Surfaces

Aluminum nitride (AlN) thin films were deposited on SiO₂ substrates by RF-magnetron sputtering at varying powers (110–140 W) and subsequently subjected to thermal annealing at 450 °C under nitrogen atmosphere. A comprehensive multi-technique investigation—including X-ray reflectometry (XRR), X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), optical profilometry, spectroscopic ellipsometry (SE), and electrical measurements—was performed to explore the physical structure, morphology, and optical and electrical properties of the films. The analysis of the film structure by XRR revealed that increasing sputtering power resulted in thicker, denser AlN layers, while thermal treatment promoted densification by reducing density gradients but also induced surface roughening and the formation of island-like morphologies. Optical studies confirmed excellent transparency (>80% transmittance in the near-infrared region) and demonstrated the tunability of the refractive index with sputtering power, critical for optoelectronic applications. The electrical characterization of Au/AlN/Al sandwich structures revealed a transition from Ohmic to trap-controlled space charge limited current (SCLC) behavior under forward bias—a transport mechanism frequently present in a material with very low mobility, such as AlN—while Schottky conduction dominated under reverse bias. The systematic correlation between deposition parameters, thermal treatment, and the resulting physical properties offers valuable pathways to engineer AlN thin films for next-generation optoelectronic and high-frequency device applications. Full article

Bioactive glasses are known for their surface reactivity and ability to bond with bone tissue through the formation of hydroxyapatite. This study investigates the effects of substituting ultrapure water with natural geothermal waters from the Azores in the sol–gel synthesis of 45S5 and MgO-modified bioglasses. Using high-resolution X-ray photoelectron spectroscopy (XPS), we examined how the mineral composition of the waters influenced the chemical environment and network connectivity of the glass surface. The presence of trace ions, such as Mg²⁺, Sr²⁺, Zn²⁺, and B³⁺, altered the silicate structure, as evidenced by binding energy shifts and peak deconvolution in O 1s, Si 2p, P 2p, Ca 2p, and Na 1s spectra. Thermal treatment further promoted polymerization and reduced hydroxylation. Our findings suggest that mineral-rich waters act as functional agents, modulating the reactivity and structure of bioactive glass surfaces in eco-sustainable synthesis routes. Full article

Microbial extracellular polymeric substances (EPSs) are emerging as sustainable alternatives to conventional corrosion inhibitors due to their eco-friendly nature, biodegradability, and functional versatility. Secreted by diverse microorganisms including bacteria, fungi, archaea, and algae, EPSs are composed mainly of polysaccharides, proteins, lipids, and nucleic acids. These biopolymers, chiefly polysaccharides and proteins, are accountable for surface corrosion prevention through biofilm formation, allowing microbial survival and promoting their environmental adaptation. Usually, EPS-mediated corrosion inhibitions can take place via different mechanisms: protective film formation, metal ions chelation, electrochemical property alteration, and synergy with inorganic inhibitors. Even though efficacious EPS corrosion prevention has been demonstrated in several former studies, the application of such microbial inhibitors remains, so far, a controversial topic due to the variability in their composition and compatibility toward diverse metal surfaces. Thus, this review outlines the microbial origins, biochemical properties, and inhibition mechanisms of EPSs, emphasizing their advantages and challenges in industrial applications. Advances in synthetic biology, nanotechnology, and machine learning are also highlighted and could provide new opportunities to enhance EPS production and functionality. Therefore, the adoption of EPS-based corrosion inhibitors represents a promising strategy for environmentally sustainable corrosion control. Full article

It is widely recognized that fine surface structures found in nature contribute to surface functionality, and studies on the design of functional materials based on biomimetics have been actively conducted. In this study, polymer thin films with hierarchically ordered surface structure were prepared by combining both nanoimprinting using anodically oxidized porous alumina (AAO) as a template and surface-initiated atom transfer radical polymerization (SI-ATRP). To prepare such polymer films, we designed a new copolymer (poly{[2-(4-methyl-2-oxo-2H-chromen-7-yloxy)ethyl methacrylate]-co-[2-(2-bromo-2-methylpropionyloxy)ethyl methacrylate]}; poly(MCMA-co-HEMABr)) with coumarin moieties and α-haloester moieties in the pendants. The MCMA repeating units function to fix the pillar structure by photodimerization, and the HEMABr ones act as the polymerization initiation sites for SI-ATRP on the pillar surfaces. Surface structures consisting of vertically oriented multiple pillars were fabricated on the spin-coated poly(MCMA-co-HEMABr) thin films by nanoimprinting using an AAO template. Then, the coumarin moieties inside each pillar were crosslinked by UV light irradiation to fix the pillar structure. SEM observation confirmed that the internally crosslinked pillar structures were maintained even when immersed in organic solvents such as 1,2-dichloroethane and anisole, which are employed as solvents under SI-ATRP conditions. Finally, poly(2,2,2-trifluoroethyl methacrylate) and poly(N-isopropylacrylamide) chains were grafted onto the thin film by SI-ATRP, respectively, to prepare the hierarchically ordered surface structure. Furthermore, in this study, the surface properties as well as the thermoresponsive hydrophilic/hydrophobic switching of the obtained polymer films were investigated. The surface morphology and chemistry of the films with and without pillar structures were compared, especially the interfacial properties expressed as wettability. Grafting poly(TFEMA) increased the static contact angle for both flat and pillar films, and the con-tact angle of the pillar film surface increased from 104° for the flat film sample to 112°, suggesting the contribution of the pillar structure. Meanwhile, the pillar film surface grafted with poly(NIPAM) brought about a significant change in wettability when changing the temperature between 22 °C and 38 °C. Full article

Understanding strain behavior near grain boundaries is critical for controlling structural distortions and oxygen vacancy migration in perovskite oxides. However, conventional techniques often lack the spatial resolution needed to analyze phase and domain evolution at the nanoscale. In this paper, polarization-dependent second-harmonic generation (SHG) imaging is employed as a tool to probe local symmetry breaking and complex domain structures in the vicinity of a low-angle grain boundary of SrTiO₃ (STO) bicrystals. We show that the anisotropic strain introduced by a tilted grain boundary produces strong local distortions, leading to the coexistence of tetragonal and rhombohedral domains. By analyzing SHG intensity and variations in the second-order nonlinear optical susceptibility, we map the distribution of strain fields and domain configurations near the boundary. In pristine samples, the grain boundary acts as a localized source of strain accumulation and symmetry breaking, while in samples subjected to intentional electrical stressing, the SHG response becomes broader and more uniform, suggesting strain relaxation. This work highlights SHG imaging as a powerful technique for visualizing grain-boundary-driven structural changes, with broad implications for the design of strain-engineered functional oxide devices. Full article

This study presents the influence of pH control agents and pH value on the physical properties of ZnO thin films obtained by chemical bath deposition. ZnO thin films were synthesized on glass substrates using precursor solutions of different pHs prepared from two bases: sodium hydroxide (NaOH) and ammonia (NH₃). The effect of pH values on the morphological, structural, and optical properties of ZnO thin films was investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and UV–Visible spectroscopy. XRD results showed that all the synthesized ZnO thin films are polycrystalline and crystallize in a hexagonal wurtzite structure. The crystallite size, calculated using the Debye–Scherrer formula, varied from 10.50 nm to 11.69 nm for ZnO thin films obtained with NH₃ and from 20.79 nm to 27.76 nm for those obtained with NaOH. FTIR analysis confirmed the presence of functional groups. SEM images indicated that not only the base but also the pH affects the morphology of the films, giving rise to different granular shapes. Overall, the ZnO thin films obtained with NaOH looked more mesoporous compared to those obtained with NH₃. Optical characterization results showed that whatever the base used, the pH of the precursor solution affected the ZnO thin film transmittance. Films synthesized with NH₃ exhibited the best transmittance (80%) at pH 8.5, while the best transmittance (81%) of films synthesized with NaOH was obtained at pH 8 in the visible region. Based on optical and morphological properties, ZnO films obtained from NH₃ at pH 8.5 are found to be more suitable as photoanodes in dye-sensitized solar cells. Full article

To promote the optimization of the anti-friction and anti-wear behavior of lightweight TiAl alloys, γ-TiAl-10 wt.% Ag self-lubricating composites were fabricated, and their mechanical and tribological properties were tested. The results showed that the silver in TiAl-10 wt.% Ag slightly reduced its mechanical properties compared with those of pure TiAl alloys. A silver-enriched lubrication film formed on a wear scar, which was helpful in improving the friction and wear behavior. It was found that a large amount of silver gathered at a wear scar, gradually spread out under the action of the sliding friction force, and then increased the silver distribution areas on the wear scar, leading to the good formation of a silver-rich film. Furthermore, an identification model was established to calculate the specific area η of the silver film. A quantitative relationship indicated that an increase in the Ag distribution area improved the tribological behavior of γ-TiAl-10 wt.% Ag. When the specific area η of a silver-rich film was maintained at 44–51%, the small friction coefficient (almost 0.28) and wear rate (about 2.25 × 10⁻⁴ mm³·N⁻¹·m⁻¹) were well stabilized. This provides a new research method to improve the tribological performance of TiAl-Ag samples. Full article

Electroless silver (Ag) plating has emerged as a simple yet effective surface modification technique, garnering significant attention in consumer electronics and composite materials. This study systematically investigates the influence of glucose dosage on the microstructural refinement of Ag coatings deposited from silver–ammonia solutions onto iron (Fe) particles while also evaluating the oxidation resistance of Ag-plated particles through thermogravimetric analysis. Optimal results were achieved at a silver nitrate concentration of 0.02 mol/L and a glucose concentration of 0.05 mol/L, producing Fe particles with a uniform and dense silver coating featuring an average Ag grain size of 76 nm. The moderate excess glucose played a dual role: facilitating Ag⁺ ion reduction while simultaneously inhibiting the growth of Ag atomic clusters, thereby ensuring microstructural refinement of the silver layer. Notably, the Ag-plated particles demonstrated superior oxidation resistance compared to their uncoated counterparts. These findings highlight the significance of fine-grained electroless Ag plating in developing high-temperature conductive metal particles and optimizing interfacial structures in composite materials. Full article

Thin films of manganese–nickel–cobalt oxide with graphene (G@MNCO) were deposited on copper foam using electrochemical deposition. NiCo₂O₄ is the main phase in these films. As the proportion of graphene in the precursor solution increases, the oxygen vacancies in the samples also increase. The microstructure of these samples evolves into hierarchical vertical flake structures. Cyclic voltammetry measurements conducted within the potential range of 0–1.2 V reveal that the electrode with the highest graphene content achieves the highest specific capacitance, approximately 475 F/g. Furthermore, it exhibits excellent cycling durability, maintaining 95.0% of its initial capacitance after 10,000 cycles. The superior electrochemical performance of the graphene-enhanced, manganese-doped nickel–cobalt oxide electrode is attributed to the synergistic contributions of the hierarchical G@MNCO structure, the three-dimensional Cu foam current collector, and the binder-free fabrication process. These features promote quicker electrolyte ion diffusion into the electrode material and ensure robust adhesion of the active materials to the current collector. Full article

Growing demand for chemically resistant, thermally stable, and anti-icing coatings has intensified interest in boron nitride (BN)-based materials and surface coatings. In this study, BN coatings were developed on mild steel (MS) via chemical vapour deposition (CVD) at 1200 °C for 15, 30, and 60 min, and their structural, surface, and water-repellent characteristics were evaluated. X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) spectroscopy confirmed the successful formation of BN, while water contact angle measurements indicated high hydrophobicity, demonstrating excellent barrier properties. Scanning electron microscopy (SEM) revealed morphological evolution from flower- and needle-like BN structures in the sample placed in the CVD furnace for 15 min to dense, coral-like, and tubular networks in the samples placed for 30 and 60 min. These findings highlight that BN coatings, particularly the one obtained after 30 min of deposition, have a high hydrophobic character following the Cassie–Baxter model and can be used for corrosion resistance and anti-icing on MS, making them ideal for industrial applications requiring long-lasting protection. Full article

Polyaryletherketone (PAEK) polymers inherently exhibit low surface activity, leading to poor adhesive bonding performance when using epoxy-based adhesives. In this study, low-temperature plasma surface modification was conducted on carbon fiber-reinforced polyetherketone ketone (CF/PEKK) composites to investigate the influence of plasma treatment parameters on their lap shear strength. Surface characterization was systematically performed using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and contact angle analysis to evaluate morphological, chemical, and wettability changes induced via plasma treatment. The results demonstrated a significant enhancement in lap shear strength after plasma treatment. Optimal bonding performance was achieved at a treatment speed of 10 mm/s and a nozzle-to-substrate distance of 5 mm, yielding a maximum shear strength of 28.28 MPa, a 238% improvement compared to the untreated control. Notably, the failure mode transitioned from interfacial fracture in the untreated sample to a mixed-mode failure dominated by cohesive failure of the adhesive and substrate. Plasma treatment substantially reduced the contact angle of CF/PEKK, indicating improved surface wettability. SEM micrographs revealed an increased micro-porous texture on the treated surface, which enhanced mechanical interlocking between the composite and adhesive. XPS analysis confirmed compositional alterations, specifically elevated oxygen-containing functional groups on the plasma-treated surface. These modifications facilitated stronger chemical bonding between CF/PEKK and the epoxy resin, thereby validating the efficacy of plasma treatment in optimizing surface chemical activity and adhesion performance. Full article

The failure of a porcelain insulator on a transmission line is a crucial cause of power supply interruptions, leading to poor reliability and revenue loss. The insulator’s performance is adversely affected by environmental contaminants, and wettability intensifies this adverse effect by developing a conductive path along the insulator’s surface, leading to premature flashover and insulator failure. This work aims to analyze the response of the electric field distribution and current density using the finite element method (FEM) under different wettability conditions. Discrete water droplets were placed along the surface, and the contact angle was varied to represent different levels of surface hydrophobicity. Abrupt rises and spikes were observed on the plots for the electric field and current density distribution, indicating distortion; however, the distortion kept on decreasing with the increase in the contact angle. Overall, the average stress followed a declining pattern, where the values of the electric field were reduced from 2.588 to 2.412 kV/cm, and current the density was reduced from 0.187 to 0.068 nA/cm² for an increase in the contact angle from 60° to 140°. Simulation results advocate for hydrophobic insulator surfaces. Therefore, a proper coating is necessary to enrich hydrophobicity and mitigate the adversity of wettability. Polyurethane, due to its excellent hydrophobic and insulating properties, offers a potential coating. Flashover voltage tests have been performed for the coated insulator under dry and wet conditions, where the flashover voltage improved from 79.14 kV to 82.04 kV and 48.4 kV to 53.8 kV, respectively, which supports the simulations’ outcomes. Full article

Graphene oxide (GO) films have attracted significant attention due to their potential in separation and filtration applications. Based on their unique lamellar structure and ultrathin nature, GO films are difficult to maintain in a free-standing form and typically require substrate support. Consequently, understanding their film formation behavior and mechanisms on substrates is of paramount importance. This work employs commonly used nonwoven fibrous membranes as substrates and guided by the coffee-ring theory, systematically investigates the film formation behaviors, film morphology, and underlying mechanisms of GO films on fibrous membranes with varying wettability. Fibrous membranes with different wetting properties—hydrophilic, hydrophobic, and superhydrophobic—were prepared via electrospinning and initiated chemical vapor deposition (iCVD) surface modification techniques. The spreading behaviors, deposition dynamics, capillary effects, and evaporation-induced film formation mechanisms of GO suspensions on these substrates were thoroughly examined. The results showed that GO formed belt-like, ring-like, and circular patterns on the three fibrous membranes, respectively. GO films encapsulated more than the upper half, approximately the upper half, and the top portion of fibers, respectively. Pronounced wrinkling of GO films was observed except for those on the hydrophilic fibrous membrane. This work demonstrates that tuning the wettability of fibrous substrates enables precise control over GO film morphology, including fiber encapsulation, wrinkling, and coverage area. Furthermore, it deepens the understanding of the interactions between 1D nanofibers and 2D GO sheets at low-dimensional scales, laying a foundational basis for the optimized design of membrane engineering. Full article

Transition metal dichalcogenides, especially molybdenum disulfide (MoS₂), exhibit exceptional properties that make them suitable for a wide range of applications. However, the interaction between MoS₂ and technologically relevant substrates, such as platinum (Pt) electrodes, can significantly influence its properties. This study investigates the growth and properties of MoS₂ thin films on Pt substrates using ionized jet deposition, a versatile, low-cost vacuum deposition technique. We explore the effects of the roughness of Pt substrates and self-heating during deposition on the chemical composition, structure, and strain of MoS₂ films. By optimizing the deposition system to achieve crystalline MoS₂ at room temperature, we compare as-deposited and annealed films. The results reveal that as-deposited MoS₂ films are initially amorphous and conform to the Pt substrate roughness, but crystalline growth is reached when the sample holder is sufficiently heated by the plasma. Further post-annealing at 270 °C enhances crystallinity and reduces sulfur-related defects. We also identify a change in the MoS₂–Pt interface properties, with a reduction in Pt–S interactions after annealing. Our findings contribute to the understanding of MoS₂ growth on Pt and provide insights for optimizing MoS₂-based devices in catalysis and electronics. Full article

Porous PZT films offer significant potential due to tunable electromechanical properties, yet the polarization behavior remains insufficiently understood because of discontinuous morphology and domain structures. In this work, we study the impact of porosity on the spontaneous polarization and electromechanical response of PZT thin films fabricated using a multilayer spin-coating technique with various concentrations (0–14%) of polyvinylpyrrolidone (PVP) as a porogen. Atomic force microscopy (AFM) and piezoresponse force microscopy (PFM) were employed to analyze the local topography, domain distribution, and polarization behavior of the films. The results indicate that increasing porosity leads to substantial changes in grain morphology, dielectric permittivity, and polarization response. Films with higher porosity exhibit a more fragmented polarization distribution and reduced piezoresponse, while certain orientations demonstrate enhanced domain mobility. Despite the decrease in overall polarization, the local coercive field remains relatively stable, suggesting structural stability during the local polarization switching. The findings highlight the crucial role of grain boundaries and local charge redistribution in determining local polarization behavior. Full article

Titanium thin films with thicknesses of up to 105 nm were deposited on borosilicate glass implementing low-power continuous (25 W) and pulsed (85 W, with an ultra-low duty cycle) DC magnetron sputtering. The characteristics of the resulting films were studied via atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), VIS spectroscopy, and four-point-probe measurements. Both deposition modes yield films with low surface roughness, and AFM analysis showed no topographical features indicative of columnar-and-void structures. The films exhibited high optical reflectivity and stable transmittance and reflectance across the visible spectrum. The electric resistivity could be measured even at single nanometer thickness, emphasizing the metallic character of the films and approaching the bulk titanium value at higher film thicknesses. The low power regime of magnetron sputter deposition not only offers the possibility of studying the development of physical characteristics during the growth of ultra-thin films but also provides the advantage of extremely low heat development and no evident mechanical stress on the substrate during the coating process. These results outline a path for low-power DC sputtering as a reliable approach for studying the evolution of functional properties in ultra-thin films and for the gentle fabrication of coatings where thermal stress must be avoided, making the method compatible with temperature-sensitive applications. Full article

Magnetic shape memory alloys have attracted considerable attention due to their multifunctional properties. Among these materials, Ni-Mn-Ga alloys are distinguished by their ability to achieve up to 10% strain when exposed to a magnetic field, a characteristic predominantly observed in single-crystal samples. Consequently, it is essential to develop nanomaterials with a crystal structure closely resembling that of a single crystal. In this study, an epitaxial Ni-Mn-Ga thin film was fabricated using Pulsed Laser Deposition on an Al₂O₃ $\left(11\overline{2}0\right)$ single-crystal substrate. The crystal structure was characterised through X-ray diffraction methodologies, such as symmetrical $2\theta -\omega$ scans, pole figures, and reciprocal space maps. The results indicated that the sample was mainly in a slightly distorted cubic austenite phase, and some incipient martensite phase also appeared. A detailed microstructural analysis, performed by transmission electron microscopy, confirmed that certain regions of the sample exhibited an incipient transformation to the martensite phase. Regions closer to the substrate retained the austenite phase, suggesting that the constraint imposed by the substrate inhibits the phase transition. These results indicate that it is possible to grow high crystalline quality thin films of Ni-Mn-Ga by Pulsed Laser Deposition. Full article

The combination of the catalytic properties of Al₂O_3/TiO₂ formed an efficient system to degrade the ubiquitous pollutants TPA and PET. The coating (Al₂O₃)_0.75TiO₂ was characterized by X-ray diffraction. Stainless steel disks with photo-catalyst coating were placed transversely in a 3.0 L vertical glass reactor with ascending airflow for supplying oxygen to the reaction medium and visible light lamps for photo-activation. The analysis of the coating homogeneity, morphology and particle size distribution of the TiO₂ coatings and (Al₂O₃)_0.75TiO₂ system were confirmed by SEM. Optical properties and band-gap energy were calculated by using the Tauc equation. UV–Vis spectrophotometry (UV–Vis) and chemical oxygen demand (COD) were the quantitative techniques to measure the reduction in the initial TPA and PET concentrations. Full article

In this study, polymer films based on the inorganic sorbents Al₂O₃, ZrO₂ and SiO₂-phenyl with repellent N,N-diethyl-3-methylbenzamide were prepared and used as functional textile coatings. The high sorption activity of oxides with respect to N,N-diethyl-3-methylbenzamide (63–239 mg/g) allows for the use of these compounds as repellent carrier materials, and their mixture with polyacrylates allows for the formation of functional coatings–polymer films. Scanning electron microscopy and Fourier transform infrared spectroscopy results revealed that the inorganic sorbents Al₂O₃, ZrO₂ and SiO₂-phenyl were successfully anchored in the polyacrylate structure, and the FTIR spectra confirmed the presence of repellent molecules. The thermal diffusion parameters of N,N-diethyl-3-methylbenzamide were also calculated via thermogravimetric analysis and high-performance liquid chromatography with diode array detection. The highest thermal diffusion rates and concentrations were observed for the material with Al₂O₃ (up to 148.3∙10⁻⁹ mol at 200 °C), and lower values for ZrO₂ and SiO₂-phenyl (up to 15.2∙10⁻⁹ mol and 34.3∙10⁻⁹ mol at 200 °C, respectively). The heat flux parameter J_f was also calculated according to Onsager’s theory and Fourier’s law. The release of repellent from polymeric materials can be achieved by applying less heat than that required to reach the boiling point of N,N-diethyl-3-methylbenzamide. Full article