Synthesis of iron borophosphates and phosphates with zeo-type structures

Tuncel, Selcan
New iron phosphate and borophosphate compounds were synthesized and characterized by single crystal/powder X-ray diffraction, infrared spectroscopy, raman spectroscopy, thermogravimetric analysis, electron microscopy and elemental analysis. Using several compositions, Fey B(PO4)x type of compounds were attempted to be prepared by solid state reactions. The solid state reactions of boron compounds with a phosphating agent has been completed at 950oC. A new product Fe2BP3O12 is synthesized and indexed in this work which is isostructural with Cr2 BP3O12 A single crystal of iron ammonium phosphate, (NH4)3-xHxFeP3O12, was synthesized by a hydrothermal method and characterized. Its X-ray powder diffraction pattern was indexed in orthorhombic system. The unit cell parameters were found to be as a = 7.775 (A), b = 7.445(A), c = 14.331(A) The compound with the formula NH4FeBP2O8OH was synthesized by hydrothermal method. Its X-ray powder diffraction pattern was indexed in monoclinic system. The unit cell parameters were found to be a = 9.336, b = 8.278, c =9.642A, and x = 101.60o, which are good agreement with the literature values. Ferro-axinite type of compound was discovered as single crystals resembling the axinite mineral. The compound was indexed in triclinic system with the unit cell parameters of a = 7.167, b = 8.840 , c = 9.455A, a = 64.83o, d = 64.83o, ? = 69.42o. A zeotype Fe(H2O)2BP2O8.H2O, which was obtained by hydrothermal methods before, was synthesized by a precipitation method using different initial reactant. In this case, instead of Fe+2, Fe+3 compound was used as a reactant. All the compounds have been investigated by FTIR spectroscopy and the assignments of the functional BO3, BO4 and PO4 groups have been done.


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Citation Formats
S. Tuncel, “Synthesis of iron borophosphates and phosphates with zeo-type structures,” M.S. - Master of Science, Middle East Technical University, 2004.