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Shell ferromagnetism is a new functional property of certain Heusler alloys which was recently observed in Ni50Mn45In5. We report the results of a comparative study of the magnetic microstructure of bulk Ni50Mn45In5 Heusler alloys using magnetometry, synchrotron x-ray diffraction, and magnetic small-angle neutron scattering (SANS). By combining unpolarized and spin-polarized SANS (so-called POLARIS) we demonstrate that a number of important conclusions regarding the mesoscopic spin structure can be made. In particular, the analysis of the magnetic neutron data suggests that nanoprecipitates with an effective ferromagnetic component form in an antiferromagnetic matrix on field annealing at 700K. These particles represent sources of perturbation, which seem to give rise to magnetically disordered regions in the vicinity of the particle-matrix interface. Analysis of the spin-flip SANS cross section via the computation of the correlation function yields a value of ∼55 nm for the particle size and ∼20 nm for the size of the spin-canted region.

This work reports on the pressure dependence of the octahedral tilts and mean Fe-O bond lengths in RFeO3 (R = Nd, Sm, Eu, Gd, Tb, and Dy), determined through synchrotron x-ray diffraction and Raman scattering, and their role on the pressure-induced phase transition displayed by all of these compounds. For larger rare-earth cations (Nd-Sm), both anti- and in-phase octahedral tilting decrease as pressure increases, whereas the reverse behavior is observed for smaller ones (Gd-Dy). EuFeO3 stands at the borderline, with nearly pressure-independent tilt angles. For the compounds where the tilts increase with pressure, the FeO6 octahedra are compressed at lower rates than for those ones exhibiting opposite pressure tilt dependence. The crossover between the two opposite pressure behaviors is discussed in relation to the general rules proposed from different theoretical approaches. The similarity of the pressure-induced isostructural insulator-to-metal phase transition, observed in the whole series, points out that the tilts play a minor role in its driving mechanisms. A clear relationship between octahedral compressibility and critical pressure is ascertained.

The synchrotron through-the-substrate X-ray microdiffraction technique is applied to the structural study of microvolumes of randomly oriented crystals embedded in polished thin sections. The whole procedure is discussed in detail with the help of examples from petrology, and possible future developments are envisaged., The synchrotron through-the-substrate X-ray microdiffraction technique (tts-μXRD) is extended to the structural study of microvolumes of crystals embedded in polished thin sections of compact materials [Rius, Labrador, Crespi, Frontera, Vallcorba & Melgarejo (2011 ▸). J.Synchrotron Rad. 18, 891–898]. The resulting tts-μXRD procedure includes some basic steps: (i) collection of a limited number of consecutive two-dimensional patterns (frames) for each randomly oriented crystal microvolume; (ii) refinement of the metric from the one-dimensional diffraction pattern which results from circularly averaging the sum of collected frames; (iii) determination of the reciprocal lattice orientation of each randomly oriented crystal microvolume which allows assigning the hkl indices to the spots and, consequently, merging the intensities of the different frames into a single-crystal data set (frame merging); and (iv) merging of the individual crystal data sets (multicrystal merging) to produce an extended data set suitable for structure refinement/solution. Its viability for crystal structure solution by Patterson function direct methods (δ recycling) and for accurate single-crystal least-squares refinements is demonstrated with some representative examples from petrology in which different glass substrate thicknesses have been employed. The section of the crystal microvolume must be at least of the same order of magnitude as the focus of the beam (15 × 15 µm in the provided examples). Thanks to its versatility and experimental simplicity, this method­ology should be useful for disciplines as disparate as petrology, materials science and cultural heritage.