Laser induced periodic surface structures (LIPSS) have been produced at the surface of a WC-Co turning insert by femtosecond pulsed laser ablation. Wavelengths of approx. 500 nm have been obtained with a 1030 nm incident radiation and with a spot size of 30 mu m. No thermal damage is induced by following this procedure, although a slight surface stress relaxation is detected as fluence increases. The higher material removal needed for chamfering operations requires accumulated fluences over 1 kJ/cm2. At lower energy densities, material removal is not completed. If fluence is increased by reducing the laser spot size, material removal is also inefficient since signicant amount of debris is accumulated on the irradiated areas. Best chamfering strategy involves the combination of relatively large spot sizes and fluences. Form factors (Kappa) of the chamfered cutting edges range from 4 to 10 although the laser is oriented at 45 degrees of the rake face. Lower K values can be obtained by adjusting the laser focus along the machining process.

A new method has been developed for measuring residual stresses at the surface of hardmetal components with higher spatial resolution than standard X-ray diffraction methods. It is based on measuring the surface dis-placements produced when stresses are partially released by machining a thin slit perpendicularly to the tested surface. Slit machining is carried out by focused ion beam (FIB). Measurement of the displacement fields around the FIB slit are performed by applying an advanced digital image correlation algorithm based on Fourier analysis with sub-pixel resolution. This method compares SEM images of the same area of the hardmetal surface before and after slitting. The method has been successfully applied to as-ground and femto-laser textured surfaces showing good correlation with the standard sin2 psi XRD technique. It is concluded that texturing induced by laser pulses in the femtoseconds regime is not perfectly adiabatic, since residual stresses are reduced by 15%.

In many practical situations, the distribution of residual stresses can have a paramount influence on the fatigue and fracture response of materials. In this paper, we describe a method for the local measurement of residual stresses. It consists of Digital Image Correlation (DIC) of Scanning Electron Microscope (SEM) images of a surface, before and after milling a slit using a Focused Ion Beam (FIB). The DIC algorithm used in this work is based on Fourier analysis, which can reach sub-pixel resolution. In order to calculate the internal stresses released during the milling process, the displacements detected with the DIC algorithm are fitted to Finite Element Method (FEM) simulations. Residual stresses measured by this method on a hard metal sample subjected to different laser surface treatments are successfully compared with X-ray diffraction measurements.

ZnO conductometric gas sensors have been widely studied due to their good sensitivity, cost-efficiency, long stability and simple fabrication. This work is focused on NO2 sensing, which is a toxic and irritating gas. The developed sensor consists of interdigitated electrodes covered by a ZnO sensing layer. ZnO has been grown by means of the aerosol assisted chemical vapor deposition technique and then nanostructured by laser interference lithography with a UV laser. The SEM and XRD results show vertically oriented growth of ZnO grains and a 2D periodic nanopatterning of the material with a period of 800 nm. Nanostructuring lowers the base resistance of the developed sensors and modifies the sensor response to NO2. Maximum sensitivity is obtained at 175 degrees C achieving a change of 600% in sensor resistance for 4 ppm NO(2)versus a 400% change for the non-nanostructured material. However, the most relevant results have been obtained at temperatures below 125 degrees C. While the non-nanostructured material does not respond to NO2 at such low temperatures, nanostructured ZnO allows NO2 sensing even at room temperature. The room temperature sensing capability possibly derives from the increase of both the surface defects and the surface-to-volume ratio. The long stability and the gas sensing under humid conditions have also been tested, showing improvements of sensitivity for the nanostructured sensors.

Aerosol-assisted Chemical Vapor Deposition (AACVD) is a thermally activated CVD technique that uses micro-droplets as deposition precursors. An AACVD system with a custom-designed reaction chamber has been implemented to grow ZnO thin films using zinc chloride as a precursor. The present work aims to study the impact of the deposition parameters on the thin film, as well as the microstructure evolution and growth kinetics. Aerosol flow has an effect on the density of nucleation sites and on the grain size. The temperature affects the morphology of the grown ZnO, showing a preferential orientation along the c-axis for 350 degrees C, 375 degrees C and 400 degrees C substrate temperatures. The microstructural evolution and the growth kinetics are also presented. A different evolution behavior has been observed for 350 degrees C, where nucleation site density is the highest at the early stages and it decreases over time in contrast with the cases of 375 degrees C and 400 degrees C, where there is an initial increase and a subsequent decrease. The activation energy of the chemical reaction is 1.06 eV. The optical characterization of the material has been performed through reflection measurements showing a relationship between the spectrum and the ZnO film thickness. The electrical characterization has been done by means of an interdigital capacitor, with which it is possible to measure the grain and grain boundary resistance of the material. Both resistances are of the order of 10(5)-10(6) omega.

The electrical and electrochemical properties of two ionogel materials based on the poly(N-isopropylacrylamide) gel with 1-ethyl-3-methylimidazolium ethyl sulfate and trihexyltetradecylphosphonium dicyanamide ionic liquids are investigated. The current-voltage curves show a current rectification for both ionogels and ionic liquids after inducing ion adsorption on gold electrode surface. The polymer matrix of the ionogels mitigates ion adsorption, resulting in lower rectification ratios when comparing with the corresponding ionic liquids. The stability and the electrochemical window (ECW) of the ionogels are calculated from cyclic voltammograms and compared with the ones obtained for the ionic liquids. The widest electrochemical window is achieved by the phosphonium ionic liquid and its ionogel. Finally, the effect of the absorbed atmospheric water and the mutual coefficient diffusion of the redox active species inside the IO is calculated. This work widens the knowledge of the behavior of ionogel materials characterized on gold electrode interfaces. (C) 2020 Elsevier Ltd. All rights reserved.

A room temperature benzene and formaldehyde gas sensor system with an ionogel as sensing material is presented. The sensing layer is fabricated employing poly(N-isopropylacrylamide) polymerized in the presence of 1-ethyl-3-methylimidazolium ethyl sulfate ionic liquid onto gold interdigitated electrodes. When the ionogel is exposed to increasing formaldehyde concentrations employing N-2 as a carrier gas, a more stable response is observed in comparison to the bare ionic liquid, but no difference in sensitivity occurs. On the other hand, when air is used as carrier gas the sensitivity of the system towards formaldehyde is decreased by one order of magnitude. At room temperature, the proposed sensor exhibited in air higher sensitivities to benzene, at concentrations ranging between 4 and 20 ppm resulting, in a limit of detection of 47 ppb, which is below the standard permitted concentrations. The selectivity of the IL towards HCHO and C6H6 is demonstrated by the absence of response when another IL is employed. Humidity from the ambient air slightly affects the resistance of the system proving the protective role of the polymeric matrix. Furthermore, the gas sensor system showed fast response/recovery times considering the thickness of the material, suggesting that ionogel materials can be used as novel and highly efficient volatile organic compounds sensors operating at room temperature.

A combination of atomic layer deposition and photolithography is applied to fabricate interdigitated electrodes of aluminum-doped zinc oxide embedded in polyethylene terephthalate substrates. Various designs with different gap to widths ratios are realized and important characteristics of the electrodes, including thickness, surface roughness, and electrical properties with different ZnO:Al2O3 ratios are studied. Oxygen plasma is applied to etch the polyethylene terephthalate surface and to embed the electrodes, a methodology which is a breakthrough toward ultimately thin devices fabrication. Moreover, the influence of oxygen plasma on the electrical properties of aluminum-doped zinc oxide is analyzed in more detail. Electrochemical impedance spectroscopy studies of two different stimuli responsive ionogels are performed using the fabricated electrodes. The results show the suitability of the use of the fabricated electrodes to monitor changes in ion motion and morphology of stimuli responsive materials. These electrodes and the process of characterization of the ionogels presented could be implemented to monitor electrochemical changes in real applications such as protective coatings.

The characterization of thermo-responsive ionogels with electrochemical impedance spectroscopy using gold interdigitated electrodes is described. The ionogels are synthesized using poly(N-isopropylacrylamide) as thermo-responsive gel and polymerized in the presence of two ionic liquids: ethyl-3-methylimidazolium ethyl sulfate or trihexyltetradecyl-phosphonium dicyanamide. The changes on the charge-transfer resistance show a clear dependence on the porosity and on the chemical structure of the ionogel. Moreover, the charge-transfer resistance parameter can be used to track in real time the photopolymerization and the hydration process of the ionogels. After exposing them to several drying/rehydration cycles the switching performance is fully understood. The results show that theionogel with 1-ethyl-3-methylimidazolium ethyl sulfate requires less time to absorb and release water and is excellent for fast response applications. On the contrary, the one with the trihexyltetradecyl-phosphonium dicyanamide ionic liquid presents a more robust actuator behavior and a huge potential to be included in long-term applications. Finally, the observed microstructures have been correlated with the measured charge-transfer resistance providing a better understanding of the actuator behavior of these smart materials. (c) 2017 Elsevier B.V. All rights reserved.

A conductometric sensor based on ZnO nanoneedles for the detection of NO2 is described. The material is grown on chip over Pt interdigitated electrodes patterned on alumina substrates without the need of a catalyst layer. The nanostructure growth relies on two different mechanisms (Vapor-Solid and Liquid-Solid) so nanoneedles with few mu m of length and wurtzite structure are obtained. The procedure is optimized on chip, which supposes a significant advantage in the fabrication of nanostructures on sensing devices. The sensor response has been measured under a target gas (NO2) and two interfering pollutants (benzene and formaldehyde). Lower working temperatures than other pure ZnO nanostructures found in the literature have been achieved and limit of detection (LOD) in the order of ppb has been reached. The significant higher response to NO2 with respect to benzene and formaldehyde makes this sensing device suitable for selective NO2 detection indoors.