电火花分散法制备纳米石墨及其热氧化性能研究

А. Satyvaldiev, G.E. Satyvaldieva, Zh.B Bakеnov
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摘要

本文介绍了用电火花分散法制备纳米石墨的可能性的研究结果。通过粉末x射线衍射和透射电镜证实了EUZ-3级石墨在蒸馏水和95%乙醇中电火花分散过程中纳米石墨的形成。在水和醇中获得的纳米石墨的衍射模式是相同的,并且它们具有属于石墨的线反射。纳米晶具有相同的面间距和晶格参数。纳米石墨的晶格参数值表明,石墨在电火花分散的条件下没有改变其结构,纳米石墨具有六方晶格的特征。计算了相干散射区的大小和TEM照片中粒子的平均直径,证实了纳米石墨的形成。在水中形成的纳米石墨的分散性(d CSR = 6.5 nm, d av = 6±1 nm)高于在醇中形成的纳米石墨(d CSR = 9.8 nm, d av = 10±2 nm)。通过对衍生图的分析,建立了衍生图的TG和DTA曲线的变化与合成纳米石墨的液体介质性质的关系。对纳米微球的衍生图分析表明,衍生图的热重和差热分析曲线的走向取决于纳米微球所处液体介质的性质。在200-700℃的温度范围内,纳米石墨在水中的氧化分为三个阶段。当这种纳米石墨在空气中加热到1000℃时,由于石墨形式的碳氧化,样品的质量下降了92.0%。在衍生图上,合成的纳米石墨在400 ~ 700℃的温度范围内呈现出强烈的放热双重效应,样品质量下降95.75%。
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SYNTHESIS OF NANOGRAPHITE BY ELEKTROSPARK DISPERSION AND STUDY OF ITS THERMAL OXIDATION
The paper presents the results of studying the possibility of obtaining nanosized graphite by the method of electrospark dispersion. The formation of nanographite during electrospark dispersion of EUZ-3 grade graphite in distilled water and 95 % ethanol was confirmed by powder X-ray diffraction and transmission electron microscopy.The diffraction patterns of nanographites obtained in water and alcohol are identical, and they have line reflexes that belong to graphite. The nanographites have the same interplanar spacing and lattice parameter. The value of the lattice parameter of nanographites indicates that graphite does not change its structure under the conditions of electrospark dispersion, and nanographites are characterized by a hexagonal crystal lattice. The results of calculating the size of the coherent scattering region and determining the average diameter of particles from TEM photographs confirm the formation of nanographite. More highly dispersed (d CSR = 6.5 nm, d av. = 6±1 nm) nanographite is formed in water than in alcohol (d CSR = 9.8 nm, d av. = 10±2 nm). When analyzing the derivatograms, the dependence of the change in the TG and DTA curves of the derivatograms on the properties of the liquid medium where nanographite was synthesized was established. An analysis of the derivatograms of nanographites shows that the course of the TG and DTA curves of the derivatograms depends on the nature of the liquid medium in which the nanographite was obtained. Oxidation of nanographite obtained in water occurs in three stages in the temperature range of 200–700 °C. When this nanographite is heated to 1000 °C in air, the decrease in the mass of the sample, due to the oxidation of carbon in the form of graphite, is 92.0 %. On the derivatogram, the oxidation of nanographite synthesized in alcohol is characterized by an intense doublet of exothermic effects covering the temperature range of 400–700 °C and the decrease in the mass of the sample is 95.75 %.
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