Novel Method for Synthesis of Well-Crystallized Vanadyl(2+) Hydrogen Phosphate Hemihydrate: Crystallization in Organic Media Containing a Small Amount of Water |
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Authors: | Hiroshi Kominami Kentarou Matsuo Yoshiya Kera |
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Affiliation: | Department of Applied Chemistry, Faculty of Science and Engineering, Kinki University, Higashiosaka, Osaka 577-8502, Japan |
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Abstract: | Vanadyl(2+) hydrogen phosphate hemihydrate (VOHPO40.5H2O, VHP) that had high crystallinity and showed a strong (001) peak in its X-ray diffractometry (XRD) pattern was synthesized via thermal treatment of a mixture of vanadyl(2+) acetylacetonate and triethyl phosphate at 200°C in organic solvents that contained a small amount of water. Scanning electron microscopy observations revealed that the product consisted of thin plates (2-4 µm wide and <0.5 µm thick). When the reaction was conducted at 250°C, a VHP sample was formed that exhibited stronger XRD peaks and had a plate width of >20 µm. The present VHP sample was topotactically transformed to divanadyl(2+) pyrophosphate, which showed a strong (020) XRD peak, via thermal treatment in a nitrogen atmosphere at 500°C. |
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