Themed collection Spectroscopy and scattering for chemistry

Kirsten M. Ø. Jensen, Dorota Koziej and Serena DeBeer introduce the Nanoscale themed issue on spectroscopy and scattering for chemistry: new possibilities and challenges with large scale facilities.

Pair distribution function, PDF, analyses are emerging as a powerful tool to characterize non-ideal metal–organic framework (MOF) materials with compromised ordering.

Combined analyses by operando soft X-ray spectroscopy and high-energy X-ray scattering offers opportunities to unravel electronic and atomic structures that underpin interfacial catalysis.

A new photon-in/photon-out magnetic probe empowers an in situ estimation of size distribution and atomic structure of iron oxide nanoparticles in suspension.

The formation mechanism of amorphous tantalum oxides was studied by total scattering experiments starting from alkoxide precursors. Hydrolysed Ta_xO_yH_z clusters form in highly dilute solutions which were transformed into L-Ta₂O₅ by calcination.

We report a full characterization of PuO₂ nanoparticles at the atomic level and probe their local and electronic structure by a variety of methods available at the synchrotron and theoretical approaches.

We use pair distribution function analysis of in situ total scattering data and complementary techniques to reveal how molten NaNO₃ modifies the decomposition pathways of a hydrated magnesium carbonate to the formation of MgO.

The combination of X-ray absorption with X-ray emission spectroscopy requires careful consideration of the experimental protocol. The article discusses general aspects with examples for bio-catalysis and colloidal magnetic nanoparticles.

The gold nanoparticle nucleation stage identified by XAS is accompanied in SAXS by an abrupt shrinkage of the size of molecular pre-nucleation clusters into gold nuclei, which is interpreted as a non-classical nucleation mechanism.

We investigate the structure-activity correlations of methanation catalysts obtained by thermal decomposition of a Ni-based metal-organic framework, using pair distribution function, X-ray absorption spectroscopy and X-ray diffraction.

The effect of cobalt on the catalytic activity of a NiCoO dry methane reforming catalyst was investigated by in situ XES and HERFD XAS. Co is shown to hamper the reduction of the Ni in the NiCoO catalyst by modulation of its electronic structure.

Material ejection in pulsed laser ablation in liquids is analysed by X-ray in situ methods to resolve particle formation and oxidation.

The local atomic structure of two stacked thin films is probed by applying grazing incidence x-ray total scattering at variable incidence angle and resolving pair distribution functions for each individual layer.

Nanosheets of molybdenum(VI) oxide supported on carbon spheres were carburized and utilized for the dry reforming of methane (DRM). A molybdenum oxycarbide phase was identified as active for DRM and characterised by XANES and TEM methods.

Iron(III) hydroxide phosphate hydrate Fe_1.13(PO₄)(OH)_0.39(H₂O)_0.61 is investigated for the first time as a Na-ion battery cathode. The material exhibits similar storage capacities for Na- and Li-ions at relatively low current rates (i.e. C/10).

Crystalline and amorphous cubane-type coordination polymers were synthesized and investigated by X-ray total scattering and single crystal diffraction.

Hard ferrimagnetic CoFe₂O₄ nanoparticles become softer in the presence of neighbouring soft ferrimagnetic MnFe₂O₄ nanoparticles.

The relationship between nanoparticle morphology, self-induced atomic/magnetic texture and magnetic properties of high-performance hexaferrite magnets is elucidated using neutron/X-ray pole figure analysis and neutron/synchrotron powder diffraction.

In situ neutron powder diffraction (NPD) was employed for investigating gram-scale reduction of hard magnetic CoFe₂O₄ (spinel) nanoparticles into CoFe₂O₄/CoFe₂ exchange-spring nanocomposites via H₂ partial reduction.

The redox properties of five common solvents under solvothermal conditions are demonstrated through synthesis and characterization of 3d metal based materials.

The presence of a capping agent (CTAB) on Pd nanoparticles produces a strong static disorder in the surface region.

PdCu bimetallic colloidal nanoparticles-catalyzed Sonogashira coupling is demonstrated proceed by a quasi-homogeneous pathway with involvement of an alkynylcopper intermediate.