Part 3 of the ISO 14577 ¡°Instrumented indentation test for hardness and materials parameters¡° (IIT) concerns the calibration of reference blocks. Besides the widely spread activities for supplying reference blocks in the nano and micro range it is needed to be taken into account the macro range too. The paper reports on test results on ceramic materials which are tailored for reference blocks. The specimens made of Si3N4, SiC, or Al2O3 ceramics are highly homogenous and exhibit an increased quality with a roughness Ra ¡Ü 0.005 ¦Ìm. They are successfully used for reference blocks of the traditional Vickers and Knoop hardness. In comparison, the capability of hardened steel which is used for traditional hardness techniques is studied.
In this paper EXAFS was used to determine bond lengths in the structures of zeunerite and meta-zeunerite. The atomic distances between heavy and light scatterers observed using EXAFS in meta-zeunerite deviate approximately 0.1 Å from literature data of single-crystal X-ray diffraction measurements. Because this difference is significant higher than the error limits of EXAFS measurements, the complete crystal structure of meta-zeunerite, Cu[UO2AsO4]2·8 H2O, is revised by X-ray structure analysis. The bond length determinations by EXAFS and the revised XRD data agree within the experimental error limits. In this study EXAFS spectroscopy has proven to be an useful tool for determining precise local bond lengths in the environment of heavy atoms. Moreover, the crystal structure of zeunerite, Cu[UO2AsO4]2·12 H2O, hitherto not been described in the literature, was investigated. Reflex broadening effects and intergrowth relationship between zeunerite and meta-zeunerite show that meta-zeunerite grows in nature due to dehydration of zeunerite. The structural transition from zeunerite to meta-zeunerite is connected with a change in the uranyl arsenate layer arrangement and the crystal water content.
Determination of structures using x-ray powder diffraction is complicated if the reflection intensities are mainly influenced by the scattering from heavy atoms and the atomic coordinates of light atoms remain uncertain. A method like EXAFS, which is sensitive to short range order, gives reliable atomic distances in the surroundings of heavy atoms with a precision of ±0.02 Å. The probability for obtaining the complete structure from x-ray powder diffraction increases if one includes parameters derived from EXAFS measurements as restraints during the procedure of structure solving. We demonstrate the potential of combining EXAFS and x-ray powder diffraction by solving the structure UO2[H2AsO4]2H2O. The procedure starts with the determination of space group and cell parameters from XRD powder data. In a second step the absolute values of the structure factor |F| are separated by iterating a decomposition formula. The heavy atom positions are determined by direct methods. In the third step atomic distances of coordination polyhedra are estimated using EXAFS. Subsequently, the complete coordination geometries around the heavy atoms including reliable distances are used as restraints in the structure solving and refinement procedure.