One-phase, one-pot synthesis of Ag(0) nanoparticles capped with alkanethiolate molecules has been optimized to easily achieve a pure product in quantitative yield. We report the synthesis of dodecanethiolate-capped silver particles and the chemophysical, structural, and morphologic characterization performed by way of UV-vis, (1)H NMR, and X-ray photoelectron (XPS) spectroscopies, X-ray powder diffraction (XRD) and X-ray absorption fine structure analysis (XFAS), electron diffraction and high-resolution transmission electron microscopy (HR-TEM), and scanning and transmission electron microscopy (SEM and TEM). Depending on the molar ratio of the reagents (dodecylthiosulphate/Ag(+)), the mean Ag(0) particle size D(XRD) is tuned from 4 to 3 nm with a narrow size distribution. The particles are highly soluble, very stable in organic solvents (hexane, toluene, dichloromethane, etc.), and resistant to oxidation; the hexane solution after one year at room temperature does not show any precipitation or formation of oxidation byproducts.
Magnetite nanoparticles having mean diameter of about 8 nm have been prepared by a thermo-chemical route. Different amounts (5 and 10% wt) of a stable dispersion of magnetite nanoparticles in n-hexane were added to polyethylene glycol diacrylate (PEGDA-600) oligomer containing 2% wt of radicalic photoinitiator. The homogenized mixture was poured on a silica glass substrate and the resulting film was photoreticulated in N2 atmosphere using a UV lamp. As a result, a polymer-based magnetic nanocomposite was obtained, where the magnetic nanoparticles are dispersed in the diamagnetic matrix, as checked by SEM. Morphology, composition, and size of as-prepared nanoparticles were checked by SEM and X-ray diffraction. The magnetic properties of magnetite nanoparticles prior to and after inclusion in the polymeric matrix have been studied by means of an alternating-gradient magnetometer (T interval: 10–300 K, HMAX: 18 kOe). FC-ZFC curves were obtained in the same temperature interval. The results show that the nanocomposites cannot be simply described as containing superparamagnetic particles undergoing an anisotropy-driven blocking and that collective magnetic interactions play a non-negligible role. Low-temperature hysteretic properties indicate that the polymeric matrix affects the effective anisotropy of magnetite nanoparticles. Dispersion of magnetite NPs in PEGDA has non-trivial consequences on their magnetic propertie
Rhombohedral shaped, single crystal hematite particles with narrow size distribution (D(TEM) = 93 +/- 2 nm) were prepared by hydrolysis of iron chloride and polymerisation in water. The results of field dependent magnetization measurements at different warming-cooling rates and ac susceptibility measurements at varying frequencies are reported and discussed. Thermal hysteresis (DeltaT(M)) associated with the Morin transition and field dependence of the Morin temperature (T(M)) are observed in warming-cooling cycles (DeltaT(M) = 25 and 13 K for H = 0.1 and 3 T, respectively) due to the first order phase transition. A frequency dependence of ac susceptibility is observed above T(M), as a result of the relaxation of the magnetic moment of hematite particles in the weak-ferromagnetic phase.
Hydrophilic magnetite nanoparticles in the size range 30-10nm are easily and rapidly prepared under ultrasonic irradiation of Fe(OH)(2) in di- and tri-ethylene glycol/water solution with volume ratio varying between 7:3 and 3:7. Structural (XRD) and morphological (SEM) characterization reveal good crystalline and homogeneous particles whereas, when solvothermally prepared, the particles are inhomogeneous and aggregated. The sonochemically prepared particles are versatile, i.e. well suited to covalently bind molecules because of the free glycol hydroxylic groups on their surface or exchange the diethylene or triethylene glycol ligand. They can be easily transferred in hydrophobic solvents too. Room-temperature magnetic hysteresis properties measured by means of Vibrating Sample Magnetometer (VSM) display a nearly superparamagnetic character. The sonochemical preparation is easily scalable to meet industrial demand.
A dispersion of magnetite nanoparticles in hexane has been added to 1,6‐hexanediol diacrylate at 5–40 phr. The obtained formulations have been polymerized by means of UV light in the absence of any radical photoinitiator and the cured films have been fully characterized. The photoinitiator activity of the magnetite nanoparticles is demonstrated: upon photoexcitation, Fe3O4 can generate radicals which in turn start polymerization chains. Isothermal magnetization curves showed that at room temperature, the cured material exhibits no hysteretic features, indicating a superparamagnetic‐like behavior. At temperatures below 100 K, a significant magnetic hysteresis gradually appears but a substantial fraction of magnetic nanoparticles is still in the superparamagnetic phase even at T = 10 K. magnified image
Acrylic based films containing thermo-chemically synthesized magnetite nanoparticles (NPs) were prepared by UV-curing. A stable dispersion of Fe3O4 NPs in n-hexane was added to polyethylene glycol diacrylate (PEGDA) oligomer or to hexanediol diacrylate (HDDA) oligomer, producing a blend whose viscosity matches the processing requirements for inkjet printing technology. Morphologic characterization is provided by means of Field Effect SEM on a representative nanocomposite section.By real-time FT-IR analysis it was shown that Fe3O4 NPs are able to initiate radical chain-grown polymerization under UV light, for what concerns the HDDA matrix. Tight cross-linked transparent polymeric films were obtained after 1 minute of UV irradiation.The magnetic properties of the produced films were studied by means of an Alternating-Gradient Force Magnetometer (AGFM) in the temperature range 10 – 300 K and up to 18 kOe. The isothermal magnetization curves of both HDDA and PEGDA -based nanocomposites showed that these hybrid systems must be described as interacting superparamagnets (ISP) characterized by inter-particle magnetic interactions dominating over intra-particle effects.
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