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Chemical co-precipitation from ferrous and ferric salts at a 1:1.9 stoichiometric ratio in NH4OH base with ultrasonication (sonolysis) in a low vacuum environment has been used for obtaining colloidal suspensions of Fe3O4 nanoparticles coated with citric acid. Before coating, the nanoparticles were processed by electrohydraulic discharges with a high discharge current (several tens of amperes) in a water medium using a pulsed direct current. Magnetite nanoparticles were obtained with an average crystallite diameter D = 25–28 nm as obtained by XRD and particle sizes of 25 nm as measured by small-angle X-ray scattering. Magnetometry showed that all samples were superparamagnetic. The saturation magnetization for the citric acid covered samples after electrohydraulic processing showed higher value (58 emu/g) than for the directly coated samples (50 emu/g). Ultraviolet-visible spectroscopy and Fourier transform infrared spectroscopy showed the presence and binding of citric acid to the magnetite surface by chemisorption of carboxylate ions. Hydrodynamic sizes obtained from DLS and zeta potentials were 93 and 115 nm, −26 and −32 mV for the citric acid covered nanoparticles and 226 nm and 21 mV for the bare nanoparticles, respectively. The hydraulic discharge treatment resulted in a higher citric acid coverage and better particle dispersion. The developed method can be used in nanoparticle synthesis for biomedical applications. [ABSTRACT FROM AUTHOR]

Superparamagnetic iron oxide nanoparticles (SPIONs) have attracted the particular interest of scientists from various disciplines since their obtaining to the present day. The physicochemical and pharmacokinetic properties of SPIONs-containing magnetic nanofluids, and their applicability in biomedicine, largely depend on the stability of the colloidal system, particle size, size distribution, net magnetic moment, phase composition, and type and properties of stabilizers. Also, in some cases, when using magnetic nanoparticles for biomedical purposes, it is necessary that the stabilizing ligands of nanoparticles should not significantly change the magnetic properties. From this point of view, the preparation of stable colloidal systems containing bare iron oxide nanoparticles (BIONs) in water at physiological pH attracts particular attention and becomes increasingly popular in scientific circles. This study is focused on the development of the synthesis of aqueous suspensions of SPIONs stabilized with various organic molecules (oleic acid [OA] and poly(ethylene glycol) monooleate - with molecular weights 460 and 860) using a modified controlled chemical coprecipitation reaction, as well as stable nanofluids containing BIONs in an aqueous medium at neutral pH (near-physiological). The obtained samples were characterized using X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy, small-angle x-ray scattering (SAXS), dynamic light scattering (DLS), electrophoretic light scattering (ELS), and Vibrating Sample Magnetometry. [ABSTRACT FROM AUTHOR]

The gamma irradiation induced aging of thermoplastic polymer Estane 5703 in air and water environments was studied by small-angle neutron scattering (SANS), Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC), and X-ray diffraction (XRD). The degree of phase mixing was increased after irradiation, accompanied by the increase of domain distance and decrease of domain size. The hard domain distance increased from 9.8 to 11.2 nm and 14.4 nm for the samples irradiated in air and water with a dose up to 500 kGy, respectively. The GPC results indicated progressive formation of larger linked structures with very high molar mass with increasing absorbed doses. The samples irradiated in water exhibited a stronger aging effect than those irradiated in air. The FTIR results suggested that the cross-linking occurred among the secondary alkyl radicals, and the interactions in hard domains weakened because of the loss of inter-urethane H-bonds. The volume fraction of well-ordered soft segments in Estane increased upon irradiation. [ABSTRACT FROM AUTHOR]

The sonochemical coprecipitation reaction with moderate ultrasound irradiation in a low vacuum environment was used to obtain aqueous colloidal suspensions of iron oxide nanoparticles (IONPs). The synthesized magnetite nanoparticles were conjugated directly by folic acid using electrohydraulic discharges as a processing technique before modification of the surface of the nanoparticles. Electrohydraulic discharges were applied in two operational modes with high and low power pulsed direct currents between the electrodes. The physical and chemical properties of the obtained samples were studied using X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), dynamic light scattering (DLS) and small angle X-ray scattering (SAXS). The investigation proved an inverse cubic spinel structure of magnetite with folic acid attachment to the magnetite surface (mean crystallite diameter in the samples, D, ranges 25-31 nm by XRD and SAXS). It was found that the processing with electrohydraulic discharges increased the colloidal stability of the folic acid-magnetite nanoparticle dispersions. [ABSTRACT FROM AUTHOR]

In this research, a group of segmented polyurethane (PU) copolymers with different hard segment (HS) contents were successfully synthesized. The microstructure of the PU copolymers was characterized via Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and small-angle neutron scattering (SANS). Then, the PU copolymers were selected as polymer binder for coating an insensitive high explosive 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) to prepare polymer bonded explosives (PBXs). When the HS concentration of PU copolymers increased from 14 to 34 wt %, a 14.6 times increase in the creep rupture time of PBXs under 60 °C/3 MPa and a 52.3% decrease in the steady-state creep strain rate under 60 °C/1 MPa were observed. The experimental results indicated that a wide variety of structure and properties of PU copolymer could be customizable through the adjustment of the HS contents, and consequently, provided an efficient route to tune the creep performance of the PBXs over a wide range. [ABSTRACT FROM AUTHOR]

A new A 3 B porphyrin structure, namely: 5-(4-phenoxyphenyl)-10,15,20-tris(4-pyridyl)-porphyrin was synthetized and characterized by FT-IR, UV–vis, Fluorescence, MS, 1 H NMR, TLC and HPLC. Novel hybrid-silica porphyrin nanomaterials were obtained by immobilizing the porphyrin in silica supports synthesized from tetraethoxysilane, tetramethoxysilane or mixtures of tetraethoxysilane/methyltriethoxysilane. Since the behavior and performance of immobilized porphyrin molecules in the silica matrices strongly depend on the structure of the porous network, a comparative characterization of the silica support and the hybrid porphyrin-silica materials was carried out using specific physicochemical characterization methods: UV–vis, Fluorencence, FT-IR spectroscopy, thermal analysis, AFM, nitrogen adsorption and small-angle neutron scattering. The UV–vis spectra show that no protonation and aggregation of porphyrin takes place in the gels made from methyltriethoxysilane precursor. Most of the emission spectra preserve both the shape and the intensity of the corresponding free porphyrin. Due to the lack of aggregation, when using the methyltriethoxysilane precursor, the quenching of fluorescence is also diminished. No matter of the preparation method the specific surface areas increase in the following order: TEOS < TMOS < TEOS/MTES 3:1 < TEOS/MTES 2:1 < TEOS/MTES 1:1. Due to their optical properties, both the novel porphyrin and its derived hybrid materials, especially those synthesized in situ with mixtures of silica precursors TEOS/MTES will be sent for further medical trials in PDT, having characteristics of second generation photosensitizers. Due to large specific surface areas, the same materials will be used as sensitive materials in microsensors for air quality control, to detect the presence of CO, NO x , excess of CO 2 and low level of O 2 . [ABSTRACT FROM AUTHOR]