ABSTRACTA MgLi dilute alloy (6% wt. Li) has been studied by x‐ray emission spectroscopy in the ultra‐soft x‐ray range, 40–60 eV. For this purpose, a high‐resolution reflection zone plate spectrometer, working as a variable line grating spectrometer, was used on an electron probe microanalyser. With the experimental conditions, current and acceleration voltage of the incident electron beam, geometry, CCD detection, the Mg L emission band is easily observed. The Fermi edge of this band shifts toward the low photon energies with the Li content. The Li K emission band is hardly detectable despite the non‐negligible lithium mass fraction in the alloy. This is explained by the reabsorption of the lithium emission by the magnesium atoms, the reabsorption effect being strong in the present geometrical conditions of the experiment.

ABSTRACTHafnium compounds are fascinating due to their applications across diverse fields such as electronics, catalysis, nuclear energy, and biomedical materials. The study of chemical effects in hafnium compounds is necessary to check their purity and tailor their properties to meet the specific application requirements. The x‐ray intensity ratios, ILk/ILα (k = l, β, γ1,5, γ2,3, γ4), for 72Hf foil and its different compounds have been measured by tuning the synchrotron radiation energies across its Li (i = 1–3) absorption‐edge energies in order to investigate the influence of chemical effects on these intensity ratios in the presence of the many‐body effects. The present measured intensity ratios (ILk/ILα) have been compared with two sets of values calculated using the nonrelativistic Hartree–Fock–Slater model‐based Li (i = 1–3) subshell photoionization cross sections, the Dirac–Fock model‐based x‐ray emission rates, and two sets of the fluorescence and Coster–Kronig yields. The shift in L3 absorption‐edge of hafnium in its compounds has been deduced from the XANES spectra recorded in this study.

ABSTRACTThis study aims to understand the composition and application of red rock art from the Pedra do Maçaranduba archaeological site, located on the coast of Piauí (Brazil). This is a pioneering study of archaeological rock art sites found in the coastal region of Brazil. The research combines the techniques of optical microscopy, x‐ray fluorescence spectrometry, and Raman spectroscopy. The results suggest, through these techniques, that the pigments were applied in a liquid form (suspension with more diluent than raw material) and that wear caused by saline efflorescence and natural weathering is the primary conservation issue for the archaeological heritage. X‐ray fluorescence measurements showed the highest percentages of iron, ranging from 4.3% to 19.4% (w/w), with the intensity of the pigment's color increasing in proportion to the iron content. In addition, elements such as silicon (Si), aluminum (Al), phosphorus (P), sulfur (S), potassium (K), and calcium (Ca) were detected, suggesting their presence is due both to the substrate and to materials added to the paint to enhance properties like fixation and consistency. Raman spectroscopy indicated that hematite (α‐Fe2O3) is the main mineral component in the analyzed samples. These results enhance our understanding of prehistoric painting techniques and inform future conservation strategies for coastal rock art in Brazil.

ABSTRACTMaraging steels are high strength alloys used in applications that require both high mechanical strength and toughness. To achieve these properties, one of the heat treatments applied is solution treatment, although it can reduce toughness. This study compares the effect of two solution treatment temperatures, 910°C and 1100°C, on the microstructure and mechanical properties of a niobium‐containing maraging steel. Microstructural analysis was performed using X‐ray diffraction (XRD), electron backscatter diffraction (EBSD), light optical microscopy (LOM), and scanning electron microscopy (SEM). XRD analysis showed that dislocation density was higher for the sample treated at 1100°C. The XRD data were analyzed using the Williamson‐Hall method to estimate dislocation densities, and the Scherrer equation was applied to calculate crystallite sizes. EBSD revealed that solution treatment at 1100°C resulted in larger grain sizes and greater dissolution of Mo, Nb‐rich precipitates. Vickers hardness and Charpy impact tests were used to evaluate the mechanical properties. The Vickers hardness was slightly higher for the sample treated at 910°C due to the higher amount of precipitates present. In contrast, Charpy toughness increased with solution treatment temperature, reaching 98 J for the 1100°C condition, indicating greater impact energy absorption. Fractography showed predominantly ductile fractures in both conditions.

ABSTRACTThis paper presents a detailed study of L‐shell x‐ray intensity ratios, across the periodic table, including theoretical calculations, using the Multi‐Configuration Dirac‐Fock (MCDF) method, as well as empirical and semi‐empirical approaches. Our results are compared with existing values to assess the accuracy and reliability of the different methods. In‐depth data analysis reveals significant trends that could enhance the understanding of interaction mechanisms in L‐shell transitions. The results indicate a reasonable correlation with other studies, thereby providing a more comprehensive perspective on the L‐line intensity ratios and their applications in the field of atomic physics.

ABSTRACT Iridium and platinum have adjacent atomic numbers that account for the proximity of their x‐ray transition energies and thus the overlapping peaks in their x‐ray fluorescence spectra. This presents a challenge for the quantitative elemental analysis of IrO 2 ⋅2H 2 O‐Pt binary catalyst coatings, especially where the ‘Fundamental Parameter’ method is unavailable, as in the Niton XL3t energy dispersive x‐ray fluorescence analyser. Therefore, we studied the spectral resolution of the Lα, Lη and Lβ peaks for Ir and Pt as recorded on a Niton XL3t to identify the optimal regions of interest. These ROIs were used to measure a set of discrete Ir and Pt standard samples—in which the elemental loadings were derived from the mass and formulation of the catalyst coatings—for constructing correlation graphs to enable the conversion of x‐ray intensity data (cps μA −1 ) to elemental loading (mg cm −2 ). These correlation data were fitted to a quadratic regression. The overall measurement uncertainty for the elemental loadings was determined by combining the residual standard error in the quadratic regression with the uncertainty for the elemental loadings used in the construction of the correlation graph, yielding ±0.07 mg cm −2 for Ir (ROI: 9.00–9.18 keV) and ± 0.04 mg cm −2 for Pt (ROI: 9.36–9.65 keV). The quadratic functions and their corresponding ROIs were programmed into the analyser to measure a set of IrO 2 ⋅2H 2 OPt binary standard samples. This revealed a strong agreement between the elemental loadings as displayed on the analyser and those derived from the mass and formulation of these standard samples.

ABSTRACT This manuscript details the advancements in developing a unique multimodal imaging setup, specifically the integration of X‐AFM on a synchrotron beamline that currently combines STXM and XRF. This triplet configuration operates within the soft x‐ray regime (< 2.5 keV) and necessitates high vacuum instrumentation, targeting sub‐micrometric applications with nanometric precision. Building on a previously successful prototype, the paper presents the current setup, the challenges encountered, and the solutions implemented. Additionally, it highlights significant custom developments in specialized electronics that enabled practical utilization of the new instrument. In particular, multiple samples, including asbestos fibers from a broader high‐impact research project, were measured and characterized in situ for the first time. The overall performance is critically evaluated through an ex‐situ comparison with a commercial single‐modality AFM system. Finally, the manuscript discusses the roadmap for future advancements in related instrumentation, methods, and applications.

ABSTRACTIn x‐ray fluorescence analysis (XRFA), the use of secondary targets to suppress measurement background is a common practice aimed at reducing detection limits. However, conventional polarized secondary targets often exhibit low conversion efficiency of primary x‐rays. In this paper, we propose a novel hemispherical secondary target designed to exploit a focusing‐like phenomenon for primary x‐rays, thereby enhancing the conversion efficiency and achieving improved background suppression. The optimal dimensions of the hemispherical secondary target are determined through theoretical calculations, and further validated through Monte Carlo simulations and experimental analysis. Our findings reveal a substantial enhancement in the peak‐to‐background ratio when compared to traditional polarized secondary targets. Specifically, for a 1000‐ppm Ce sample, the peak‐to‐background ratio increased from 8.45 to 9.78 with the implementation of the hemispherical secondary target. Similar improvements were observed when measuring a 1000‐ppm Ce sample, relative to direct excitation. Furthermore, the relative error between the system and the ICP‐MS measurement results of the rare earth sample remains within 5%, underscoring the effectiveness of the hemispherical secondary target in XRFA applications.