Enhanced multiwavelength holographic profilometry by laser mode selection

A method for improving the accuracy of surface shape measurement by multiwavelength holography is presented. In our holographic setup, a Bi12TiO20 photorefractive crystal was the holographic recording medium, and a multimode diode laser emitting in the red region was the light source in a two-wave mixing scheme. on employing such lasers the resulting holographic image appears covered with interference fringes corresponding to the object relief, and the interferogram spatial frequency is proportional to the diode laser's free spectral range (FSR). Our method consists in increasing the effective free spectral range of the laser by positioning a Fabry-Perot etalon at the laser output for mode selection. As larger effective values of the laser FSR were achieved, higher-spatial-frequency interferograms were obtained and therefore more sensitive and accurate measurements were performed. The quantitative evaluation of the interferograms was made through the phase-stepping technique, and the phase map unwrapping was carried out through the cellular-automata method. For a given surface, shape measurements with different interferogram spatial frequencies were performed and compared with respect to measurement noise and visual inspection. (c) 2007 Society of Photo-Optical Instrumentation Engineers.

XPS investigation of plasma-deposited polysiloxane films irradiated with helium ions

This work describes an XPS investigation of plasma-deposited polysiloxane films irradiated with 170 keV He+ ions at fluences, Phi, ranging from 1 x 10(14) to 1 x 10(16) cm(-2). Modifications in the atomic concentrations of the surface atoms with (D were revealed by changes in the [O]/[Si], [O]/[C] and [C]/[Si] atomic ratios. Surface chemical structure modifications were evidenced by the increasing C1s peak width and asymmetry as Phi was increased, due to the formation of ether and carboxyl functionalities. Moreover, structural transformations were indicated by the positive binding energy shift of the Si2p peaks, due to the increasing Si oxidation. Correlations of the XPS data with other results from previous work on polysiloxanes illustrate the role of ion beam-induced bond breaking on the structural modifications.

Electrochemical oxidation of methanol on Pt nanoparticles dispersed on RuO2

Pt-modified RuO2 was prepared by a sol-gel procedure on titanium substrates in the form of thin films of similar to2-mum thickness. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses showed that these films actually consist of Pt nanoparticles dispersed in RuO2 and that neither metallic Ru nor Pt-Ru alloy are present on the surface. Electrodes with different Pt:Ru nominal compositions were prepared and their electrocatalytic activity for the oxidation of methanol was investigated by potential sweeps and chronoamperometry. The results obtained show an enhancement effect for methanol oxidation that can be interpreted as associated to the formation of hydrous oxides on the RuO2 surface.

Oxygen stoichiometry effects in spinel-type NiMn2O4-delta samples

We report the effects of oxygen stoichiometry in the structure and magnetic response of spinel-type NiMn2O4-delta polycrystalline samples controlled by heat-treatments in different atmospheric conditions.The post-annealed samples were analyzed by Scanning Electron Microscopy associated to X-ray Energy Dispersion Spectrometry, X-ray Photoelectron Spectroscopy and AC/DC magnetic measurements.Results indicate that the oxygen stoichiometry highly influences the magnetic interactions between the ferromagnetic, and antiferromagnetic sublattices in these compounds due to the presence of manganese in three possible valence states. (c) 2005 Elsevier Ltd. All rights reserved.

Electrosprayed superhydrophobic PTFE: a non-contaminating surface

This paper reports on the exposure of superhydrophobic polytetrafluoroethylene ( PTFE) coatings to common aqueous solutions which are used in biology, biotechnology and chemical sensor applications. Advancing contact angles as high as 173 degrees for aqueous solutions were measured on the PTFE surface. Water drop sliding angles at 2 degrees show a very low contact angle hysteresis. X-ray photoelectron spectroscopy measurements confirm that aqueous solutions can move or stay on the superhydrophobic surface without contamination. Owing to the chemical inertness of the polymer, these results indicate that superhydrophobic PTFE can be used in lab-on-a-chip and multi-sensor devices as well as in biological cultures, where aqueous solutions meet solid surfaces, without contaminating the interface.

Sol-gel prepared Pt-modified oxide layers: Synthesis, characterization, and electrocatalytic activity

Thin films of pure RuO2 and IrO2 and mixed Ru0.5Ir0.5O2 oxide modified with Pt particles were prepared by a sol-gel method in the form of thin films of similar to 2 mu m thickness on Ti substrates. Surface morphology of these Pt- modified oxides was examined by scanning electron microscopy and was found to exhibit a significant influence of the chemical composition of the oxide matrix. Element mapping showed homogeneous distribution of the metals. X- ray diffraction and X- ray photoelectron spectroscopy analyses showed that these films consist of metallic Pt particles dispersed in an oxide matrix. Cyclic voltammetry in acid solutions showed that the sol- gel prepared layers have relatively high Pt surface areas. The electrocatalytic activity of these materials toward the anodic oxidation of formaldehyde and methanol was compared in terms of onset potential and current density and was found to follow the sequence: Pt- Ru0.5Ir0.5O2/ Ti > Pt- RuO2/ Ti > Pt- IrO2/ Ti.

Study on the initial stages of water corrosion of fluorozirconate glasses

The surface corrosion process associated with the hydrolysis of fluorozirconate glass, ZBLAN (53ZrF(4), 20BaF(2), 20NaF, 4LaF(2), 3AlF(3)) was investigated using X-ray photoelectron spectroscopy (XPS), grazing-incidence small angle X-ray scattering (GISAXS), X-ray reflectivity (XRR) and scanning electron microscopy (SEM). After a short exposure period (25 min) of the glass surface to deionized water the XPS data indicate an increase of the oxygen content accompanied by a decrease of fluorine concentration. The analysis of the chemical bonding structure identified the predominant surface reaction products as zirconium hydroxyfluoride and oxyfluoride species. The second most abundant glass component, bariumfluoride, remains almost unaffected by oxygen, while sodium fluoride is completely removed from the attacked surface region. The detected structural and compositional changes are related to the selective dissolution of the glass components leading to the formation of a new surface phase. This process is accompanied by a visible surface roughening caused by reprecipitated species, observed by SEM. The modification of the glass surface is responsible for an increase of the GISAXS intensity. The scattering was attributed to nanovoids formed at the surface region of the glass with an average size of 2.4 +/- 0.05 nm. (C) 2004 Elsevier B.V. All rights reserved.

Holographic recording in [Sb(Po-3)(3)](n)-Sb2O3 glassy films by photoinduced volume and refraction index changes

Glassy films of 0.2[Sb(PO3)(3)]-0,8Sb(2)O(3) with 0.8 mum-thickness were deposited on quartz substrates by electron beam evaporation. A contraction in the film thickness (photoinduced decrease in volume) and photobleaching effect associated with a decrease of up to 25% in the index of refraction has been observed in the films after irradiation near the bandgap (3.89 eV), using the 350.7 nm (3.54 eV) Kr+ ion laser line with 2.5 W/cm(2) for 30 min. A loss of 30% in the phosphorus concentration was measured by wavelength dispersive X-ray microanalysis in the film after laser irradiation with 5.0 W/cm(2) for 1.0 h. These photoinduced changes in the samples are dependent on the power density and intensity profile of the laser beam. Using a Lloyd's mirror setup for continuous wave holography it was possible to record holographic gratings with period from 500 nm up to 20 mum and depth profile of similar to50 nm in the films after laser irradiation with 5.0 W/cm(2) for 1 h. Real-time diffraction efficiency measurements have shown that ultraviolet irradiation induces first a refractive index grating formation, and after this, the photocon traction effect takes place generating an irreversible relief grating. Diffraction efficiency up to 10% was achieved for the recorded gratings. 3D-refraction index measurements and atomic force microscopy images are presented. (C) 2004 Elsevier B.V. All rights reserved.

Progress on holographic techniques to measure real-time phase and amplitude gratings in photosensitive materials

In this paper we present and demonstrate a technique that allows simultaneous and independent measurement of small changes in the refractive index and the absorption coefficient produced in photosensitive materials during holographic exposure. The technique is based on the synchronous detection of two-wave mixing signals in both directions of the transmitted interfering beams. By processing both signals it is possible to separate the diffraction contributions of the refractive index from the absorption coefficient and simultaneously stabilize the incident fringe pattern. The demonstration of this technique is undertaken by following the temporal evolution of the phase and amplitude modulations in photoresist films. To check the ability of the technique to perform numeric evaluations, for a positive photoresist the changes in the optical constants were measured and compared with those obtained using independent methods.

Nanostructure and properties of ZnO films produced by the pyrosol process

Indium doped ZnO films were deposited by the pyrosol process on glass substrates at different temperatures from solutions containing In/Zn molar ratios up to 10%. The nanostructure of the films was investigated using grazing-incidence small angle X-ray scattering (GISAXS). The mass density was determined by X-ray reflectivity and the composition by X-ray photoelectron spectroscopy. The GISAXS measurements revealed an anisotropic pattern for films deposited at 573 and 623 K and a isotropic one for those deposited at higher temperatures. The anisotropic patterns indicate the presence of elongated nanopores with their long axes perpendicular to the film surface. In contrast, the isotropic nature of GISAXS patterns of films grown at high temperatures (673 and 723 K) suggests the presence of spherical voids. The pore size distribution function determined from the isotropic patterns indicates a multimodal size distribution. on the other hand, the measured mass density of the doped films with isotropic nanotexture is higher than that of the anisotropic films while the electric resistivity is significantly lower. This is in agreement with the detected strong reduction of the void density and specific surface area at approximately constant pore size.

Photo-induced effects in Ge25Ga10S65 glasses studied by XPS and XAS

The present paper focuses on the structural, electronic, and compositional properties of Ge25Ga10S65 glasses before and after UV illumination in air using X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS) techniques. The XPS Ge 3d spectra reveal the existence of Ge-O bonds in the surface region of illuminated glass. In the case of this sample, XAS O K-edge spectra showed the formation of an enriched region of oxygen atoms in the glass bulk, indicating a different bonding structure of oxygen at the surface and in the bulk of the glass. Moreover, the structural changes that occur after UV illumination in the glass sample are identified as the formation of a homogeneous germanium oxide surface layer followed by an intermediary Ge25Ga10S65-yOz subsurface region. (c) 2005 Elsevier B.V. All rights reserved.

Improvement of the chemical resistance of zirconium fluoride glasses coated with a Tiron (R) modified tin oxide layer prepared by the sol-gel process

In order to improve the chemical resistance of zirconium fluoride glass a protective transparent SnO2 layer was deposited by the solgel dip-coating process in the presence of Tiron (R) as particle surface modifier agent. After water immersion for different periods of time, both coated and non-coated fluoride glasses were analyzed by scanning electron microscopy, mass loss evaluation, infrared spectroscopy and X-ray photoelectron spectroscopy. In contrast to the effects occurring for non-coated glass, where the surface undergoes a rapid selective dissolution of the most soluble species, the results for the SnO2-coated glass showed that the filling of the film nanopores by dissolved glass material results in a hermetic barrier protecting the glass surface. The selective glass dissolution was confirmed by liquid chromatography measurements of the etching solution after each exposure time. (c) 2006 Elsevier B.V. All rights reserved.

Composition and electronic structure of Zn7-xMxSb2O12 (M = Ni and Co) spinel compounds

The relation between the composition and electronic structure of the perfectly inverse spinel compound Zn7-xMxSb2O12 (M = Ni and Co) has been studied by powder X-ray diffraction and X-ray photoelectron spectroscopy. Changes in the site occupancy are associated with shifts in the core levels as observed in the core level spectral analyses. The configuration of the density of states in the valence band due to the Co and Ni states can be observed in the valence band spectra. (C) 2004 Elsevier B.V. All rights reserved.

Anodic oxidation of formaldehyde on Pt-modified SnO2 thin film electrodes prepared by a sol-gel method

Pt-modified SnO2 electrodes were prepared onto titanium substrates in the form of thin films of similar to2 mum at different temperatures in the range from 200 to 400degreesC. Surface morphology was examined by scanning electron microscopy (SEM). It was found that Pt-SnO2 sol-gel layers are significantly rough and have a low porosity. X-ray diffraction (XRD) studies showed that the films consist of Pt nanoparticles with average size varying from about 5 to 10 nm, depending on the preparation temperature, and amorphous tin oxide. X-ray photoelectron spectroscopy (XPS) was employed to determine the superficial composition of the electrodes and demonstrated the presence of Sn4+ in all the samples. XPS spectra of the Pt 4f electrons showed the presence of Pt in the zero-valence state as well as in ionic forms. The general electrochemical behavior was characterized by cyclic voltammetry in 1 mol l(-1) HClO4 and the electrocatalytic activity towards the oxidation of formaldehyde was investigated by potential sweeps and chronoamperometry. The results obtained show that the Pt-SnO2/Ti system exhibits a significant catalytic activity for the oxidation of formaldehyde, with an onset potential below 0.1 V. (C) 2004 Elsevier Ltd. All rights reserved.

Ferroelectric characteristics of BiFeO3 thin films prepared via a simple chemical solution deposition

BiFeO3 (BFO) thin films were fabricated on Pt(111)/Ti/SiO2/Si substrates by using a polymeric precursor solution under appropriate crystallization conditions. The capacitance dependence on voltage is strongly nonlinear, confirming the ferroelectric properties of the films resulting from the domain switching. The leakage current density increases with annealing temperature. The polarization electric field curves could be obtained in BFO films annealed at 500 degrees C, free of secondary phases. X-ray photoelectron spectroscopy spectra of films annealed at 500 degrees C indicated that the oxidation state of Fe was purely 3+, demonstrating that our films possess stable chemical configurations. (c) 2007 American Institute of Physics.