Search Results (52)

The Po Nagar Towers (Thap Ba) complex, an iconic heritage site of Cham culture and a nationally recognized special relic, has stood in Nhatrang, Vietnam, for over a thousand years. We report here a preliminary analysis of original ancient Cham bricks from the Po Nagar Towers using a combination of appropriate characterization techniques, including X-ray fluorescence (XRF), X-ray diffraction (XRD), Raman micro-spectroscopy, thermal dilatometry, compressive strength testing, and water sorption. Mechanical properties and firing temperatures of the ancient bricks have been determined to support the discussion on the likely technology used to make them. Specifically, they were made from clay, sand, plagioclases/feldspar, and grog mixed with intentionally added carbon precursor (charcoal powder), then fired at temperatures between 800 °C and 1000 °C to form lightweight bricks with a mass density of 1.3–1.6 kg/dm³ and an open porosity of 18–25%. The ancient Cham bricks have their texture and porosity to meet the requirements of the thin rubbing joint technique in tower construction and to contribute to the carvability and durability of Cham towers. A comparison is made with the bricks for tower restoration during the 2000s. Full article

Polyamorphic transitions driven by high-energy mechanical milling (nanomilling) are studied in thioarsenide As₄Se_n-type glassy alloys obtained by melt quenching deviated from arsenic triselenide As₂Se₃ stoichiometry towards tetraarsenic pentaselenide (g-As₄Se₅) and tetraarsenic tetraselenide (g-As₄Se₄). This employs a multiexperimental approach based on powder X-ray diffraction (XRD) analysis complemented by thermophysical heat transfer, micro-Raman scattering (micro-RS) spectroscopy, and revised positron annihilation lifetime (PAL) analysis. Microstructure scenarios of these nanomilling-driven transformations in arsenoselenides are identified by quantum-chemical modeling using the authorized modeling code CINCA (the Cation Interlinked Network Cluster Approach). A straightforward interpretation of a medium-range structure response of a nanomilling-driven polyamorphism in the arsenoselenides is developed within the modified microcrystalline model. Within this model, the diffuse peak-halos arrangement in the XRD patterning is treated as a superposition of the Bragg-diffraction contribution from inter-planar correlations supplemented by the Ehrenfest-diffraction contribution from inter-atomic (inter-molecular) correlations related to derivatives of network As₂Se₃-type and molecular As₄Se₄-type conformations. Changes in the medium-range structure of examined glassy arsenoselenides subjected to nanomilling occur as an interplay between disrupted intermediate-range ordering and enhanced extended-range ordering. The domination of network-forming conformations in arsenoselenides deviated from As₂Se₃ stoichiometry (such as g-As₄Se₅) results in rather slight changes in their calorimetric heat-transfer and micro-RS responses. At the atomic-deficient level probed by PAL spectroscopy, these changes are accompanied by reduced positron trapping rate of agglomerated multiatomic vacancies and vacancy-type clusters in an amorphous As-Se network. Under an increase in As content beyond the g-As₄Se₅ composition approaching g-As₄Se₄, nanomilling-driven polyamorphic transitions, which can be classified as reamorphization (amorphous I-to-amorphous II) phase transitions, are essentially enhanced due to the higher molecularity of these glassy alloys enriched in thioarsenide-type As₄Se₄ cage-like molecular entities and their low-order network-forming derivatives. Full article

X-ray radiation treatments are largely adopted in radiotherapy, and Fourier-transform infrared microspectroscopy (μ-FTIR) has already been demonstrated to be a useful instrument for monitoring radiotherapy effects. Previous works in this field have focused on studying the changes occurring in cells when they are fixed immediately after the irradiation or 24 and 48 h later. In the present paper, changes occurring in SH-SY5Y neuroblastoma cells in the first hours after the irradiation are examined to obtain information on the processes taking place in this not-yet-investigated time window by using μ-FTIR. For this purpose, cell samples were fixed immediately after X-ray exposure, and 2 and 4 h after irradiation and investigated along with unexposed cells. Different data analysis procedures were implemented to estimate the changes in lipid, protein, and DNA spectral contributions. The present investigation on the effects of X-ray in the first hours after the exposure is helpful for better describing the processes occurring in this time window that offer the possibility of a timely check on the efficacy of X-ray treatments and can potentially be applied for planning personalized treatment as required by the most advanced medical therapy. Full article

A novel double-impurity doping process for silicon (Si) surfaces was developed, utilizing nanosecond-laser melting of an 11 nm thick gold (Au) top film and a Si wafer substrate in a laser plasma-activated liquid nitrogen (LN) environment. Scanning electron microscopy revealed a fluence- and exposure-independent surface micro-spike topography, while energy-dispersive X-ray spectroscopy identified minor Au (~0.05 at. %) and major N (~1–2 at. %) dopants localized within a 0.5 μm thick surface layer and the slight surface post-oxidation of the micro-relief (oxygen (O), ~1.5–2.5 at. %). X-ray photoelectron spectroscopy was used to identify the bound surface (SiN_x) and bulk doping chemical states of the introduced nitrogen (~10 at. %) and the metallic (<0.01 at. %) and cluster (<0.1 at. %) forms of the gold dopant, and it was used to evaluate their depth distributions, which were strongly affected by the competition between gold dopants due to their marginal local concentrations and the other more abundant dopants (N, O). In this study, 532 nm Raman microspectroscopy indicated a slight reduction in the crystalline order revealed in the second-order Si phonon band; the tensile stresses or nanoscale dimensions of the resolidified Si nano-crystallites envisioned by the main Si optical–phonon peak; a negligible a-Si abundance; and a low-wavenumber peak of the Si₃N₄ structure. In contrast, Fourier transform infrared (FT-IR) reflectance and transmittance studies exhibited only broad structureless absorption bands in the range of 600–5500 cm⁻¹ related to dopant absorption and light trapping in the surface micro-relief. The room-temperature electrical characteristics of the laser double-doped Si layer—a high carrier mobility of 1050 cm²/Vs and background carrier sheet concentration of ~2 × 10¹⁰ cm⁻² (bulk concentration ~10¹⁴–10¹⁵ cm⁻³)—are superior to previously reported parameters of similar nitrogen-implanted/annealed Si samples. This novel facile double-element laser-doping procedure paves the way to local maskless on-demand introductions of multiple intra-gap intermediate donor and acceptor bands in Si, providing related multi-wavelength IR photoconductivity for optoelectronic applications. Full article

Microplastics (MPLs) and nanoplastics (NPLs) are smaller particles derived from larger plastic material, polymerization, or refuse. In context to environmental health, they are separated into the industrially-created “primary” category or the degradation derivative “secondary” category where the particles exhibit different physiochemical characteristics that attenuate their toxicities. However, some particle types are more well documented in terms of their fate in the environment and potential toxicological effects (secondary) versus their industrial fabrication and chemical characterization (primary). Fourier Transform Infrared Spectroscopy (FTIR/µ-FTIR), Raman/µ-Raman, Proton Nuclear Magnetic Resonance (H-NMR), Curie Point-Gas Chromatography-Mass Spectrometry (CP-gc-MS), Induced Coupled Plasma-Mass Spectrometry (ICP-MS), Nanoparticle Tracking Analysis (NTA), Field Flow Fractionation-Multiple Angle Light Scattering (FFF-MALS), Differential Scanning Calorimetry (DSC), Thermogravimetry (TGA), Differential Mobility Particle [Sizing] (DMPS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Scanning Transmission X-ray Microspectroscopy (STXM) are reviewed as part of a suite of characterization methods for physiochemical ascertainment and distinguishment. In addition, Optical-Photothermal Infrared Microspectroscopy (O-PTIR), Z-Stack Confocal Microscopy, Mueller Matrix Polarimetry, and Digital Holography (DH) are touched upon as a suite of cutting-edge modes of characterization. Organizations, like the water treatment or waste management industry, and those in groups that bring awareness to this issue, which are in direct contact with the hydrosphere, can utilize these techniques in order to sense and remediate this plastic polymer pollution. The primary goal of this review paper is to highlight the extent of plastic pollution in the environment as well as introduce its effect on the biodiversity of the planet while underscoring current characterization techniques in this field of research. The secondary goal involves illustrating current and theoretical avenues in which future research needs to address and optimize MPL/NPL remediation, utilizing nanotechnology, before this sleeping giant of a problem awakens. Full article

The aim of the presented research is to evaluate the potential performance of a new bending magnet X-ray beamline—PolyX, designed for microimaging and microspectroscopy at the National Synchrotron Radiation Centre SOLARIS in Krakow. Due to the short beamline length (<15 m), PolyX uses compact polycapillary and single-bounce monocapillary optics for X-ray focusing in the 4–15 keV energy range. Polycapillary optics require a dedicated approach for an efficient simulation of X-ray propagation in multiple capillary channels. Therefore, the PolyX beamline was ray traced by combining XRT (XRayTracer) and polycap libraries. In addition, to estimate the X-ray fluorescence spectra excited by focused beams, Monte Carlo simulations were conducted using XMI-MSIM. All simulations were aimed to estimate the crucial X-ray beam properties, i.e., the flux, the spot size, and the energy spectrum, for monochromatic and polychromatic X-ray beams. Full article

Solution-based inorganic–organic halide perovskites are of great interest to researchers because of their unique optoelectronic properties and easy processing. However, polycrystalline perovskite films often show inhomogeneity due to residual strain induced during the film’s post-processing phase. In turn, these strains can impact both their stability and performance. An exhaustive study of residual strains can provide a better understanding and control of how they affect the performance and stability of perovskite films. In this work, we explore this complex interrelationship between residual strains and electrical properties for methylammonium ${\mathrm{CH}}_3{\mathrm{NH}}_3{\mathrm{PbI}}_{3-\mathrm{x}}{\mathrm{Cl}}_{\mathrm{x}}$ films using grazing incidence X-ray diffraction (GIXRD). We correlate their resistivity and carrier mobility using the Hall effect. The ${\sin }^2\left(\psi \right)$ technique is used to optimize the annealing parameters for the perovskite films. We also establish that temperature-induced relaxation can yield a significant enhancement of the charge carrier transports in perovskite films. Finally, we also use Raman micro-spectroscopy to assess the degradation of perovskite films as a function of their residual strains. Full article

The study seeks to unravel the intricate operational sequence involved in preparing prehistoric pigments for rock art within the Puerto Roque rock art shelter. Sixteen pigment samples were meticulously collected from specific figurative representations. Additionally, three ochre samples were sourced from the shelter’s soil. Employing a comprehensive multi-analytical approach, including Raman microspectroscopy, X-ray microfluorescence (EDxrf), Fourier-transform infrared spectroscopy (ATR-FTIR), and scanning electron microscopy (SEM-EDS), all nineteen samples underwent thorough analysis. Notably, darker pigments revealed a composition of hematite with the added presence of carbon. Meanwhile, one sample exhibited an orange hue primarily composed of goethite and bright red pigments predominantly characterised by hematite, as confirmed by Raman analysis. EDxrf analysis demonstrated an elemental composition akin to the three ochre pieces examined. Furthermore, ATR-FTIR spectroscopy suggested the potential influence of a heating process in enhancing red coloration, corroborated by spectral results from specific samples. This finding aligns with prior research, underscoring the technological sophistication embedded in early artistic endeavours. Full article

The impact of the anthropic activities in Antarctica is a concerning issue. According to the Scientific Committee on Antarctic Research, attention has to be paid to the next-generation contaminants deriving from both long-range atmospheric transport and local sources. In this study, the capabilities of transmission electron microscopy with energy-dispersive X-ray spectroscopy and Raman micro-spectroscopy were exploited to evaluate the size, morphology, and chemical composition of small micro- and nanoparticles, as well as their aggregates, in surface snow samples collected during the 2020–2021 austral summer in the coastal area of Victoria Land near the Mario Zucchelli research station. The presence of biological particles, mineral dust, sea salts, and small carbonaceous and plastic micro- and nanoparticles was assessed. Sulfate, carbonate, and nitrate minerals were detected in all the samples, whereas polyethylene, poly(ethylene-co-vinyl-acetate), and different kinds of carbonaceous materials were predominantly identified in the samples closest to the research base. The presence of small micro- and nanoparticles containing heavy metals and plastic polymers in samples collected in the areas surrounding the Italian research base highlights the impact of anthropogenic activities on the polar environment, suggesting the need for continuous monitoring to evaluate possible threats to the delicate Antarctic ecosystem. Full article

Lithium fluoride (LiF) film detectors for extreme ultraviolet radiation, soft and hard X-rays, based on the photoluminescence of radiation-induced electronic defects, have been proposed and are currently under further development and investigation. LiF film detectors are versatile and can be integrated in different experimental apparatus and imaging configurations. LiF can be grown in the form of polycrystalline thin films and it is compatible with several substrates. The radiation-induced color center (CCs) photoluminescence (PL) response can be enhanced through the appropriate choice of substrates and multilayer designs, and by tailoring the micro-structural properties of polycrystalline LiF films through the control of the growth conditions. In this work, we present the characterization, through fluorescence and Raman micro-spectroscopy, of LiF films, thermally evaporated on different substrates with thicknesses of up to 1 μm, irradiated with soft X-rays produced by a laser plasma source. The combination of these micro-spectroscopy techniques could represent an advanced method to investigate the role of the polycrystalline film structures in CC formation efficiency at the microscopic level, a fundamental aspect of the development of LiF film radiation-imaging detectors. Full article

Raman microspectroscopy and X-ray microcomputed tomography (micro-CT) were used for assessment of the quality of the femur and tibia bones in apolipoprotein-deficient mice compared to control littermates. The cortical and trabecular bone was investigated separately. Raman spectra revealed no differences in the bioapatite-to-collagenous matrix ratio of the cortical bone. The quantities of calcium and collagen, which were measured using atomic absorption spectrometry and thermogravimetric analysis, respectively, were also found to be equal in the two groups. Density and morphometric parameters, which were measured using micro-CT, verified the cortical mineral stability. Bone quality indices were measured using Raman spectra. A decreased collagen crosslink (trivalent-to-divalent) ratio revealed delayed maturation of the collagen network. Such a decrease has been reported in the literature to be connected to decreased bone strength. For the trabecular bone, micro-CT revealed severe osteoporosis in the knock-out group, which was evident from a decreased mineral density, trabecular thickness and increased bone surface/volume ratio. The trabecular bone was not accessible for Raman spectroscopy. According to these results, the cortical and trabecular femur bone is expected to exhibit proneness to fracturing, each for a different reason. A combination of the two techniques was regarded as necessary for an overall assessment of bone quality. Full article

High amounts of coal combustion products, such as fly ash and bottom ash, are generated every year; however, only 64% are used, which means that a significant part is landfilled despite containing valuable materials such as ferrospheres, which may be used as catalysts, substituting critical raw materials (e.g., platinoids). In commercial coals, pyrite contents are reduced as a pre-combustion S-emissions control measure, so low amounts of ferrospheres are expected in the respective ashes. However, given the large amounts of ash being generated from these coals, it may provide a reliable source of catalysts, with ferrospheres being easily recovered via magnetic separation. Several studies have been conducted regarding these morphotypes; however, there is a lack of investigation considering the ash derived from highly beneficiated coals and the variations with location and time. In this study, bottom ash, economizer grits, and fly ash samples from a Portuguese power plant burning Colombian commercial coal were fractionated using ferrite (Fe-MC fraction) and Nd (Nd-MC fraction) magnets, and a multi-technique approach was used to assess their properties (magnetic parameters, particle size distribution, mineralogy, particle morphology, microtexture, and chemical composition). The Fe-MC presented higher Fe concentrations (up to 44 wt.% Fe₂O₄) than the Nd-MC (up to 7 wt.% Fe₂O₄). Once it was a sequential process, Nd magnets essentially collected Fe-bearing aluminosilicate glass, and Fe-bearing minerals were residual when compared to the Fe-MC, where magnetite, magnesioferrite, hematite, and maghemite accounted for up to 30 wt.%. Among the Fe-MC, the sample collected from electrostatic precipitator fly ash (ESP FA), despite having a lower yield, presented higher Fe concentrations than the ones from bottom ash and economizer grits, which was related to the mode of occurrence of Fe-bearing phases: in the Fe-MC from ESP FA, discrete ferrospheres predominated, while in the remaining Fe-bearing phases, they were often embedded in aluminosilicate glass. All Fe-MC samples showed an increase of Fe-substituting elements (e.g., Mn and Ni) and their concentration tended to increase with decreasing particle size along with Fe. The integrated study of cross-sections enabled the identification of oxidation rims, martitization aspects, and the co-existence of hematite and magnesioferrite. Full article

We evaluated the pharmaceutical properties of levofloxacin (LV) in the form of an orally disintegrating tablet (LV_ODT) to find a new usefulness of low frequency (LF) Raman spectroscopy. LV_ODT contained dispersed granules with diameters in the order of several hundred micrometers, which were composed of the active pharmaceutical ingredient (API), as confirmed by infrared (IR) microspectroscopy. On the contrary, the API and inactive pharmaceutical ingredients (non-APIs) were homogeneously distributed in LV tablet (LV_T) formulations. Microscopic IR spectroscopy and thermal analyses showed that LV_ODT and LV_T contained the API in different crystalline forms or environment around the API each other. Furthermore, powder X-ray diffraction showed that LV_T contained a hemihydrate of the API, while LV_ODT showed a partial transition to the monohydrate form. This result was confirmed by microscopic LF Raman spectroscopy. Moreover, this method confirmed the presence of thin layers coating the outer edges of the granules that contained the API. Spectra obtained from these thin layers indicated the presence of titanium dioxide, suggesting that the layers coexisted with a polymer that masks the bitterness of API. The microscopic LF Raman spectroscopy results in this study indicated new applications of this method in pharmaceutical science. Full article

The absorption of light in the near-infrared region of the electromagnetic spectrum by Au-hyperdoped Si has been observed. While silicon photodetectors in this range are currently being produced, their efficiency is low. Here, using the nanosecond and picosecond laser hyperdoping of thin amorphous Si films, their compositional (energy-dispersion X-ray spectroscopy), chemical (X-ray photoelectron spectroscopy), structural (Raman spectroscopy) and IR spectroscopic characterization, we comparatively demonstrated a few promising regimes of laser-based silicon hyperdoping with gold. Our results indicate that the optimal efficiency of impurity-hyperdoped Si materials has yet to be achieved, and we discuss these opportunities in light of our results. Full article

Preserving and analytically examining daguerreotypes is particularly challenging because of their multi-material and multi-component structure. Various sensors have been exploited to examine mainly the image plates of the daguerreotypes even though the degradation goes beyond this component. Micro-analyses have been the preferred method due to the nanoscale structure of the image particles. In this work, we propose comprehensive multi-modal non-invasive sensing to investigate the corrosion products present in nine daguerreotypes from the Fondazione Alinari per la Fotografia (FAF, Florence, Italy). The methodology proposed includes chemical and morphological analyses: portable X-ray fluorescence spectrometry (pXRF), Raman microspectroscopy (μ-Raman), and micro-Fourier transform infrared spectroscopy in reflection mode (μ-rFTIR) for the chemical identification. For the first time, optical coherence tomography (OCT) was deployed to record the cross-sectional and morphological data of the relevant corrosion formations on daguerreotypes in a contactless way. The results allowed the characterization, in a non-invasive mode at a microscopic level, of a wide range of degradation products produced by the interaction of the different elements present in the structure of the daguerreotypes. The aim was to verify the performance of the proposed methodology and to link the chemical and physical complexity of the entire structure, disclosed by the state-of-art sensors, to the daguerreotype degradation. The results draw attention to the need to monitor not only the image condition but the whole object as a partially closed system in constant interaction internally and with the environment. Full article