Search Results (113)

Graphene oxide (GO) and reduced graphene oxide (rGO) are widely studied two-dimensional carbon nanomaterials for optoelectronic devices. Because the oxygen content and degree of reduction govern the electronic structure of GO-derived films, controlling the reduction process is essential for tailoring their properties. Laser-induced reduction provides a tunable, contact-free route to transparent and conductive graphene-based layers. In this work, 80 nm spray-coated GO layers were reduced using a KrF excimer laser (248 nm, 20 ns) at a fluence of 20 mJ cm⁻², while systematically varying the number of laser pulses (LP) from 1 to 1000. We tuned the degree of GO reduction by stepwise increasing the number of LP and followed the resulting changes in surface composition using X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine-structure (NEXAFS) spectroscopy. The surface composition evolves non-monotonically with the number of laser pulses, revealing a multi-step reduction mechanism. At low laser doses, epoxide groups are preferentially removed or converted, generating a more disordered distribution of hydroxyl-containing sites on the GO sheets. At intermediate laser doses, oxygen-containing groups are depleted, and sp² conjugation is restored. After extended irradiation in air, however, oxygenated surface species partially re-form. Conductivity measurements show that the sheet resistance reaches a minimum at approximately 300 LP, consistent with efficient chemical reduction and recovery of the conjugated carbon network. These results provide molecular-level guidelines for optimizing laser-induced GO reduction toward graphene-based transparent conductive layers. Full article

Graphene-based composite materials have attracted much attention for a range of applications in various fields, including electronics, sensing, catalysis, energy storage and conversion. Single-step large-scale microwave plasma synthesis of graphene and nitrogen-doped graphene (N-graphene) composite materials has been demonstrated. The developed atmospheric pressure plasma method allows continuous synthesis of different graphene-based hybrids in a controllable and environmentally friendly manner. Control over the synthesis process, i.e., size, uniformity, surface distribution of the nanoparticles and graphene/N-graphene quality, was provided by adjusting plasma parameters and injection configuration. Protocols for the production of particular composites, i.e., graphene-MnO, N-graphene-MnO, N-graphene-MnS, and N-graphene-Fe_xO_y, have been established using methane and acetonitrile as precursors. A comprehensive physicochemical characterization of the produced composites was conducted using high-resolution transmission electron microscopy, scanning transmission electron microscopy, Raman spectroscopy, X-ray diffraction, and near-edge X-ray-absorption fine-structure and X-ray photoelectron spectroscopies. Full article

Gold nanorods (AuNRs) were synthesized and optimized with the aim of obtaining strongly hydrophilic nanomaterials, suitable as a drug delivery system (DDS) for copper-based drugs. After careful purification, AuNRs were characterized by ultraviolet–visible–near-infrared spectroscopy (UV–Vis–NIR), showing two typical localized surface plasmon resonance (LSPR) bands in the range 550–750 nm. Fourier Transform Infrared (FT-IR) and high-resolution X-ray photoelectron (HR-XPS) spectroscopies verified the surface functionalization. Transmission electron microscopy (TEM) showed AuNRs with regular shape and size, with an aspect ratio (AR) of 2.6. Dynamic Light Scattering (DLS) measurements confirmed the size and the stability in water for up to 3 months. The AuNRs were conjugated with copper(I) drugs, i.e., [Cu(PTA)₄]BF₄ (PTA = 1,3,5-triaza-7-phosphadamantane). The drug loading procedures and efficiency were optimized, and the best loading was η (%) = 50 ± 7%. The non-covalent interactions of the Cu(I) complex with the AuNRs were studied by means of UV–Vis–NIR, ζ-potential, HR-TEM, FT-IR, synchrotron radiation-induced X-ray photoelectron (SR-XPS), and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy measurements. The MTT assay performed on Vero E6 cells showed that AuNRs and AuNR-Cu(I) conjugates had no significant effect on cell viability, being biocompatible, causing a reduction in cell viability only after prolonged exposure. Full article

A lens-coupled high-speed X-ray camera, “Hayaka”, was developed for quick imaging of X-ray absorption fine structure (XAFS) and time-resolved high-speed computed tomography (CT) using synchrotron radiation (SR). This camera is a lens-coupled type, composed of a scintillator, an imaging lens system, and a high-speed visible light sCMOS, capable of imaging with a minimum exposure time of 1 μs and a maximum frame rate of 5000 frames/s (fps). A feasibility study using white and monochromatic SR at the beamline BL07 of the SAGA Light Source showed that fine X-ray images with a spatial resolution of 77 μm can be captured with an exposure time of 10 μs. Furthermore, quick imaging XAFS, combined with high-speed energy scanning of a small Ge double crystal monochromator of the same beamline, enabled spectral image data to be acquired near the Cu K-edge in a minimum of 0.5 s. Additionally, an in coquendo 4DCT (time-resolved 3D observation of cooking processes) observation combined with a high-speed rotation table revealed the boiling process of Japanese somen noodles over 150 s with a time resolution of 0.5 s. Full article

L. ferrooxidans and their metabolic products have been explored as viable flotation reagents of pyrite and chalcopyrite for froth flotation. Scanning electron microscopy (SEM), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, time-of-flight secondary ion mass spectrometry (ToF-SIMS) and captive bubble contact angle measurements have been used to examine the surface physicochemical properties of pyrite upon exposure to L. ferrooxidans grown in HH medium at pH 1.8. C K-edge NEXAFS spectra, collected using scanning transmission X-ray microscopy (STXM), indicate hydrophilic lipids, fatty acids, and biopolymers are formed at the mineral–bacterium interface within hours of exposure. The Fe L-edge NEXAFS show oxidation of the mineral surface from Fe (II) sulfide to Fe (III) oxyhydroxides. The leaching of the iron species at the pyrite surface is accelerated in the presence of L. ferrooxidans and extracellular polymeric substances (EPS) as compared to HH medium controls, as shown by ToF-SIMS. The surface chemical changes induced by the interaction with L. ferrooxidans show a significant decrease in surface hydrophobicity within the first 2 h of exposure. The implications of these findings are the potential use of EPS, produced during early attachment of L. ferrooxidans, as a depressant for bioflotation or to enhance bioleaching. Full article

Composite materials based on low-density polyethylene (LDPE) embedded with iron-manganese nanoparticles with compositions Fe_0.9Mn_0.1 and Fe_0.8Mn_0.2 were prepared and investigated. The newly created composites were characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray absorption near-edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and Mössbauer spectroscopy. The composition, electronic, and atomic structure of the nanoparticles were established. The study confirms that the nanoparticles possess a ‘core-shell’ structure, the nature of which depends on the manganese content. The nanoparticles of Fe_0.8Mn_0.2 in LDPE exhibit a three-layered structure: a metallic α-Fe core is coated with an intermediate oxidized layer structurally close to Fe₂O₃, while the outermost shell consists of manganese oxide (Mn₂O₃). In contrast, nanoparticles with lower Mn content Fe_0.9Mn_0.1 show a predominantly fully oxidized structure. This structural evolution is consistent with thermodynamic principles, where manganese, having a higher oxide formation enthalpy, migrates to the surface. The core–shell architecture is promising for applications requiring stable magnetic components or tailored catalytic interfaces within a polymer matrix. 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

Carbon nanotubes (CNTs) have remarkable mechanical, electrical, and thermal properties, making them highly attractive as foundational elements for advanced materials. However, translating their nanoscale potential into macroscale reliability and longevity requires a holistic design approach that integrates precise architectural control with robust damage mitigation strategies. This review presents a synergistic perspective on enhancing the durability of CNT-based systems by critically examining the interplay between molecular assembly, self-repair mechanisms, and the advanced characterization techniques required for their validation. We first establish how foundational architectural control—achieved through strategies like chemical functionalization, field-directed alignment, and dispersion—governs the ultimate performance of CNT materials. A significant focus is placed on advanced functionalization, such as fluorination, and its verification using high-powered spectroscopic tools, including X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. Subsequently, this manuscript delves into the mechanisms of self-repair, systematically analyzing both the intrinsic capacity of the carbon lattice to heal atomic-level defects and the extrinsic strategies that incorporate engineered healing agents into composites. This discussion is uniquely supplemented by an exploration of the experimental techniques, such as electron energy loss spectroscopy (EELS) and Auger electron spectroscopy (AES), that provide crucial evidence for irradiation-induced healing dynamics. Finally, we argue that a “characterization gap” has limited the field’s progress and highlight the critical role of techniques like in situ Raman spectroscopy for quantitatively monitoring healing efficiency at the molecular level. By identifying current challenges and future research frontiers, this review underscores that the creation of truly durable materials depends on an integrated understanding of how to build, repair, and precisely measure CNT-based systems. Full article

Ce₂Pt₆Ga₁₅ is a heavy fermion compound near the quantum critical point (QCP). Its crystal structure may exhibit magnetic frustration due to a honeycomb arrangement; however, stacking faults in the crystal hinder structural analysis. As a local structure probe, extended X-ray absorption fine structure (EXAFS) is less sensitive to stacking faults and is a powerful tool for crystal structure determination. We synthesized single-crystal Ce₂Pt₆Ga₁₅, performed single-crystal and powder X-ray diffraction experiments, and conducted X-ray absorption spectroscopy (XAS) measurements. The composition of Ce₂Pt₆Ga₁₅ deviates from stoichiometry, suggesting Ce and Ga enrichment or Pt site deficiencies. A comparison of X-ray absorption near-edge structure (XANES) at the Ce L₃-edge with reference materials suggests that Ce valence is likely trivalent. To determine the exact structure, we simultaneously analyzed EXAFS spectra at the Ce L₃-, Pt L₃-, and Ga K-edges. The EXAFS spectra of Ce₂Pt₆Ga₁₅ are inconsistent with the hexagonal Sc_0.6Fe₂Si_4.9-type structure but are better explained by an orthorhombic structure with a honeycomb arrangement. Full article

The total-ion-yield (TIY) near-edge X-ray absorption fine-structure (NEXAFS) spectra of two dipeptides were measured and analyzed to identify the excitation sites of core electrons and the corresponding destination molecular orbitals. Peptide molecules were transferred to the gaseous phase using traditional heating and MALDI methods, ensuring that the resulting NEXAFS spectra and fragmentation products were consistent across both approaches. Mass spectra obtained at various excitation energies revealed the branching ratios of products at each energy level, offering insights into specific dissociation phenomena. Notably, variations in excitation energy demonstrated a selective dissociation process, with certain products forming more efficiently. This specificity appears closely linked to dissociations near the peptide bond, where the nodal planes of destination molecular orbitals are located. These findings were validated using both small peptide models and peptoid molecules, highlighting consistent patterns in the dissociation behavior. Full article

This study explores the phase composition, local atomic structure, and magnetic properties of biogenic nanomaterials synthesized through microbially mediated biomineralization by the sulfate-reducing bacterium Desulfovibrio species strain A2 (Cupidesulfovibrio). Using X-ray diffraction (XRD), transmission electron microscopy (TEM), Mössbauer spectroscopy, X-ray absorption near-edge structure (XANES) spectroscopy, extended X-ray absorption fine structure (EXAFS) spectroscopy, and magnetic measurements, we identified a mixture of vivianite (Fe₃(PO₄)₂·8H₂O) and sulfur-containing crystalline phases (α-sulfur). XRD analysis confirmed that the vivianite phase, with a monoclinic I2/m structure, constitutes 44% of the sample, while sulfur-containing phases (α-sulfur, Fddd) account for 56%, likely as a result of bacterial sulfate-reducing activity. X-ray absorption spectroscopy (XAS) and EXAFS revealed the presence of multiple sulfur oxidation states, including elemental sulfur and sulfate (S⁶⁺), underscoring the role of sulfur in the sample’s structure. Mössbauer spectroscopy identified the presence of ferrihydrite nanoparticles with a blocking temperature of approximately 45 K. Magnetic measurements revealed significant coercivity (~2 kOe) at 4.2 K, attributed to the blocked ferrihydrite nanoparticles. The results provide new insights into the structural and magnetic properties of these microbially mediated biogenic nanomaterials, highlighting their potential applications in magnetic-based technologies. Full article

MgZnO possesses a tunable bandgap and can be prepared at relatively low temperatures, making it suitable for developing optoelectronic devices. Mg_xZn_1−xO (x~0.1) films were grown on sapphire by metal–organic vapor phase epitaxy under different substrate-growth temperatures T_s of 350–650 °C and studied by multiple characterization technologies like X-ray diffraction (XRD), spectroscopic ellipsometry (SE), Raman scattering, extended X-ray absorption fine structure (EXAFS), and first-principle calculations. The effects of T_s on the optical, structural, and surface properties of the Mg_0.1Zn_0.9O films were studied penetratively. An XRD peak of nearly 35° was produced from Mg_0.1Zn_0.9O (0002) diffraction, while a weak peak of ~36.5° indicated MgO phase separation. SE measurements and analysis determined the energy bandgaps in the 3.29–3.91 eV range, obeying a monotonically decreasing law with increasing T_s. The theoretical bandgap of 3.347 eV, consistent with the SE-reported value, demonstrated the reliability of the SE measurement. Temperature-dependent UV-excitation Raman scattering revealed 1LO phonon splitting and temperature dependency. Zn-O and Zn-Zn atomic bonding lengths were deduced from EXAFS. It was revealed that the surface Mg amount increased with the increase in T_s. These comprehensive studies provide valuable references for Mg_0.1Zn_0.9O and other advanced materials. Full article

Two new Ag(I) complexes with coumaric carboxylic acid derivatives have been synthesized. Structural studies of these noncrystalline complexes have been performed using a methodology that combines laboratory and synchrotron techniques, supported by density functional theory calculations. The arrangement of ligands around the Ag(I) cation has been refined using infrared, extended X-ray absorption fine structure, and X-ray absorption near edge structure spectroscopies. Different coordination modes of carboxylate ligands are observed for the studied compounds. Carboxylate bridges are characteristic for the Ag(I) complex with 4-oxo-4H-1-benzopyran-2-carboxylic acid (1), while a bidentate chelating motif was found for the complex with 2-oxo-2H-1-benzopyran-3-carboxylic acid (2). Additionally, the carbonyl oxygen atom of the coumarin ring coordinates to the silver cation in complex 2, while it is inactive in complex 1. Antimicrobial evaluation has been performed for both compounds. The complexes show activity against selected bacteria as well as Candida yeast. This activity is slightly lower for bacteria and the same or higher for Candida in relation to the reference substances: ciprofloxacin or fluconazole. Full article

This study conducted adsorption experiments using Europium (Eu(III)) on geological materials collected from Taiwan. Batch tests on argillite, basalt, granite, and biotite showed that argillite and basalt exhibited strong adsorption reactions with Eu. X-ray diffraction (XRD) analysis also clearly indicated differences before and after adsorption. By combining X-ray absorption near-edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and wavelet transform (WT) analyses, we observed that the Fe₂O₃ content significantly affects the Eu-Fe distance in the inner-sphere layer during the Eu adsorption process. The wavelet transform analysis for two-dimensional information helps differentiate two distances of Eu-O, which are difficult to analyze, with hydrated outer-sphere Eu-O distances ranging from 2.42 to 2.52 Å and inner-sphere Eu-O distances from 2.27 to 2.32 Å. The EXAFS results for Fe₂O₃ and SiO₂ in argillite and basalt reveal different adsorption mechanisms. Fe₂O₃ exhibits inner-sphere surface complexation in the order of basalt, argillite, and granite, while SiO₂ forms outer-sphere ion exchange with basalt and argillite. Wavelet transform analysis also highlights the differences among these materials. Full article

GaN on Si plays an important role in the integration and promotion of GaN-based wide-gap materials with Si-based integrated circuits (IC) technology. A series of GaN film materials were grown on Si (111) substrate using a unique plasma assistant molecular beam epitaxy (PA-MBE) technology and investigated using multiple characterization techniques of Nomarski microscopy (NM), high-resolution X-ray diffraction (HR-XRD), variable angular spectroscopic ellipsometry (VASE), Raman scattering, photoluminescence (PL), and synchrotron radiation (SR) near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. NM confirmed crack-free wurtzite (w-) GaN thin films in a large range of 180–1500 nm. XRD identified the w- single crystalline structure for these GaN films with the orientation along the c-axis in the normal growth direction. An optimized 700 °C growth temperature, plus other corresponding parameters, was obtained for the PA-MBE growth of GaN on Si, exhibiting strong PL emission, narrow/strong Raman phonon modes, XRD w-GaN peaks, and high crystalline perfection. VASE studies identified this set of MBE-grown GaN/Si as having very low Urbach energy of about 18 meV. UV (325 nm)-excited Raman spectra of GaN/Si samples exhibited the GaN E₂(low) and E₂(high) phonon modes clearly without Raman features from the Si substrate, overcoming the difficulties from visible (532 nm) Raman measurements with strong Si Raman features overwhelming the GaN signals. The combined UV excitation Raman–PL spectra revealed multiple LO phonons spread over the GaN fundamental band edge emission PL band due to the outgoing resonance effect. Calculation of the UV Raman spectra determined the carrier concentrations with excellent values. Angular-dependent NEXAFS on Ga K-edge revealed the significant anisotropy of the conduction band of w-GaN and identified the NEXAFS resonances corresponding to different final states in the hexagonal GaN films on Si. Comparative GaN material properties are investigated in depth. Full article