温,在水中剥离,得到厚度约20μm的聚酰亚胺薄膜。
性能测试:
按照如下方法对实施例1-3及对比例1制备得到的聚酰亚胺薄膜进行介电常数(Dk)和损耗因子(Df)测量:将聚酰亚胺薄膜浸泡于去离子水中10min,然后置于烘箱中在100℃烘烤30min;再利用网路分析仪分别测量上述聚酰亚胺薄膜的介电常数和损耗因子。测试结果见下表。
介电常数(Dk) | 损耗因子(Df) | |
实施例1 | 2.19 | 0.007 |
实施例2 | 2.23 | 0.009 |
实施例3 | 2.46 | 0.011 |
对比例1 | 3.05 | 0.038 |
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种低介电常数聚酰亚胺薄膜的制备方法,其特征在于,通过将芳香二胺与聚四氟乙烯分散液混合后,与脂肪族二酐进行聚合、亚胺化制备得到;所述聚四氟乙烯分散液包括聚四氟乙烯微粉、全氟烷基乙氧基硅烷、油性溶剂;聚四氟乙烯分散液中,聚四氟乙烯微粉占聚四氟乙烯分散液重量的40-60%;聚四氟乙烯微粉与全氟烷基乙氧基硅烷的重量比为60-80:5-15;所述脂肪族二酐选自1,2,3,4-环戊四羧酸二酐或双环[2.2.2]辛-7-烯-2 ,3,5 ,6-四羧酸二酐。
2.根据权利要求1所述的低介电常数聚酰亚胺薄膜的制备方法,其特征在于,所述聚四氟乙烯微粉的平均粒径为0.05-10μm。
3.根据权利要求1所述的低介电常数聚酰亚胺薄膜的制备方法,其特征在于,所述聚四氟乙烯微粉的平均粒径为0.05-0.5μm。
4.根据权利要求1所述的低介电常数聚酰亚胺薄膜的制备方法,其特征在于,所述全氟烷基乙氧基硅烷为十三氟辛基三乙氧基硅烷。
5.根据权利要求1所述的低介电常数聚酰亚胺薄膜的制备方法,其特征在于,所述油性溶剂为酮类溶剂。
6.根据权利要求1所述的低介电常数聚酰亚胺薄膜的制备方法,其特征在于,所述聚四氟乙烯微粉的重量与所述芳香二胺和脂肪族二酐的总重量的比为0.5-2:1。
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