The purpose of this study is to elucidate the nature of the phase transformations of lead monoxide powder. Lead monoxide is prepared by calcination of a lead oxalate precursor salt, and its phase transformations are studied using X-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TG). Analysis reveals that the phase transformations observed for oxalate-derived lead monoxide powder are highly dependent on the firing atmosphere. In nitrogen, as the temperature is increased 1 deg/min from room temperature, lead monoxide undergoes a reconstructive litharge-to-massieot phase transformation in a temperature range of 525-575~ In air, litharge, metastable at room temperature, slowly oxidizes to the Pb304 phase at a temperature of 350~ and rapidly reduces to litharge at 560~ At temperatures greater than 560~ litharge converts to massieot. With heating rates of 10 deg/min or higher, formation of Pb304 is not observed.
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