Adelina-Carmen Ianculescu

A novel high-entropy perovskite powder with the composition Bi_0.2K_0.2Ba_0.2Sr_0.2Ca_0.2TiO₃ was successfully synthesized using a modified Pechini method. The precursor powder underwent characterization through Fourier Transform Infrared Spectroscopy and thermal analysis. The resultant Bi_0.2K_0.2Ba_0.2Sr_0.2Ca_0.2TiO₃ powder, obtained post-calcination at 900 °C, was further examined using a variety of techniques including X-ray diffraction, Raman spectroscopy, X-ray fluorescence, scanning electron microscopy, and transmission electron microscopy. Ceramic samples were fabricated by conventional sintering at various temperatures (900, 950, and 1000 °C). The structure, microstructure, and dielectric properties of these ceramics were subsequently analyzed and discussed. The ceramics exhibited a two-phase composition comprising cubic and tetragonal perovskites. The grain size was observed to increase from 35 to 50 nm, contingent on the sintering temperature. All ceramic samples demonstrated relaxor behavior with a dielectric maximum that became more flattened and shifted towards lower temperatures as the grain size decreased.

Magnesium oxide (MgO) was synthesized by three different methods: the sol–gel (SG), microwave-assisted sol–gel (MW), and hydrothermal (HT) methods for comparing the influence of the preparation conditions on the properties of the products. The powders were annealed at 450 °C. The samples were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM/HRTEM), selected area electron diffraction (SAED), energy-dispersive X-ray spectroscopy (EDX), BET specific surface area and porosity, photoluminescence, and UV–Vis spectroscopy. The samples consisted mainly of periclase as a crystalline phase, and the MW and HT preparation methods generated particles with higher specific surface areas. The powders had less-defined morphologies and high levels of aggregation. The optical band gaps of the samples were determined from UV DRS, and the photocatalytic activities of the magnesium oxides obtained by the three methods towards the degradation of methyl orange (MO) under UV light irradiation was evaluated.

Two new families of zinc/cobalt/aluminum-based pigments, with a unique composition, were obtained through the polyol method. The hydrolysis process of a mixture of Co(CH₃COO)₂, Zn(acac)₂ and Al(acac)₃ (acac⁻ = acetylacetonate ion) in 1,4-butanediol afforded dark blue gels (wPZn_xCo_1−xAl), in the presence of a supplementary amount of water, and light green powders (PZn_xCo_1−xAl), respectively, for the water-free procedure (x = 0, 0.2, 0.4). The calcination of the precursors yielded dark green (wZn_xCo_1−xAl) and blue (Zn_xCo_1−xAl) products. XRD measurements and Rietveld refinement indicate the co-existence of three spinel phases, in different proportions: Zn_xCo_1−xAl₂O₄, Co₃O₄ and the defect spinel, γ-Al_2.67O₄. The Raman scattering and XPS spectra are in agreement with the compositions of the samples. The morphology of wZn_xCo_1−xAl consists of large and irregular spherical particle aggregates (ca. 5–100 mm). Smaller agglomerates (ca. 1–5 mm) with a unique silkworm cocoon-like hierarchical morphology composed of cobalt aluminate cores covered with flake-like alumina shells are formed for Zn_xCo_1−xAl. TEM and HR-TEM analyses revealed the formation of crystalline, polyhedral particles of 7–43 nm sizes for wZn_xCo_1−xAl, while for Zn_xCo_1−xAl, a duplex-type morphology, with small (7–13 nm) and larger (30–40 nm) particles, was found. BET assessment showed that both series of oxides are mesoporous materials, with different pore structures, with the water-free samples exhibiting the largest surface areas due, most likely, to the high percent of aluminum oxide. A chemical mechanism is proposed to highlight the role of the water amount and the nature of the starting compounds in the hydrolysis reaction products and, further, in the morpho-structural features and composition of the resulting spinel oxides. The CIE L*a*b* and C* colorimetric parameters indicate that the pigments are bright, with a moderate degree of luminosity, presenting an outstanding high blueness.

Using the microwave-assisted sol–gel method, Zn- and Cu-doped TiO₂ nanoparticles with an anatase crystalline structure were prepared. Titanium (IV) butoxide was used as a TiO₂ precursor, with parental alcohol as a solvent and ammonia water as a catalyst. Based on the TG/DTA results, the powders were thermally treated at 500 °C. XRD and XRF revealed the presence of a single-phase anatase and dopants in the thermally treated nanoparticles. The surface of the nanoparticles and the oxidation states of the elements were studied using XPS, which confirmed the presence of Ti, O, Zn, and Cu. The photocatalytic activity of the doped TiO₂ nanopowders was tested for the degradation of methyl-orange (MO) dye. The results indicate that Cu doping increases the photoactivity of TiO₂ in the visible-light range by narrowing the band-gap energy.

The tin-doped TiO₂ powders obtained by sol-gel and microwave-assisted sol-gel methods were investigated. The synthesis took place in a basic medium (pH 10, ammonium hydroxide, 25%) starting from tetrabutyl orthotitanate in its parental alcohol. In the case of the dopant, Tin(II) 2-ethylhexanoate as SnO₂ precursor was used in the amount of 1, 2, or 4 mol % SnO₂. Based on thermal analysis data, the powders were thermally treated in air, at 500 °C. The comparative investigation of the structure and morphology of the nanopowders annealed at 500 °C was performed by scanning electron microscopy (SEM), high-resolution transmission electron microscopy with selected area electron diffraction (HRTEM/SAED), scanning transmission electron microscopy (STEM) coupled with EDX mapping, Fourier transmission infrared (FTIR), UV–Vis, Raman and photoluminescence (PL) spectroscopy, X-ray diffraction (XRD), and X-ray florescence spectroscopy (XRF). The obtained materials were tested for the photocatalytic removal of methyl orange dye from aqueous solutions. High degradation efficiencies (around 90%) were obtained by Sn doping after 3 h of UV light irradiation.

The use of Fe films as multi-element targets in space radiation experiments with high-intensity ultrashort laser pulses requires a surface structure that can enhance the laser energy absorption on target, as well as a low concentration and uniform distribution of light element contaminants within the films. In this paper, (110) preferred orientation nanocrystalline Fe thin films with controlled morphology and composition were grown on (100)-oriented Si substrates by oblique angle RF magnetron sputtering, at room temperature. The evolution of films key-parameters, crucial for space-like radiation experiments with organic material, such as nanostructure, morphology, topography, and elemental composition with varying RF source power, deposition pressure, and target to substrate distance is thoroughly discussed. A selection of complementary techniques was used in order to better understand this interdependence, namely X-ray Diffraction, Atomic Force Microscopy, Scanning and Transmission Electron Microscopy, Energy Dispersive X-ray Spectroscopy and Non-Rutherford Backscattering Spectroscopy. The films featured a nanocrystalline, tilted nanocolumn structure, with crystallite size in the (110)-growth direction in the 15–25 nm range, average island size in the 20–50 nm range, and the degree of polycrystallinity determined mainly by the shortest target-to-substrate distance (10 cm) and highest deposition pressure (10⁻² mbar Ar). Oxygen concentration (as impurity) into the bulk of the films as low as 1 at. %, with uniform depth distribution, was achieved for the lowest deposition pressures of (1–3) × 10⁻³ mbar Ar, combined with highest used values for the RF source power of 125–150 W. The results show that the growth process of the Fe thin film is strongly dependent mainly on the deposition pressure, with the film morphology influenced by nucleation and growth kinetics. Due to better control of film topography and uniform distribution of oxygen, such films can be successfully used as free-standing targets for high repetition rate experiments with high power lasers to produce Fe ion beams with a broad energy spectrum.