NiO(x)GDC((1-x)) nanopowders were stoichiometrically prepared with x = 0 to 1 by self-sustained combustion solution method and subsequently calcined at 600 degrees C. The prepared samples were examined using the X-ray diffraction pattern having integral breadth (beta) of reflection and analyzed using the Voigt (V) adjustment in order to characterize the microstructure in terms of the crystallite size and microstrain. The results of X-ray diffraction analysis were compared with those derived from high-resolution transmission electron microscopy.