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Monitoring the Reaction Mechanism in Model Biogas Reforming by InSitu Transient and Steady-State DRIFTS Measurements

Bobadilla, LF; Garcilaso, V; Centeno, MA; Odriozola, JA
Chemsuschem, 10 (2017) 1193-1201


In this work, the reforming of model biogas was investigated on a Rh/MgAl2O4 catalyst. In situ transient and steady-state diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) measurements were used to gain insight into the reaction mechanism involved in the activation of CH4 and CO2. It was found that the reaction proceeds through of an initial pathway in which methane and CO2 are both dissociated on Rh metallic sites and additionally a bifunctional mechanism in which methane is activated on Rh sites and CO2 is activated on the basic sites of the support surface via a formate intermediate by H-assisted CO2 decomposition. Moreover, this plausible mechanism is able to explain why the observed apparent activation energy of CO2 is much lower than that of CH4. Our results suggest that CO2 dissociation facilitates CH4activation, because the oxygen-adsorbed species formed in the decomposition of CO2 are capable of reacting with the CHx species derived from methane decomposition.

Marzo, 2017 | DOI: 10.1002/cssc.201601379

Large-Scale Storage of Concentrated Solar Power from Industrial Waste

Perejon, Antonio; Valverde, Jose Manuel; Miranda-Pizarro, Juan; Sanchez-Jimenez, Pedro E.; Perez-Maqueda, Luis A.
ACS Sustainable Chemistry & Engineering, 5 (2017) 2265-2272


Deep penetration of renewable energies into the grid relies on the development of large-scale energy storage technologies using cheap, abundant, and nontoxic materials. Concentrated solar power (CSP) is particularly suitable to massively store thermal energy for dispatchable electricity generation. This is currently accomplished in a few demonstration plants by using molten salts albeit in a not competitive way yet. Process simulation studies indicate that thermochemical energy storage of CSP by means of the calcium looping (CaL) technology would reduce the cost of storage and increase the flexibility of energy supply provided that widely available and cheap CaO precursors with high and stable multicycle activity are used. In this work, we investigate the behavior of calcium rich steel slag at CaL conditions that would expectedly maximize the efficiency of CSP energy storage and power production. When treated with acetic acid, this nontoxic widely abundant waste yields a CaO rich solid with stable conversion near 0.8 over successive carbonation/calcination cycles at these CaL conditions

Marzo, 2017 | DOI: 10.1021/acssuschemeng.6b02576

Aperiodic Metal-Dielectric Multilayers as Highly Efficient Sunlight Reflectors

Alberto Jiménez-Solano; Miguel Anaya; Mauricio E. Calvo; Mercedes Alcon-Camas; Carlos Alcañiz; Elena Guillén; Noelia Martínez; Manuel Gallas; Thomas Preussner; Ramón Escobar-Galindo; Hernán Míguez
Advanced Optical Materials, 5 (2017) 1600833


The optimum reflection of the solar spectrum at well-defined incident directions as well as its durability in time are, both, fundamental requirements of the optics of thermosolar and photovoltaic energy conversion systems. The stringent high performance needed for these applications implies that, almost exclusively, second face mirrors based on silver are employed for this purpose. Herein, the possibility to develop solar mirrors using other metals, such as copper and aluminum, is theoretically and experimentally analyzed. It is found that reflectors based on these inexpensive metals are capable of reflecting the full solar spectrum with efficiencies comparable to that of silver-based reflectors. The designs herein proposed are based on aperiodic metal-dielectric multilayers whose optimized configuration is chosen employing a code based on a genetic algorithm that allows selecting the best one among 108 tested reflectors. The use of metals with wider spectral absorption bands is compensated by the use of multilayered designs in which metal absorption is almost suppressed, as the analysis of the electric field intensity distribution demonstrates. The feasibility of the proposed mirrors is demonstrated by their actual fabrication by large area deposition techniques amenable for mass production.

Marzo, 2017 | DOI: 10.1002/adom.201600833

Strong Quantum Confinement and Fast Photoemission Activation in CH3NH3PbI3 Perovskite Nanocrystals Grown within Periodically Mesostructured Films

Miguel Anaya; Andrea Rubino; Teresa Cristina Rojas; Juan Francisco Galisteo-López; Mauricio Ernesto Calvo; Hernán Míguez
Advanced Optical Materials


In this Communication, a synthetic route is demonstrated to obtain stabilized MAPbI3 nanocrystals embedded in thin metal oxide films that display well-defined and adjustable quantum confinement effects over a wide range of 0.34 eV. Mesostructured TiO2 and SiO2 films displaying an ordered 3D pore network are prepared by evaporation-induced self-assembly of a series of organic supramolecular templates in the presence of metal oxide precursors. The pores in the inorganic films obtained after thermal annealing are then used as nanoreactors to synthesize MAPbI3crystallites with narrow size distribution and average radius comprised between 1 and 4 nm, depending on the template of choice. Both the static and dynamic photoemission properties of the ensemble display features distinctive of the regime of strong quantum confinement. Photoemission maps demonstrate that the spectral and intensity properties of the luminescence extracted from the perovskite quantum dot loaded films are homogeneous over squared centimeters areas. At variance with their bulk counterparts, constant emission intensity is reached in time scales at least four orders of magnitude shorter.

Marzo, 2017 | DOI: 10.1002/adom.201601087

Solid lubricant behavior of MoS2 and WSe2-based nanocomposite coatings

Dominguez-Meister, S; Rojas, TC; Brizuela, M; Sanchez-Lopez, JC
Science and Tecnology of Advances Materials, 18 (2017) 1


Tribological coatings made of MoS2 and WSe2 phases and their corresponding combinations with tungsten carbide (WC) were prepared by non-reactive magnetron sputtering of individual targets of similar composition. A comparative tribological analysis of these multiphase coatings was done in both ambient air (30-40% relative humidity, RH) and dry nitrogen (RH<7%) environments using the same tribometer and testing conditions. A nanostructural study using advanced transmission electron microscopy of the initial coatings and examination of the counterfaces after the friction test using different analytical tools helped to elucidate what governs the tribological behavior for each type of environment. This allowed conclusions to be made about the influence of the coating microstructure and composition on the tribological response. The best performance obtained with a WSe x film (specific wear rate of 2 x 10(-8) mm(3) N(-1)m(-1) and a friction coefficient of 0.03-0.05) was compared with that of the well-established MoS2 lubricant material.

Marzo, 2017 | DOI: 10.1080/14686996.2016.1275784

Ceramics of Ta-doping stabilized orthorhombic ZrO2 densified by spark plasma sintering and the effect of post-annealing in air

Sponchia, G; Moshtaghioun, BM; Benedetti, A; Riello, P; Gomez-Garcia, D; Dominguez-Rodriguez, A; Ortiz, AL
Scripta Materialia, 130 (2017) 128-132


16 mol% Ta-doped ZrO2 powders were synthesized and densified by spark-plasma sintering (SPS) in vacuum, followed by post-SPS annealing in air, thus obtaining two ultrafine-grained ceramics consisting of Ta-doping stabilized orthorhombic ZrO2. The as-SPSed ceramic is black because it is actually a suboxide essentially with reduced cations and abundant oxygen vacancies, whereas the post-annealed ceramic is white because it is an oxide without vacancies and with only partially reduced cations. Both ceramics are relatively hard and brittle, but the as-SPSed ceramic was slightly more so, attributable to crystallographic and microstructural differences. Implications of interest for the ceramics community are discussed.

Marzo, 2017 | DOI: 10.1016/j.scriptamat.2016.11.021

Morphology control of uniform CaMoO4 microarchitectures and development of white light emitting phosphors by Ln doping (Ln = Dy3+, Eu3+)

Laguna, Mariano; Nuñez, Nuria O.; Becerro, Ana I.; Ocaña, Manuel
Crystengcomm, 19 (2017) 1590-1600


A very simple synthesis procedure based on precipitation reactions at moderate temperature (120 degrees C) from solutions containing calcium nitrate and sodium molybdate, using mixed solvents (polyols and water) has been developed, which produces uniform tetragonal CaMoO4 microarchitectures with different morphologies (peanuts, cocoons, spindles and spheres) composed of self-assembled entities. The morphology and crystal size of such assemblies could be tuned by a simple change of the nature of the components of the solvent mixture or their volumetric ratio in such a mixture. All particles presented similar excitation and emission spectra arising from a charge transfer process within the MoO4 2-groups. The emitted light presented a bluish-green color and its intensity was higher for the spindle-type particles. This synthesis procedure was also suitable for doping peanut-like CaMoO4 architectures with Eu3+ or Dy3+ cations up to a 1% molar ratio (Ln/Ln + Ca), without altering their morphology or crystalline structure. The so prepared phosphors emitted an intense red (Eu-doped) or greenish (Dy-doped) light when excited through the MoO42- group excitation band, indicating the presence of an energy transfer process from such groups to the Ln(3+) cations. Finally, a white light emitting phosphor with chromaticity coordinates x = 0.335 and y = 0.365 and a correlated color temperature of 5407 K was developed by codoping peanut-type CaMoO4 particles with suitable amounts of Dy3+ (0.35%) and Eu3+ (0.15%) cations, which could find applications in white light emitting diodes.

Marzo, 2017 | DOI: 10.1039/c6ce02611g

Preferential oxidation of CO on a La-Co-Ru perovskite-type oxide catalyst

Pereniguez, R; Caballero, A; Ferri, D
Catalysis Communication, 92 (2017) 75-79


A Ru-containing perovskite-type oxide La(Co,Ru)O3 of nominal composition LaCo0.8Ru0.2O3 was prepared by ultrasonic spray combustion and tested for the preferential oxidation of CO (PROX). EXAFS indicated that Ru adopted the coordination environment of Co in LaCoO3 while Co was present as LaCoO3 and Co3O4. PROX activity was replaced by CO hydrogenation activity above 250 °C. Short oxidation at 500 °C between temperature programmed reaction ramps did not restore the initial La(Co,Ru)O3 structure but generated a catalyst with improved PROX activity compared to the initial La(Co,Ru)O3. Under reductive PROX conditions the material experienced structural changes that improved its overall catalytic activity only if the catalyst was oxidized after each temperature programmed ramp.

Marzo, 2017 | DOI: 10.1016/j.catcom.2016.12.020

A Promising approach to the kinetics of crystallization processes: The sample controlled thermal analysis

Perejon, A; Sanchez-Jimenez, PE; Criado, JM; Perez-Maqueda, LA
Journal of the American Ceramic Society, 100 (2017) 1125-1133


Constant Rate Thermal Analysis (CRTA) method implies controlling the temperature in such a way that the reaction rate is maintained constant all over the process. This method allows determining simultaneously both the kinetic parameters and the kinetic model from a single experiment as the shape of the CRTA -T curves strongly depends on the kinetic model. CRTA method has been developed in the market only for thermogravimetric and thermodilatometric systems and, therefore, its use has been limited until now to the kinetic study of processes involving changes in mass or size of the samples, respectively. To overcome this obstacle, a method has been developed in this work for using the DSC signal for controlling the process rate in such a way that CRTA would be applied to the kinetic analysis of either phase transformations or crystallizations. The advantages of CRTA for performing the kinetics of crystallization processes have been here successfully demonstrated for the first time after selecting the crystallization of zirconia gel as test reaction.

Marzo, 2017 | DOI: 10.1111/jace.14604

Antibacterial response of titanium oxide coatings doped by nitrogen plasma immersion ion implantation

Esparza, J; Fuentes, GF; Bueno, R; Rodriguez, R; Garcia, JA; Vitas, AI; Rico, V; Gonzalez-Elipe, AR
Surface and Coatings Technology, 314 (2017) 67-71


Plasma immersion ion implantation technology has been utilized to enhance the photocatalytic activity of the anatase phase of TiO2 thin films deposited by cathodic arc evaporation PVD. The main objective of this study is to shift the light absorbance of the titania in order to obtain antibacterial activity under visible light irradiation. TiO2 thin films, deposited on polished stainless steel AISI 304 and silicon wafers, were implanted with nitrogen ions (N+/N2+) at 20 kV energy and different temperatures between 250 and 350 °C. The antibacterial activity of nitrogen implanted titania coatings has been monitored for Escherichia coli under visible light irradiation. Additionally ultra violet/visible spectrophotometry tests have been carried out to measure the changes in the light absorbance of the doped films. Further characterization has been performed, including X-ray photoelectron spectroscopy, X-ray diffraction and glow discharge optical emission spectrometry. As a result of Nitrogen implantation, the light absorption peak shifted from ultra violet region (UV-A) to visible wavelength range, which led to an increase of the antibacterial efficacy under visible light irradiation.

Marzo, 2017 | DOI: 10.1016/j.surfcoat.2016.11.002

On the effect of wall slip on the determination of the yield stress of magnetorheological fluids

Caballero-Hernandez, J; Gomez-Ramirez, A; Duran, JDG; Gonzalez-Caballero, F; Zubarev, AY; Lopez-Lopez, MT
Applied Rheology, 27 (2017) 15001 (8 pages)


We study the effect of wall slip on the measured values of the yield stress of magnetorheological (MR) fluids. For this aim we used a rheometer provided with parallel-plate geometries of two types, distinguished by having smooth or rough surfaces. We found that wall slip led to the underestimation of the yield stress when measuring geometries with smooth surfaces were used, and that this underestimation was more pronounced for the static than for the dynamic yield stress. Furthermore, we analysed the effect that both irreversible particle aggregation due to colloidal interactions and reversible magnetic fieldinduced particle aggregation had on the underestimation provoked by wall slip. We found that the higher the degree of aggregation the stronger the underestimation of the yield stress. At low intensity of the applied magnetic field irreversible particle aggregation was dominant and, thus, the underestimation of the yield stress was almost negligible for well-dispersed MR fluids, whereas it was rather pronounced for MR fluids suffering from irreversible aggregation. As the magnetic field was increased the underestimation of the yield stress became significant even for the best dispersed MR fluid.

Marzo, 2017 | DOI: 10.3933/ApplRheol-27-15001

Reliability of new poly (lactic-co-glycolic acid) membranes treated with oxygen plasma plus silicon dioxide layers for pre-prosthetic guided bone regeneration processes

Castillo-Dali, G; Castillo-Oyague, R; Batista-Cruzado, A; Lopez-Santos, C; Rodriguez-Gonzalez-Elipe, A; Saffar, JL; Lynch, CD; Gutierrez-Perez, JL; Torres-Lagares, D
Medicina Oral Patología Oral y Cirugia Oral, 22 (2017) E242-E250


Background: The use of cold plasmas may improve the surface roughness of poly(lactic-co-glycolic) acid (PLGA) membranes, which may stimulate the adhesion of osteogenic mediators and cells, thus accelerating the biodegradation of the barriers. Moreover, the incorporation of metallic-oxide particles to the surface of these membranes may enhance their osteoinductive capacity. Therefore, the aim of this paper was to evaluate the reliability of a new PLGA membrane after being treated with oxygen plasma (PO2) plus silicon dioxide (SiO2) layers for guided bone regeneration (GBR) processes. 
Material and Methods: Circumferential bone defects (diameter: 11 mm; depth: 3 mm) were created on the top of eight experimentation rabbits' skulls and were randomly covered with: (1) PLGA membranes (control), or (2) PLGA/ PO2/SiO2 barriers. The animals were euthanized two months afterwards. A micromorphologic study was then performed using ROI (region of interest) colour analysis. Percentage of new bone formation, length of mineralised bone, concentration of osteoclasts, and intensity of ostheosynthetic activity were assessed and compared with those of the original bone tissue. The Kruskal-Wallis test was applied for between-group com asignificance level of a=0.05 was considered. 
Results: The PLGA/ PO2/SiO2 membranes achieved the significantly highest new bone formation, length of miner-alised bone, concentration of osteoclasts, and ostheosynthetic activity. The percentage of regenerated bone supplied by the new membranes was similar to that of the original bone tissue. Unlike what happened in the control group, PLGA/PO2/SiO2 membranes predominantly showed bone layers in advanced stages of formation. Conclusions: The addition of SiO2 layers to PLGA membranes pre-treated with PO2 improves their bone-regeneration potential. Although further research is necessary to corroborate these conclusions in humans, this could be a promising strategy to rebuild the bone architecture prior to rehabilitate edentulous areas.

Marzo, 2017 | DOI: 10.4317/medoral.21512

High vacuum synthesis and ambient stability of bottom-up graphene nanoribbons

Fairbrother, A; Sanchez-Valencia, JR; Lauber, B; Shorubalko, I; Ruffieux, P; Hintermann, T; Fasel, R
Nanoscale, 9 (2017) 2785-2792


Carbon-based nanomaterials such as graphene are at a crucial point in application development, and their promising potential, which has been demonstrated at the laboratory scale, must be translated to an industrial setting for commercialization. Graphene nanoribbons in particular overcome one limitation of graphene in some electronic applications because they exhibit a sizeable bandgap. However, synthesis of bottom-up graphene nanoribbons is most commonly performed under ultra-high vacuum conditions, which are costly and difficult to maintain in a manufacturing environment. Additionally, little is known about the stability of graphene nanoribbons under ambient conditions or during transfer to technologically relevant substrates and subsequent device processing. This work addresses some of these challenges, first by synthesizing bottom-up graphene nanoribbons under easily obtained high vacuum conditions and identifying water and oxygen as the residual gases responsible for interfering with proper coupling during the polymerization step. And second, by using Raman spectroscopy to probe the stability of nanoribbons during storage under ambient conditions, after transfer to arbitrary substrates, and after fabrication of field-effect transistor devices, which shows structurally intact nanoribbons even several months after synthesis. These findings demonstrate the potential of graphene nanoribbon technologies by addressing some limitations which might arise in their commercialization.

Febrero, 2017 | DOI: 10.1039/C6NR08975E

Cholesterol biosensing with a polydopamine-modified nanostructured platinum electrode prepared by oblique angle physical vacuum deposition

Martin, M; Salazar, P; Alvarez, R; Palmero, A; Lopez-Santos, C; Gonzalez-Mora, JL; Gonzalez-Elipe, AR
Sensors and Actuators B-Chemical, 240 (2017) 37-45


This paper reports a novel cholesterol biosensor based on nanostructured platinum (Pt) thin films prepared by Magnetron Sputtering (MS) in an oblique angle (OAD) configuration. Pt thin films were deposited onto a gold screen-printed electrode and characterized using Rutherford Back Scattering (RBS), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Cyclic Voltammetry (CV), X-ray Photo-electron Spectroscopy (XPS), Atomic Force Microscopy (AFM) and wetting analysis. Our results confirmed that the film is highly porous and formed by tilted nanocolumns, with an inclination of around 40 degrees and a total thickness of 280 nm. XRD and CV analysis confirmed the polycrystalline nature of the Pt thin film. Cholesterol oxidase (ChOx) was covalently immobilized using a bioinspired polymer, polydopamine (PDA), via Schiff base formation and Michael-type addition. After being immobilized, ChOx displayed apparent activation energy of 34.09 kJ mol(-1) and Michaelis constant (K-M) values of 34.09 kJ mol(-1) and 3.65 mM, respectively, confirming the high affinity between ChOx and cholesterol and the excellent ability of the PDA film for immobilizing biological material without degradation. Under optimized working conditions the developed biosensor presented a sensitivity of 14.3 mA M(-1)cm(-2) (R-2:0.999) with a linear range up to 0.5 mM and a limit of detection of 10.5 mu M (S/N= 3). Furthermore, the biosensor exhibited a fast response (<8 s), good anti-interference properties and high stability after relatively long-term storage (2 months). 

Febrero, 2017 | DOI: 10.1016/j.snb.2016.08.092

Comprehensive and Systematic Analysis of the Immunocompatibility of Polyelectrolyte Capsules

Zyuzin, MV; Diez, P; Goldsmith, M; Carregal-Romero, S; Teodosio, C; Rejman, J; Feliu, N; Escudero, A; Almendral, MJ; Linne, U; Peer, D; Fuentes, M; Parak, WJ
Bioconjugate Chemistry, 28 (2017) 556-564


The immunocompability of polyelectrolyte capsules synthesized by layer-by-layer deposition has been investigated. Capsules of different architecture and composed of either non-degradable or biodegradable polymers, with either positively or negatively charged outer surface, and with micrometer size, have been used, and the capsule uptake by different cell lines has been studied and quantified. Immunocompatibility studies were performed with peripheral blood mononuclear cells (PBMCs). Data demonstrate that incubation with capsules, at concentrations relevant for practical applications, did not result in a reduced viability of cells, as it did not show an increased apoptosis. Presence of capsules also did not result in an increased expression of TNF-α, as detected with antibody staining, as well as at mRNA level. It also did not result in increased expression of IL-6, as detected at mRNA level. These results indicate that the polyelectrolyte capsules used in this study are immunocompatible.

Febrero, 2017 | DOI: 10.1021/acs.bioconjchem.6b00657

Preparation of ytterbium substituted BiFeO3 multiferroics by mechanical activation

Gil-Gonzalez, E; Perejon, A; Sanchez-Jimenez, PE; Hayward, MA; Perez-Maqueda, LA
Journal of the European Ceramic Society, 37 (2017) 945-954


Samples in the system Bi1-xYbxFeO3 (0.02 <= x <= 0.07) have for the first time been prepared by mechanical activation followed by sintering. XRD and DSC measurements show that the solubility limit of ytterbium in the R3c Bi1-xYbxFeO3 system is reached at x similar to 0.03. Higher ytterbium contents lead to a two-phase mixture of a main R3c phase of approximate composition Bi0.97Yb0.03FeO3 and ytterbium enriched secondary phases that cannot be readily indexed or quantified due to their small amount. DSC and temperature-dependent XRD showed that while the magnetic ordering temperature, T-N, was unaffected by Yb substitution, the ferroelectric ordering, T-C, declined. Temperature-dependent XRD patterns show that all samples exhibit rhombohedral R3c to orthorrhombic Pnma phase transitions. Diffuse reflectance spectroscopy suggests the potential use of the samples in photocatalytic applications due to their low band gap energy. Impedance spectroscopy and magnetic measurements show that samples are electrically homogenous and highly insulating, exhibiting antiferromagnetic behaviour at room temperature. 

Febrero, 2017 | DOI: 10.1016/j.jeurceramsoc.2016.09.014

Fabrication of black-gold coatings by glancing angle deposition with sputtering

Vitrey, A; Alvarez, R; Palmero, A; Gonzalez, MU; Garcia-Martin, JM
Beilstein Journal of Nanotechnology, 8 (2017) 434–439


The fabrication of black-gold coatings using sputtering is reported here. Glancing angle deposition with a rotating substrate is needed to obtain vertical nanostructures. Enhanced light absorption is obtained in the samples prepared in the ballistic regime with high tilt angles. Under these conditions the diameter distribution of the nanostructures is centered at about 60 nm and the standard deviation is large enough to obtain black-metal behavior in the visible range.

Febrero, 2017 | DOI: 10.3762/bjnano.8.46

Identification of Outer and Inner Nickel Particles in a Mesoporous Support: How the Channels Modify the Reducibility of Ni/SBA-15 Catalysts

Rodriguez-Gomez, A; Caballero, A
Chemnanomat, 3 (2017) 94-97


Two different nickel supported on SBA-15 catalytic systems have been prepared by means of impregnation (Ni/SBA-15-ImU) and deposition-precipitation (Ni/SBA-15-DP) methodologies. Upon calcination, Ni/SBA-15DP presents a well-developed nickel phyllosilicate phase, which after reduction gives rise to a dispersed and homogeneous metallic phase, mainly located inside the 5 nm in diameter mesoporous structure of the support. On the contrary, as evidenced by XRD and a double temperature programmed reduction (TPR) peak, the Ni/SBA-15-ImU catalyst presents two different NiO phases, which after reduction in hydrogen generate nickel particles in a wide range of sizes. In situ XAS and XPS have unambiguously showed that the distinct TPR profiles obtained for each system are related with particles located in and out the mesoporous structure of the SBA-15 channels. The particles inside the porous are more difficult to reduce, clearly showing a kind of confinement effect of the SBA-15 mesostructure, modifying the reducibility of the NiO phase.

Febrero, 2017 | DOI: 10.1002/cnma.201600297

Preparation and Optimization of Fluorescent Thin Films of Rosamine-SiO2/TiO2 Composites for NO2 Sensing

Guillen, MG; Gamez, F; Suarez, B; Queiros, C; Silva, AMG; Barranco, A; Sanchez-Valencia, JR; Pedrosa, JM; Lopes-Costa, T
Materials, 10 (2017) art 124


The incorporation of a prototypical rosamine fluorescent dye from organic solutions into transparent and microstructured columnar TiO2 and SiO2 (MO2) thin films, prepared by evaporation at glancing angles (GAPVD), was evaluated. The aggregation of the adsorbed molecules, the infiltration efficiency and the adsorption kinetics were studied by means of UV-Vis absorption and fluorescence spectroscopies. Specifically, the infiltration equilibrium as well as the kinetic of adsorption of the emitting dye has been described by a Langmuir type adsorption isotherm and a pseudosecond order kinetic model, respectively. The anchoring mechanism of the rosamine to the MO2 matrix has been revealed by specular reflectance Fourier transform infrared spectroscopy and infiltration from aqueous solutions at different pH values. Finally, the sensing performance towards NO2 gas of optimized films has been assessed by following the changes of its fluorescence intensity revealing that the so-selected device exhibited improved sensing response compared to similar hybrid films reported in the literature.

Febrero, 2017 | DOI: 10.3390/ma10020124

Precision and accuracy of stress measurement with a portable X-ray machine using an area detector

Lee, SY; Ling, JJ; Wang, SH; Ramirez-Rico, J
Journal of Applied Crystallography, 50 (2017) 131-144


The use of portable X-ray stress analyzers, which utilize an area detector along with the newly adopted 'cos alpha' or full-ring fitting method, has recently attracted increasing interest. In laboratory conditions, these measurements are fast, convenient and precise because they employ a single-exposure technique that does not require sample rotation. In addition, the effects of grain size and orientation can be evaluated from the Debye ring recorded on the area detector prior to data analysis. The accuracy of the measured stress, however, has been questioned because in most cases just a single reflection is analyzed and the sample-to-detector distances are relatively short. This article presents a comprehensive analysis of the uncertainty associated with a state-of-the-art commercial portable X-ray device. Annealed ferrite reference powders were used to quantify the instrument precision, and the accuracy of the stress measurement was tested by in situ tensile loading on 1018 carbon steel and 6061 aluminium alloy bar samples. The results show that the precision and accuracy are sensitive to the instrument (or sample) tilt angle (0) as well as to the selected hkl reflection of the sample. The instrument, sample and data analysis methods all affect the overall uncertainty, and each contribution is described for this specific portable X-ray system. Finally, on the basis of the conclusions reached, desirable measurement/analysis protocols for accurate stress assessments are also presented.

Febrero, 2017 | DOI: 10.1107/S1600576716018914