Phase Transformation of Metastable ZnSnO 3 Upon Thermal Decomposition by In‐Situ Temperature‐Dependent Raman Spectroscopy

Temperature‐dependent in‐situ Raman spectroscopy is used to investigate the phase transformation of zinc metastannate (ZnSnO 3 ) to zinc orthostannate (Zn 2 SnO 4 ) induced upon annealing in the ambient. ZnSnO 3 microcubes ( MC s) were synthesized at room temperature using a simple aqueous synthesis process, followed by characterization using electron microscopy, X‐ray diffraction ( XRD ), Fourier transform infrared ( FTIR ) spectroscopy, and thermogravimetric analysis ( TGA ). Annealing of the ZnSnO 3 MC s was carried out up to 1000°C, while recording the Raman spectra in‐situ at regular intervals. Phase transformation from metastannate to orthostannate was found to begin around 500°C with an activation energy of ~0.965 eV followed by the recrystallization into the inverse spinel orthostannate phase at ~750°C. Results from this study provide detailed understanding of the phase transformation behavior of perovskite ZnSnO 3 to inverse spinel Zn 2 SnO 4 upon thermal annealing.