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We report the synthesis of tetragonal β-In2S3nanoparticles (NPs). The present approach is intended to produce volatile side products to achieve organic molecule-free NPs for better optoelectronic applications. The obtained NPs possess a bulk tetragonal structure with an average size of 8.08 ± 3.76 nm. The expected quantum confinement was observed in a spectrochemically determined band gap (2.45 eV). A surprising finding is that these NPs showed a broad solid state emission (500–800 nm) with a FWHM of 197 nm.
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