This study investigated the effect of synthesis time on the microstructure of Cu3BiS3 powders prepared by the polyol method. The variations in the lattice constants and crystallite size, analyzed from the X-ray diffraction patterns, were attributed to changes in the microstrain within the Cu3BiS3 samples. Field-emission scanning electron microscopy observations revealed that the average size of the spherical structures increased between 60 and 80 min, followed by a decrease at synthesis times exceeded 100 min. The size of the spherical structures and the variation in the Cu/Bi ratio, as determined by energy-dispersive X-ray spectroscopy, were affected by the synthesis time.
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