Cadmium(II) thiosemicarbazone complexes were prepared and characterized by elemental analysis and IR and NMR spectroscopy. The complexes were then investigated as potential single‐source precursors for the synthesis of oleylamine‐capped cadmium sulfide nanoparticles by solvothermal decomposition. The resulting nanomaterials were characterized by powder XRD, TEM, HRTEM, energy‐dispersive X‐ray analysis, and UV/Vis spectroscopy. Peak broadening in the XRD patterns confirmed the presence of relatively small hexagonal CdS nanocrystals. The TEM studies evidenced that the chlorido precursors produced CdS nanostructures whose morphologies differed from those obtained from the iodido precursors. CdS nanoparticles in the form of cubes/spheres/rods and nanodendrite structures were obtained from CdCl2 and CdI2 thiosemicarbazone complexes, respectively. The UV/Vis spectra revealed that the as‐synthesized CdS nanoparticles exhibited a quantum effect due to their sharp band edges, which are blueshifted relative to those of bulk CdS. The size, morphology and shape of the nanoparticles were also shown to depend on the temperature of formation.

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Cubic Co 9 S 8 and hexagonal CoS nanocrystallites were prepared by pyrolysis and solvothermal decomposition methods using Co(LH) 2 Cl 2 and CoL 2 (where LH = thiosemicarbazones of furfuraldehyde, cinnamaldehyde and 4-fluoro-acetophenone) as single-source precursors. These nanocrystallites were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), selected area electron diffraction, UV-Vis, PL and Raman spectroscopic techniques. From TEM images, the average grain size of asprepared cobalt sulphide nanocrystallites was found to be 7-10 nm. Depending on experimental conditions, various morphologies such as spherical, pyramidal, hollow spheres, etc. are observed in the TEM images.

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