0000000000003324
AUTHOR
N. Guigue-millot
showing 8 related works from this author
Chemical heterogeneities in nanometric titanomagnetites prepared by soft chemistry and studied ex situ : evidence for fe-segregation and oxidation ki…
2001
Nanocrystalline Fe-based spinels with composition Fe3-xTixO4 are synthesized using soft chemistry. Two steps are involved: precipitation in an aqueous solution followed by thermal annealing under a reducing mixture of N2/H2/H2O gases. Fe-segregation is found inside stoichiometric particles when the powders are studied ex situ; they exhibit a strong surface iron enrichment. This heterogeneity is related to kinetic effects linked to the difference of mobility between Fe2+ and Ti4+ cations during the partial oxidation of cations occurring ex situ. Stresses in the grains induced by oxidation govern the oxidation kinetics and lead to an abrupt compositional variation inside each particle. These…
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…
Apparent magic numbers in embedded Ti-O clusters
2003
Stable clusters constituted of four ${\mathrm{TiO}}_{2}$ entities have been evidenced in nanometer-sized spinel oxides by a combination of diffraction and x-ray-absorption experiments. Contrary to free clusters, the size of the embedded clusters is strongly determined by the constraints imposed by the surrounding matrix so that the magic number of four is in fact specific to the matrix and only then apparent.
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…
Phénomènes de ségrégation dans les ferrites de titane nanométriques : apports complémentaires de différentes techniques expérimentales (DRX, XPS, EXA…
2002
Grâce a la complementarite de diverses techniques deux phenomenes de segregation ont ete mis en evidence dans les ferrites de titane nanostructures: une segregation cinetique (dite dynamique) et une segregation thermodynamique. Par des techniques d'analyse locales (MET, XPS) et statistiques (DRX...), des heterogeneites au sein des grains de poudre contenant des cations Fe 2+ ont ete mises en evidence lors de leur etude a l'air. Leur origine est cinetique et decoule d'une oxydation incomplete des cations Fe 2+ . Des affinement de Rietveld de diagrammes de diffraction des rayons X et diffraction de neutrons ont permis de montrer quant a eux que le titane ainsi que toutes les lacunes creees lo…
Sintering of copper nanopowders under hydrogen: an in situ X-ray diffraction analysis.
2003
Abstract The reduction by hydrogen gas of the cuprite layer on copper nanocrystals and the subsequent sintering of the nano-particles were studied using in-situ X-ray diffraction and dilatometry. Spherical nanocrystals produced by evaporation and condensation have an average size of 35 nm, exhibiting a large surface curvature. Each nanoparticle is coated with a 3.5 nm layer of Cu 2 O, which is rough and disordered, as revealed by high-resolution electron microscopy. Reduction by hydrogen of this curved cuprite layer occurs at 363 K, which is ≈65 K lower than is observed on a layer supported by micrometer-sized or bulk copper with a flat surface. The reduction process and its effect on the s…
Control of grain size and morphologies of nanograined ferrites by adaptation of the synthesis route: mechanosynthesis and soft chemistry
2003
Abstract Nanocrystalline Fe-based spinels with composition Fe 2.5 Ti 0.5 O 4 can be synthesized using two different routes: soft chemistry and high-energy ball milling. This paper is focussed on the fact that each type of synthesis process can lead to powders with a crystallite size of about 15 nm but with significant differences in the grain size distribution and the agglomeration state. Whereas in the case of mechanosynthesis, the ball-milled powders consist of aggregates, those obtained by soft chemistry are very well dispersed. Moreover the chosen investigated nanopowders present a blocked/superparamagnetic transition depending on the grain size. The grain size morphologies obtained by …
Evidence for the verwey transition in highly nonstoichiometric nanometric fe-based ferrites
2001
The nanometric scale allows an investigation of the Verwey transition: the impact of varying degree of oxidation of Fe cations on this transition was studied by means of zero-field-cooled superconducting quantum interference device measurements in nanometric highly nonstoichiometric particles of pure and Ti-substituted magnetite synthesized using soft chemistry route. It is clearly shown that (i) there is a shift of the transition towards higher temperatures for nanometer scaled compounds and (ii) the amplitude, the temperature, and the order of the transition are only depending on the number of ${\mathrm{Fe}}^{2+}{/\mathrm{F}\mathrm{e}}^{3+}$ pairs in octahedral coordination.