Summary: | Indium selenides (In<sub><i>x</i></sub>Se<sub><i>y</i></sub>) have been shown to retain several desirable properties, such as ferroelectricity, tunable photoluminescence through temperature-controlled phase changes, and high electron mobility when confined to two dimensions (2D). In this work we synthesize single-layer, ultrathin, subnanometer-wide In<sub><i>x</i></sub>Se<sub><i>y</i></sub> by templated growth inside single-walled carbon nanotubes (SWCNTs). Despite the complex polymorphism of In<sub><i>x</i></sub>Se<sub><i>y</i></sub> we show that the phase of the encapsulated material can be identified through comparison of experimental aberration-corrected transmission electron microscopy (AC-TEM) images and AC-TEM simulations of known structures of In<sub><i>x</i></sub>Se<sub><i>y</i></sub>. We show that, by altering synthesis conditions, one of two different stoichiometries of sub-nm In<sub><i>x</i></sub>Se<sub><i>y</i></sub>, namely InSe or β-In<sub>2</sub>Se<sub>3</sub>, can be prepared. Additionally, <i>in situ</i> AC-TEM heating experiments reveal that encapsulated β-In<sub>2</sub>Se<sub>3</sub> undergoes a phase change to γ-In<sub>2</sub>Se<sub>3</sub> above 400 °C. Further analysis of the encapsulated species is performed using X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), energy dispersive X-ray analysis (EDX), and Raman spectroscopy, corroborating the identities of the encapsulated species. These materials could provide a platform for ultrathin, subnanometer-wide phase-change nanoribbons with applications as nanoelectronic components.
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