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Development of two new approaches for preparation of zirconium silicate systems at low temperature

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Abstract

Homogeneous and stable zirconium silicate sols and gels were prepared via the sol-gel process. Two synthesis procedures were explored based on using acetylacetone (acac) and acetic acid (HOAc) as modifying agents. The homogeneous sols were characterized by small angle x-ray scattering (SAXS) and 29Si NMR in the early stages of polymerization. Zr addition to the Si sols caused significant modification of the extent of condensation of the Si species as determined by 29Si NMR. TGA and DTA of the two types of xerogels revealed differences attributed to the modifying agents. Fourier Transform Infrared (FTIR) spectroscopy of acac xerogels showed a band at 1600 cm−1, assigned to acac bonded to Zr. FTIR spectra of the HOAc xerogels were consistent with OAc bidentate ligands bonded to Zr. UV-Vis spectroscopy results of the HOAc2.3 thin film presented a band assigned to OAc singly coordinated to Zr.

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Author notes

  1. J. Mendez-Vivar

    Present address: Depto. de Quimica, Universidad Autonoma Metropolitana-Iztapalapa, A. P. 55-534, 09340, Mexico, D. F., Mexico

Authors and Affiliations

  1. Advanced Materials Laboratory (University of New Mexico/Sandia National Laboratories), 1001 University Blvd. SE, 87106, Albuquerque, NM, USA

    J. Mendez-Vivar

  2. Advanced Materials Laboratory (University of New Mexico/Sandia National Laboratories), 1001 University Blvd. SE, 87106, Albuquerque, NM, USA

    C. J. Brinker

  3. Ceramic Synthesis and Inorganic Chemistry Department 1846 Sandia National Laboratories, 87105-5800, Albuquerque, NM, USA

    C. J. Brinker

Authors
  1. J. Mendez-Vivar
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Mendez-Vivar, J., Brinker, C.J. Development of two new approaches for preparation of zirconium silicate systems at low temperature. J Sol-Gel Sci Technol 2, 393–397 (1994). https://doi.org/10.1007/BF00486277

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