CN105502343A - 一种适用于不同柔性基底上原位生长CNTs阵列的制备方法 - Google Patents
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Abstract
本发明涉及一种适用于不同柔性基底上原位生长CNTs阵列的制备方法,使用油墨打印的方式,实现了打印CNTs制备所需的催化剂油墨在不同耐高温柔性基底制备CNTs阵列的方法。催化剂以高活性纳米铁、钴、镍粉,以及其纳米合金粉,以高分子聚合物为粘合剂和分散剂,采用高剪切分散法制备催化剂油墨,将制备好的催化剂油墨加入到油墨打印机中,打印在耐高温柔性基底上,采用CVD方法实现其CNTs的低温短时的阵列式生长。
Description
技术领域
本发明属于在柔性基底上原位生长CNTs阵列的制备方法,具体涉及将CNTs生长所需的催化剂使用油墨打印的方式负载在柔性基底上,CVD实现CNTs在柔性基底上的阵列式生长,具体涉及一种用于催化剂油墨浆料的配制以及在不同耐高温柔性基底上CVD制备CNTs的方法。
背景技术
碳纳米管具有大的比表面积、良好的导热导电性、低密度以及优异的电学和力学性能,目前已成功用于超级电容器电极材料、场发射三极管、功能涂层、力学增强材料、电磁屏蔽与吸波材料等诸多领域。然而,如何实现碳纳米管以及它的复合材料在各个领域都发挥其优异的性能仍然存在很多问题,比如碳纳米管难均匀分散在各种液体中,以及加入表面活性剂有利于分散,但是将使得碳纳米管的缺陷增多,比如结晶性、长径比等。使得碳纳米管优异的性能得不到充分的发挥。在CNTs作为超级电容器电极材料时,通常需要将电极材料加粘结剂和导电剂形成浆料涂覆在集流体(铜箔等基底)上,粘结剂的添加增加了其电极材料的电阻,使其电化学性能得不到充分的发挥,并且传统的超级电容器都是将电极材料涂覆在集流体上组装形成一个连续的膜状结构,然而使用油墨打印催化剂在基底上实现其碳纳米管的阵列式生长,这种超级电容器的结构设计有利于电解质离子以及电子与电极材料表面的充分接触,有利于提高其电化学性能。
目前实现CNTs阵列式生长的方法主要是传统的光刻、电子束光刻,首先将在基底上进行光刻得到所需要的图形,然后沉积催化剂,进行碳纳米管的图案化生长。然而光刻技术由于其工艺过程复杂,时间并且需要苛刻的设备条件,限制其工艺在各个领域的可扩展性。在柔性基底上实现碳纳米管的阵列式结构的方式主要是通过油墨打印碳纳米管溶液,由于碳纳米管难分散的特性,且形成不均匀的碳纳米管分散液,易造成喷头的堵塞,使得油墨打印碳纳米管溶液在柔性基底上也面临许多难点。
在各种柔性基底上原位生长CNTs的方法主要采用CVD方法。CVD方法具有简单可控的优势,适用于大批量的生产,其过程主要包括催化剂的引入过程以及CNTs的气相生长过程。其中CVD生长的温度多集中在650℃-1000℃,反应时间在30min-120min左右,存在反应温度高、时间长的问题,难以在大多数柔性基底上实现其CNTs阵列式负载的普适性,也不利于降低其成本。
发明内容
要解决的技术问题
为了避免现有技术的不足之处,本发明提出一种适用于不同柔性基底上原位生长CNTs阵列的制备方法,适用于该工艺的催化剂油墨制备和在柔性基底上CNTs的生长工艺。
技术方案
一种适用于不同柔性基底上原位生长CNTs阵列的制备方法,其特征在于步骤如下:
步骤1:在CAD中编辑打印的阵列图形,采用催化剂油墨将阵列图形打印转移到柔性耐高温基底上;
步骤2:将具有阵列图形的柔性基底置于管式炉中,采用化学气相沉积CVD在基底上生长CNTs;工艺条件为:以丙酮为碳源,反应温度在500-800℃,保温时间为0-30min,以氢气和氩气/氮气混合气作为载气,其氢气的体积比为10-20%,反应时间为5-20min,当反应完成后,在惰性气体的保护下冷却至室温,实现在不同柔性基底上有效负载CNTs。
所述催化剂油墨的黏度为2~50mpa.s。
当步骤1中采用卷对卷连续打印在柔性衬底时,步骤2中采用卷对卷连续CNTs生长工艺。
一种用于权利要求1~3所述任一项适用于不同柔性基底上原位生长CNTs阵列的制备方法的催化剂油墨,其特征在于组份的质量分数为:1-10%的高活性纳米催化剂、1-10%的高分子聚合物,及余量为有机溶剂;所述有机溶剂为能够溶于高分子聚合物的任何有机溶剂。
所述高分子聚合物为聚乙烯吡咯烷酮或聚四氟乙烯。
所述高活性纳米催化剂为纳米镍粉、纳米铁粉、纳米钴粉及它们的纳米合金粉。
所述有机溶剂为酮类、醇类、以及混合溶剂。
所述有机溶剂为乙醇或丙酮。
一种制备权利要求4~8所述任一项催化剂油墨的制备方法,其特征在于步骤如下:
步骤1):将高分子聚合物溶于有机溶剂中得到高分子分散溶液;
步骤2):在高分子分散溶液中添加高活性的纳米催化剂,使用高剪切分散方法分散均匀,制备含催化剂的油墨;
所述三种组份的质量分数为:1-10%的高活性纳米催化剂、1-10%的高分子聚合物,及余量为有机溶剂。
有益效果
本发明提出的一种适用于不同柔性基底上原位生长CNTs阵列的制备方法,使用油墨打印的方式,实现了打印CNTs制备所需的催化剂油墨在不同耐高温柔性基底制备CNTs阵列的方法。催化剂以高活性纳米铁、钴、镍粉,以及其纳米合金粉,以高分子聚合物为粘合剂和分散剂,采用高剪切分散法制备催化剂油墨,将制备好的催化剂油墨加入到油墨打印机中,打印在耐高温柔性基底上,采用CVD方法实现其CNTs的低温短时的阵列式生长。
附图说明
图1是本发明的工艺流程示意图。
图2打印催化剂油墨在铜箔上的光学示意图。
图3是生长在铜箔基底上的的CNTs阵列低倍SEM示意图
图4是生长在铜箔基底上CNTs阵列的高倍SEM示意图
图5是生长在石墨基底上CNTs阵列的低倍SEM示意图
图6是生长在石墨基底上CNTs阵列的低倍SEM示意图
图7是生长在石墨基底上CNTs阵列的高倍SEM示意图
具体实施方式
现结合实施例、附图对本发明作进一步描述:
实施例1:
通过油墨打印在铜箔基底上上制备CNTs阵列,具体步骤如下:
(1)以无水乙醇为有机溶剂,以聚乙烯吡咯烷酮为溶质,按照100:3的质量分数比配制聚乙烯吡咯烷酮溶液。
(2)将步骤(1)中的溶液超声分散10-30min,得到完全溶解的聚乙烯吡咯烷酮液。
(3)以步骤(2)中的溶液为母料,按照聚乙烯吡咯烷酮溶液:纳米镍粉=3:1的质量分数比配制催化剂油墨。
(4)将步骤(3)中的溶液超声分散10-30min,得到均匀分散的催化剂油墨。
2催化剂在柔性基底上的阵列式负载与CVDCNTs的生长过程
(5)取20ml催化剂油墨放入在清洁的墨盒中,在CAD中绘制出阵列图形,将墨盒中的催化剂油墨转移到铜箔上,形成催化剂阵列。将基底放入70-100℃烘箱,烘干10min。
(6)将步骤(5)中干燥后的基底,采用CVD法在基底上生长CNTs,工艺条件为:以丙酮为碳源,反应温度500-600℃,保温时间10min,氢气流量0-50sccm,Ar气流量70-100sccm,反应时间5min。所得CNTs的光学和电镜照片如图2、3和4所示。
实施例2:
具体方法和步骤同实施例1,不同的是CVD生长时间的变化,生长时间为10-15min,在铜箔基底上可得到具有不同高度的CNTs阵列。
实施例3:
具体方法和步骤同实施例1,不同的是基底改为石墨纸基底,可得到具有不同CNTs形貌的阵列。所得CNTs的电镜照片如图5、6和7所示。
实施例4:
具体方法和步骤同实施例2,不同的是CVD生长时间的变化,生长时间为5-10min,在石墨基底上可得到具有不同高度的CNTs阵列。
Claims (9)
1.一种适用于不同柔性基底上原位生长CNTs阵列的制备方法,其特征在于步骤如下:
步骤1:在CAD中编辑打印的阵列图形,采用催化剂油墨将阵列图形打印转移到柔性耐高温基底上;
步骤2:将具有阵列图形的柔性基底置于管式炉中,采用化学气相沉积CVD在基底上生长CNTs;工艺条件为:以丙酮为碳源,反应温度在500-800℃,保温时间为0-30min,以氢气和氩气/氮气混合气作为载气,其氢气的体积比为10-20%,反应时间为5-20min,当反应完成后,在惰性气体的保护下冷却至室温,实现在不同柔性基底上有效负载CNTs。
2.根据权利要求1所述适用于不同柔性基底上原位生长CNTs阵列的制备方法,其特征在于:所述催化剂油墨的黏度为2~50mpa.s。
3.根据权利要求1所述适用于不同柔性基底上原位生长CNTs阵列的制备方法,其特征在于:当步骤1中采用卷对卷连续打印在柔性衬底时,步骤2中采用卷对卷连续CNTs生长工艺。
4.一种用于权利要求1~3所述任一项适用于不同柔性基底上原位生长CNTs阵列的制备方法的催化剂油墨,其特征在于组份的质量分数为:1-10%的高活性纳米催化剂、1-10%的高分子聚合物,及余量为有机溶剂;所述有机溶剂为能够溶于高分子聚合物的任何有机溶剂。
5.根据权利要求4所述的适催化剂油墨,其特征在于:所述高分子聚合物为聚乙烯吡咯烷酮或聚四氟乙烯。
6.根据权利要求4所述的适催化剂油墨,其特征在于:所述高活性纳米催化剂为纳米镍粉、纳米铁粉、纳米钴粉及它们的纳米合金粉。
7.根据权利要求4所述的适催化剂油墨,其特征在于:所述有机溶剂为酮类、醇类、以及混合溶剂。
8.根据权利要求4或7所述的催化剂油墨,其特征在于:所述有机溶剂为乙醇或丙酮。
9.一种制备权利要求4~8所述任一项催化剂油墨的制备方法,其特征在于步骤如下:
步骤1):将高分子聚合物溶于有机溶剂中得到高分子分散溶液;
步骤2):在高分子分散溶液中添加高活性的纳米催化剂,使用高剪切分散方法分散均匀,制备含催化剂的油墨;
所述三种组份的质量分数为:1-10%的高活性纳米催化剂、1-10%的高分子聚合物,及余量为有机溶剂。
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