ABSTRACT
Ultra-small magnetic Fe3O4 nanoparticles are successfully synthesized in basic solutions by using the radiolytic method of the partial reduction in FeIII in the presence of poly-acrylate (PA), or by using the coprecipitation method of FeIII and FeII salts in the presence of PA. The optical, structural, and magnetic properties of the nanoparticles were examined using UV-Vis absorption spectroscopy, high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and SQUID magnetization measurements. The HRTEM and XRD analysis confirmed the formation of ultra-small magnetite nanoparticles in a spinel structure, with a smaller size for radiation-induced particles coated by PA (5.2 nm) than for coprecipitated PA-coated nanoparticles (11 nm). From magnetization measurements, it is shown that the nanoparticles are superparamagnetic at room temperature. The magnetization saturation value Ms = 50.1 A m2 kg-1 of radiation-induced nanoparticles at 60 kGy is higher than Ms = 18.2 A m2 kg-1 for coprecipitated nanoparticles. Both values are compared with nanoparticles coated with other stabilizers in the literature.
ABSTRACT
One-step colloidal synthesis of subnanometer CdS clusters in hydrophobic MFI-type zeolite crystals in the presence of 3-mercaptopropyl-trimethoxysilane (MPS), cadmium precursor, and tetrapropylammonium hydroxide (TPAOH) is performed. MPS is used as the bifunctional agent, as it hydrolyzes fast, cross-links with the silica framework, and provides thiol groups to anchor Cd(2+), and subsequently forms CdS clusters. The MFI crystals with the thiol groups not only function as a nanochamber for the formation of CdS but also prevent further moisture-induced agglomeration of the clusters. Direct evidence for the presence of asymmetric shaped subnanometer CdS clusters aligned in the channels of MFI crystals stabilized in suspensions and films is provided by high resolution transmission electron microscopy (HRTEM), grazing incidence X-ray diffraction (GI-XRD), and photoluminescence spectra (emission < 350 nm). The CdS clusters are stable for months in colloidal suspensions and films without any particular precaution against water. The hydrophobicity of the MFI zeolite and the presence of the organic template in the channels favor the stabilization of small CdS clusters, which are available for further applications.
