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In situ Raman and Time-Resolved Luminescence Investigation of the Local Structure of ZrO2 in the Amorphous to Crystalline Phase Transition

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    In situ Raman and Time-Resolved Luminescence Investigation of the Local Structure of ZrO2 in the Amorphous to Crystalline Phase Transition
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    † National Institute for Laser, Plasma and Radiation Physics, P.O. Box MG-36, RO 76900, Bucharest-Magurele, Romania
    ‡ University of Bucharest, Department of Chemical Technology and Catalysis 4 − 12 Regina Elisabeta Bvd., Bucharest 030016, Romania
    § National Institute for Laser, Plasma and Radiation Physics, Instituto de Química Avanzada de Cataluña, Consejo Superior de Investigaciones Científicas (IQAC-CSIC), CIBER en Biotecnología, Biomateriales y Nanomedicina (CIBER BBN), Jordi Girona 18-26, 08034 Barcelona, Spain
    ∥ Centro de Investigación en Materiales Avanzados, S. C. (CIMAV), Unidad Monterrey, GENES-Group of Embedded Nanomaterials for Energy Scavenging, Alianza Norte 202, Parque de Investigación e Innovación Tecnológica, 66600 Apodaca, Nuevo León, Mexico
    ⊥ Kungliga Tekniska Högskolan (KTH), School of Chemistry, Div. of Chemical Technology, Teknikringen 42, SE-10044, Stockholm, Sweden
    *E-mail: [email protected]
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    The Journal of Physical Chemistry C

    Cite this: J. Phys. Chem. C 2012, 116, 31, 16776–16783
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    https://doi.org/10.1021/jp3040538
    Published June 5, 2012
    Copyright © 2012 American Chemical Society
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    Abstract

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    The local structure of europium doped and impregnated ZrO2 in the amorphous state and during crystallization is investigated by in situ X-ray diffraction and in situ Raman, high-resolution transmission electron microscopy (HRTEM) and time-resolved photoluminescence spectroscopy. From Raman spectra excited at three different wavelengths (λex= 488, 514, and 633 nm), both phonon modes of ZrO2 and photoluminescence (PL) corresponding to europium electronic transitions were investigated. In the as-synthetized state, samples were X-ray and Raman amorphous with few tetragonal (also monoclinic) crystallites being observed under HRTEM microscopy. In situ XRD patterns show that all samples crystallize in the tetragonal phase around 450 °C. The time-resolved PL spectra of europium doped and impregnated ZrO2 show spectral dynamics with time delay after lamp/laser pulse which is assigned to the coexistence of the different amorphous and crystalline components or unreacted europium precursor. From in situ Raman spectra, crystallization was detected at 300–350 °C, monitoring for the characteristic tetragonal-like 5D0–7F2 emission of europium at 606 nm. The ratio of tetragonal to amorphous emission increased abruptly from ca. 2–4% at 300–400 °C to almost 25% at 400–450 °C, whereas at 500 °C the emission is mostly tetragonal. A similar trend was found with the ex situ calcined samples, but relative strong tetragonal emission was observed at lower temperature in the range of 350 to 400 °C.

    Copyright © 2012 American Chemical Society

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    Supporting Information

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    HRTEM and STEM pictures, EDS experimental data, and excitation, Raman, and FT-IR spectra. This material is available free of charge via the Internet at http://pubs.acs.org.

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    The Journal of Physical Chemistry C

    Cite this: J. Phys. Chem. C 2012, 116, 31, 16776–16783
    Click to copy citationCitation copied!
    https://doi.org/10.1021/jp3040538
    Published June 5, 2012
    Copyright © 2012 American Chemical Society
    Request reuse permissions

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