Sérgio L. Morelhão

Nanostructure of sol–gel films by x-ray specular reflectivity

Recently, several studies have been carried out on sol–gel films for optical applications, mostly motivated by the quickness and low cost of the film preparation process. In order to preserve the coherence properties of the light, improvements in the current quality of such films are necessary as well as appropriated techniques for structural characterization and quality control. X-ray specular reflectivity could be one of such techniques, but it is limited by the complexity of the internal nanostructure of the films. In this work, we have developed a procedure to extract the exact density profile of sol–gel films, and applied it to analyze a sol–gel derived Er2O3 film.

Observation of coherent hybrid reflection with synchrotron radiation

High resolution synchrotron radiation has been used to investigate the occurrence of coherent hybrid reflections (CHR) in the In0.49Ga0.51P/GaAs(001) structure. Several φ scans at the 002 layer reflection were carried out. The scanned φ intervals are correlated by the [001] axis symmetry and should present the same pattern. A break in the symmetry is observed due to constructive/destructive interference of the hybrid amplitudes with the amplitude from the 002 layer reflection. The effects of substrate miscut and interface distance are taken into account to explain the observed patterns. The application of CHR as a high sensitive tool to analyze epitaxial growth is discussed.

X-ray imaging in advanced studies of ophthalmic diseases

Microscopic characterization of pathological tissues has one major intrinsic limitation, the small sampling areas with respect to the extension of the tissues. Mapping possible changes on vast tissues and correlating them with large ensembles of clinical cases is not a feasible procedure for studying most diseases, as for instance vision loss related diseases and, in particular, the cataract. Although intraocular lens implants are successful treatments, cataract still is a leading public-health issue that grows in importance as the population increases and life expectancy is extended worldwide. In this work we have exploited the radiation-tissue interaction properties of hard x-rays--very low absorption and scattering--to map distinct lesions on entire eye lenses. At the used synchrotron x-ray photon energy of 20 keV (wavelength lambda=0.062 nm), scattering and refraction are angular resolved effects. It allows the employed x-ray image technique to efficiently characterize two types of lesions in eye lenses under cataractogenesis: distributions of tiny scattering centers and extended areas of fiber cell compaction. The data collection procedure is relatively fast; allowing dozens of samples to be totally imaged (scattering, refraction, and mass absorption images) in a single day of synchrotron beam time. More than 60 cases of canine cataract, not correlated to specific causes, were investigated in this first application of x-rays to image entire lenses. Cortical opacity cases, or partial opacity, could be related to the presence of calcificated tissues at the cortical areas, clearly visible in the images, whose elemental contents were verified by micro x-ray fluorescence as very rich in calcium. Calcificated tissues were also observed at nuclear areas in some cases of hypermature cataract. Total opacity cases without distinguishable amount of scattering centers consist in 70% of the analyzed cases, where remarkable fissure marks owing to extended areas of fiber cell compaction are diagnosed.

Hybrid reciprocal space for X-ray diffraction in epitaxic layers

Even after several decades of systematic usage of X-ray diffraction as one of the major analytical tool for epitaxic layers, the vision of the reciprocal space of these materials is still a simple superposition of two reciprocal lattices: one from the substrate and the other from the layer. In this work, the general theory accounting for hybrid reflections in the reciprocal space of layer/substrate systems is presented. It allows insight into the non-trivial geometry of such reciprocal space as well as into many of its interesting properties. Such properties can be further exploited even on conventional-source X-ray diffractometers, leading to alternative, very detailed and comprehensive analyses of such materials.

Structural properties of Bi2Te3 topological insulator thin films grown by molecular beam epitaxy on (111) BaF2 substrates

Structural properties of topological insulator bismuth telluride films grown epitaxially on (111) BaF2 with a fixed Bi2Te3 beam flux were systematically investigated as a function of substrate temperature and additional Te flux. A layer-by-layer growth mode is observed since the early stages of epitaxy and remains throughout the whole deposition. Composition of the epitaxial films produced here stays between Bi2Te3 and Bi4Te5, as determined from the comparison of the measured x-ray diffraction curves with calculations. The substrate temperature region, where the growth rate remains constant, is found to be the most appropriate to obtain ordered Bi2Te3 films. Line width of the L = 18 Bi2Te3 diffraction peaks as low as 140 arcsec was obtained, indicating high crystalline quality. Twinning domains density rises with increasing growth temperature and reducing Te extra flux. X-ray reflectivity curves of pure Bi2Te3 films with thickness from 165 to 8 nm exhibited well defined interference fringes, evidencing ho...

Hybrid reciprocal lattice: application to layer stress determination in GaAlN/GaN(0001) systems with patterned substrates

Epitaxy of semiconductors is a process of tremendous importance in applied science and optoelectronic industry. Controlling of defects introduced during epitaxial growth is a key point in manufacturing devices of high efficiency and durability. In this work, we demonstrate how useful hybrid reflections are on the study of epitaxial structures with anisotropic strain gradients due to patterned substrates. High accuracy to detect and distinguish elastic and plastic relaxations are one of the greatest advantages of measuring this type of reflection, as well as the fact that it can be exploited in symmetrical reflection geometry on a commercial high-resolution diffractometer.

Strength tuning of multiple waves in crystals

In this work, the linear polarization of synchrotron radiation is explored as a tuning key for the strength of the simultaneously diffracted X-ray waves in crystals. The relative strength of the waves has been defined by the reflectivities of the Bragg reflections involved in each multiple-diffraction case and it has limited the applicability of the multiple-diffraction phenomenon. With a proper choice of the wavelength and the polarization direction of the incident synchrotron radiation, it is demonstrated how the intensity ratios of the simultaneously diffracted beams can be drastically changed.

Accurate triplet phase determination in non-perfect crystals – a general phasing procedure

A completely different approach to the problem of physically measuring the invariant triplet phases by three-beam X-ray diffraction is proposed. Instead of simulating the three-beam diffraction process to reproduce the experimental intensity profiles, the proposed approach makes use of a general parametric equation for fitting the profiles and extracting the triplet phase values. The inherent flexibility of the parametric equation allows its applicability to be extended to non-perfect crystals. Exploitation of the natural linear polarization of synchrotron radiation is essential for eliminating systematic errors and to provide accurate triplet phase values. Phasing procedures are suggested and demonstrative examples from simulated data are given.

Two-dimensional intensity profiles of effective satellites

The observation of a new X-ray scattering process with synchrotron radiation is reported. The phenomenon is analogous to three-beam diffraction in a single crystal; however, the features in the azimuthal scans are provided by superlattice-satellite reflections instead of bulk reflections. These features were named effective satellites and they are observed over the ordinary satellite reflections as a function of the azimuthal angle. Their occurrences have been monitored in completely different superlattices by mapping the incidence and azimuthal angles of the incident X-ray beam. Effects of structural parameters of the superlattices on the effective satellites as well as the information that can be extracted by measuring their positions are discussed.

X-ray phase measurements as a probe of small structural changes in doped nonlinear optical crystals

X-ray multiple diffraction experiments with synchrotron radiation were carried out on pure and doped nonlinear optical crystals: NH4H2PO4 and KH2PO4 doped with Ni and Mn, respectively. Variations in the intensity profiles were observed from pure to doped samples, and these variations correlated with shifts in the structure factor phases, also known as triplet phases. This result demonstrates the potential of X-ray phase measurements to study doping in this type of single crystal. Different methodologies for probing structural changes were developed. Dynamical diffraction simulations and curve fitting procedures were also necessary for accurate phase determination. Structural changes causing the observed phase shifts are discussed.