Search Results (409)

This work presents a comparative study of graphene exfoliation technologies from various graphite precursors—spectral graphite and thermally expanded graphite (Graflex)—using ultrasonic treatment and electrochemical methods in the presence of the ionic surfactant Nafion. The influence of exfoliation parameters, the nature of the starting material, and the presence of surfactant additives on the morphology, dispersibility, stability, and structural characteristics of the resulting graphene-containing dispersions was investigated. Particular attention is paid to a two-step technology combining pulsed electrochemical exfoliation with subsequent mild ultrasonic treatment. Comprehensive characterization of the samples was carried out using UV–Vis spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), electron microscopy, electron diffraction (ED), dynamic light scattering (DLS), and X-ray photoelectron spectroscopy (XPS). It was found that the use of Nafion significantly enhances exfoliation efficiency and contributes to the stabilization of the dispersions. Graphene sheets obtained from Graflex exhibit significantly larger lateral dimensions (up to 1 μm or more) compared to those exfoliated from spectral graphite (100–300 nm). The approach combining the use of Graflex and pulsed electrochemical exfoliation in the presence of Nafion with subsequent low-power ultrasonic treatment enables the production of few-layer graphene (1–3 layers) with high stability. Full article

X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) are analytical techniques enabling precise analysis of the electronic structure and local atomic environment in chemical compounds and materials. Their application spans materials science, chemistry, biology, and environmental sciences, supporting studies on catalytic mechanisms, redox processes, and metal speciation. A key advantage of both techniques is element selectivity, allowing the analysis of specific elements without matrix interference. Their high sensitivity to chemical state and coordination enables determination of oxidation states, electronic configuration, and local geometry. These methods are applicable to solids, liquids, and gases without special sample preparation. Modern XAS and XES studies are typically performed using synchrotron radiation, which provides an intense, monochromatic X-ray source and allows advanced in situ and operando experiments. Sub-techniques such as XANES (X-ray absorption near-edge structure), EXAFS (Extended X-ray Absorption Fine Structure), and RIXS (resonant inelastic X-ray scattering) offer enhanced insights into oxidation states, local structure, and electronic excitations. Despite their broad scientific use, applications in pharmaceutical research remain limited. Nevertheless, recent studies highlight their potential in analyzing crystalline active pharmaceutical ingredients (APIs), drug–biomolecule interactions, and differences in drug activity. This review introduces the fundamental aspects of XAS and XES, with an emphasis on practical considerations for pharmaceutical applications, including experimental design and basic spectral interpretation. Full article

Accelerated artificial aging of zinc oxide (ZnO)-based acrylic artists’ paint, filled with calcium carbonate (CaCO₃) as an extender, was carried out for a total of 1963 h (~8 × 10⁷ lux·h), with assessments at specific intervals. The total color difference ΔE* was <2 (CIELab-76 system) over 1725 h of aging, while the human eye notices color change at ΔE* > 2. Oxidative degradation of organic components in the paint to form volatile products was revealed by attenuated total reflectance–Fourier transform infrared (ATR-FTIR) spectroscopy, micro-Raman spectroscopy, and scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS). It appears that deep oxidation of organic intermediates and volatilization of organic matter may be responsible for the relatively small value of ΔE* color difference during aging of the samples. To elucidate the degradation pathways, principal component analysis (PCA) was applied to the spectral data, revealing: (1) the catalytic role of ZnO in accelerating photodegradation, (2) the Kolbe photoreaction, (3) the decomposition of the binder to form volatile degradation products, and (4) the relative photoinactivity of CaCO₃ compared with ZnO, showing slower degradation in areas with a higher CaCO₃ content compared with those dominated by ZnO. These results provide fundamental insights into formulation-specific degradation processes, offering practical guidance for the development of more durable artist paints and conservation strategies for acrylic artworks. Full article

The Hard X-ray Modulation Telescope (HXMT), China’s first X-ray astronomy satellite, has significantly contributed to the study of fast variability in black hole X-ray binaries through its broad energy coverage (1–250 keV), high timing resolution, and sensitivity to hard X-rays. This review presents a comprehensive overview of timing analysis techniques applied to black hole X-ray binaries using Insight-HXMT data. We introduce the application and comparative strengths of several time-frequency analysis methods, including traditional Fourier analysis, wavelet transform, bicoherence analysis, and Hilbert-Huang transform. These methods offer complementary insights into the non-stationary and nonlinear variability patterns observed in black hole X-ray binaries, particularly during spectral state transitions and quasi-periodic oscillations. We discuss how each technique has been employed in recent Insight-HXMT studies to characterize timing features such as low-frequency QPOs, phase lags, and power spectrum evolution across different energy bands. Moreover, we present novel phenomena revealed by Insight-HXMT observations, including the detection of high-energy QPOs, spectral parameter modulation with QPO phase, and a new classification scheme for QPO types. The integration of multiple analysis methods enables a more nuanced understanding of the accretion dynamics and the geometry of the inner accretion flow, shedding light on fundamental physical processes in relativistic environments. Full article

Lead-free perovskite variants have emerged as promising candidates due to their self-trapped exciton emission. However, in ASnX₃ systems, facile oxidation of Sn(II) to Sn(IV) yields A₂SnCl₆ vacancy-ordered derivatives. Paradoxically, despite possessing a direct bandgap, these variants exhibit diminished photoluminescence (PL). Doping engineering thus becomes essential for precise optical tailoring of A₂SnX₆ materials. Herein, through integrated first-principles calculations and spectroscopic analysis, we elucidate the luminescence mechanism in Te⁴⁺-doped (NH₄)₂SnCl₆ lead-free perovskites. Density functional theory, X-ray diffraction (XRD) patterns and X-ray photoelectron spectroscopy (XPS) confirm Te⁴⁺ substitution at Sn sites via favorable chemical potentials. Spectral interrogations, including absorption and emission profiles, reveal that the intense emission originates from the triplet STE recombination (³P₁ → ¹S₀) of Te centers. Temperature-dependent PL spectra further demonstrate strong electron–phonon coupling that induces symmetry-breaking distortions to stabilize STEs. Complementary electronic band structure and molecular orbital calculations unveil the underlying photophysical pathway. Leveraging these distinct thermal responses of PL intensity and peak position, 0.5%Te:(NH₄)₂SnCl₆ emerges as a highly promising candidate for non-contact, dual-parameter optical thermometry over an ultra-broad range (100–400 K). This work provides fundamental insights into the exciton dynamics and thermal engineering of optical properties in this material system, establishing its significant potential for advanced temperature-sensing applications. Full article

$\gamma$ Cas analogs is an enigmatic group of Be stars with unusually hard X-rays and an X-ray luminosity of ${10}^{31}$–${10}^{33}$erg $s^{-1}$, which is higher than a typical value for classical Be stars. The evolutionary status of these mysterious objects and the nature of their X-ray emission remains disputable. I suppose that our understanding of this mystery is in the detailed studies of their optical and X-ray variability on the various time scales from very short to very long. In the present paper the optical and X-ray spectral and photometric observations of these stars are reviewed. The contemporary assumptions on the mechanisms of X-ray radiation generation of $\gamma$ Cas analogs are discussed. It is concluded that the analysis of the binarity of $\gamma$ Cas analog helps to understand their inexplicable nature. Full article

The growing demand for sustainable, gluten-free alternatives has positioned breadfruit (Artocarpus altilis) flour as a promising multifunctional ingredient. This study comprehensively evaluated commercial breadfruit flour from Mauritius using advanced analytical techniques, including volatiles analysis, Fourier-Transform Infrared Spectroscopy, X-ray diffraction, and rheometry. The flour exhibited interesting techno-functional properties with significant water-binding capacity (6.18 ± 0.45 H₂O/g DM) and concentration-dependent pasting behavior, achieving 17.895 mPa·s peak viscosity at 16% suspensions with elastic-dominated gel characteristics. Notably, FT-IR spectral analysis revealed a high similarity (95.68%) to acarbose (GLUCOBAY), warranting further biochemical investigation. The flour demonstrated superior oxidative stability (46.3 h) and significant antioxidant capacity, with methanolic extracts yielding 2.27 ± 0.31 mg GAE/g phenolic content and enhanced radical scavenging activities against 2,2-diphenyl-1-picrylhydrazyl (DPPH) 2.81 ± 0.23 μg TE/g and 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) 31.24 ± 0.26 μg TE/g. These findings establish breadfruit flour as a multifunctional ingredient combining excellent technological properties, exceptional oxidative stability, and bioactive applications, positioning it as a valuable sustainable alternative for gluten-free products and functional foods targeting metabolic health management. Full article

Multispectral remote sensing offers powerful capabilities for mineral exploration, particularly in regions with complex geological settings. This study investigates the mineralization potential of the Tidili region in Morocco, located between the South Atlasic and Anti-Atlas Major Faults, using Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) imagery to extract hydrothermal alteration zones. Key techniques include band ratio analysis and Principal Components Analysis (PCA), supported by the Crósta method, to identify spectral anomalies associated with alteration minerals such as Alunite, Kaolinite, and Illite. To validate the remote sensing results, field-based geological mapping and mineralogical analysis using X-ray diffraction (XRD) were conducted. The integration of satellite data with ground-truth and laboratory results confirmed the presence of argillic and phyllic alteration patterns consistent with porphyry-style mineralization. This integrated approach reveals spatial correlations between alteration zones and structural features linked to Pan-African and Hercynian deformation events. The findings demonstrate the effectiveness of combining multispectral remote sensing images analysis with field validation to improve mineral targeting, and the proposed methodology provides a transferable framework for exploration in similar tectonic environments. Full article

Three new series of indolizines (5a–f, 6a–f and 7a–g), functionalized with bromine or ethyl ester substituents on the pyridine ring, were designed and synthesized as promising anticancer agents. The synthesis of indolizine derivatives was carried out using the 1,3-dipolar cycloaddition of pyridinium N-ylides to ethyl propiolate as a key step. Spectral characterization (using NMR, FT-IR, HRMS and X-ray diffraction) showed that two types of cycloadducts 5a–f and 6a–f were obtained when the ylides generated by the 3-bromopyridinium salts were used as 1,3-dipoles in Huisgen cycloaddition reactions to ethyl propiolate. The anticancer effect of selected compounds was in vitro assessed against the National Cancer Institute (NCI) panel of 60 human tumor cells, at 10 μM concentration, with three compounds (5c, 6c and 7g) showing promising inhibitory activity on the growth of several cell lines including lung, brain, renal cancer and melanoma, as well as a cytotoxic effect against HOP-62 non-small cell lung cells (34% for compound 5c and 15% for compound 7g) and SNB-75 glioblastoma cells (15% for compound 5c and 14% for derivative 7c). Molecular docking revealed favorable binding affinities for 5c, 6c and 7g (–9.22 to –9.88 kcal/mol) at the colchicine-binding site of tubulin with key interactions involving βASN-258, βALA-317, and βLYS-352 residues for 5c, βASN-258 in case of 6c, and αVAL-181 and βLYS-254 for derivative 7g. According to the in silico ADMET analysis, the active compounds are predicted to exhibit good oral bioavailability, promising drug-like qualities and low toxicity risks. Full article

Schiff base ligands prepared from salicylaldehyde and 2-, 3- and 4-methoxybenzylamine were used to prepare copper(II) complexes, characterized by spectral methods, elemental analysis and X-ray crystallography in the case of complex 4a derived from 2-methoxybenzylamine. The DNA cleavage activity of the prepared complexes was exceptional, with best activities of over 95% one-strand cleavage for 4c at 3 mM and full double-strand cleavage for complex 4a at 5 mM. Absorption titration studies with ct-DNA revealed good binding constants (at 10⁵ M⁻¹) with a decrease of up to 56% light absorption. Meanwhile, the EB–DNA displacement method and viscosity studies revealed groove binding as a possible binding mode. For BSA binding studies, all three complexes showed K_BSA values in the optimal range for reversible BSA binding (10⁴ M⁻¹). The copper(II) complexes showed significant cytotoxic effects (67–96% at 1 mM) in mitochondrial activity monitoring assays. Cytotoxicity was confirmed against cancer cell lines (A549 and HepG2) and HEL cells. The complexes 4a and 4c exhibited high activity against HepG2 cancer cells (IC50 < 22 μM), comparable to cisplatin. The radical scavenging activity was determined by the INT method with the best IC50 for 4c (189 ± 11 μM). Overall, complexes 4a and 4c with a methoxy group in the ortho and para positions show high potential in most determined activities, but mainly as DNA cleavers and as cytotoxic agents with selectivity against HepG2 cells. Full article

The analysis of historical pigments contributes significantly to understanding the materials and techniques used in artworks and in preserving cultural heritage. This work introduces a novel methodology for classifying historical pigments combining X-ray fluorescence (XRF) spectroscopy with machine learning techniques. We applied this approach to a representative heterogeneous dataset of historical pigments from the open-access spectral library INFRA-ART, as well as commercial oil colors and pigments with different particle sizes. A comparative analysis through principal component analysis (PCA) and hierarchical cluster analysis (HCA) demonstrates the advantages of the full-spectrum method over conventional peak-based strategies, offering improved classification performances and robustness. Employing the entire spectrum, it is possible to access additional key features for pigment discrimination that are discarded during the computation of the traditional methods and it is possible to have an efficient feature extraction even in more complex samples. This approach offers significant advantages by allowing the simultaneous processing of extensive datasets, which is useful for interpreting real-world scenarios in cultural heritage that are characterized by high heterogeneity. Full article

Background/Objectives: This study aimed to evaluate the efficacy of a 445 nm diode laser in enhancing enamel resistance to acid-induced demineralization and to investigate the associated compositional and structural modifications using scanning electron microscopy (SEM), electron spectroscopy for chemical analysis (ESCA), and X-ray diffraction (XRD) crystallographic analysis. Methods: A total of 126 extracted human teeth were used. A total of 135 (n = 135) enamel discs (4 × 4 mm) from 90 teeth were assigned to either a laser-irradiated group or an untreated control group for SEM, ESCA, and XRD analyses. Additionally, 24 mono-rooted teeth were used to measure pulp temperature changes during laser application. Laser irradiation was performed using a 445 nm diode laser with a pulse width of 200 ms, a repetition rate of 1 Hz, power of 1.25 W, an energy density of 800 J/cm², a power density of 3980 W/cm², and a 200 µm activated fiber. Following acid etching, SEM was conducted to assess microstructural and ionic alterations. The ESCA was used to evaluate the Ca/P ratio, and XRD analyses were performed on enamel powders to determine changes in phase composition and crystal lattice parameters. Results: The laser protocol demonstrated thermal safety, with minimal pulp chamber temperature elevation (0.05667 ± 0.04131 °C). SEM showed that laser-treated enamel had a smoother surface morphology and reduced acid-induced erosion compared with controls. Results of the ESCA revealed no significant difference in the Ca/P ratio between groups. XRD confirmed the presence of hydroxyapatite structure in laser-treated enamel and detected an additional diffraction peak corresponding to a pyrophosphate phase, potentially enhancing acid resistance. Results of the spectral analysis showed the absence of α-TCP and β-TCP phases and a reduction in the carbonate content in the laser group. Furthermore, a significant decrease in the a-axis lattice parameter suggested lattice compaction in laser-treated enamel. Conclusions: Irradiation with a 445 nm diode laser effectively enhances enamel resistance to acid demineralization. This improvement may be attributed to chemical modifications, particularly pyrophosphate phase formation, and structural changes including prism-less enamel formation, surface fusion, and decreased permeability. These findings provide novel insights into the mechanisms of laser-induced enhancement of acid resistance in enamel. Full article

PSR B1259-63/LS 2883 is a well-studied gamma-ray binary hosting a pulsar in a 3.4-year eccentric orbit around a Be-type star. Its non-thermal emission spans from radio to TeV energies, exhibiting a significant increase near the periastron passage. This paper is dedicated to the analysis of INTEGRAL observations of the system following its last periastron passage in June 2024. We aim to study the spectral evolution of this gamma-ray binary in the soft (0.3–10 keV) and hard (30–300 keV) X-ray energy bands. We performed a joint analysis of the data taken by INTEGRAL/ISGRI in July–August 2024 and quasi-simultaneous Swift/XRT observations. The spectrum of the system in the 0.3–300 keV band is well described by an absorbed power law with a photon index of $\Gamma =1.42\pm 0.03$. We place constraints on potential spectral curvature, limiting the break energy $E_{\mathrm{b}}>30$ keV for $\Delta \Gamma >0.3$ and cutoff energy $E_{\mathrm{cutoff}}>150$ keV at a 95% confidence level. For one-zone leptonic emission models, these values correspond to electron distribution spectral parameters of $E_{\mathrm{b},\mathrm{e}}>0.8$ TeV and $E_{\mathrm{cutoff},\mathrm{e}}>1.7$ TeV, consistent with previous constraints derived by H.E.S.S. Full article

The object of this study is welded joints of AISI 321 and Ti-6Al-4V, obtained by diffusion welding on developed conical surfaces. The problem of creating bimetallic joints of AISI 321 and Ti-6Al-4V with developed conical contact surfaces, using diffusion welding through an intermediate Electrolytic Tough Pitch Copper (Cu-ETP) copper layer, was solved. The joints were studied using micro-X-ray spectral analysis, microstructural analysis, and mechanical tests. High mutual diffusion of copper and titanium, along with increased concentrations of Cr and V in copper, was detected. The shear strength of the obtained welded joints is 250 MPa and 235 MPa at 30 min and 15 min, respectively, which is higher than the copper layer’s strength (180 MPa). The obtained results are explained by the dislocation diffusion mechanism in the volume of grains and beyond, due to thermal deformations during welding. Under operating conditions of internal pressure and cryogenic temperatures, the strength of the connection is ensured by the entire two-layer structure, and tightness is ensured by a vacuum-tight diffusion connection. The obtained strength of the connection (250 MPa) is sufficient under the specified operating conditions. Analysis of existing solutions in the literature review indicates that industrial application of technology for manufacturing bimetallic adapters from AISI 321 stainless steel and Ti-6Al-4V titanium alloy is limited to butt joints with small geometric dimensions. Studies of the transition zone structure and diffusion processes in bimetallic joints with developed conical contact surfaces enabled determination of factors affecting joint structure and diffusion coefficients. The obtained bimetallic adapters, made of Ti-6Al-4V titanium alloy and AISI 321 stainless steel, can be used to connect titanium high-pressure vessels with stainless steel pipelines. Full article

The Sierra Minera de Cartagena-La Unión, located in southeast of the Iberian Peninsula, has been significantly impacted by historical mining activities, which resulted in environmental degradation, including acid mine drainage (AMD) and heavy metal contamination. This study evaluates the potential of PRISMA hyperspectral imagery for multi-temporal mapping of AMD-related minerals in two mining-affected drainage basins: Beal and Gorguel. Key minerals indicative of AMD—iron oxides and hydroxides (hematite, jarosite, goethite), gypsum, and aluminium-bearing clays—were identified and mapped using band ratios applied to PRISMA data acquired over five dates between 2020 and 2024. Additionally, Sentinel-2 data were incorporated in the analysis due to their higher temporal resolution to complement iron oxide and hydroxide evolution from PRISMA. Results reveal distinct temporal and spatial patterns in mineral distribution, influenced by seasonal precipitation and climatic factors. Jarosite was predominant after torrential precipitation events, reflecting recent AMD deposition, while gypsum exhibited seasonal variability linked to evaporation cycles. Goethite and hematite increased in drier conditions, indicating transitions in oxidation states. Validation using X-ray diffraction (XRD), laboratory spectral curves, and a larger time-series of Sentinel-2 imagery demonstrated strong correlations, confirming PRISMA’s effectiveness for iron oxides and hydroxides and gypsum identification and monitoring. However, challenges such as noise, striping effects, and limited image availability affected the accuracy of aluminium-bearing clay mapping and limited long-term trend analysis. Full article