In this study, new synthetic approaches for the preparation of thin films of Mg-Al layered double hydroxides (LDHs) have been developed. The LDHs were fabricated by reconstruction of mixed-metal oxides (MMOs) in deionized water. The MMOs were obtained by calcination of the precursor gels. Thin films of sol–gel-derived Mg-Al LDHs were deposited on silicon and stainless-steel substrates using the dip-coating technique by a single dipping process, and the deposited film was dried before the new layer was added. Each layer in the preparation of the Mg-Al LDH multilayers was separately annealed at 70 °C or 300 °C in air. Fabricated Mg-Al LDH coatings were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), and atomic force microscopy (AFM). It was discovered that the diffraction lines of Mg₃Al LDH thin films are sharper and more intensive in the sample obtained on the silicon substrate, confirming a higher crystallinity of synthesized Mg₃Al LDH. However, in both cases the single-phase crystalline Mg-Al LDHs have formed. To enhance the sol–gel processing, the viscosity of the precursor gel was increased by adding polyvinyl alcohol (PVA) solution. The LDH coatings could be used to protect different substrates from corrosion, as catalyst supports, and as drug-delivery systems in medicine.

Porous 3D Cu layers with the following average parameters: thickness ~35 µm, pore density ~4.0 × 10⁶ cm⁻², and pore sizes ~25 µm were electrodeposited from an acidic sulphate electrolyte, and the suitability of different electrochemically active surface area determination methods for characterising these electrodes was assessed. Structural characterisation of the samples was conducted using SEM and an optical profiler, while electrochemical measurements were performed using cyclic voltammetry and electrochemical impedance spectroscopy. The evaluation of electrochemically active surface area involved the underpotential deposition of Tl and Pb monolayers as well as double-layer capacitance measurements. The results obtained indicate that both methods yield similar results for non-porous Cu electrodes. However, for Cu 3D nanostructures, the evaluation mode significantly influences the results. Double-layer capacitance measurements show significantly higher values for the electrochemically active surface area compared to the underpotential deposition (UPD) technique. The complex spatial structure of the Cu 3D layer hinders the formation of a continuous monolayer during the UPD process, which is the principal reason for the observed differences.

Sol-gel derived calcium hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂; CHA) thin films were deposited on stainless steel substrates with transverse and longitudinal patterned roughness employing a spin-coating technique. Each layer in the preparation of CHA multilayers was separately annealed at 850 °C in air. Fabricated CHA coatings were placed in simulated body fluid (SBF) for 2, 3, and 4 weeks and investigated after withdrawal. For the evaluation of obtained and treated with SBF coatings, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), X-ray diffraction (XRD) analysis, Raman spectroscopy, XPS spectroscopy, scanning electron microscopy (SEM) analysis, and contact angle measurements were used. The tribological properties of the CHA coatings were also investigated in this study.

Environmentally friendly alternatives to chromium—phosphate/molybdate and cerium-modified phosphate/molybdate conversion coatings—were deposited on a carbon steel surface. Different surface analytic techniques were applied to obtain complementary information on the composition, element distribution morphology and inner structure of the coatings in order to establish the relationship between coating properties and corrosion performance. The higher protective and stronger self-healing abilities were found for phosphate/molybdate/cerium conversion coating deposited in a sulphate-containing solution. The protective barrier strength was found to be related with certain aspects of the coating morphology such like homogeneous distribution of fine crystallites and, hence, lower number of structural defects. The self-healing ability depended on both, the composition (higher amount of Ce(IV)) and micro-structural characteristics, such as defectiveness, of the conversion layer.

We present a crack-free optically active SiO₂ glass-composite material containing YAG:Ce synthesized via a modified sol–gel technique. A glass-composite material consisting of yttrium aluminum garnet doped with Ce³⁺ (YAG:Ce) was entrapped into a SiO₂ xerogel. This composite material was prepared using a sol–gel technique with modified gelation and a drying process to obtain crack-free optically active SiO₂ glass. The concentration of the YAG:Ce was from 0.5 to 2.0 wt%. All synthesized samples were characterized via X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, confirming their exceptional quality and structural integrity. The luminescence properties of the obtained materials were studied. Overall, the prepared samples’ excellent structural and optical quality makes them great candidates for further investigation, or even potential practical application. Furthermore, boron-doped YAG:Ce glass was synthesized for the first time.

Porous Cu foam electrodes, suitable for cathodic CO2 reduction, were deposited in an acidic sulphate solution with different additives to obtain structures with a high real surface area and an adequate mechanical stability. The influence of the electrodeposition time and solution composition on the porosity parameters, microstructure and stiffness of Cu 3D structures was evaluated. Neither ammonium acetate nor polyethylene glycol were found to be effective additives to the Cu sulphate electrolyte to achieve the main objectives. Only the presence of Cl– ions in the deposition solution resulted in a threefold increase in the real surface area and the achievement of a sufficient mechanical stability of the Cu 3D structure. The latter effect is related to the specific influence of Cl– ions during the electrodeposition process on the microstructural characteristics, such as the size of micropores in the walls of holes and crystallite aggregates that form dendritic branches. These structural changes, in contrast to the Cu samples deposited in a solution without additives, resulted in larger real surface areas, while the denser structures deposited in the presence of Cl– ions ensured the mechanical stability of the 3D structure.