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.