Boron coatings were deposited by RF magnetron sputtering in an Ar atmosphere at a constant power of 80 W, varying the working pressure in the 0.6–5 Pa range. Plasma diagnostics were performed by means of a Langmuir probe to determine the electron temperature and electron density under different operating conditions. Within the investigated pressure range, the deposition rate remained nearly constant, whereas a significant decrease in coating mass density was observed with increasing pressure. The coatings display a columnar structure at all investigated pressures, with no significant differences in bulk morphology. Pressure primarily affects the surface features, leading to an increase in the density, lateral dimensions, and height of surface agglomerates with increasing pressure. Compositional analysis by EDX revealed a substantial oxygen incorporation in the films, with the lowest oxygen content (~11 at.%) measured for the coating deposited at 0.6 Pa. XPS depth profiling confirmed the presence of oxygen and evidenced the formation of boron oxide species, while the boron concentration exceeded 80 at.% in all samples. These results highlight the strong sensitivity of boron film density and oxygen uptake to sputtering pressure.

This work aims to develop a controlled ball milling strategy for preparing FeCoCrNiCu high-entropy alloy (HEA) powders with improved compositional homogeneity while maintaining limited oxygen uptake. Specifically, a novel two-step combined ball milling strategy integrating gradient ball-size configurations with a sequential milling procedure is proposed and systematically evaluated. Compared with conventional single-step milling, the mixed-ball and two-step configurations enhance mechanical alloying (MA) efficiency and promote the formation of more stable FCC and BCC dual-phase structures, as confirmed by X-ray diffraction (XRD) analysis. Compositional standard deviation derived from energy-dispersive X-ray spectroscopy (EDS) measurements indicates improved macroscopic uniformity, while oxygen/nitrogen/hydrogen (ONH) analysis verifies that oxygen incorporation remains limited within the tested processing window. Systematic comparison of jar filling degrees and sampling interruptions further reveals the coupled influence of collision energy distribution and exposure frequency on oxidation behavior. The results demonstrate that controlled energy distribution and minimized atmospheric disturbance are critical for balancing alloying efficiency and oxygen control in FeCoCrNiCu powders.

This study investigates the development and characterization of bioactive films incorporating silver nanoparticles (AgNPs) into biocompatible polymers, namely alginate and chitosan, fabricated using two methods, spin-coating and drop-casting, and aiming to enhance their antimicrobial properties. Dynamic light scattering (DLS) and electrophoretic mobility (EM) of the film precursor solutions revealed significant changes in the nanoparticles’ size and Zeta potential (ZP), reflecting the influence of polymer coatings. Alginate contributed to high electrostatic stability due to its negative charge, while chitosan facilitated specific interactions with negatively charged surfaces. Raman spectroscopy revealed that spin-coating conditions did not successfully result in film formation, highlighting the need for further optimization. Therefore, subsequent characterization studies were conducted only for the films formed by drop-casting. Topographical and nanomechanical assessments of these drop-cast films, using atomic force microscopy (AFM) and force spectroscopy, demonstrated that AgNPs reduced adhesion and elasticity in alginate films, while increasing rigidity and adhesion in chitosan-based films. Antimicrobial tests confirmed the efficacy of AgNPs in both precursor solutions and polymer films, with chitosan-based films that retained structural integrity, which makes them suitable for prolonged applications, while alginate films displayed rapid gelation upon hydration, potentially advantageous in short-term applications. The findings underscore the potential of these biopolymer-AgNP composites in creating antimicrobial materials for food packaging, wound dressings, and other biomedical applications. However, challenges related to film deposition methods, such as spin-coating, require further optimization to improve film formation and reproducibility.

Kraft paper, commonly known as brown paper, has been widely used in the preservation of various food products and is increasingly explored in the development of active packaging materials with antimicrobial functionality by incorporating metal nanoparticles. This study aimed to comparatively investigate the surface modification of Kraft paper with silver nanoparticles (AgNPs) using dip-coating and drop-casting techniques. AgNPs were produced via green synthesis and incorporated onto the surface of Kraft paper samples. The modified samples were characterized using physicochemical techniques, including atomic force microscopy (AFM), Raman spectroscopy and light microscopy, as well as nanomechanical characterization via force spectroscopy. The antimicrobial activity of the modified papers was assessed using the disk diffusion method. The results demonstrated that the modification techniques resulted in distinct surface characteristics. Samples treated with the drop-casting method exhibited the highest AgNP surface loading; however, this was accompanied by pronounced surface heterogeneity and a tendency toward reduced load-bearing capacity. Overall, the findings indicate that the choice of deposition technique plays a key role in controlling nanoparticle distribution and surface properties. Within the limitations of the techniques evaluated, the incorporation of nanomaterials with potential antimicrobial activity into Kraft paper may offer opportunities for the development of active food packaging, although further optimization is required.

Poly(ethylene terephthalate) (PET) is a widely used commodity polymer owing to its low cost, excellent mechanical properties, and high processability. Chemical modification of PET surfaces to impart specific functionalities represents an effective strategy for transforming PET into high-value-added materials without altering its bulk properties. In this study, we investigated the surface functionalization of PET substrates using surface-initiated atom transfer radical polymerization (SI-ATRP). ATRP initiation sites were introduced onto PET surfaces through mild surface hydrolysis followed by polyethyleneimine coating. To further enhance the grafting density, an inimer-based strategy was employed, in which a bifunctional monomer containing both a polymerizable group and a latent initiation site was used to form hyperbranched polymer structures on the PET surface, thereby amplifying the number of active initiation sites. Using these modified PET substrates, SI-ATRP of functional methacrylate monomers was successfully carried out. Grafting of poly(2,2,2-trifluoroethyl methacrylate) imparted highly hydrophobic surface properties, yielding water contact angles above 120°, whereas grafting of poly([2-(methacryloyloxy)ethyl]trimethylammonium chloride) produced hydrophilic surfaces with contact angles below 20°. Surface characterization by X-ray photoelectron spectroscopy confirmed successful graft polymerization and effective surface coverage. While the macroscopic wettability was primarily governed by the chemical nature of the grafted polymers, the inimer-based initiation-site amplification significantly enhanced the surface electrostatic properties of the polycationic polymer–grafted surfaces, increasing the ζ-potential from approximately +20 mV to over +100 mV. Antibacterial tests using Escherichia coli K-12 as a model bacterium demonstrated that PET substrates grafted with poly([2-(methacryloyloxy)ethyl]trimethylammonium chloride) exhibited clear contact-active antibacterial activity, achieving up to 2-log reduction in viable bacterial counts after 3 h of contact incubation. These results highlight the importance of molecular-level control of grafting architecture and surface electrostatic properties in the design of functional antibacterial PET surfaces.

In this paper, we show that the sphere-in-contact model can predict long-range surface adsorption phenomena based on adsorbate-adsorbate repulsions and their geometric distance, assuming that their negative surface-induced charge is smeared on the surface of the adsorbate atoms. Additionally, it can be used to model collective surface diffusion mechanisms such as the domino-type surface diffusion of adsorbate rows on close-packed metal HCP and FCC surfaces. We have recently shown that the sphere-in-contact model can be used as an educational and research tool in various contexts, such as the visualization of carbon structures (e.g., graphene, carbon nanotubes, carbon nanocones, and graphite), heterogeneous catalysts, metal nanoparticles, and organic molecules. Here we present how it can be used to model the adsorbate structure of monoatomic elements on the hexagonal close-packed surface of HCP and FCC metals to study long-range ordering phenomena of monoatomic adsorbates on metals. We have used atoms of varying radius and color to represent the metal surface atoms and the adsorbate atoms. The study reveals that many surface configurations are possible for a fixed adsorbate coverage (θ) by the movement of the adsorbate atoms in response to surface adsorbate-adsorbate repulsions. The movement of the particles (e.g., particle diffusion) can be seen directly in the model, and this is caused by the user intervention. This has great educational and research value, as one can directly see how the adsorbate atoms reorder on the surface of a metal and therefore study diffusion mechanisms. We calculate the repulsive interaction energy of adsorbates using the sphere-in-contact model and can identify which surface-adsorbed configuration is the lowest energy. We find that at a surface coverage of 1/3 (0.333 ML), the most stable adsorbate configuration places adsorbates at the third nearest neighbor 3-fold hollow sites, forming a hexagonal pattern. We find that this model will be useful in the rational design of catalytic materials and material coatings with new technological applications where long-range ordering of surface adsorbates is essential and adsorbate interactions are mainly repulsive interatomic interactions.

Wheat bran (WB) is an abundant agro-industrial residue rich in starch and structural polysaccharides, representing an attractive feedstock for sustainable biorefinery applications. In this work, an integrated strategy combining mild hydrothermal extraction and catalytic hydrothermal conversion was proposed to promote sugar recovery from unmilled WB and its subsequent transformation into organic acids. Conventional (HE-CH) and microwave-assisted hydrothermal extraction (HE-MW) were compared at 80–100 °C and 5–30 min. Under these soft conditions, total sugar recoveries of up to 6.45 g/100 g WB (5 min) and 8.71 g/100 g WB (30 min) were achieved, with a clear predominance of bound sugars and preferential extraction of hemicellulosic (C5) fractions, without formation of degradation products. Microwave-assisted extraction enhanced sugar recovery and selectivity by improving access to the wheat bran cell wall through volumetric heating and enhanced mass transfer. The resulting liquid extracts were subsequently converted at 180 °C and 40 bar (N2) using a mesoporous hydrated ZrO2 catalyst. In the absence of a catalyst, the system exhibited autothermal behavior but low efficiency (X < 20%). In contrast, catalytic conversion led to total sugar conversions above 75% at 90 min, with high lactic acid yields and LA/GA ratios consistently above unity, particularly for HE-MW-derived extracts. Overall, this work demonstrates that coupling microwave-assisted extraction under mild conditions with heterogeneous catalysis enables efficient access to WB cell-wall carbohydrates and their selective upgrading into value-added organic acids, offering a low-severity and sustainable route for wheat bran valorization.

While advanced imaging techniques and ordered porous materials like MOFs have gained prominence, gas sorption remains the indispensable tool for characterizing the multiscale heterogeneity of industrially important disordered solids, such as catalysts and shales. This review examines recent developments in gas sorption methodologies specifically tailored for rigid, disordered porous media. We discuss experimental advances, including the choice of adsorbate and the utility of the overcondensation method for probing macroporosity and ensuring saturation. Furthermore, we critically evaluate theoretical approaches for determining pore size distributions (PSDs), contrasting classical methods with Density Functional Theory (DFT) and Grand Canonical Monte Carlo (GCMC) simulations. Special emphasis is placed on the impact of pore-to-pore cooperative effects, such as advanced condensation, cavitation, and pore-blocking, on the interpretation of sorption isotherms. We highlight how complementary techniques, including integrated mercury porosimetry, NMR, and computerized X-ray tomography (CXT), are essential for deconvolving these complex network effects and validating void space descriptors. We conclude that, while “brute force” molecular simulations on image-based reconstructions are progressing, “minimalist” pore network models, which incorporate cooperative mechanisms, currently offer the most empirically adequate approach. Ultimately, gas sorption remains unique in its ability to statistically characterize void spaces from Angstroms to millimeters in a single experiment.

Quaternary Ni-Zn-Mg-Al metallic mixed oxide (MMO) catalysts were synthesized by co-precipitation from layered double hydroxide precursors. The effect of varying Zn content on physicochemical properties and catalytic performance was evaluated. Mg-Al and ternary Ni-Mg-Al and Zn-Mg-Al catalysts were synthetized for comparative purposes. XRD, N2 sorption, MP-AES, CO2-TPD, NH3-TPD, SEM, and EDS characterized the materials’ physicochemical properties. The tested reaction was the transesterification between glycerol and dimethyl carbonate to obtain glycerol carbonate to improve the biodiesel industry. The catalyst containing both Ni and Zn showed the highest glycerol conversion among the evaluated materials. This was related to the increased number and strength of surface basic and acid active sites. Specifically, a high density of strong basic sites and acid ones in the quaternary catalysts was required for the reaction mechanism. The catalyst with 20 at% of Zn (MMO-Ni15Zn20) achieved the highest glycerol carbonate yield (89.6%) under mild reaction conditions and was solvent-free. MMO-Ni15Zn20 catalytic performance was associated with its high total basicity and predominance of strong basic sites and a moderate amount of acid sites. The differences observed between catalytic performances suggest that these results depend on the influence of structural, textural, acid, and basic properties. Reuse tests of the MMO-Ni15Zn20 catalyst showed moderate stability, with a progressive decrease in activity due to the loss of strong basic sites and the formation of agglomerated regions. Nevertheless, MMO-Ni15Zn20 maintained a GC selectivity of 100% in the successive cycles.

Dye-sensitized solar cells (DSSCs) are a promising alternative to traditional silicon-based technologies due to their low production costs, ease of fabrication, and wide range of applications. Among the semiconductors used in DSSCs, TiO2 stands out for its simple, inexpensive synthesis and lower environmental impact. However, TiO2 has limitations due to its wide bandgap and high charge-carrier recombination. In this study, the incorporation of rGO and its effect on the degree of GO reduction on Cu-doped TiO2 particles were evaluated to enhance light interaction, improve electronic mobility, and suppress recombination. Electrophoretic deposition was employed as an alternative method to obtain Cu-doped, rGO-decorated mesoporous TiO2 films, which were evaluated for power conversion efficiency (PCE) in DSSCs. The materials were characterized using SEM, ICP-OES, UV-Vis, XRD, BET, DLS, and TEM, while the photoanodes were analyzed using FTIR, chronoamperometry, and photovoltaic efficiency tests. The results showed clusters between 1.4 and 2.6 µm, confirming doping, a decrease in the energy gap to 2.99 eV, a stable anatase crystalline phase, and an increase in the specific surface area to 234.82 m2/g. The fabricated cells exhibited a PCE of 2.26% with a TiO2:Cu-rGO photoanode after 20 min of GO reduction, compared to 0.96% for DSSCs with a conventional configuration.