作者：龚水水¹, 光善仪³, 柯福佑¹, 徐洪耀^1,2

作者单位：1. 东华大学材料科学与工程学院 纤维材料改性国家重点实验室, 上海 201620;
2. 东华大学分析测试中心, 上海 201620;
3. 东华大学化学化工与生物工程学院, 上海 201620

关键词：傅里叶红外光谱;氧化石墨烯(GO);苯甲酸;羧基官能团;氧化度

摘要：

建立一种红外光谱法测定氧化石墨烯中羧基对应氧化度的方法。利用改进Hummers法制备氧化石墨烯(GO),基于苯甲酸具有类似结构的原理,采用苯甲酸作为标准物质,苯甲酸傅里叶红外光谱在1 591,1504,1 423 cm-1 3处为苯环骨架伸缩振动特征吸收峰,在1 692 cm-1处为羧基中C=O的伸缩振动特征吸收峰,而GO的傅里叶红外光谱在1 630 cm-1为类苯环架构C=C的伸缩振动,在1 730 cm-1为羧基中C=O的伸缩振动特征吸收峰,这样,可利用苯甲酸上苯环和羧基中C=O的峰面积比值与GO上C=C和羧基中C=O的峰面积比值,通过结构分析和相关公式的计算,得到氧化度的值。并且利用紫外可见光谱,X衍射光谱,拉曼光谱,以及原子力显微镜对其进行对比验证,证明红外光谱的方法可行。可为氧化石墨烯羧基氧化度的测定提供一种操作简单、行之有效的方法。关键词:傅里叶红外光谱;氧化石墨烯(GO);苯甲酸;羧基官能团;氧化度

Determination of the content of carboxyl functional groups of graphene oxide by infrared spectroscopy

GONG Shuishui¹, GUANG Shanyi³, KE Fuyou¹, XU Hongyao^1,2

1. The State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China;
2. Analysis and Test Center and National Authorized Computation & Attestation Centers, Donghua University, Shanghai 201620, China;
3. College of Chemistry and Bioengineering, Donghua University, Shanghai 201620, China

Abstract: A method for measuring oxidation degree of graphene oxide by infrared spectroscopy was designed. Graphene oxide was prepared by modified Hummers method andthen benzoic acidwas used as standard substance to measure the oxidation degree based on its analogous structure. The Fourier infrared spectrum of benzoic acid illustrated the peaks ofbenzene ring frame vibration(1 591 cm^-1, 1 504 cm^-1 and 1 423 cm^-1) and carbonyl stretching vibration(1 692 cm^-1). The Fourier infrared spectrum of GO illustrated C=C stretching vibration(1 630 cm^-1) and the characteristic absorption peaks of C=O stretching vibration (1 730 cm^-1). In this way, the ratio of C=O peak areas in benzene ring andcarboxyl on benzoic acid and the ratio of C=O peak areas in C=C and carboxyl on grapheme oxide can be used to calculate and obtain the oxidation degree via structural analysis and correlation formula. Moreover, ultraviolet-visible absorption spectroscopy, Raman spectroscope, X-ray diffraction patterns and atomic force microscopy were also used to further verify the results. It has provedthat infrared spectroscopy is feasible and also has provideda simple and effective method to determine theoxidation degree of graphene oxide carboxyl.

Keywords: Fourier infrared spectroscopy;graphene oxide(GO);benzoic acid;carboxyl group;oxidation degree

2016, 42(4): 38-44  收稿日期: 2015-09-30;收到修改稿日期: 2015-11-13

基金项目: 国家自然科学基金项目(21271040)

作者简介: 龚水水(1989-),女,湖北黄石市人,硕士研究生,专业方向为石墨烯聚苯胺杂化材料。

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