This article provides a demonstration of tools for operando pair distribution function analysis of nanocrystalline functional materials. The particular case used is 3 nm TiO₂-bronze nanocrystals as active electrode material in a Li-ion battery.

Grazing-incidence total X-ray scattering allows for orientational pair distribution function analysis of indium oxide thin films with only a single measurement. Elucidation of information such as effects of film anisotropy on bond lengths in specific orientations relative to the substrate and determination of orientation in X-ray amorphous films is demonstrated.

Contributions to plasticity from hard matrix and binder metal in nanocrystalline cermets were studied by molecular dynamics simulations.

Structural information on nanocrystalline materials from X-ray total scattering data has been obtained with a massively parallel Mythen II detector using atomic pair distribution function analysis.

Operando high-resolution X-ray absorption spectroscopy of BiVO₄ photoanodes was performed in an electrochemical cell at both cation absorption edges. Small but significant variations of the spectra induced by electrochemical polarization were detected which were interpreted in terms of changes in the occupation of electronic states.

Commentary is provided on recent magnetic SANS experiments on highly inhomogeneous high-pressure-torsion manufactured metals. The ensuing progress in the theoretical description of magnetic SANS using micromagnetic theory is highlighted.

The size and size anisotropy of nanocrystals is determined together with the distribution of amorphous phases inside a seven-capillary model reactor filled with various nanomaterials. This is achieved by diffraction scattering computed tomography followed by Rietveld refinement and multivariate analysis of Rietveld backgrounds.

This work presents a discussion of the possibilities offered by X-ray absorption spectroscopy (XAS) to study the local structure of nanomaterials. The current state of the art for the interpretation of extended X-ray absorption fine structure (EXAFS), including an advanced approach based on the use of classical molecular dynamics, is described and exemplified in the case of NiO nanoparticles. In addition, the limits and possibilities of X-ray absorption near-edge spectroscopy (XANES) in determining several effects associated with the nanocrystalline nature of materials are also discussed in connection with the development of ZnO-based dilute magnetic semiconductors and iron oxide nanoparticles.

The structural changes occurring during pyrolysis from pre-ceramic polymer to polymer-derived ceramic are traditionally challenging to characterize, and the inclusion of nanoparticle filler throughout the matrix complicates this further. In this work, the authors demonstrate the value of synchrotron X-ray scattering and pair distribution function analysis to track these structural changes with isolation of nanoparticle–matrix interactions at the local scale.

Biological materials obtain their properties through hierarchical structuring. Understanding such materials calls for multimodal and multiscale approaches. Based on two example systems, bone and shell, we discuss current analytical approaches, their capabilities and limits, and how to tie them together to fully cover the different length scales involved in understanding materials' functions. We will further discuss advances in this area and future developments, the possible roadblocks (radiation damage, data quantity, sample preparation) and potential ways to overcome them.