CN103854804A - 透明导电元件的制备方法 - Google Patents

透明导电元件的制备方法 Download PDF

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CN103854804A
CN103854804A CN201210493750.8A CN201210493750A CN103854804A CN 103854804 A CN103854804 A CN 103854804A CN 201210493750 A CN201210493750 A CN 201210493750A CN 103854804 A CN103854804 A CN 103854804A
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carbon nano
tube
tube film
thermoplastic polymer
preparation
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CN103854804B (zh
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姜开利
李群庆
魏洋
范守善
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Priority to TW101146224A priority patent/TWI483894B/zh
Priority to US13/902,289 priority patent/US9150000B2/en
Priority to JP2013214539A priority patent/JP5795041B2/ja
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Abstract

本发明涉及一种透明导电元件的制备方法，其包括以下步骤：提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管线并排且间隔设置，以及多个碳纳米管搭接在该相邻碳纳米管线之间；将该碳纳米管膜设置于一软化的聚合物基底表面；拉伸该聚合物基底和该碳纳米管膜；以及硬化该聚合物基底以保持该碳纳米管膜拉伸后的状态。

Description

透明导电元件的制备方法
技术领域
本发明涉及一种透明导电元件的制备方法，尤其涉及一种基于碳纳米管的透明导电元件的制备方法。
背景技术
碳纳米管(Carbon Nanotube, CNT)是一种新型碳材料，1991年由日本研究人员Iijima在实验室制备获得（请参见，Helical Microtubules of Graphitic Carbon, Nature, V354, P56~58 (1991)）。碳纳米管膜因具有良好的导电性和透光性而备受关注。
Baughma等人2005于文献“Strong, Transparent, Multifunctional, Carbon Nanotube Sheets”Mei Zhang, Shaoli Fang, Anvar A. Zakhidov, Ray H. Baughman, etc.. Science, Vol.309, P1215-1219(2005)中揭示了一种透明导电的碳纳米管膜的制备方法。所述碳纳米管膜可从一碳纳米管阵列中拉取制备。该碳纳米管阵列为一生长在一基底上的碳纳米管阵列。然而，所制备的碳纳米管膜的透光度不够好。
为克服上述问题，申请人于2009年5月22日申请的CN101585533B号专利中揭示了一种透明碳纳米管膜的制备方法，该方法包括以下步骤：从一碳纳米管阵列中拉取一碳纳米管膜，该碳纳米管膜包括多个碳纳米管基本平行于碳纳米管膜的表面；以及采用激光扫描该碳纳米管膜，使该碳纳米管膜由于部分碳纳米管被氧化而变薄，从而提高其透光度。该方法制备的透明碳纳米管膜可应用于透明电极、薄膜晶体管、触摸屏等领域。该透明碳纳米管膜使用时设置于一玻璃基底或树脂基底表面。
然而，该方法通过激光扫描处理碳纳米管膜来提高其透光性，效率较低，而且采用激光扫描成本较高。
发明内容
因此，确有必要提供一种既高效且成本低廉的制备碳纳米管透明导电元件的方法。
一种透明导电元件的制备方法，其包括以下步骤：提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管线并排且间隔设置，以及多个碳纳米管搭接在该相邻碳纳米管线之间；将该碳纳米管膜设置于一热塑性聚合物基底表面；加热软化该热塑性聚合物基底；沿垂直于碳纳米管线的方向拉伸该热塑性聚合物基底和该碳纳米管膜；以及硬化该热塑性聚合物基底以保持该碳纳米管膜拉伸后的状态。
一种透明导电元件的制备方法，其包括以下步骤：提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管线并排且间隔设置，以及多个碳纳米管搭接在该相邻碳纳米管线之间；将该碳纳米管膜设置于一软化的聚合物基底表面；拉伸该聚合物基底和该碳纳米管膜；以及硬化该聚合物基底以保持该碳纳米管膜拉伸后的状态。
本发明提供的制备碳纳米管透明导电元件的方法具有以下优点：其一，通过拉伸该聚合物基底和该碳纳米管膜可以增大碳纳米管膜的面积并提高碳纳米管膜的透光性；其二，通过拉伸该聚合物基底和该碳纳米管膜的方法制备透明导电元件，工艺简单，成本低廉。
附图说明
图1为本发明第一实施的透明导电元件的制备方法的工艺流程图。
图2为图1中的碳纳米管膜的局部放大结构示意图。
图3为本发明第一实施的碳纳米管膜的扫描电镜照片。
图4为本发明第二实施的透明导电元件的制备方法的工艺流程图。
主要元件符号说明
透明导电元件 10
碳纳米管膜 100
碳纳米管线 102
碳纳米管 104
聚合物基底 106
固定装置 110
如下具体实施例将结合上述附图进一步说明本发明。
具体实施方式
以下将结合附图详细说明本发明实施例提供的碳纳米管透明导电元件的制备方法。
请同时参阅图1，本发明第一实施例提供一种透明导电元件10的制备方法，具体包括以下步骤：
S10，提供一碳纳米管膜100；
S20，将该碳纳米管膜100设置于一热塑性聚合物基底106表面；
S30，加热软化该热塑性聚合物基底106；
S40，拉伸该热塑性聚合物基底106和该碳纳米管膜100；以及
S50，硬化该热塑性聚合物基底106。
所述步骤S10中，所述碳纳米管膜100的制备方法具体包括以下步骤：
首先，提供一碳纳米管阵列，优选地，该阵列为超顺排碳纳米管阵列。
所述碳纳米管阵列的制备方法可为化学气相沉积法。也可为石墨电极恒流电弧放电沉积法、激光蒸发沉积法等。本实施例中，该碳纳米管阵列为一采用化学气相沉积法制备在硅基底表面的顺排碳纳米管阵列。
其次，采用一拉伸工具从所述碳纳米管阵列中拉取获得一碳纳米管膜100。
所述碳纳米管膜100的制备方法具体包括以下步骤：（a）从上述碳纳米管阵列中选定一定宽度的多个碳纳米管片断，本实施例优选为采用具有一定宽度的胶带接触碳纳米管阵列以选定一定宽度的多个碳纳米管片断；（b）以一定速度沿基本垂直于碳纳米管阵列生长方向拉取该多个碳纳米管片断，以形成一连续的碳纳米管膜100。
在上述拉取过程中，该多个碳纳米管片段在拉力作用下沿拉伸方向逐渐脱离基底的同时，由于范德华力作用，该选定的多个碳纳米管片断分别与其它碳纳米管片断首尾相连地连续地被拉出，从而形成一碳纳米管膜100。本实施例中，该碳纳米管膜100的宽度与碳纳米管阵列所生长的基底的尺寸有关，该碳纳米管膜100的长度不限，可根据实际需求制得。该碳纳米管膜100的厚度与选取的碳纳米管片段有关，其厚度范围为0.5纳米~100微米。本发明实施例中，所述碳纳米管膜100的厚度为50纳米。
进一步参阅图2和图3，所述碳纳米管膜100包括多个碳纳米管线102并排且间隔设置，以及多个的碳纳米管104搭接在该相邻碳纳米管线102之间。所述碳纳米管线102的延伸方向与该碳纳米管膜100的拉取方向相同。所述碳纳米管线102由多个首尾相连的碳纳米管组成。所述碳纳米管线102中的碳纳米管基本沿碳纳米管线102的轴向排列延伸，且碳纳米管之间通过范德华力紧密连接。所述碳纳米管线102之间通过范德华力紧密连接。所述碳纳米管线102均匀分布在碳纳米管膜100中且沿第一方向排列。该第一方向为D1方向。相邻的碳纳米管线102之间具有多个碳纳米管104。该碳纳米管104可与至少两个相互并排设置的碳纳米管线102接触。可以理解，所述碳纳米管线102之间也可包括多个首尾相连的碳纳米管104。所述多个碳纳米管104的延伸方向与所述碳纳米管线102的延伸方向成一夹角α，该夹角α大于零度且小于90度。所述多个碳纳米管线102和多个碳纳米管104相互搭接，从而使该碳纳米管膜100中的所有碳纳米管形成一导电网络。进一步，所述碳纳米管膜100为一自支撑结构。所谓自支撑结构即所述碳纳米管膜100只需部分设置在一支撑体上即可维持其膜状结构，且碳纳米管膜100本身的结构不会发生变化。例如，将所述碳纳米管膜100设置在一框架或两个间隔设置的支撑结构上，位于中间未与框架或支撑结构接触的碳纳米管膜100可悬空设置。
所述碳纳米管膜100的长度、宽度及厚度不限，可根据实际需求制备。所述碳纳米管膜100的厚度优选为大于等于0.5纳米且小于等于1毫米。所述碳纳米管膜100中的碳纳米管的直径大于等于0.5纳米且小于等于50纳米。所述碳纳米管的长度为大于等于50微米且小于等于5毫米。
所述碳纳米管膜100在垂直于碳纳米管线102的方向上受力后发生形变。该垂直于碳纳米管线102的方向为D2方向。该D2方向垂直于D1方向。当所述碳纳米管膜100在D2方向上被拉伸时，碳纳米管膜100发生形变，碳纳米管线102之间的距离发生变化。具体地，所述碳纳米管线102之间的距离随碳纳米管膜100形变率的增加而增大。同时，所述碳纳米管104的延伸方向与所述碳纳米管线102的延伸方向的夹角α变大。可以理解，该夹角α最大为90度。所述碳纳米管膜100在D2方向的形变率小于等于300%。当所述碳纳米管膜100在D2方向的形变太大时，该碳纳米管膜100的整体性会受到破坏，即，该碳纳米管膜100中的碳纳米管无法形成一完整导电网络，而形成多个分散的导电通路。所述相邻的碳纳米管线102之间的距离大于0微米且小于等于50微米。该相邻的碳纳米管线102之间的距离随碳纳米管膜100的形变率的增加而增大。
所述碳纳米管膜100在D2方向上的形变率与碳纳米管膜100的厚度及密度有关。所述碳纳米管膜100的厚度及密度愈大，其在D2方向上的形变率愈大。进一步地，所述碳纳米管膜100的形变率与碳纳米管线102之间的碳纳米管104的含量有关。在一定含量范围内，所述碳纳米管线102之间的碳纳米管104的含量越多，所述碳纳米管膜100在D2方向上的形变率越大。所述碳纳米管膜100在D2方向上的形变率小于等于300%。本发明实施例中，所述碳纳米管膜100的厚度为50纳米，其在D2方向上的形变率可达到150%。
所述碳纳米管膜100的透光度（光透过比率）与碳纳米管膜100的厚度及密度有关。所述碳纳米管膜100的厚度及密度越大，所述碳纳米管膜100的透光度越小。进一步地，所述碳纳米管膜100的透光度与碳纳米管线102之间的距离及碳纳米管104的含量有关。所述碳纳米管线102之间的距离越大，碳纳米管104的含量越少，则所述碳纳米管膜100的透光度越大。所述碳纳米管膜100的透光度大于等于60%且小于等于95%。本发明实施例中，当碳纳米管膜100的厚度为50纳米时，拉伸前该碳纳米管膜100的透光度为大于等于67%且小于等于82%。当其形变率为120%时，所述碳纳米管膜100的透光度为大于等于84%且小于等于92%。以波长为550纳米的绿光为例，拉伸前所述碳纳米管膜100的透光度为78%，当形变率为120%时，该碳纳米管膜100的透光度可达89%。
所述步骤S20中，所述碳纳米管膜100可以直接设置并贴合在所述热塑性聚合物基底106的一表面。
可以理解，进一步本实施例还可以将多个碳纳米管膜100层叠设置于所述热塑性聚合物基底106同一表面，且该多个碳纳米管膜100中的碳纳米管线102沿同一方向延伸。进一步，本实施例还可以将多个碳纳米管膜100分别设置于所述热塑性聚合物基底106相对的两个表面，且该多个碳纳米管膜100中的碳纳米管线沿同一方向延伸。进一步，本实施例还可以将所述碳纳米管膜100设置于两个层叠设置的热塑性聚合物基底106之间。
所述热塑性聚合物基底106为一热塑性聚合物薄膜，其形状和大小不限。所述热塑性聚合物薄膜的厚度为1微米~2毫米，优选地，所述厚度为100微米~1毫米。所述热塑性聚合物基底106的材料为聚乙烯(PE)、聚氯乙烯(PVC)、聚四氟乙烯(PTFE)、聚丙烯(PP)、聚苯乙烯(PS)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚对苯二甲酸丁二酯(PBT)、聚酰胺(PA)、聚醚酮(PEK)、聚砜(PS)、聚醚砜(PES)、纤维素酯、热塑性聚酰亚胺(PI)、聚对苯二甲酸乙二酯(PET) 、苯并环丁烯(BCB)、聚醚酰亚胺(PEI)、聚苯醚(PPO)、聚苯硫醚(PPS)以及聚乙酸乙烯酯(PVAC)中的一种或者几种。本实施例中，所述热塑性聚合物基底106为一厚度100微米的矩形PET薄膜。
所述步骤S30中，所述加热软化该热塑性聚合物基底106的装置为金属双辊、平板热压成型机、热压机、平板硫化机或烘箱。所述步骤S30的目的为使该热塑性聚合物基底106软化为高弹态。
本实施例中，该步骤采用金属双辊实现。该金属双辊包括两个可以沿相反方向旋转的金属碾压辊以及一对金属碾压辊进行加热的装置。将上述设置有碳纳米管膜100的热塑性聚合物基底106慢慢通过加热的金属双辊，速度控制在1毫米/分~10米/分。该金属双辊的温度要高于所选的热塑性聚合物基底106的软化温度，目的是使得热塑性聚合物基底106能够软化，与碳纳米管膜100紧密接触，并将碳纳米管膜100与热塑性聚合物基底106之间的空气排除。其中，金属双辊的温度与所选用的热塑性聚合物基底106的材料有关，根据不同的热塑性聚合物基底106的材料，金属双辊的温度不同。进一步，由于金属双辊给所述碳纳米管膜100和热塑性聚合物基底106施加一压力，从而使该碳纳米管膜100至少部分嵌入该软化的热塑性聚合物基底106之中。本实施例中，所述热塑性聚合物基底106为一PET薄膜，所述软化温度为150℃~200℃。
可以理解，所述步骤S30也可以在一真空环境下进行。该方法可以更有效的将碳纳米管膜100与热塑性聚合物基底106之间的空气排出。
所述步骤S40中，所述拉伸该软化的热塑性聚合物基底106和碳纳米管膜100的方向不限，只要该拉力在沿着D2方向上形成一分力即可。优选地，直接沿垂直于碳纳米管线102的方向拉伸该软化的热塑性聚合物基底106和碳纳米管膜100。
本实施例中，先通过两个固定装置110分别将该热塑性聚合物基底106平行于碳纳米管线102延伸方向的相对两边固定，然后沿着D2方向给该两个固定装置110分别施加相反的拉力，从而沿着D2方向拉伸该软化的热塑性聚合物基底106。可以理解，采用两个固定装置110拉伸的碳纳米管膜100和软化的热塑性聚合物基底106，可以确保碳纳米管膜100和软化的热塑性聚合物基底106受力均匀。
所述拉力的大小和拉伸速度不限，可根据所要拉伸的碳纳米管膜100和软化的热塑性聚合物基底106具体进行选择。如果拉伸速度太大，则软化的热塑性聚合物基底106和碳纳米管膜100容易发生破裂，导致碳纳米管膜100的整体性受到破坏。优选地，所述拉伸速度小于20厘米每秒。本实施例中，所述拉伸速度为5厘米每秒。所述拉伸后的碳纳米管膜100中，多个碳纳米管线102和多个碳纳米管104相互搭接，从而使该碳纳米管膜100中的所有碳纳米管形成一导电网络。
由于所述碳纳米管膜100固定在所述软化的热塑性聚合物基底106上，故在拉力的作用下，随着所述软化的热塑性聚合物基底106被拉伸，该碳纳米管膜100也随之被拉伸。当所述碳纳米管膜100在D2方向上被拉伸时，碳纳米管线102之间的距离变大，同时，所述碳纳米管104的延伸方向与所述碳纳米管线102的延伸方向的夹角α也变大。其中，拉伸前所述并排设置的碳纳米管线102之间的距离大于0微米且小于10微米，拉伸后并排设置的碳纳米管线102之间的距离最大可达50微米。所述碳纳米管膜100被拉伸后仍维持膜状结构。所述碳纳米管膜100的形变率小于等于300%，且可基本维持碳纳米管膜100的形态。即所述碳纳米管膜100可在原有尺寸的基础上增加300%。本实施例中，所述碳纳米管膜100为单层碳纳米管膜，拉伸方向为沿垂直于碳纳米管线102的方向，即D2方向。所述碳纳米管膜100在D2方向上的形变率可达150%。
所述步骤S50中，所述硬化该软化的热塑性聚合物基底106的方法为降温硬化。本实施例中，通过自然冷却法将上述加热软化的热塑性聚合物基底106降温至室温从而硬化以保持该碳纳米管膜100拉伸后的状态。
请同时参阅图4，本发明第二实施例提供一种透明导电元件10的制备方法，具体包括以下步骤：
S10，提供一碳纳米管膜100；
S20，将该碳纳米管膜100设置于一软化的热固性聚合物基底106表面；
S30，拉伸该热固性聚合物基底106和该碳纳米管膜100；以及
S40，硬化该热固性聚合物基底106。
本发明第二实施例提供的透明导电元件10的制备方法与第一实施例提供一种透明导电元件10的制备方法基本相同，其区别在于，所述聚合物基底106为一热固性聚合物基底，且该碳纳米管膜100设置于两个热固性聚合物基底106之间。
所述热固性聚合物基底106的材料可以为酚醛树脂、环氧树脂、双马来酰亚胺树脂、聚苯并恶嗪树脂、氰酸酯树脂、聚酰亚胺树脂和不饱和聚酰树脂中的一种或者几种。
所述硬化该热固性聚合物基底106的方法为加热硬化。所述加热硬化的温度可以根据热固性聚合物基底106的材料选择。
本发明实施例提供的透明导电元件的制备方法具有以下优点：其一，通过拉伸该聚合物基底和该碳纳米管膜可以增大碳纳米管膜的面积并提高碳纳米管膜的透光性；其二，通过拉伸该聚合物基底和该碳纳米管膜的方法制备透明导电元件，工艺简单，成本低廉。
另外，本领域技术人员还可在本发明精神内做其他变化，当然，这些依据本发明精神所做的变化，都应包含在本发明所要求保护的范围之内。

Claims (15)

1.一种透明导电元件的制备方法，其包括以下步骤：
提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管线并排且间隔设置，以及多个碳纳米管搭接在该相邻碳纳米管线之间；
将该碳纳米管膜设置于一热塑性聚合物基底表面；
加热软化该热塑性聚合物基底；
沿垂直于碳纳米管线的方向拉伸该热塑性聚合物基底和该碳纳米管膜；以及
硬化该热塑性聚合物基底以保持该碳纳米管膜拉伸后的状态。
2.如权利要求1所述的透明导电元件的制备方法，所述碳纳米管膜为直接从一碳纳米管阵列中拉取获得，所述碳纳米管线的延伸方向与该碳纳米管膜的拉取方向相同，所述多个碳纳米管的延伸方向与所述碳纳米管线的延伸方向成一夹角，且该夹角大于零度小于90度。
3.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述碳纳米管膜直接设置并贴合在所述热塑性聚合物基底表面。
4.如权利要求1所述的透明导电元件的制备方法，其特征在于，进一步包括将多个碳纳米管膜层叠设置于所述热塑性聚合物基底同一表面，且该多个碳纳米管膜中的碳纳米管线沿同一方向延伸。
5.如权利要求1所述的透明导电元件的制备方法，其特征在于，进一步包括将多个碳纳米管膜分别设置于所述热塑性聚合物基底相对的两个表面，且该多个碳纳米管膜中的碳纳米管线沿同一方向延伸。
6.如权利要求1所述的透明导电元件的制备方法，其特征在于，进一步包括将所述碳纳米管膜设置于两个层叠设置的热塑性聚合物基底之间。
7.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述热塑性聚合物基底的材料为聚乙烯、聚氯乙烯、聚四氟乙烯、聚丙烯、聚苯乙烯、聚甲基丙烯酸甲酯、聚对苯二甲酸乙二酯、聚碳酸酯、聚对苯二甲酸丁二酯、聚酰胺、聚醚酮、聚砜、聚醚砜、热塑性聚酰亚胺、聚醚酰亚胺、聚苯醚、聚苯硫醚、聚乙酸乙烯酯或聚对苯撑苯并双惡唑中的一种或者几种的混合物。
8.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述热塑性聚合物基底为一热塑性聚合物薄膜，所述热塑性聚合物薄膜的厚度为1微米~2毫米。
9.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述加热软化该热塑性聚合物基底的装置为金属双辊、平板热压成型机、热压机、平板硫化机或烘箱。
10.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述加热软化该热塑性聚合物基底的同时，给所述碳纳米管膜施加一压力，从而使该碳纳米管膜至少部分嵌入该软化的热塑性聚合物基底之中。
11.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述拉伸该热塑性聚合物基底和该碳纳米管膜的速度小于20厘米每秒。
12.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述碳纳米管膜在垂直于碳纳米管线的方向的形变小于300%。
13.如权利要求1所述的透明导电元件的制备方法，其特征在于，所述拉伸后的碳纳米管膜中的多个碳纳米管线和多个碳纳米管相互搭接形成一导电网络。
14.一种透明导电元件的制备方法，其包括以下步骤：
提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管线并排且间隔设置，以及多个碳纳米管搭接在该相邻碳纳米管线之间；
将该碳纳米管膜设置于一软化的聚合物基底表面；
拉伸该聚合物基底和该碳纳米管膜；以及
硬化该聚合物基底以保持该碳纳米管膜拉伸后的状态。
15.如权利要求14所述的透明导电元件的制备方法，其特征在于，所述聚合物基底为一热固性聚合物基底。
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