Search results for "Soft chemistry"

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…

Experimental set up for determining the temperature-oxygen partial pressure conditions during synthesis of spinel oxide nanoparticles

1997

Abstract Nanometric spinel oxide powders, Fe 3− x M x O 4 , where M is a transition element, have been synthetized by soft chemistry. This method generally leads to a non-stoichiometric phase, Fe 3− x M x O 4+δ where δ is the deviation from stoichiometry so that further annealing at low temperatures around 450°C and low oxygen partial pressure around 10 −25 Pa given by N 2 /H 2 /H 2 O gas mixtures is required: this enables a stoichiometric compound to be obtained and a nanometric size to be maintained. The complete set up consisting of a gas mixer, a thermogravimetric apparatus and a preparative furnace is described. Some results concerning the conditions of temperature and oxygen partial p…

Synthesis, characterization, and hierarchical organization of tungsten oxide nanorods: spreading driven by Marangoni flow.

2009

Tungsten oxide nanorods were synthesized by a soft chemistry approach using tungsten alkoxide and trioctyl amine and oleic acid as the surfactants. The optical properties of the nanorods were studied. The nanorods were found to be soluble in a wide range of solvents like chloroform, cyclohexane, and so on. Upon solvent evaporation, the nanorods formed hierarchically organized solid state structures. Depending on the solvent used, the nanorods organized in different mesostructures. Moreover, the organization of the nanorods from mixtures of polar and nonpolar solvents was studied. Here, the Marangoni effect resulting from differences in the surface tensions of the two solvents was found to p…

Synthesis and Stability Region of Stoichiometric Nanocrystalline Vanadium−Iron Spinel Powders

2000

Vanadium-iron spinels with nanometric sizes have been synthesized by a soft chemistry route. This way of elaboration consists of a coprecipitation followed by thermal treatments at low temperatures. The last thermal annealing is performed under a reducing atmosphere in order to obtain the exact oxygen stoichiometry (four oxygen atoms for three metal atoms in AB 2 O 4 ). Because of the low temperatures used, very low oxygen partial pressures (between 10 -20 and 10 -30 Pa) have to be applied. For this purpose, a reducing setup has been used. It consists of H 2 /N 2 /H 2 O gas mixtures, creating a reducing atmosphere with low oxygen partial pressure. This atmosphere can be applied to a sample …

In situ and time resolved study of the - transition in nanometric particles

2007

In situ and real-time study of the {gamma} to {alpha}-Fe{sub 2}O{sub 3} transition is carried out on the H10 beamline at LURE (France). {gamma}-Fe{sub 2}O{sub 3} particles are synthesized by soft chemistry. These particles have an average diameter evaluated by X-ray diffraction of 9{+-}1nm and a specific surface area of 116m{sup 2}g{sup -1}. The size of produced {alpha}-Fe{sub 2}O{sub 3} particles is determined by in situ and time resolved X-ray diffraction measurements at different temperatures. An amazing evolution of size with time is revealed: an abrupt doubling of the {alpha}-Fe{sub 2}O{sub 3} particle size is observed whatever the heating temperature. Some assumptions are given in ord…

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.

Total oxidation of VOCs on mesoporous iron oxide catalysts: Soft chemistry route versus hard template method

2016

9 figures, 3 tables.-- Supplemantary information available

Mechanical activation conditions of the Fe2O3 and V2O3 mixture powders in order to obtain a nanometric vanadium spinel ferrite

1999

Abstract Co-milling of iron and vanadium oxides allows to obtain an intimate oxides mixture at a nanoscale, similar to a coprecipitate elaborated by soft chemistry. Reduction of such a mixture in the same temperature and oxygen partial pressure conditions (500°C and 10−25 Pa) as the soft chemistry products leads to a nanometric vanadium ferrite with the only spinel phase. The characterization of the powders is achieved by X-ray diffraction (XRD), scanning electron microscopy, infrared (IR) spectrometry, thermogravimetry and calorimetry. Homogeneity of grain size and chemical composition is reached if the initial oxides have similar grain size.

New Ceramics for the Information Storage: Nanoparticles of Titanium Ferrites. Influence of Oxidation and Reduction Reactions upon the Coercivity

1997

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 …