Search results for "Soft chemistry"
showing 6 items of 16 documents
XPS and EELS investigations of chemical homogeneity in nanometer scaled Ti-ferrites obtained by soft chemistry
1999
Abstract Nanocrystalline Ti-ferrites with composition Fe 3− x Ti x O 4 with 0≤ x ≤1 are synthesized using the soft chemistry route. Heterogeneities in precipitate and annealed powders are investigated by a combination of XPS and EELS techniques. As-prepared powder consists in particles with spinel structure and grain size of about 15 nm. Due to high reactivity towards oxygen of nanoparticules, a significant amount of Fe 2+ cations oxidize during precipitation, so that precipitated powders present large deviation from oxygen-metal stoichiometry. Moreover precipitated particles are evidenced to exhibit a strong surface titanium enrichment and an iron richer core. Observation of such cation se…
Correlation between oxidation states of transition metal ions and variation of the coercivity in mixed-valence defect spinel ferrites
1997
Abstract Due to the very high dispersion of mixed-valence spinel ferrites prepared by ‘soft chemistry’ it becomes possible to oxidize in the spinel lattice, not only ferrous ions but also different transition metal ions (Cr 3+ , Mn 2+ , Mn 3+ , Mo 3+ , Mo 4+ V 2+ , V 3+ , Cu + ), by ‘soft’ oxidation between 150 and 500°C, under formation of non-stoichiometric spinels cation vacancies. The oxidation state with the coordination and the oxidation temperature of the cations have been determined in coppermanganese ferrites by derivative thermogravimetry (DTG), based on the specific solid-state reactivity of cations in the redox reaction. For Co-modified non-stoichiometric spinels, which present…
Valence states of copper in copper ferrite spinels CuxFe3−xO4 (0 < x ≤ 1) fine powders: Evidence of copper insertion
1997
Abstract The oxidation in cation deficient spinels of copper iron spinels Cu x Fe 3− x O 4 (0 x ≤ 1) synthesized by soft chemistry with a grain size x per mole of ferrite, three oxidation phenomena corresponding to Cu + at B-sites (130°C), Fe 2+ at B-sites (180°C) and Cu + at A-sites (240°C) have been found in close relation with the cation-oxygen distance of each oxidizable cation. For nonstoichiometric synthesized spinels Cu x Fe 3− x O 4+ δ with δ x , the presence of additional interstitial Cu + ions has been envisaged. The oxidation temperature of these interstitial ions (> 300°C) is higher than that for Cu + ions at Asites suggesting that interstitial copper ions also essentially resid…
Syntheses of TiO2 anatase nanocrystals with controlled size distribution. Influence of the crystallites size on the Raman spectrum and investigation …
2006
The determination of the size and the size distribution of anatase TiO2 nanopowders using Raman spectroscopy is presented. Several synthesis methods (soft chemistry, water-in-oil microemulsion, continuous hydrothermal synthesis) are used in order to control the size (from 3 to 20 nm), shape, phase and size distribution. The shift and width of the anatase Eg peak are often used to obtain the nanoparticles size. Homever, this peak is also sensitive to nonstoichiometry and others parameters. Low-frequency Raman scattering does not suffer from this problem. Size distibutions obtained by Raman spectroscopy and MET micrographs are compared. Finally, in situ Raman spectroscopy is used to study the…
Suivi par diffraction de rayons X “in situ” de l'évolution du paramètre de maille du ferrite nanométrique γ-Fe2O3lors de l'isotherme d'adsorption d'e…
2002
La methode de synthese par chimie douce a ete utilisee pour synthetiser des nanoparticules de maghemite γ-Fe 2 O 3 dans une gamme de taille allant de 9 a 14 nm. Ces poudres, parfaitement cristallisees en phase spinelle, exemptes d'impuretes, avec une stoechiometrie en oxygene parfaitement controlee, ont servi de materiaux modeles pour cette etude. Le parametre de maille de ce materiau (0,8346 nm) s'avere etre non dependant de la taille. Cependant, le suivi en Diffraction de Rayons X in-situ revele des variations de ce parametre avec la modification de la surface en presence de vapeur d'eau. Les phenomenes de chimisorption et de physisorption jouent un role preponderant dans les evolutions o…
Influence of Grain Size, Oxygen Stoichiometry, and Synthesis Conditions on the γ-Fe2O3 Vacancies Ordering and Lattice Parameters
2002
The soft chemistry method has been used to synthesize γ-Fe2O3 nanoparticles: various synthesis temperature were applied to obtain nanometric powders with crystallite size in the 9–14 nm range. Powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectrophotometry, surface area measurements, and electron microscopy (TEM, SEM). It is clearly shown that these nanometric powders are very well crystallized as indicated by XRD and IR spectra which present substructural bands attributed to vacancies ordering (P4132). Based on these model materials and in the crystallite size range studied here, cell parameter appears to be not linked to crystallite size. It rat…