RESUMO
Single domain superparamagnetic ferrite nanoparticles with the composition MFe2O4 (M = Fe, Co, Zn) have been prepared by thermal decomposition of metal acetylacetonates in diphenyl ether or dibenzyl ether, using oleic acid in the presence of oleylamine as a stabilizing agent. The Fe, Co and Zn ferrite nanoparticles are monodisperse with diameters of 4.9, 4.4 and 4.7 nm, respectively. The TG and IR results indicate that four or six carboxylate groups per nm2 are bonded at the surface of the particles acting as chelating and/or bridging bidentate ligands depending on the composition. The oleate groups minimize the interparticle interactions in Fe and Zn ferrite samples, while in the Co ferrite sample dipolar interactions produce broad maxima in the ZFC and energy barriers distribution curves. The inversion degree has been estimated from the Raman spectra and the obtained x values have been used to calculate the saturation magnetization and compare them with the experimental MS values. Compared to bulk materials, the magnetization value is higher for the Zn ferrite sample due to its mixed spinel cation distribution. For the Co ferrite sample, and probably for the Fe one, the low value of saturation magnetization seems to be due to the surface disordered layer of canted spins. Compared to non-coated nanoparticles with the same composition and similar size, the oleate groups, covalently bonded to the superficial cations, increase the anisotropy field and decrease the magnetization.
RESUMO
The production of high-quality colloidal crystals demands precise quantitative characterization of their nanostructures. While small-angle radiation scattering is the technique of choice, a procedure for a comprehensive quantitative modeling of the data is still pending. A novel theory based on the pertinent radial pair distribution which takes into account orientational, positional, stacking disorder and grain effects is developed here. We also show how the scattering length density of the particles can be estimated from the positions of minima in the form factor. The obtained results can be cast as sums of analytical functions over the distribution function and, as such, are suitable for easy (automatic) parallelization. On the experimental side, we report on a strong extinction effect coming from grazing incidence specular reflection that we have been able to model analytically.
RESUMO
Assemblies of colloidal particles are frequently used in novel applications, and this requires nondestructive methods allowing overall characterization of the sample and collection of information about the quality of the arrays. From suspensions of polystyrene, poly[styrene-co-(2-hydroxyethylmethacrylate)], poly[styrene-co-acrylic acid], and poly[styrene-co-methacrylic acid], assemblies of spherical particles were obtained by elimination of the solvent in different ways-evaporation, gravity deposition, and filtration. These latex particle packings were characterized by scanning and transmission electron microscopy and by gas adsorption to determine the efficiency of packing. The surface area, total pore volume, and pore size distributions obtained from the adsorption and desorption data were related to characteristic parameters calculated for cubic close-packed spherical particles.