In the present work, we have synthesized p-type copper antimony selenide (Cu 3 SbSe 4 ) thin films in an aqueous alkaline medium using a microwave assisted synthesis technique. The deposited thin films were characterized by UV-Vis-NIR spectroscopy, X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and thermoelectric techniques. On the basis of experimental results, a possible reaction mechanism has been discussed in detail. The band gap of the as deposited film is 1.94 eV and after annealing it reaches 1.87 eV for Cu 3 SbSe 4 . XRD results indicate that the as deposited thin films of CuSbSe 2 have an orthorhombic crystal structure with secondary mixed phases and after annealing this is converted to Cu 3 SbSe 4 having a pure tetragonal crystal structure. FESEM micrographs of Cu 3 SbSe 4 showed a spherically diffused granular morphology having an average grain size of 25 nm. The HRTEM result of Cu 3 SbSe 4 shows good crystallinity with a lattice spacing of 0.327 nm along the (112) plane. The EDS spectrum shows the presence of Cu, Sb and Se elements. The thermoelectric figure of merit (ZT) of the as deposited film is calculated to be 0.059 at 300 K and that of annealed Cu 3 SbSe 4 is found to be 0.141 at 300 K.

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The improvement of the thermoelectric performance of semiconducting chalcogenides is an important task. The principal challenge in this field is to tailor the thermoelectric properties, such as electrical conductivity, Seebeck coefficient, and thermal conductivity, to improve the figure of merit (ZT). Herein, we present an improvement in the thermoelectric properties of InIII‐doped p‐type Cu3SbSe4 thin films deposited by using a microwave‐assisted technique. The deposited thin films were characterized for their optical, structural, morphological, compositional, and electrical transport properties to show the applicability of the materials in thermoelectric energy conversion. The improvement in ZT is achieved with InIII doping because of the enhancement in the charge carrier density of Cu3SbSe4 thin films. A maximum ZT of 0.183 was achieved for Cu3(Sb0.94In0.06)Se4 at 300 K. Our results show that this deposition strategy and doping process can provide an effective solution to fabricate Cu3SbSe4‐based materials for thermoelectric applications.