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Use of in situ combined X-ray diffraction and X-ray absorption spectroscopy for the study of the thermal decomposition of zinc peroxide to zinc oxide is reported here. Comparison of data extracted from both X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) with thermo gravimetric analysis (TGA) enabled us to follow the nature of the conversion of ZnO2 to ZnO. A temperature range between 230 and 350 o C appears to show that a very poorly crystalline ZnO is formed prior to the formation of an ordered ZnO material. Both the decrease in white line intensity in the Zn K-edge XANES and resulting lower coordination numbers estimated from analysis of the Zn K-edge data of ZnO heated at 500 o C, in comparison to bulk ZnO, suggest that the ZnO produced by this method has significant defects in the system.

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