浓硫酸氧化改性天然辉钼矿及其电催化性能研究.pdf

北京大学学报( 自然科学版) 第 54 卷 第 3 期 2018 年 5 月 Acta Scientiarum Naturalium Universitatis Pekinensis, Vol. 54, No. 3 (May 2018) doi: 10.13209/j.0479-8023.2017.083 浓硫酸氧化改性天然辉钼矿及其电催化性能研究 强静雅 传秀云† 造山带与地壳演化教育部重点实验室 , 北京大学地球与空间科学学院 , 北京 100871; † 通信作者 , E-mail: xychuan@pku.edu.cn 摘要 用浓硫酸加热氧化法 , 获得提纯的辉钼矿。利用 X 射线荧光光谱(XRF) 、X 射线衍射(XRD) 、X 射线 光电子能谱(XPS) 、扫描电子显微镜(SEM)和拉曼光谱(Raman), 对氧化前后的样品进行表征 , 并测试样品的 电催化性能。经浓硫酸氧化后, MoS2 的(002) 晶面晶粒的平均粒径减小 14%, 层间距增加 0.04 Å, 且 S2−被氧 化为 S6+ 。结果表明, 经过浓硫酸氧化, MoS2 的片层能够在一定程度上被剥离, 辉钼矿对于对硝基苯酚的还原 作用增强, 还原峰电位发生正向移动。 关键词 辉钼矿 ; 酸浸氧化; X 射线衍射 ; 拉曼光谱 ; 电化学催化 中图分类号 O614; P579 Oxidation Modification of Natural Molybdenite Using Concentrated Sulfuric Acid and Its Electrocatalytic Properties QIANG Jingya, CHUAN Xiuyun† The Key Laboratory of Orogenis Belts and Crustal Evolution (MOE), School of Earth and Space Sciences, Peking University, Beijing 100871; † Corresponding author, E-mail: xychuan@pku.edu.cn Abstract The purified molybdenite were obtained using concentrated sulfuric acid and heating oxidation method, and the samples before and after oxidation were characterized systematically based on X-ray fluorescence spectrum (XRF), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and Raman spectroscopy. Moreover, its electrocatalytic properties were tested and analyzed. The results show that the average grain size of MoS2 (002) crystal plane direction decreases by 14% and interlayer spacing increases 0.04Å after c