Papers by Author: Agnese Stunda

Abstract: Modification of surface morphology and composition of niobophosphate glass and glass-ceramic in the system P₂O₅-CaO-Nb₂O₅-Na₂O was investigated. Amorphous, partly crystalline and crystalline samples were prepared in shape of pellet with diameter 10 mm. Samples were treated in 1 and 5 days in citric acid at 37°C and 3h in boiling HCl. Surface morphology before and after treatment was investigated by scanning electron microscopy (SEM), phase composition by X-ray powder diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX). Glass sample was smooth, after treatment in citric acid it had cracks and pit-holes on the surface. Partly crystalline sample was smooth and contained inclusions of crystalline Ca₃(PO₄)₂ and Ca₂P₂O₇. Platy crystals of Ca₃(PO₄)₂ dissolved first, than bulky Ca₂P₂O₇. Crystalline samples contained Na₄Nb₈P₄O₃₂ and calcium phosphate phases; surface was rough before and after treatment. EDX showed that amount of phosphorous is proportional to amount of calcium and inversely proportional to amount of sodium and niobium in glass-ceramic samples.

Abstract: Phase transition during crystallization of glass to glass-ceramic in system P2O5-CaO-Nb2O5-Na2O was studied. Several heating rates were compared – 1, 2, 5, 11 and 20°Cmin-1. DTA, XRD, FTIR and Raman analyses were performed. Niobophosphate glass-ceramic is found to form utterly different crystalline phases depending on maximal heating temperature, heating rate and time of maximal temperature maintenance. Crystallization temperatures of the same phases are strongly dependent on heating rate, while crystallinity of obtained phases is not. At lower temperatures poorly crystalline phosphates (Ca3(PO4)2, Ca10Na(PO4)7, Ca2P2O7) and niobates (NaNbO3 and Nb2O5) are identified. At higher temperatures a large amount of well crystalline niobophosphate (Na4(Nb8P4O32) and Ca2P2O7 forms. With increasing amount of Na4(Nb8P4O32), amount of NaNbO3 and Nb2O5 decreases.