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Prospects of electron probe X-ray microanalysis techniques for composition determination of nanosized lead zirconate-titanate films


I.P. Pronin, E.Yu. Kaptelov, S.V. Senkevich, E.Yu. Flegontova, V.P. Pronin, D.M. Dolgintsev

This paper deals with the assessment of possibilities of the electron-probe X-ray microanalysis to determine the composition of practically significant oxide films of lead zirconate titanate PZT of submicron and nanoscale thicknesses. RF magnetron sputtered PZT films were formed on the Pt/SiO2/Si (SiO2/Si) substrates using two-stage technology. The films were deposited at a temperature nearly of 150°C and then heat treated at high temperatures in the range of 530...570oC. The elemental composition of the films was analyzed in the thickness range 100-700 nm. The measurements were performed on a scanning electron microscope EVO-40 attached with energy dispersive analizer INCA. It is shown that the accuracy of the content elements of the films did not exceed 2.5%. With decreasing thickness of less than 300-400 nm, PZT films were manifested size effects, which lead to a distortion in the composition of the films. It is shown that the observed effects are caused, in particular, by the difference in absorption coefficients for various lengths of x-rays and the difference in the threshold energies of deep levels of the atoms the film. The presence of a platinum sublayer on the surface of SiO2/Si substrate increased the distortions in determining the composition of the films. For the two energies of the incident electron beam is correction curves are constructed, you can use to recover the actual composition of the films of different thicknesses. It was found that during high temperature annealing at 550 ... 570 °C the main losses of lead in PZT films occur at the interfaces during as the crystallization of perovskite phase from the pyrochlore phase and perovskite phase recrystallization. The cause of increased migration capacity of lead oxide at the interfaces is the formation of multiple nanopores on the phase borders
May 29, 2020

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