含石墨烯纳米碳材料的形貌和结构特征

E. Belonogov, Sergey B. Kushev, Sergey A. Soldatenko, T. L. Turaeva
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摘要

石墨纳米结构粉末(GSM-2;Taunit-M;采用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、x射线衍射(XRD)、反射高能电子衍射(RHEED)、拉曼光谱等方法对热膨胀石墨(TEG)进行了表征。通过叠加理论衍射最大值解释了实验XRD晕,发现了x射线非晶石墨相。发现x射线非晶相以石墨纳米化的极限程度为特征。根据衍射环的宽度,估计了石墨纳米晶体的最大尺寸,在[0001]和[]方向上分别不超过5 nm和10 nm。揭示了碳纳米管和涡层石墨烯板。纳米结构材料“Taunit-M”的结构和形态参数已经确定-直径高达10 nm的多壁纳米管通过x射线无定形碳中间层组合成宽达40 nm的扁平带状。暗场TEM图像(反射)显示,由于电子束的双重衍射,在重叠的石墨烯片上出现了莫尔纹图案。研究发现,在热膨胀石墨中,石墨烯片的旋转范围为3 ~ 4°。在石墨烯薄片内,发现了Burgers向量b = 1/2的完全位错[1010]。莫尔维尔图像的傅里叶分析可以确定石墨烯片的相互方向,揭示多层石墨烯的区域,并识别涡层石墨烯。研究表明,结合RHEED、TEM和傅里叶变换对电子显微镜图像的周期性对比是一种很有前途的方法,可以分析含有石墨烯和其他碳的同素异形体修饰的纳米级碳材料的亚结构和形态。
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Morphology and structure characteristics of nanoscale carbon materials containing graphene
A comprehensive study of the nanostructured powders (graphite GSM-2; Taunit-M; thermally expanded graphite (TEG)) by methods of transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffractometry (XRD), reflection high-energy electron diffraction (RHEED), Raman spectroscopy, was carried out. The experimental XRD halo was interpreted by superimposing theoretical diffraction maxima, and an X-ray amorphous graphite phase was revealed. It was found that the X-ray amorphous phase is characterized by the limiting degree of graphite nanostructuring. From the width of the diffraction rings, the maximum sizes of graphite nanocrystals were estimated, which do not exceed 5 and 10 nm in the [0001] and [ ] directions, respectively. Carbon nanotubes and plates of turbostratic graphene were revealed. The structural and morphological parameters of the nanostructured material “Taunit-M” have been established – multi-walled nanotubes with a diameter of up to 10 nm are combined through an interlayer of X-ray amorphous carbon into flat ribbons up to 40 nm wide. Dark-field TEM images (in reflections of ) revealed moiré patterns that appear on overlapping graphene sheets due to double diffraction of the electron beam. It was found that in thermally expanded graphite, the rotation of graphene sheets ranges from 3 to 4°. Within the graphene sheets, complete dislocations with the Burgers vector b = 1/2 were revealed [1010]. The Fourier analysis of moiré images made it possible to determine the mutual orientation of graphene sheets, to reveal regions of multilayer graphene, and to identify turbostratic graphene. It is shown that the combination of RHEED, TEM, and Fourier transformations of periodic contrast of electron microscopic images is a promising approach to the analysis of the substructure and morphology of nanoscale carbon materials containing graphene and other allotropic modifications of carbon.
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