CN107089653A - 一种还原氧化石墨烯碳支持膜透射电镜载网及其制备方法 - Google Patents
一种还原氧化石墨烯碳支持膜透射电镜载网及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种还原氧化石墨烯碳支持膜透射电镜载网及其制备方法。它的步骤如下:(1)取一片普通无碳膜电镜载网放在滤纸上;(2)将氧化石墨烯溶液均匀铺在载网上表面;(3)常温或加热条件下使溶剂挥发;(4)化学或热还原得到还原氧化石墨烯碳支持膜透射电镜载网。本发明可制备超薄的碳支持膜,实现高衬度、高分辨率。且还原后的碳支持膜显示电中性,有利于有机试剂做溶剂的纳米粒子的分散。该种制备碳支持膜方法具有操作简单、成本低廉等优点。
Description
技术领域
本发明涉及一种透射电镜载网及其制备方法,特别是涉及一种用于透射电子显微镜的还原氧化石墨烯碳支持膜透射电镜载网及其制备方法。
背景技术
透射电子显微镜因使用波长更短的电子作光源,可以看到光学显微镜无法看到的200nm以下的结构,同时保证高分辨率,因为以上特性,它在材料科学,生命科学等领域中已经成为不可或缺的检测手段。由于蛋白质及各种纳米材料的直径较小且分散性很好,为了能确保样品能够搭载载网上,会在载网上覆盖一层有机膜,称为“支持膜”。但由于支持膜导电性差,在电子束的照射下很容易产生电荷积累,使样品飘逸、跳动甚至支持膜破裂等。为了解决这个问题,可以通过在有机支持膜上喷一层碳膜来提高导电性,一般碳膜厚度在7-10nm。而超薄碳膜是指厚度在3-5nm的碳膜。碳膜的厚度越薄,它的衬度越高,分辨率越高;但是过薄的碳膜会导致其机械强度变低。现有的碳支持膜制备工艺复杂且厚度较厚,对于部分样品无法达到衬度要求。
石墨烯是由碳原子以六边形键合的二维单原子层晶体,基于它的化学结构,石墨烯具有许多超出传统材料的优异的物理化学性质,易于修饰及大规模生产。其厚度仅有0.34nm,且机械强度高。
发明内容
本发明的目的在于提供一种具有高机械强度,高有机样品粘附性且高衬度的还原氧化石墨烯碳支持膜透射电镜载网及其制备方法。
本发明的目的是通过以下技术方案实现的:一种还原氧化石墨烯碳支持膜透射电镜载网,包括承载组件,所述承载组件具有镂空孔;还包括覆盖于镂空孔上的寡层还原氧化石墨烯,所述寡层还原氧化石墨烯的层数少于10层。
一种还原氧化石墨烯碳支持膜透射电镜载网的制备方法,该方法为:将浓度为0.001~10mg/mL的氧化石墨烯溶液均匀铺在承载组件表面,晾干并还原后得到电镜载网。
进一步地,所述承载组件的材质选自铜、镍、钼、钛、金、碳。
进一步地,所述承载组件表面是否具有支持膜均可。
进一步地,氧化石墨烯溶液的溶剂由水、甲醇、乙醇、N-甲基吡咯烷酮、丙酮、二甲亚砜、吡啶、二氧六环、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、丁酮、乙二醇、二甘醇中的一种或多种按任意配比混合组成;
进一步地,氧化石墨烯溶液均匀铺在承载组件表面,通过以下方法实现:直接通过滴加方法使溶液覆盖载网;将载网浸泡在溶液中再提拉出来;或将溶液旋涂或直接涂抹于载网上;
进一步地,旋涂的速度在300~8000rpm;
进一步地,滴加在载网上的石墨烯溶液体积在2~20μL;
进一步地,将载网浸泡在溶液中再提拉出来的提拉速度在0.1~200mm/min。
进一步地,还原方法包括热还原、化学还原和光还原。
本发明的有益效果是:本发明通过简单的方法将寡层石墨烯覆盖于镂空孔上,最薄可达到单层氧化石墨烯厚度0.34nm;在保证了样品拍摄时的高衬度和高分辨率的同时兼顾了强度,确保在载样品时碳膜不会破裂;此外,由于还原氧化石墨烯表面负电性官能团在还原过程中已经被脱去,呈现电中性,所以对于有机溶剂分散的样品具有很好的粘附作用;氧化石墨烯制备工艺简单且已有规模化生产,该种碳膜的制备方法步骤简单,原料廉价易得。
附图说明
图1是本发明制备的超薄碳膜载网的扫描电镜图及局部放大图;
图2是本发明制备的超薄碳膜载网的电子衍射图;
图3是本发明制备的超薄碳膜载网负载硅颗粒的电镜图。
图4是本发明制备的超薄碳膜载网的拉曼光谱图。
具体实施方式
一种氧化石墨烯碳支持膜透射电镜载网及其制备方法,它的步骤如下:(1)取一片普通无碳膜电镜载网放在滤纸上;(2)将氧化石墨烯溶液均匀铺在载网上表面;(3)常温或加热条件下使溶剂挥发。
本发明于提供一种具有高机械强度,高样品粘附性、高衬度的超薄碳膜的制备方法。
下面通过实施例对本发明进行具体描述,本实施例只用于对本发明做进一步的说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的内容做出一些非本质的改变和调整,均属于本发明的保护范围。
实施例1:
(1)取无支持膜的1000目的透射电镜铜载网放在滤纸上;
(2)用移液枪移取浓度为0.1mg·mL-1的氧化石墨烯水溶液5μL,自然滴落在铜网表面;
(3)将上述整体样品放在干净无尘的室温环境中,直到水自然挥发干。
(4)将上述样品整体放在水合肼气氛中,七十摄氏度下还原八小时。
由图1看出石墨烯片层平铺在镂空孔上,图2的电子衍射图看出,在最厚的地方仅由三层石墨烯组成。将该载网用于纳米硅颗粒的制样,如图3所示,在图3中可以看出,该种石墨烯支持膜强度较高,在负载了纳米硅颗粒后依旧保持支持膜的完整性。图4可以看出还原后,还原氧化石墨烯碳支持膜的还原程度较高。
实施例2:
(1)取具有微栅支持膜的200目的透射电镜载网,将其浸入浓度为0.5mg·mL-1的氧化化石墨烯乙醇溶液再以1mm/min的速度均匀提拉上来;
(2)将上述样品放在干净无尘的烘箱中40℃加热,直到水自然挥发干。
(3)将上述样品整体高温1000℃氢气气氛下还原2小时。通过测试,该石墨烯支持膜强度较高,衬度高。
实施例3:
(1)取具有微栅支持膜的300目的透射电镜载网,将浓度为0.001mg/mL的氧化化石墨烯乙醇溶液对透射电镜载网进行旋涂5-10s,旋涂的速度为300rpm;
(2)将上述样品放在干净无尘的烘箱中40℃加热,直到水自然挥发干。
(3)将上述样品整体高温1000℃氢气气氛下还原2小时。通过电子衍射测试,在最厚的地方仅由10层石墨烯组成,该石墨烯支持膜强度较高,衬度高。
实施例4:
(1)取具有微栅支持膜的300目的透射电镜载网,将其浸入浓度为10mg/mL的氧化化石墨烯四氢呋喃溶液再以1mm/min的速度均匀提拉上来;
(2)将上述样品放在干净无尘的烘箱中40℃加热,直到水自然挥发干。
(3)将上述样品整体高温1000℃氢气气氛下还原2小时。通过测试,该石墨烯支持膜强度较高,衬度高。
Claims (10)
1.一种还原氧化石墨烯碳支持膜透射电镜载网,包括承载组件,所述承载组件具有镂空孔;其特征在于,还包括覆盖于镂空孔上的寡层还原氧化石墨烯,所述寡层还原氧化石墨烯的层数少于10层。
2.一种权利要求1所述的还原氧化石墨烯碳支持膜透射电镜载网的制备方法,其特征在于,该方法为:将浓度为0.001~10mg/mL的氧化石墨烯溶液均匀铺在承载组件表面,晾干并还原后得到电镜载网。
3.如权利要求2所述的制备方法,其特征在于:所述承载组件的材质选自铜、镍、钼、钛、金、碳等。
4.根据权利要求2所述的制备方法,其特征在于,所述承载组件表面是否具有支持膜均可。
5.如权利要求2所述的制备方法,其特征在于:氧化石墨烯溶液的溶剂由水、甲醇、乙醇、N-甲基吡咯烷酮、丙酮、二甲亚砜、吡啶、二氧六环、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、四氢呋喃、丁酮、乙二醇、二甘醇中的一种或多种按任意配比混合组成。
6.如权利要求2所述的制备方法,其特征在于:氧化石墨烯溶液均匀铺在承载组件表面,通过以下方法实现:直接通过滴加方法使溶液覆盖载网;将载网浸泡在溶液中再提拉出来;或将溶液旋涂或直接涂抹于载网上。
7.如权利要求6所述的制备方法,其特征在于:旋涂的速度在300~8000rpm。
8.如权利要求6所述的制备方法,其特征在于:滴加在载网上的石墨烯溶液体积在2~20μL。
9.如权利要求6所述的制备方法,其特征在于:将载网浸泡在溶液中再提拉出来的提拉速度在0.1~200mm/min。
10.如权利要求2所述的制备方法,其特征在于:还原方法包括热还原、化学还原和光还原等。
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