Temperature-induced structure and microstructure evolution of nanostructured Ni0.9Zn0.1O

The crystal structure and microstructure of as-prepared and annealed Ni0.9Zn0.1O were refined at room temperature in both the Fm (3) over barm and R (3) over barm space groups. It is shown that below the Neel point (458 K), where magnetic ordering triggers the presence of a trigonal strain, the common usage of a higher-symmetry non-admissible space group for crystal structure and microstructure analysis via the Rietveld method may result in both an incorrect structure description and incorrect microstructure parameters (size and strain). More realistic microstructure data can be obtained by whole powder pattern modelling of the powder diffraction data. Increasing the annealing temperature causes a reduction of the trigonal distortion as well as an increase in domain size. Simultaneously, the Raman spectra become less resolved, a clear indication of domain growth and structural evolution of the structure towards cubic symmetry (R (3) over barm -> Fm (3) over barm).