ELECTROCHEMICAL DISPERSION OF GRAPHITE IN 58% NITRIC ACID TO PRODUCE MULTILAYER GRAPHENE OXIDE

E. Yakovleva, A. Yakovlev, I. N. Frolov, A. Mostovoy, V. Tseluikin
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Abstract

Electrochemical oxidation of graphite powder in 58% HNO3 was studied. Samples of oxidized graphite were obtained with a imparting of the amount of electricity 500, 700, 1500 mAh g-1. The character of the galvanostatic dependencies allows to select a region of the formation of intercalated compounds of graphite prior to the accumulation of quantity of electricity of 500 mA h g-1. It was found that when the quantity of electricity of over 700 mA h g-1 the process of electrochemical peroxidation of intercalated graphite begins with the formation of multilayer graphene oxide, as confirmed by comprehensive studies using X-ray diffraction, scanning electron microscopy, FTIR spectroscopy, laser diffraction. The synthesized multilayer graphene oxide is characterized by the presence of a spectrum of oxygen-containing functional groups, mainly hydroxyl, as well as carboxyl, epoxy and alkoxyl. X-ray images show a peak at 2θ = 11.45° which intensity increases for re-oxidized graphite compounds and also indicate the formation of a multilayer graphene oxide with an interlayer distance of 7.8 Å. The synthesized material in aqueous suspensions under the action of ultrasound is dispersed with a 7-11-fold reduction in particle size. Graphene layers remains layered structure but the degree of their deformation increases, and the thickness of the layers decreases with an increase in the imparted amount of electricity.
石墨在58%硝酸中电化学分散制备多层氧化石墨烯
研究了石墨粉在58% HNO3中的电化学氧化。在500、700、1500毫安时g-1的电注入下得到氧化石墨样品。恒电流依赖性的特性允许在积累500 mA h g-1的电量之前选择石墨插层化合物形成的区域。通过x射线衍射、扫描电镜、傅里叶红外光谱、激光衍射等综合研究发现,当电量大于700 mA h g-1时,插层石墨的电化学过氧化过程开始形成多层氧化石墨烯。合成的多层氧化石墨烯的特点是存在一系列含氧官能团,主要是羟基,还有羧基、环氧基和烷氧基。x射线图像显示,再氧化石墨化合物在2θ = 11.45°处有一个峰值,其强度增加,也表明形成了多层氧化石墨烯,层间距离为7.8 Å。在超声作用下,水相悬浮液中合成的材料分散,粒径减小7-11倍。石墨烯层保持层状结构,但其变形程度增加,层的厚度随着输入电量的增加而减小。
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