Silviu Preda

Advanced functionalization of organoclay nanoparticles by silylation and their polystyrene nanocomposites obtained by miniemulsion polymerization

Four types of alkoxysilanes with different organosilyl groups were used for the silylation of a commercial alkylammonium-modified montmorillonite (Cloisite 30B). TGA, XPS, DLS, FTIR, XRD, and contact angle measurements were performed for the characterization of the silylated clays. Furthermore, the behavior of these advanced hydrophobic clays in the miniemulsion polymerization process of styrene and the characterization of nanocomposites materials were followed. The hydrophobic nature is a combined result of the length of the organic chain and of the amount of silane groups grafted onto clay edges, reflected also in the final properties of the nanocomposite latexes.

High-Tc phase obtained in the Pb/Sb doped Bi-Sr-Ca-Cu-O system

Abstract Partial replacement of Bi by Pb and Sb produces materials of high- T c pure phase, with antimony playing an important role in accelerating the formation of the phase with the higher superconductive transition in the Bi–Sr–Ca–Cu–O system. The influence of the antimony precursors on the superconducting phases mechanism formation was examined. Using a solid state reaction route, two nominal compositions Bi 1.6 Pb 0.3 Sb 0.1 Sr 2 Ca 2 Cu 3 Oy and Bi 1.6 Pb 0.4 Sb 0.1 Sr 2 Ca 2 Cu 4 Oy were investigated. The sources of antimony were Sb 2 O 3 , α Sb 2 O 4 and a prepared mixture Bi 1.9 Sb 0.1 O x . The mechanism formation of the phases upon annealing was investigated using X-ray diffraction and simultaneous thermal analysis. Electrical properties of the obtained materials were evaluated. The presence of the antimony ions determined a higher reactivity of the system as well as the promotion of the superconducting high- T c phase enhancement.

Green Synthesis Methods of CoFe2O4 and Ag-CoFe2O4 Nanoparticles Using Hibiscus Extracts and Their Antimicrobial Potential

The cobalt ferrite CoFe2O4 and silver-cobalt ferrite Ag-CoFe2O4 nanoparticles were obtained through self-combustion and wet ferritization methods using aqueous extracts of Hibiscus rosa-sinensis flower and leaf. X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, and magnetic measurements were used for the characterization of the obtained oxide powders. The antimicrobial activity of the cobalt ferrite and silver-cobalt ferrite nanoparticles against Gram-positive and Gram-negative bacteria, as well as fungal strains, was investigated by qualitative and quantitative assays. The most active proved to be the Ag-CoFe2O4 nanoparticles, particularly those obtained through self-combustion using hibiscus leaf extract, which exhibited very low minimal inhibitory concentration values 0.031–0.062 mg/mL against all tested microbial strains, suggesting their potential for the development of novel antimicrobial agents.

Polymer-clay nanocomposites obtained by solution polymerization of vinyl benzyl triammonium chloride in the presence of advanced functionalized clay

AbstractPolymer-clay nanocomposites were synthesized by solution polymerization method using advanced functionalized clay and vinyl benzyl trimethyl ammonium chloride as monomer. First stage consisted in the silylation of a commercial organo-modified clay-Cl 20A using alkoxysilanes with different chain lengths. In the second step, the synthesis and characterization of polymer-nanocomposites were followed. To evaluate the clay functionalization process as well as the final polymer-clay products, thermogravimetric, X-ray diffraction, dynamic light scattering, Fourier transform infrared spectroscopy and three test liquid contact angles analyses were used. The loss of ammonium ions from commercial clay, the grafting degree, the lengths and the nature of alkyl chain influence the dispersion of the advanced modified clay into the polymer solution and, furthermore, the properties of the final polymer-clay nanocomposite film. Graphical AbstractPolymer-clay nanocomposites were obtained by solution polymerization using advanced functionalized clay and a water soluble monomer. The loss of ammonium ions, the grafting degree, the lengths and the nature of alkyl chain influenced the dispersion of the modified clay into the polymer solution and the properties of the final hybrid film.

Microstructure, surface characterization and long-term stability of new quaternary Ti-Zr-Ta-Ag alloy for implant use

The novel Ti-20Zr-5Ta-2Ag alloy was characterised concerning its microstructure, morphology, mechanical properties, its passive film composition and thickness, its long-term electrochemical stability, corrosion resistance, ion release rate in Ringer solution of acid, neutral and alkaline pH values and antibacterial activity. The new alloy has a crystalline α microstructure (by XRD). Long-term XPS and SEM analyses show the thickening of the passive film and the deposition of hydroxyapatite in neutral and alkaline Ringer solution. The values of the electrochemical parameters confirm the over time stability of the new alloy passive film. All corrosion parameters have very favourable values in time which attest a high resistance to corrosion. Impedance spectra evinced a bi-layered passive film formed by the barrier, insulating layer and the porous layer. The monitoring of the open circuit potentials indicated the stability of the protective layers and their thickening in time. The new alloy releases (by ICP-MS measurements) very low quantities of Ti, Zr, Ag ions and no Ta ions. The new alloy exhibits a low antibacterial activity.

Surface Analysis, Microstructural, Mechanical and Electrochemical Properties of New Ti-15Ta-5Zr Alloy

This paper describes the synthesis of a novel Ti-15Ta-5Zr alloy with an α + ß stable, homogeneous, biphasic microstructure (by optical microscopy, X-ray diffraction and scanning electron microscopy) and the determination of its mechanical properties, hardness and a Young’s modulus of 42.2 GPa. The alloy passive film composition and thickness were analyzed by X-ray photoelectron spectroscopy; a thick, compact native passive film containing the protective oxides of all constituent elements (TiO2, Ta2O5, ZrO2) was identified. The electrochemical parameters confirmed a nobler behaviour and a more capacitive, resistant passive film on the alloy surface compared to Ti and other existing implant alloys; these facts are due to the alloying elements that, by their oxides stabilize and reinforce the alloy passive film. This passive film thickened in time, which increased its protective capacity. The new alloy had no susceptibility to galvanic or local corrosion. Ti-15Ta-5Zr alloy is recommended as an advanced orthopaedic implant material.

Influence of the substrate type on the microstructural, optical and electrical properties of sol–gel ITO films

AbstractIndium tin oxide (ITO) is recognized as the best transparent and conductive material [transparent conducting oxide (TCO)] until now and its properties are dependent on the preparation method. In the present work ITO films with In:Sn atomic ratio 9:1 were prepared by a sol–gel route on different substrates (microscope glass slides, microscope glass covered with one layer of SiO2 and Si wafers) for TCO applications. The multilayer ITO films were obtained by successive deposition by the dip-coating method and the films were characterized from the structural, morphological, optical, and electrical points of view using X-ray diffraction, scanning electron microscopy, atomic force microscopy, spectroscopic ellipsometry and by Hall effect measurements, respectively. The results showed that the thickness, optical constants and carrier numbers depend strongly on the type of substrate, number of deposited layers and sol concentration. The optical properties of ITO films are closely related to their electrical properties. The enhancement of the conductivity was possible with the increase of crystallite size (which occurred after thermal treatment) and with the reduction of surface roughness.

Novel Hydrogel-Advanced Modified Clay Nanocomposites as Possible Vehicles for Drug Delivery and Controlled Release

Present study refers to the synthesis of new advanced materials based on poly(methacrylic acid) (PMAA) with previously reported own advanced modified clays by edge covalent bonding. This will create the premises to obtain nanocomposite hydrogels with combined hydrophilic-hydrophobic behavior absolutely necessary for co-delivery of polar/nonpolar substances. For the synthesis, N,N’-methylenebisacrylamide was used as cross-linker and ammonium persulphate as initiator. As a consequence of the inclusion of clay into the polymer matrix and the intercalation of PMAA between the layers as well as the presence of hydrophobic interactions occurred between partners, the final hydrogel nanocomposites possessed greater swelling degrees, slower de-swelling process and enhanced mechanical properties depending on the clay type in comparison with pure hydrogel. In vitro MTS ([3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium, inner salt]) colorimetric assay showed that direct exposure with PMMA-clay-based constructs did not affect cell viability and proliferation in time (24 and 48 h) on either normal or adenocarcinoma cell lines.

Tubular and Spherical SiO2 Obtained by Sol Gel Method for Lipase Immobilization and Enzymatic Activity

A wide range of hybrid biomaterials has been designed in order to sustain bioremediation processes by associating sol-gel SiO2 matrices with various biologically active compounds (enzymes, antibodies). SiO2 is a widespread, chemically stable and non-toxic material; thus, the immobilization of enzymes on silica may lead to improving the efficiency of biocatalysts in terms of endurance and economic costs. Our present work explores the potential of different hybrid morphologies, based on hollow tubes and solid spheres of amorphous SiO2, for enzyme immobilization and the development of competitive biocatalysts. The synthesis protocol and structural characterization of spherical and tubular SiO2 obtained by the sol gel method were fully investigated in connection with the subsequent immobilization of lipase from Rhizopus orizae. The immobilization is conducted at pH 6, lower than the isoelectric point of lipase and higher than the isoelectric point of silica, which is meant to sustain the physical interactions of the enzyme with the SiO2 matrix. The morphological, textural and surface properties of spherical and tubular SiO2 were investigated by SEM, nitrogen sorption, and electrokinetic potential measurements, while the formation and characterization of hybrid organic-inorganic complexes were studied by UV-VIS, FTIR-ATR and fluorescence spectroscopy. The highest degree of enzyme immobilization (as depicted from total organic carbon) was achieved for tubular morphology and the hydrolysis of p-nitrophenyl acetate was used as an enzymatic model reaction conducted in the presence of hybrid lipase–SiO2 complex.

Synthesis of Oxide Nanotubes/Nanorods by Hydrothermal Method

Titanate nanotubes and ZnO nanorods are the most studied 1D oxide nanostructures, due to their specific structure, morphology, and special properties. Several physical and chemical methods of preparation have been developed for their preparation. Among the chemical methods, the mostly used are the template-assisted sol–gel method, hydrothermal method, and anodic oxidation. In the following chapter, a short review of the results obtained by hydrothermal preparation of titanate nanotubes and ZnO nanorods and their structural, morphological, and thermal characterization is presented. In the case of titanate nanotubes, the factors influencing the hydrothermal synthesis as well as factors influencing the post-hydrothermal treatment of resulted titanate were discussed. The influence of the microwaves on the hydrothermal preparation of titanate nanotubes is also presented. In the case of ZnO nanorods/nanotubes, the different experimental conditions for their preparation by hydrothermal method were established. Among the different precursors and reagents involved in the hydrothermal procedure for the ZnO nanorod/nanotube preparation, the zinc nitrate–hexamethylenetetramine system is one of the mostly used, and it was approached in more details. The obtaining of ZnO nanorods and their transformation into nanotubes in the mentioned system was discussed. At the same time, the possibility of doping ZnO nanotubes and their growth as aligned ZnO nanorods on the different substrates was presented. Besides titanate nanotubes and ZnO nanorods/nanotubes, several other oxides (V2O5, MoO3, WO3, SnO2, Fe2O3) that could be obtained by hydrothermal method were discussed.