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Synthesis and characterization of rare earth borophosphates

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2004
Özdil, Yasemin
In this thesis, solid state reactions of Ln2O3, Y2O3, B2O3 and (NH4)2HPO4 were investigated to synthesize LnBP2O8 (Ln= Dy, Ho, Er) and YBP2O8 type of borophosphates which were not reported before. The products were analyzed by XRD, IR, DTA, SEM and EDX methods. In the first part of this thesis, synthesis of YBP2O8 through the solid state reaction of Y2O3 + 4(NH4)2HPO4 + B2O3 have been studied in the range 800-1140 °C. Orthophosphates of Dysprosium, Holmium, Erbium and Yttrium have tetragonal xenotime (YPO4) or zircon (ZrSiO4) structure. Examination of X-ray powder diffraction data at 1140 ðC showed that the obtained structure was xenotime type together with weak BPO4 and Y(PO3)3 lines. The formula was calculated as YBxP1+xO4+4x through EDX and XRD data. The pattern was indexed in tetragonal system with the unit cell parameters of a= 6.8863, c= 6.016 Å and s.g. is I41/amd. In the second part of this research, synthesis of LnBP2O8 through the solid state reaction of Ln2O3 + 4(NH4)2HPO4 + B2O3 (Ln= Dy, Ho, Er) have been studied in the range 800-1200 ðC. At 1200 ðC DyBP2O8 was obtained with tetragonal structure with the unit cell parameters of a= 6.905, c= 6.051 Å and s.g. I41/amd. Using the same procedure HoBP2O8 was obtained at 1100-1200 ðC and the XRD pattern was indexed in tetragonal system with the unit cell parameters of a= 6.887, c= 6.024 Å and s.g. I41/amd. In the structural analysis of ErBP2O8 obtained by the same reaction, the system was found as tetragonal and was indexed with a= 6.849, c= 5.998 Å and s.g. I41/amd. Examination of the unit cell parameters with respect to ionic radius showed that the unit cell parameters decrease depending on the lanthanide contraction. The structures of the compounds obtained throughout this thesis were examined by IR spectroscopy and relation between the spectra and IR vibrational modes were established. The presence of