Amorphous precursors of LaNbO4 have been prepared by coprecipitation a
nd mechanical alloying. Powder characteristics before and after calcin
ation were studied by thermogravimetric analysis, differential thermal
analysis, Fourier transform-infrared spectroscopy and X-ray diffracti
on, and the crystallographic changes during thermal treatment were doc
umented by high-temperature X-ray diffraction. The tetragonal structur
e was stabilized at room temperature for the mechanically alloyed prod
uct; cells dimensions were determined from the X-ray diffraction patte
rns and volume change between monoclinic and tetragonal phase was eval
uated and is discussed.