Small sized bismuth particles are prepared by an electrochemical method using a triple voltage pulse technique. The bath composition and electrochemical parameters are optimized to yield monodisperse particles. The particles have been characterized by scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, UV-visible spectroscopy and X-ray diffraction technique. The particles, as deposited, are highly crystalline in nature and the particle size and shape get tuned depending on the conditions of deposition.
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