Thermal Stability of Quasi-1D NbS₃ Nanoribbons and Their Transformation to 2D NbS₂: Insights from in Situ Electron Microscopy and Spectroscopy

In situ electron microscopy imaging and spectroscopy enabled us to study the evolution of quasi-1D NbS3-IV nanoribbons with respect to morphology and chemical structure at temperatures between room temperature and 1000 °C. Scanning transmission electron microscopy (STEM) experiments included imaging in the secondary electron, (transmitted) bright field, and high-angle annular dark-field modes while operating in the low kV regime. The results showed that NbS3-IV samples transform dramatically from smooth nanoribbons into highly textured configurations featuring polyhedral divots and steps. Similar in situ heating experiments conducted with aberration-corrected STEM revealed that bilayers of NbS3-IV chains convert topotactically into aligned 2H-NbS2 sheets upon loss of sulfur. Atomic resolution imaging, fast Fourier transform analysis, and electron energy loss spectroscopy confirmed these chemical changes, from which we propose an atomistic mechanism for the NbS3-IV → 2H-NbS2 conversion.