National Institute Of Materials Physics - Romania

Y-modified LDHs with atomic Mg2+/(Al3+ + Y3+) of 3 and Al3+/Y3+ ratios of 0.5, 1 and 1.5 were prepared following two preparation methods, i.e. the co-precipitation and mechano-chemical one. The substitution of Al by Y in the brucite-type layer was less effective for the samples prepared by co-precipitation compared to those prepared via mechano-chemical route. In spite the fact yttrium has a larger ionic radius (0.9 angstrom) the structural characterizations of these solids confirmed that the layered structure incorporates part of it in the octahedral positions. Further, the reconstruction of the layered structure after an exposure to water for 1 h was more effective for the solid prepared by co-precipitation. The yttrium modified LDHs showed better catalytic activities for cyclohexene oxidation to the corresponding epoxide than the un-modified LDH sample. Then, mixed oxides derived from yttrium-LDH showed very high conversions and selectivities for the synthesis of chalcone.

In this work, a complementary ultraviolet-visible (UV-VIS) spectroscopy and photoluminescence (PL) study on melatonin (MEL) hydrolysis in the presence of alkaline aqueous solutions and the photodegradation of MEL is reported. The UV-VIS spectrum of MEL is characterized by an absorption band with a peak at 278 nm. This peak shifts to 272 nm simultaneously with an increase in the band absorbance at 329 nm in the presence of an NaOH solution. The isosbestic point localized at 308 nm indicates the generation of some chemical compounds in addition to MEL and NaOH. The MEL PL spectrum is characterized by a band at 365 nm. There is a gradual decrease in the MEL PL intensity as the alkaline solution concentration added at the drug solution is increased. In the case of the MEL samples interacting with an alkaline solution, a new photoluminescence excitation (PLE) band at 335 nm appears when the exposure time to UV light reaches 310 min. A down-shift in the MEL PLE band, from 321 to 311 nm, as a consequence of the presence of excipients, is also shown. These changes are explained in reference to the MEL hydrolytic products.

In this paper, we investigate the origin of point defects revealed by electron spin resonance (ESR) and photoluminescence (PL) emission in correlation with the photocatalytic activity of ZnO nanocrystals subjected to thermal annealing at various temperatures. Two ESR signals at g similar to 1.96 and similar to 2.003 were consistently observed in all annealed ZnO samples. However, their relative intensities have changed, indicating that the point defect densities were influenced by the annealing temperature. Interestingly, when doping nanoZnO with Cr3+, the Q-band ESR measurements at T = 100 K did show that the g similar to 1.96 signal was completely passivated, suggesting that the origin of the signal lies in the electrons located near the conduction band, i.e. at a shallow-donor level. The intensity of the g similar to 2.003 signal decreased by rising the annealing temperature, and this is attributed to the depopulation of zinc interstitials through the thermally induced migration process and/or recombination with the zinc vacancies. The green PL emission line at similar to 520 nm, which is dominant in the 700 degrees C annealed ZnO sample, shows a correlation with the ESR signal at g similar to 1.96, whose origin is attributed to the radiative transition of the electron from the shallow donor level to the singly ionized zinc vacancy. Furthermore, the high density of the shallow donor electron states was found to be primarily responsible for the high photocatalytic activity in the degradation of methylene blue.

This work investigates the structural, magnetic and magneto-optical properties of a new zinc phosphate-tellurite glass belonging to the 45ZnO-10Al(2)O(3)-40P(2)O(5)-5TeO(2)system. The glass was prepared by a wet method of processing the starting reagents followed by suitable melting-stirring-quenching-annealing steps. Specific parameters such as density, average molecular mass, molar volume, oxygen packaging density, refractive index, molar refractivity, electronic polarizability, reflection loss, optical transmission, band gap and optical basicity have been reported together with thermal, magnetic and magneto-optical characteristics. Absorption bands appear in the blue and red visible region, while over 600 nm the glass becomes more transparent. FTIR and Raman spectra evidenced phosphate-tellurite vibration modes proving the P(2)O(5)and TeO(2)network forming role. Magnetic measurements reveal the diamagnetic character of the Te-doped glass with an additional weak ferromagnetic signal, specific to diluted ferromagnetic oxides. Positive Faraday rotation angle with monotonous decreasing value at increasing wavelength was evidenced from magneto-optical measurements. The final product is a composite material comprising of a non-crystalline vitreous phase and Te-based nanoclusters accompanied by oxygen vacancies. The metallic-like Te colloids are responsible for the dark reddish color of the glass whereas the accompanying oxygen vacancies might be responsible for the weak ferromagnetic signal persisting up to room temperature.

This study addresses the deposition with improved adhesion of TiO2:N/SiO(2)mixture, with different concentrations of the nano-powders (NPs) (1:0,5; 1:1 and 1:1,5) on 100% cotton fabrics. The characteristics of the deposited thin films were investigated by scanning electron microscopy (SEM), Rutherford backscattering spectrometry (RBS), Raman scattering, FTIR, and UV-VIS absorption spectroscopy. To improve the treatment durability to the external factors, the different crosslinking methods were used. Photocatalytic activity of functionalized textile fabrics was evaluated by determining the photodegradation efficiency of the methylene blue (MB) dye and forest juice, measuring the color difference of the irradiated samples compared with non-irradiated samples. Washing durability of the samples was achieved qualitatively by determining the photocatalytic activity remaining on the textile fabrics after 1 and 5 washing cycles. The samples treated with the mixture of TiO2:N/SiO(2)have demonstrated improved self-cleaning properties, the highest photocatalytic activity being obtained for the highest value of TiO2:N/SiO(2)NPs molar concentrations equal to 1:1.

Hydroxyapatite (HAp) and samarium doped hydroxyapatite, Ca10-xSmx(PO4)(6)(OH)(2),x(Sm)= 0.05, (5SmHAp), coatings were prepared by sol-gel process using the dip coating method. The stability of 5SmHAp suspension was evaluated by ultrasound measurements. Fourier transform infrared spectroscopy (FTIR) was used to examine the optical characteristics of HAp and 5SmHAp nanoparticles in suspension and coatings. The FTIR analysis revealed the presence of the functional groups specific to the structure of hydroxyapatite in the 5SmHAp suspensions and coatings. The morphology of 5SmHAp nanoparticles in suspension was evaluated by transmission electron microscopy (TEM). Moreover, scanning electron microscope (SEM) was used to evaluate the morphology of nanoparticle in suspension and the morphology of the surface on the coating. The SEM and TEM studies on 5SmHAp nanoparticles in suspension showed that our samples consist of nanometric particles with elongated morphology. The SEM micrographs of HAp and 5SmHAp coatings pointed out that the coatings are continuous and homogeneous. The surface morphology of the 5SmHAp coatings was also assessed by Atomic Force Microscopy (AFM) studies. The AFM results emphasized that the coatings presented the morphology of a uniformly deposited layer with no cracks and fissures. The crystal structure of 5SmHAp coating was characterized by X-ray diffraction (XRD). The surface composition of 5SmHAp coating was analyzed by X-ray photoelectron spectroscopy (XPS). The XRD and XPS analysis shown that the Sm(3+)ions have been incorporated into the 5SmHAp synthesized material. The antifungal properties of the 5SmHAp suspensions and coatings were studied usingCandida albicansATCC 10231 (C. albicans) fungal strains. The quantitative results of the antifungal assay showed that colony forming unity development was inhibited from the early phase of adherence in the case of both suspensions and coatings. Furthermore, the adhesion, cell proliferation and biofilm formation of theC. albicanswere also investigated by AFM, SEM and Confocal Laser Scanning Microscopy (CLSM) techniques. The results highlighted that theC. albicansadhesion and cell development was inhibited by the 5SmHAp coatings. Moreover, the data also revealed that the 5SmHAp coatings were effective in stopping the biofilm formation on their surface. The toxicity of the 5SmHap was also investigated in vitro using HeLa cell line.

This study develops, for the first time, composite coatings based on silver and zinc doped hydroxyapatite in chitosan matrix (AgZnHApCs). The AgZnHApCs composite coatings were prepared by dip coating method. The hydroxyapatite (HAp), biocompatible material for regenerating and strengthening damaged bones were doped with silver and zinc ions and coated with chitosan in order to produce a uniform and homogenous coating with biocompatibility and antimicrobial properties. The stability of AgZnHApCs suspensions was evaluated by ultrasound measurements. The value of stability parameters of AgZnHApCs suspension is in good agreement with the value of bidistilled water used as reference fluid. Homogeneously dispersed solutions of AgZnHApCs were synthesized to endeavor to optimize the physico-chemical and biological characteristics of the coatings obtained at room temperature. The AgZnHApCs composite suspension and coatings were analyzed using various investigation techniques, such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), MTT (3-[4,5-dimethylthiazol-2-yl]-2,5-diphenylte-2H-tetrazolium bromide) assay and antimicrobial studies. The optical spectroscopy, atomic force microscopy (AFM), metallographic examination and X-ray photoelectron spectroscopy (XPS) on AgZnHApCs composite coatings were also conducted. Cell culture and MTT assays demonstrate that AgZnHApCs composite suspension and coatings have no negative effect on the cell viability and proliferation. The cell morphology was not affected in presence of AgZnHApCs composite suspension and coatings. The antimicrobial assays conducted againstStaphylococcus aureusATCC 25923,Escherichia coliATCC 25922, andCandida albicansATCC 90029 microbial strains revealed that both the AgZnHApCs composite suspension and coatings exhibited great antimicrobial properties.

Complexes with mixed ligands [Cu(N-N)(2)(pmtp)](ClO4)(2)((1) N-N: 2,2 '-bipyridine; (2) L: 1,10-phenanthroline and pmpt: 5-phenyl-7-methyl-1,2,4-triazolo[1,5-a]pyrimidine) were synthesized and structurally and biologically characterized. Compound (1) crystallizes into space groupPaand (2) inP-1. Both complexes display an intermediate stereochemistry between the two five-coordinated ones. The biological tests indicated that the two compounds exhibited superoxide scavenging capacity, intercalative DNA properties, and metallonuclease activity. Tests on various cell systems indicated that the two complexes neither interfere with the proliferation ofSaccharomyces cerevisiaeor BJ healthy skin cells, nor cause hemolysis in the active concentration range. Nevertheless, the compounds showed antibacterial potential, with complex (2) being significantly more active than complex (1) against all tested bacterial strains, both in planktonic and biofilm growth state. Both complexes exhibited a very good activity against B16 melanoma cells, with a higher specificity being displayed by compound (1). Taken together, the results indicate that complexes (1) and (2) have specific biological relevance, with potential for the development of antitumor or antimicrobial drugs.

The first electrochemical immunosensor for the determination of the 20S proteasome (P20S) was developed, entailing the immobilization of an antibody on an aminophenylboronic/poly-indole-6-carboxylic acid-modified electrode. The proposed electrochemical bioplatform is a simple and feasible analytical tool applicable for the determination of P20S in human plasma, considering its high clinical and biological relevance. Cyclic voltammetry, electrochemical impedance spectroscopy, and square wave voltammetry (SWV) were used to determine the optimal step-by-step process to obtain the electrochemical immunosensor. The interaction of P20S with the recognition layer of the immobilized antibody on the nanostructured surface took place by incubating the electrode in a P20S solution at 20 degrees C for 2 h. Using SWV as an electro-analytical technique, this immunosensor can quantify P20S. The current was linear with the P20S concentration within two dynamic concentration ranges from 20.0 to 80.0 and 80.0 to 200.0 ng.mL(-1) (r(2) = 0.992 and 0.98, respectively) with a limit of detection and quantification of 6 and 18 ng.mL(-1), respectively. Moreover, the immunosensor showed considerable repeatability and reproducibility, when the determination was done in human serum, which confirms that it is a promising alternative for direct detection of P20S in biological fluids with minimal interference.