液相界面法石墨烯薄膜构筑初探

论文总字数：29401字

摘 要

富勒烯、碳纳米管和石墨烯是庞大的纳米级碳家族中最为广泛研究的三种材料，而石墨烯更是这其中中潜力和发展最大的材料，在各方面都有很多应用,被各国所看好。宏观石墨烯薄膜因为其在单方向上的极易制成性而成为应用范围最广的。石墨烯薄膜的层状结构赋予他们特别好的光透型、机械性、电特性和热学性质，在实际应用方面有很大潜力。

宏观石墨烯薄膜的简单制备方法包括真空辅助过滤，溶液浇铸,层层组装，柱涂层，浸涂，旋转涂层，喷涂，电泳沉积等等，这些方法在薄膜制备时都是高度可控的，能使石墨烯薄膜具有不同的厚度、维度和结构。

本论文基于2014年提出的一种新方法——液相界面法，即石墨烯在液相界面上进行自组装。论文的主要工作是：超声剥离法制石墨烯溶液、液相界面法制备石墨烯薄膜、透射电子显微镜观察并分析实验用品。通过改变pH值、温度等这些影响因素。

通过本论文的实验，得到的结论有：

（1）酸性越大则薄膜厚度越大，连续性越差，碱性越大薄膜连续性越好，但是机械强度差；

（2）温度能影响溶液间的对流；

（3）不同试剂及不同的添加顺序对于实验都有很大影响，这与它们的溶解度和表面张力有关；

（4）气流能改善薄膜的连续性。

本论文的创新点在于：

尤其是第4点，本论文首次了发现气流对薄膜连续性的影响，并加以探讨，这是本论文重要的创新之处。通过本论文所进行的研究，我们希望能确定每个影响因素的最佳范围，并总结出一套切实可行的实验流程，为液相界面法提供切实可行的工艺。

关键词：石墨烯，宏观薄膜，自组装，液相界面法，工艺优化

Abstract

Graphene、fullerenes and CNTs are the three most famous sp2 nanocarbons in the huge carbon family.Among them,graphene has been especially popular in the recent ten years.Various applications can be applied in all kinds of materials,so many countries have shown great interest in it.A macroscopic 2D film is one of the most applicable forms of graphene due to its extraordinary availability along the lateral direction.Graphene films exhibit much regular and layered structure that endows them with superior specific optical transparency, mechanical, electrical, and thermal properties,showing great potential in practical applications.

The conventional wet methods for 2D graphene films include vacuum-assisted filtration, solution-casting, layer-by-layer assembly,bar-coating, dip-coating, spin-coating, spray-coating,electrophoretic deposition, and so on, all of which are highly controllable during the fabrication, resulting in graphene films with varied thickness, dimension, and structure.

This article aims to discuss and develop another process known as liquid interface method,which is presented in 2014.This process happens at the liquid interface.The main job during the process includes ultrasonic stripping method for graphene solution,liquid interface method for graphene films,the observation and analysis of the TEM image of the graphene. With changing influence factors such as pH value,temperature and so on,not only the microstructure,but also the macro structure have proved to be different.

Some conclusions follow the experiments:

1. the pH value and the film continuity have the positive correlation,while the value and the Mechanical strength have the negative correlation;
2. convection between the solutions can be affected by the temperature;
3. different solutions and different adding order has a great influence for the experiment, which related to their solubility and surface tension;
4. Air can improve the continuity of the membrane.

By completing these series of experiments,we wish we could confirm the optimal value of those influence factors and afterwards an easy and effective industry process could be accessible.

keywords: graphene,micro films,self-assembly,liquid interface method,optimization technique

目录

第一章 绪论

1.1引言..............................................................................................................................7

1.2石墨烯薄膜制备方法的研究进展..............................................................................8

1.2.1制备石墨烯薄膜的湿法 ....................................................................................8

1.2 .1.1真空辅助过滤.......................................................................................8

1.2.1.2滴定制备法............................................................................................9

1.2.1.3旋涂法....................................................................................................10

1.2.1.4浸涂........................................................................................................10

1.2.1.5喷涂........................................................................................................11

1.2.1.6层层组装................................................................................................11

1.2.1.7电泳沉积................................................................................................11

1.2.1.8 L-B组装................................................................................................12

1.2.2在接触面上组装石墨烯薄膜............................................................................13

1.2.3连续的湿纺石墨烯薄膜....................................................................................14

1.3本论文的主要工作和创新点 ....................................................................................15

第二章 石墨烯的制备及表征技术.........................................................................................18

2.1 石墨烯的制备方法 ....................................................................................................18

2.1.1 氧化还原法制备石墨烯..................................................................................18

2.1.2 超声剥离法制备石墨烯..................................................................................21

2.1.3 方法选择及原因分析......................................................................................21

2.2 石墨烯的透射电镜表征 ............................................................................................21

第三章 液相界面法石墨烯薄膜构筑初探 ............................................................................24

3.1 实验条件 ....................................................................................................................24

3.2 薄膜构筑实验方法和流程........................................................................................24

3.3 实验结果和分析........................................................................................................24

第四章 影响自组装成膜的因素探讨.....................................................................................26

4.1 试剂的添加顺序对成膜的影响................................................................................26

4.2 试剂的体积比例对成膜的影响................................................................................27

4.3 温度对成膜的影响....................................................................................................28

4.4 pH值对成膜的影响.................................................................................................29

4.5 试剂的种类对成膜的影响.........................................................................................35

4.5.1 甲醇-NMP体系成膜实验设计........................................................................36

4.5.2 乙醇-NMP体系成膜实验设计.........................................................................37

4.5.3 丙酮-NMP体系成膜实验设计.........................................................................38

4.5.4正己烷-NMP体系成膜实验设计.......................................................................38

4.6 气流对成膜的影响........................................................................................................39

4.7 小结................................................................................................................................40

第五章 实验结论与展望.........................................................................................................42

致谢...........................................................................................................................................44

参考文献...................................................................................................................................45

第一章 绪 论

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