National Institute Of Materials Physics - Romania

Magnetic ceramic nanoparticles system xNd(2)O(3)-(1-x)alpha-Fe2O3 (x = 0.1, 0.3 and 0.5) was synthesized by mechanochemical activation starting from hematite and neodymium oxide precursors and characterized by X-ray diffraction (XRD) and Mossbauer spectroscopy. Rietveld refinement of XRD data evidenced the formation of neodymium orthoferrite NdFeO3 as an end-product with a particle size of about 22 nm, determined using the Scherrer method for x = 0.5. The Mossbauer spectra were typically analyzed considering 2 sextets, corresponding to hematite and neodymium orthoferrite and a doublet, representing superparamagnetic particles (SPM). The recoilless fractions were determined using our dual absorber method and were found consistent with a decrease in particle size as consequence of the ball milling process performed.

Detailed tests and analysis of ageing effects of high irradiation dose on Multi-Strip Multi-Gap Resistive Plate Counters (MSMGRPC) based on low resistivity glass electrodes, foreseen to be used for the most forward polar angles covered by the Time-of Flight (ToF) sub-detector of the Compressed Baryonic Matter (CBM) experiment at Facility for Antiprotons and Ion Research (FAIR) - Darmstadt are reported. The tests were performed at a multi-purpose irradiation facility of IFIN-HH based on Co-60 source. MSMGRPC efficiency, cluster size, surface and volume resistivity of the glass electrodes after irradiation are measured and compared with their values before irradiation. The results of a comprehensive analysis of the composition and properties of the deposited layers on the glass electrodes, based on different methods, i.e. Scanning Electron Microscope (SEM), X-ray Photoelectron Spectroscopy (XPS), foil Elastic Recoil Detection Analysis (ERDA), Rutherford Backscattering Spectrometry (RBS), Atomic Force Microscopy (AFM) and Terahertz Time Domain Spectroscopy (THz-TDS), are presented.

In an attempt to increase the biological activity of the 1,2,4-triazolo[1,5-a]pyrimidine scaffold through complexation with essential metal ions, the complexes trans-[Cu(mptp)(2)Cl-2] (1), [Zn(mptp)Cl-2(DMSO)] (2) (mptp: 5-methyl-7-phenyl-1,2,4-triazolo[1,5-a]pyrimidine), [Cu-2(dmtp)(4)Cl-4]center dot 2H(2)O (3) and [Zn(dmtp)(2)Cl-2] (4) (dmtp: 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine), were synthesized and characterized as new antiproliferative and antimicrobial species. Both complexes (1) and (2) crystallize in the P2(1)/n monoclinic space group, with the tetrahedral surroundings generating a square-planar stereochemistry in the Cu(II) complex and a tetrahedral stereochemistry in the Zn(II) species. The mononuclear units are interconnected in a supramolecular network through pi-pi interactions between the pyrimidine moiety and the phenyl ring in (1) while supramolecular chains resulting from C-H center dot center dot center dot pi interactions were observed in (2). All complexes exhibit an antiproliferative effect against B16 tumor cells and improved antibacterial and antifungal activities compared to the free ligands. Complex (3) displays the best antimicrobial activity against all four tested strains, both in the planktonic and biofilm-embedded states, which can be correlated to its stronger DNA-binding and nuclease-activity traits.

Recently, a simple model was proposed for the microscopic energy associated to the ferroelectric phase, to be used in a statistical approach in order to derive the equations of state for a ferroelectric thin film [C. M. Teodorescu, Phys. Chem. Chem. Phys., 2021, 23, 4085-4093]. The stabilization energy for an elemental dipole in a polar thin film is the result of the interaction of this dipole with the field generated by charges accumulated at surfaces or interfaces of the thin film. An essential parameter of this interaction is the permittivity of the film, assumed to be a material constant, together with the maximum value of an elemental dipole and the density of the elemental dipoles. These can be connected to three experimental parameters which are the saturation polarization P-s, the coercive field at zero temperature E-c((0)) and the Curie temperature T-C. However, for a ferroelectric material both the global and the differential permittivity depend on the temperature and on the polarization. This raises the question whether such a non-constant permittivity should be used in the stabilization energy of the ferroelectric phase, and whether it can be identified self-consistently with the function resulting after applying the statistics based on the microscopic model. In such case, a mutual interdependence should exist between P-s, E-c((0)) and T-C. A model is built up, able to predict coercitivity, however E-c((0)) and T-C yield values several orders of magnitude higher than the experimental ones. Therefore, one has to introduce a background dielectric constant of several hundreds to accommodate the result of the model with the experimental data. The poling history of the film has to be taken into account, together with the presence of a small bias field. The model is able to predict self-consistently the equation of state of a ferroelectric, and in particular the linear decrease of the coercive field with temperature. The microscopic parameters, in particular the background dielectric constant and the density of elemental dipoles may be expressed directly from experimental quantities.

The physico-chemical properties of two anhydrous AZA forms and their interaction with typical pharmaceutical excipients were assessed by applying various methods (such as PXRD, HPLC, TG/DSC, IR, Raman, PL or UV-Vis) in order to highlight new directions for drug formulation. The stability assessment of AZA anhydrous forms I and II was performed in order to determine the risk of degradation of the active ingredient by accidental exposure to nonstandard conditions in the industrial environment, under different storage, transport or processing conditions. The benefits of form II include increased resistance to chemical degradation over a wide range of pH, but further control of storage and processing conditions is necessary to avoid polymorphic transformation into form I. The solubility assessment on the AZA solid forms in different environments that simulate the conditions of the gastrointestinal tract has the advantage of a significantly increased solubility of form II compared with the commercial form I due to the modification of the crystalline structure. In the case of capsules compared to AZA form I or II as powder, an improvement in their solubility was observed, promoted by the presence of one or more excipients in the formulation mixture.

Zr0.8Sn0.2TiO3 (ZST) powders synthesized by solid-state reaction were subject to processing by spark plasma sintering (SPS). A single-phase ceramic with a high relative density of 95.7% and 99.6% was obtained for sintering temperatures of 1150 degrees C and 1200 degrees C, respectively, and for a dwell time of 3 min. In order to reduce the oxygen vacancies, as-sintered discs were annealed in air at 1000 degrees C. The dielectric loss of the annealed samples, expressed by the Q x f product, measured in the microwave (MW) domain, varied between 35 THz and 50 THz. The intrinsic losses (Q x f ~ 60 THz) were derived by using terahertz time-domain spectroscopy (THz-TDS).

Luminescent nanocrystals embedded into silica microspheres were shown to be useful for silica labeling for biological applications, ensuring mechanical and chemical stability, nontoxicity, biocompatibility and optical properties. We used sol-gel technology to prepare silica nanospheres embedded with fluorescent and magnetic Eu3+(1 mol%)-doped CeO2 nanocrystals. The X-ray diffraction pattern analysis and transmission electron microscopy investigations showed CeO2:Eu3+(1 mol%) nanocrystals of about 9 nm size and Ce3+ ions substitution by the Eu3+ ions; the nanocrystals dispersed inside the nanosized silica spheres of about 400 nm diameters. The photoluminescence spectra recorded under UV-light excitation showed Eu3+ ions luminescence peaks (D-5(0)-F-7(J), J = 0-4) accompanied by a weaker 425 nm luminescence due to the silica matrix; the quantum yield was 0.14. The weak hysteresis loop and magnetization curves recorded up to 20,000 Oe showed dominantly paramagnetic behavior associated with the silica matrix; a slight opening of the hysteresis loop to a very small magnetic field (about 0.005 Oe) was due to the presence of the two rare earth ions. The photonic crystal properties of SiO2-CeO2:Eu3+(1 mol%) silica nanospheres deposited as films on quartz plates were revealed by the two weak attenuation peaks at 420 and 500 nm and were associated with the reflection from different planes. The SiO2-CeO2:Eu3+(1 mol%) nanospheres are attractive potential candidates for photonics-related applications or for multifunctional bio-labels by combining the luminescence and magnetic properties of the nanocrystals.

Small multilayered laminated samples consisting of stacks of W (or K-doped W) foils without an interlayer or with interlayers from Cu, V, and Ti were exposed to a pulsed electron beam with an energy of 6 MeV in several irradiation sessions. All samples maintained their macroscopic integrity, suggesting that the W-metal laminate concept is compatible with high heat flux applications. The surface of the samples was analyzed using a scanning electron microscope (SEM) before and after each irradiation session. The experimental results indicate that electron beam irradiation induces obvious modifications on the surface of the samples. Morphological changes such as the appearance of nanodroplets, nanostructures, and melting and cracking, depending on the sample type and the electron beam fluence, are observed. The irradiation is carried out in a vacuum at a pressure of 2 to 4 x 10(-2) torr, without active cooling for the samples. The structures observed on the surface of the samples are likely due to electron beam heating and vaporization followed by vapor condensation in the volume adjacent to the surface.

Ag/Ga were incorporated into resorbable orthopaedic phosphate bioactive glasses (PBG, containing P, Ca, Mg, Na, and Fe) thin films to demonstrate their potential to limit growth of Staphylococcus aureus and Escherichia coli in post-operative prosthetic implantation. Dual target consecutive co-sputtering was uniquely employed to produce a 46 nm Ag:PBG composite observed by high resolution TEM to consist of uniformly dispersed similar to 5 nm metallic Ag nano-particles in a glass matrix. Ga3+ was integrated into a phosphate glass preform target which was magnetron sputtered to film thicknesses of similar to 400 or 1400 nm. All coatings exhibited high surface energy of 75.4-77.3 mN/m, attributed to the presence of hydrolytic P-O-P structural surface bonds. Degradation profiles obtained in deionized water, nutrient broth and cell culture medium showed varying ion release profiles, whereby Ga release was measured in 1400 nm coating by ICP-MS to be similar to 6, 27, and 4 ppm respectively, fully dissolving by 24 h. Solubility of Ag nanoparticles was only observed in nutrient broth (similar to 9 ppm by 24 h). Quantification of colony forming units after 24 h showed encouraging antibacterial efficacy towards both S. aureus (4-log reduction for Ag:PBG and 6-log reduction for Ga-PBG approximate to 1400 nm) and E. coli (5-log reduction for all physical vapour deposited layers) strains. Human Hs27 fibroblast and mesenchymal stem cell line in vitro tests indicated good cytocompatibility for all sputtered layers, with a marginal cell proliferation inertia in the case of the Ag:PBG composite thin film. The study therefore highlights the (i) significant manufacturing development via the controlled inclusion of metallic nanoparticles into a PBG glass matrix by dual consecutive target co-sputtering and (ii) potential of PBG resorbable thin-film structures to incorporate and release cytocompatible/antibacterial oxides. Both architectures showed prospective bio-functional performance for a future generation of endo-osseous implant-type coatings.

The As2S3-Cu interface was studied by dielectric spectroscopy measurements on Cu-As2S3-Cu thin film heterostructure samples to assess the charge carriers' contribution to the electrical properties of such an interface. Three-dimensional printed masks ensured good reproducibility during the PLD deposition of heterostructure samples. The samples were tested for electrical conductivity and AC photoconductivity by dielectric spectroscopy measurements. DC bias voltages and light were applied to the samples. The electrical capacity of the thin film heterostructure can be modified electrically and optically. We observed long-term photoconductivity with a time dependency that was not exponential, and a quick change of the electrical capacity, indicating the potential of the heterostructure cells as photodetector candidates.