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Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method

  • Original Paper: Nano- and macroporous materials (aerogels, xerogels, cryogels, etc.)
  • Published:
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Abstract

Synthesis of chlorine-free, rare earth oxide aerogels from the lanthanide series was achieved using a modified epoxide-assisted sol-gel method. An ethanolic solution of the hydrated metal nitrate, propylene oxide, and ammonium carbonate was found to gel upon heating to 333 K. Critical point drying of the wet gel in CO2 yielded monolithic aerogels. Most of the aerogels were amorphous as-prepared, but became nano-crystalline after calcination at 923 K in air. The aerogels had high surface areas (up to 150 m2/g), low densities (40–225 mg/cm3), and were photoluminescent.

Highlights

  • Rare earth oxide aerogels were prepared by epoxide-assisted sol-gel route.

  • Rare earth oxide aerogels are monolithic, chlorine-free, and possess large surface areas.

  • Calcination at 923 K results in nano-crystalline aerogels, with particles less than 25 nm in diameter.

  • Characterization of these aerogels includes photoluminescence spectroscopy, Rietveld refinements, and electron microscopy.

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Acknowledgements

We like to thank the German Science Foundation (DFG) for financial support in the scientific large instrument program under the project number INST144/435-1FUGG. JI and MB gratefully acknowledge funding by the DFG through the graduate school 1860 “Micro-, meso- and macroporous nonmetallic Materials: Fundamentals and Applications”. This work is partially developed in the scope of the projects CICECO—Aveiro Institute of Materials (UID/CTM/50011/2013) financed by national funds through the Fundação para a Ciência e a Tecnologia/Ministério da Educação e Ciência (FCT/MEC) and when applicable co-financed by FEDER under the PT2020 Partnership Agreement. We acknowledge the Fraunhofer Institute for Manufacturing Technology and Advanced Materials (Bremen, Germany) for the provision of access to their TEM facility and Karsten Thiel for assistance. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344, through LDRD awards 13-LW-099 and 16-ERD-051.

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Authors and Affiliations

  1. Physical and Life Sciences Division, Lawrence Livermore National Laboratory, 7000 East Ave, Livermore, CA, 94551, USA

    M. A. Worsley, A. J. Nelson & A. E. Gash

  2. Institute of Applied and Physical Chemistry & Center for Environmental Research and Sustainable Technology, University of Bremen, Leobener Strasse 6, D-28359, Bremen, Germany

    J. Ilsemann, V. Zielasek & M. Bäumer

  3. Solid State Chemical Crystallography, Institute of Inorganic Chemistry and Crystallography, University of Bremen, Leobener Strasse 7, D-28359, Bremen, Germany

    Th. M. Gesing

  4. MAPEX Center for Materials and Processes, University of Bremen, Bibliothekstrasse 1, D-28359, Bremen, Germany

    Th. M. Gesing & M. Bäumer

  5. Department of Physics and CICECO—Aveiro Institute of Materials, University of Aveiro, 3810-193, Aveiro, Portugal

    R. A. S. Ferreira & L. D. Carlos

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  1. M. A. Worsley
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Worsley, M.A., Ilsemann, J., Gesing, T.M. et al. Chlorine-free, monolithic lanthanide series rare earth oxide aerogels via epoxide-assisted sol-gel method. J Sol-Gel Sci Technol 89, 176–188 (2019). https://doi.org/10.1007/s10971-018-4811-y

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