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Incipient crystallization of transition-metal tungstates under microwaves probed by Raman scattering and transmission electron microscopy

  • Special Issue: Nanostructured Materials 2010
  • Published:
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Abstract

Microwave synthesis was used to produce nanosized transition-metal tungstates in environmentally friendly conditions not yet reported by the literature: 110 and 150 °C, for times of 10 and 20 min. X-ray diffraction evidenced incipient crystallized materials, while transmission electron microscopy indicates nanostructured regions of about 2–5 nm inside an amorphous matrix. Raman spectroscopy was used to probe short-range ordering in the achieved samples and also to obtain a reliable set of spectra containing all the Raman-active bands predicted by group-theory calculations. The vibrational spectra showed no extra feature, indicating that the microwave processing was able to produce short-range ordered materials without tetrahedral distortions. These distortions are frequently reported when commercially modified kitchen microwave units are employed. In this work, the syntheses were conducted in a commercial apparatus especially designed for fully controlled temperature–time–pressure conditions.

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Acknowledgments

The authors acknowledge the financial support from CAPES, CNPq, FINEP, and FAPEMIG. The authors would like to thank the Center of Microscopy—UFMG for technical support with transmission electron microscopy (TEM and HRTEM).

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Authors and Affiliations

  1. Departamento de Química, Universidade Federal de Ouro Preto, Campus Morro do Cruzeiro, ICEB II, Sala 67, Ouro Preto-MG, 35400-000, Brazil

    Kisla P. F. Siqueira & Anderson Dias

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  1. Kisla P. F. Siqueira
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  2. Anderson Dias
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Correspondence to Anderson Dias.

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Siqueira, K.P.F., Dias, A. Incipient crystallization of transition-metal tungstates under microwaves probed by Raman scattering and transmission electron microscopy. J Nanopart Res 13, 5927–5933 (2011). https://doi.org/10.1007/s11051-011-0248-8

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  • DOI: https://doi.org/10.1007/s11051-011-0248-8

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