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Thermal synthesis and structural characterization of the orthorhombic Th2(PO4)(P3O10)

AuthorsGarcía-Glez, Jorge; Alfonso, Belén F.; Huidobro, José A.; Khainakov, Sergei ; Castro, Germán R. ; Trobajo, Camino
Thorium phosphate-triphosphate
Thermal decomposition
Issue Date2014
CitationJournal of Thermal Analysis and Calorimetry 118(2): 759-765 (2014)
AbstractPolycrystalline thorium(IV) phosphate-triphosphate, Th2(PO4)(P3O10) (1), was obtained by (NH4)2Th(PO4)2·H2O (2) heating from room temperature to 1,273 K. 1 crystallizes in the orthorhombic space group Pn21 a (a = 11.6846(2) Å, b = 7.1746(1) Å, c = 12.9320(3) Å, Z = 4). Combining powder synchrotron X-ray diffraction data and DFT geometry optimization, a structural model is proposed for 1. The structure is built on ThO8 polyhedral chains along the b-axis. PO4 3− and P3O10 5− groups coexist in the structure and the latter group forms non-linear chains. Cohesion of the structure is made by the linkage of ThO8 chains by PO4 and P3O10 groups. Thermal transformation from 2 to 1 was monitored by thermogravimetric analysis (activation energy as a function of the extent of conversion was obtained from Kissinger–Akahira–Sunose (KAS) isoconversional method) and powder X-ray thermo-diffraction. For 2, the dehydration process takes place in two steps, with the apparition of a layered intermediate phase, (NH4)2Th(PO4)2·nH2O (0 < n < 1, d = 6.42 Å), previously to the formation of (NH4)2Th(PO4)2 (d = 6.31 Å). The condensation process produces an amorphous material that crystallizes to α-ThP2O7 (3) when the temperature increases. At 1,273 K, 3 slowly transforms to 1.
Identifiersdoi: 10.1007/s10973-014-3922-0
issn: 1388-6150
e-issn: 1572-8943
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