Wear of coated and uncoated PCBN cutting tool used in turning and milling

This licentiate thesis has the main focus on evaluation of the wear of coated and uncoated polycrystalline cubic boron nitride cutting tool used in cutting operations against hardened steel. And to exam the surface finish and integrity of the work material used. Harder work material, higher cutting speed and cost reductions result in the development of harder and more wear resistance cutting tools. Although PCBN cutting tools have been used in over 30 years, little work have been done on PVD coated PCBN cutting tools. Therefore hard turning and hard milling experiments with PVD coated and uncoated cutting tools have been performed and evaluated. The coatings used in the present study are TiSiN and TiAlN. The wear scar and surface integrity have been examined with help of several different characterization techniques, for example scanning electron microscopy and Auger electron spectroscopy.   The results showed that the PCBN cutting tools used displayed crater wear, flank wear and edge micro chipping. While the influence of the coating on the crater and flank wear was very small and the coating showed a high tendency to spalling. Scratch testing of coated PCBN showed that, the TiAlN coating resulted in major adhesive fractures. This displays the importance of understanding the effect of different types of lapping/grinding processes in the pre-treatment of hard and super hard substrate materials and the amount and type of damage that they can create. For the cutting tools used in turning, patches of a adhered layer, mainly consisting of FexOy were shown at both the crater and flank. And for the cutting tools used in milling a tribofilm consisting of SixOy covered the crater. A combination of tribochemical reactions, adhesive wear and mild abrasive wear is believed to control the flank and crater wear of the PCBN cutting tools. On a microscopic scale the difference phases of the PCBN cutting tool used in turning showed different wear characteristics. The machined surface of the work material showed a smooth surface with a Ra-value in the range of 100-200 nm for the turned surface and 100-150 nm for the milled surface. With increasing crater and flank wear in combination with edge chipping the machined surface becomes rougher and showed a higher Ra-value. For the cutting tools used in milling the tendency to micro edge chipping was significant higher when milling the tools steels showing a higher hard phase content and a lower heat conductivity resulting in higher mechanical and thermal stresses at the cutting edge.

Estudo exploratório da deposição de filmes de diamante em alguns substratos cerâmicos

o presente trabalho é um estudo exploratório a respeito da síntese de filmes de diamante via deposiçãoquímica a vapor (CVD) sobre alguns substratos cerâmicos: diboreto de titânio (TiB2), ítria (Y20a), zircão (ZrSi04), zircônia parcialmente e totalmente estabilizada com ítria (Zr02), pirofilita ( Al2Si4OlO(OHh), .alumina (Al2Oa) e nitreto de boro hexagonal (h-BN). Estes substratos foram produzidos, em sua maioria, a partir da sinterização de pós micrométricos em altas temperaturas. Além do estudo em relação a possíveis candidatos alternativos ao tradicional silício para o crescimento de filmes auto-sustentáveis, procuramos encontrar substratos onde o filme aderisse bem e cujas propriedades tribológicas pudessem ser melhoradas com o recobrimento com filme de diamante.Dentre os materiais selecionados, constatamos que a topografia da superfície relacionada à densidade de contornos de grão, desempenha um papel relevante na nucleação do diamante. Além disso, os materiais que favorecem a formação de carbonetos conduziram a melhores resultados na nucleação e crescimento do filme, indicando que a ação da atmosfera reativa do CVD com o substrato também contribui decisivamente para o processo de nucleação. A partir dos resultados obtidos, concluímos que a aderência do filme de diamante ao zircão é excelente, assim como a qualidade do filme, o que pode serexplorado convenientemente caso as propriedades mecânicas do sinterizado de zircão sejam adequadas. No caso da zircônia parcialmente estabilizada, os resultados obtidos foram surpreendentes e este material poderia substituir o convencional substrato de silício para a deposição de filmes auto-sustentados de diamante, com inúmeras vantagens, dentre elas o fato de ser reutilizável e de não ser necessário ataque com ácidos para remoção do substrato, o que evita a geração de resíduos químicos.

Effect of cooling rate on properties of plasma nitrided AISI 1010 steel

In this work, AISI 1010 steel samples were plasma nitrided into 20% N 2 100 Pa and 400 Pa for N 2 and H 2 , respectively), temperatures of 500 and 580 °C, during 2 h. Three different procedures for cooling were accomplished after nitriding. In the first procedure the cooling occurred naturally, that is, the sample was kept on substrate holder. In the second one the sample was pulled off and cooling in a cold surface. Finally, in the third cooling process the sample was pulled off the substrate holder down into special reservoir filled with oil held at ambient temperature. The properties of the AISI 1010 steel samples were characterized by optical and electron microscopy, X-ray diffraction, Mössbauer spectroscopy and microhardness tests. Thermal gradient inside the sample kept on substrate holder during cooling process was measured by three inserted thermocouples at different depths. When samples were cooled rapidly the transformation of ϵ-Fe 2 − 3 N to γ′-Fe 4 N was inhibited. Such effect is indicated by the high concentration of ϵ-Fe compound zone. To get solid state solution of nitrogen in the diffusion zone, instead of precipitates of nitride phases, the cooling rate should be higher than a critical value of about 0.95 °C/s. When this value is reached at any depth of the diffusion zone, two distinct diffusion zones will appear. Temperature gradients were measured inside the samples as a consequence of the plasma treatment. It's suggested the need for standardization of the term “treatment temperature” for plasma treatment because different nitrided layer properties could be reported for the same “treatment temperature”.

Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film

Estudo da sinterabilidade de ligas de níquel obtidas por meio dos portadores de liga sic, si3n4 ou si metálico com grafita

Nickel alloys are frequently used in applications that require resistance at high temperatures associated with resistance to corrosion. Alloys of Ni-Si-C can be obtained by means of powder metallurgy in which powder mixtures are made of metallic nickel powders with additions of various alloying carriers for such were used in this study SiC, Si3N4 or Si metal with graphite. Carbonyl Ni powder with mean particle size of 11 mM were mixed with 3 wt% of SiC powders with an average particle size of 15, 30 and 50 μm and further samples were obtained containing 4 to 5% by mass of SiC with average particle size of 15 μm. Samples were also obtained by varying the carrier alloy, these being Si3N4 powder with graphite, with average particle size of 1.5 and 5 μm, respectively. As a metallic Si graphite with average particle size of 12.5 and 5 μm, respectively. The reference material used was nickel carbonyl sintered without adding carriers. Microstructural characterization of the alloys was made by optical microscopy and scanning electron microscopy with semi-quantitative chemical analysis. We determined the densities of the samples and measurement of microhardness. We studied the dissociation of carriers alloy after sintering at 1200 ° C for 60 minutes. Was evaluated also in the same sintering conditions, the influence of the variation of average particle size of the SiC carrier to the proportion of 3% by mass. Finally, we studied the influence of variation of the temperatures of sintering at 950, 1080 and 1200 ° C without landing and also with heights of 30, 60, 120 and 240 minutes for sintering where the temperature was 950 °C. Dilatometry curves showed that the SiC sintered Ni favors more effectively than other carriers alloy analyzed. SiC with average particle size of 15 μm active sintering the alloy more effectively than other SiC used. However, with the chemical and morphological analyzes for all leagues, it was observed that there was dissociation of SiC and Si3N4, as well as diffusion of Si in Ni matrix and carbon cluster and dispersed in the matrix, which also occurred for the alloys with Si carriers and metallic graphite. So the league that was presented better results containing Si Ni with graphite metallic alloy as carriers, since this had dispersed graphite best in the league, reaching the microstructural model proposed, which is necessary for material characteristic of solid lubricant, so how we got the best results when the density and hardness of the alloy

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

Avaliação de catalisadores a base de carbeto e nitreto de molibdênio na obtenção de lactitol via hidrogenação da lactose

Seeking a greater appreciation of cheese whey was developed to process the hydrogenation of lactose for the production of lactitol, a polyol with high added value, using the catalyst Ni / activated carbon (15% and 20% nickel), the nitride Mo2N, the bimetallic carbide Ni-Mo/ activated carbon and carbide Mo2C. After synthesis, the prepared catalysts were analyzed by MEV, XRD, laser granulometry and B.E.T. The reactor used in catalytic hydrogenation of lactose was the type of bed mud with a pressure (68 atm), temperature (120 oC) and stirring speed (500 rpm) remained constant during the experiments. The system operated in batch mode for the solid and liquid and semi-continuous to gas. Besides the nature of the catalyst, we studied the influence of pH of reaction medium for Mo2C carbide as well as evaluating the character of the protein inhibitor and chloride ions on the activity of catalysts Ni (20%)/Activated Carbon and bimetallic carbide Ni-Mo/Activated Carbon. The decrease in protein levels was performed by coagulation with chitosan and adsorption of chloride ions was performed by ion exchange resins. In the process of protein adsorption and chloride ions, the maximum percentage extracted was about 74% and 79% respectively. The micrographs of the powders of Mo2C and Mo2N presented in the form of homogeneous clusters, whereas for the catalysts supported on activated carbon, microporous structure proved impregnated with small particles indicating the presence of metal. The results showed high conversion of lactose to lactitol 90% for the catalyst Ni (20%)/Activated Carbon at pH 6 and 46% for the carbide Mo2C pH 8 (after addition of NH4OH) using the commercial lactose. Monitoring the evolution of the constituents present in the reaction medium was made by liquid chromatography. A kinetic model of heterogeneous Langmuir Hinshelwood type was developed which showed that the estimated constants based catalysts promoted carbide and nitride with a certain speed the adsorption, desorption and production of lactitol

Immobilization of uricase in layer-by-layer films used in amperometric biosensors for uric acid

The layer-by-layer technique was exploited to immobilize the enzyme uricase onto indium tin oxide substrates coated with a layer of Prussian Blue. Uricase layers were alternated with either poly(ethylene imine) or poly(diallyidimethylammoniumchloride), and the resulting films were used as amperometric biosensors for uric acid. Biosensors with optimum perfomance had a limit of detection of 0.15 mu A mu mol 1(-1) cm(-2) with a linear response between 0.1 and 0.6 mu M of uric acid, which is sufficient for use in clinical tests. Bioactivity was preserved for weeks, and there was negligible influence from interferents, as detection was carried out at 0.0 V vs saturated calomel electrode.

Phytase immobilization on modified electrodes for amperometric biosensing

Phytase (myo-inositol hexaphosphate phosphohydrolase) and phytic acid (myo-inositol hexaphosphate) play an important environmental role, in addition to being a health issue in food industry. Phytic acid is antinutritional due to its ability to chelate metal ions and may also react with proteins decreasing their bioavailability. In this work, we produced biosensors with phytase immobilized in Layer-by-Layer (LbL) films, which could detect phytic acid with a detection limit of 0.19 mmol L-1, which is sufficient to detect phytic acid in seeds of grains and vegetables. The biosensosrs consisted of LbL films containing up to eight bilayers of phytase alternated with poly(allylamine) hydrochloride (PAH) deposited onto an indium-tin oxide (ITO) substrate modified with Prussian Blue. Amperometric detection was conducted in an acetate buffer solution (at pH 5.5) at room temperature, with the biosensor response attributed to the formation of phosphate ions. In subsidiary experiments with the currents measured at 0.0 V (vs. SCE), we demonstrated the absence of effects from some interferents, pointing to a good selectivity of the biosensor. (c) 2007 Elsevier B.V. All rights reserved.

Molecular architecture and electrical properties in evaporated films of cobalt phthalocyanine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Filtros acústicos em cristais fonônicos

In this work, we have studied the acoustic phonon wave propagation within the periodic and quasiperiodic superlattices of Fibonacci type. These structures are formed by phononic crystals, whose periodicity allows the raise of regions known as stop bands, which prevent the phonon propagation throughout the structure for specific frequency values. This phenomenon allows the construction of acoustic filters with great technological potential. Our theoretical model were based on the method of the transfer matrix, thery acoustics phonons which describes the propagation of the transverse and longitudinal modes within a unit cell, linking them with the precedent cell in the multilayer structure. The transfer matrix is built taking into account the elastic and electromagnetic boundary conditions in the superllatice interfaces, and it is related to the coupled differential equation solutions (elastic and electromagnetic) that describe each model under consideration. We investigated the piezoelectric properties of GaN and AlN the nitride semiconductors, whose properties are important to applications in the semiconductor device industry. The calculations that characterize the piezoelectric system, depend strongly on the cubic (zinc-bend) and hexagonal (wurtzite) crystal symmetries, that are described the elastic and piezoelectric tensors. The investigation of the liquid Hg (mercury), Ga (gallium) and Ar (argon) systems in static conditions also using the classical theory of elasticity. Together with the Euler s equation of fluid mechanics they one solved to the solid/liquid and the liquid/liquid interfaces to obtain and discuss several interesting physical results. In particular, the acoustical filters obtained from these structures are again presented and their features discussed

Confinamento de fónons ópticos em estruturas piezoelétricas periódicas e quasiperiódicas

We study the optical-phonon spectra in periodic and quasiperiodic (Fibonacci type) superlattices made up from III-V nitride materials (GaN and AlN) intercalated by a dielectric material (silica - SiO2). Due to the misalignments between the silica and the GaN, AlN layers that can lead to threading dislocation of densities as high as 1010 cm−1, and a significant lattice mismatch (_ 14%), the phonon dynamics is described by a coupled elastic and electromagnetic equations beyond the continuum dielectric model, stressing the importance of the piezoelectric polarization field in a strained condition. We use a transfer-matrix treatment to simplify the algebra, which would be otherwise quite complicated, allowing a neat analytical expressions for the phonon dispersion relation. Furthermore, a quantitative analysis of the localization and magnitude of the allowed band widths in the optical phonon s spectra, as well as their scale law are presented and discussed

Filmes nanométricos de FeN e ALN crescidos por sputtering e aplicações do efeito peltier

This study will show the capability of the reactive/nonreactive sputtering (dc/rf) technique at low power for the growth of nanometric thin films from magnetic materials (FeN) and widegap semiconductors (AlN), as well as the technological application of the Peltier effect using commercial modules of bismuth telluride (Bi2Te3). Of great technological interest to the high-density magnetic recording industry, the FeN system represents one of the most important magnetic achievements; however, diversity of the phases formed makes it difficult to control its magnetic properties during production of devices. We investigated the variation in these properties using ferromagnetic resonance, MOKE and atomic force microscopy (AFM), as a function of nitrogen concentration in the reactive gas mixture. Aluminum nitride, a component of widegap semiconductors and of considerable interest to the electronic and optoelectronic industry, was grown on nanometric thin film for the first time, with good structural quality by non-reactive rf sputtering of a pure AlN target at low power (≈ 50W). Another finding in this study is that a long deposition time for this material may lead to film contamination by materials adsorbed into deposition chamber walls. Energy-dispersive X-ray (EDX) analysis shows that the presence of magnetic contaminants from previous depositions results in grown AlN semiconductor films exhibiting magnetoresistance with high resistivity. The Peltier effect applied to commercially available compact refrigeration cells, which are efficient for cooling small volumes, was used to manufacture a technologically innovative refrigerated mini wine cooler, for which a patent was duly registered

Polaritons de exciton em super-redes semicondutoras

In this work we study the spectrum (bulk and surface modes) of exciton-polaritons in infinite and semi-infinite binary superlattices (such as, ···ABABA···), where the semiconductor medium (A), whose dielectric function depends on the frequency and the wavevector, alternating with a standard dielectric medium B. Here the medium A will be modeled by a nitride III-V semiconductor whose main characteristic is a wide-direct energy gap Eg. In particular, we consider the numerical values of gallium nitride (GaN) with a crystal structure wurtzite type. The transfer-matrix formalism is used to find the exciton-polariton dispersion relation. The results are obtained for both s (TE mode: transverse electric) and p (TM mode: transverse magnetic) polarizations, using three diferent kind of additional boundary conditions (ABC1, 2 e 3) besides the standard Maxwell's boundary conditions. Moreover, we investigate the behavior of the exciton-polariton modes for diferent ratios of the thickness of the two alternating materials forming the superlattice. The spectrums shows a confinement of the exciton-polariton modes due to the geometry of the superlattice. The method of Attenuated Total Reflection (ATR) and Raman scattering are the most adequate for probing this excitations

Caracterização magnética e estrutural de filmes depositados por gaiola catódica

Iron nitrite films, with hundred of nanometers thick, were deposited using the Cathodic cage plasma nitriding method, with a N2/H2 plasma, over a common glass substract. The structure, surface morphology and magnetic properties were investigated using X-ray diffractometry (XRD), atomic force microscopy (AFM) and vibrating sample magnetometer (VSM). XRD shows the formation of γ FeN phase and a combination of ζFe2N + ɛFe3N phases. The film s saturation magnetization and coercivity depends on morphology, composition, grain size and treatment temperature. Temperature raising from 250 ºC to 350 ºC were followed by an increase in saturation magnetization and film s surface coercivity on the parallel direction in relative proportion. This fact can be attributed to the grain sizes and to the different phases formed, since iron rich fases, like the ɛFe3N phase, emerges more frequently on more elevated treatment s temperature. Using this new and reasonably low cost method, it was possible to deposit films with both good adhesion and good magnetic properties, with wide application in magnetic devices