Characterization of Cu3SnS4 Nanoparticles and Nanostructured Flowers Synthesized by a Microwave-Refluxing Method

Cu3SnS4 nanoparticles and nanostructured flowers were synthesized by 100, 300, 600, and 800 W microwave refluxing of the mixture containing 3 mmol CuCl2 center dot 2H(2)O, 1 mmol SnCl2 center dot 2H(2)O, and 4 mmol thiosemicarbazide (NH2NHCSNH2) in 50 ml ethylene glycol (HOCH2CH2OH). X-ray diffraction (XRD), selected area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS), scanning and transmission electron microscopy (SEM and TEM), Raman analysis, and photoluminescence (PL) spectrophotometry revealed the morphology transformation of pure tetragonal Cu3SnS4 with nanoparticles at 100 W into three-dimensional (3D) hierarchical flower-like structure at 800 W, including the presence of 2Cu(+), Cu2+, Sn4+, and 4S(2-) containing in the sulfide, the PL emission of the 3D hierarchical flower-like Cu3SnS4 at 366 nm, and the prominent Raman peak of Cu-Sn vibration at 319 cm(-1). In this research, a formation mechanism was also proposed according to the experimental results. (C) 2013 The Japan Society of Applied Physics