Nanostructure Development in Alkoxide-Carboxylate-Derived Precursor Films of Barium Titanate


Stawski, T.M. and Veldhuis, S.A. and Besselink, R. and Castricum, H.L. and Portale, G. and Blank, D.H.A. and Elshof, J.E. ten (2012) Nanostructure Development in Alkoxide-Carboxylate-Derived Precursor Films of Barium Titanate. Journal of Physical Chemistry C: Nanomaterials and interfaces, 116 (1). 425 - 434. ISSN 1932-7447

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Abstract:The structural evolution in wet alkoxide-carboxylate sol–gel precursor films of barium titanate upon drying was investigated by time-resolved small-angle X-ray scattering (SAXS). The morphology of as-dried amorphous precursor thin films was investigated by transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). Sols were prepared from titanium(IV) iso-propoxide in 2-methoxyethanol and barium acetate in acetic acid. The structures that were visible with SAXS could be divided into oligomeric structures with fractal-like scattering characteristics, and randomly packed agglomerates of nanoparticles of similar size. The fractal-like morphologies disappeared during film drying, probably because they were not stable in the absence of a solvent matrix. Only the ordered agglomerate-like structures remained in the as-dried films. EELS on as-dried films showed that spatial separation between barium and titanium-rich domains occurred during the drying of the thin films on a length scale of nanometers, depending on hydrolysis ratio. This demonstrates that as-dried films are not necessarily uniform on the mesoscopic level.
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