We present a novel, straightforward, and reproducible one-pot heating up technique to synthesize core/crown SnSe/SnS nanosheets by a careful adjustment of the sulfur and selenium precursor reactivity. Here, the SnSe nanosheets are prepared via a wet-chemical route using SnCl2 and selenium phosphines. By adding a highly reactive S-oleylamine complex during the growth of the SnSe sheets at 240 °C, SnS crowns were formed within the SnSe sheets. The number of SnS crowns can be tailored upon repeated addition of S-oleylamine. A combination of transmission electron microscopy, high-resolution transmission electron microscopy, atomic force microscopy, scanning transmission electron microscopy, and energy-dispersive X-ray spectroscopy proves the formation of highly crystalline core/crown structures.
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