CN111286055B - 一种高耐水、高机械强度的聚酰亚胺复合薄膜及其制备方法 - Google Patents
一种高耐水、高机械强度的聚酰亚胺复合薄膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种高耐水、高机械强度的聚酰亚胺复合薄膜及其制备方法,该制备方法包括以下步骤:S1、将氟改性水滑石‑碳纳米管复合填料加入溶剂中,超声分散均匀,得到分散液;S2、将二酐、二胺加入溶剂中进行缩聚反应,得到聚酰胺酸溶液;S3、将所述分散液与聚酰胺酸溶液混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,即得。本发明制备的聚酰亚胺复合薄膜不仅能满足绝缘性能的要求,而且兼具高强度和高耐水性,尺寸稳定性高,具有良好的耐用性。
Description
技术领域
本发明涉及聚酰亚胺薄膜技术领域,尤其涉及一种高耐水、高机械强度的聚酰亚胺复合薄膜及其制备方法。
背景技术
聚酰亚胺薄膜不仅具有优良的机械性能以及电气性能,而且耐高温、耐化学溶剂、耐辐射性能也极为突出,在航空航天、电子电器、信息通讯等领域得到广泛的应用。但是,聚酰亚胺薄膜具有一定的吸水性,给薄膜的尺寸稳定性带来不利的影响,在微电子封装技术越来越向着高度集成化发展的前提下,传统的聚酰亚胺薄膜已经越来越难以满足市场的需求。目前,有研究通过在聚酰亚胺薄膜的制备过程中加入纳米级的聚四氟乙烯粉体提高薄膜的耐水性,但是聚四氟乙烯的强度低,而且与聚酰亚胺的相容性差,对聚酰亚胺薄膜的机械性能带来较大的负面效应。因此,开发兼具高强度和高耐水性的聚酰亚胺薄膜,成为急需解决的问题。
发明内容
基于背景技术存在的技术问题,本发明提出了一种高耐水、高机械强度的聚酰亚胺复合薄膜及其制备方法。
本发明提出的一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入溶剂中,超声分散均匀,得到分散液;
S2、在氮气保护下,将二酐、二胺加入溶剂中进行缩聚反应,得到聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜。
优选地,所述氟改性水滑石-碳纳米管复合填料的制备方法如下:
(1)、将适量硝酸镁、硝酸铝溶于水中,然后加入碳纳米管分散均匀,得到混合液;
(2)、在氮气保护下,将所述混合液与氢氧化钠水溶液在搅拌条件下同时滴加到全氟辛酸水溶液中,调节pH至9-9.5,得到反应浆液,然后在100-110℃水热反应20-30h,经过洗涤、干燥,即得。
优选地,所述混合液中,硝酸铝的浓度为0.1-0.3mol/L,碳纳米管的质量分数为0.5-1%,硝酸镁、硝酸铝的摩尔比为(2-4):1。
优选地,所述氢氧化钠水溶液的浓度为1.5-2mol/L;所述全氟辛酸水溶液的浓度为0.05-0.1mol/L。
优选地,所述混合液与全氟辛酸水溶液的体积比为(5-10):1。
优选地,所述二酐、二胺的摩尔比为(0.95-1.05):1;所述聚酰胺酸溶液的固含量为20-26%;所述二酐为均苯四甲酸二酐、2,2'-双(3,4-二羧苯基)六氟丙烷四酸二酐中的至少一种;所述二胺为4,4'-二氨基二苯醚、2,2'-双三氟甲基-4,4'-联苯二胺中的至少一种。
优选地,所述分散液的固含量为1.5-2%。
优选地,所述分散液与聚酰胺酸溶液的重量比为(0.3-0.4):1。
优选地,所述溶剂为N,N-二甲基乙酰胺或者N-甲基吡咯烷酮。
一种高耐水、高机械强度的聚酰亚胺复合薄膜,由所述的制备方法制成。
本发明的有益效果如下:
本发明以硝酸镁、硝酸铝作为水滑石合成的前驱体,全氟辛酸作为疏水改性剂,通过共沉淀法合成了氟改性水滑石-碳纳米管复合填料,其中水滑石负载在碳纳米管表面,具有片状二维结构,与一维管状结构的碳纳米管起到协效作用,既能在薄膜中形成相互连接的网络结构,从而提高薄膜的力学性能,又能提高薄膜的致密性,降低薄膜的吸水能力,从而改善薄膜的耐水性;全氟辛酸既能在共沉淀过程中通过插层效应插入水滑石的层间,又能吸附在碳纳米管上,从而使形成的复合填料具有优良的疏水性能,大幅度提高聚酰亚胺复合薄膜的耐水性。本发明制备的聚酰亚胺复合薄膜不仅能满足绝缘性能的要求,而且兼具高强度和高耐水性,尺寸稳定性高,具有良好的耐用性,广泛应用于微电子封装领域。
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。
实施例1
一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入溶剂中,超声分散均匀,得到分散液;
S2、在氮气保护下,将二酐、二胺加入溶剂中进行缩聚反应,得到聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜。
实施例2
一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入N-甲基吡咯烷酮中,超声分散均匀,得到固含量为1.5%的分散液;
S2、在氮气保护下,将均苯四甲酸二酐、4,4'-二氨基二苯醚加入N-甲基吡咯烷酮中进行缩聚反应,均苯四甲酸二酐、4,4'-二氨基二苯醚的摩尔比为0.95:1,得到固含量为20%的聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液按重量比为0.3:1混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜。
氟改性水滑石-碳纳米管复合填料的制备方法如下:
(1)、将硝酸镁、硝酸铝溶于水中,然后加入碳纳米管分散均匀,得到混合液,其中硝酸铝的浓度为0.1mol/L,碳纳米管的质量分数为0.5%,硝酸镁、硝酸铝的摩尔比为2:1;
(2)、在氮气保护下,将所述混合液与1.5mol/L的氢氧化钠水溶液在搅拌条件下同时滴加到0.05mol/L的全氟辛酸水溶液中,混合液与全氟辛酸水溶液的体积比为5:1,调节pH至9,得到反应浆液,然后在100℃水热反应20h,经过洗涤、干燥,即得。
实施例3
一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入N-甲基吡咯烷酮中,超声分散均匀,得到固含量为2%的分散液;
S2、在氮气保护下,将均苯四甲酸二酐、4,4'-二氨基二苯醚加入N-甲基吡咯烷酮中进行缩聚反应,均苯四甲酸二酐、4,4'-二氨基二苯醚的摩尔比为1.05:1,得到固含量为26%的聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液按重量比为0.4:1混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜。
氟改性水滑石-碳纳米管复合填料的制备方法如下:
(1)、将硝酸镁、硝酸铝溶于水中,然后加入碳纳米管分散均匀,得到混合液,其中硝酸铝的浓度为0.3mol/L,碳纳米管的质量分数为1%,硝酸镁、硝酸铝的摩尔比为4:1;
(2)、在氮气保护下,将所述混合液与2mol/L的氢氧化钠水溶液在搅拌条件下同时滴加到0.1mol/L的全氟辛酸水溶液中,混合液与全氟辛酸水溶液的体积比为10:1,调节pH至9.5,得到反应浆液,然后在110℃水热反应30h,经过洗涤、干燥,即得。
实施例4
一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入N-甲基吡咯烷酮中,超声分散均匀,得到固含量为1.8%的分散液;
S2、在氮气保护下,将均苯四甲酸二酐、4,4'-二氨基二苯醚加入N-甲基吡咯烷酮中进行缩聚反应,均苯四甲酸二酐、4,4'-二氨基二苯醚的摩尔比为1:1,得到固含量为25%的聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液按重量比为0.35:1混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜。
氟改性水滑石-碳纳米管复合填料的制备方法如下:
(1)、将硝酸镁、硝酸铝溶于水中,然后加入碳纳米管分散均匀,得到混合液,其中硝酸铝的浓度为0.2mol/L,碳纳米管的质量分数为0.8%,硝酸镁、硝酸铝的摩尔比为3:1;
(2)、在氮气保护下,将所述混合液与1.5mol/L的氢氧化钠水溶液在搅拌条件下同时滴加到0.075mol/L的全氟辛酸水溶液中,混合液与全氟辛酸水溶液的体积比为8:1,调节pH至9,得到反应浆液,然后在105℃水热反应24h,经过洗涤、干燥,即得。
试验例
对实施例2-4制得的聚酰亚胺复合薄膜进行性能测试,膜厚为25μm。拉伸强度按照GBT 13542-2006的标准测试,吸水率的测试方法如下:将薄膜在去离子水中浸泡96h,然后用滤纸吸干表面水分,用热失重分析仪测定吸水率。
测试结果如表1所示:
表1聚酰亚胺复合薄膜的性能测试结果
实施例2 | 实施例3 | 实施例4 | |
拉伸强度(MPa) | 166 | 171 | 170 |
吸水率(%) | 0.087 | 0.079 | 0.052 |
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 (9)
1.一种高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,包括以下步骤:
S1、将氟改性水滑石-碳纳米管复合填料加入溶剂中,超声分散均匀,得到分散液;
S2、在氮气保护下,将二酐、二胺加入溶剂中进行缩聚反应,得到聚酰胺酸溶液;
S3、将所述分散液与聚酰胺酸溶液混合均匀,然后涂覆在基底上,经过干燥、热亚胺化,得到高强度高导热聚酰亚胺复合薄膜;
其中,所述氟改性水滑石-碳纳米管复合填料的制备方法如下:
(1)、将适量硝酸镁、硝酸铝溶于水中,然后加入碳纳米管分散均匀,得到混合液;
(2)、在氮气保护下,将所述混合液与氢氧化钠水溶液在搅拌条件下同时滴加到全氟辛酸水溶液中,调节pH至9-9.5,得到反应浆液,然后在100-110℃水热反应20-30h,经过洗涤、干燥,即得。
2.根据权利要求1所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述混合液中,硝酸铝的浓度为0.1-0.3mol/L,碳纳米管的质量分数为0.5-1%,硝酸镁、硝酸铝的摩尔比为(2-4):1。
3.根据权利要求1或2所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述氢氧化钠水溶液的浓度为1.5-2mol/L;所述全氟辛酸水溶液的浓度为0.05-0.1mol/L。
4.根据权利要求1或2所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述混合液与全氟辛酸水溶液的体积比为(5-10):1。
5.根据权利要求1或2所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述二酐、二胺的摩尔比为(0.95-1.05):1;所述聚酰胺酸溶液的固含量为20-26%;所述二酐为均苯四甲酸二酐、2,2'-双(3,4-二羧苯基)六氟丙烷四酸二酐中的至少一种;所述二胺为4,4'-二氨基二苯醚、2,2'-双三氟甲基-4,4'-联苯二胺中的至少一种。
6.根据权利要求1所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述分散液的固含量为1.5-2%。
7.根据权利要求1所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述分散液与聚酰胺酸溶液的重量比为(0.3-0.4):1。
8.根据权利要求1所述的高耐水、高机械强度的聚酰亚胺复合薄膜的制备方法,其特征在于,所述溶剂为N,N-二甲基乙酰胺或者N-甲基吡咯烷酮。
9.一种高耐水、高机械强度的聚酰亚胺复合薄膜,其特征在于,由权利要求1-8任一项所述的制备方法制成。
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