Search Results (19)

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. Full article

The annealing process is one of the most common methods used to study the thermal stability of multilayers. To study the effect of the annealing process on the microstructural variation in NiV/B₄C multilayers, different annealing experiments were performed on NiV/B₄C multilayers with a d-spacing of 8 nm. This work provides a foundation for the fabrication of non-periodic NiV/B₄C multilayers. The NiV/B₄C multilayers were investigated by grazing-incidence X-ray reflectometry (GIXR), X-ray diffuse scattering (XRS), atomic force microscopy (AFM), X-ray diffraction (XRD), grazing-incidence small-angle X-ray scattering (GISAXS) and transmission electron microscopy (TEM). The temperature-dependent experiments showed that annealing at 70–290 °C slightly increased the period thickness and interface width. Annealing at higher temperatures resulted in significant structural changes and thickness ratio (Г = d_NiV/d) changes from 0.4 to 1/3 at 340 °C. The time-dependent results showed that the microstructural variations primarily occurred after 60 min. The XRD, XRS, GISAXS and TEM were further used to study microstructural changes. It was found that the NiV/B₄C multilayers exhibited a microcrystal structure after annealing, and that enhanced crystallinity and an increase in interface roughness were the main reasons for the microstructural changes. Full article

Grazing incidence small angle X-ray scattering (GISAXS) was used to study the structure and interparticle spacing of monolayers of organic ligand-stabilized iron oxide nanocrystals floating at the air–water interface on a Langmuir trough, and after transfer to a solid support via the Langmuir–Blodgett technique. GISAXS measurements of the nanocrystal arrangement at the air–water interface showed that lateral compression decreased the interparticle spacing of continuous films. GISAXS also revealed that Langmuir–Blodgett transfer of the nanocrystal layers to a silicon substrate led to a stretching of the film, with a significant increase in interparticle spacing. Full article

Femtosecond high-intensity laser pulses at intensities surpassing 10¹⁴ W/cm² can generate a diverse range of functional surface nanostructures. Achieving precise control over the production of these functional structures necessitates a thorough understanding of the surface morphology dynamics with nanometer-scale spatial resolution and picosecond-scale temporal resolution. In this study, we show that single XFEL pulses can elucidate structural changes on surfaces induced by laser-generated plasmas using grazing-incidence small-angle X-ray scattering (GISAXS). Using aluminium-coated multilayer samples we distinguish between sub-picosecond (ps) surface morphology dynamics and subsequent multi-ps subsurface density dynamics with nanometer-depth sensitivity. The observed subsurface density dynamics serve to validate advanced simulation models representing matter under extreme conditions. Our findings promise to open new avenues for laser material-nanoprocessing and high-energy-density science. Full article

The functionality and reliability of nanoscale multilayer devices and components are influenced by changes in stress and microstructure throughout fabrication, processing, and operation. NiV/B₄C multilayers with a d-spacing of 3 nm were prepared by magnetron sputtering, and two groups of annealing experiments were performed. The stress, microstructure, and interface changes in NiV/B₄C after annealing were investigated by grazing-incidence X-ray reflectometry (GIXR), grazing-incidence X-ray diffraction (GIXRD), X-ray diffuse scattering, and grazing-incidence small-angle X-ray scattering (GISAXS). The temperature dependence experiments revealed a gradual shift in the multilayer stress from compression to tension during annealing from 70 °C to 340 °C, with the stress approaching near-zero levels between 70 °C and 140 °C. The time-dependent experiments indicated that most of the stress changes occurred within the initial 10 min, which showed that prolonged annealing was unnecessary. Combining the X-ray diffraction and X-ray scattering measurements, it was found that the changes in the thickness, interface roughness, and lateral correlation length, primarily due to crystallization, drove the changes in stress and microstructure. Full article

Grazing-incidence small-angle X-ray scattering (GISAXS) is a powerful method for the structural analysis of ordered arrays of nanoparticles, quantum dots, or similar objects. However, for the correct interpretation of the measured GISAXS intensity distributions, a proper data analysis, including a suitable model, is required. Here, we demonstrate a software platform, GisaxStudio, aimed at the analysis and simulation of 2D GISAXS intensity distributions from ordered lattices of different nanoparticles. It contains several models that satisfactorily describe the GISAXS from 3D lattices or crystals of nanoparticles prepared by the self-assembly processes, pre-pattering, or ion-beam interaction with the material within their tracks. It also supports different shapes of nanoparticles, including core-shell structure with the center of core possibly displaced from the center of the shell. The software is very useful for fast and accurate GISAXS data analysis. Full article

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. Full article

Various types of 2D organic–inorganic perovskite solar cells have been developed and investigated due to better electron transport behavior and environmental stability. Controlling the formation of phases in the 2D perovskite films has been considered to play an important role in influencing the stability of perovskite materials and their performance in optoelectronic applications. In this work, Lewis base urea was used as an effective additive for the formation of 2D Ruddlesden—Popper (RP) perovskite (BA)₂(MA)_n−1Pb_nI_3n+1 thin film with mixed phases (n = 2~4). The detailed structural morphology of the 2D perovskite thin film was investigated by in situ X-ray diffraction (XRD), grazing-incidence small-angle X-ray scattering (GISAXS) and photoluminescence mapping. The results indicated that the urea additive could facilitate the formation of 2D RP perovskite thin film with larger grain size and high crystallinity. The 2D RP perovskite thin films for solar cells exhibited a power conversion efficiency (PCE) of 7.9% under AM 1.5G illumination at 100 mW/cm². Full article

Polyether ether ketone (PEEK) films irradiated with 170 keV protons were calculated by the stopping and ranges of ions in matter (SRIM) software. The results showed that the damage caused by 170 keV protons was only several microns of the PEEK surface, and the ionization absorbed dose and displacement absorbed dose were calculated. The surface morphology and roughness of PEEK after proton irradiation were studied by atomic force microscope (AFM). GISAXS was used to analyze the surface structural information of the pristine and irradiated PEEK. The experimental results showed that near the surface of the pristine and irradiated PEEK exists a peak, and the peak gradually disappeared with the increasing of the angles of incidence and the peak changed after irradiation, which implies the 170 keV protons have an effect on PEEK structure. The influences of PEEK irradiated with protons on the melting temperature and crystallization temperature was investigated by differential scanning calorimetry (DSC). The DSC results showed that the crystallinity of the polymer after irradiation decreased. The structure and content of free radicals of pristine and irradiated PEEK were studied by Fourier transform infrared spectroscopy (FTIR) and electron paramagnetic resonance (EPR). The stress and strain test results showed that the yield strength of the PEEK irradiated with 5 × 10¹⁵ p/cm² and 1 × 10¹⁶ p/cm² was higher than the pristine, but the elongation at break of the PEEK irradiated with 5 × 10¹⁵ p/cm² and 1 × 10¹⁶ p/cm² decreased obviously. Full article

Quantum dots are under intense research, given their amazing properties which favor their use in electronics, optoelectronics, energy, medicine and other important applications. For many of these technological applications, quantum dots are used in their ordered self-assembled form, called superlattice. Understanding the mechanism of formation of the superlattices is crucial to designing quantum dots devices with desired properties. Here we review some of the most important findings about the formation of such superlattices that have been derived using grazing incidence scattering techniques (grazing incidence small and wide angle X-ray scattering (GISAXS/GIWAXS)). Acquisition of these structural information is essential to developing some of the most important underlying theories in the field. Full article

GISAXS has been used to study morphology change of α-Fe₂O₃ nanocubes after annealing processes. A submonolayer of the nanocubes was deposited on a Si(100) substrate. While an annealing at 400 °C in vacuum does not change a GISAXS pattern from as-prepared nanocubes submonolayer, subsequent annealing in air at the same temperature altered the GISAXS pattern significantly. SEM images showed that the air-annealed nanocubes were coated with thin layers which were identified as amorphous carbon layers based on Raman measurements. GISAXS simulations from morphologies of nanocube with 38 nm side-length and core-shell (nanocube-core and 7 nm thick carbon-shell) reproduced measured patterns from the vacuum- and the air-annealed nanocubes, respectively. The current study provides new approach for in-situ characterization of carbon deposition on a uniform shape nanoparticle through monitoring of deposited carbon thickness. Full article

On the basis of the major application for block copolymers to use them as separation membranes, lithographic mask, and as templates, the preparation of highly oriented nanoporous thin films requires the selective removal of the minor phase from the pores. In the scope of this study, thin film of polystyrene-block-poly(ethylene oxide) block copolymer with a photocleavable junction groups based on ortho-nitrobenzylester (ONB) (PS-hν-PEO) was papered via the spin coating technique followed by solvent annealing to obtain highly-ordered cylindrical domains. The polymer blocks are cleaved by means of a mild UV exposure and then the pore material is washed out of the polymer film by ultra-pure water resulting in arrays of nanoporous thin films to remove one block. The removal of the PEO materials from the pores was proven using the grazing-incidence small-angle X-ray scattering (GISAXS) technique. The treatment of the polymer film during the washing process was observed in real time after two different UV exposure time (1 and 4 h) in order to draw conclusions regarding the dynamics of the removal process. In-situ X-ray reflectivity measurements provide statistically significant information about the change in the layer thickness as well as the roughness and electron density of the polymer film during pore formation. 4 H UV exposure was found to be more efficient for PEO cleavage. By in-situ SFM measurements, the structure of the ultra-thin block copolymer films was also analysed and, thus, the kinetics of the washing process was elaborated. The results from both measurements confirmed that the washing procedure induces irreversible change in morphology to the surface of the thin film. Full article

This work presents the preparation of cross-linking Au nanoparticle (NP) monolayer membranes by the thiol exchange reaction and their enhanced mechanical properties. Dithiol molecules were used as a cross-linking mediator to connect the adjacent nanoparticles by replacing the original alkanethiol ligand in the monolayer. After cross-linking, the membrane integrity was maintained and no significant fracture was observed, which is crucial for the membrane serving as a nanodevice. TEM (Transmission Electron Microscopy), UV–Vis absorption spectrum, and GISAXS (grazing incidence small angle X-ray scattering) were performed to characterize the nanostructure before and after cross-linking. All results proved that the interparticle distance in the monolayer was controllably changed by using dithiols of different lengths as the cross-linking agent. Moreover, the modulus of the cross-linking monolayer was measured by atomic force microscopy (AFM) and the result showed that the membrane with a longer dithiol molecule had a larger modulus, which might derive from the unbroken and intact structure of the cross-linking monolayer due to the selected appropriately lengthed dithiol. This study provides a new way of producing a nanoparticle monolayer membrane with enhanced mechanical properties. Full article

Over the past decades, the development of nano-scale electronic devices and high-density memory storage media has raised the demand for low-cost fabrication methods of two-dimensional (2D) arrays of magnetic nanostructures. Here, we present a chemical solution deposition methodology to produce 2D arrays of cobalt ferrite (CFO) nanodots on Si substrates. Using thin films of four different self-assembled block copolymers as templates, ordered arrays of nanodots with four different characteristic dimensions were fabricated. The dot sizes and their long-range arrangement were studied with scanning electron microscopy (SEM) and grazing incident small-angle X-ray scattering (GISAXS). The structural evolution during UV/ozone treatment and the following thermal annealing was investigated through monitoring the atomic arrangement with X-ray absorption fine structure spectroscopy (EXAFS) and checking the morphology at each preparation step. The preparation method presented here obtains array types that exhibit thicknesses less than 10 nm and blocking temperatures above room temperature (e.g., 312 K for 20 nm diameter dots). Control over the average dot size allows observing an increase of the blocking temperature with increasing dot diameter. The nanodots present promising properties for room temperature data storage, especially if a better control over their size distribution will be achieved in the future. Full article

The application of the grazing-incidence small-angle X-ray scattering (GISAXS) technique for the investigation of three-dimensional lattices of nanostructures is demonstrated. A successful analysis of three-dimensionally ordered nanostructures requires applying a suitable model for the description of the nanostructure ordering. Otherwise, it is possible to get a good agreement between the experimental and the simulated data, but the parameters obtained by fitting may be completely incorrect. In this paper, we theoretically examine systems having different types of nanostructure ordering, and we show how the choice of the correct model for the description of ordering influences the analysis results. Several theoretical models are compared in order to show how to use GISAXS in the investigation of self-assembled arrays of nanoparticles, and also in arrays of nanostructures obtained by ion-beam treatment of thin films or surfaces. All models are supported by experimental data, and the possibilities and limitations of GISAXS for the determination of material structure are discussed. Full article