National Institute Of Materials Physics - Romania

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.

Polyvinylidene fluoride-iron oxide (PVDF-Fe2O3) nanocomposites have been obtained my melt mixing of PVDF with Fe2O3 nanoparticles. The interactions between the polymeric matrix and the nanofiller have been investigated by wide angle X-ray scattering (WAXS), Fourier transform infrared spectroscopy (FTIR), and Raman spectroscopy, using both red and green excitations (lasers). WAXS, FTIR, and Raman spectra confirm that all samples contain alpha PVDF as the major crystalline form of the polymeric matrix. Experimental data revealed small changes in the positions of X-ray lines as well as modifications of the width of X-ray lines upon loading by Fe2O3 nanoparticles. FTIR and Raman spectra are dominated by the lines of the polymeric matrix. Within the experimental errors, the positions of Raman lines are not affected by the wavelength of the incoming electromagnetic radiation, although they are sensitive to the strain of the polymeric matrix induced by addition of the nanofiller. The loading of the polymeric matrix with nanoparticles stretches the macromolecular chains, affecting their vibrational spectra (FTIR and Raman). A complex dependence of the positions of some Raman and FTIR lines on the loading with Fe2O3 is reported. The manuscript provides a detailed analysis of the effects of nanofiller on the position of WAXS, FTIR, and Raman lines. (c) 2020 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020, 137, 48907.

This paper outlines a method of extraction of iron from water in the form of iron oxyhydroxide natural nanoclusters at comparatively low concentrations and varied ranges of pH using zinc acetate salt. The zinc acetate salt dissociates into Zn(2+)and acetate ions in water where Zn(2+)interacts with iron clusters present in a solution of a given iron concentration and pH, while the acetate ion helps in charge-neutralization based coagulation and consequent precipitation of such nanoclusters. The Zn(2+)ions may also lead to the growth of layered zinc hydroxide (LZH) nanosurfaces at pH >= 6 at sufficient loading. The advantage of this method is the active chemical interaction of Zn(2+)with Fe clusters, followed by growth, which ensures that only some added Zn ions remain in the water while the rest precipitate out along with the residual iron oxyhydroxide, especially at higher pH. The solid that precipitated under various different conditions was successfully evaluated by XRD (formation of ferrihydrite-like nanoclusters (n-Fh)), FTIR (the presence of acetate in the solid n-Fh), TEM (the presence of zinc at higher pH), and EXAFS (local structural characterization). ICP analysis of the obtained solid and the corresponding filtrate revealed the removal efficiency of iron and zinc from the solution at various initial concentrations and pH values. This method of extracting soluble Fh-like nanoclusters by charge neutralization appears to be a suitable promising tool for water purification, because ferrihydrite is capable of isolating other adsorbed contaminants from water, along with itself.

Graphene-based photocatalytic layers were prepared by reactive matrix assisted pulsed laser evaporation technique. Binary, nitrogen doped reduced graphene oxide (RGO)/TiO2 and ternary RGO/TiO2/graphitic carbon nitride (g-C3N4) compounds were synthesized and simultaneously deposited onto solid substrates. Aqueous dispersions of commercial graphene oxide platelets and TiO2 nanoparticles were prepared. NH3 or melamine powder was added to the dispersions to achieve enhanced nitrogen doping and synthesis of g-C3N4 during laser irradiation. The photocatalytic efficiency of the layers towards degradation of antibiotic, chloramphenicol and organic dye molecules was systematically investigated and correlated with structural, compositional, and morphological features. This study provides new insights into the importance of TiO2 crystal facets and the synergistic effects between TiO2 nanocrystals and the other constituents, nitrogen doped RGO and g-C3N4 of the hybrid layers. As a result of combined effect of constituent materials, TiO2, RGO, and g-C3N4 as well as N doping of RGO, through the generation of quaternary and pyrrolic N functionalities, the composite layers showed high photocatalytic efficiency for degradation of organic molecules. Stability and reusability experiments indicated that the composite layers maintain their high photodegradation efficiency towards organic molecules during consecutive degradation cycles. Active radical scavenging experiments were also carried out in order to determine the role of the main active species involved in the photocatalytic degradation process.

Iron oxides such as magnetite and maghemite coated with cetyltrimethylammonium bromide (CTAB) are very promising materials for wastewater treatment because iron oxide can be easily separated from solutions using the magnetic separation procedure Iron oxide (IO) coated CTAB was synthesized by an adapted co-precipitation method. In the present study, the IO-CTAB was used for removing arsenic from water for the first time. In the present study, the performance of iron oxide coated CTAB biocomposites as an adsorbent for arsenic removal from aqueous solutions was examined. X-ray diffraction (XRD) analysis and the results revealed a cubic phase Fd-3 m of Fe(3)O(4)with lattice a = 8.40 angstrom and average crystal size equal to 17.26 +/- 3 nm. The mean particle size calculated from transmission electron microscopy (TEM) was 19.86 +/- 1.7 nm. The results of the adsorption batch experiments and the data determined using the Langmuir and Freundlich models emphasized that IO-CTAB nanoparticles were favorable for the adsorption of As(III) ions from aqueous solutions. Ultrasound measurements have shown that IO-CTAB is a cost-effective biocomposite for removing arsenic from contaminated solutions. Moreover, x-ray photoelectron spectroscopy (XPS) has shown that during the process of arsenic absorption, there is oxidation from As(III) to As(V), which leads to a decrease in toxicity during this process. The results of the cytotoxic assays confirmed that the IO-CTAB nanoparticles did not induce any morphological changes in the HeLa cells and did not affect their proliferation after 24 h of incubation.

Polymer-based nanocomposites have recently received considerable attention due to their unique properties, which makes them feasible for applications in optics, sensors, energy, life sciences, etc. The present work focuses on the synthesis of nanocomposites consisting of a polytetrafluorethylene-like matrix in which metallic nano-silver are embedded, by using multiple magnetron plasmas. By successively exposing the substrate to separate RF magnetrons using as combination of target materials polytetrafluorethylene (PTFE) and silver, individual control of each deposition process is insured, allowing obtaining of structures in which silver nanoparticles are entrapped in-between two PTFE layers with given thicknesses. The topographical and morphological characteristics investigated by means of Scanning Electron Microscopy and Atomic Force Microscopy techniques evidenced the very presence of Ag nanoparticles with typical dimension 7 nm. The chemical composition at various depositing steps was evaluated through X-ray Photoelectron Spectroscopy. We show that the presence of the top PTFE layer prevents silver oxidation, while its thickness allows the tailoring of optical properties, as evidenced by spectroellipsometry. The appearance of chemical bonds between silver atoms and PTFE atoms at interfaces is observed, pointing out that despite of pure physical deposition processes, a chemical interaction between the polymeric matrix and metal is promoted by plasma.

Covalent immobilization of antibodies to protein G beads is a basic molecular biology method, although the beads present poor recovery results. Our aim was to reuse the immobilized antibody-protein G complex on a very small scale, therefore we optimized the crosslinking procedure to be used on the wells of a standard 96-well microplate. The method used involves the affinity binding of the antibody to the protein G surface, followed by the immobilization step using different crosslinking reagents, DMP and BS3, quenching the crosslinking reaction, and binding the antibody-specific antigen. By scaling down the procedure, we were able to reuse the anti-EGFR crosslinked wells more than 20 times. This method can be used to perform assays on a wide range of solid supports containing the protein G in an immobilized form, including functionalized nanosensors, for immunoprecipitation, protein and cell lysate purification, target protein enrichment.

With the aim of demonstrating phase coexistence of two magnetic phases in an intermediate annealing regime and obtaining highly coercive FePt nanocomposite magnets, two alloys of slightly off-equiatomic composition of a binary Fe-Pt system were prepared by dynamic rotation switching and ball milling. The alloys, with a composition Fe(53)Pt(47)and Fe55Pt45, were subsequently annealed at 400 degrees C and 550 degrees C and structurally and magnetically characterized by means of X-ray diffraction,Fe-57 Mossbauer spectrometry and Superconducting Quantum Interference Device (SQUID) magnetometry measurements. Gradual disorder-order phase transformation and temperature-dependent evolution of the phase structure were monitored using X-ray diffraction of synchrotron radiation. It was shown that for annealing temperatures as low as 400 degrees C, a predominant, highly ordered L1(0)phase is formed in both alloys, coexisting with a cubic L1(2)soft magnetic FePt phase. The coexistence of the two phases is evidenced through all the investigating techniques that we employed. SQUID magnetometry hysteresis loops of samples annealed at 400 degrees C exhibit inflection points that witness the coexistence of the soft and hard magnetic phases and high values of coercivity and remanence are obtained. For the samples annealed at 500 degrees C, the hysteresis loops are continuous, without inflection points, witnessing complete exchange coupling of the hard and soft magnetic phases and further enhancement of the coercive field. Maximum energy products comparable with values of current permanent magnets are found for both samples for annealing temperatures as low as 500 degrees C. These findings demonstrate an interesting method to obtain rare earth-free permanent nanocomposite magnets with hard-soft exchange-coupled magnetic phases.