No Arabic abstract
For obtaining reliable nanostructural details of large amounts of sample --- and if it is applicable --- Small-Angle Scattering (SAS) is a prime technique to use. It promises to obtain bulk-scale, statistically sound information on the morphological details of the nanostructure, and has thus led to many a researcher investing their time in it over the last eight decades of development. Due to pressure both from scientists requesting more details on increasingly complex nanostructures, as well as the ever improving instrumentation leaving less margin for ambiguity, small-angle scattering methodologies have been evolving at a high pace over the last few decades. As the quality of any results can only be as good as the data that goes into these methodologies, the improvements in data collection and all imaginable data correction steps are reviewed here. This work is intended to provide a comprehensive overview of all data corrections, to aid the small-angle scatterer to decide which are relevant for their measurement and how these corrections are performed. Clear mathematical descriptions of the corrections are provided where feasible. Furthermore, as no quality data exists without a decent estimate of its precision, the error estimation and propagation through all these steps is provided alongside the corrections. With these data corrections, the collected small-angle scattering pattern can be made of the highest standard allowing for authoritative nanostructural characterisation through its analysis. A brief background of small-angle scattering, the instrumentation developments over the years, and pitfalls that may be encountered upon data interpretations are provided as well.
Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering (SAXS): if it is not done sufficiently well, this may become evident during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended, comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction. When applied in the proposed order, the resulting data will provide a high degree of accuracy for both solid samples and dispersions. The solution here can be applied without modification to any pinhole-collimated instruments with photon-counting, direct detection area detectors.
In metal nanoparticles (NPs) supracrystals, the metallic core provides some key properties, e.g. magnetization, plasmonic response or conductivity, with the ligand molecules giving rise to others like solubility, assembly or interaction with biomolecules. The formation of these supracrystals depends on a complex interplay between many forces, some stemming from the core, some from the ligands. At present, there is no known approach to characterize the local order of ligand molecules or their dynamics with atomic spatial resolution. Here, we develop a methodology based on small-angle ultrafast electron diffraction combined with angular cross-correlation analysis to characterize a two-dimensional supracrystal of dodecanethiol-coated gold NPs. We retrieve the static arrangement of the ligands, showing that at equilibrium they order in a preferential orientation on the NPs surface and throughout the two-dimensional supracrystal. Upon light excitation, positional disorder is induced in the supracrystal, while its overall homogeneity is surprisingly found to transiently increase. This suggests that transient annealing of the supracrystal takes place within few picoseconds (ps). This methodology will enable the systematic investigation of the dynamical structural properties of nano-assembled materials containing light elements, relevant for biological applications.
We present a novel methodology of augmenting the scattering data measured by small angle neutron scattering via an emerging deep convolutional neural network (CNN) that is widely used in artificial intelligence (AI). Data collection time is reduced by increasing the size of binning of the detector pixels at the sacrifice of resolution. High-resolution scattering data is then reconstructed by using AI deep super-resolution learning method. This technique can not only improve the productivity of neutron scattering instruments by speeding up the experimental workflow but also enable capturing kinetic changes and transient phenomenon of materials that are currently inaccessible by existing neutron scattering techniques.
Exploiting small angle X-ray and neutron scattering (SAXS/SANS) on the same sample volume at the same time provides complementary nanoscale structural information at two different contrast situations. Compared with an independent experimental approach, the truly combined SAXS/SANS experimental approach ensures the exactness of the probed samples particularly for in-situ studies. Here, we introduce an advanced portable SAXS system that is dimensionally suitable for installation at D22 zone of ILL. The SAXS apparatus is based on a RIGAKU copper/molybdenum switchable microfocus rotating anode X-ray generator and a DECTRIS detector with a changeable sample-to-detector distance of up to 1.6 m in a vacuum chamber. A science case has been presented to demonstrate the uniqueness of the newly established method at ILL. Temporal structural rearrangements of both, organic stabilizing agents and organically capped gold colloidal particles during gold nanoparticle growth are simultaneously probed, enabling immediate correlated structural information. The newly established nano-analytical method at ILL will open the way for real time investigations of a wide range of innovative nanomaterials and will enable comprehensive in-situ studies on biological systems. A potential development of a fully-automated SAXS/SANS system with a common control environment and additional sample environments, permitting a continual and efficient operation of the system at the hands of ILL users, has also been introduced.
We present the calculation of the elastic and inelastic high--energy small--angle electron--positron scattering with a {it per mille} accuracy. PACS numbers 12.15.Lk, 12.20.--m, 12.20.Ds, 13.40.--f