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Nanostructured hematite (α-Fe₂O₃) films exhibit significant potential for energy, environmental, and medical applications. In the present work, a large-scale spray coating deposition method, scanning electron microscopy, and in situ grazing-incidence small-angle X-ray scattering are combined to investigate the structure formation mechanism of pure poly(styrene)-b-poly(4-vinyl pyridine) (PS-b-P4VP) and hybrid PS-b-P4VP/FeCl₃ films during and after spray deposition. Under the film deposition conditions specified in this experiment, a layered pure PS-b-P4VP film, a sponge-like hybrid PS-b-P4VP/FeCl₃ film, and a porous α-Fe 2 O 3 film are obtained upon completion of the deposition. The morphological differences between the investigated pure PS-b-P4VP and hybrid PS-b-P4VP/FeCl₃ films result from the interplay among the complexation between FeCl₃ and P4VP segments, the crystallization of the P4VP segment, and the surface diffusion of the FeCl 3 species. The findings of this work can offer both experimental and theoretical guidance for designing spray-deposited block copolymer and hybrid films.

This article aims to provide an overview of broad range of applications of synchrotron scattering methods in the investigation of nanoscale materials. These scattering techniques allow the elucidation of the structure and dynamics of nanomaterials from sub-nm to micron size scales and down to sub-millisecond time ranges both in bulk and at interfaces. A major advantage of scattering methods is that they provide the ensemble averaged information under in situ and operando conditions. As a result, they are complementary to various imaging techniques which reveal more local information. Scattering methods are particularly suitable for probing buried structures that are difficult to image. Although, many qualitative features can be directly extracted from scattering data, derivation of detailed structural and dynamical information requires quantitative modeling. The fourth-generation synchrotron sources open new possibilities for investigating these complex systems by exploiting the enhanced brightness and coherence properties of X-rays.

The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities for in situ and in operando GISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

Existing beamlines for in situ grazing‐incidence small‐angle scattering on liquids are either limited in angular range or incompatible with the large sample–detector distance required for submicrometre resolution. We present a low‐cost, easily assembled beam‐tilting extension for synchrotron‐based ultra‐small‐angle X‐ray scattering (USAXS) facilities, enabling grazing‐incidence and transmitted scattering (GIUSAXS, GTUSAXS) studies on liquid surfaces. The setup is compatible with standard USAXS beamlines and requires only ∼0.5 m of additional space at the sample stage. It allows X‐ray beam incidence angles of up to ∼0.6° at the liquid surface, equal to twice the angle of incidence on a reflector and below its critical angle of typical materials (e.g. silicon, germanium, etc.), and provides access to a q‐range of approximately 0.003–0.5 nm−1. The system was tested at P03 beamline (DESY) using polystyrene nanoparticles (∼197 nm) self‐assembled at the air/water interface. The recorded GIUSAXS and GTSAXS patterns revealed features characteristic of near‐surface hexagonally ordered monolayers and multilayer assemblies, validating the system's resolution and sensitivity. The proposed scheme enables selective depth profiling and expands the research capabilities of existing small‐angle X‐ray scattering synchrotron facilities for in situ studyies of submicrometre nanostructured objects at liquid surfaces under grazing‐incidence geometry, while remaining fully compatible with complementary techniques such as grazing‐incidence wide‐angle scattering and total reflection X‐ray fluorescence. We present an easily assembled, low‐cost beam‐tilting extension for synchrotron‐based ultra‐small‐angle X‐ray scattering (USAXS) / small‐angle X‐ray scattering (SAXS) beamlines enabling grazing‐incidence (GIUSAXS) and transmitted (GTUSAXS) experiments on liquid surfaces with negligible loss of X‐ray flux. The setup is implemented at the sample stage with ∼0.5 m of additional space and provides incidence angles up to ∼0.6°, corresponding to approximately twice the critical angle of typical reflector materials.

Nanostructured hematite (α‐Fe₂O₃) films exhibit significant potential for energy, environmental, and medical applications. In the present work, a large‐scale spray coating deposition method, scanning electron microscopy, and in situ grazing‐incidence small‐angle X‐ray scattering are combined to investigate the structure formation mechanism of pure poly(styrene)‐b‐poly(4‐vinyl pyridine) (PS‐b‐P4VP) and hybrid PS‐b‐P4VP/FeCl₃ films during and after spray deposition. Under the film deposition conditions specified in this experiment, a layered pure PS‐b‐P4VP film, a sponge‐like hybrid PS‐b‐P4VP/FeCl₃ film, and a porous α‐Fe2O3 film are obtained upon completion of the deposition. The morphological differences between the investigated pure PS‐b‐P4VP and hybrid PS‐b‐P4VP/FeCl₃ films result from the interplay among the complexation between FeCl₃ and P4VP segments, the crystallization of the P4VP segment, and the surface diffusion of the FeCl3 species. The findings of this work can offer both experimental and theoretical guidance for designing spray‐deposited block copolymer and hybrid films. The structure formation mechanism of pure poly(styrene)‐b‐poly(4‐vinyl pyridine) (PS‐b‐P4VP) and hybrid PS‐b‐P4VP/FeCl₃ films during and after spray deposition is investigated. The morphological differences result from the interplay among the complexation between FeCl₃ and P4VP segments, the crystallization of the P4VP segment, and the surface diffusion of the FeCl3 species.

We demonstrate a grazing-incidence X-ray platform that simultaneously records time-resolved grazing-incidence small-angle X-ray scattering (GISAXS) and grazing-incidence X-ray diffraction (GID) from a femtosecond-laser-irradiated gold film above the melting threshold, with picosecond resolution using an X-ray free-electron laser (XFEL). By tuning the X-ray incidence angle, the probe depth is set to tens of nanometres, enabling depth-selective sensitivity to near-surface dynamics. GISAXS resolves ultrafast changes in surface nanomorphology (correlation length, roughness), while GID quantifies subsurface lattice compression, grain orientation, melting and recrystallization. The approach overcomes photon-flux limitations of synchrotron grazing-incidence geometries and provides stringent, time-resolved benchmarks for complex theoretical models of ultrafast laser–matter interaction and warm dense matter. Looking ahead, the same depth-selective methodology is well suited to inertial confinement fusion (ICF): it can visualize buried-interface perturbations and interfacial thermal resistance on micron to sub-micron scales that affect instability seeding and burn propagation.

Fluorine-doped tin oxide thin films (SnO2:F) are widely used as transparent conductive oxide electrodes in thin-film solar cells because of their appropriate electrical and optical properties. The surface morphology of these films influences their optical properties and therefore plays an important role in the overall efficiencies of the solar cells in which they are implemented. At rough surfaces light is diffusely scattered, extending the optical path of light inside the active layer of the solar cell, which in term improves light absorption and solar cell conversion efficiency. In this work, we investigated the surface morphology of undoped and doped SnO2 thin films and their influence on the optical properties of the films. We have compared and analysed the results obtained by several complementary methods for thin-film surface morphology investigation: atomic force microscopy (AFM), transmission electron microscopy (TEM), and grazing-incidence small-angle X-ray scattering (GISAXS). Based on the AFM and TEM results we propose a theoretical model that reproduces well the GISAXS scattering patterns.

Organosilicate glass-based porous low dielectic constant films with different ratios of terminal methyl to bridging organic (methylene, ethylene and 1,4-phenylene) groups are spin-on deposited by using a mixture of alkylenesiloxane with organic bridges and methyltrimethoxysilane, followed by soft baking at 120–200 °C and curing at 430 °C. The films’ porosity was controlled by using sacrificial template Brij® L4. Changes of the films’ refractive indices, mechanical properties, k-values, porosity and pore structure versus chemical composition of the film’s matrix are evaluated and compared with methyl-terminated low-k materials. The chemical resistance of the films to annealing in oxygen-containing atmosphere is evaluated by using density functional theory (DFT). It is found that the introduction of bridging groups changes their porosity and pore structure, increases Young’s modulus, but the improvement of mechanical properties happens simultaneously with the increase in the refractive index and k-value. The 1,4-phenylene bridging groups have the strongest impact on the films’ properties. Mechanisms of oxidative degradation of carbon bridges are studied and it is shown that 1,4-phenylene-bridged films have the highest stability. Methylene- and ethylene-bridged films are less stable but methylene-bridged films show slightly higher stability than ethylene-bridged films.

An environmentally friendly as well as scalable synthesis route of nanostructured titania thin films is of interest for many state‐of‐the‐art devices, from solar cells to battery materials. Beta‐lactoglobulin (ß‐lg) enables water‐based and tunable titania thin film templating, allowing for different domain sizes, porosities, and morphologies. When printed with a slot‐die coater, the titania films can be tailored to specific applications with simple changes to the solution chemistry. Films printed at acidic pH conditions form significantly different final morphologies than films printed at a neutral pH value. The protein concentration plays a more limited role in the final nanostructure. With in situ grazing incidence small‐angle/wide‐angle X‐ray scattering (GISAXS/GIWAXS), the structure formation is followed with an excellent time resolution during the printing process. From the GISAXS measurements, the size evolution of the titania clusters is understood, showing significant differences for different pH values. Crystal phases and corresponding crystal orientations are investigated with GIWAXS. The combination of a water‐based titania synthesis with the scalable film deposition via slot die coating makes the presented results interesting for potential environmentally friendly mass production of nanostructured titania films. The synthesis route for the fabrication of nanostructured titania thin films focuses on water‐based solutions, abundant, nontoxic materials, and a highly scalable deposition technique. Using beta‐lactoglobulin enables tunable titania thin film templating and allows for different domain sizes, porosities, and morphologies.

Grazing incidence small- and wide-angle X-ray scattering (GISAXS, GIWAXS) has been widely applied for the study of functional thin films, be it for the characterization of nanostructured morphologies in block copolymers, nanocomposites, and nanoparticle assemblies, or for the packing and orientation of aromatic molecules or conjugated polymers. Solution-processed thin films are typically uniaxial powders, with a specific crystallographic plane oriented parallel to the substrate surface while ordered domains assume random orientations laterally. The convenient GISAXS/GIWAXS scattering geometry facilitates obtaining complete information about thin film structure as well as the ability to study samples in well-defined sample environments, as controlled by temperature, exposure to solvent vapor and drying, or coating processes. Moreover, with suitable X-ray sources and detectors, information about the ordering kinetics and phase transitions can be obtained down to the millisecond scale. The scattering geometry and an interactive graphical tool to index such scattering patterns will be discussed here. Furthermore, it will be demonstrated that proper indexing of the X-ray scattering patterns can provide deep insight into thin film structure–property relationships and the kinetics of structure formation. Recent examples of nanostructures and molecular organization in thin films will be discussed, as well as self-assembly processes leading to such structures.