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Synthesis of VO2 Nanopowders. Part II. Hydrolysis of Vanadium Alkoxide/Citric Acid Premixes: VO2 Nanostructures of Controlled Shape

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Abstract

Reaction of VO(OiPr)3/citric acid premixes with excess water produces stable, blue dispersions of VxOy gel nanoparticles (5–100 nm in diameter) that can be isolated via acetone precipitation. Annealing under reducing conditions transforms these gel particles into crystalline, faceted VO2 nanoparticles of similar size. Larger VxOy gel particles (75–200 nm in diameter) form when VxOy nanogel dispersions are aged with aqueous ammonia. Upon annealing, these larger gel particles transform into crystalline VO2 rods of 50 nm–10 μm in length. Hysteresis loops confirming a semiconductor-to-metal phase transition near 68 °C expected for crystalline VO2 particles are recorded by variable-temperature electrical resistance and powder X-ray diffraction measurements.

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Acknowledgments

Financial support from the National Science Foundation (No. DMR-0210785) and an industrial sponsor is gratefully acknowledged by C.M.L. We also thank the Vanderbilt University Institute for Integrative Biosystems Research and Education for fabrication of the IDA micro-electrode used in this study. A.G.H. acknowledges support by the National Science Foundation Graduate Research Fellowship under Grant No. DGE 0909667. Partial support by the National Science Foundation Tennessee Solar Conversion and Storage using Outreach, Research and Education (TN-SCORE) under NSF EPS 1004083 is also acknowledged.

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Correspondence to Charles M. Lukehart.

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Morris, W.H., Harris, A.G. & Lukehart, C.M. Synthesis of VO2 Nanopowders. Part II. Hydrolysis of Vanadium Alkoxide/Citric Acid Premixes: VO2 Nanostructures of Controlled Shape. J Clust Sci 25, 323–334 (2014). https://doi.org/10.1007/s10876-013-0670-4

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