The influence of high-temperature sintering on microstructure and mechanical properties of free-standing APS CeO-YO -ZrO coatings

In this study, ceria-yttria co-stabilized zirconia (CYSZ) free-standing coatings, deposited by air plasma spraying (APS), were isothermally annealed at 1315 °C in order to explore the effect of sintering on the microstructure and the mechanical properties (i.e., hardness and Young's modulus). To this aim, coating microstructure, before and after heat treatment, was analyzed using scanning electron microscopy, and image analysis was carried out in order to estimate porosity fraction. Moreover, Vickers microindentation and depth-sensing nanoindentation tests were performed in order to study the evolution of hardness and Young's modulus as a function of annealing time. The results showed that thermal aging of CYSZ coatings leads to noticeable microstructural modifications. Indeed, the healing of finer pores, interlamellar, and intralamellar microcracks was observed. In particular, the porosity fraction decreased from ~10 to ~5% after 50 h at 1315 °C. However, the X-ray diffraction analyses revealed that high phase stability was achieved, as no phase decomposition occurred after thermal aging. In turn, both the hardness and Young's modulus increased, in particular, the increase in stiffness (with respect to "as produced" samples) was equal to ~25%, whereas the hardness increased to up to ~60%. © 2010 Springer Science+Business Media, LLC.

Insight of the interface of electroless Ni-P/SiC composite coating on aluminium alloy, LM24

Electroless nickel composite coatings with silicon carbide, SiC, as reinforcing particles deposited with Ni–P onto aluminium alloy, LM24, having zincating as under layer were subjected to heat treatment using air furnace. The changes at the interface were investigated using scanning electron microscope (SEM) and energy dispersive X-ray (EDX) to probe the chemistry changes upon heat treatment. Microhardness tester with various loads using both Knoop and Vickers indenters was used to study the load effect clubbed with the influence of second phase particles on the coating at the vicinity of the interface. It was observed that zinc was absent at the interface after elevated temperature heat treatment at 400–500 °C. Precipitation of copper and nickel with a distinct demarcation (copper rich belt) along the coating interface was seen with irregular thickness of the order of 1 μm. Migration of copper from the bulk aluminium alloy could have been the factor. Brittleness of the coating was confirmed on heat treatment when indented with Vickers. However, in composite coating the propagation of the microcrack was stopped by the embedded particles but the microcracks continue in the matrix when not interrupted by second phase particles (SiC).

Electroless nickel composite (Ni-P/SiC) coating - A study on interface and corrosion characteristic

Surface behaviour is of paramount importance as failure and degradation tend to initiate from the surface. Electroless composite coating (NiP/SiC) was developed using SiC as reinforcing particles. As heat treatment plays a vital role in electroless nickel coating owing to the changes in microstructure, phase structure and mechanical properties, an insight at the interface changes in chemistry and micromechanical behaviour was investigated using scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) and microindentation techniques. Corrosion performance was analysed using electrochemical impedance spectroscopy (EIS). Absence of zinc and migration of copper at the interface was detected. Brittleness and microcracks was seen long the interface when indenting at load of 500 gf (Vickers). Corrosion performance is weaker than particles free coating. However, a thin blanket of NiP could enhance the resistance to corrosive medium.

Influence of service loading and the resulting micro-cracks on chloride resistance of concrete

Chloride-induced corrosion of steel in reinforced concrete structures is one of the main problems affecting their durability, but most previous research projects and case studies have focused on concretes without cracks or not subjected to any structural load. Although it has been recognised that structural cracks do influence the chloride transport and chloride induced corrosion in reinforced concrete structures, there is little published work on the influence of micro-cracks due to service loads on these properties. Therefore the effect of micro-cracks caused by loading on chloride transport into concrete was studied. Four different stress levels (0%, 25%, 50% and 75% of the stress at ultimate load – fu) were applied to 100 mm diameter concrete discs and chloride migration was measured using a bespoke test setup based on the NT BUILD 492 test. The effects of replacing Portland cement CEMI by ground granulated blast-furnace slag (GGBS), pulverised fuel ash (PFA) and silica fume (SF) on chloride transport in concrete under sustained loading were studied. The results have indicated that chloride migration coefficients changed little when the stress level was below 50% of the fu; however, it is desirable to keep concrete stress less than 25% fu if this is practical. The effect of removing the load on the change of chloride migration coefficient was also studied. A recovery of around 50% of the increased chloride migration coefficient was found in the case of concretes subjected to 75% of the fu when the load was removed.

Effect of reinforcement and heat treatment on elevated temperature sliding of electroless Ni–P/SiC composite coatings

The investigation is focused on the wear behaviour at elevated test temperature of composite Ni–P/SiC deposit, with varying concentration of the reinforcing SiC particles. The phase evolution measured by X-ray diffraction suggests slight crystallisation during wear testing at 200 °C. In coating without reinforcing particles, adhesive wear is accompanied by microcracks. The thermal heat generated and the cyclic loading could have induced sub-surface microcracks. Owing to the effective matrix-ceramics system in composite coatings, fine grooves, abrasive polishing and uniform wearing are observed. Reinforcing particles in the matrix hinder microcrack formation and significantly reduce the wear rate. Triboxidation is confirmed from energy dispersive X-ray spectrometry.

Development of Polymer Cement Composites

Research in the field of polymer modified cement has been carried out for the last 70 years or more. Polymers are mostly used to enhance durability and sustainability of cement concrete and in combination with classical construction materials a synergistic effect is obtained. In this work different polymers were added to Portland cement in various proportions and the mechanical and chemical resistance properties of the resultant composites when exposed to chemical environments were studied. Microstructural studies were also carried out to investigate the morphology of the composite and analyse the nature of interactions taking place between the cement and polymer phases. Though most polymers did not improve the compressive strength of the cement paste, it was found that they enhanced the resistance of the virgin cement paste to external chemical environments. The polymers seal the pores in the cement matrix and bridge the microcracks within the composite. Some of the polymers underwent chemical interactions with the cement paste thereby interfering in the hydration of cement. Polymers also decreased the leachability of water soluble components of virgin cement resulting in composites having improved durability. An attempt to correlate the structure of the polymers with the properties of the resultant composites is also presented.

Optimierung der laserinduzierten Plasmaspektroskopie an Metallen durch Femtosekunden-Doppelpulse für die Entwicklung eines hochauflösenden 3D-Rasterabbildungsverfahrens

Die laserinduzierte Plasmaspektroskopie (LIPS) ist eine spektrochemische Elementanalyse zur Bestimmung der atomaren Zusammensetzung einer beliebigen Probe. Für die Analyse ist keine spezielle Probenpräparation nötig und kann unter atmosphärischen Bedingungen an Proben in jedem Aggregatzustand durchgeführt werden. Femtosekunden Laserpulse bieten die Vorteile einer präzisen Ablation mit geringem thermischen Schaden sowie einer hohen Reproduzierbarkeit. Damit ist fs-LIPS ein vielversprechendes Werkzeug für die Mikroanalyse technischer Proben, insbesondere zur Untersuchung ihres Ermüdungsverhaltens. Dabei ist interessant, wie sich die initiierten Mikrorisse innerhalb der materialspezifschen Struktur ausbreiten. In der vorliegenden Arbeit sollte daher ein schnelles und einfach zu handhabendes 3D-Rasterabbildungsverfahren zur Untersuchung der Rissausbreitung in TiAl, einer neuen Legierungsklasse, entwickelt werden. Dazu wurde fs-LIPS (30 fs, 785 nm) mit einem modifizierten Mikroskopaufbau (Objektiv: 50x/NA 0.5) kombiniert, welcher eine präzise, automatisierte Probenpositionierung ermöglicht. Spektrochemische Sensitivität und räumliches Auflösungsvermögen wurden in energieabhängigen Einzel- und Multipulsexperimenten untersucht. 10 Laserpulse pro Position mit einer Pulsenergie von je 100 nJ führten in TiAl zum bestmöglichen Kompromiss aus hohem S/N-Verhältnis von 10:1 und kleinen Lochstrukturen mit inneren Durchmessern von 1.4 µm. Die für das Verfahren entscheidende laterale Auflösung, dem minimalen Lochabstand bei konstantem LIPS-Signal, beträgt mit den obigen Parametern 2 µm und ist die bislang höchste bekannte Auflösung einer auf fs-LIPS basierenden Mikro-/Mapping-Analyse im Fernfeld. Fs-LIPS Scans von Teststrukturen sowie Mikrorissen in TiAl demonstrieren eine spektrochemische Sensitivität von 3 %. Scans in Tiefenrichtung erzielen mit denselben Parametern eine axiale Auflösung von 1 µm. Um die spektrochemische Sensitivität von fs-LIPS zu erhöhen und ein besseres Verständnis für die physikalischen Prozesse während der Laserablation zu erhalten, wurde in Pump-Probe-Experimenten untersucht, in wieweit fs-Doppelpulse den laserinduzierten Abtrag sowie die Plasmaemission beeinflussen. Dazu wurden in einem Mach-Zehnder-Interferometer Pulsabstände von 100 fs bis 2 ns realisiert, Gesamtenergie und Intensitätsverhältnis beider Pulse variiert sowie der Einfluss der Materialparameter untersucht. Sowohl das LIPS-Signal als auch die Lochstrukturen zeigen eine Abhängigkeit von der Verzögerungszeit. Diese wurden in vier verschiedene Regimes eingeteilt und den physikalischen Prozessen während der Laserablation zugeordnet: Die Thermalisierung des Elektronensystems für Pulsabstände unter 1 ps, Schmelzprozesse zwischen 1 und 10 ps, der Beginn des Abtrags nach mehreren 10 ps und die Expansion der Plasmawolke nach über 100 ps. Dabei wird das LIPS-Signal effizient verstärkt und bei 800 ps maximal. Die Lochdurchmesser ändern sich als Funktion des Pulsabstands wenig im Vergleich zur Tiefe. Die gesamte Abtragsrate variiert um maximal 50 %, während sich das LIPS-Signal vervielfacht: Für Ti und TiAl typischerweise um das Dreifache, für Al um das 10-fache. Die gemessenen Transienten zeigen eine hohe Reproduzierbarkeit, jedoch kaum eine Energie- bzw. materialspezifische Abhängigkeit. Mit diesen Ergebnissen wurde eine gezielte Optimierung der DP-LIPS-Parameter an Al durchgeführt: Bei einem Pulsabstand von 800 ps und einer Gesamtenergie von 65 nJ (vierfach über der Ablationsschwelle) wurde eine 40-fache Signalerhöhung bei geringerem Rauschen erzielt. Die Lochdurchmesser vergrößerten sich dabei um 44 % auf (650±150) nm, die Lochtiefe um das Doppelte auf (100±15) nm. Damit war es möglich, die spektrochemische Sensitivität von fs-LIPS zu erhöhen und gleichzeitig die hohe räumliche Auflösung aufrecht zu erhalten.

Rate-dependent fracture toughness of polycrystalline ice

A series of three-point bend tests using single edge notched testpieces of pure polycrystalline ice have been performed at three different temperatures (–20°C, –30°C and –40°C). The displacement rate was varied from 1 mm/min to 100 mm/min, producing the crack tip strain rates from about 10–3 to 10–1 s–1. The results show that (a) the fracture toughness of pure polycrystalline ice given by the critical stress intensity factor (K IC) is much lower than that measured from the J—integral under identical conditions; (b) from the determination of K IC, the fracture toughness of pure polycrystalline ice decreases with increasing strain rate and there is good power law relationship between them; (c) from the measurement of the J—integral, a different tendency was appeared: when the crack tip strain rate exceeds a critical value of 6 × 10–3 s–1, the fracture toughness is almost constant but when the crack tip strain rate is less than this value, the fracture toughness increases with decreasing crack tip strain rate. Re-examination of the mechanisms of rate-dependent fracture toughness of pure polycrystalline ice shows that the effect of strain rate is related not only to the blunting of crack tips due to plasticity, creep and stress relaxation but also to the nucleation and growth of microcracks in the specimen.

Influence of Er,Cr : YSGG laser treatment on the microtensile bond strength of adhesives to dentin

Purpose: In light of the concept of minimally invasive dentistry, erbium lasers have been considered as an alternative technique to the use of diamond burs for cavity preparation. The purpose of this study was to assess the bonding effectiveness of adhesives to Er,Cr:YSGG laser-irradiated dentin using irradiation settings specific for cavity preparation. Materials and Methods: Fifty-four midcoronal dentin surfaces, obtained from sound human molars, were irradiated with an Er,Cr:YSGG laser or prepared with a diamond bur using a high-speed turbine. One etch-and-rinse (Optibond FL/Kerr) and three self-etching adhesives (Adper Prompt L-Pop/3M ESPE, Clearfil SE Bond/Kuraray, and Clearfil S-3 Bond/Kuraray) were used to bond the composite to dentin. The microtensile bond strength (mu TBS) was determined after 24 h of storage in water at 37 degrees C. The Kruskal-Wallis test was used to determine pairwise statistical differences (p < 0.05). Prepared dentin surfaces, adhesive interfaces, and failure patterns were analyzed using a stereo microscope and Field-emission gun Scanning Electron Microscopy (Feg-SEM). Results: Significantly lower mu TBS was observed to laser-irradiated than to bur-cut dentin (p < 0.05), irrespective of the adhesive employed. Feg-SEM photomicrographs of lased dentin revealed an imbricate patterned substrate and the presence of microcracks at the dentin surface. Conclusion: Morphological alterations produced by Er,Cr:YSGG laser-irradiation adversely influence the bonding effectiveness of adhesives to dentin. Keywords: dentin, adhesion, adhesives, laser, ErCr:YSGG.

Efeito da adição de microfibras de lã de vidro na tenacidade à ruptura de pastas de cimento para poços de petróleo

Although there are a wide variety of additives that act in fresh state, to adjust the properties of cement, there is also a search by additions that improve the tenacity of the cement in the hardened state. This, in turn, can often be increased by inserting fibers, which act on the deflection of microcracks. This study aimed to use a microfiber glass wool (silica-based) as an additive reinforcing the cement matrix, improving the rupture tenacity, in order to prevent the propagation of microcracks in the cement sheath commonly found in oil wells submitted to high temperatures. The fibers were added at different concentrations, 2 to 5% (BWOC) and varied average sizes, grinding for 90 s, 180 s, 300 s, 600 s. The cement slurries were made with a density of 1,90 g/ cm3 (15,6 lb/gal), using Portland cement CPP- Special Class as the hydraulic binder and 40% silica flour. The characterization of the fiber was made by scanning electron microscopy (SEM), particle size by sieving, X-ray fluorescence (XRF), X-ray diffraction (XRD) and thermogravimetry (TG / DTG). Were performed technological tests set by the API (American Petroleum Institute) by rheology, stability, free water, compressive strength, as well as testing rupture energy, elastic modulus and permeability. The characterization results showed good thermal stability of the microfiber glass wool for application in oil wells submitted to steam injection and, also, that from the particle size data, it was possible to suggest that microfibers milled up to 300 s, are ideal to act as reinforcement to the cement slurries. The rheological parameters, there was committal of plastic viscosity when larger lengths were inserted of microfiber (F90). The values obtained by free water and stability were presented according to API. The mechanical properties, the incorporation of microfiber to the cement slurries gave better rupture tenacity, as compared to reference cement slurries. The values of compressive strength, elastic modulus and permeability have been maintained with respect to the reference cement slurries. Thus, cement slurries reinforced with microfiber glass wool can ensure good application for cementing oil wells submitted to steam injection, which requires control of microcracks, due to the thermal gradients

Avaliação microscópica dos fragmentos ósseos obtidos por diferentes métodos de osteotomia e de irrigação em aloenxertos irradiados e congelados de coelho

Oral and facial bone defects can undertake appearance, psychosocial well-being and stomathognatic function of its patients. Over the yerars several strategies for bone defect regeneration have arised to treat these pathologies, among them the use of frozen and irradiated bone allograft. Manipulation of bone grafts it s not determined yet, and several osteotomy alternatives can be observed. The present work evaluated with a microscope the bone fragments obtained from different osteotomy methods and irrigation on rings and blocks allografts irradiated and frozen at 80° negative in a rabbit model. The study is experimental in vitro and it sample was an adult male New Zealand rabbit. The animal was sacrificed to obtain long bones, that were submitted to freezing at 80º negative and irradiated with Cobalt- 60. Then the long bones were sectioned into 24 bone pieces, divided into 4 groups: G1 (n=06) osteotomy was performed with bur No. 6 forming rings with 5 mm thickness with high-speed handpiece with manual irrigation; G2 (n=06) osteotomy was performed with bur No. 6 forming rings with 5 mm thick with surgical motor with a manual irrigation rotation 1500 rpm; GA (n=06), osteotomy with trephine using manual irrigation with saline; and GB (n=06), osteotomy with trephine using saline from peristaltic pumps of surgical motor. Five bone pieces of each group were prepared for analysis on light microscopy (LM) and one on electronic scan electronic microscopy (SEM). On the SEM analysis edges surface, presence of microcracks and Smear Layer were evaluated. Analyzing osteotomy technics on SEM was observed: increased presence of microcracks cutting with high speed; increased presence of areas covered by Smear Layer when cutting with motor implant. The irrigation analysis with SEM was observed: that the presence of microcracks does not depend on the type of irrigation; on manual irrigation, there was greater discrepancy between the cutting lines. The descriptive analysis of the osteotomy and irrigation process on LM showed: histological analysis showing the bony margins with clear tissue changed layer, composed of blackened tissue of charred appearance near to the cortical bone; on the edges of the bony part, bone fragments that were displaced during the bone cut and bone irregularities were observed. After analysis of results we can conclude: that there was greater regularity of the bone cut using high-speed handpiece than using motor implant; the cut with trephine using saline irrigated from peristaltic pumps of surgical motor showed greater homogeneity when compared with manual irrigation; charred tissue was found in all obtained bone samples, whit no significant statistically difference on the proportion of carbonization of the two analysed technics

Nanoindentation mechanical properties characterization of glassy polymeric carbon treated with ion beam

Phenolic resins when heat treated in inert atmosphere up to 1000 degreesC become glassy polymeric carbon (GPC), a chemically inert and biocompatible material useful for medical applications, such as in the manufacture of heart valves and prosthetic devices. In earlier work we have shown that ion bombardment can modify the surface of GPC, increasing its roughness. The enhanced roughness, which depends on the species, energy and fluence of the ion beam, can improve the biocompatibility of GPC prosthetic artifacts. In this work, ion bombardment was used to make a layer of implanted ions under the surface to avoid the propagation of microcracks in regions where cardiac valves should have pins for fixation of the leaflets. GPC samples prepared at 700 and 1500 degreesC were bombarded with ions of silicon. carbon, oxygen and gold at energies of 5, 6, 8 and 10 MeV, respectively, and fluences between 1.0 x 10(13) and 1.0 x 10(16) ions/cm(2). Nanoindentation hardness characterization was used to compare bombarded with non-bombarded samples prepared at temperatures up to 2500 degreesC. The results with samples not bombarded showed that the hardness of GPC increases strongly with the heat treatment temperature. Comparison with ion bombarded samples shows that the hardness changes according to the ion used, the energy and fluence. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Effects of surface treatments on the fatigue strength of AISI 4340 aeronautical steel

Internal residual stresses significantly influence the fatigue strength of coated materials. It is well known that chromium plating is the most used electrodeposited coating for important industrial applications. However, pressure to identify alternatives or to improve the chromium electroplating process have increased in recent years, related to the reduction in fatigue strength of the base material and to environmental requirements. The high efficiency and fluoride free hard chromium electroplating there called accelerated) is an improvement to the conventional process. One environmentally safer and cleaner alternative to hard chromium plating is tungsten carbide thermal spray coating applied by the High Velocity Oxy-Fuel (HVOF) process. To increase the fatigue strength of chromium plated materials, coating thickness and microcracks density are important parameters to be controlled. Techniques as compressive residual stresses induced by shot peening and multilayers, are also used. The aim of this study was to analyse the effects on AISI 4340 steel, in the rotating bending fatigue behaviour, of the: tungsten carbide thermal spray coating applied by HP/HVOF process; chemical nickel underplate, and shot peening process applied before coating deposition, in comparison to hard chromium electroplatings. Rotating bending fatigue test results indicate better performance for the conventional hard chromium plating in relation to the accelerated hard chromium electroplating. Tungsten carbide thermal spray coating and accelerated hard chromium plate over nickel resulted in higher fatigue strength when compared to samples conventional or accelerated hard chromium plated. Shot peening showed to be an excellent alternative to increase fatigue strength of AISI 4340 steel hard chromium electroplated. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Improvement in the fatigue strength of chromium electroplated AISI 4340 steel by shot peening

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Evaluation of WC-10Ni thermal spraying coating by HVOF on the fatigue and corrosion AISI 4340 steel

Shot peening is a surface process widely used to improve the fatigue strength of materials, through compressive residual stresses induced in their surface layers. Considering mechanical components for high responsible applications, wear and corrosion control is currently accomplished by the use of coated materials.In the case of chrome plating or hard anodizing, lower fatigue strength in comparison to uncoated parts are associated to high residual tensile stresses and microcracks density. Under constant or variable amplitude loading microcracks will propagate and cross the interface coating substrate without impediment.The aim of the present study is to analyze the influence of WC-10Ni coating applied by HVOF process on the axial fatigue strength of AISI 4340 steel. The shot peening effect on the fatigue performance of coated AISI 4340 steel was also evaluated. The fractured fatigue specimens were investigated using a scanning electron microscope in order to obtain information about the crack initiation points. (C) 2010 Published by Elsevier Ltd.