期刊
SYNTHESIS AND REACTIVITY IN INORGANIC METAL-ORGANIC AND NANO-METAL CHEMISTRY
卷 45, 期 2, 页码 217-224出版社
TAYLOR & FRANCIS INC
DOI: 10.1080/15533174.2013.831884
关键词
dithiocarbamate; thioureide; precursor; chemical vapor deposition; powder diffraction; transmission electron microscope; semiconductor nanoparticles
Chemical vapor deposition method for the synthesis of beta-HgS (meta cinnabar) nanoparticles is reported with bis (cinnamylpiperazinedithiocarbamato)mercury(II) as the single source precursor. Crystalline structure, size, morphology and composition of the products are characterized by X-ray powder diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) analysis. PXRD shows (111), (220), (200), (311), (222), (400), (331), (420) reflections characteristic of beta-HgS nanoparticles. SEM micrographs display the spherical nature of the b-HgS nanoparticles. EDX analysis showed the presence of Hg and S. HRTEM images confirm the spherical nature of the nanoparticles with their size in the range of 5-10 nm. The results are in agreement with those estimated from the XRD pattern. XPS signals observed at 162.6, 162.8, 222.3, 99.9, and 104.1 eV are due to S-2p (3/2,S- 1/2), S-2s (1/2), and Hg-4f ((7/2, 5/2)) respectively. The precursor [Hg (cpzdtc)(2)] was synthesized and characterized by IR and NMR (H-1 and C-13). Single crystal X-ray crystallography of precursor shows the presence of HgS4 distorted tetrahedral coordination environment, with a distinct Hg-S bond asymmetry.
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