This paper presents, for the first time, the nanocrystalline, semiconducting antimony selenoiodide (SbSeI) grown in multi-walled carbon nanotubes (CNTs). It was prepared sonochemically using elemental Sb, Se, and I in the presence of ethanol under ultrasonic irradiation (35 kHz, 2.6 W/cm2) at 323 K for 3 h. The CNTs filled with SbSeI were characterized by using techniques such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, high-resolution transmission electron microscopy, selected area electron diffraction, and optical diffuse reflection spectroscopy. These investigations exhibit that the SbSeI filling the CNTs is single crystalline in nature and in the form of nanowires. It has indirect allowed energy band gap EgIf=1.61(6) eV.

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