One‐Pot Approach for Metastable Orthorhombic AgInS 2 ‐Based Nanostructures with Excellent Photoluminescence Property

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The photoluminescence (PL) properties of metastable I‐III‐VI nanoparticles, such as the orthorhombic ( o ‐)AgInS 2 have suffered from the giant Stokes shifts, spectral broadening, and low PL quantum yield (PLQY) due to their large size and rich defect states. Herein, a novel one‐pot approach under atmospheric conditions was developed by heating the [Ag((C 4 H 9 ) 2 NCS 2 )] ([AgR]), [In((C 4 H 9 ) 2 NCS 2 ) 3 ] ([InR 3 ]) and zinc stearate (ZnSt 2 ) with molar ratio of 2:1:1 in 1‐dodecanethiol (DDT) and dodecane for the metastable o ‐AgInS 2 based nanostructures with intense, narrow and steady red PL emission. Such nanostructures exhibited relatively narrow full width at half maximum (FWHM) of 87 nm and high absolute PLQY of 53% at 659 nm among the reported o ‐AgInS 2 ‐based nanomaterials. The excellent PL property could be attributed to the high quality of the products without the Ag 2 S and surface oxidation. The growth mechanism was elucidated that the sequential decomposition of precursors with DDT led to the formation of amorphous Ag 2 S nanoparticles first, then the seeded growth mechanism led to the Ag 2 S‐AgInZn x S 2+ x heteronanostructrures, and finally led to the luminescent o ‐AgInS 2 ‐based nanostructures ( o ‐AgInS 2 ‐dominated nanoparticles and AgInS 2 ‐AgInZn x S 2+ x heteronanorods) and nonluminous Ag 2 S‐ o ‐AgInS 2 ‐AgInZn x S 2+ x heteronanoparticles, which were separated by centrifugation due to their different sizes, structures, and densities.