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Thermal and X-ray diffraction analysis studies during the decomposition of ammonium uranyl nitrate
Kim, B. H.,Lee, Y. B.,Prelas, M. A.,Ghosh, T. K. Springer Netherlands 2012 Journal of radioanalytical and nuclear chemistry Vol.292 No.3
<P>Two types of ammonium uranyl nitrate (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O and NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB>, were thermally decomposed and reduced in a TG-DTA unit in nitrogen, air, and hydrogen atmospheres. Various intermediate phases produced by the thermal decomposition and reduction process were investigated by an X-ray diffraction analysis and a TG/DTA analysis. Both (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O and NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> decomposed to amorphous UO<SUB>3</SUB> regardless of the atmosphere used. The amorphous UO<SUB>3</SUB> from (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O was crystallized to γ-UO<SUB>3</SUB> regardless of the atmosphere used without a change in weight. The amorphous UO<SUB>3</SUB> obtained from decomposition of NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> was crystallized to α-UO<SUB>3</SUB> under a nitrogen and air atmosphere, and to β-UO<SUB>3</SUB> under a hydrogen atmosphere without a change in weight. Under each atmosphere, the reaction paths of (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O and NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> were as follows: under a nitrogen atmosphere: (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB> → NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → γ-UO<SUB>3</SUB> → U<SUB>3</SUB>O<SUB>8</SUB>, NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → α-UO<SUB>3</SUB> → U<SUB>3</SUB>O<SUB>8</SUB>; under an air atmosphere: (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB> → NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → γ-UO<SUB>3</SUB> → U<SUB>3</SUB>O<SUB>8</SUB>, NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → α-UO<SUB>3</SUB> → U<SUB>3</SUB>O<SUB>8</SUB>; and under a hydrogen atmosphere: (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·2H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB>·H<SUB>2</SUB>O → (NH<SUB>4</SUB>)<SUB>2</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>4</SUB> → NH<SUB>4</SUB>UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → γ-UO<SUB>3</SUB> → α-U<SUB>3</SUB>O<SUB>8</SUB> → UO<SUB>2</SUB>, NH<SUB>4</SUB> UO<SUB>2</SUB>(NO<SUB>3</SUB>)<SUB>3</SUB> → A-UO<SUB>3</SUB> → β-UO<SUB>3</SUB> → α-U<SUB>3</SUB>O<SUB>8</SUB> → UO<SUB>2</SUB>.</P>