974 resultados para Microscopy of materials


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Polymethyl methacrylate (PMMA) bone cement–multiwalled carbon nanotube (MWCNT) nanocomposites with a weight loading of 0.1% were prepared using 3 different methods of MWCNT incorporation. The mechanical and thermal properties of the resultant nanocomposite cements were characterised in accordance with the international standard for acrylic resin cements. The mechanical properties of the resultant nanocomposite cements were influenced by the type of MWCNT and method of incorporation used. The exothermic polymerisation reaction for the PMMA bone cement was significantly reduced when thermally conductive functionalised MWCNTs were added. This reduction in exotherm translated in a decrease in thermal necrosis index value of the respective nanocomposite cements, which potentially could reduce the hyperthermia experienced in vivo. The morphology and degree of dispersion of the MWCNTs in the PMMA matrix at different scales were analysed using scanning electron microscopy. Improvements in mechanical properties were attributed to the MWCNTs arresting/retarding crack propagation through the cement by providing a bridging effect into the wake of the crack, normal to the direction of crack growth. MWCNT agglomerations were evident within the cement microstructure, the degree of these agglomerations was dependent on the method used to incorporate the MWCNTs into the cement.

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Poly (methyl methacrylate) (PMMA) bone cement—multi walled carbon nanotube (MWCNT) nanocomposites with weight loadings ranging from 0.1 to 1.0 wt% were prepared. The MWCNTs investigated were unfunctionalised, carboxyl and amine functionalised MWCNTs. Mechanical properties of the resultant nanocomposite cements were characterised as per international standards for acrylic resin cements. These mechanical properties were influenced by the type and wt% loading of MWCNT used. The morphology and degree of dispersion of the MWCNTs in the PMMA matrix at different length scales were examined using field emission scanning electron microscopy. Improvements in mechanical properties were attributed to the MWCNTs arresting/retarding crack propagation through the cement by providing a bridging effect and hindering crack propagation. MWCNTs agglomerations were evident within the cement microstructure, the degree of these agglomerations was dependent on the weight fraction and functionality of MWCNTs incorporated into the cement.

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The strategic incorporation of bioresorbable polymeric additives to calcium-deficient hydroxyapatite cement may provide short-term structural reinforcement and modify the modulus to closer match bone. The longer-term resorption properties may also be improved, creating pathways for bone in-growth. The aim of this study was to investigate the resorption process of a calcium phosphate cement system containing either in polyglycolic acid tri-methylene carbonate particles or polyglycolic acid fibres. This was achieved by in vitro aging in physiological conditions (phosphate buffered solution at 37°C) over 12 weeks. The unreinforced CPC exhibited an increase in compressive strength at 12 weeks, however catastrophic failure was observed above a critical loading. The fracture behaviour of cement was improved by the incorporation of PGA fibres; the cement retained its cohesive structure after critical loading. Gravimetric analysis and scanning electron microscopy showed a large proportion of the fibres had resorbed after 12 weeks allowing for the increased cement porosity, which could facilitate cell infiltration and faster integration of natural bone. Incorporating the particulate additives in the cement did not provide any mechanism for mechanical property augmentation or did not demonstrate any appreciable level of resorption after 12 weeks.

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The light emission spectrum from a scanning tunnelling microscope (LESTM) is investigated as a function of relative humidity and shown to provide a novel and sensitive means for probing the growth and properties of a water meniscus on the nanometre scale. An empirical model of the light emission process is formulated and applied successfully to replicate the decay in light intensity and spectral changes observed with increasing relative humidity. The modelling indicates a progressive water filling of the tip-sample junction with increasing humidity or, more pertinently, of the volume of the localized surface plasmons responsible for light emission; it also accounts for the effect of asymmetry in structuring of the water molecules with respect to the polarity of the applied bias. This is juxtaposed with the case of a non-polar liquid in the tip-sample nanocavity where no polarity dependence of the light emission is observed. In contrast to the discrete detection of the presence/absence of a water bridge in other scanning probe experiments through measurement of the feedback parameter for instrument control, LESTM offers a means of continuously monitoring the development of the water bridge with sub-nanometre sensitivity. The results are relevant to applications such as dip-pen nanolithography and electrochemical scanning probe microscopy.

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A maraging steel with a composition of Fe–12·94Ni–1·61Al–1·01Mo–0·23Nb (wt-%) was investigated. Optical, scanning electron and transmission electron microscopy and X-ray diffraction analysis were employed to study the microstructure of the steel after different aging periods at temperatures of 450–600°C. Hardness and Charpy impact toughness of the steel were measured. The study of microstructure and mechanical properties showed that nanosized precipitates were formed homogeneously during the aging process, which resulted in high hardness. As the aging time is prolonged, precipitates grow and hardness increases. Fractography of the as forged steel has shown mixed ductile and brittle fracture and has indicated that the steel has good toughness. Relationships among heat treatment, microstructure and mechanical properties are discussed. Further experiments using tensile testing and impact testing for aged steel were carried out.

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The microstructure evolution of a 10Cr ferritic/martensitic heat-resistant steel during creep at 600°C was investigated in this work. Creep tests demonstrated that the 10Cr steel had higher creep strength than conventional ASME-P92 steel at 600°C. The microstructure after creep was studied by transmission electron microscopy, scanning electron microscopy and electron probe microanalysis. It was revealed that the martensitic laths were coarsened with time and eventually developed into subgrains after 8354 h. Laves phase was observed to grow and cluster along the prior austenite grain boundaries during creep and caused the fluctuation of solution and precipitation strengthening effects, which was responsible for the two slope changes on the creep rupture strength vs rupture time curve. It was also revealed that the microstructure evolution could be accelerated by stress, which resulted in the lower hardness in the deformed part of the creep specimen, compared with the aging part.

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A convenient microwave method in preparation of zinc oxide nanoparticles (ZnONPs) using an ionic liquid, trihexyltetradecylphosphonium bis{(trifluoromethyl)sulfonyl}-imide, [P-66614][NTf2], as a green solvent is described in this paper. To the best of our knowledge, there is no report for synthesizing any nanoparticle using this ionic liquid. Trihexyltetradecylphosphonium bis{(trifluoromethyl)sulfonyl}-imide has low interface tension and thus it can enhance the nucleation rate, which is favorable to the formation of smaller ZnONPs. The fabricated ZnONPs were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and UV-vis spectroscopy. The XRD pattern reveals that the ZnONPs have hexagonal wurtzite structure. The strong intensity and narrow width of ZnO diffraction peaks indicate that the resulting nanoparticles are of high crystallinity. The synthesized ZnONPs show direct band gap of 3.43 eV. The UV-vis absorption spectrum of ZnONPs dispersed in ethylene glycol at room temperature revealed a blue-shifted onset of absorption. (C) 2011 Elsevier Ltd. All rights reserved.

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Ethanol adsorption-desorption isotherms on well-organized mesoporous silica and titania films with hexagonal pores structure were studied by ellipsometric porosimetry. The mesopore volume Was calculated from the change of the effective refractive index at the end points of the isotherm. An improved Derjaguin-Broekhoff-de Boer (IDBdB) model for cylindrical pores is proposed for the determination of the pore size. In this model, the disjoining pressure isotherms were obtained by measuring the thickness of the ethanol film on a non-porous film with the same chemical composition. This approach eliminates uncertainties related to the application of the statistical film thickness determined via t-plots in previous versions of the DBdB model. The deviation in the surface tension of ethanol in the mesopores from that of a flat interface was described by the Tolman parameter in the Gibbs-Tolman-Koening-Buff equation. A positive value of the Tolman parameter of 0.2 nm was found from the fitting of the desorption branch of the isotherms to the experimental data obtained by Low Angle X-ray Diffraction (LA-XRD) and Transmission Electron Microscopy (TEM) measurements in the range of pore diameters between 2.1 and 8.3 nm. (C) 2009 Elsevier Inc. All rights reserved.

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Austenitization with lower temperature and intercritical annealing were introduced in the treatment of a maraging steel with a composition of Fe–12.94Ni–1.61Al–1.01Mo–0.23Nb (wt.%). Scanning electron microscopy was employed to study the microstructure after austenitization at 950 °C and intercritical annealing, followed by aging at 485 and 600 °C. X-ray diffraction (XRD) analysis was applied to evaluate the formation of retained or reverted austenite. Thermodynamic calculation was employed to calculate equilibrium phase mole fractions. Hardness and Charpy impact toughness of the steel were measured. Intercritical annealing treatments did not result in significant increase of hardness either before or after aging. The Charpy impact toughness of the alloy in aged condition was enhanced after austenitization at 950 °C. No austenite was observed in XRD. However, suspected reverted austenite was found after austenitization at 950 °C followed by aging at 600 °C for 4 h. Relationships among heat treatment, microstructure and mechanical properties are discussed.

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Thin (50-500 nm) films of TiO2 may be deposited on glass substrates by the atmospheric pressure chemical vapor deposition (APCVD) reaction of TiCl4 with ethyl acetate at 400600 C. The TiO2 films are exclusively in the form of anatase, as established by Raman microscopy and glancing angle X-ray diffraction. X-ray photoelectron spectroscopy gave a 1:2 Ti:O ratio with Ti 2P(3/2) at 458.6 eV and O 1s is at 530.6 eV. The water droplet contact angle drops from 60degrees to

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Probing the functionality of materials locally by means of scanning probe microscopy (SPM) requires a reliable framework for identifying the target signal and separating it from the effects of surface morphology and instrument non-idealities, e.g. instrumental and topographical cross-talk. Here we develop a linear resolution theory framework in order to describe the cross-talk effects, and apply it for elucidation of frequency-dependent cross-talk mechanisms in piezoresponse force microscopy. The use of a band excitation method allows electromechanical/electrical and mechanical/topographic signals to be unambiguously separated. The applicability of a functional fit approach and multivariate statistical analysis methods for identification of data in band excitation SPM is explored.

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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.