Search Results (190)

Background/Objectives: The precise characterization of the key microstructural and physicochemical attributes in sustained-release microspheres remains a technical bottleneck, hindering the understanding of drug release mechanisms, and limiting insights into the “process–structure–performance” relationship. To address this, we developed novel methods to conduct in-depth research on the microscopic properties of microspheres. Methods: Scanning electron microscopy (SEM) combined with a deep learning-based image segmentation (DLIS) algorithm was established for quantitative analysis of the pore structure. Laser confocal Raman spectroscopy (LCRS) was employed for in situ, non-destructive, three-dimensional (3D) visualization and quantitative mapping of the active pharmaceutical ingredient (API) distribution within microspheres. Results: This study successfully developed and applied SEM-DLIS and LCRS as reliable tools for microstructural and physicochemical characterization. SEM-DLIS analysis revealed significant differences in surface and internal pore structure among microspheres from different manufacturers and between particles of different sizes from the same batch. LCRS imaging further identified distinct API distribution patterns: uniform dispersion, outer-layer enrichment, and heterogeneous distribution. The combined data elucidate that the initial burst release is governed by the synergistic effect of surface porosity and API surface enrichment, whereas the sustained release kinetics are jointly regulated by the internal pore structure, particle size, and API spatial distribution. Conclusions: The findings establish that microstructure dictates release behavior and that all observed structural variations are linked to critical process parameters (CPPs), validating the “process determines structure” hypothesis. The established methodology provides a critical technical framework for the reverse engineering and quality equivalence assessment of generic microspheres, as well as for the quality-by-design-based optimization of innovative drug products, thereby advancing both pharmaceutical development and regulatory science. Full article

Hybrid conductive materials have attracted increasing attention due to their combined electrical conductivity, mechanical flexibility, and sustainability. In this work, new hybrid materials based on polyaniline (PANI)-wrapped multi-walled carbon nanotubes (MWCNTs) and microfibrous cellulosic substrates were developed and assessed for photocatalytic degradation of a model dye pollutant. First, in situ oxidative polymerization of aniline in formic acid (FA) was conducted in the presence of MWCNTs to afford stable dispersions of carboxylated polyaniline-wrapped carbon nanotubes (c-PANI/MWCNTs). Next, the dispersions were used for affordable impregnation of microfibrous cellulosic filter paper. The influence of the initiator type—potassium peroxodisulfate (KPS) and hydrogen peroxide—on polymer–nanotube interactions, stabilization and surface deposition was emphasized. The structural, surface, morphological and thermal properties of the obtained dispersions and cellulose nanocomposites were systematically investigated using Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy and thermal gravimetric analysis. The results revealed strong interfacial interactions between c-PANI and the pristine MWCNTs, resulting in improved dispersion stability and effective and even surface deposition of the conductive c-PANI/MWCNT hybrids into the cellulose fiber mesh. The photocatalytic degradation of 5 ppm methylene blue (MB) dye in the presence of the developed nanocomposite materials under UV-A illumination was studied. The results showed that the c-PANI@MWCNT-impregnated cellulose substrates exhibited enhanced photocatalytic ability (up to 83% degree of degradation of MB dye) in comparison with the pure c-PANI. Full article

This study presents a multi-analytical investigation of two Baroque gilded terracotta sculptures—Hercules and the Nemean Lion (Hercules A) and Hercules and the Lernaean Hydra (Hercules B)—attributed to Lorenzo Vaccaro (1655–1706) and preserved at the Museo Civico Gaetano Filangieri in Naples. This research aimed to reconstruct the original manufacturing technique, characterize materials introduced by successive restoration interventions, and identify active degradation mechanisms. A systematic diagnostic approach integrating UV fluorescence imaging, digital optical microscopy, portable energy-dispersive X-ray fluorescence spectroscopy (EDXRF), Raman spectroscopy, Fourier-transform infrared spectroscopy in attenuated total reflectance mode (FTIR-ATR), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS), and spectrocolorimetry was applied. The original gilding system—comprising a ferruginous silico-aluminous terracotta substrate, a calcium sulfate ground, a lead-white imprimitura, an iron-rich bole, and a thin gold leaf—is consistent with documented Baroque mission gilding practices in Southern Italy. Analytical evidence further documented extensive non-original interventions, including copper-based artificial patination, bronze powder (porporina) integration, poly (vinyl acetate) adhesives, and acrylic protective coatings. Raman spectroscopy identified the in situ conversion of intentionally applied tenorite (CuO) to malachite (Cu₂CO₃(OH)₂) as an active degradation pathway. Spectrocolorimetric measurements quantified chromatic alterations of up to ΔE = 52 attributable to accumulated surface deposits. The proposed integrated methodology constitutes a replicable diagnostic framework for investigating gilded terracotta artefacts in museum collections. Full article

Three types of graphene–single crystal titanium dioxide composite (GR–TiO₂SCs) were prepared using the hydrothermal method, employing TiF₄ and graphite as raw materials with hydrofluoric acid serving as the morphology-directing agent. The phase composition and morphological features of the resultant composites were systematically characterized by X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy, and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy and X-ray diffraction. These complementary characterization results clearly demonstrate that graphene and TiO₂ single crystals have been successfully hybridized to form a well-defined heterostructure, rather than a simple physical mixture. Photocatalytic performances were evaluated by monitoring the photodegradation behaviors of methylene blue, rhodamine B, and methyl orange solutions under simulated light irradiation, with real-time concentration variations recorded by UV–visible absorption spectroscopy. The composite sample in which TiO₂SCs were in situ grown and uniformly anchored onto graphene oxide substrates effectively suppressed the self-stacking and agglomeration of individual crystallites, thus delivering the best photocatalytic response. Increased exposure of the active catalytic interfaces of TiO₂SCs was found to play a key role in elevating the overall photocatalytic activity. The hierarchical assembly protocol developed in this work provides a feasible pathway for the rational design of functional composites with controllable microstructures and tailored properties, which can be further extended to the development of advanced sensing materials. Full article

To improve the adhesion and tribological performance of diamond-like carbon (DLC) coatings on steel substrate, a Ti-enhanced plasma nitriding (PNTi) layer was formed on the surface of 38CrMoAl steel, followed by deposition of a Cr-based interlayer (mainly CrN) and then a W interlayer. Finally, a DLC coating was deposited, resulting in a novel PNTi/DLC coating. For comparison, a conventional PN/DLC coating was prepared under the same processing conditions. Optical microscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, hardness tests, and tribological experiments were performed to systematically investigate the effect of TiN-enriched PNTi supporting layer on the performances of the PNTi/DLC composite coating. The results show that comparing with PN/DLC composite coating, the critical load (Lc₂) of the PNTi/DLC coating was increased from 28.89 N to 43.25 N—about a 50% enhancement. The microhardness was increased from 2650 HV_0.05 to 4400 HV_0.05 (corresponding to 28.2 GPa to 44.1 GPa). The friction coefficient was decreased from 0.28 to 0.11, about a 60% reduction, and the wear rate declined more than 40%, from 4.81 × 10⁻⁶ to 2.90 × 10⁻⁶ mm³·N⁻¹·m⁻¹. The introduction of Ti promoted the in situ formation of TiN phase in the nitrided layer, which significantly improved the compactness of the nitrided layer and the adhesion at the film–substrate interface. Consequently, the PNTi/DLC composite coating exhibited excellent wear resistance and friction stability under high-load and severe tribological conditions. This study provides a promising perspective for engineering applications of steel-based DLC coatings in harsh service environments. Full article

This study aims to enhance and develop the properties of materials used as supercapacitors. The synthesis of graphene oxide (GO) was achieved via a modified Hummer’s method, whereas the fabrication of polyaniline (PANI)/GO nanocomposites was conducted utilizing an in situ chemical polymerization technique. Subsequently, the PANI/GO layered films were deposited on fluorine-doped tin oxide (FTO) glass for supercapacitor applications. The materials were analyzed using X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and cyclic voltammetry (CV). The experimental results demonstrated that a reaction time of 30 min, along with a weight ratio of aniline (ANI) monomer to GO of 1:1.5, yielded an optimal specific capacitance of 13.30 F/g. The robust electrochemical performance of the PANI/GO electrode may stem from the increased active sites for PANI deposition, attributable to the large surface areas of GO. Full article

Wool fibers undergo significant structural changes during industrial stretching, which directly impact their mechanical properties and textile performance, making monitoring of the stretching process essential for optimizing wool products. In this study, we demonstrate the effective use of polarized second harmonic generation (P-SHG) imaging for monitoring the wool fiber stretching process. P-SHG is highly sensitive to non-centrosymmetric structures, enabling clear observation of changes in α-keratin alignment and the reconstruction of cortical interfaces during stretching. Quantitative P-SHG analysis revealed a significant decrease in the effective pitch angle (θ_e) from 54° ± 1° to 33° ± 3° after stretching, confirming the dipole orientation changes in keratin molecules. These findings were further validated through additional characterization techniques, including scanning electron microscopy (SEM), polarizing optical microscopy (POM), X-ray diffraction (XRD), and Raman spectroscopy (RS). The results show that the industrial stretching process of wool alters the morphology at the surface scale, enhances the alignment of macroscopic fibers, and induces a transition from α-helix to β-sheet. Our technique is simple, effective, and capable of in situ monitoring of the structural changes in wool fibers, making it highly promising for applications in the wool industry. Full article

In response to thermal failure risks in ultra-high voltage (UHV) bushing online monitoring devices and maintenance equipment—caused by high heat generation of electronic components and the intrinsically low thermal conductivity of conventional resin encapsulation materials—this study proposes a novel modification strategy based on flash Joule heating (FJH). Distinct from conventional interface modification methods, the proposed approach enables cross-scale, in situ microsoldering between multi-walled carbon nanotubes (MWCNTs) and carbon fibers (CFs), constructing a multiscale reinforcement network with integrated thermal transport and mechanical load transfer pathways. The transient ultra-high-temperature thermal shock generated by FJH not only effectively removes inert impurities on CF surfaces but also drives carbon structural reconstruction, enabling graphitic-level welding of MWCNTs onto the fiber surface. This micro-welded architecture fundamentally differs from traditional filler dispersion or interface coating strategies, which often suffer from the trade-off between interfacial thermal transport and mechanical bonding. By contrast, the FJH-induced carbon–carbon bonded nodes form a continuous conductive and load-bearing network at the micro–nano scale. Characterizations using scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) confirm successful in situ welding of MWCNTs onto CF surfaces. Meanwhile, FJH treatment effectively removes oxygen-containing functional groups and surface impurities. Analysis of carbon bonding evolution indicates that the welding efficiency reaches its maximum at 90 V. Macroscopic performance tests demonstrate that, compared with epoxy resin, the thermal conductivity of the multiscale reinforced system increases by approximately 168%, while the mechanical strength improves by 62.72%. This study provides new theoretical insights and technical pathways for the development of next-generation polymer composite materials with both high thermal conductivity and high mechanical strength. Full article

A novel ternary nanocomposite, comprising reduced graphene oxide/polyaniline/gadolinium oxide (RGO-PANI-Gd₂O₃), was successfully synthesized using the Hummers method, followed by in situ emulsion polymerization of polyaniline. The final composite was produced by hydrothermally adding gadolinium nitrate. The composite was subjected to a systematic analysis that included optical, microstructural, physical, and Raman spectroscopic analysis, as well as current-voltage (J-V) measurements. The morphology of this composite material was investigated using scanning electron microscopy (SEM). The addition of Gd₂O₃ nanoparticles decreases the band gap energy from 3.5 eV (PANI) to 2.7 eV (RGO-PANI-Gd₂O₃). The UV–Vis spectra revealed a redshift in the π-π* transition peak from 318 nm (PANI) to 346 nm, indicating increased conjugation length and synergistic effects. This eco-friendly material has excellent catalytic activity for triiodide reduction. The manufactured counter-electrode (CE) demonstrated remarkable transparency and conversion efficiency comparable to platinum, with a current density of 11.7 mA·cm⁻² versus 8.2 mA·cm⁻² for platinum. Under simulated solar light (AM 1.5 G, 100 mW·cm⁻²), the RGO-PANI-Gd₂O₃ based nanocomposite CE achieved an excellent 4.3% photo conversion efficiency. These findings indicate that RGO-PANI-Gd₂O₃ nanocomposites have potential as efficient, platinum-free counter electrodes in dye-sensitized solar cells (DSSCs). Full article

The 17th-century stucco altar dedicated to St. Michael the Archangel is an interesting, but very damaged, artwork located in the complex of St. Angel in the little town of Barbarano Romano in Central Italy. During the recent and quite necessary restoration carried out by University of Tuscia students on the Conservation and Restoration of Cultural Heritage Master’s program, some problems with the surface coating were encountered in the cleaning phase. Diagnostic and scientific analyses were crucial to better understanding the composition of these materials to perform the safest and most efficient cleaning procedures. The first of many steps required by this approach was an in situ analysis, starting from on-site analysis and diagnostic documentation through X-ray fluorescence spectroscopy and ultraviolet fluorescence photography, followed by laboratory investigations. The latter included µ-Raman and Fourier transform infrared spectroscopies, gas chromatography coupled with mass spectrometry, and scanning electron microscopy equipped with an energy-dispersive detector. Each technique provided useful data to determine the chemical composition of the white surface coating, which was found to be a non-original overpaint containing lead and organic binder. This overpaint had been applied to retouch the white stucco during a previous restoration project. All this new information contributed to achieving the final decision to remove this layer. Full article

This study deals with diamond films grown via the microwave plasma-enhanced chemical vapor deposition technique (MWPECVD) on molybdenum (Mo) substrates of different roughness. This work is motivated by the necessity of overcoming the poor adhesion of diamond films on smooth Mo substrates, to ensure their effective application as cathodes for aerospace propulsion. The deposition process was monitored in situ using pyrometric interferometry (PI), thus enabling the real-time monitoring of both the rate and the temperature of deposition. The characterization of the obtained diamond films was performed using different techniques, such as Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The poor adhesion of diamond films on Mo substrates was solved by roughening their surface, which promotes residual stress reduction in the diamond films. In this work, the PI technique was also exploited to support the prediction of the adhesion and stability of diamond films before their exposure in air through the monitoring of the deposition temperature. This represents a novel point of our work that has never been discussed in other research papers, as pyrometric interferometry is generally mainly used to assess the rate and the temperature of deposition. Full article

In this work, the effect of aqueous dispersions of graphene oxide (GO) and nanosized graphene oxide (nGO) on the enzymatic polymerization of polyaniline (PANI) was studied. The enzymatic polymerization of PANI was carried out in aqueous medium using toluenesulfonic acid (TSA) as the dopant, horseradish peroxidase (HRP) as the catalyst, and hydrogen peroxide (H₂O₂) as the oxidant, using 1.0, 2.5, and 5.0 wt% of GO and nGO. The morphology of PANI-GO/nGO composites was studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Further characterization was performed by thermogravimetric analysis (TGA) and spectroscopic techniques such as ultraviolet–visible (UV–Vis), Fourier-transform infrared (FTIR), Raman and X-ray photoelectronics (XPS). SEM images showed that during enzymatic polymerization, PANI completely covers the GO/nGO sheets. Furthermore, physicochemical results confirmed the production of a hybrid PANI-GO/nGO material with Van der Waals-type interactions between the oxygen-based functional groups of GO and the secondary amino bond (-NH-) of PANI. Also, cyclic voltammetry experiments were carried out in situ during the polymerization of PANI-GO/nGO films. The electrochemical response of PANI-GO/nGO composites reflects two broad oxidation peaks around 300 mV and 500 mV during anodic scanning, with reversible oxidation during cathodic scanning. Classical molecular dynamics simulations were used to understand the mechanism of the composite film’s growth. Full article

Thermoelectric (TE) materials represent a critical frontier in sustainable energy conversion technologies, providing direct thermal-to-electrical energy conversion with solid-state reliability. The optimizations of TE performance demand a nuanced comprehension of structure–property relationships across diverse length scales. This review summarizes established and emerging spectroscopic and microscopic techniques used to characterize inorganic and polymer TE materials, specifically poly(3,4-ethylenedioxythiophene): poly(styrenesulfonate) (PEDOT:PSS). For inorganic TE, ultraviolet–visible (UV–Vis) spectroscopy, energy-dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS) are widely applied for electronic structure characterization. For phase analysis of inorganic TE materials, Raman spectroscopy (RS), electron energy loss spectroscopy (EELS), and nuclear magnetic resonance (NMR) spectroscopy are utilized. For analyzing the surface morphology and crystalline structure, chemical scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) are commonly used. For polymer TE materials, ultraviolet−visible–near-infrared (UV−Vis−NIR) spectroscopy and ultraviolet photoelectron spectroscopy (UPS) are generally employed for determining electronic structure. For functional group analysis of polymer TE, attenuated total reflectance–Fourier-transform infrared (ATR−FTIR) spectroscopy and RS are broadly utilized. XPS is used for elemental composition analysis of polymer TE. For the surface morphology of polymer TE, atomic force microscopic (AFM) and SEM are applied. Grazing incidence wide-angle X-ray scattering (GIWAXS) and XRD are employed for analyzing the crystalline structures of polymer TE materials. These techniques elucidate electronic, structural, morphological, and chemical properties, aiding in optimizing TE properties like conductivity, thermal stability, and mechanical strength. This review also suggests future research directions, including in situ methods and machine learning-assisted multi-dimensional spectroscopy to enhance TE performance for applications in electronic devices, energy storage, and solar cells. Full article

Surface-enhanced Raman spectroscopy (SERS) enables ultra-sensitive molecular detection and has broad analytical and biomedical applications; recent advances focus on high-performance substrates and innovative detection strategies. However, achieving controllable and reproducible substrate fabrication—particularly using natural templates such as hair—remains challenging, limiting SERS application in trace analysis and on-site detection. This study developed a single-hair in situ SERS platform using a natural hair template. Confinement within hair cuticle grooves and capillary-evaporation assembly enables dense arrangement of cetyltrimethylammonium bromide-coated Au nanorods and polyvinylpyrrolidone-coated Au nanoparticles, forming uniform plasmonic nanoarrays. Spectroscopy and microscopy analyses confirmed the regular alignment of nanostructures along the hair axis with denser packing at the edges. The platform detected crystal violet at 10⁻⁹ M, yielding clear signals, negligible background, and stable peaks after repeated washing. For p-phenylenediamine, enhancement was observed down to 10⁻⁶ M. On the platform, a concentration-dependent response appeared within 10⁻³–10⁻⁵ M, with spatial Raman imaging along the hair axis. Capillary-evaporation coupling and interfacial wettability facilitated solute enrichment from larger to smaller gap hotspots, improving signal-to-noise ratio and reproducibility. This portable, low-cost, and scalable method supports rapid on-site screening in complex matrixes, offering a general strategy for hotspot engineering and programmable assembly on natural templates. Full article

Chemical sensors have undergone transformative advances in recent years, driven by the convergence of nanomaterials, advanced fabrication strategies, and state-of-the-art characterization methods. This review emphasizes recent developments, with particular attention to progress achieved over the past decade, and highlights the role of the United States as a major driver of global innovation in the field. Nanomaterials such as graphene derivatives, MXenes, carbon nanotubes, metal–organic frameworks (MOFs), and hybrid composites have enabled unprecedented analytical performance. Representative studies report detection limits down to the parts-per-billion (ppb) and even parts-per-trillion (ppt) level, with linear ranges typically spanning 10–500 ppb for volatile organic compounds (VOCs) and 0.1–100 μM for biomolecules. Response and recovery times are often below 10–30 s, while reproducibility frequently exceeds 90% across multiple sensing cycles. Stability has been demonstrated in platforms capable of continuous operation for weeks to months without significant drift. In parallel, additive manufacturing, device miniaturization, and flexible electronics have facilitated the integration of sensors into wearable, stretchable, and implantable platforms, extending their applications in healthcare diagnostics, environmental monitoring, food safety, and industrial process control. Advanced characterization techniques, including in situ Raman spectroscopy, X-ray Photoelectron Spectroscopy (XPS, Atomic Force Microscopy (AFM), and high-resolution electron microscopy, have elucidated interfacial charge-transfer mechanisms, guiding rational material design and improved selectivity. Despite these achievements, challenges remain in terms of scalability, reproducibility of nanomaterial synthesis, long-term stability, and regulatory validation. Data privacy and cybersecurity also emerge as critical issues for IoT-integrated sensing networks. Looking forward, promising future directions include the integration of artificial intelligence and machine learning for real-time data interpretation, the development of biodegradable and eco-friendly materials, and the convergence of multidisciplinary approaches to ensure robust, sustainable, and socially responsible sensing platforms. Overall, nanomaterial-enabled chemical sensors are poised to become indispensable tools for advancing public health, environmental sustainability, and industrial innovation, offering a pathway toward intelligent and adaptive sensing systems. Full article