RESUMO
The elemental distribution within a Ti-Si-Al-C-N coating grown by physical vapour deposition on a Cr-doped WC-Co cemented carbide substrate has been investigated by atom probe tomography. Special attention was paid to the coating/substrate interface region. The results indicated a diffusion of substrate binder phase elements into the Ti-N adhesion layer. The composition of this layer, and the Ti-Al-N interlayer present between the adhesion layer and the main Ti-Si-Al-C-N layer, appeared to be sub-stoichiometric. The analysis of the interlayer showed the presence of internal surfaces, possibly grain boundaries, depleted in Al. The composition of the main Ti-Al-Si-C-N layer varied periodically in the growth direction; layers enriched in Ti appeared with a periodicity of around 30 nm. Laser pulsing resulted in a good mass resolution that made it possible to distinguish between N(+) and Si(2+) at 14 Da.
RESUMO
Compared to atom probe analysis of metallic materials, the analysis of carbide phases results in an enhanced formation of molecular ions and multiple events. In addition, many multiple events appear to consist of two or more ions originating from adjacent sites in the material. Due to limitations of the ion detectors measurements generally underestimate the carbon concentration. Analyses using laser-pulsed atom probe tomography have been performed on SiC, WC, Ti(C,N) and Ti(2)AlC grains in different materials as well as on large M(23)C(6) precipitates in steel. Using standard evaluation methods, the obtained carbon concentration was 6-24% lower than expected from the known stoichiometry. The results improved remarkably by using only the (13)C isotope, and calculating the concentration of (12)C from the natural isotope abundance. This confirms that the main reason for obtaining a too low carbon concentration is the dead time of the detector, mainly affecting carbon since it is more frequently evaporated as multiple ions. In the case of Ti(C,N) and Ti(2)AlC an additional difficulty arises from the overlap between C(2)(+), C(4)(2+) and Ti(2+) at the mass-to-charge 24 Da.
RESUMO
Burgers vectors of matrix dislocations in mullite have been determined by the defocus large-angle convergent beam electron diffraction technique. Vectors of the types [100], [010], [110] and [112] were identified. These Burgers vectors are discussed in relation to the open channels and the oxygen vacancy distribution in the mullite structure. It is suggested that a short-range ordering of oxygen vacancies may account for a Burgers vector of the type [112].
RESUMO
This study was performed to examine whether a clinical classification of different phenotypes of amelogenesis imperfecta could be discernible at the ultrastructural level. Seventeen primary teeth from 16 children with hypomineralization, hypomaturation, or hypoplastic variants of the disease were collected for histologic studies of the enamel by means of polarized light microscopy, scanning electron microscopy (SEM), and secondary ion mass spectrometry (SIMS). Polarization microscopy showed that the enamel was hypomineralized; in six teeth a wavy configuration of the enamel prisms also appeared. Three histomorphologic main types could be discerned. In 10 of the teeth extensive hypomineralization of the bulk of the enamel was found. One tooth had an unusually thick enamel with only a thin normally mineralized surface layer. SIMS images showed less pronounced signals from Ca2+ and Na+ but with stronger signals from Cl- and CN-, representing the organic component of enamel. The SEM images showed an irregular prism pattern with marked interprismatic areas. Irrespective of the clinical appearance or the hereditary pattern the main findings were hypomineralized enamel with or without wavy bands. Neither of the analytical methods used in this paper distinguishes between the clinical phenotypes of amelogenesis imperfecta.
