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In Situ Synchrotron XRD Study of the Pr–Ce–Ni–O System

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Abstract

Samples of the Pr–Ce–Ni–O system with Ce content relative to Pr: 5, 25, 50 mol % were synthesized by a modified Pechini method and studied using in situ synchrotron XRD in the temperature range of 30–700–30°C first in an inert gas flow then in a synthetic air flow. The formation of a first-order Ruddlesden–Popper phase, as well as two cubic fluorite-type phases, was observed for a 5 mol % Ce : Pr sample. A sample with 25 mol % Ce : Pr comprised two fluorite phases. During heating in an inert gas flow, reversible Pr7O12-type phase formation was observed from some part of the fluorite phases. A sample with 50 mol % Ce : Pr comprised a single fluorite phase that turned out to be inhomogeneous with some close cation content distribution, which could be seen in the oxygen incorporation region upon heating in a synthetic air flow after thermocycling in an inert gas flow. It is seen under these conditions since the fluorite lattice parameter is sensitive to oxygen release (a sharp increase in the lattice parameters) and oxygen incorporation (a sharp decrease in the lattice parameters).

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Funding

This work was supported by the Ministry of Science and Higher Education of the Russian Federation within the governmental order for Synchrotron radiation facility SKIF, Boreskov Institute of Catalysis.

The synchrotron in situ XRD experiments were done at the Shared Research Center SSTRC on the basis of the VEPP-4 – VEPP-2000 complex at BINP SB RAS.

The XRD study using a Bruker D8 Advance diffractometer was carried out using facilities of the shared research center “National center of investigation of catalysts” at Boreskov Institute of Catalysis.

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Authors and Affiliations

  1. Synchrotron Radiation Facility SKIF, Boreskov Institute of Catalysis, SB RAS, 630559, Koltsovo, Russia

    D. D. Mishchenko & A. N. Shmakov

  2. Boreskov Institute of Catalysis, SB RAS, 630090, Novosibirsk, Russia

    M. V. Arapova

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  1. D. D. Mishchenko
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  2. M. V. Arapova
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  3. A. N. Shmakov
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Correspondence to D. D. Mishchenko.

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Mishchenko, D.D., Arapova, M.V. & Shmakov, A.N. In Situ Synchrotron XRD Study of the Pr–Ce–Ni–O System. J. Surf. Investig. 17, 1302–1312 (2023). https://doi.org/10.1134/S1027451023060137

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  • DOI: https://doi.org/10.1134/S1027451023060137

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