Multiple-data-set Rietveld analysis using isotopes in powder neutron diffraction. 2. Positional and anisotropic thermal displacement parameter determinations in CuO (tenorite) at 2 K and 300 K

Abstract

The technique of isotope-substitution neutron diffraction (ISND) and combined-data-set Rietveld analysis from powder neutron data of crystalline materials is presented and compared with single-data-set powder refinement methods. The rationale behind improvements in the precision and accuracy of the refined model as a result of reduction in parameter correlation in the least-squares technique is described. The improvements are demonstrated practically through a study of isotopically copper-substituted tenorite, CuO, at 2 and 300 K. Typically, the estimated errors on structural parameters from the combined analysis technique are 30% lower than separate single-data-set analyses. Comparison of the precision and accuracy of the structural models obtained from this investigation with previous single-crystal X-ray studies are also presented.