Influence of selenization pressure on the growth of Cu2ZnSnSe4 films from stacked metallic layers

Cu2ZnSnSe4 (CZTSe) is a p-type semiconductor with a high absorption coefficient, 104 to 105 cm-1, and is being seen as a possible replacement for Cu(In,Ga)Se2 in thin film solar cells. Yet, there are some fundamental properties of CZTSe that are not well known, one of them is its band gap. In order to resolve its correct value it is necessary to improve the growth conditions to ensure that single phase crystalline thin films are obtained. One of the problems encountered when growing CZTSe is the loss of Sn through evaporation of SnSe. Stoichiometric films are then difficult to obtain and usually there are other phases present. One possible way to overcome this problem is to increase the pressure of growth of CZTSe. This can be done by introducing an atmosphere of an inert gas like Ar or N2. In this work we report the results of morphological, structural and optical studies of the properties of CZTSe thin films grown by selenization of DC magnetron sputtered metallic layers under different Ar pressures. The films are analysed by SEM/EDS, Raman scattering and XRD.

Analysis of the nano-surface of a modified glassy carbon electrode by pseudo phase plane method

This paper presents the Pseudo phase plane (PPP) method for detecting the existence of a nanofilm on the nitroazobenzene-modified glassy carbon electrode (NAB-GC) system. This modified electrode systems and nitroazobenze-nanofilm were prepared by the electrochemical reduction of diazonium salt of NAB at the glassy carbon electrodes (GCE) in nonaqueous media. The IR spectra of the bare glassy carbon electrodes (GCE), the NAB-GC electrode system and the organic NAB film were recorded. The IR data of the bare GC, NAB-GC and NAB film were categorized into five series consisting of FILM1, GC-NAB1, GC1; FILM2, GC-NAB2, GC2; FILM3, GC-NAB3, GC3 and FILM4, GC-NAB4, GC4 respectively. The PPP approach was applied to each group of the data of unmodified and modified electrode systems with nanofilm. The results provided by PPP method show the existence of the NAB film on the modified GC electrode.

Microstructure, mechanical properties and chemical degradation of brazed AISI 316 stainless steel/alumina systems

The main aims of the present study are simultaneously to relate the brazing parameters with: (i) the correspondent interfacial microstructure, (ii) the resultant mechanical properties and (iii) the electrochemical degradation behaviour of AISI 316 stainless steel/alumina brazed joints. Filler metals on such as Ag–26.5Cu–3Ti and Ag–34.5Cu–1.5Ti were used to produce the joints. Three different brazing temperatures (850, 900 and 950 °C), keeping a constant holding time of 20 min, were tested. The objective was to understand the influence of the brazing temperature on the final microstructure and properties of the joints. The mechanical properties of the metal/ceramic (M/C) joints were assessed from bond strength tests carried out using a shear solicitation loading scheme. The fracture surfaces were studied both morphologically and structurally using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction analysis (XRD). The degradation behaviour of the M/C joints was assessed by means of electrochemical techniques. It was found that using a Ag–26.5Cu–3Ti brazing alloy and a brazing temperature of 850 °C, produces the best results in terms of bond strength, 234 ± 18 MPa. The mechanical properties obtained could be explained on the basis of the different compounds identified on the fracture surfaces by XRD. On the other hand, the use of the Ag–34.5Cu–1.5Ti brazing alloy and a brazing temperature of 850 °C produces the best results in terms of corrosion rates (lower corrosion current density), 0.76 ± 0.21 μA cm−2. Nevertheless, the joints produced at 850 °C using a Ag–26.5Cu–3Ti brazing alloy present the best compromise between mechanical properties and degradation behaviour, 234 ± 18 MPa and 1.26 ± 0.58 μA cm−2, respectively. The role of Ti diffusion is fundamental in terms of the final value achieved for the M/C bond strength. On the contrary, the Ag and Cu distribution along the brazed interface seem to play the most relevant role in the metal/ceramic joints electrochemical performance.

InOx thin films deposited by plasma assisted evaporation: application in light shutters

An integration of undoped InOx and commercial ITO thin films into laboratory assembled light shutter devices is made. Accordingly, undoped transparent conductive InOx thin films, about 100 nm thick, are deposited by radiofrequency plasma enhanced reactive thermal evaporation (rf-PERTE) of indium teardrops with no intentional heating of the glass substrates. The process of deposition occurs at very low deposition rates (0.1-0.3 nm/s) to establish an optimized reaction between the oxygen plasma and the metal vapor. These films show the following main characteristics: transparency of 87% (wavelength, lambda = 632.8 nm) and sheet resistance of 52 Omega/sq; while on commercial ITO films the transparency was of 92% and sheet resistance of 83 Omega/sq. The InOx thin film surface characterized by AFM shows a uniform grain texture with a root mean square surface roughness of Rq similar to 2.276 nm. In contrast, commercial ITO topography is characterized by two regions: one smoother with Rq similar to 0.973 nm and one with big grains (Rq similar to 3.617 nm). For the shutters assembled using commercial ITO, the light transmission coefficient (Tr) reaches the highest value (Tr-max) of 89% and the lowest (Tr-min) of 1.3% [13], while for the InOx shutters these values are 80.1% and 3.2%, respectively. Regarding the electric field required to achieve 90% of the maximum transmission in the ON state (E-on), the one presented by the devices assembled with commercial ITO coated glasses is 2.41 V/mu m while the one presented by the devices assembled with InOx coated glasses is smaller, 1.77 V/mu m. These results corroborate the device quality that depends on the base materials and fabrication process used. (C) 2014 Elsevier Ltd. All rights reserved.

High-performance flexible hybrid field-effect transistors based on cellulose fiber paper

IEEE Electron Device Letters, VOL. 29, NO. 9,

Fully transparent ZnO thin-film transistor produced at room temperature

Advanced Materials, Vol. 17, nº 5

Electrochemical response of 70Co-30Ni highly branched 3D-dendritic structures for charge storage electrodes

A 70Co-30Ni dendritic alloy was produced on stainless steel by pulse electrodeposition in the cathodic domain, and oxidized by potential cycling. X-ray diffraction (XRD) identified the presence of two phases and scanning electron microscopy (SEM) evidenced an open 3D highly branched dendritic morphology. After potential cycling in 1 M KOH, SEM and X-ray photoelectron spectroscopy (XPS) revealed, respectively, the presence of thin nanoplates, composed of Co and Ni oxi-hydroxides and hydroxides over the original dendritic film. Cyclic voltammetry tests showd the presence of redox peaks assigned to the oxidation and reduction of Ni and Co centres in the surface film. Charge/discharge measurements revealed capacity values of 121 mAh g(1) at 1 mA cm(2). The capacity retention under 8000 cycles was above 70%, stating the good reversibility of these redox materials and its suitability to be used as charge storage electrodes. Electrochemical impedance spectroscopy (EIS) spectra, taken under different applied bias, showed that the capacitance increased when the electrode was fully oxidized and decreased when the electrode was reduced, reflecting different states-of-charge of the electrode. (C) 2015 Elsevier Ltd. All rights reserved.

Impact of antihelminthic treatment on infection by Ascaris lumbricoides, Trichuris trichiura and hookworms in Covas, a rural community of Pernambuco, Brazil

This work aims to evaluate the impact of drug treatment on infection by Ascaris lumbricoides (Al), Trichuris trichiura (Tt) and hookworms (Hook) in a rural community from the sugar-cane zone of Pernambuco, Brazil. Four parasitological surveys were carried out from March 2001 to March 2002. Individual diagnosis was based on eight slides (four by the Kato-Katz method and four by the Hoffman method) per survey. Infected subjects were assigned to two groups for treatment with either albendazole (n = 62) or mebendazole (n = 57). Prevalence of infection fell significantly (p < 0.05) one month after treatment: Al (from 47.7% to 6.6%); Tt (from 45.7% to 31.8%) and Hook (from 47.7% to 24.5%). One year after treatment, infections by Tt and Hook remained significantly below pre-control levels. A substantial decrease in single-infection cases and multiple infections was found. Egg-negative rate was significant for Al (94.0%), Hook (68.3%) but not for Tt (45.5%), and did not differ significantly between subjects treated with mebendazole or albendazole. Egg counts fell significantly in the individuals remaining positive for Tt. It is recommended that antihelminthic treatment should be selective and given at yearly intervals preferably with albendazole, due to its cost-effectiveness.

A comparison between thin film solar cells made from co-evaporated CuIn1-xGaxSe2using a one-stage process versus a three-stage process

Until this day, the most efficient Cu(In,Ga)Se2 thin film solar cells have been prepared using a rather complex growth process often referred to as three-stage or multistage. This family of processes is mainly characterized by a first step deposited with only In, Ga and Se flux to form a first layer. Cu is added in a second step until the film becomes slightly Cu-rich, where-after the film is converted to its final Cu-poor composition by a third stage, again with no or very little addition of Cu. In this paper, a comparison between solar cells prepared with the three-stage process and a one-stage/in-line process with the same composition, thickness, and solar cell stack is made. The one-stage process is easier to be used in an industrial scale and do not have Cu-rich transitions. The samples were analyzed using glow discharge optical emission spectroscopy, scanning electron microscopy, X-ray diffraction, current–voltage-temperature, capacitance-voltage, external quantum efficiency, transmission/reflection, and photoluminescence. It was concluded that in spite of differences in the texturing, morphology and Ga gradient, the electrical performance of the two types of samples is quite similar as demonstrated by the similar J–V behavior, quantum spectral response, and the estimated recombination losses.

Effect of surfactant on PDLC films with and without permanent memory effect

Dissertação para obtenção do Grau de Mestre em Engenharia Química e Bioquímica

Structural, mechanical and piezoelectric properties of polycrystalline AlN films sputtered on titanium bottom electrodes

Polycrystalline AlN coatings deposited on Ti-electrodes films were sputtered by using nitrogen both as reactive gas and sputtering gas, in order to obtain high purity coatings with appropriate properties to be further integrated into wear resistance coatings as a piezoelectric monitoring wear sensor. The chemical composition, the structure and the morphology of the films were investigated by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and atomic force microscopy techniques. These measurements show the formation of highly (101), (102) and (103) oriented AlN films with good piezoelectric and mechanical properties suitable for applications in electronic devices. Through the use of lower nitrogen flow a densification of the AlN coating occurs in the microstructure, with an improvement of the crystallinity along with the increase of the hardness. Thermal stability of aluminum nitride coatings at high temperature was also examined. It was found an improvement of the piezoelectric properties of the highly (10x) oriented AlN films which became c-axis (002) oriented after annealing. The mechanical behavior after heat treatment shows an important enhancement of the surface hardness and Young’s modulus, which decrease rapidly with the increase of the indentation depth until approach constant values close to the substrate properties after annealing. Thus, thermal annealing energy promotes not only the rearrangement of Al–N network, but also the occurrence of a nitriding process of unsaturated Al atoms which cause a surface hardening of the film.

Thin films composed of gold nanoparticles dispersed in a dielectric matrix: the influence of the host matrix on the optical and mechanical responses

Gold nanoparticles were dispersed in two different dielectric matrices, TiO2 and Al2O3, using magnetron sputtering and a post-deposition annealing treatment. The main goal of the present work was to study how the two different host dielectric matrices, and the resulting microstructure evolution (including both the nanoparticles and the host matrix itself) promoted by thermal annealing, influenced the physical properties of the films. In particular, the structure and morphology of the nanocomposites were correlated with the optical response of the thin films, namely their localized surface plasmon resonance (LSPR) characteristics. Furthermore, and in order to scan the future application of the two thin film system in different types of sensors (namely biological ones), their functional behaviour (hardness and Young's modulus change) was also evaluated. Despite the similar Au concentrations in both matrices (~ 11 at.%), very different microstructural features were observed, which were found to depend strongly on the annealing temperature. The main structural differences included: (i) the early crystallization of the TiO2 host matrix, while the Al2O3 one remained amorphous up to 800 °C; (ii) different grain size evolution behaviours with the annealing temperature, namely an almost linear increase for the Au:TiO2 system (from 3 to 11 nm), and the approximately constant values observed in the Au:Al2O3 system (4–5 nm). The results from the nanoparticle size distributions were also found to be quite sensitive to the surrounding matrix, suggesting different mechanisms for the nanoparticle growth (particle migration and coalescence dominating in TiO2 and Ostwald ripening in Al2O3). These different clustering behaviours induced different transmittance-LSPR responses and a good mechanical stability, which opens the possibility for future use of these nanocomposite thin film systems in some envisaged applications (e.g. LSPR-biosensors).

Composition and structure variation for magnetron sputtered tantalum oxynitride thin films, as function of deposition parameters

Tantalum oxynitride thin films were produced by magnetron sputtering. The films were deposited usinga pure Ta target and a working atmosphere with a constant N2/O2ratio. The choice of this constant ratiolimits the study concerning the influence of each reactive gas, but allows a deeper understanding of theaspects related to the affinity of Ta to the non-metallic elements and it is economically advantageous.This work begins by analysing the data obtained directly from the film deposition stage, followed bythe analysis of the morphology, composition and structure. For a better understanding regarding theinfluence of the deposition parameters, the analyses are presented by using the following criterion: thefilms were divided into two sets, one of them produced with grounded substrate holder and the otherwith a polarization of −50 V. Each one of these sets was produced with different partial pressure of thereactive gases P(N2+ O2). All the films exhibited a O/N ratio higher than the N/O ratio in the depositionchamber atmosphere. In the case of the films produced with grounded substrate holder, a strong increaseof the O content is observed, associated to the strong decrease of the N content, when P(N2+ O2) is higherthan 0.13 Pa. The higher Ta affinity for O strongly influences the structural evolution of the films. Grazingincidence X-ray diffraction showed that the lower partial pressure films were crystalline, while X-rayreflectivity studies found out that the density of the films depended on the deposition conditions: thehigher the gas pressure, the lower the density. Firstly, a dominant -Ta structure is observed, for lowP(N2+ O2); secondly a fcc-Ta(N,O) structure, for intermediate P(N2+ O2); thirdly, the films are amorphousfor the highest partial pressures. The comparison of the characteristics of both sets of produced TaNxOyfilms are explained, with detail, in the text.

Multifunctional Ti–Me (Me=Al, Cu) thin film systems for biomedical sensing devices

Ti-Me binary intermetallic thin films based on a titanium matrix doped with increasing amounts of Me (Me = Al, Cu) were prepared by magnetron sputtering (under similar conditions), aiming their application in biomedical sensing devices. The differences observed on the composition and on the micro(structural) features of the films, attributed to changes in the discharge characteristics, were correlated with the electrical properties of the intermetallic systems (Ti-Al and Ti-Cu). For the same Me exposed areas placed on the Ti target (ranging from 0.25 cm2 to 20 cm2) the Cu content increased from 3.5 at.% to 71.7 at.% in the Ti-Cu system and the Al content, in Ti-Al films, ranged from 11 to 45 at.%. The structural characterization evidenced the formation of metastable Ti-Me intermetallic phases for Al/Ti atomic ratios above 0.20 and for Cu/Ti ratios above 0.25. For lower Me concentrations, the effect of the α-Ti(Me) structure domains the overall structure. With the increase amount of the Me into Ti structure a clear trend for amorphization was observed. For both systems it was observed a significant decrease of the electrical resistivity with increasing Me/Ti atomic ratios (higher than 0.5 for Al/Ti atomic ratio and higher than 1.3 for Cu/Ti atomic ratio). Although similar trends were observed in the resistivity evolution for both systems, the Ti-Cu films presented lower resistivity values in comparison to Ti-Al system.

Tailored deposition of coloured coatings: on the widening of the available colour range

Dissertação de mestrado integrado em Engenharia de Materiais