Synthesis and characterization of gallium(III) dithiocarbamates as suitable nano-gallium(III) sulfide precursors

Abstract

Gallium(III) complexes [Ga(chmdtc) 3 ] (1) and [Ga(chedtc) 3 ] (2) (where chmdtc=cyclohexylmethyldithiocarbamate and chedtc=cyclohexylethyldithiocarbamate) have been prepared and characterized by infrared, nuclear magnetic resonance ( 1 H and 13 C) spectra, thermogravimetry, X-ray photoelectron spectroscopy, and single crystal X-ray diffraction (XRD). The thermogravimetric curves obtained for both complexes are almost similar. The final residue corresponded to gallium sulfide (Ga 2 S 3) above 700°C for complexes (1) and (2). In the single crystal X-ray structure of [Ga(chedtc) 3 ] (2), Ga-S bonds, and the associated C-S bonds show asymmetry as a requirement of packing. The complex shows distorted octahedral geometry due to its bite angle variations. Nano-α-Ga 2 S 3 was prepared from single source precursors [Ga(chmdtc) 3 ] (1) and [Ga(chedtc) 3 ] (2). Prepared nano-Ga 2 S 3 have been characterized by powder XRD, energy-dispersive X-ray spectroscopy technique, and transmission electron microscopy (TEM)-selected area electron diffraction analysis showing the nano-sized nature of Ga 2 S 3. TEM micrographs confirmed the size of the particles to be 50 nm.