The results of both a line-broadening study on a ceria sample and a size–strain round robin on diffraction line-broadening methods, which was sponsored by the Commission on Powder Diffraction of the International Union of Crystallography, are presented. The sample was prepared by heating hydrated ceria at 923 K for 45 h. Another ceria sample was prepared to correct for the effects of instrumental broadening by annealing commercially obtained ceria at 1573 K for 3 h and slowly cooling it in the furnace. The diffraction measurements were carried out with two laboratory and two synchrotron X-ray sources, two constant-wavelength neutron and a time-of-flight (TOF) neutron source. Diffraction measurements were analyzed by three methods: the model assuming a lognormal size distribution of spherical crystallites, Warren–Averbach analysis and Rietveld refinement. The last two methods detected a relatively small strain in the sample, as opposed to the first method. Assuming a strain-free sample, the results from all three methods agree well. The average real crystallite size, on the assumption of a spherical crystallite shape, is 191 (5) Å. The scatter of results given by different instruments is relatively small, although significantly larger than the estimated standard uncertainties. The Rietveld refinement results for this ceria sample indicate that the diffraction peaks can be successfully approximated with a pseudo-Voigt function. In a common approximation used in Rietveld refinement programs, this implies that the size-broadened profile cannot be approximated by a Lorentzian but by a full Voigt or pseudo-Voigt function. In the second part of this paper, the results of the round robin on the size–strain line-broadening analysis methods are presented, which was conducted through the participation of 18 groups from 12 countries. Participants have reported results obtained by analyzing data that were collected on the two ceria samples at seven instruments. The analysis of results received in terms of coherently diffracting, both volume-weighted and area-weighted apparent domain size are reported. Although there is a reasonable agreement, the reported results on the volume-weighted domain size show significantly higher scatter than those on the area-weighted domain size. This is most likely due to a significant number of results reporting a high value of strain. Most of those results were obtained by Rietveld refinement in which the Gaussian size parameter was not refined, thus erroneously assigning size-related broadening to other effects. A comparison of results with the average of the three-way comparative analysis from the first part shows a good agreement.

ENGIN-X, a new time-of-flight (TOF) neutron diffractometer optimized to measure elastic strains at precise locations in bulky specimens recently commissioned at the ISIS Facility in the Rutherford Laboratory, UK, is described. Fast counting times, together with a flexible and accurate definition of the instrumental gauge volume are the main requirements of neutron strain scanning and have been addressed on ENGIN-X through the design of a novel TOF diffractometer with a tuneable resolution and interchangeable radial collimators. Further, the routine operation of the instrument has been optimized by creating a virtual instrument,i.e.a three-dimensional computer representation of the diffractometer and samples, which assists in the planning and execution of experiments. On comparing ENGIN-X with its predecessor ENGIN, a 25× gain in performance is found, which has allowed the determination of stresses up to 60 mm deep in steel specimens. For comparison with constant-wavelength diffractometers, special attention has been paid to the absolute number of counts recorded during the experiments. A simple expression is presented for the estimation of counting times in TOF neutron strain scanning experiments.

Macrostrain variations in engineering components are frequently examined using neutron diffraction, at both reactors and pulsed sources. It is desirable to minimize the sampling volume in order to maximize the spatial resolution, although this increases the required measurement time. At reactors, macrostrain behavior is inferred from a single lattice reflection (deemed to be representative of the bulk response). At a pulsed source, a complete diffraction pattern is recorded and accordingly it is natural to fit the entire diffraction spectra using a Rietveld [J. Appl. Cryst. 2, 65 (1969)] refinement. This means that an idealized crystal structure is fit to the measured distorted crystal structure, which includes deviation of the measured lattice reflections from the ideal due to elastoplastic strain anisotropies, which are dependent on the particular lattice reflection (hkl) considered. We show that elastic macrostrains calculated from lattice parameter changes in Rietveld refinements (without accounting for hkl dependent anisotropies) are almost identical to the bulk elastic response and are comparable to the response obtained from a single lattice reflection typically used by practitioners at a steady state source. Moreover good refinements on the complete pattern are obtained with short measurement times compared to what is required for good statistics for single reflections. By incorporating a description of the elastic strain anisotropy expected in cubic materials into the Rietveld code, an empirical prediction of plastic strain history is possible. The validity of these arguments is demonstrated by analysis of a uniaxial tensile load test and a reanalysis of previously reported data taken on a deformed stainless steel ring. The plastic strain predictions compare favorably with a finite element model.