Finite element and dimensional analysis algorithm for the prediction of mechanical properties of bulk materials and thin films

In this work, the applicability of a new algorithm for the estimation of mechanical properties from instrumented indentation data was studied for thin films. The applicability was analyzed with the aid of both three-dimensional finite element simulations and experimental indentation tests. The numerical approach allowed studying the effect of the substrate on the estimation of mechanical properties of the film, which was conducted based on the ratio h(max)/l between maximum indentation depth and film thickness. For the experimental analysis, indentation tests were conducted on AISI H13 tool steel specimens, plasma nitrated and coated with TiN thin films. Results have indicated that, for the conditions analyzed in this work, the elastic deformation of the substrate limited the extraction of mechanical properties of the film/substrate system. This limitation occurred even at low h(max)/l ratios and especially for the estimation of the values of yield strength and strain hardening exponent. At indentation depths lower than 4% of the film thickness, the proposed algorithm estimated the mechanical properties of the film with accuracy. Particularly for hardness, precise values were estimated at h(max)/l lower than 0.1, i.e. 10% of film thickness. (C) 2010 Published by Elsevier B.V.

Raman spectroscopy analysis of structural photoinduced changes in GeS(2) + Ga(2)O(3) thin films

Photoexpansion and photobleaching effects have been observed in amorphous GeS(2) + Ga(2)O(3) (GGSO) thin films, when their surfaces were exposed to UV light. The photoinduced changes on the surface of the samples are indications that the structure has been changed as a result of photoexcitation. In this paper, micro-Raman, energy dispersive X-ray analysis (EDX) and backscattering electrons (BSE) microscopy were the techniques used to identify the origin of these effects. Raman spectra revealed that these phenomena are a consequence of the Ge-S bonds` breakdown and the formation of new Ge-O bonds, with an increase of the modes associated with Ge-O-Ge bonds and mixed oxysulphide tetrahedral units (S-Ge-O). The chemical composition measured by EDX and BSE microscopy images indicated that the irradiated area is oxygen rich. So, the present paper provides fundamental insights into the influence of the oxygen within the glass matrix on the considered photoinduced effects. (C) 2010 Elsevier B.V. All rights reserved.

Effect of Mn concentration and atomic structure on the magnetic properties of Ge thin films

This work reports on the magnetic properties of Ge(100-x)Mn(x) (x=0-24 at. %) films prepared by cosputtering a Ge+Mn target and submitted to cumulative thermal annealing treatments up to 500 degrees C. Both as-deposited and annealed films were investigated by means of compositional analysis, Raman scattering spectroscopy, magnetic force microscopy, superconducting quantum interference device magnetometry, and electrical resistivity measurements. All as-deposited films (either pure or containing Mn) exhibit an amorphous structure, which changes to crystalline as the annealing treatments are performed at increasing temperatures. In fact, the magnetic properties of the present Ge(100-x)Mn(x) films are very sensitive to the Mn content and whether their atomic structure is amorphous or crystalline. More specifically: whereas the amorphous Ge(100-x)Mn(x) films (with high x) present a characteristic spin glass behavior at low temperature; after crystallization, the films (with moderate Mn contents) are ferromagnetic at room temperature. Moreover, the magnetic behavior of the films scales with their Mn concentration and tends to be more pronounced after crystallization. Finally, the semiconducting behavior of the films, experienced by previous optical studies, was confirmed through electrical measurements, which also indicate the dependence of the resistivity with the atomic composition of the films. (C) 2010 American Institute of Physics. [doi: 10.1063/1.3520661]

Electro-optically sensitive diamond-like carbon thin films deposited by reactive magnetron sputtering for electronic device applications

The goal of this work is to study and relate electrical and optical properties of diamond-like carbon (DLC) thin films for applications in electronic devices. DLC films were deposited in a reactive RF magnetron sputtering system on p-type silicon and glass substrates. The target was a 99.9999% pure, 6 in. diameter graphite plate and methane was used as processing gas. Eight DLC films were produced for each substrate, varying deposition time, the reactor pressure between 5 mTorr and 10 mTorr while the RF power was applied at 13.56 MHz and varied between 100, 150, 200 and 250W. After deposition, the films were analyzed by I-V and C-V measurements (Cheng et al. (2004) [1]) in order to determine the electric resistivity, photo-current response and dielectric constant, optical transmittance, used to find the optical gap by the Tauc method; and by photoluminescence analysis to determine the photoemission and confirm the optical band gap. These characteristics are compared and the influence of the deposition parameters is discussed. (C) 2011 Published by Elsevier B.V.

Effects of mechanical properties, residual stress and indenter tip geometry on instrumented indentation data in thin films

In this work, an axisymmetric two-dimensional finite element model was developed to simulate instrumented indentation testing of thin ceramic films deposited onto hard steel substrates. The level of film residual stress (sigma(r)), the film elastic modulus (E) and the film work hardening exponent (n) were varied to analyze their effects on indentation data. These numerical results were used to analyze experimental data that were obtained with titanium nitride coated specimens, in which the substrate bias applied during deposition was modified to obtain films with different levels of sigma(r). Good qualitative correlation was obtained when numerical and experimental results were compared, as long as all film properties are considered in the analyses, and not only sigma(r). The numerical analyses were also used to further understand the effect of sigma(r) on the mechanical properties calculated based on instrumented indentation data. In this case, the hardness values obtained based on real or calculated contact areas are similar only when sink-in occurs, i.e. with high n or high ratio VIE, where Y is the yield strength of the film. In an additional analysis, four ratios (R/h(max)) between indenter tip radius and maximum penetration depth were simulated to analyze the combined effects of R and sigma(r) on the indentation load-displacement curves. In this case, or did not significantly affect the load curve exponent, which was affected only by the indenter tip radius. On the other hand, the proportional curvature coefficient was significantly affected by sigma(r) and n. (C) 2010 Elsevier B.V. All rights reserved.

Structural characterization of supported nanocrystalline ZnO thin films prepared by dip-coating

Nanocrystalline ZnO thin films prepared by the sol-gel dip-coating technique were characterized by grazing incidence X-ray diffraction (GIXD), atomic force microscopy (AFM), X-ray reflectivity (XR) and grazing incidence small-angle X-ray scattering (GISAXS). The structures of several thin films subjected to (i) isochronous annealing at 350, 450 and 550 degrees C, and (ii) isothermal annealing at 450 degrees C during different time periods, were characterized. The studied thin films are composed of ZnO nanocrystals as revealed by analysing several GIXD patterns, from which their average sizes were determined. Thin film thickness and roughness were determined from quantitative analyses of AFM images and XR patterns. The analysis of XR patterns also yielded the average density of the studied films. Our GISAXS study indicates that the studied ZnO thin films contain nanopores with an ellipsoidal shape, and flattened along the direction normal to the substrate surface. The thin film annealed at the highest temperature, T = 550 degrees C, exhibits higher density and lower thickness and nanoporosity volume fraction, than those annealed at 350 and 450 degrees C. These results indicate that thermal annealing at the highest temperature (550 degrees C) induces a noticeable compaction effect on the structure of the studied thin films. (C) 2011 Elsevier B.V. All rights reserved.

Er : YAB nanoparticles and vitreous thin films by the polymeric precursor method

The synthesis of Y(0.9)Er(0.1)Al(3)(BO(3))(4) crystalline powders and vitreous thin films were studied. Precursor solutions were obtained using a modified polymeric precursor method using D-sorbitol as complexant agent. The chemical reactions were described. Y(0.)9Er(0.1)Al(3)(BO(3))(4) composition presents good thermal stability with regard to crystallization. The Y(0.9)Er(0.1)Al(3)(BO(3))(4) crystallized phase can be obtained at 1,150 degrees C, in agreement with other authors. Crack- and porosity-free films were obtained with very small grain size and low RMS roughness. The films thickness revealed to be linearly dependent on precursor solution viscosity, being the value of 25 mPa s useful to prepare high-quality amorphous multi-layers (up to similar to 800 nm) at 740 degrees C during 2 h onto silica substrates by spin coating with a gyrset technology.

Photocatalytic degradation of methylene blue by TiO(2)-Cu thin films: Theoretical and experimental study

In this work the effect of doping concentration and depth profile of Cu atoms on the photocatalytic and surface properties of TiO(2) films were studied. TiO(2) films of about 200 nn thickness were deposited on glass substrates on which a thin Cu layer (5 nm) was deposited. The films were annealed during 1 s to 100 degrees C and 400 degrees C, followed by chemical etching of the Cu film. The grazing incidence X-ray fluorescence measurements showed a thermal induced migration of Cu atoms to depths between 7 and 31 nm. The X-ray photoelectron spectroscopy analysis detected the presence of TiO(2), Cu(2)O and Cu(0) phases and an increasing Cu content with the annealing temperature. The change of the surface properties was monitored by the increasing red-shift and absorption of the ultraviolet-visible spectra. Contact angle measurements revealed the formation of a highly hydrophilic surface for the film having a medium Cu concentration. For this sample photocatalytic assays, performed by methylene blue discoloration, show the highest activity. The proposed mechanism of the catalytic effect, taking place on Ti/Cu sites, is supported by results obtained by theoretical calculations. (C) 2010 Elsevier B.V. All rights reserved.

Leakage current, ferroelectric and structural properties in Pb(1-x)Ba(x)TiO(3) thin films prepared by chemical route

Single-phase perovskite structure Pb(1-x)Ba(x)TiO(3) thin films (x = 0.30, 0.50 and 0.70) were deposited on Pt/Ti/SiO(2)/Si substrates by the spin-coating technique. The dielectric study reveals that the thin films undergo a diffuse type ferroelectric phase transition, which shows a broad peak. An increase of the diffusivity degree with the increasing Barium contents was observed, and it was associated to a grain decrease in the studied composition range. The temperature dependence of the phonon frequencies was used to characterize the phase transition temperatures. Raman modes persist above tetragonal to cubic phase transition temperature, although all optical modes should be Raman inactive. The origin of these modes was interpreted in terms of breakdown of the local cubic symmetry by chemical disorder. The absence of a well-defined transition temperature and the presence of broad bands in some interval temperature above FE-PE phase transition temperature Suggested a diffuse type phase transition. This result corroborates the dielectric constant versus temperature data, which showed a broad ferroelectric phase transition in these thin films. The leakage Current density of the PBT thin films was studied at different temperatures and the data follow the Schottky emission model. Through this analysis the Schottky barrier height values 0.75, 0.53 and 0.34 eV were obtained to the PBT70, PBT50 and PBT30 thin films, respectively. (C) 2008 Elsevier Ltd. All rights reserved.

Nanostructured thin films obtained by electrodeposition over a colloidal crystal template: applications in electrochemical devices

Colloidal particles have been used to template the electrosynthesis of several materials, such as semiconductors, metals and alloys. The method allows good control over the thickness of the resulting material by choosing the appropriate charge applied to the system, and it is able to produce high density deposited materials without shrinkage. These materials are a true model of the template structure and, due to the high surface areas obtained, are very promising for use in electrochemical applications. In the present work, the assembly of monodisperse polystyrene templates was conduced over gold, platinum and glassy carbon substrates in order to show the electrodeposition of an oxide, a conducting polymer and a hybrid inorganic-organic material with applications in the supercapacitor and sensor fields. The performances of the resulting nanostructured films have been compared with the analogue bulk material and the results achieved are depicted in this paper.

Structure of disordered gold-polymer thin films using small angle x-ray scattering

We have investigated the structure of disordered gold-polymer thin films using small angle x-ray scattering and compared the results with the predictions of a theoretical model based on two approaches-a structure form factor approach and the generalized Porod law. The films are formed of polymer-embedded gold nanoclusters and were fabricated by very low energy gold ion implantation into polymethylmethacrylate (PMMA). The composite films span (with dose variation) the transition from electrically insulating to electrically conducting regimes, a range of interest fundamentally and technologically. We find excellent agreement with theory and show that the PMMA-Au films have monodispersive or polydispersive characteristics depending on the implanted ion dose. (C) 2010 American Institute of Physics. [doi:10.1063/1.3493241]

Depth-dependent local structures in thin films unraveled by grazing-incidence X-ray absorption spectroscopy

A method of using X-ray absorption spectroscopy together with resolved grazing-incidence geometry for depth profiling of atomic, electronic or chemical local structures in thin films is presented. The quantitative deconvolution of thickness-dependent spectral features is performed by fully considering both scattering and absorption formalisms. Surface oxidation and local structural depth profiles in nanometric FePt films are determined, exemplifying the application of the method.

Estimation of the thickness and the optical parameters of several stacked thin films using optimization

The reverse engineering problem addressed in the present research consists of estimating the thicknesses and the optical constants of two thin films deposited on a transparent substrate using only transmittance data through the whole stack. No functional dispersion relation assumptions are made on the complex refractive index. Instead, minimal physical constraints are employed, as in previous works of some of the authors where only one film was considered in the retrieval algorithm. To our knowledge this is the first report on the retrieval of the optical constants and the thickness of multiple film structures using only transmittance data that does not make use of dispersion relations. The same methodology may be used if the available data correspond to normal reflectance. The software used in this work is freely available through the PUMA Project web page (http://www.ime.usp.br/similar to egbirgin/puma/). (C) 2008 Optical Society of America

Study of phase transition in (Pb,Ba)TiO(3) thin films

Dielectric and Raman scattering experiments were performed on polycrystalline Pb(1-x)Ba(x)TiO(3) thin films (x=0.40 and 0.60) as a function of temperature. The dielectric study on single phase compositions revealed that a diffuse-type phase transition occurred upon transformation of the cubic paraelectric to the tetragonal ferroelectric phase in all thin films, which showed a broadening of the dielectric peak. Diffusivity was found to increase with increasing barium contents in the composition range under study. In addition, the temperature dependence of Raman scattering spectra was investigated through the ferroelectric phase transition. The temperature dependence of the phonon frequencies was used to characterize the phase transitions. Raman modes persisted above the tetragonal to cubic phase transition temperature, although all optical modes should be Raman inactive. The origin of these modes was interpreted as a breakdown of the local cubic symmetry by chemical disorder. The lack of a well-defined transition temperature and the presence of broadbands in some temperature intervals above the paraferroelectric phase transition temperature suggest a diffuse-type phase transition. (C) 2008 American Institute of Physics.

Diffraction gratings fabricated in DLC thin films

This work presents the fabrication of two-dimensional diffraction gratings in diamond-like carbon (DLC) thin films, with applications in computer-generated holography and micro optics. In order to achieve high diffraction efficiency and to have a very simple manufacturing process, the device is designed to modulate only the phase of an incoming coherent monochromatic laser beam (632.8 nm, HeNe laser). This modulation is obtained by implementing a binary microrelief in the DLC film, responsible for generating a localized optical path difference of half a wavelength. This microrelief is obtained by anisotropic reactive ion etching of the DLC surface in an oxygen based plasma. The DLC layer was grown by reactive magnetron sputtering, using a methane-based plasma chemistry. AFM measurements show a low-level surface roughness of less than 1% of the operation wavelength, and optical characterization shows a good quality of the reconstructed diffraction patterns. (C) 2010 Elsevier B.V. All rights reserved.