Grain size measurements in Mg-Al high pressure die castings using electron back-scattered diffraction (EBSD)

Optical metallographic techniques for grain-size measurement give unreliable results for high pressure diecast Mg-Al alloys and electron back-scattered diffraction mapping (EBSD) provides a good tool for improving the quality of these measurements. An application of EBSD mapping to this question is described, and data for some castings are presented. Ion-beam milling was needed to prepare suitable samples, and this technique is detailed. As is well-known for high pressure die castings, the grain size distribution comprises at least two populations. The mean grain size of the fine-grained population was similar in both AZ91 and AM60 and in two casting thicknesses (2 mm and 5 mm) and, contrary to previously published reports, it did not vary with depth below the surface.

Yielding Behaviour of Electron Beam Lithography and Focused Ion Beam Made Nanocrystalline Micro/Nanopillars

Electron beam lithography (EBL) and focused ion beam (FIB) methods were developed in house to fabricate nanocrystalline nickel micro/nanopillars so to compare the effect of fabrication on plastic yielding. EBL was used to fabricate 3 μm and 5 μm thick poly-methyl methacrylate patterned substrates in which nickel pillars were grown by electroplating with height to diameter aspect ratios from 2:1 to 5:1. FIB milling was used to reduce larger grown pillars to sizes similar to EBL grown pillars. X-ray diffraction, electron back-scatter diffraction, scanning electron microscopy, and FIB imaging were used to characterize the nickel pillars. The measured grain size of the pillars was 91±23 nm, with strong <110> and weaker <111> and <110> crystallographic texture in the growth. Load-controlled compression tests were conducted using a MicroMaterials nano-indenter equipped with a 10 μm flat punch at constant rates from 0.0015 to 0.03 mN/s on EBL grown pillars, and 0.0015 and 0.015 mN/s on FIB-milled pillars. The measured Young’s modulus ranged from 55 to 350 GPa for all pillars, agreeing with values in the literature. EBL grown pillars exhibited stochastic strain-bursts at slow loading rates, attributed to local micro yield events, followed by work hardening. Sharp yield points were also observed and attributed to the gold seed layer de-bonding between the nickel pillar and substrate due to the shear stress associated with end effects that arise from the substrate constraint. The onset of yield ranged from 108 to 1800 MPa, which is greater than bulk nickel, but within values given in the literature. FIB-milled pillars demonstrated stochastic yield behaviour at all loading rates tested, yielding between 320 and 625 MPa. Deformation was apparent at FIB-milled pillar tops, where the smallest cross-sectional area was measured, but still exhibited superior yield strength to bulk nickel. The gallium damage at the outer surface of the pillars likely aids in dislocation nucleation and plasticity, leading to lower yield strengths than for the EBL pillars. Thermal drift, substrate effects, and noise due to vibrations within the indenter system contributed to variance and inconsistency in the data.

Mesoscale plasticity anisotropy at the earliest stages of cavitation-erosion damage of a high nitrogen austenitic stainless steel

A high nitrogen austenitic stainless steel (0.9wt% N) and an ordinary 304 austenitic stainless steel were submitted to cavitation-erosion tests in a vibratory apparatus operating at a frequency of 20 kHz. The high nitrogen stainless steel was obtained by high temperature gas nitriding a 1-mm thick strip of an UNS 31803 duplex stainless steel. The 304 austenitic stainless steel was used for comparison purposes. The specimens were characterized by scanning electron microscopy and Electron Back Scatter Diffraction. The surface of the cavitation damaged specimens was analyzed trying to find out the regions where cavitation damage occurred preferentially. The distribution of sites where cavitation inception occurred was extremely heterogeneous, concentrating basically at (i) slip lines inside some grains and (ii) Sigma-3 coincidence site lattice (CSL) boundaries (twin boundaries). Furthermore, it was observed that the CE damage spread faster inside those grains which were more susceptible to damage incubation. The damage heterogeneity was addressed to plasticity anisotropy. Grains in which the crystallographic orientation leads to high resolved shear stress show intense damage at slip lines. Grain boundaries between grains with large differences in resolved shear stress where also intensely damaged. The relationship between crystallite orientation distributions, plasticity anisotropy and CE damage mechanisms are discussed. (C) 2009 Elsevier B.V. All rights reserved.

Eutectic solidification mode in sodium modified Al-7 mass %Si-3.5 mass %Cu-0.2 mass %Mg casting alloys

The influence of sodium (Na) on nucleation and growth of the Al-Si eutectic in a commercial hypoeutectic Al-Si-Cu-Mg foundry alloy has been investigated. The microstructural evolution during eutectic solidification was studied by a quenching technique. By comparing the orientation of the aluminium in the eutectic to that of the surrounding primary aluminium dendrites by EBSD, the eutectic solidification mode could be determined. The results show that the eutectic solidification starts near the mould wall and evolves with front growth opposite the thermal gradient on a macro-scale, and on a micro-scale with independent heterogeneous nucleation of eutectic grains in interdendritic spaces. Na-modified alloys therefore behave significantly differently from those modified by other elemental additions.

Ocean acidification reduces the crystallographic control in juvenile mussel shells

Global climate change threatens the oceans as anthropogenic carbon dioxide causes ocean acidification and reduced carbonate saturation. Future projections indicate under saturation of aragonite, and potentially calcite, in the oceans by 2100. Calcifying organisms are those most at risk from such ocean acidification, as carbonate is vital in the biomineralisation of their calcium carbonate protective shells. This study highlights the importance of multi-generational studies to investigate how marine organisms can potentially adapt to future projected global climate change. Mytilus edulis is an economically important marine calcifier vulnerable to decreasing carbonate saturation as their shells comprise two calcium carbonate polymorphs: aragonite and calcite. M. edulis specimens were cultured under current and projected pCO2 (380, 550, 750 and 1000 µatm), following 6 months of experimental culture, adults produced second generation juvenile mussels. Juvenile mussel shells were examined for structural and crystallographic orientation of aragonite and calcite. At 1000 µatm pCO2, juvenile mussels spawned and grown under this high pCO2 do not produce aragonite which is more vulnerable to carbonate under-saturation than calcite. Calcite and aragonite were produced at 380, 550 and 750 µatm pCO2. Electron back scatter diffraction analyses reveal less constraint in crystallographic orientation with increased pCO2. Shell formation is maintained, although the nacre crystals appear corroded and crystals are not so closely layered together. The differences in ultrastructure and crystallography in shells formed by juveniles spawned from adults in high pCO2 conditions may prove instrumental in their ability to survive ocean acidification.

Solidification mechanisms of unmodified and strontium-modified hypereutectic aluminium-silicon alloys

The effects of strontium on the solidi. cation mode of hypereutectic aluminium-silicon alloys have been studied. Samples were prepared from an aluminium-17wt% silicon-based alloy and strontium was added at several different concentrations. The development of the microstructure was investigated by cooling curve analysis, interrupted solidi. cation experiments and optical and scanning electron microscopy. It was found that nucleation of primary silicon is suppressed by additions of strontium. The suppressed nucleation results in supersaturation of the liquid prior to nucleation, and an increased growth rate after nucleation. As a result, the silicon crystals become less faceted and more dendritic with increasing strontium additions. Increasing the strontium concentration slightly refined the eutectic spacing and introduced a small amount of fibrous silicon. Electron back-scatter diffraction measurements were performed to determine the crystallographic relation between the primary and eutectic silicon phases. The eutectic silicon in the unmodified alloy does not have any crystallographic relationship with the primary silicon crystals. In contrast, the eutectic silicon crystals in the strontium-modified alloys often share an identical or twin relationship with nearby primary silicon crystals. The incidence of twinning within primary silicon crystals was relatively low and did not appear to increase with strontium additions.

Determination of eutectic solidification mode in Sr-modified hypoeutectic Al-Si alloys by EBSD

The effect of eutectic modification by strontium on nucleation and growth of the eutectic in hypoeutectic Al-Si foundry alloys has been investigated by electron back-scattering diffraction (EBSD) mapping. Specimens were prepared from three hypoeutectic AlSi base alloys with 5, 7 and 10 mass%Si and with different strontium contents up to 740 ppm for modification of eutectic silicon. By comparing the orientation of the aluminium in the eutectic to that of the surrounding primary aluminium dendrites? the growth mode of the eutectic could be determined. The mapping results indicate that the eutectic grew from the primary phase in unmodified alloys. When the eutectic was modified by strontium, eutectic grains nucleated separately from the primary dendrites. However, in alloys with high strontium levels, the eutectic again grew from the primary phase. These observed effects of strontium additions on the eutectic solidification mode are independent of silicon content in the range between 5 and 10 mass%Si.

Eutectic growth mode in strontium, antimony and phosphorus modified hypoeutectic Al-Si foundry alloys

The effect of strontium (Sr), antimony (Sb) and phosphorus (P) on nucleation and growth mode of the eutectic in hypoeutectic Al-10 mass%Si alloys has been investigated by electron back-scattering diffraction (EBSD) mapping. Specimens were prepared from a hypoeutectic Al-10 mass%Si base alloy, adding different levels of strontium, antimony and phosphorus for modification of eutectic silicon. By comparing the orientation of the aluminium in the eutectic to that of the surrounding primary aluminium dendrites, the solidification mode of the eutectic could be determined. The results of these studies show that the eutectic nucleation mode, and subsequent growth mode, is strongly dependent on additive elements. The EBSD mapping results indicate that the eutectic grew from the primary phase in unmodified and phosphorus-containing alloys. When the eutectic was modified by strontium or antimony, eutectic grains nucleated and grew separately from the primary dendrites.

Mecanismos de deformación en aceros inoxidables austeníticos metaestables

La deformación plástica puede inducir a la transformación de la austenita a martensita en los aceros inoxidables austeníticos metaestables. Para analizar este hecho, el inoxidable austenítico metaestable grado AISI 301 LN fue estudiado en dos condiciones diferentes: recocido y laminado en frío. En el primer caso, el acero era completamente austenítico, mientras que después de la laminación presentaba un importante porcentaje de α’-martensita. Se evaluó el cambio de fase cuando el acero es sometido a ensayos monotónicos y cíclicos, así como cuando ha sido modificada la superficie mediante el granallado o se han realizado tratamientos térmicos de reversión. Se utilizaron diferentes técnicas de caracterización microestructural para detectar y cuantificar la martensita, como microscopía óptica, difracción de rayos-X (DRX) y difracción de electrones retrodispersados (EBSD); como también de caracterización mecánica para evaluar el comportamiento de los aceros, trabajo esencial de fractura (TEF), conformabilidad, fatiga de alto número de ciclos (HCF) y nanoindentación. Los resultados mostraron un incremento en la resistencia mecánica del acero laminado en comparación al acero recocido; este hecho está relacionado con la presencia de martensita originada por la laminación. Sin embargo, en términos de deformación y endurecimiento el acero recocido presenta un mejor desempeño como consecuencia del elevado porcentaje de fase austenítica. Así mismo, revertir la martensita de laminación a austenita y refinar la austenita presente permite obtener un acero con una propiedades mecánicas similares a cuando esta en la condición laminado.

Orientation dependence of stored energy of cold work in semi-processed electrical steels after temper rolling

Microhardness measurements were carried out in a low carbon lamination steel after 6% of temper rolling, in order to evaluate local variations of work hardening as a function of crystallographic orientation. EBSD (electron back scattered diffraction) was used to determine grain orientations with respect to individual rolling planes and rolling directions. Hardness was shown to increase with the local Taylor factor. TEM observations and a well-known dislocation hardening model were used to confirm the equivalence between hardness values and the stored energy of cold work. A definite correlation between stored energy and Taylor factors could therefore be established, being more consistent than previous data reported in the literature. The improvement was thought to be related to the rather small plastic deformation, during which Taylor factors could be considered to remain constant. (c) 2006 Elsevier B.V. All rights reserved.

Interaction between recrystallization and strain-induced precipitation in a high Nb- and N-bearing austenitic stainless steel: influence of the interpass time

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Microanalysis of quenched and self-extinguished aluminium rods burned in oxygen

Promoted ignition tests and quench tests have been conducted and analysed for 3.2 mm aluminum rods in 99.995% oxygen. Tests have been conducted in oxygen pressures varying from 538 kPa to 773 kPa. Samples that self-extinguished or were quenched were selected for further analysis. The microstructure of the selected samples were analysed by electron microscopy, using energy dispersive spectrometry and electron back-scatter techniques, to identify and visualize, respectively, the species present. The grain structures of these samples were etched, viewed and photographed under polarized light by an optical microscope. From the micrographs produced by the post-test analysis, clearly defined boundaries between the oxide and the melted and resolidified metal have been observed. In both the melted and resolidified metal and the oxide layer, significant numbers of gas bubbles, solid inclusions and several diffuse oxide bubbles have been captured during the cooling process. It is concluded that convective movement is occurring within the molten drop and that analysis of quenched samples provides more useful information on the state of the burning droplet than samples allowed to cool slowly to room temperature. Recommendations are made regarding future investigations into aluminum burning, focusing on the transport of reactants through the liquid oxide layer.

Progetto di un sistema a microcontrollore per modulazione back-scattering uwb

La tesi tratta il progetto di una piattaforma di simulazione per modulazioni back-scatter UWB su un sistema a microcontrollore PIC. Il sistema utilizza uno switch a UWB per eseguire la modulazione, modificando le condizioni di carico d'antenna; il software implementa la modulazione attraverso la variazione del segnale di controllo dello switch e si interfaccia con l'utente attraverso l'uso di una periferica USB, permettendo la modifica runtime della configurazione. Si interfaccia inoltre con strumenti esterni attraverso segnali di sincronizzazione.

Structural characterization of intermediate and metastable phases by electron microscopy

Structure characterization of nanocrystalline intermediates and metastable phases is of primary importance for a deep understanding of synthetic processes undergoing solid-to-solid state phase transitions. Understanding the evolution from the first nucleation stage to the final synthetic product supports not only the optimization of existing processes, but might assist in tailoring new synthetic paths. A systematic investigation of intermediates and metastable phases is hampered because it is impossible to produce large crystals and only in few cases a pure synthetic product can be obtained. Structure investigation by X-ray powder diffraction methods is still challenging on nanoscale, especially when the sample is polyphasic. Electron diffraction has the advantage to collect data from single nanoscopic crystals, but is limited by data incompleteness, dynamical effects and fast deterioration of the sample under the electron beam. Automated diffraction tomography (ADT), a recently developed technique, making possible to collect more complete three-dimensional electron diffraction data and to reduce at the same time dynamical scattering and beam damage, thus allowing to investigate even beam sensitive materials (f.e. hydrated phases and organics). At present, ADT is the only technique able to deliver complete three-dimensional structural information from single nanoscopic grains, independently from other surrounding phases. Thus, ADT is an ideal technique for the study of on-going processes where different phases exist at the same time and undergo several structural transitions. In this study ADT was used as the main technique for structural characterization for three different systems and combined subsequently with other techniques, among which high-resolution transmission electron microscopy (HRTEM), cryo-TEM imaging, X-ray powder diffraction (XRPD) and energy disperse X-ray spectroscopy (EDX).rnAs possible laser host materials, i.e. materials with a broad band emission in the near-infrared region, two unknown phases were investigated in the ternary oxide system M2O-Al2O3-WO3 (M = K, Na). Both phases exhibit low purity as well as non-homogeneous size distribution and particle morphology. The structures solved by ADT are also affected by pseudo-symmetry. rnSodium titanate nanotubes and nanowires are both intermediate products in the synthesis of TiO2 nanorods which are used as additives to colloidal TiO2 film for improving efficiency of dye-sensitized solar cells (DSSC). The structural transition from nantubes to nanowires was investigated in a step by step time-resolved study. Nanowires were discovered to consist of a hitherto unknown phase of sodium titanate. This new phase, typically affected by pervasive defects like mutual layer shift, was structurally determined ab-initio on the basis of ADT data. rnThe third system is related with calcium carbonate nucleation and early crystallization. The first part of this study is dedicated to the extensive investigations of calcium carbonate formation in a step by step analysis, up to the appearance of crystalline individua. The second part is dedicated to the structure determination by ADT of the first-to-form anhydrated phase of CaCO3: vaterite. An exhaustive structure analysis of vaterite had previously been hampered by diffuse scattering, extra periodicities and fast deterioration of the material under electron irradiation. rn

Using two dimensional sectional distributions to infer three dimensional volumetric distributions - Validation using tomography

The critical process parameter for mineral separation is the degree of mineral liberation achieved by comminution. The degree of liberation provides an upper limit of efficiency for any physical separation process. The standard approach to measuring mineral liberation uses mineralogical analysis based two-dimensional sections of particles which may be acquired using a scanning electron microscope and back-scatter electron analysis or from an analysis of an image acquired using an optical microscope. Over the last 100 years, mathematical techniques have been developed to use this two dimensional information to infer three-dimensional information about the particles. For mineral processing, a particle that contains more than one mineral (a composite particle) may appear to be liberated (contain only one mineral) when analysed using only its revealed particle section. The mathematical techniques used to interpret three-dimensional information belong, to a branch of mathematics called stereology. However methods to obtain the full mineral liberation distribution of particles from particle sections are relatively new. To verify these adjustment methods, we require an experimental method which can accurately measure both sectional and three dimensional properties. Micro Cone Beam Tomography provides such a method for suitable particles and hence, provides a way to validate methods used to convert two-dimensional measurements to three dimensional estimates. For this study ore particles from a well-characterised sample were subjected to conventional mineralogical analysis (using particle sections) to estimate three-dimensional properties of the particles. A subset of these particles was analysed using a micro-cone beam tomograph. This paper presents a comparison of the three-dimensional properties predicted from measured two-dimensional sections with the measured three-dimensional properties.