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CO and VOCs oxidation over Pt/SiO2 catalysts prepared using silicas obtained from stainless steel slags

Dominguez, MI; Barrio, I; Sanchez, M; Centeno, MA; Montes, M; Odriozola, JA
Catalysis Today, 133 (2008) 467-474


Stainless steels slags are mainly composed of low specific surface area calcium silicates together with a variable amount of metallic cations dispersed in such silicate matrix. These silicates due to their heavy metals content have to be considered as hazardous wastes that cannot be reclaimed easily. An alternative to reclamation is the production of valuable materials designed to accomplish processes without economic profit as the abatement of VOCs. In this paper we describe a method for obtaining high specific surface area (up to 290 m(2) g(-1)) metal-doped SiO2 and SiO2/ Al2O3 supports for catalytic applications using as raw materials stainless steel slags. The acid digestion of these slags followed by a hydrothermal treatment results in transition metal oxides doped silicas and silica-aluminas that are used as support for platinum catalysts. The prepared catalysts are active in the total oxidation of CO and toluene, showing comparable activities to those shown by Pt catalysts supported on commercial SiO2.(

April, 2008 | DOI: 10.1016/j.cattod.2007.11.033

Degradation of gold and false golds used as gildings in the cultural heritage of Andalusia, Spain

Duran, A; Perez-Rodriguez, JL; de Haro, MCJ; Herrera, LK
Journal of Cultural Heritage, 9 (2008) 184-188


The causes and degree of alteration of metals such as gold, tin, silver and bronze powders from ornamental implements of Andalusia Cultural Heritage have been studied. The unaltered gold is lost due to the alteration of the material used to adhere the leaf gold on the ceramic. Tin is transformed to romarchite and is lost due to a similar alteration as with the gold leaf adhesive. Silver is altered to Ag2S due to environmental contamination. Part of the bronze powders and silver used in Huercal-Overa altarpiece are altered to atacamite and AgCl, respectively, due to an unsuitable cleaning process.

April, 2008 | DOI: 10.1016/j.culher.2007.10.005

Modification of the photocatalytic activity of Pd/TiO2 and Zn/TiO2 systems through different oxidative and reductive calcination treatments

Aramendia, MA; Borau, V; Colmenares, JC; Marinas, A; Marinas, JM; Navio, JA; Urbano, FJ
Applied Catalysis B-Environmental, 80 (2020) 88-97


Two different solids consisting of Pd or Zn-containing titania systems (metal/titanium nominal ratio of 1%) were submitted to diverse oxidative and reductive calcination treatments and tested for gas-phase selective photooxidation of 2-propanol. As regards the Pd system, reduction at low temperature (<= 500 degrees) resulted in a gradual increase in catalytic activity which was ascribed to the gradual reduction of bulk palladium to Pd-0. Thermal treatment of the system at high temperature (850 degrees C) in static air, air flow or hydrogen flow led to a decrease in activity as the result of the sharp decrease in surface area. Nevertheless, those systems containing Pd-0 only were more active than the one consisting of Pd + PdO. Finally, Pd-system overcame I'd migration to the surface on reduction at 850 degrees C which resulted in a significant increase in selectivity to acetone up to 97% for a time on stream of 5 h. As regards the Zn-containing system, none of the applied treatments resulted in improvement in photocatalytic activity. It seems that the most favourable situation for photocatalysis is that on which Zn atoms are substituting titanium ones in the lattice, whereas segregation of Zn to form small ZnO clusters is especially detrimental to activity.

April, 2008 | DOI: 10.1016/j.apcatb.2007.11.017

The effect of ultrasound in the synthesis of clays used as catalysts in oxidation reactions

Perez, A; Centeno, MA; Odriozola, JA; Molina, R; Moreno, S
Catalysis Today, 133 (2020) 526-529


The effect of ultrasound in the modification of a Colombian bentonite pillared with mixed solutions of Al-Ce and Al-Ce-Fe was obtained. The solids were characterized by means of X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. The catalysts were very efficient in the phenol oxidation reaction in diluted aqueous medium under mild experimental conditions (298 K and atmospheric pressure) and in the CO oxidation reaction. The use of ultrasound showed a clear effect in the synthesis of this type of solids allowing to make their synthesis in a shorter period of time and conserving the physical-chemical characteristics as well as catalytic activity in the oxidation reactions. 

April, 2008 | DOI: 10.1016/j.cattod.2007.12.129

Surface plasmon resonance and magnetism of thiol-capped gold nanoparticles

Guerrero, E.; Munoz-Marquez, M. A.; Garcia, M. A.; Crespo, P.; Fernandez-Pinel, E.; Hernando, A.; Fernandez, A.
Nanotechnology, 19 (2008) 17501


Surface plasmon resonance measurements and magnetic characterization studies have been carried out for two types of thiol-capped gold nanoparticles (NPs) with similar diameters between 2.0 and 2.5 nm and different organic molecules linked to the sulfur atom: dodecanethiol and tiopronin. In addition, Au NPs capped with tetraoctyl ammonium bromide have also been included in the investigation since such capping molecules weakly interact with the gold surface atoms and, therefore, this system can be used as a model for naked gold NPs; such particles presented a bimodal size distribution with diameters around 1.5 and 5 nm. The plasmon resonance is non-existent for tiopronin-capped NPs, whereas a trace of such a feature is observed for NPs covered with dodecanethiol molecules and a bulk-like feature is measured for NPs capped with tetralkyl ammonium salts. These differences would indicate that the modification of the surface electronic structure of the Au NPs depends on the geometry and self-assembling capabilities of the capping molecules and on the electric charge transferred between Au and S atoms. Regarding the magnetization, dodecanethiol-capped NPs have a ferromagnetic-like behaviour, while the NPs capped with tiopronin exhibit a paramagnetic behaviour and tetralkyl ammonium-protected NPs are diamagnetic across the studied temperature range; straight chains with a well-defined symmetry axis can induce orbital momentum on surface electrons close to the binding atoms. The orbital momentum not only contributes to the magnetization but also to the local anisotropy, giving rise to permanent magnetism. Due to the domain structure of the adsorbed molecules, orbital momentum is not induced for tiopronin-capped NPs and the charge transfer only induces a paramagnetic spin component.

April, 2008 | DOI: 10.1088/0957-4484/19/17/175701

Phase composition-dependent physical and mechanical properties of YbxZr1-xO2-x/2 solid solutions

Hartmanova, M; Kubel, F; Bursikova, V; Lomonova, EE; Holgado, JP; Navratil, V; Navratil, K; Kundracik, F
Journal of Physics and Chemistry of Solids, 69 (2008) 805-814


The paper represents a detailed insight into the correlation between changes of the phase composition of crystalline YbxZr1-xO2-x/2 solid solutions and their structural, electrical, mechanical and optical properties. Particularly, the effect of the crystal growth conditions and stabilizer amount in the range of 1.5-13.8 mol% of Yb2O3 are studied in terms of Rietveld analysis of powder X-ray diffraction data, electrical conductivity measured by impedance spectroscopy, absorption coefficient and refractive index measurements, Vickers microhardness (classical technique) as well as the plastic microhardness and effective elastic modulus (DSI-depth-sensing indentation technique). Potential applications of the investigated systems Lire discussed in view of the results obtained.

April, 2008 | DOI: 10.1016/j.jpcs.2007.09.002

Self-assembled polyhydroxy fatty acids vesicles: a mechanism for plant cutin synthesis

Heredia-Guerrero, JA; Benitez, JJ; Heredia, A
Bioessays, 30 (2008) 273-277


Despite its biological importance, the mechanism of formation of cutin, the polymeric matrix of plant cuticles, has not yet been fully clarified. Here, for the first time, we show the participation in the process of lipid vesicles formed by the self-assembly of endogenous polyhydroxy fatty acids. The accumulation and fusion of these vesicles (cutinsomes) at the outer part of epidermal cell wall is proposed as the mechanism for early cuticle formation.

March, 2008 | DOI: 10.1002/bies.20716

Relation between growth dynamics and the spatial distribution of intrinsic defects in self-assembled colloidal crystal films

Lozano, G; Miguez, H
Applied Physics Letters, 92 (2008) 091904


Herein we establish a clear relation between the parameters that govern the growth dynamics and the structural quality of colloidal crystal films. We report an optical analysis of the spatial distribution of intrinsic defects in colloidal crystal films and correlate our results with a theoretical model describing the growth dynamics of such lattices. We find that the amount of defects fluctuates periodically and decreases along the growth direction of the lattice. We demonstrate that these spatial variations are a direct consequence of the temporal oscillations of the crystal film formation velocity, which are inherent to the colloidal particle deposition process.

March, 2008 | DOI: 10.1063/1.2883943

A universal curve for the magnetocaloric effect: an analysis based on scaling relations

Colodrero, Silvia; Ocana, Manuel; Miguez, Hernan
Langmuir, 24, (2008) 4430–4434


Herein we present a fast, reliable method for building nanoparticle-based 1D photonic crystals in which a periodic modulation of the refractive index is built by alternating different types of nanoparticles and by controlling the level of porosity of each layer. The versatility of the method is further confirmed by building up optically doped photonic crystals in which the opening of transmission windows due to the creation of defect states in the gap is demonstrated. The potential of this new type of structure as a sensing material is illustrated by analyzing the specific color changes induced by the infiltration of solvents of different refractive indexes.

March, 2008 | DOI: 10.1021/la703987r

Nanostructured Ti-M mixed-metal oxides: Toward a visible light-driven photocatalyst

Kubacka, A.; Fernandez-Garcia, M.; Colon, G.
Journal of Catalysis, 254 (2008) 272-284


In this report we investigate the structure-activity relationship in Ti-M (M = V, Mo, Nb, W) mixed-metal oxides with anatase structure used for the photoelimination of toluene under sunlight-type excitation. These systems were prepared by a microemulsion method, and their physicochemical properties were characterized by a multitechnique approach using X-ray diffraction-Rietveld, photoelectron spectroscopy, and Raman and UV-visible spectroscopy. The preparation method allowed the incorporation of up to around 20 at % of Mo, Nb, and W, whereas a significantly inferior solubility limit, below 5 at % was observed for V. The presence of nonpunctual defects, intimately related to the existence of MOx clustering, produced electronic mid-gap states involved in charge recombination and appeared to be the most negative factor influencing photoactivity. The maximization of photoactivity occurred for Ti-M samples with the highest doing level, together with a minimum structural disturbance of the anatase-type structure. The physicochemical bases for the photoactivity behavior of the Ti-M samples as function of the M content and, in particular, the presence of partial (for a specific Ti-M series) or global maxima are discussed. 

March, 2008 | DOI: 10.1016/j.jcat.2008.01.005

Sorption properties of mesoporous multilayer thin films

Fuertes, MC; Colodrero, S; Lozano, G; Gonzalez-Elipe, AR; Grosso, D; Boissiere, C; Sanchez, C; Soler-Illia, GJDAA; Miguez, H
Journal of Physical Chemistry C, 112 (2008) 3157-3163


The vapor sorption properties of multilayers made of ordered mesoporous thin films with tailored composition and mesostructure are herein investigated. Optical reflectance measurements versus partial pressure of several vapors are performed to analyze the interplay between the affinity to and the accessibility of the different types of layers in the structure. We find that the behavior of a mesoporous oxide layer within the multilayer largely differs from that of the isolated thin film, its sorption properties being determined by the interaction with neighboring films. An explanation of the phenomena observed in these complex systems is provided in terms of the pore size, the affinity of each type of layer to specific compounds, and the effect of neighboring layers in the sorption properties of bilayers by an independent environmental ellipsometric study.

March, 2008 | DOI: 10.1021/jp710612y

Preparation of Au-CeO2 and Au-Al2O3/AISI 304 austenitic stainless steel monoliths and their performance in the catalytic oxidation of CO

Martinez, LM; Frias, DM; Centeno, MA; Paul, A; Montes, M; Odriozola, JA
Chemical Engineering Journal, 136 (2008) 390-397


The use of austenitic stainless steel (AISI 304) as metallic substrate for monolithic catalytic devices is explored in this work as well as an alternative procedure to the washcoating of Al2O3 and CeO2 supported Au catalysts. Thermal treatment of the metallic surface ensured a good adherence of the catalysts. Some preparation parameters, like the number of dipping and drying steps, were controlled in order to obtain an homogeneous and adherent layer of catalyst. The resulting surfaces were characterized by X-ray diffraction (XRD), N-2 Sorption and scanning electron microscopy (SEM), and were tested in the CO oxidation reaction. The highest conversion to CO2 was obtained with the monolith coated with 1% Au-CeO2 in the presence of water.

March, 2008 | DOI: 10.1016/j.cej.2007.05.040

Reaction-formation mechanisms and microstructure evolution of biomorphic SiC

Varela-Feria, FM; Ramirez-Rico, J; de Arellano-Lopez, AR; Martinez-Fernandez, J; Singh, M
Journal of Materials Science, 43 (2008) 933-941


Biomorphic SiC is fabricated by liquid Si infiltration of a carbon preform obtained from pyrolized wood that can be selected for tailored properties. The microstructure and reaction kinetics of biomorphic SiC have been investigated by means of TEM, SEM, EBSD, and partial infiltration experiments. The microstructure of the material consists of SiC and Si and a small fraction of unreacted C. The SiC follows a bimodal size distribution of grains in the micrometer and the nanometer range with no preferential orientation. The infiltration-reaction constant has been determined as 18 x 10(-3) s(-1). These observations suggest that the main mechanism for SiC formation is solution-precipitation in the first stage of growth. If the pores in the wood are small enough they can be choked by SiC grains that act as a diffusion barrier between Si and C. If that is the case, Si will diffuse through SiC forming SiC grains in the nanometer range.

February, 2008 | DOI: 10.1007/s10853-007-2207-4

Getting more out of X2T2O7 compounds with thortveltite structure: The bond-valence model

Alba, MD; Becerro, AI; Chain, P; Escudero, A; Gonzalez-Carrascosa, T
Journal of Solid State Chemistry, 181 (2008) 340-344


C-M2Si2O7 (M = RE and In) and crystals of composition X2T2O7 (T = P, As, Ge) with ionic radius of X less than 0.97 angstrom (X = Ni, Cd, Mg, Zn, Cu, Ca) are isostructural with the natural-occurring mineral thortveitite. In those compounds, the T-O bridging distance values vary considerably and there is no explanation to this fact in the literature. This paper will bring their structural characteristics out by the bond-valence model. It has been concluded that T-O bridging distance and mean T-O distance are linearly correlated to the total atomic valence of the bridging oxygen and the T atom (T = Si, P, As, Ge), respectively, and they are a function of the principal quantum number (n) in the valence shell of the atom T. Finally, we have applied successfully the model for the prediction of Ge-O distances of (In,A)(2)Ge2O7 (A = Fe,Y,Gd) compounds. 

February, 2008 | DOI: 10.1016/j.jssc.2007.11.027

Interface effects in the Ni 2p x-ray photoelectron spectra of NiO thin films grown on oxide substrates

Preda, I; Gutierrez, A; Abbate, M; Yubero, F; Mendez, J; Alvarez, L; Soriano, L
Physical Review B, 77 (2008) 075411


We report the Ni 2p x-ray photoelectron spectra of NiO thin films grown on different oxide substrates, namely, SiO2, Al2O3, and MgO. The main line of the Ni 2p spectra is attributed to the bulk component, and the shoulder at 1.5 eV higher binding energies to the surface component. The spectra of the NiO thin films show strong differences with respect to that of bulk NiO. The energy separation between the main peak and the shoulder increases with the substrate covalence. This indicates the strong covalent interactions between the NiO thin films and the oxide substrates, and reflects changes in the bonding at the interface from a more ionic to a more covalent interaction. These conclusions are supported by cluster model calculations with a reduced O 2p-Ni 3d hybridization.

February, 2008 | DOI: 10.1103/PhysRevB.77.075411

Carbothermal synthesis of silicon nitride(Si3N4): Kinetics and diffusion mechanism

Ortega, A.; Alcala, M. D.; Real, C.
Journmal of Materials Processing Technology, 195 (2008) 224-231


Sample controlled reaction temperature (SCRT) has been used for the first time to study the kinetics of the carbothermal reduction of silica in nitrogen to obtain silicon nitride (Si3N4). It is noteworthy to point out that SCRT method allows both a good control of pressure in the sample surroundings and the use of reaction rates low enough to keep temperature gradients at a negligible level to avoid any heat or mass transfer phenomena. It has been shown that the carbothermal synthesis of silicon nitride is best described by a two-dimensional diffusion kinetic model with an activation energy of about 306 kJ/mol. Effects of experimental parameters on the activation energy has been investigated. By using SCRT it has been possible to obtain ceramic powder with a determined phase composition and a controlled microstructure. 

January, 2008 | DOI: 10.1016/j.jmatprotec.2007.05.004

Influence of amine template on the photoactivity of TiO2 nanoparticles obtained by hydrothermal treatment

Colon, G; Hidalgo, MC; Navio, JA; Melian, EP; Diaz, OG; Dona, JM
Applied Catalysis B-Environmental, 78 (2008) 176-182


TiO2 nanoparticles have been prepared by amine template-assisted sol-gel precipitation and further hydrothermal treatment. We have investigated the effect of different amines (hydrazine and triethylamine) in the final surface and structural properties. It has been stated that the different amounts of amine could act as an interesting template upon hydrothermal treatment. Further thermal treatment also leads to a significant improvement in the photocatalytic properties of the studied systems. Surface and morphological features notably differ from TiO2 prepared using different synthetic routes. Wide surface and structural characterization of the samples have been carried out, and correlations with precipitation pH are pointed out from this characterization. In all cases, amine template TiO2 obtained exhibit high conversion values for phenol photo-oxidation reaction. Further calcination treatment of all the studied systems clearly leads to photocatalytic conversions higher than that exhibited by TiO2 Degussa P25. 

January, 2008 | DOI: 10.1016/j.apcatb.2007.09.019

Thermal Behavior of Ground Talc Mineral

Balek, V; Subrt, J; Perez-Maqueda, LA; Benes, M; Bountseva, IM; Beckman, IN; Perez-Rodriguez, JL
Journal of Mining and Metallurgy Section B-Metallurgy, 44 (2008) 7-17


Microstructure development and thermal behavior of ground talc mineral samples (from locality Puebla de Lillo,Spain) was characterized by X-ray diffraction, scanning electron microscopy(SEM),surface area measurements differential thermal analysis, thermogravimetry and emanation thermal analysis (ETA). A vibratory mill and grinding time 5 min. was used to prepare the ground talc sample. It was found that grinding caused an increase in the surface area of the natural talc from 3 m(2)g(-1) to 110 m(2) g(-1). A decrease of particle size after sample grinding was observed by SEM. The increase of structure disorder of the ground sample and the crystallite size reduction from 40 to 10 nm were determined from the XRD results. ETA results revealed a closing up of surface micro-cracks and healing of microstructure irregularities on heating in the range 200 - 500 degrees C of both un-ground and ground talc samples. For the ground talc sample a crystallization of non-crystalline phase into orthorhombic enstatite was characterized as by a decrease of radon mobility in the range 785-825 degrees C and by a DTA exothermal effect with the maximum at 830 degrees C. ETA results were used for the assessment of transport properties of the talc samples on heating.

January, 2008 | DOI: 10.2298/JMMB0801007B

Syntesis by reactive grinding of molibdenum iron bimetallic nitride

Roldan, MA; Ortega, A; Palencia, I; Real, C
Revista de Metalurgia, 44 (2008) 13-18


The transition metal nitride ternary show similar properties to the binary nitride and some times this behaviour are improved. In the present work, the molybdenum-iron nitride has been prepared by reactive grinding from the two metals under nitrogen atmosphere at a pressure of 11 bar. The characterization of the compound is presented and it is also shown a study of the stability of the nitride under several atmospheres.

January, 2008 | DOI:

Spectral Response of Opal-Based Dye-Sensitized Solar Cells

Mihi, A.; Calvo, M. E.; Anta, J. A.; Miguez, H.
Journal of Physical Chemistry C, 112 (2008) 13-17


Herein we present an experimental study of the spectral dependence of the photogenerated current of opal-based solar cells. We analyze the incident photon-to-current conversion efficiency (IPCE) for dye-sensitized solar cells in which colloidal crystals are introduced in different configurations. We prove that a dye-sensitized nanocrystalline titanium oxide electrode moulded in the shape of an inverse opal shows a decrease of efficiency for the spectral region in which a photonic stop band opens up. Contrarily, when a standard thin film of disordered titania nanocrystallites is coupled to an inverse opal, the mirror effect of the photonic crystal at band gap frequencies increases the light harvesting efficiency of the cell and thus the IPCE. This effect is further demonstrated by coupling an inverse opal multilayer to a homogeneous electrode, with two well-defined spectral ranges of increased photogenerated current being detected.

January, 2008 | DOI: 10.1021/jp7105633