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Two-Step Synthesis of VO2 (M) with Tuned Crystallinity

Research paper by Shian Guan, Aline Rougier, Oudomsack Viraphong, Dominique Denux, Nicolas Penin, Manuel Gaudon

Indexed on: 17 Jul '18Published on: 16 Jul '18Published in: Inorganic Chemistry



Abstract

Vanadium dioxide is the key thermochromic compound for the next generation of smart windows. Monoclinic vanadium dioxide with tuned crystallinity is synthesized by a two-step thermal treatment: thermolysis of vanadyl ethylene glycolate and postannealing of the poorly crystallized VO2 powder. The proportion of crystallized VO2, calculated with the Fullprof program, increases from 44% to 79% and 100% with increasing annealing temperature up to 700 °C. Besides, V2O3 and V2O5 with particular microstructures are also successfully prepared using this method.Highly crystallized monoclinic vanadium dioxide, VO2 (M), is successfully synthesized by a two-step thermal treatment: thermolysis of vanadyl ethylene glycolate (VEG) and postannealing of the poorly crystallized VO2 powder. In the first thermolysis step, the decomposition of VEG at 300 °C is investigated by X-ray diffraction and scanning electron microscopy (SEM). A poorly crystallized VO2 powder is obtained at a strict time of 3 min, and it is found that the residual carbon content in the powder played a critical role in the post crystallization of VO2 (M). After postannealing at 500 and 700 °C in an oxygen-free atmosphere, VO2 particles of various morphologies, of which the crystallite size increases with increasing temperature, are observed by SEM and transmission electron microscopy. The weight percent of crystalline VO2, calculated using the Fullprof program, increases from 44% to 79% and 100% after postannealing. The improved crystallinity leads to an improvement in metal–insulator transition behaviors demonstrated by sharper and more intense differential scanning calorimetry peaks. Moreover, V2O3 and V2O5 with novel and particular microstructures are also successfully prepared with a similar two-step method using postannealing treatment under reductive or oxidizing atmospheres, respectively.

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