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材料研究学报  2015, Vol. 29 Issue (2): 155-160    DOI: 10.11901/1005.3093.2014.316
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氧化石墨烯的制备和定性定量分析
赖奇1,2(),罗学萍2
1. 攀枝花学院材料学院 攀枝花 617000
2. 攀枝花学院 石墨深加工实验室 攀枝花 617000
Qualitative and Quantitative Analysis of Graphene Oxides by UV Spectroscopy
Qi LAI1,2,**(),Xueping LUO2
1. College of Material Engineering, Panzhihua University, Panzhihua 617000, China
2. Deep-processing Laboratory of Graphite, Panzhihua University, Panzhihua 617000, China
引用本文:

赖奇,罗学萍. 氧化石墨烯的制备和定性定量分析[J]. 材料研究学报, 2015, 29(2): 155-160.
Qi LAI, Xueping LUO. Qualitative and Quantitative Analysis of Graphene Oxides by UV Spectroscopy[J]. Chinese Journal of Materials Research, 2015, 29(2): 155-160.

全文: PDF(1652 KB)   HTML
摘要: 

以鳞片石墨为原料, 采用硫酸和高锰酸钾, 通过化学插层氧化-破碎方法制备了氧化石墨烯(GO), 通过扫描电镜(SEM)、激光粒度分析、红外光谱(FT-IR)、紫外-可见光谱(UV-vis)和原子力显微镜(AFM)等测试手段对所制备的氧化石墨烯进行了分析和表征。结果发现230 nm附近的紫外可见光谱可以把氧化石墨烯与氧化石墨进行区分。结果表明紫外光谱可对氧化石墨烯溶液进行定性分析和定量分析。通过这一方法可获得氧化石墨烯制备的较优条件。机理分析结果表明: 氧化石墨烯的不连续的π-π*共轭体系为主的结构特点是其紫外光谱在230 nm附近产生多个强度不同的吸收峰的原因。

关键词 无机非金属材料氧化石墨烯定量紫外机理    
Abstract

Graphene oxide (GO) was prepared by chemical oxidation-sonicated crushing method with flake graphite, sulfuric acid and potassium permanganate as raw materials. The prepared GO was characterized by means of spectroscopy SEM, laser granulometer, FT-IR, UV-vis and AFM. The results show that the few-layered GO could be differentiated from the multi-layered graphite oxide in a solution of the mixture of the two by observing the variation of the intensity and the profile of absorption peaks around 230 nm in the UV-vis spectroscopy. Based on this phenomenon, the qualitative and quantitative analysis of graphene oxides in the solution can be realized. Thereby the optimal conditions for the preparation of graphene oxide can be obtained. It is proposed that the appearence of multi absorption peaks nearby 230 nm in the UV spectra of GO may be attributed to the existence of a peculiar structure of discontinues p-p* conjugated system in the graphene oxide.

Key wordsinorganic non-metallic materials    graphene oxide    quantitative analysis    UV-vis spectroscopy    Mechanism
收稿日期: 2014-07-01     
基金资助:* 四川省高校重点实验室2013002资助项目。
图1  不同高锰酸钾用量时的氧化石墨烯的紫外光谱
图2  氧化石墨烯的原子力显微镜图(a-d)和高度图(c-h)
图3  氧化石墨烯的粒度仪测试结果
图4  氧化石墨的扫描电镜图
图5  不同氧化剂用量条件下氧化石墨烯的红外光谱
图6  GO的标准曲线
Measurement values / mgmL-1 Real values / mgmL-1 Error/%
C1 0.023 0.024 4.2
C2 0.086 0.88 2.3
C3 0.079 0.084 6
  
图7  不同破碎时间和不同破碎功率下SK350氧化石墨烯溶液紫外-可见光谱
图8  不连续的p键
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