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In-situ monitoring of vanadium dioxide formation using high-temperature XRD

Rodriguez, Marko A.; Bell, Nelson S.; Griego, James J.M.; Edney, Cynthia E.; Clem, Paul G.

The monoclinic-to-tetragonal phase transition (∼70 °C) in vanadium dioxide (VO2) strongly impacts the infrared properties, which enables its use in applications such as smart window devices. Synthesis of VO 2 can be challenging due to the variability of vanadium oxide phases that may be formed. We have employed high-temperature X-ray diffraction (HTXRD) to monitor the reaction process of vanadium oxide precursor powders to form the desired tetragonal VO2 phase. Single-phase tetragonal VO2 was formed within 30 min at 420 °C in flowing N2 gas (∼50 ppm O2). The monoclinic-to-tetragonal phase transformation was observed via HTXRD at ∼70 °C with the typical ∼10 °C hysteresis (i.e. approached from above or below the transition). © International Centre for Diffraction Data 2014.