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改进Hummers法制备氧化石墨烯的机理研究

作者：徐博，李春丽，张浩月，弓哲，于颖，邱广明

单位：内蒙古工业大学能源与动力工程，呼和浩特 010000

关键词：改进Hummers法；氧化石墨烯；氧化程度；热稳定性

DOI号：

分类号： TQ127.11

出版年,卷(期):页码： 2021,41(6):18-26

摘要：

本文基于改进Hummers法，在不使用硝酸纳的情况下制备氧化石墨烯（Graphene Oxide, GO），实验研究了制备过程中氧化剂用量及中温阶段氧化反应时间对GO氧化程度的影响。采用扫描电镜（SEM）对GO样品的形态结构进行表征；傅里叶红外光谱（FT-IR）、X射线能谱分析（EDS）、激光显微拉曼光谱（Raman）对样品的官能团及氧化程度进行分析；热重分析（TG-DTG）对样品进行热稳定性测试。SEM图片显示，氧化剂用量和氧化反应时间在一定程度上影响所制备GO的表面形貌；Raman光谱表明制备的GO具有不同的缺陷密度；FT-IR和EDS分析发现GO表面含丰富含氧官能团，不同GO样品的含氧量在33%-43%之间，C/O在1.9-1.1之间；TGA分析与元素分析结果相关，表明热失重与元素组成有明显的依赖关系，由于氧含量提高，GOc-3具有最大的失重，而GOa-1具有较高的热稳定性。本研究所得的基于改进的Hummers法制备GO的氧化剂用量和氧化时间的结果分析为后续GO功能化改性提供了理论和数据支撑。

Based on the improved Hummers method, graphene oxide (GO) was prepared without sodium nitrate.The effects of oxidant dosage and oxidation reaction time at medium temperature on the GO oxidation degree were studied in this experiment.The morphological structure of GO samples was characterized by SEM; The functional groups and oxidation degree of the samples were analyzed by Fourier infrared spectroscopy (FT-IR), X-ray energy spectrum analysis (EDS), laser microscopic Raman spectroscopy (Raman) ;The thermal stability of the samples was tested by Thermogravimetric analysis (TG-DTG).The SEM image showed that the amount of oxidant and the oxidation reaction time affected the surface morphology of the prepared GO to some extent; Raman spectra showed that the prepared GO had different defect densities; FT-IR and EDS analysis showed that the surface of GO was rich in oxygen-containing functional groups, The oxygen content of different GO samples was between 33%-43%, and the C/O was between 1.9-1.1;The correlation between TGA analysis and elemental analysis results indicated that the thermal weight loss is obviously dependent on element composition, due to the increase of oxygen content, GOc-3 had the largest weight loss, while GOa-1 had better thermal stability.The analysis of the oxidant dosage and oxidation time of GO prepared by the improved Hummers method provides theoretical and data support for the subsequent functional modification of GO.

基金项目：

内蒙古自然科学基金（2019MS05067、2020MS05033）

作者简介：

徐博（1996-），男，吉林省公主岭市人，硕士生，研究方向为膜分离水处理技术，E-mail：914739874@qq.com

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