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Synthesis and characterization of single- and few-layer mica nanosheets by the microwave-assisted solvothermal approach

机译:微波辅助溶剂热法合成单层和多层云母纳米片及表征

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摘要

We have successfully fabricated single- and few-layer mica nanosheets, by means of using a solvothermal method in conjunction with a microwave irradiated expansion process. In the solvothermal process, dissolved potassium ions were intercalated onto the interlayer space of the mica. Following this, microwave irradiation facilitates the exfoliation of individual nanosheets. The synthesized products were characterized by field emission scanning electron microscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction, x-ray photoelectron spectroscopy (XPS), and Raman spectroscopy measurements. AFM and TEM studies claimed the existence of single-layer mica. High-resolution TEM (HR-TEM) investigations revealed that the exfoliated product corresponded to a crystalline mica structure, being comprised of Si, Al, O, and K elements. XPS spectra exhibited the major constituent peaks, including O 1s, Si 2p, Al 2p, and K 2p. In addition, C atomic concentration has been slightly increased by the contamination during exfoliation, presumably due to the increase of the exposed mica surface. The C 1s XPS spectra revealed that the C-C bonding in organic surface contaminants was broken, whereas the Si-C bonding was enhanced, by the exfoliation process. The O 1s XPS spectra revealed that the Si-O bonding in mica was broken, generating the O-Si-C bonding. This study paves the way towards the fabrication of single- or few-layer inorganic nanosheets of desired materials, via a convenient and efficient route.
机译:我们已经成功地通过使用溶剂热法结合微波辐照膨胀工艺成功地制备了单层和多层云母纳米片。在溶剂热过程中,溶解的钾离子插入到云母的层间空间中。此后,微波辐照促进单个纳米片的剥离。通过场发射扫描电子显微镜,透射电子显微镜(TEM),原子力显微镜(AFM),X射线衍射,X射线光电子能谱(XPS)和拉曼光谱测量来表征合成的产物。 AFM和TEM研究声称存在单层云母。高分辨率TEM(HR-TEM)研究显示,剥落的产品对应于晶体云母结构,由Si,Al,O和K元素组成。 XPS光谱显示出主要的组成峰,包括O 1s,Si 2p,Al 2p和K 2p。另外,由于剥落过程中的污染,碳原子浓度略有增加,这可能是由于暴露的云母表面增加所致。 C 1s XPS光谱显示,通过剥落过程,有机表面污染物中的C-C键被破坏,而Si-C键被增强。 O 1s XPS光谱表明,云母中的Si-O键断裂,产生了O-Si-C键。这项研究为通过方便有效的途径制备所需材料的单层或多层无机纳米片铺平了道路。

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