CN108002364B - 透明导电层的制备方法 - Google Patents

透明导电层的制备方法 Download PDF

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CN108002364B
CN108002364B CN201610942312.3A CN201610942312A CN108002364B CN 108002364 B CN108002364 B CN 108002364B CN 201610942312 A CN201610942312 A CN 201610942312A CN 108002364 B CN108002364 B CN 108002364B
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carbon nanotubes
nanotube film
transparent conductive
conductive layer
carbon nanotube
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CN108002364A (zh
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李东琦
魏洋
姜开利
范守善
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Abstract

一种透明导电层的制备方法，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；提供一导电基底，该导电基底上设置一层绝缘层；将所述碳纳米管膜设置在所述绝缘层上；将碳纳米管膜放置在扫描电镜下，调整扫描电镜的加速电压为5～20千伏，驻留时间为6～20微秒，放大倍数为1万～10万倍，采用扫描电镜对所述碳纳米管膜拍摄照片；获得碳纳米管膜的照片，照片中碳纳米管分布在衬底上，比衬底颜色浅的碳纳米管为金属型碳纳米管，比衬底颜色深的碳纳米管为半导体型碳纳米管；按照和照片相同的比例，在实物上相同的位置对半导体型的碳纳米管进行标识，并除去半导体型的碳纳米管。

Description

透明导电层的制备方法
技术领域
本发明涉及一种透明导电层的制备方法，尤其设置一种基于碳纳米管的透明导电层的制备方法。
背景技术
碳纳米管膜作为透明导电层，被越来越多的领域应用。现有技术中，碳纳米管膜通过一定方法获得之后，便直接拿来用作透明导电层。然而，由于碳纳米管可以分为金属型和半导体型两种类型，半导体型的碳纳米管导电性能差，因此，在采用碳纳米管膜作为透明导电层时，碳纳米管膜中的半导体型的碳纳米管影响了透明导电层的导电性能。因此，采用传统方法获得的碳纳米管透明导电膜的导电性能不好，需要进一步改善。
发明内容
有鉴于此，确有必要提供一种透明导电层的制备方法，该透明导电层的制备方法可以克服以上缺点。
一种透明导电层的制备方法，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；提供一导电基底，该导电基底上设置一层绝缘层，将所述碳纳米管膜设置在所述绝缘层上；将碳纳米管膜放置在扫描电镜下，调整扫描电镜的加速电压为5～20千伏，驻留时间为6～20微秒，放大倍数为1万～10万倍，采用扫描电镜对所述碳纳米管膜拍摄照片；获得碳纳米管膜的照片，照片中碳纳米管分布在衬底上，比衬底颜色浅的碳纳米管为金属型碳纳米管，比衬底颜色深的碳纳米管为半导体型碳纳米管；按照和照片相同的比例，在实物上相同的位置对半导体型的碳纳米管进行标识，并除去半导体型的碳纳米管。
相较于现有技术，本发明所提供的透明导电层的制备方法中，包括一除去半导体型碳纳米管的步骤，使得透明导电层中的碳纳米管均为金属型碳纳米管，因此，获得的透明导电层的导电性能良好。
附图说明
图1为本发明第一实施例提供的透明导电层的制备方法的流程示意图。
图2为本发明第一实施例提供的碳纳米管类型的判断方法所获得的碳纳米管的照片。
图3为图2的示意图。
图4为现有技术中，采用扫描电镜获得的碳纳米管照片。
图5为图4的示意图。
主要元件符号说明
无
如下具体实施方式将结合上述附图进一步说明本发明。
具体实施方式
以下将结合附图对本发明的提供的透明导电层的制备方法进一步的详细说明。
请参阅图1，本发明第一实施例提供透明导电层的制备方法，其包括以下步骤：
S1：提供一碳纳米管膜，该碳纳米管膜包括多个碳纳米管；
S2：提供一导电基底，该导电基底上设置一层绝缘层，将碳纳米管膜设置于所述绝缘层上；
S3：将碳纳米管膜放置在扫描电镜下，调整扫描电镜的加速电压为5～20千伏，驻留时间为6～20微秒，放大倍数为1万～10万倍，采用扫描电镜对所述碳纳米管膜拍摄照片；
S4：获得碳纳米管膜的照片，照片中碳纳米管分布在衬底上，比衬底颜色浅的碳纳米管为金属型碳纳米管，比衬底颜色深的碳纳米管为半导体型碳纳米管；以及
S5：按照和照片相同的比例，在实物上相同的位置对半导体型的碳纳米管进行标识，并除去半导体型的碳纳米管。
在步骤S1中，所述碳纳米管膜包括多个碳纳米管。该碳纳米管可以为单壁碳纳米管、双壁碳纳米管或多壁碳纳米管。该碳纳米管可以为金属型或者半导体型。碳纳米管的直径不限，可以为0.5纳米～150纳米，在某些实施例中，碳纳米管的直径可以为1纳米～10纳米。所述多个碳纳米管的排列方向不限，可以交叉排列或平行排列。本实施例中，碳纳米管膜中的多个碳纳米管相互平行，并且平行于绝缘层的表面。
在步骤S2中，所述导电基底的材料不限，只要是导电材料即可，可以为金属、导电有机物或掺杂的导电材料。本实施例中，选用掺杂的硅作为导电基底材料。所述绝缘层的材料为绝缘材料，可以为氧化物或者高分子材料。本实施例中，选用氧化硅材料。所述绝缘层的厚度为50-300纳米。所述碳纳米管膜设置于绝缘层上之后，碳纳米管膜中的碳纳米管平行于绝缘层的表面。
在步骤S3中，优选地，加速电压为15-20千伏，驻留时间为10-20微秒。本实施例中，加速电压为10千伏，驻留时间为20微秒，放大倍数为2万倍。
在步骤S4中，获得碳纳米管膜的照片如图2所示，其示意图如图3所示。图2/图3中包括衬底以及形成在衬底上的碳纳米管的影像。从图2/图3可以看出，一部分碳纳米管的颜色比衬底的颜色浅，一部分碳纳米管的颜色比衬底的颜色深。比衬底颜色浅的碳纳米管为金属型碳纳米管；比衬底颜色深的碳纳米管为半导体型碳纳米管。
本发明所提供的透明导电层的制备方法中，采用扫描电镜对碳纳米管膜中的碳纳米管进行区分，对比现有技术中采用扫描电镜表征碳纳米管的方法所获得的碳纳米管的照片图4/图5，和采用本发明实施例区分碳纳米管类型的方法所获得的碳纳米管照片图2/图3，可以得出以下区别：
第一，采用传统方法获得的碳纳米管扫描电镜照片中，碳纳米管的导电性能与照片中的颜色有关，颜色越浅，导电性能越好，但是，碳纳米管的颜色都是比衬底的颜色浅。当照片中同时存在金属型碳纳米管和半导体型碳纳米管时，对于处于中间色的碳纳米管，如灰色的碳纳米管，在判断这些碳纳米管的种类时，常会发生错误。因此，传统的扫描电镜区分碳纳米管的方法在辨识碳纳米管种类时，准确度不够高，常常会出现误判或者难以判断。而采用本发明实施例所获得的碳纳米管照片中，金属型碳纳米管比衬底的颜色浅，半导体型的碳纳米管比衬底的颜色深，因此在判断碳纳米管属于金属型还是半导体型时，便可以一目了然。
第二，采用传统方法获得的碳纳米管扫描电镜照片中，由于无论金属型还是半导体型的碳纳米管，在照片中显示的颜色均比衬底颜色浅，当照片中只存在一种类型的碳纳米管时，难以区分照片中的碳纳米管是金属型还是半导体型。而采用本发明所提供的碳纳米管区分方法所获得的碳纳米管照片中，金属型碳纳米管比衬底的颜色浅，半导体型的碳纳米管比衬底的颜色深，即使照片中只存在一种类型的碳纳米管，也可以快速区分其类型。
第三，相对于图2/图3，图4/图5的对比度更高，视觉上更容易观察碳纳米管，而且照片比较美观，而本发明实施例所获得的扫描电镜照片图2中，分辨率相对较低，照片也不够美观，所以现有技术中均是采用低加速电压对碳纳米管进行表征和区分。但是现有技术中区分碳纳米管类型的方法所获得的照片难以准确地区分碳纳米管的种类。本发明提供的区分碳纳米管类型的方法，能够快速而准确的判断碳纳米管的种类，克服了技术偏见。
第四，相对于图4/图5，图2/图3中碳纳米管成像的宽度较小，因此，对于密度较高的多个碳纳米管，本发明所提供的碳纳米管类型的判断方法更加适合。
步骤S5的具体步骤可以为：
S51：在照片上建立一坐标系，并读出半导体型碳纳米管的具体坐标值；
S52：按照和照片相同的比例，在实体碳纳米管膜上建立坐标系，根据半导体型碳纳米管的坐标值标识出半导体型的碳纳米管，并将半导体型的碳纳米管除去。
本实施例中，用电子束曝光的方法，将该金属型的碳纳米管进行保护，将半导体型的碳纳米管露出，采用等离子体刻蚀的方法将半导体型的碳纳米管去除。
本发明所提供的透明导电层的制备方法由于采用了上述方法区分碳纳米管膜中的碳纳米管，因此，可以准确快速的判断出碳纳米管的类别，从而除去半导体型的碳纳米管，得到仅包括金属型碳纳米管的透明导电层，因此，制备出的透明导电层的导电性好。
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 (10)

1.一种透明导电层的制备方法，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；
提供一导电基底，该导电基底上设置一层绝缘层，将所述碳纳米管膜设置在所述绝缘层上；
将碳纳米管膜放置在扫描电镜下，调整扫描电镜的加速电压为5～20千伏，驻留时间为6～20微秒，放大倍数为1万～10万倍，采用扫描电镜对所述碳纳米管膜拍摄照片；
获得碳纳米管膜的照片，照片中碳纳米管分布在衬底上，比衬底颜色浅的碳纳米管为金属型碳纳米管，比衬底颜色深的碳纳米管为半导体型碳纳米管；
按照和照片相同的比例，在实物上相同的位置对半导体型的碳纳米管进行标识，并除去半导体型的碳纳米管。
2.如权利要求1所述的透明导电层的制备方法，其特征在于，所述导电基底的材料为金属、导电有机物或掺杂的导电材料。
3.如权利要求1所述的透明导电层的制备方法，其特征在于，所述绝缘层的材料为氧化物或者高分子材料。
4.如权利要求1所述的透明导电层的制备方法，其特征在于，所述绝缘层的厚度为50-300纳米。
5.如权利要求1所述的透明导电层的制备方法，其特征在于，所述碳纳米管膜包括多根碳纳米管，该多根碳纳米管包括金属型碳纳米管和半导体型碳纳米管。
6.如权利要求1所述的透明导电层的制备方法，其特征在于，所述碳纳米管膜包括多根碳纳米管，所述多根碳纳管平行于绝缘层的表面。
7.如权利要求1所述的透明导电层的制备方法，其特征在于，所述扫描电镜的加速电压为15-20千伏。
8.如权利要求1所述的透明导电层的制备方法，其特征在于，所述驻留时间为10-20微秒。
9.如权利要求1所述的透明导电层的制备方法，其特征在于，所述按照和照片相同的比例，在实物上相同的位置对半导体型的碳纳米管进行标识的步骤包括：在照片上建立一坐标系，并读出半导体型碳纳米管的具体坐标值；按照和照片相同的比例，在实体碳纳米管膜上建立坐标系，根据半导体型碳纳米管的坐标值标识出半导体型的碳纳米管。
10.如权利要求1所述的透明导电层的制备方法，其特征在于，所述除去半导体型的碳纳米管的步骤包括：用电子束曝光的方法，将该金属型的碳纳米管进行保护，将半导体型的碳纳米管露出，采用等离子体刻蚀的方法将半导体型的碳纳米管去除。
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