CN106633142A - 一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料及其制备方法 - Google Patents

一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料及其制备方法 Download PDF

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CN106633142A
CN106633142A CN201611245098.2A CN201611245098A CN106633142A CN 106633142 A CN106633142 A CN 106633142A CN 201611245098 A CN201611245098 A CN 201611245098A CN 106633142 A CN106633142 A CN 106633142A
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夏斌
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Abstract

本发明公开了一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料，由下列重量份的原料制成：N，N‑二甲基乙酰胺150‑180、十八胺50‑55、均苯四甲酸二酐50‑55、钛酸钡100‑110、石墨烯36‑38、纳米结晶纤维素23‑25、丙酮100‑105、硝酸亚铈50‑55、氧化银50‑55、硝酸适量、柠檬酸适量、去离子水适量、聚乙二醇1.3‑1.6、多壁碳纳米管0.6‑0.8、玻璃酸钠1.5‑2、纳米丝光沸石1‑1.3、纳米碳溶胶1.5‑1.8。本发明通过使用纳米丝光沸石、玻璃酸钠将多壁碳纳米管、纳米碳溶胶粘结在薄膜上，提高了薄膜的比电容。

Description

一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材 料及其制备方法
技术领域
本发明涉及电容器薄膜材料技术领域，尤其涉及一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料及其制备方法。
背景技术
随着科技的发展，拥有高介电常数的电介质材料在无源器件、高储能电容器、微波材料等领域中，特别是在薄膜电容器中有着广泛的应用。对于叠片式薄膜电容器而言，控制介电层的厚度、介电层膜的均匀性以及如何使介电层与导电层一体化制备是一技术难点。而高介电常数的无机/聚合物复合材料作为一种良好的高性能材料，不仅可以大面积制备，还可以避免单一无机介电材料的高温烧结，因此在介电领域具有广阔的发展前景。本文尝试采用新型成膜方法，以高介电常数的无机/聚合物复合材料作为介电层，以石墨纸做导电层，研究复合薄膜一体化制备工艺，从而展望制备一体化复合薄膜电容器。实验中，先利用溶液混合法制备钛酸钡/聚酰胺酸混合液，再以石墨纸做电极且为复合薄膜的载体，利用提拉法得到单片石墨纸-钛酸钡/聚酰亚胺一体化复合薄膜。通过红外（FT-IR）、热失重（TGA）、X射线衍射（XRD）、扫描电镜（SEM）等测试手段考察复合薄膜的热稳定性以及微观结构。通过电化学阻抗谱（EIS）仪、LCR测试仪等考察复合薄膜的介电性能。主要内容和结果如下：（1）利用两步法制备聚酰亚胺，先通过二酸酐与二胺的缩合反应制备了前驱体——聚酰胺酸，讨论了制备过程中的注意事项，对聚酰胺酸进行的热酰亚胺化反应，通过热失重、紫外等测试手段对各温度梯度薄膜进行表征，研究讨论了聚酰胺酸转变为聚酰亚胺的转变过程。（2）采用溶液混合法制备了钛酸钡/聚酰胺酸混合液，以石墨纸为载体和电极材料，利用提拉法制备了钛酸钡/聚酰胺酸涂覆膜，再通过程序升温热处理热酰亚胺化后得到石墨纸-钛酸钡/聚酰亚胺复合薄膜。利用红外（FT-IR）、热失重（TGA）、X射线衍射（XRD）、扫描电镜（SEM）等测试手段对复合薄膜进行了表征。（3）采用电化学阻抗谱（EIS）仪、LCR测试仪等技术测试复合薄膜的介电性能。研究钛酸钡/聚酰亚胺复合薄膜的介电性能与频率、介电性能与钛酸钡含量的关系，对比不同测试手段之间的差异。（4）研究了介电模型，并利用几种常用的基本模型和经验模型对钛酸钡/聚酰亚胺复合膜的实测介电常数进行分析，并利用线性拟合寻找适合本体系的模型。
《石墨纸钛酸钡聚酰亚胺一体化复合薄膜的制备与研究》一文得到的电容器薄膜材料的介电常数还需要提高，导电性能需要提高，还需要提高薄膜材料的比电容。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料及其制备方法。
本发明是通过以下技术方案实现的：
一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料，由下列重量份的原料制成：N，N-二甲基乙酰胺150-180、十八胺50-55、均苯四甲酸二酐50-55、钛酸钡100-110、石墨烯36-38、纳米结晶纤维素23-25、丙酮100-105、硝酸亚铈50-55、氧化银50-55、硝酸适量、柠檬酸适量、去离子水适量、聚乙二醇1.3-1.6、多壁碳纳米管0.6-0.8、玻璃酸钠1.5-2、纳米丝光沸石1-1.3、纳米碳溶胶1.5-1.8。
所述高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料的制备方法，包括以下步骤：
（1）将纳米结晶纤维素加入丙酮中，搅拌均匀，再加入石墨烯搅拌均匀，超声分散8-10分钟，涂覆在玻璃基板上，厚度为100-120μm，干燥，在500-550℃下处理55-60分钟，取下薄膜，得到石墨烯薄膜；
（2）按摩尔比铈：银=1:0.16-0.18称取硝酸亚铈、氧化银，在氧化银中加入硝酸至溶解，与硝酸亚铈一起加入100-105重量份的去离子水中，得到溶液，再加入柠檬酸和聚己二醇，柠檬酸与金属离子的摩尔比为1-1.2：1，搅拌溶解后，在85-87℃水浴中搅拌至变成凝胶，将石墨烯薄膜浸渍在凝胶中15-20分钟，取出，在110-115℃下干燥，然后在500-520℃下处理2-2.2小时，得到改性石墨烯膜；
（3）将多壁碳纳米管、玻璃酸钠、纳米丝光沸石、纳米碳溶胶混合均匀，得到混合物料；
（4）将十八胺加入N，N-二甲基乙酰胺中，搅拌至十八胺完全溶解，再分批加入均苯四甲酸二酐，每次加入0.5-0.6g，搅拌至完全溶解，再搅拌4-4.3小时，十八胺：均苯四甲酸二酐的摩尔比为1:1，得到固含量为15-20%的聚酰胺酸溶液，再加入其他剩余成分，得到混合液；
（5）将混合液与混合物料混合均匀，使用浸渍提拉机，将改性石墨烯膜以4cm/min的速度在混合液中浸渍、提拉、成膜、晾干，得到薄膜；
（6）将薄膜置于烤胶机上在60-62℃下加热1-1.2小时，在120-122℃下加热1-1.2小时，在180-183℃下加热1-1.2小时，在240-245℃下加热1-1.2小时，在270-275℃下加热1-1.2小时，冷却至室温，取出薄膜，即得。
本发明的优点是：本发明使用石墨烯和纳米结晶纤维素制成薄膜，高温处理除去纳米结晶纤维素，留下了微孔，再用硝酸亚铈、氧化银形成溶胶，对孔隙进行填充，在孔隙中形成了纳米级掺杂银离子的氧化铈颗粒，提高了石墨烯的密度和导电性，提高了电容器的电容率和蓄电性能；通过使用纳米丝光沸石、玻璃酸钠将多壁碳纳米管、纳米碳溶胶粘结在薄膜上，提高了薄膜的比电容。
具体实施方式
一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料，由下列重量份（公斤）的原料制成：N，N-二甲基乙酰胺150、十八胺50、均苯四甲酸二酐50、钛酸钡100、石墨烯36、纳米结晶纤维素23、丙酮100、硝酸亚铈50、氧化银50、硝酸适量、柠檬酸适量、去离子水适量、聚乙二醇1.3、多壁碳纳米管0.6、玻璃酸钠1.5、纳米丝光沸石1、纳米碳溶胶1.5。
所述高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料的制备方法，包括以下步骤：
（1）将纳米结晶纤维素加入丙酮中，搅拌均匀，再加入石墨烯搅拌均匀，超声分散8分钟，涂覆在玻璃基板上，厚度为100μm，干燥，在500℃下处理55分钟，取下薄膜，得到石墨烯薄膜；
（2）按摩尔比铈：银=1:0.16称取硝酸亚铈、氧化银，在氧化银中加入硝酸至溶解，与硝酸亚铈一起加入100重量份的去离子水中，得到溶液，再加入柠檬酸和聚己二醇，柠檬酸与金属离子的摩尔比为1：1，搅拌溶解后，在85℃水浴中搅拌至变成凝胶，将石墨烯薄膜浸渍在凝胶中15分钟，取出，在110℃下干燥，然后在500℃下处理2小时，得到改性石墨烯膜；
（3）将多壁碳纳米管、玻璃酸钠、纳米丝光沸石、纳米碳溶胶混合均匀，得到混合物料；
（4）将十八胺加入N，N-二甲基乙酰胺中，搅拌至十八胺完全溶解，再分批加入均苯四甲酸二酐，每次加入0.5g，搅拌至完全溶解，再搅拌4小时，十八胺：均苯四甲酸二酐的摩尔比为1:1，得到固含量为15%的聚酰胺酸溶液，再加入其他剩余成分，得到混合液；
（5）将混合液与混合物料混合均匀，使用浸渍提拉机，将改性石墨烯膜以4cm/min的速度在混合液中浸渍、提拉、成膜、晾干，得到薄膜；
（6）将薄膜置于烤胶机上在60℃下加热1小时，在120℃下加热1小时，在180℃下加热1小时，在240℃下加热1小时，在270℃下加热1小时，冷却至室温，取出薄膜，即得。
实验数据：
该实施例薄膜的介电损耗为1.6%，介电常数为41,10%失重温度为496℃、581℃。

Claims (2)

1.一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料，其特征在于：由下列重量份的原料制成：N，N-二甲基乙酰胺150-180、十八胺50-55、均苯四甲酸二酐50-55、钛酸钡100-110、石墨烯36-38、纳米结晶纤维素23-25、丙酮100-105、硝酸亚铈50-55、氧化银50-55、硝酸适量、柠檬酸适量、去离子水适量、聚乙二醇1.3-1.6、多壁碳纳米管0.6-0.8、玻璃酸钠1.5-2、纳米丝光沸石1-1.3、纳米碳溶胶1.5-1.8。
2.根据权利要求1所述高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料的制备方法，其特征在于包括以下步骤：
（1）将纳米结晶纤维素加入丙酮中，搅拌均匀，再加入石墨烯搅拌均匀，超声分散8-10分钟，涂覆在玻璃基板上，厚度为100-120μm，干燥，在500-550℃下处理55-60分钟，取下薄膜，得到石墨烯薄膜；
（2）按摩尔比铈：银=1:0.16-0.18称取硝酸亚铈、氧化银，在氧化银中加入硝酸至溶解，与硝酸亚铈一起加入100-105重量份的去离子水中，得到溶液，再加入柠檬酸和聚己二醇，柠檬酸与金属离子的摩尔比为1-1.2：1，搅拌溶解后，在85-87℃水浴中搅拌至变成凝胶，将石墨烯薄膜浸渍在凝胶中15-20分钟，取出，在110-115℃下干燥，然后在500-520℃下处理2-2.2小时，得到改性石墨烯膜；
（3）将多壁碳纳米管、玻璃酸钠、纳米丝光沸石、纳米碳溶胶混合均匀，得到混合物料；
（4）将十八胺加入N，N-二甲基乙酰胺中，搅拌至十八胺完全溶解，再分批加入均苯四甲酸二酐，每次加入0.5-0.6g，搅拌至完全溶解，再搅拌4-4.3小时，十八胺：均苯四甲酸二酐的摩尔比为1:1，得到固含量为15-20%的聚酰胺酸溶液，再加入其他剩余成分，得到混合液；
（5）将混合液与混合物料混合均匀，使用浸渍提拉机，将改性石墨烯膜以4cm/min的速度在混合液中浸渍、提拉、成膜、晾干，得到薄膜；
（6）将薄膜置于烤胶机上在60-62℃下加热1-1.2小时，在120-122℃下加热1-1.2小时，在180-183℃下加热1-1.2小时，在240-245℃下加热1-1.2小时，在270-275℃下加热1-1.2小时，冷却至室温，取出薄膜，即得。
CN201611245098.2A 2016-12-29 2016-12-29 一种高比电容薄膜电容器用石墨烯钛酸钡聚酰亚胺复合膜材料及其制备方法 Pending CN106633142A (zh)

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