CN108020572B - 碳纳米管的表征方法 - Google Patents

碳纳米管的表征方法 Download PDF

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CN108020572B
CN108020572B CN201610933463.2A CN201610933463A CN108020572B CN 108020572 B CN108020572 B CN 108020572B CN 201610933463 A CN201610933463 A CN 201610933463A CN 108020572 B CN108020572 B CN 108020572B
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carbon nanotubes
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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

一种碳纳米管表征方法,其包括以下步骤:提供一导电基底,该导电基底上设置一层绝缘层;在所述绝缘层上设置一碳纳米管结构;将碳纳米管结构放置在扫描电镜下,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结构拍摄照片;获得碳纳米管结构的照片,碳纳米管结构中的碳纳米管分布在照片衬底上。

Description

碳纳米管的表征方法
技术领域
本发明涉及一种碳纳米管的表征方法,尤其设置一种采用扫描电镜对碳纳米管进行表征的方法。
背景技术
单壁碳纳米管是一种非常具有研究潜能的纳米材料。基于其纳米级的尺寸以及特殊的结构,单壁碳纳米管具有良好的电学性能、光电性能以及半导体型能。单壁碳纳米管可以分为金属型和半导体型两种类型。由于这两种碳纳米管的应用范围不同,需要对其进行区分。随着碳纳米管的应用越来越广泛,如何区分金属型碳纳米管和半导体型碳纳米管成为研究的热点。
传统的常用的区分金属型碳纳米管和半导体型碳纳米管的方法为拉曼光谱法或者电学测量的方法。但是由于操作复杂导致效率较低。扫描电镜因其具有较高的辨别效率,被越来越多的人用来表征碳纳米管。请参见图1及图2,传统的采用扫描电镜区表征碳纳米管的方法中,为了获得清晰而且对比度高的照片,采用较低的(1千伏左右)的加速电压。采用传统表征方法获得的碳纳米管照片中,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,传统的扫描电镜表征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。而且,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,难以判断照片中的碳纳米管是金属型还是半导体型。
发明内容
有鉴于此,确有必要提供一种碳纳米管表征方法,该碳纳米管表征方法可以克服以上缺点。
一种碳纳米管表征方法,其包括以下步骤:提供一导电基底,该导电基底上设置一层绝缘层;在所述绝缘层上设置一碳纳米管结构;将碳纳米管结构放置在扫描电镜下,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结构拍摄照片;获得碳纳米管结构的照片,碳纳米管结构中的碳纳米管分布在照片衬底上。
相较于现有技术,本发明所提供的碳纳米管表征方法中,扫描电镜的加速电压远高于传统的碳纳米管的表征方法中扫描电镜的加速电压,因此获得的碳纳米管结构的照片中,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,可以方便的判断出碳纳米管的种类。
附图说明
图1为现有技术中,采用扫描电镜表征碳纳米管获得的照片。
图2为图1的示意图。
图3为本发明实施例提供的碳纳米管表征方法的流程示意图。
图4为本发明实施例提供的碳纳米管的表征方法所获得的碳纳米管的照片。
图5为图4的示意图。
主要元件符号说明
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碳纳米管的表征方法进一步的详细说明。
请参阅图3,本发明第一实施例提供碳纳米管的表征方法,其包括以下步骤:
S1:提供一导电基底,该导电基底上设置一层绝缘层;
S2:在所述绝缘层上设置一碳纳米管结构;
S3:将碳纳米管结构放置在扫描电镜下,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结构拍摄照片;以及
S4:获得碳纳米管结构的照片,碳纳米管结构中的碳纳米管分布在照片衬底上。
在步骤S1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。
在步骤S2中,碳纳米管结构包括一根碳纳米管或者多根碳纳米管。碳纳米管可以平行于绝缘层的表面。当碳纳米管结构包括多根碳纳米管时,该多根碳纳米管可以包括金属型碳纳米管和/或半导体型碳纳米管。本实施例中,碳纳米管结构包括多根金属型碳纳米管和半导体型碳纳米管。
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,获得碳纳米管结构的照片如图4所示,其示意图如图5所示。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4/图5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。
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1)和采用本发明实施例碳纳米管的表征方法所获得的碳纳米管照片(图4),可以得出以下区别:
第一,采用传统表征方法获得的碳纳米管照片中,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,传统的扫描电镜表征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,采用传统表征方法获得的碳纳米管照片中,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,难以判断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表征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,也可以快速判断其种类。
第三,相对于图4,图1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照片图3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。但是现有技术中碳纳米管的表征方法所获得的照片难以准确地判断碳纳米管的种类。本发明提供的碳纳米管的表征方法,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1,图4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的表征方法更加适合。
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 (7)

1.一种碳纳米管的表征方法,其包括以下步骤:
提供一导电基底,该导电基底上设置一层绝缘层,所述绝缘层的材料为氧化物或者高分子材料,所述绝缘层的厚度为50-300纳米;
在所述绝缘层上设置一碳纳米管结构;
将碳纳米管结构放置在扫描电镜下,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结构拍摄照片;以及
获得碳纳米管结构的照片,碳纳米管结构中的碳纳米管分布在照片衬底上,所述碳纳米管结构的照片中,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。
2.如权利要求1所述的碳纳米管的表征方法,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所述的碳纳米管的表征方法,其特征在于,所述碳纳米管结构包括一根或多根碳纳米管。
4.如权利要求1所述的碳纳米管的表征方法,其特征在于,所述碳纳米管结构包括多根碳纳米管,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。
5.如权利要求4所述的碳纳米管的表征方法,其特征在于,所述多根碳纳管平行于绝缘层的表面。
6.如权利要求1所述的碳纳米管的表征方法,其特征在于,所述扫描电镜的加速电压为15-20千伏。
7.如权利要求1所述的碳纳米管的表征方法,其特征在于,所述驻留时间为10-20微秒。
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