Composition and microstructure of zirconium and hafnium germanates obtained by different chemical routes

Journal Article · Wed Jan 15 04:00:00 EST 2014 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2013.10.037· OSTI ID:22274180

Prokip, V. E.; Baklanova, N. I.

The phase composition and morphology of zirconium and hafnium germanates synthesized by ceramic and co-precipitation routes were studied. The products were characterized using high-temperature X-ray diffraction analysis (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and thermal (TG/DTA) analysis. To investigate the phase composition and stoichiometry of compounds the unit cell parameters were refined by full-profile Rietveld XRD analysis. The morphology of products and its evolution during high-temperature treatment was examined by SEM analysis. It was stated that there is the strong dependence of the phase composition and morphology of products on the preparation route. The ceramic route requires a multi-stage high-temperature treatment to obtain zirconium and hafnium germanates of 95% purity or more. Also, there are strong diffusion limitations to obtain hafnium germanate Hf{sub 3}GeO{sub 8} by ceramic route. On the contrary, the co-precipitation route leads to the formation of nanocrystalline single phase germanates of stoichiometric composition at a relatively low temperatures (less than 1000 °C). The results of quantitative XRD analysis showed the hafnium germanates are stoichiometric compounds in contrast to zirconium germanates that form a set of solid solutions. This distinction may be related to the difference in the ion radii of Zr and Hf. - Graphical abstract: The phase composition and morphology of zirconium and hafnium germanates synthesized by ceramic and co-precipitation routes were studied. It was stated that there is the strong dependence of the phase composition and morphology of products on the preparation route. Display Omitted - Highlights: • Zr and Hf germanates were synthesized by ceramic and co-precipitation routes. • The morphology of products depends on the synthesis parameters. • Zirconium germanates forms a set of solid solutions. • Hafnium germanates are stoichiometric compounds.

• OSTI ID: 22274180
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. 209; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
CERAMICS
COPRECIPITATION
CRYSTALS
DIFFERENTIAL THERMAL ANALYSIS
GERMANATES
HAFNIUM
HYDROFLUORIC ACID
MICROSTRUCTURE
NANOSTRUCTURES
RAMAN SPECTRA
RAMAN SPECTROSCOPY
SCANNING ELECTRON MICROSCOPY
SOLID SOLUTIONS
SYNTHESIS
TEMPERATURE RANGE 0400-1000 K
X-RAY DIFFRACTION
ZIRCONIUM