Low-dose electron microscopy imaging for beam-sensitive metal–organic frameworks

This topical review discusses the recent progress in low-dose high-resolution imaging of metal–organic framework materials and gives a brief outlook on possible future directions.

The promise of GaAs 200 in small-angle neutron scattering for higher resolution

A Bonse–Hart camera using a Bragg reflection with a small crystallographic structure factor will enable one to access correspondingly low Q values in small-angle diffraction. This is demonstrated for a neutron double-crystal diffractometer using GaAs 200 reflections, resulting in an increase in Q resolution by a factor of 6.1 as compared with a standard Si 220 setup.

Laboratory-based 3D X-ray standing-wave analysis of nanometre-scale gratings

The 3D X-ray standing wave (XSW) technique is a new method for characterization of the 3D atomic profiles of planar periodic nanostructures, like nanometre-sized gratings or pillar arrays. The laboratory 3D XSW analysis of TiN gratings with nanometre-sized pitches is demonstrated here.

Flow-Xl: a new facility for the analysis of crystallization in flow systems

A new in situ facility (Flow-Xl) for the characterization of crystallization systems in flow using combined in situ X-ray diffraction and Raman spectroscopy is presented. This article highlights commissioning and calibration experiments on case-study systems that stress the utility of the instrument for extracting reproducible qualitative and quantitative phase information during crystallization processes.

Revealing nanoscale sorption mechanisms of gases in a highly porous silica aerogel

This research uses contrast-matched small-angle neutron scattering to investigate the adsorption behaviour of deuterated methane in a silica aerogel in the pressure range from 0 to 1000 bar. The results reveal a classical reversible two-phase adsorption in the 2.5–50 nm pore size region and no evidence of condensation in the sub-nanometre pores.

Ptychographic phase retrieval via a deep-learning-assisted iterative algorithm

This paper proposes a ptychographic phase-retrieval algorithm combined with a deep neural network (DNN). The proposed method allows the measurement model to be explicitly incorporated into the DNN-based approach, improving imaging capability and robustness to changes in experimental conditions.

Effect of specimen displacement in X-ray powder diffraction measurements with laboratory diffractometers

The effect of specimen displacement for different experimental geometries has been investigated. The new results allow the accurate analysis of data collected with large displacements.

Revisiting the ‘magic condition’ on the basis of the Takagi–Taupin theory

Takagi–Taupin dynamical X-ray diffraction simulations of cylindrically bent Laue crystals show that, in specific diffraction geometries, the focusing behaviour of such crystals is significantly influenced by dynamical effects, causing the foci of different energies to deviate from the predictions of the `magic condition' derived from geometric optics theory.

Pushing the limits of accessible length scales via a modified Porod analysis in small-angle neutron scattering on ordered systems

This work presents a novel method for the analysis of small-angle scattering data from a highly aligned domain structure based on a modification of the well known Porod law. The analysis approach allows the range of accessible length scales to be extended from 1 µm to up to 40 µm using a conventional small-angle neutron scattering setup.

Determining pair distribution functions of thin films using laboratory-based X-ray sources

A method is showcased whereby the pair distribution function of thin films can be measured with laboratory X-ray tubes down to 80 nm thickness. These findings clear the path for the possibility of utilizing standard modern diffraction equipment to determine thin film pair distribution functions.

Coherent X-ray diffraction imaging of single particles: background impact on 3D reconstruction

Reconstruction methods for coherent diffractive imaging of single particles with ultrashort X-ray pulses were tested with various amounts of background noise, investigating the effect on resolution.

Maximally efficient exchange in thin flow cells using density gradients

Confidence that fluids have completely exchanged in flow cells is crucial for data interpretation and reproducibility. Using a neutron reflectometry liquid flow cell as an example, this article presents a method for harnessing buoyancy effects to fill flow cells that minimizes required sample volume and ensures complete fluid exchange.

Powder-diffraction-based structural comparison for crystal structure prediction without prior indexing

A new method is presented for utilizing experimental powder diffraction patterns to rank in silico structures generated using a crystal structure prediction protocol.

Simulation and modelling of the detergent corona around the membrane protein MhsT based on SAXS data

Small-angle X-ray scattering-based modelling of various detergents around a multi-hydro­phobic substrate transporter correlates a variation in the shape of the detergent corona with the detergent tail length.

Effect of the crystallographic orientation of the surface of single-crystal Si wafers on the endotaxial growth of NiSi₂ nanoplates

This work examines the effect of the crystallographic orientation of the surface of single-crystal Si wafers on the morphology of NiSi₂ nanocrystals, which grow endotaxially within the Si due to thermally diffused Ni atoms from a nickel-doped thin film deposited on the wafer surface. Regardless of the crystallographic orientation or annealing temperature, NiSi₂ nanoplates consistently align with Si{111} planes. Although annealing did not substantially change the nanoplate dimensions, crystallographic orientation influenced the number of nanoplates formed.

Multidimensional Rietveld refinement of high-pressure neutron diffraction data of PbNCN

The results are presented of a high-pressure neutron powder diffraction study on lead cyanamide, carried out with the novel method of multidimensional Rietveld refinement. In addition to better resolution than the standard one-dimensional case, the results show the first evidence of changing C—N bond multiplicities as a function of pressure, numerically quantified from density functional theory calculations.

Coordinate-based simulation of pair distance distribution functions for small and large molecular assemblies: implementation and applications

Methods for calculation of pair distance distribution functions from coordinate models are evaluated in terms of trade-offs between computation time and accuracy. The results demonstrate approaches that are well suited for application to large nanoscale materials and biological assemblies (>1 MDa molecular weight, >10⁵ non-hydrogen atoms).

Structural characteristics of Bi₂O₂CO₃ nanosheets synthesized by nano-pulsed discharges in water

Bismuth oxycarbonate nanosheets, synthesized by nanosecond-pulsed discharges in water, adopt a pinacoid shape dictated by the 4/m2/m2/m point group. The growth mechanism based on the presence of jogs, both on the terraces and fronts, has been clarified.

Determination of the average crystallite size and the crystallite size distribution: the envelope function approach EnvACS

A procedure to determine the average crystallite size and its distribution using the radial distribution function G(r) of long-wavelength diffraction experiments is presented and tested.

Influence of silicon interlayers on the structural and reflective X-ray characteristics of Ni/Ti multilayer mirrors

The influence of Si interlayers on the microstructure of the films and boundaries and on the reflective characteristics of Ti/Ni multilayer mirrors have been studied. It has been established that such Si layers perform different functions at different interfaces.

Twinning and homo-epitaxy cooperation in the already rich growth morphology of CaCO₃ polymorphs. II. Calcite

A theoretical investigation is presented of the homo-epitaxies among the three {10.4}-cleavage, {01.2}-steep and {01.8}-flat rhombohedra of calcite.

The AUREX cell: a versatile operando electrochemical cell for studying catalytic materials using X-ray diffraction, total scattering and X-ray absorption spectroscopy under working conditions

The AUREX operando electrocatalytic cell is demonstrated to be a versatile setup for elucidating structure–property relations by means of X-ray total scattering and multimodal absorption and diffraction techniques using an Ag electrocatalyst for proof of concept.

Measurable structure factors of dense dispersions containing polydisperse optically inhomogeneous particles

The influence of optical inhomogeneities of polydisperse particles on measurable structure factors is analysed.

Energy-dispersive Laue diffraction analysis of the influence of statherin and histatin on the crystallographic texture during human dental enamel demineralization

Energy-dispersive Laue diffraction gives insights on local crystallographic texture variations in demineralized dental enamel and the role of salivary proteins in protecting the enamel structure.

Characterization of sub-micrometre-sized voids in fixed human brain tissue using scanning X-ray microdiffraction

Using scanning X-ray microdiffraction, we discovered that the small-angle scattering from human brain tissue is due largely to the presence of sub-micrometre-sized voids formed during dehydration of the fixed tissue, while the intensity at wide angles derives from the macromolecular material surrounding the voids. The ability to detect and map the presence of voids within thin sections of fixed tissue has the potential to provide novel information on the degradation of human brain tissue in neurodegenerative disease.

In situ counter-diffusion crystallization and long-term crystal preservation in microfluidic fixed targets for serial crystallography

User-friendly in situ counter-diffusion crystallization and long-term storage setups in microfluidic fixed targets provide a reliable approach to forming large crystals and maintaining their hydration for weeks, allowing ample time to grow, select and preserve the best crystal batches before X-ray beam time.

Pinhole small-angle neutron scattering based approach for desmearing slit ultra-small-angle neutron scattering data

This study presents a new, methodologically robust approach for accurately desmearing slit-smeared ultra-small-angle neutron scattering (USANS) data. The proposed technique, validated on porous anodized aluminium oxide membranes, facilitates the precise merging of USANS and small-angle neutron scattering data, offering improved data analysis capabilities in the mesoscale structural research domain.

Deconstructing 3D growth rates from transmission microscopy images of facetted crystals as captured in situ within supersaturated aqueous solutions

The crystal growth rate of the basal plane {010} face of β-form L-glutamic acid is estimated from the shadow widths of the prismatic {021} faces in optical microscopy images. This new approach for the in situ characterization of 3D crystal shape and size is part of wider research into digital crystallization process engineering, encompassing machine learning, morphological population balance modelling and crystallizer hydro­dynamics simulation.

Data quality in laboratory convergent-beam X-ray total scattering

The influence of instrument resolution effects on reduced atomic pair distribution function data in a convergent-beam laboratory X-ray diffractometer is demonstrated.

Simulation of diffraction patterns for Ruddlesden–Popper (RP) tetragonal structures with RP faults

A theoretical analysis of diffraction patterns is presented for two representatives of layered perovskite-type tetragonal phases of the Ruddlesden–Popper (RP) series, containing RP faults in a wide range of concentrations.

Electronic angle focusing for neutron time-of-flight powder diffractometers

A wide-angle short-pulse spallation neutron detector bank is shown to provide an opportunity for data processing to make a pseudo-constant wavelength powder diffraction pattern.

Link between b.c.c.–f.c.c. orientation relationship and austenite morphology in CF8M stainless steel

The microstructural properties of duplex stainless steel are studied on a wide range of scales using a large electron backscatter diffraction data set. Image analysis techniques are coupled with crystallographic data analysis to extract relevant features from a complex microstructure.

Practical courses on advanced methods in macromolecular crystallization: 20 years of history and future perspectives

Since 2004, the University of South Bohemia has been establishing a tradition in protein crystallography through practical crystallization courses organized under the auspices of the Federation of Biochemical Societies.

Free tools for crystallographic symmetry handling and visualization

In crystallography there exist a wide variety of online resources such as web pages, interactive applets, databases and programs that can be implemented in both virtual and traditional classrooms. Among these, the Bilbao Crystallographic Server, the Cambridge Structural Database, Mercury, VESTA and Jmol are highlighted for teaching fundamental crystallography since they are useful resources for crystallographic symmetry handling and visualization.

Towards dynamically configured databases for CIFs: the new modulated structures open database at the Bilbao Crystallographic Server

The conceptual exploitation of the CIF scheme allows the design of databases without deep programming knowledge. With this approach, the modulated structures open database B-IncStrDB, the official International Union of Crystallography repository for this type of material already available through the Bilbao Crystallographic Server, has been re-implemented.

SUBGROUPS: a computer tool at the Bilbao Crystallographic Server for the study of pseudo-symmetric or distorted structures

Documentation is presented for the SUBGROUPS tool at the Bilbao Crystallographic Server for the exploration of all possible symmetries resulting from the distortion of a higher-symmetry parent structure (provided that the relation between the lattices of the distorted and parent structures is known).

MIPDS: a comprehensive database on the molecular interactions in protein dimer structures

A database has been developed that comprises protein dimeric structures and their respective interactions. This database provides valuable insights into the type of interaction, including those mediated by water or small molecules and direct interactions.

FullProfAPP: a graphical user interface for the streamlined automation of powder diffraction data analysis

This paper presents FullProfAPP, a graphical user interface for highly automated powder diffraction data analysis.

Use of a confocal optical device for centring a diamond anvil cell in single-crystal X-ray diffraction experiments

Centring a diamond anvil cell prior to X-ray diffraction measurements is facilitated by use of a confocal optical device.

X-ray-based technologies in emerging fuel cell research

This article reports a workshop to discuss the current X-ray-based methods for advancing fuel cell technologies, addressing their limitations and exploring improvements alongside non-X-ray-based techniques.