Preparation of Al2TiO5-Al2O3 and Al2TiO5-Al2O3-TiO2 Ceramics by High-Energy Ball Milling and Sintering

The present work reports on the preparation of Al2O3-TiO2 ceramics by high-energy ball milling and sintering, varying the molar fraction in 1:1 and 3:1. The powder mixtures were processed in a planetary Fritsch P-5 ball mill using silicon nitride balls (10 mm diameter) and vials (225 mL), rotary speed of 250 rpm and a ball-to-powder weight ratio of 5:1. Samples were collected into the vial after different milling times. The milled powders were uniaxially compacted and sintered at 1300 and 1500 degrees C for 4h. The milled and sintered materials were characterized by X-ray diffraction and electron scanning microscopy (SEM). Results indicated that the intensity of Al2O3 and TiO2 peaks were reduced for longer milling times, suggesting that nanosized particles can be achieved. The densification of Al2O3-TiO2 ceramics was higher than 98% over the relative density in samples sintered at 1500 degrees C for 4h, which presented the formation of Al2TiO5.

Turning of compacted graphite iron using commercial tiN coated Si 3N4 under dry machining conditions

Due to their high hardness and wear resistance Si3N4 based ceramics are one of the most suitable cutting tool materials for machining hardened materials. Therefore, their high degree of brittleness usually leads to inconsistent results and sudden catastrophic failures. Improvement of the functional properties these tools and reduction of the ecological threats may be accomplished by employing the technology of putting down hard coatings on tools in the state-of-the-art PVD processes, mostly by improvement of the tribological contact conditions in the cutting zone and by eliminating the cutting fluids. However in this paper was used a Si3N4 based cutting tool commercial with a layer TiN coating. In this investigation, the performance of TiN coating was assessed on turning used to machine an automotive grade compacted graphite iron. As part of the study were used to characterise the performance of cutting tool, flank wear, temperature and roughness. The results showed that the layer TiN coating failed to dry compacted graphite iron under aggressive machining conditions. However, using the measurement of flank wear technique, the average tool life of was increased by VC=160 m/min.The latter was also observed using a toolmakers microscope and scanning electron microscopy (SEM).

Usinagem da liga de níquel inconel 718 com pastilhas de cerâmica

The machining of super alloys resistant to high temperatures such as nickel alloys, inconel 718 specifically, is a very difficult job to obtain improvements in the process, due to the difficulty of machining at high cutting speeds, the use of these alloys in industries showed great developments in recent years, its application in aeronautical industry spread being used in vane turbo, compressor parts, props and set elements. The automotive, chemical, medical and others also took advantage of the great features of inconel 718 and has used the material. The high temperature resistant alloys have high machining difficulty, a fact that is associated with high cutting forces generated during machining which result in high temperatures. High levels of temperatures can cause deterioration of the cutting edge, with subsequent deformation or breakage, wear most common obtained in machining such materials are flank wear the formation of built-up edge for cutting and notch wear. The experimental part of the work consists in machining of nickel-based alloy Inconel 718 heat treated for hardness, using a tool based ceramic silicon nitride Sandvik (Si3N4) in order to compare the best results obtained in the master's thesis of SANTOS (2010) who used a tool ceramics also the basis of silicon nitride which was developed in the doctoral thesis of SOUZA (2005). Assays were performed on a CNC lathe and was noted for each cutting edge results obtained. Tests were made starting from an initial condition of the tool with cutting speed of 200 m/min, feed 0.5 mm and 0.5 mm depth of cut was reduced cutting speed for the subsequent tests with the same conditions of feed and depth of cut. The tool presented wear instant under two 200 m/min and 100 m/min, premature rupture of 50 m/min and finally cut provided with difficulty... (Complete abstract click electronic access below)

Caracterização de cerâmicas a base de nitreto de silício para aplicações estruturais

The need for development of new materials is a natural process in the companies’ technological point of view, seeking improvements in materials and processes. Specifically, among the materials, ceramic exhibit valuable properties, especially the covalent ceramics which have excellent properties for applications which requires the abrasion resistance, hardness, high temperatures, resistence, etc. being a material that has applications in several areas. Most studies are related to improvement of properties, specially fracture toughness that allows the expansion of its application. Among the most promising ceramic materials are silicon nitride (Si3N4) which has excellent properties. The goal of this work was the development and caracterization of Si3N4-based ceramics, doped with yttrium oxide (Y2O3), rar earth concentrate (CTR2O3) and cerium oxide (CeO2) in the same proportion for the evaluation of properties. The powders' mixtures were homogenized, dried and compressed under pressure uniaxial and isostatic. Sintering was carried out in 1850 ⁰C under pressure of 0,1MPa N2 for 1 h with a heating rate of 25 ⁰C / min and cooling in the furnace inertia. The characterizations were performed using Archimedes principle to relative density, weight loss by measuring before and after sintering, phase analysis by X-ray diffraction, microstructure by scanning electron microscope (SEM), hardness and fracture toughness by the method Vickers indentation. The results obtained showed relative density of 97-98%, Vickers hardness 17 to 19 GPa, fracture toughness 5.6 to 6.8 MPa.m1/2, with phases varying from α-SiAlON and β-Si3N4 depending the types of additives used. The results are promising for tribological applications and can be defined according to the types of additives to be used

Efficient 1535 nm light emission from an all-Si-based optical micro-cavity containing Er3+ and Yb3+ ions

This work reports on the construction and spectroscopic analyses of optical micro-cavities (OMCs) that efficiently emit at ~1535 nm. The emission wavelength matches the third transmission window of commercial optical fibers and the OMCs were entirely based on silicon. The sputtering deposition method was adopted in the preparation of the OMCs, which comprised two Bragg reflectors and one spacer layer made of either Er- or ErYb-doped amorphous silicon nitride. The luminescence signal extracted from the OMCs originated from the 4I13/2→4I15/2 transition (due to Er3+ ions) and its intensity showed to be highly dependent on the presence of Yb3+ ions.According to the results, the Er3+-related light emission was improved by a factor of 48 when combined with Yb3+ ions and inserted in the spacer layer of the OMC. The results also showed the effectiveness of the present experimental approach in producing Si-based light-emitting structures in which the main characteristics are: (a) compatibility with the actual microelectronics industry, (b) the deposition of optical quality layers with accurate composition control, and (c) no need of uncommon elements-compounds nor extensive thermal treatments. Along with the fundamental characteristics of the OMCs, this work also discusses the impact of the Er3+-Yb3+ ion interaction on the emission intensity as well as the potential of the present findings.

A simple-versatile approach to achieve all-Si-based optical micro-cavities

At present, solid thin films are recognized by their well established and mature processing technology that is able to produce components which, depending on their main characteristics, can perform either passive or active functions. Additionally, Si-based materials in the form of thin films perfectly match the concept of miniaturized and low-consumption devices-as required in various modern technological applications. Part of these aspects was considered in the present work that was concerned with the study of optical micro-cavities entirely based on silicon and silicon nitride thin films. The structures were prepared by the sputtering deposition method which, due to the adopted conditions (atmosphere and deposition rate) and arrangement of layers, provided cavities operating either in the visible (at ~ 670 nm) or in the near-infrared (at ~ 1560 nm) wavelength ranges. The main differential of the work relies on the construction of optical microcavities with a reduced number of periods whose main properties can be changed by thermal annealing treatments. The work also discusses the angle-dependent behavior of the optical transmission profiles as well as the use of the COMSOL software package to simulate the microcavities.

Etching and microstructure of engineering ceramics

Engineering ceramics are often difficult to prepare metallographically because of their hardness, wear resistance and chemical inertness. Two silicon carbides, a silicon nitride and a sialon, are prepared and etched using several different techniques. The most efficient methods are identified. © 1995.

Design, fabrication and characterization of resonant waveguide grating based optical biosensors

The absence of rapid, low cost and highly sensitive biodetection platform has hindered the implementation of next generation cheap and early stage clinical or home based point-of-care diagnostics. Label-free optical biosensing with high sensitivity, throughput, compactness, and low cost, plays an important role to resolve these diagnostic challenges and pushes the detection limit down to single molecule. Optical nanostructures, specifically the resonant waveguide grating (RWG) and nano-ribbon cavity based biodetection are promising in this context. The main element of this dissertation is design, fabrication and characterization of RWG sensors for different spectral regions (e.g. visible, near infrared) for use in label-free optical biosensing and also to explore different RWG parameters to maximize sensitivity and increase detection accuracy. Design and fabrication of the waveguide embedded resonant nano-cavity are also studied. Multi-parametric analyses were done using customized optical simulator to understand the operational principle of these sensors and more important the relationship between the physical design parameters and sensor sensitivities. Silicon nitride (SixNy) is a useful waveguide material because of its wide transparency across the whole infrared, visible and part of UV spectrum, and comparatively higher refractive index than glass substrate. SixNy based RWGs on glass substrate are designed and fabricated applying both electron beam lithography and low cost nano-imprint lithography techniques. A Chromium hard mask aided nano-fabrication technique is developed for making very high aspect ratio optical nano-structure on glass substrate. An aspect ratio of 10 for very narrow (~60 nm wide) grating lines is achieved which is the highest presented so far. The fabricated RWG sensors are characterized for both bulk (183.3 nm/RIU) and surface sensitivity (0.21nm/nm-layer), and then used for successful detection of Immunoglobulin-G (IgG) antibodies and antigen (~1μg/ml) both in buffer and serum. Widely used optical biosensors like surface plasmon resonance and optical microcavities are limited in the separation of bulk response from the surface binding events which is crucial for ultralow biosensing application with thermal or other perturbations. A RWG based dual resonance approach is proposed and verified by controlled experiments for separating the response of bulk and surface sensitivity. The dual resonance approach gives sensitivity ratio of 9.4 whereas the competitive polarization based approach can offer only 2.5. The improved performance of the dual resonance approach would help reducing probability of false reading in precise bio-assay experiments where thermal variations are probable like portable diagnostics.

An 8x8 thermopile based uncooled infrared sensor

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Estudo da molhabilidade de ligas de adição à base de prata sobre insertos cerâmicos para aplicação em brocas perfuração de poços de petróleo

Metal-ceramic interfaces are present in tricone drill bits with hard ceramic inserts for oil well drilling operations. The combination of actions of cutting, crushing and breaking up of rocks results in the degradation of tricone drill bits by wear, total or partial rupture of the drill bit body or the ceramic inserts, thermal shock and corrosion. Also the improper pressfitting of the ceramic inserts on the bit body may cause its total detachment, and promote serious damages to the drill bit. The improvement on the production process of metal-ceramic interfaces can eliminate or minimize some of above-mentioned failures presented in tricone drill bits, optimizing their lifetime and so reducing drilling metric cost. Brazing is a widely established technique to join metal-ceramic materials, and may be an excellent alternative to the common mechanical press fitting process of hard ceramic inserts on the steel bit body for tricone drill bit. Wetting phenomena plays an essential role in the production of metal/ceramic interfaces when a liquid phase is present in the process. In this work, 72Silver-28Copper eutectic based brazing alloys were melted onto zirconia, silicon nitride and tungsten carbide/Co substrates under high vacuum. Contact angle evolution was measured and graphically plotted, and the interfaces produced were analysed by SEM-EDX. The AgCu eutectic alloy did not wet any ceramic substrates, showing high contact angles, and so without chemical interaction between the materials. Better results were found for the systemns containing 3%wt of titanium in the AgCu alloy. The presence os titanium as a solute in the alloy produces wettable cand termodinamically stable compounds, increasing the ceramics wetting beahviour

Effect of argon ion energy on the performance of silicon nitridemultilayer permeation barriers grown by hot-wire CVD on polymers

One of the authors (S.M.) acknowledges Direction des Relations Extérieures of Ecole Polytechnique for financial support.

Enhanced sensitivity detection of protein immobilization by fluorescent interference on oxidized silicon.

We present a silicon chip-based approach for the enhanced sensitivity detection of surface-immobilized fluorescent molecules. Green fluorescent protein (GFP) is bound to the silicon substrate by a disuccinimidyl terephtalate-aminosilane immobilization procedure. The immobilized organic layers are characterized by surface analysis techniques, like ellipsometry, atomic force microscopy (AFM) and X-ray induced photoelectron spectroscopy. We obtain a 20-fold enhancement of the fluorescent signal, using constructive interference effects in a fused silica dielectric layer, deposited before immobilization onto the silicon. Our method opens perspectives to increase by an order of magnitude the fluorescent response of surface immobilized DNA- or protein-based layers for a variety of biosensor applications.

Properties of nitrogen doped silicon films deposited by low-pressure chemical vapor deposition from silane and ammonia

Nitrogen doped silicon (NIDOS) films have been deposited by low-pressure chemical vapor deposition from silane SiH4 and ammonia NH3 at high temperature (750°C) and the influences of the NH3/SiH4 gas ratio on the films deposition rate, refractive index, stoichiometry, microstructure, electrical conductivity, and thermomechanical stress are studied. The chemical species derived from silylene SiH2 into the gaseous phase are shown to be responsible for the deposition of NIDOS and/or (silicon rich) silicon nitride. The competition between these two deposition phenomena leads finally to very high deposition rates (100 nm/min) for low NH3/SiH4 gas ratio (R¿0.1). Moreover, complex variations of NIDOS film properties are evidenced and related to the dual behavior of the nitrogen atom into silicon, either n-type substitutional impurity or insulative intersticial impurity, according to the Si¿N atomic bound. Finally, the use of NIDOS deposition for the realization of microelectromechanical systems is investigated.

Si3N4 single-crystal nanowires grown from silicon micro- and nanoparticles near the threshold of passive oxidation

A simple and most promising oxide-assisted catalyst-free method is used to prepare silicon nitride nanowires that give rise to high yield in a short time. After a brief analysis of the state of the art, we reveal the crucial role played by the oxygen partial pressure: when oxygen partial pressure is slightly below the threshold of passive oxidation, a high yield inhibiting the formation of any silica layer covering the nanowires occurs and thanks to the synthesis temperature one can control nanowire dimensions

Role of Phosphorylation of the Oxysterol Binding Protein (OSBP) in (PI(4)P) and Sterol-Containing Membrane Recognition and Binding

Studies have demonstrated that the oxysterol binding protein (OSBP) acts as a phosphatidylinositol phosphate (PIP)-sterol exchanger at membrane contact sites (MCS) of the endoplasmic reticulum (ER) and Golgi. OSBP is known to pick up phosphatidylinositol-4-phosphate (PI(4)P) from the ER, transfer it to the trans-Golgi in exchange for a cholesterol molecule that is then transferred from the trans-Golgi to the ER. Upon further examination of this pathway by Ridgway et al. (1), it appeared that phosphorylation of OSBP played a role in the localization of OSBP. The dephosphorylation state of OSBP was linked to Golgi localization and the depletion of cholesterol at the ER. To mimic the phosphorylated state of OSBP, the mutant OSBP-S5E was designed by Ridgway et al. (1). The lipid and sterol recognition by wt-OSBP and its phosphomimic mutant OSBP-S5E were investigated using immobilized lipid bilayers and dual polarization interferometry (DPI). DPI is a technique in which the protein binding affinity to immobilized lipid bilayers is measured and the binding behavior is examined through real time. Lipid bilayers containing 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC) and varying concentrations of PI(4)Ps or sterols (cholesterol or 25-hydroxycholesterol) were immobilized on a silicon nitride chip. It was determined that wt-OSBP binds differently to PI(4)P-containing bilayers compared to OSBP-S5E. The binding behavior suggested that wt-OSBP extracts PI(4)P and the change in the binding behavior, in the case of OSBP-S5E, suggested that the phosphorylation of OSBP may prevent the recognition and/or extraction of PI(4)P. In the presence of sterols, the overall binding behavior of OSBP, regardless of phosphorylation state, was fairly similar. The maximum specific bound mass of OSBP to sterols did not differ as the concentration of sterols increased. However, comparing the maximum specific bound mass of OSBP to cholesterol with oxysterol (25-hydroxycholesterol), OSBP displayed nearly a 2-fold increase in bound mass. With the absence of the wt-OSBP-PI(4)P binding behavior, it can be speculated that the sterols were not extracted. In addition, the binding behavior of OSBP was further tested using a fluorescence based binding assay. Using 22-(N-(7-nitrobenz-2-oxa-1,3-diazol-4-yl)amino)-23,24-bisnor-5-cholen-3β-ol (22-NBD cholesterol), wt-OSBP a one site binding dissociation constant Kd, of 15 ± 1.4 nM was determined. OSBP-S5E did not bind to 22-NBD cholesterol and Kd value was not obtained.