X-Ray fluorescence analysis of paraniobate based ceramics of composition Y_3–xYb_xNbO₇

Abstract

A two-stage technique for X-ray fluorescence analysis of ceramic samples of composition Y3–xYbxNbO7 (where x = 0 – 3) has been developed. At the first stage, using the method of fundamental parameters (FPM), a rapid semi-quantitative analysis of ceramic samples and products of intermediate synthesis was carried out to determine their preliminary composition. At the second stage, the quantitative composition of the samples was determined using the constructed calibration dependencies. To construct calibration dependencies a series of reference samples containing 3.16 – 56.55% Y, 8.78 – 71.0% Yb, and 12.83 – 19.70% Nb was synthesized using a method similar to that used for preparation of the ceramic samples under study. Analytical lines of elements free from spectral overlaps and XRF conditions (current and voltage of an X-ray tube, exposure time, method of taking into account the background near the analytical line) were selected. The relative standard deviation of the results of Y, Yb, and Nb determination in ceramic samples did not exceed 0.66%, the relative error was no more than 1.63%. The results obtained were compared with the calculated content of analytes in the samples of stoichiometric composition and with the results of ICP-AES analysis of real ceramic samples. The developed technique provides determination of the main components of ceramic samples and can be used for analytical control of synthesis of rare earth paraniobates.