Search Results (474)

A novel electrochemical sensing platform based on a glassy carbon electrode (GCE) modified with a juglone/mesoporous carbon composite (JUG-MC/GCE) was developed for the ultrasensitive determination of melatonin (MEL) in pharmaceutical formulations and dietary supplements. Incorporation of juglone and mesoporous carbon within the coating deposited on the glassy carbon electrode, resulted in enhanced charge-transfer characteristics at the electrode–electrolyte interface. Under optimized differential pulse voltammetry (DPV) conditions in a 0.1 mol L⁻¹ McIlvaine buffer (pH 2.8), the proposed sensor demonstrated an exceptional electrocatalytic response for melatonin oxidation via a two-electron, one-proton irreversible pathway under kinetic control. The analytical performance reveal multiple linear calibration intervals with an ultra-low limit of detection (LOD) of 0.21 µg L⁻¹ (0.9 nM). The sensor manifested robust operational repeatability (RSD ≤ 1.8%), long-term storage stability, and satisfactory selectivity toward melatonin in the presence of common tablet excipients and selected potential interferents. The practical utility of the JUG-MC/GCE platform was successfully validated through the direct quantification of melatonin in commercial tablets, capsules, and complex jelly matrices, confirming its suitability for melatonin determination in real samples. Full article

In the present work, graphene-modified zinc oxide (ZnO-rGO) and fluorine-doped tin oxide (FTO) thin films were successfully fabricated using a simple, low-cost pulsed spray pyrolysis technique. The structural, morphological, optical, electrical, and surface electronic properties of the deposited films were systematically characterized. X-ray diffraction (XRD) analysis confirmed the formation of polycrystalline ZnO- and SnO₂-based phases with crystallite sizes in the nanometer range. The crystallographic parameters, microstrain, and dislocation density of the deposited films were found to be influenced by the incorporation of reduced graphene oxide (rGO) and fluorine dopants. Scanning electron microscopy (SEM) revealed compact and homogeneous surface morphologies with good film coverage and well-defined nanocrystalline features. Optical characterization demonstrated the wide-bandgap semiconducting behavior of the deposited films, with optical bandgap energies ranging from 3.262 to 3.312 eV for the ZnO-rGO films and from 3.91 to 4.01 eV for the FTO films. Kelvin probe measurements yielded work-function values in the range of approximately 5.0–5.2 eV, indicating favorable surface electronic characteristics suitable for optoelectronic applications. Furthermore, fluorine incorporation enhanced the dielectric response of the SnO₂ films, particularly in the low-frequency region owing to increased interfacial polarization effects. The obtained results demonstrate that pulsed spray pyrolysis provides a simple, cost-effective, and efficient route for fabricating ZnO-rGO and FTO thin films with desirable structural, optical, electrical, and surface electronic properties. These findings highlight the considerable potential of the developed materials for transparent electrodes and a wide range of optoelectronic applications. Full article

This review aims to analyze defect-driven thermoelectric decoupling in pulsed laser deposition (PLD)-grown oxygen-deficient ${WO}_x$ and tungsten Magnéli thin films. While transition metal oxides offer a non-toxic, abundant alternative to conventional thermoelectrics, tungsten oxide stands out due to the profound impact of sub-stoichiometry on its transport properties. We systematically evaluate how ordered oxygen vacancies and crystallographic shear planes transform insulating ${WO}_3$ into sub-stoichiometric phases exhibiting metallic-like conductivity. Specifically, we analyze how the delocalization of W$5d$ electrons around defect-rich regions induces electronic states near the Fermi level, decoupling the Seebeck coefficient from electrical conductivity. Simultaneously, we discuss how these engineered defect networks and shear planes selectively enhance phonon scattering, drastically suppressing lattice thermal conductivity without hindering electronic transport. By establishing PLD as an effective approach for precise oxygen stoichiometry and defect architecture control, this review highlights the high-temperature potential of tungsten Magnéli phases and outlines future pathways to maximize their thermoelectric figure of merit ($ZT$). Full article

Cu-Ni co-deposit electrodes were prepared and tested in an undivided cell for the electrochemical removal of nitrate from aqueous solutions. Pulsed electrodeposition (PED) under a dynamic hydrogen bubble template and direct electrodeposition (DE) techniques were used for synthetizing porous nickel- and copper-based cathodes. Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analyses showed dendritic and cauliflower-like deposits with a uniform distribution of nickel and copper on the electrode surface, both using flat and foam nickel supports. The PED technique on nickel foam generated highly porous Cu-Ni coatings, with the largest electrochemical active surface area (ECSA) among all the investigated electrodes. Electrolysis in alkaline solutions containing nitrates was performed in an undivided cell in potentiostatic mode. The selectivity towards N₂ was strongly dependent on both copper loading and applied potential; in particular, the foam electrode containing about 23% Cu showed very low ammonia production even at the highest cathodic overpotential, evidencing its marked preference for nitrogen formation. The process performed in the undivided cell using foam-supported Cu-Ni cathodes enabled 100% of conversion of nitrate to molecular nitrogen within approximately 7 h, allowing the complete denitrification of the water. Full article

The integration of carbon nanomaterials with organic compounds offers a promising strategy for developing next-generation electrode materials with superior properties. A novel type of carbon paste electrode was fabricated by modifying a graphite matrix with functionalized multiwalled carbon nanotubes and juglone as a redox mediator, and then it was deposited by manual packing into a PEEK body (JUG-MWCNT/CPE). The surface morphology and structural parameters of the composite materials were meticulously characterized using scanning electron microscopy (SEM), nitrogen adsorption–desorption isotherms, and spectroscopic techniques, while their electrochemical properties were rigorously evaluated using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). This study demonstrates that the synergistic interaction between the conductive nanotube network and the electroactive juglone significantly reduces the oxidation overpotential and enhances the peak current response of melatonin. Under optimized DPV parameters, the developed sensor presents outstanding analytical performance, featuring a wide linear response range from 0.002 to 0.16 mg L⁻¹, a low detection limit of 0.49 µg L⁻¹, excellent long-term signal stability for up to 30 days, and valid applicability for real-sample monitoring in commercial tablets and dietary supplements. Full article

Transition metal oxides constitute an important materials platform for chromic phenomena because their optical response is strongly coupled to the changes in electronic structure, phase state, carrier concentration, and defect chemistry. This review discusses selected transition metal oxide thin films, with emphasis on VO₂ and other vanadium oxides, WO₃, NiO, and TiO₂. The review summarizes the structural and electronic characteristics of these representative oxide systems and highlights the role of phase composition, crystal structure, oxygen non-stoichiometry, and defect chemistry in determining their optical response. The main thin film preparation routes, including pulsed laser deposition, magnetron sputtering, sol–gel and aerosol spray methods, atomic layer deposition, chemical vapor deposition, electrochemical routes, and molecular beam epitaxy, are reviewed with respect their influence on obtained thin films. Particular attention is given to applications in thermochromic VO₂-and electrochromic WO₃/NiO-based smart windows, and transition metal oxide-based gasochromic hydrogen sensors. Key challenges related to transition temperature tuning, luminous transmittance, solar modulation, optical contrast, cycling stability, ion transport and large-area integration are also discussed. Overall this review provides a comparative overview of selected transition metal oxide thin films by connecting material chemistry and physics, thin film preparation technology and functionality. Full article

Diluted solar saltworks effluent, applied via fertigation, can contribute to circular economy strategies by recycling nutrients and reducing the environmental impact associated with the disposal of hypersaline effluents. However, its adoption in drip irrigation systems is still limited, as are its effects on emitter performance. This study investigated whether electronic pulses could mitigate emitter clogging by applying dilution of saltworks bittern. Three systems (freshwater + saltworks bittern + electronic pulses; freshwater without electronic pulses; and freshwater + saltworks bittern without electronic pulses) were evaluated in Mossoró, Brazil, using three emitter designs over 0–320 h. Water physicochemical properties and hydraulic performance were monitored, and deposits were characterized by SEM—EDS and FTIR. Electronic pulses did not change bulk water chemistry but were associated with lower total suspended solids. Clogging risk was mainly related to alkaline pH, high electrical conductivity, and elevated Ca²⁺ and Mg²⁺ concentrations, which kept effluent dilutions within a high-risk range. Untreated effluent reduced irrigation uniformity, whereas treated effluent performed similarly to supply water. Electronic pulses reduced deposit complexity and the severity of critical events but did not eliminate clogging, and responses dependent on the emitter labyrinth’s geometry. Full article

The long-term stability of biodegradable polymer coatings deposited by matrix-assisted pulsed laser evaporation (MAPLE) remains insufficiently understood, particularly under ultraviolet irradiation conditions where photochemical effects may accompany material transfer. In this work, thin films of poly(lactide-co-caprolactone)-block-poly(ethyleneglycol)-block-poly(lactide-co-caprolactone), also known as PLCL-PEG-PLCL, are deposited from chloroform solutions by UV-MAPLE using a nanosecond Nd:YAG laser operating at 266 nm over a wide laser fluence range (0.25–0.9 J/cm²). The effect of laser fluence on the morphological, structural, and chemical evolution of the coatings is investigated by atomic force microscopy (AFM), scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDS), focused ion beam scanning electron microscopy (FIB-SEM), and X-ray diffraction (XRD). At low laser fluence, relatively homogeneous coatings are obtained while largely preserving the characteristic functional groups of the triblock copolymer. Increasing the laser fluence progressively induces surface restructuring phenomena, including droplets, wrinkles, and the appearance of highly symmetric faceted structures. These entities develop preferentially in samples deposited at elevated fluence and frequently appear only after prolonged aging under ambient conditions, revealing delayed recrystallization behaviour associated with metastable species generated during the deposition process. EDS analyses reveal localized chlorine enrichment within the faceted structures, while FIB-SEM investigations show porous internal morphologies. XRD confirms that the polymer matrix remains predominantly amorphous. The combined observations suggest that UV-MAPLE deposition from chloroform involves not only physical material transfer but also photochemical processes that promote decomposition, recombination, and delayed crystallization phenomena. A phenomenological model describing the successive stages of surface evolution, aging, and recrystallization is proposed. These results provide new insight into the long-term evolution of laser-deposited biodegradable polymer coatings and highlight the importance of solvent selection and processing conditions in determining their stability. Full article

Nickel ferrite (NiFe₂O₄) is one of the most studied inverse-spinel ferrites because it combines moderate saturation magnetization, comparatively high electrical resistivity, chemical stability, and broad synthesis flexibility. Yet the literature shows that the measured structure and magnetism of NiFe₂O₄ are not intrinsic constants; they evolve strongly with dimensionality, size, thickness, strain state, cation distribution, surface spin disorder, and synthesis pathway. This review develops a unified theoretical and literature-based interpretation of how dimensionality reshapes the structural and magnetic behavior of NiFe₂O₄ across bulk ceramics, nanoparticles, one-dimensional nanostructures, polycrystalline thin films, and ultrathin epitaxial films. The review is anchored in the two uploaded nickel ferrite attachments and expanded using internet-sourced journal literature on spinel inversion, surface effects, mechanochemical synthesis, sputtered and pulsed laser deposited thin films, and epitaxial ultrathin-film anomalies. The central novelty of this article is the formulation of a dimensionality-dependent framework in which the observed magnetic response is governed by a competition among three coupled factors: (i) the cation-distribution function, which controls the A–B superexchange balance and therefore the net ferrimagnetic moment; (ii) the microstructural coherence function, which measures how crystallinity, strain, defects, and anti-phase boundaries preserve or degrade exchange continuity; and (iii) the surface/interface spin-order parameter, which quantifies the loss or reconfiguration of magnetic order at free surfaces and buried interfaces. Within this framework, bulk NiFe₂O₄ behaves as a near-equilibrium inverse spinel with relatively stable magnetization, whereas nanoscale NiFe₂O₄ experiences strong spin canting and finite-size suppression due to the growing fraction of disordered surface spins. Thin films introduce a distinct regime in which strain, texture, anti-phase boundaries, substrate mismatch, and growth kinetics determine both anisotropy and magnetization. In ultrathin epitaxial films, off-equilibrium cation redistribution and interface-controlled electronic reconstruction may even generate magnetization values far above bulk expectations. The review also compares major synthesis routes—solid-state reaction, sol–gel, co-precipitation, hydrothermal growth, reactive milling, combustion, pulsed laser deposition, and radio-frequency sputtering—and explains why each route biases the final dimensionality-dependent properties differently. A set of word-style equations is provided to formalize spinel inversion, finite-size suppression, anisotropy scaling, coercivity trends, and superparamagnetic crossover. Beyond summarizing the field, the review proposes a regime map linking dimensionality to characteristic structural defects and magnetic signatures, and it identifies unresolved questions concerning the true origin of enhanced magnetization in ultrathin NiFe₂O₄, the interplay between anti-phase boundaries and strain, and the distinction between intrinsic inversion changes and extrinsic substrate artifacts. The resulting article offers a submission-ready, originality-focused review that positions dimensionality as the master variable governing structure–magnetism correlations in nickel ferrite. Full article

In view of the fact that there are few reports on the preparation of NbC coating by high-power pulsed magnetron sputtering (HiPIMS) technology. In this study, the effects of NbC interlayer thickness on the microstructure, corrosion resistance and electrical conductivity of Nb/NbC/C multilayer coatings for proton exchange membrane fuel cell (PEMFC) bipolar plates were studied by using the high ionization characteristics of HiPIMS technology. A series of Nb/NbC/C multilayer coatings with varying NbC interlayer thicknesses was deposited via HiPIMS by modulating the deposition time (20, 40, and 60 min). The microstructure and properties of the coatings were characterized using scanning electron microscopy (SEM), Raman spectroscopy, interfacial contact resistance (ICR), and corrosion current, among other methods. The results indicate that as the NbC interlayer thickness increases, the total coating thickness increases from 0.43 μm to 1.42 μm. All coatings exhibit a uniform and dense microstructure lacking typical coarse columnar structures. Raman and XPS analyses show that the I_D/I_G ratio increases from 1.98 to 4.04, indicating an increase in sp²-hybridized bond content and a decrease in sp³ content. At a deposition time of 60 min, the coating achieved optimal performance, yielding a critical load (Lc1) of 31.9 N, the lowest average friction coefficient (0.27), the minimum corrosion current density, and an interfacial contact resistance of 7.5 mΩ·cm². These results demonstrate that the NbC interlayer thickness significantly governs the structure and properties of the Nb/NbC/C multilayer coatings. Specifically, an appropriate increase in the NbC interlayer thickness optimizes the sp²/sp³ hybrid bond ratio, thereby enhancing the overall coating performance. Full article

One-dimensional fibrous scaffolds with tunable bioactivity offer promise for bone tissue regeneration, yet optimal calcium phosphate phases for enhancing osteogenic performance remain underexplored. This study aimed to evaluate the impact of monetite-, brushite-, and cerium-doped phosphate deposition on electrospun nylon nanofibres functionalised via matrix-assisted pulsed laser evaporation (MAPLE). Five nylon fibre compositions were synthesised, coated with three calcium phosphate phases, and calcined at varying temperatures (500–800 °C) before laser deposition. Physicochemical properties were assessed using energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), and fibre diameter measurements, averaging $62.1\pm 23.8$ nm. Biocompatibility assays following MC3T3 preosteoblast seeding and incubation evaluated biological performance. EDX confirmed homogeneous phase deposition; SEM showed phase- and temperature-dependent morphology, with monetite yielding uniform granular structures and cerium-doped phosphate at 800 °C forming dense aggregates. Brushite-coated fibres exhibited superior preosteoblast metabolic activity, reaching $178\pm 2\%$ after 48 h (p < 0.001), indicating phase-specific stimulation of bone cell growth. These phosphate-functionalised nylon fibres retain structural integrity, hierarchical porosity, and enhanced bioactivity, providing a versatile electrospinning-MAPLE platform for customisable bone grafts with clinical potential. Full article

Controlling deposition parameters is fundamental to obtaining the desired properties of cathodic arc physical vapor deposition (PVD) coatings. Achieving uniform coatings on tools with complex, sharp geometries remains a significant challenge due to localized ion flux concentration. Pulsing the substrate bias is an effective way of controlling deposition energy. However, while widely used in cathodic arc PVD, the relationship between the actual bias waveform, coating integrity on sharp tool geometries, and resulting machining performance has not been systematically established. This study investigates the effect of pulsed bias duty cycle (20% to 90%) and frequency (1 to 20 kHz) on the microstructural evolution, residual stress state, and machining performance of AlTiN coated tools. Real-time oscilloscope measurements demonstrated that system inductance and capacitance significantly distort the ideal bias waveform. Microstructural analysis via Focused Ion Beam/Scanning Electron Microscopy (FIB/SEM) cross-sectioning confirmed that all bias parameters generated a dense microstructure. While pulse frequency had no significant influence on micromechanical properties or residual stress states, the duty cycle was the dominant variable. High-energy deposition (90% duty cycle) increased hardness to 33.9 GPa but generated severe compressive residual stresses (−5.2 GPa). This extreme compressive stress led to catastrophic edge delamination on sharp solid carbide endmills. Conversely, a low-energy 20% duty cycle generated a coating with lower hardness (29.4 GPa) and a near-neutral stress state (0.5 GPa), effectively preserving the edge integrity. Unlike the endmills, the turning inserts maintained their edge integrity across all deposition conditions. During the high-speed (350 m/min) dry turning of AISI 304 stainless steel, all evaluated coatings exhibited comparable tool life and cutting forces. Wear progression was characterized by rake cratering, combined with abrasion and adhesion-induced attrition on the flank. The results indicate that tool life in this extreme environment is governed primarily by high-temperature thermo-chemical stability rather than initial room-temperature hardness. Lower-energy pulsed bias deposition therefore represents a robust strategy for coating a wide range of tool geometries, delivering equivalent high-speed machining performance while preventing stress-induced delamination on sharp features. Full article

The growing demand for structural coloration methods that simultaneously exhibit an iridescent sheen effect and a base color on transparent substrates calls for a single-step fabrication procedure capable of periodic and localized modulation of thin-film structure. In this work, a composite thin-film structure consisting of aluminum nitride-aluminum (AlN-Al)-soda-lime glass substrate is designed, deposited, and subsequently processed using burst-mode femtosecond laser. By systematically varying the number of sub-pulses, the pulse-to-pulse distance, and the average laser power while maintaining a fixed single-sub-pulse energy (1 μJ), the precise control over thermal accumulation and surface protrusion morphology is achieved, resulting in a series of highly transparent structural colors with iridescent sheen effects. Reflectance spectra, transmittance data, confocal microscopy, scanning electron microscopy and coupled energy dispersive spectrometer analyses, and the finite-difference time-domain simulations reveal that the observed color variation originates from laser-induced air gaps between the Al and AlN layers, rather than from compositional changes, and that the resulting periodic surface protrusion structures govern the iridescent sheen effect. The proposed method enables large-scale patterning while preserving high transmittance, as demonstrated by the desired hue, saturation, and iridescent sheen. This burst-mode laser processing strategy offers a material- and production line-compatible route for realizing coupled interference- and diffraction-based structural colors, with promising applications in decorative purposes with anti-counterfeiting or encryption purposes, where both angle-independent base color and angle-dependent iridescent sheen effect are required. Full article

Laser-induced breakdown in water-rich biological media results from the interplay between primary photoionization processes and avalanche amplification of free electrons. Understanding this competition is essential for predicting ablation thresholds under ultrashort-pulse irradiation. In this work, we develop an analytical rate-equation model for the buildup of electron density in water-like biological tissues. It combines photoionization and chromophore ionization into a single seed-generation term, while avalanche ionization is described through a cascade gain factor. This formulation provides a framework for describing cascade electron-impact ionization processes in liquid-like media under strong-field excitation. Our approach gives an analytical expression for the temporal evolution of electron density driven by a Gaussian laser pulse and makes it possible to separate the contributions of direct ionization of water and ionization of chromophore centers. The analytical results are compared with numerical simulations that include carrier diffusion, bimolecular recombination and trapping. The comparison clarifies the roles of seed formation and cascade amplification in the growth of the electron population. The predicted dependence of threshold fluence on pulse duration agrees well with experimental data reported for water-like tissues such as the corneal tissues at a wavelength of 800 nm. The model provides a simple analytical picture of ultrafast plasma formation and electron-driven energy deposition in water-like biological media. Full article

Cobalt/copper (Co/Cu) multilayers are prototypical systems for giant magnetoresistance (GMR)-based spintronic devices, where interfacial quality and spin-dependent scattering critically determine performance. In this work, Co/Cu multilayers were fabricated by pulsed laser deposition (PLD) on SITAL ceramics, Si(100), and BK7 substrates, with 10, 20, and 40 bilayer repetitions, in order to elucidate the interplay between microstructure, interfacial diffusion, and magnetotransport properties. Systematic characterization combining atomic force microscopy (AFM), scanning electron microscopy (SEM), SIMS/SNMS depth profiling, vibrating sample magnetometry (VSM), and Hall effect measurements reveals that PLD enables controlled multilayer growth with low background roughness and well-defined periodic structures, despite the presence of characteristic particulates. A clear dependence of the GMR response on both bilayer number and substrate type is observed. Increasing the number of repetitions enhances spin-dependent scattering at Co/Cu interfaces, leading to a progressive increase in the magnetoresistance amplitude, reaching ~−14% for 40-period multilayers on SITAL substrates. This enhancement is attributed to the higher interface density and improved interfacial coherence, as confirmed by SIMS/SNMS analysis showing reduced interdiffusion in thicker stacks. In parallel, Hall effect measurements indicate a reduction in carrier density and an increase in carrier mobility with increasing multilayer thickness, consistent with improved charge transport stability. A pronounced substrate effect is demonstrated: SITAL-supported multilayers exhibit enhanced GMR sensitivity (up to ~44%·T⁻¹) due to increased diffuse spin-dependent scattering at rougher interfaces, whereas Si(100) substrates promote smoother growth, improved structural coherence, and more stable electronic transport. While sputtering typically enables smoother interfaces and higher GMR ratios, PLD offers enhanced flexibility in tailoring interfacial morphology and diffusion processes, which can lead to improved sensitivity under specific conditions. These results establish PLD as a versatile route for tailoring Co/Cu multilayers, enabling controlled optimization of the trade-off between sensitivity and structural quality for advanced spin-valve and magnetic sensor applications. Full article