Synthesis of rare pure phase Ni3S4 and Ni3S2 nanoparticles in different primary amine coordinating solvents
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文摘
Two nickel(II) complexes, namely piperidine (1) and tetrahydroquinoline (2) dithiocarbamate complexes were synthesized and characterized by infra-red spectroscopy, elemental analysis and thermogravimetric analyses. The single crystal X-ray structure of complex (1) was also elucidated. The as-synthesized complexes have been utilized as single source precursors to afford nickel sulfide nanoparticles Ni3S4, Ni3S2 and mixed phases via solvothermal decomposition in oleylamine (OLA), dodecylamine (DDA) and hexadecylamine (HDA) at different temperatures. Powder X-ray diffraction studies reveal that the temperature and capping agents play a significant role in determining the crystalline structure and chemical composition of the as-synthesized nanoparticles (NPs). Electron microscopy images showed formation of nanoparticles of various shapes ranging from spherical, tetrahedral and irregular shaped morphologies. Magnetization measurements indicated that Ni3S4 nanoparticles prepared at 230 °C using DDA display ferromagnetic behaviour, while rhombohedral N3S2 also prepared at 230 °C but using HDA, displayed paramagnetic property.

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