CN105038229A - 一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜及其制备方法 - Google Patents
一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜,该复合薄膜通过在聚酰亚胺薄膜制备过程中掺混介孔氧化铝、多壁碳纳米管等填料,并将多壁碳纳米管负载在介孔氧化铝中,提高其分散性和利用率,利用在有机溶剂中具有良好稳定性的聚乙烯醇膜对粉体进行包覆处理,经过硅烷偶联剂表面改性处理后的复合粉体与有机胶液界面相容性好,更易分散均匀,最后制备得到的复合薄膜材料较单纯的聚酰亚胺薄膜在介电性能上获得极大改善,且仍保持良好的力学性能和加工性能,应用前景良好。
Description
技术领域
本发明涉及高介电复合材料制备技术领域,尤其涉及一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜及其制备方法。
背景技术
随着电子技术的进步,对电容器的介电性能、储能容量等性能要求越来越高,研制高介电常数、低介电损耗的介质材料就显得尤为重要,传统的薄膜电容器介质材料主要有非极性的聚苯乙烯、聚乙烯、聚丙烯以及极性的聚酰亚胺、聚碳酸酯等材料,其中聚酰亚胺具有良好的机械性能和热稳定性、易加工性、与基材相容性好、易成膜等优点,在制备高性能的介电薄膜中表现突出。单纯的聚酰亚胺薄膜介电常数过低,不能满足生产需求,目前常见的用于提高薄膜介电常数的方法主要是使用聚合物中掺混高介电材料的方法,然而这些方法普遍的缺陷表现在膜加工性能变差、介电常数提高的同时介电损耗增大等方面。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜及其制备方法。
本发明是通过以下技术方案实现的:
一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜,该复合薄膜由以下重量份的原料制备得到:均苯四甲酸二酐10-12、4,4,-二氨基二苯基醚8-10、介孔氧化铝1-2、N-乙烯基吡咯烷酮3-5、N,N-二甲基乙酰胺20-25、无水乙醇3-5、硅烷偶联剂0.1-0.2、甲基丙烯酸羟乙酯0.4-0.5、多壁碳纳米管1.5-2、聚乙烯醇0.1-0.2、水4-5。
所述的一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜的制备方法,所述的制备方法为:
(1)表面改性介孔氧化铝负载多壁碳纳米管溶液的制备:先将多壁碳纳米管经酸处理后水洗至中性烘干,再将聚乙烯醇溶解于水配制成溶液,将前面酸处理后的干燥多壁碳纳米管、介孔氧化铝投入溶液中,超声分散20-30min后将混合浆料加热至60-80℃,恒温研磨处理30-40min,随后将所得浆料烘干,完全除去水分,所得粉体与硅烷偶联剂混合搅拌均匀,得表面改性介孔氧化铝负载多壁碳纳米管复合粉体,最后将所得复合粉体投入无水乙醇中,超声分散20-30min后所得物料备用;
(2)将4,4,-二氨基二苯基醚投入N,N-二甲基乙酰胺中,搅拌均匀后,分5步加入等量的均苯四甲酸二酐,添加完毕后反应10-12h,得聚酰胺酸胶液,随后将步骤(1)制备得到的复合粉体无水乙醇溶液加入胶液中,搅拌混合8-10h后加入其它剩余物料,继续搅拌使物料混合均匀,所得复合胶液备用;
(3)将步骤(2)制备的复合胶液涂布于玻璃板上放入鼓风烘箱中进行亚胺化处理,处理条件为:处理温度100-200℃,处理时间:1-2h,即得所述复合薄膜。
本发明的优点是:本发明通过在聚酰亚胺薄膜制备过程中掺混介孔氧化铝、多壁碳纳米管等填料,并将多壁碳纳米管负载在介孔氧化铝中,提高其分散性和利用率,利用在有机溶剂中具有良好稳定性的聚乙烯醇膜对粉体进行包覆处理,经过硅烷偶联剂表面改性处理后的复合粉体与有机胶液界面相容性好,更易分散均匀,最后制备得到的复合薄膜材料较单纯的聚酰亚胺薄膜在介电性能上获得极大改善,且仍保持良好的力学性能和加工性能,应用前景良好。
具体实施方式
实施例:
一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜,该复合薄膜由以下重量份的原料制备得到:均苯四甲酸二酐10、4,4,-二氨基二苯基醚8、介孔氧化铝1、N-乙烯基吡咯烷酮3、N,N-二甲基乙酰胺20、无水乙醇3、硅烷偶联剂0.1、甲基丙烯酸羟乙酯0.4、多壁碳纳米管1.5、聚乙烯醇0.1、水4。
所述的一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜的制备方法,所述的制备方法为:
(1)表面改性介孔氧化铝负载多壁碳纳米管溶液的制备:先将多壁碳纳米管经酸处理后水洗至中性烘干,再将聚乙烯醇溶解于水配制成溶液,将前面酸处理后的干燥多壁碳纳米管、介孔氧化铝投入溶液中,超声分散20min后将混合浆料加热至80℃,恒温研磨处理30min,随后将所得浆料烘干,完全除去水分,所得粉体与硅烷偶联剂混合搅拌均匀,得表面改性介孔氧化铝负载多壁碳纳米管复合粉体,最后将所得复合粉体投入无水乙醇中,超声分散20min后所得物料备用;
(2)将4,4,-二氨基二苯基醚投入N,N-二甲基乙酰胺中,搅拌均匀后,分5步加入等量的均苯四甲酸二酐,添加完毕后反应10h,得聚酰胺酸胶液,随后将步骤(1)制备得到的复合粉体无水乙醇溶液加入胶液中,搅拌混合8h后加入其它剩余物料,继续搅拌使物料混合均匀,所得复合胶液备用;
(3)将步骤(2)制备的复合胶液涂布于玻璃板上放入鼓风烘箱中进行亚胺化处理,处理条件为:处理温度100℃,处理时间:2h,即得所述复合薄膜。
本实施例所制得的复合薄膜的性能指标如下:
拉伸强度为:128MPa;断裂伸长率:12%;击穿场强:175KV/mm;室温条件100Hz频率下介电常数为:65;同等条件下介电损耗≤0.15%。
Claims (2)
1.一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜,其特征在于,该复合薄膜由以下重量份的原料制备得到:均苯四甲酸二酐10-12、4,4,-二氨基二苯基醚8-10、介孔氧化铝1-2、N-乙烯基吡咯烷酮3-5、N,N-二甲基乙酰胺20-25、无水乙醇3-5、硅烷偶联剂0.1-0.2、甲基丙烯酸羟乙酯0.4-0.5、多壁碳纳米管1.5-2、聚乙烯醇0.1-0.2、水4-5。
2.如权利要求1所述的一种电容器用掺混介孔氧化铝负载多壁碳纳米管的聚酰亚胺高介电复合薄膜的制备方法,其特征在于,所述的制备方法为:
(1)表面改性介孔氧化铝负载多壁碳纳米管溶液的制备:先将多壁碳纳米管经酸处理后水洗至中性烘干,再将聚乙烯醇溶解于水配制成溶液,将前面酸处理后的干燥多壁碳纳米管、介孔氧化铝投入溶液中,超声分散20-30min后将混合浆料加热至60-80℃,恒温研磨处理30-40min,随后将所得浆料烘干,完全除去水分,所得粉体与硅烷偶联剂混合搅拌均匀,得表面改性介孔氧化铝负载多壁碳纳米管复合粉体,最后将所得复合粉体投入无水乙醇中,超声分散20-30min后所得物料备用;
(2)将4,4,-二氨基二苯基醚投入N,N-二甲基乙酰胺中,搅拌均匀后,分5步加入等量的均苯四甲酸二酐,添加完毕后反应10-12h,得聚酰胺酸胶液,随后将步骤(1)制备得到的复合粉体无水乙醇溶液加入胶液中,搅拌混合8-10h后加入其它剩余物料,继续搅拌使物料混合均匀,所得复合胶液备用;
(3)将步骤(2)制备的复合胶液涂布于玻璃板上放入鼓风烘箱中进行亚胺化处理,处理条件为:处理温度100-200℃,处理时间:1-2h,即得所述复合薄膜。
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