Publications

A testing methodology and a new "anchor"geometry for tensile samples were developed for evaluation of the W/Cu joint strength between the W monoblock and the CuCrZr cooling pipe joined via the Cu interlayer in the ITER-specification monoblock. The proposed samples can be machined from the ITER-specification monoblock. These monoblock tensile samples are designed for uniaxial tests allowing their remote manipulation for testing in hot cells after neutron irradiation, which is crucial for the assessment of the effect of this irradiation. For validation purposes, tensile tests with standard miniaturised dog-bone samples were performed using prototype block-to-block joints (W/CuCrZr) produced with the field-assisted sintering technique. The results are obtained from the conventional and the new tensile samples. Conventional samples were machined from the W/CuCrZr block-to-block joints, while the new "anchor"tensile samples were machined from the W/CuCrZr block-toblock joints and ITER monoblock containing the W block and Cu interlayer. A good agreement in the evaluation of the joint strength was obtained. The fracture surfaces and the joint interface were investigated with scanning electron microscopy. Micro-hardness was characterised across the joint interface.

We report a novel approach in producing and characterizing enriched isotopic selenium-82 (82Se) thin films with trigonal hexagonal crystal structure (t-82Se), the most thermodynamically stable form of the element. The ob-tained t-82Se thin films are used as targets in accelerator based nuclear structure experiments. Several 82Se thin films with thicknesses around 5 mg/cm2 (10.4 & mu;m) were deposited on 5 mg/cm2 (3 & mu;m) tantalum (Ta) foils by vacuum evaporation-condensation method. The condensed 82Se films exhibit unstable amorphous structure (a-82Se), therefore were converted to t-82Se by means of an appropriate vacuum heat treatment developed in the target laboratory of IFIN-HH. After the thermal treatment, the microstructure, morphology and composition of the 82Se films were evaluated before and after the vacuum thermal treatment using Fourier Transform Raman Spectroscopy (FT-Raman), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM), Scanning Electron Mi-croscopy (SEM) and Energy-Dispersive X-Ray Spectroscopy (EDX) techniques. Furthermore, an in-beam & gamma;-spectroscopy experiment performed at the 9-MV tandem accelerator of IFIN-HH confirmed that the ther-mally treated t-82Se films possess high durability and high purity with no detectable contamination and no mass loss.

Motivated by the goal of developing ultralow power, smart and multifunctional nano (micro) electronic devices, research has shown unwavering interest in synthesis methods, architectures and interphase connectivity of composites containing magnetostrictive and piezoelectric phases, known as magnetoelectric (ME) materials. Herein we report on CoFe2O4/0.92Bi0.5Na0.5TiO3-0.08BaTiO3 biphasic ME composites, obtained by sol-gel chemistry, by mixing the precursor sols of the two phases into one precursor sol and further transforming it into gel, with the goal of obtaining homogeneous nanocomposites with magnetoelectric properties. The structural properties, the temperature dependance of dielectric properties, the magnetic and magnetoelectric properties of these biphasic mixtures, with various molar ratios CoFe2O4/ BNT-BT0.08 = 0.5:1, 1:1 and 1.5:1, are investigated. It is observed that the amount of CoFe2O4 and the synthesis in situ of these composites influences their macroscopic properties showing a high difficulty of carrying out an efficient poling resulting in small piezoelectric and magnetoelectric response. It was concluded that the synthesis procedure, the type of architecture and the interphase connectivity are of outmost importance for magnetoelectric properties based on lead-free materials. (c) 2023 Published by Elsevier B.V.

Probing of the free surface ferroelectric properties of thin polar films can be achieved either by estimating the band bending variance under the top-most layer or by studying the extent of the extrinsic charge accumulated outside the surface. Photoemitted or incoming low-energy electrons can be used to characterize locally both properties in a spectromicroscopic approach. Thin ferroelectric lead zirco-titanate (PZT) is investigated by combining low energy/mirror electron microscopy (LEEM/MEM) with photoemission electron microscopy (PEEM) and high-resolution photoelectron spectroscopy (XPS). Significant extrinsic negative compensation charge is proven to accumulate on the surface of the outward polarized thin film, indicated by high MEM-LEEM transition values, up to 15.3 eV, and is correlated with the surface electrostatic potential, which can be partially screened either by electrons interacting with the sample or by soft X-rays through the ejection of secondary electrons and generation of positive charge under the surface. A radiation-induced surface charge compensation effect is observed. The study indicates that air-exposed high quality ferroelectric thin films show large negative surface potentials, determined locally on the surface, which are nevertheless sensitive to beam damage and molecular desorption. These values represent a confirmation of previously estimated surface potential energy values determined from the LEED data on clean surfaces.

Properties of surface species of the nematic mixture E7 in contact with inorganic oxides (especially those containing more or less aluminium ions) are in detail investigated by infrared spectroscopy and thermogravimetry. The absorption infrared peaks were decomposed into Gaussian components, the procedure allowing an easier comparison with the behaviour of related composites. We worked at enough small concentrations of the E7 relatively to support this ratio permitting the (partial) elimination of the species belonging to the bulk. Species put here in evidence are species that are hydrogen bonded to the surface of OH groups, molecules randomly oriented on the surface, some species bonded by involvement of pi electrons of the CN group to the aluminium ions, thus implying a strong interaction to the support. Supramolecular assemblies of E7 molecules are thus followed up.

[Cu(acac)(phen)(H2O)](ClO4) and [Cu(acac)(bipy)(H2O)](ClO4) catalysts were prepared by the immobilization of mixed-ligand complexes on graphene oxide derivatized with monochloroacetic acid. These catalysts were characterized through an ensemble of techniques including XRD, FTIR, Raman, and XPS while the catalytic behavior has been investigated in the oxidation of cyclohexene, 1-octene and glycerol in the presence of molecular oxygen. Cyclohexanone was the dominant product in the oxidation of cyclohexene resulting in selectivities higher than 50% for a conversion of 14.5%. The turnover frequencies were pretty high, namely, 4.5 h(-1) for [Cu(acac)(phen)(H2O)](ClO4) and 2.3 h(-1) for Cu(acac)(bipy)(H2O)](ClO4). The oxidation of 1-octene also occurred with a pretty high selectivity in 2-octanol as the main product. The role of copper in the oxidative dehydrogenation of glyceric acid towards tartronic acid was as well confirmed. Noteworthy, these catalysts were stable and their recycling occurred with no change in the conversion or selectivity.

High-power density applications using up-conversion (UC) systems rely mostly on the Yb, Tm lanthanide couple. Herein, we investigate the extent to which Gd high energy levels can enhance the four-order UC process in NaGdF4:Yb, Er under pulsed excitation, making the Yb, Er UC system suitable for high power density applications. Unlike cw excitation, pulsed laser excitation enables higher equivalent power densities with reduced local heating effects. We found that Gd upholds the saturation level by one order of magnitude in NaGdF4:Yb, Er@NaYF4 compared to NaYF4:Yb, Er@NaYF4 nanoparticles, i.e., from 5 x 10(6) to 5 x 10(7) W cm(-2). Such an effect is determined by efficient two-step Er-Gd energy transfer, in which the Gd levels, populated by four-order Yb-Er processes, act further as the long(est)-lived reservoir level for Er UC emissions. Notably, above 10(8) W cm(-2), NaGdF4:Yb, Er@NaYF4 shows similar performance to NaGdF4:Yb, Tm@NaYF4 in terms of UC photon order, which is considered a direct indicator of spatial resolution in high power density applications. Our results showcase the promise of the Yb, (Gd) Er UC system for high power density applications, thus stimulating research for expanding the presently limited range of applicable UC systems.

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(x)Co(1-x)Al), in the presence of a supplementary amount of water, and light green powders (PZnxCo1-xAl), respectively, for the water-free procedure (x = 0, 0.2, 0.4). The calcination of the precursors yielded dark green (wZn(x)Co(1-x)Al) and blue (ZnxCo1-xAl) products. XRD measurements and Rietveld refinement indicate the co-existence of three spinel phases, in different proportions: ZnxCo1-xAl2O4, Co3O4 and the defect spinel, ?-Al2.67O4. The Raman scattering and XPS spectra are in agreement with the compositions of the samples. The morphology of wZn(x)Co(1-x)Al 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 ZnxCo1-xAl. TEM and HR-TEM analyses revealed the formation of crystalline, polyhedral particles of 7-43 nm sizes for wZn(x)Co(1-x)Al, while for ZnxCo1-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.

Microemulsions are nanocolloidal systems composed of water, an oil, and a surfactant, sometimes with an additional co-surfactant, which have found a wide range of practical applications, including the extractive removal of contaminants from polluted water. In this study, microemulsion systems, including a nonionic surfactant (Brij 30), water, and esters selected from two homologous series of C-1-C-6 alkyl acetates and ethyl C-1-C-4 carboxylates, respectively, were prepared by the surfactant titration method. Phase transitions leading to the formation of Winsor II and Winsor IV microemulsions were observed and phase diagrams were constructed. The dependences of phase transitions on the salinity and pH and the addition of isopropanol as a co-surfactant were also investigated. Some physical properties, namely density, refractive index, electrical conductivity, dynamic viscosity, and particle size, were measured for a selection of Winsor IV microemulsions, providing further insight into some other phase transitions occurring in the monophasic domains of phase diagrams. Finally, Winsor II microemulsions were tested as extraction solvents for the removal of four tricyclic antidepressant drugs from aqueous media. Propyl acetate/Brij 30/H2O microemulsions provided the best extraction yields (>90%), the highest Nernst distribution coefficients (similar to 40-88), and a large volumetric ratio of almost 3 between the recovered purified water and the resulting microemulsion extract. Increasing the ionic strength (salinity) or the pH of the aqueous antidepressant solutions led to an improvement in extraction efficiencies, approaching 100%. These results could be extrapolated to other classes of pharmaceutical contaminants and suggest ester- and nonionic surfactant-based microemulsions are a promising tool for environmental remediation.