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Mercury(II) N,N′-diarylformamidine dithiocarbamates as single-source precursors for the preparation of oleylamine-capped HgS nanoparticles
Transition Metal Chemistry ( IF 1.6 ) Pub Date : 2020-05-08 , DOI: 10.1007/s11243-020-00391-y
Segun D. Oladipo , Bernard Omondi

Mercury(II) complexes of N,N′-diarylformamidine dithiocarbamate of the general formula [Hg-(L)2] (L = N,N′-bis(2,6-dimethylphenyl)formamidine dithiocarbamate L1 (1), N,N′-bis(2,6-disopropylphenyl) formamidine dithiocarbamate L2 (2), N,N′-mesityl formamidine dithiocarbamate L3 (3), N′-(2,6-dichlorophenyl-N-(2,6-dimethylphenyl) formamidine dithiocarbamate L4 (4), N′-(2,6-dichlorophenyl)-N-(2,6-diisopropylphenyl) formamidine dithiocarbamate L5 (5) and N′-(2,6-dichlorophenyl)-N-mesityl formamidine dithiocarbamate L6 (6)) have been synthesized and characterized by physicochemical and spectroscopic techniques. The molecular structures of 1, 2 and 6 were unequivocally determined using single-crystal X-ray diffraction as mononuclear species in which the Hg(II) centers are coordinated to four sulfur atoms from two dithiocarbamate ligands resulting in distorted square planar geometries. Complexes 1, 3 and 6 were used as single-source precursors to prepare mercury sulfide nanoparticles HgS1, HgS3 and HgS6 in oleylamine which acted as the solvent as well as the capping agent. HR-TEM images of HgS1, HgS3 and HgS6 particles are nanospherical in shape with size distribution between 5 and 16 nm. Powder XRD pattern confirmed the β phase (metacinnabar) of HgS in all the nanoparticles with an average crystallite size similar for HgS1 and HgS3, 9.35 and 9.46 nm, respectively, and smaller crystallite sizes, 5.15 nm for HgS6. The optical properties information obtained from the UV–visible and photoluminescence spectra of the HgS nanoparticles showed evidence of quantum confinement.

中文翻译:

汞 (II) N,N'-二芳基甲脒二硫代氨基甲酸酯作为单源前驱体用于制备油胺封端的 HgS 纳米粒子

图 2 和图 6 是使用单晶 X 射线衍射作为单核物质明确确定的,其中 Hg(II) 中心与来自两个二硫代氨基甲酸酯配体的四个硫原子配位,导致方形平面几何形状扭曲。配合物 1、3 和 6 用作单源前驱体,在作为溶剂和封端剂的油胺中制备硫化汞纳米颗粒 HgS1、HgS3 和 HgS6。HgS1、HgS3 和 HgS6 颗粒的 HR-TEM 图像呈纳米球形,尺寸分布在 5 到 16 nm 之间。粉末 XRD 图案证实了所有纳米粒子中 HgS 的 β 相(metacinnabar),HgS1 和 HgS3 的平均晶粒尺寸分别为 9.35 和 9.46 nm,而 HgS6 的晶粒尺寸更小,为 5.15 nm。
更新日期:2020-05-08
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