The study of ternary carbides formation during SPS consolidation process in the WC-Co-steel system

Tungsten carbide has a wide range of applications, mainly cemented carbides made of WC and Co, as wear resistant materials. However, the high cost of WC-Co powders encourages the use of a substrate to manufacture a functionally graded material (FGM) tool made of WC-Co and a tool steel. These materials join the high wear resistance of the cemented carbide and the toughness of the steel. This work deals with the study interaction of the WC-Co and H13 steel to design a functionally graded material by means of spark plasma sintering (SPS). The SPS, a novel sintering technique reaching the consolidation of the powders at relatively low temperatures and short dwell times, is a promising technique in processing materials. In this study, WC, H13 steel, WC-Co, WC-H13 steel and WC-Co-H13 steel bulk samples were investigated using scanning electron microscopy and X-ray diffraction techniques to evaluate the phase transformations involved during SPS consolidation process. The W(2)C and W(3)Fe(3)C precipitation were identified after the SPS consolidation of the WC and WC-H13 steel samples, respectively. The precipitation Of W(4)Co(2)C was also identified in the WC-Co and WC-Co-H13 steel samples. The WC-H 13 steel and WC-Co-H13 steel were also evaluated after heat treatments at 1100 degrees C for 9 h, which enhanced the chemical interaction and the precipitation of W(3)Fe(3)C and W(4)Co(2)C, respectively. (C) 2009 Elsevier Ltd. All rights reserved.

TiAlN coatings deposited by triode magnetron sputtering varying the bias voltage

TiAlN films were deposited on AISI O1 tool steel using a triode magnetron sputtering system. The bias voltage effect on the composition, thickness, crystallography, microstructure, hardness and adhesion strength was investigated. The coatings thickness and elemental composition analyses were carried out using scanning electron microscopy (SEM) together with energy dispersive X-ray (EDS). The re-sputtering effect due to the high-energy ions bombardment on the film surface influenced the coatings thickness. The films crystallography was investigated using X-ray diffraction characterization. The X-ray diffraction (XRD) data show that TiAlN coatings were crystallized in the cubic NaCl B1 structure, with orientations in the {111}, {200} {220} and {311} crystallographic planes. The surface morphology (roughness and grain size) of TiAlN coatings was investigated by atomic force microscopy (AFM). By increasing the substrate bias voltage from -40 to -150 V, hardness decreased from 32 GPa to 19 GPa. Scratch tester was used for measuring the critical loads and for measuring the adhesion. (C) 2011 Elsevier B. V. All rights reserved.

Abrasion and corrosion resistance of new Ni-based coating deposited by HVOF thermal spray process

Coatings based on NiCrAlC intermetallic based alloy were applied on AISI 316L stainless steel substrates using a high velocity oxygen fuel torch. The influence of the spray parameters on friction and abrasive wear resistance were investigated using an instrumented rubber wheel abrasion test, able to measure the friction forces. The corrosion behaviour of the coatings were studied with electrochemical techniques and compared with the corrosion resistance of the substrate material. Specimens prepared using lower O(2)/C(3)H(8) ratios showed smaller porosity values. The abrasion wear rate of the NiCrAlC coatings was much smaller than that described in the literature for bulk as cast materials with similar composition and one order of magnitude higher than bulk cast and heat treated (aged) NiCrAlC alloy. All coatings showed higher corrosion resistance than the AISI 316L substrate in HCl (5%) aqueous solution at 40 degrees C.

Modeling of Plastic Deformation Effects in Ferromagnetic Thin Films

To explain the magnetic behavior of plastic deformation of thin magnetic films (Fe and permalloy) on an elastic substrate (nitinol), it is noted that unlike in the bulk, the dislocation density does not increase dramatically because of the dimensional constraint. As a result, the resulting residual stress, even though strain hardening is limited, dominates the observed magnetic behavior. Thus, with the field parallel to the stress axis, the compressive residual stress resulting from plastic deformation causes a decrease in remanence and an increase in coercivity; and with the field perpendicular to the stress axis, the resulting compressive residual stress causes an increase in remanence and a decrease in coercivity. These elements have been inserted into the model previously developed for plastic deformation in the bulk, producing the aforementioned behavior, which has been observed experimentally in the films.

Optimal conditions for the wetting balance test

Wetting balance tests of copper sheets submerged in tin solder baths were carried out in a completely automatic wetting balance. Wetting curves were examined for three different values of sheet thickness and four different solder bath temperatures. Most of the wetting curves showed a distorted shape relative to that of a standard curve, preventing calculation of important wetting parameters, such as the wetting rate and the wetting force. The wetting tests showed that the distortion increased for a thicker sheet thickness and a lower solder bath temperature, being the result of solder bath solidification around the submerged sheet substrate. (C) 2008 Elsevier B.V. All rights reserved.

Improved Bioprocess with CHO-hTSH Cells on Higher Microcarrier Concentration Provides Higher Overall Biomass and Productivity for rhTSH

Since the recombinant thyroid-stimulating hormone (rhTSH) is secreted by stably transfected Chinese hamster ovary (CHO-hTSH) cells, a bioprocess consisting of immobilizing the cells on a substrate allowing their multiplication is very suitable for rhTSH recovering from supernatants at relative high degree of purity. In addition, such a system has also the advantage of easily allowing delicate manipulations of culture medium replacement. In the present study, we show the development of a laboratory scale bioprocess protocol of CHO-hTSH cell cultures on cytodex microcarriers (MCs) in a 1 L bioreactor, for the preparation of rhTSH batches in view of structure/function studies. CHO-hTSH cells were cultivated on a fetal bovine serum supplemented medium during cell growth phase. For rhTSH synthesis phase, 75% of supernatant was replaced by animal protein-free medium every 24 h. Cell cultures were monitored for agitation (rpm), temperature (A degrees C), dissolved oxygen (% DO), pH, cell concentration, MCs coverage, glucose consumption, lactate production, and rhTSH expression. The results indicate that the amount of MCs in the culture and the cell concentration at the beginning of rhTSH synthesis phase were crucial parameters for improving the final rhTSH production. By cultivating the CHO-hTSH cells with an initial cell seeding of four cells/MC on 4 g/L of MCs with a repeated fed batch mode of operation at 40 rpm, 37 A degrees C, 20% DO, and pH 7.2 and starting the rhTSH synthesis phase with 3 x 10(6) cells/mL, we were able to supply the cultures with enough glucose, to maintain low levels of lactate, and to provide high percent (similar to 80%) of fully covered MCs for a long period (5 days) and attain a high cell concentration (similar to 9 x 10(5) cells/mL). The novelty of the present study is represented by the establishment of cell culture conditions allowing us to produce similar to 1.6 mg/L of rhTSH in an already suitable degree of purity. Batches of produced rhTSH were purified and showed biological activity.

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.

Nanostructured diamond-like carbon films characterization

In this work, we have studied the influence of the substrate surface condition on the roughness and the structure of the nanostructured DLC films deposited by high-density plasma chemical vapor deposition Four methods were used to modify the silicon wafers surface before starting the deposition processes of the nanostructured DLC films. micro-diamond powder dispersion, micro-graphite powder dispersion, and roughness generation by wet chemical etching and roughness generation by plasma etching. The reference wafer was only submitted to a chemical cleaning. It was possible to see that the final roughness and the sp(3) hybridization degree (that is related with the structure and chemical composition) strongly depend on the substrate surface conditions The surface roughness was observed by AFM and SEM and the hybridization degree of the DLC films was analyzed by Raman Spectroscopy Thus, the effects of the substrate surface on the DLC film structure were confirmed. These phenomena can be explained by the fact that the locally higher surface energy and the sharp edges may induce local defects promoting the nanostructured characteristics in the DLC films. (C) 2009 Elsevier B.V. All rights reserved.

MEMS-based incandescent microlamps for integrated optics applications

In this work we present the fabrication and operation of incandescent microlamps for integrated optics applications. This microlamp emits white and infrared light from a chromium resistor embedded in a free-standing silicon oxynitride (SiO(x)N(y)) cantilever that can be coupled to an optical waveguide. In fact, the chromium resistor is sandwiched between layers of SiO(x)N(y) that isolate it from the atmosphere, while electric current heats the resistor to incandescent temperatures. The same SiO(x)N(y) material used in the microlamp fabrication is also used to produce the optical waveguides to allow a monolithic integration of light source and optical circuit. Front-side bulk micromachining of the silicon substrate in potassium hydroxide (KOH) solution is used to fabricate the cantilevers that thermally isolate the resistors from the substrate, thus reducing the heat transfer and the current required to light the lamp.

Development and fabrication of an optimized thermo-electro-optic device using a Mach-Zehnder interferometer

The development and fabrication of a thermo-electro-optic sensor using a Mach-Zehnder interferometer and a resistive micro-heater placed in one of the device`s arms is presented. The Mach-Zehnder structure was fabricated on a single crystal silicon substrate using silicon oxynitride and amorphous hydrogenated silicon carbide films to form an anti-resonant reflective optical waveguide. The materials were deposited by Plasma enhanced chemical vapor deposition technique at low temperatures (similar to 320 degrees C). To optimize the heat transfer and increase the device response with current variation, part of the Mach-Zehnder sensor arm was suspended through front-side bulk micromachining of the silicon substrate in a KOH solution. With the temperature variation caused by the micro-heater, the refractive index of the core layer of the optical waveguide changes due to the thermo-optic effect. Since this variation occurs only in one of the Mach-Zehnder`s arm, a phase difference between the arms is produced, leading to electromagnetic interference. In this way, the current applied to the micro-resistor can control the device output optical power. Further, reactive ion etching technique was used in this work to define the device`s geometry, and a study of SF6 based etching rates on different composition of silicon oxynitride films is also presented. (C) 2007 Elsevier B.V. All rights reserved.

Tunable Bragg filter using silicon compound films

In this work, we present the simulation, fabrication and characterization of a tunable Bragg filter employing amorphous dielectric films deposited by plasma enhanced chemical vapor deposition technique on a crystalline silicon substrate. The optical device was built using conventional microelectronic processes and consisted of fifteen periodic intervals of Si3N4 layers separated by air with appropriated thickness and lengths to produce transmittance attenuation peaks in the visible region. For this, previous simulations were realized based in the optical parameters of the dielectric film, which were extracted from ellipsometry and profilometry techniques. For the characterization of the optical interferential filter, a 633 nm monochromatic light was injected on the filter, and then the transmitted output light was collected and conducted to a detector through an optical waveguide made also of amorphous dielectric layers. Afterwards, the optical filter was mounted on a Peltier thermoelectric device in order to control the temperature of the optical device. When the temperature of filter changes, a refractive index variation is originated in the dielectric film due to the thermo-optic effect, producing a shift of attenuation peak, which can be well predicted by numerical simulations. This characteristic allows this device to be used as a thermo-optic sensor. (C) 2007 Elsevier B.V. All rights reserved.

Improved moisture and hydrocarbons barrier of epoxy resin-based coating

To improve the surface characteristics of epoxy resin coatings, a treatment by fluorine-containing plasma was used to develop a coating with low surface free energy and improved chemical resistance. Through the coating analysis it was possible to verify information about the CF(n) bond formation and the fluorination depth. The best plasma process parameters presented the best fluorination depth, 90 nm, and fluorine concentration was nearly 30%. The improvement in contact angle of water was 50% and of raw petroleum was 130%. Salt spray test proves that the coating fluorination decreases the chance of substrate corrosion.

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.

Numerical study of tensile tests conducted on systems with elastic-plastic films deposited onto elastic-plastic substrates

In this work, a series of two-dimensional plane-strain finite element analyses was conducted to further understand the stress distribution during tensile tests on coated systems. Besides the film and the substrate, the finite element model also considered a number of cracks perpendicular to the film/substrate interface. Different from analyses commonly found in the literature, the mechanical behavior of both film and substrate was considered elastic-perfectly plastic in part of the analyses. Together with the film yield stress and the number of film cracks, other variables that were considered were crack tip geometry, the distance between two consecutive cracks and the presence of an interlayer. The analysis was based on the normal stresses parallel to the loading axis (sigma(xx)), which are responsible for cohesive failures that are observed in the film during this type of test. Results indicated that some configurations studied in this work have significantly reduced the value of sigma(xx) at the film/substrate interface and close to the pre-defined crack tips. Furthermore, in all the cases studied the values of sigma(xx) were systematically larger at the film/substrate interface than at the film surface. (C) 2010 Elsevier B.V. All rights reserved.

Thin titanium oxide films deposited by e-beam evaporation with additional rapid thermal oxidation and annealing for ISFET applications

Titanium oxide (TiO(2)) has been extensively applied in the medical area due to its proved biocompatibility with human cells [1]. This work presents the characterization of titanium oxide thin films as a potential dielectric to be applied in ion sensitive field-effect transistors. The films were obtained by rapid thermal oxidation and annealing (at 300, 600, 960 and 1200 degrees C) of thin titanium films of different thicknesses (5 nm, 10 nm and 20 nm) deposited by e-beam evaporation on silicon wafers. These films were analyzed as-deposited and after annealing in forming gas for 25 min by Ellipsometry, Fourier Transform Infrared Spectroscopy (FTIR), Raman Spectroscopy (RAMAN), Atomic Force Microscopy (AFM), Rutherford Backscattering Spectroscopy (RBS) and Ti-K edge X-ray Absorption Near Edge Structure (XANES). Thin film thickness, roughness, surface grain sizes, refractive indexes and oxygen concentration depend on the oxidation and annealing temperature. Structural characterization showed mainly presence of the crystalline rutile phase, however, other oxides such Ti(2)O(3), an interfacial SiO(2) layer between the dielectric and the substrate and the anatase crystalline phase of TiO(2) films were also identified. Electrical characteristics were obtained by means of I-V and C-V measured curves of Al/Si/TiO(x)/Al capacitors. These curves showed that the films had high dielectric constants between 12 and 33, interface charge density of about 10(10)/cm(2) and leakage current density between 1 and 10(-4) A/cm(2). Field-effect transistors were fabricated in order to analyze I(D) x V(DS) and log I(D) x Bias curves. Early voltage value of -1629 V, R(OUT) value of 215 M Omega and slope of 100 mV/dec were determined for the 20 nm TiO(x) film thermally treated at 960 degrees C. (C) 2009 Elsevier B.V. All rights reserved.