Deformation behaviours of coarse-grained and nanocrystalline Mg-5wt% Al alloys

Magnesium alloys have been of growing interest to various engineering applications, such as the automobile, aerospace, communication and computer industries due to their low density, high specific strength, good machineability and availability as compared with other structural materials. However, most Mg alloys suffer from poor plasticity due to their Hexagonal Close Packed structure. Grain refinement has been proved to be an effective method to enhance the strength and alter the ductility of the materials. Several methods have been proposed to produce materials with nanocrystalline grain structures. So far, most of the research work on nanocrystalline materials has been carried out on Face-Centered Cubic and Body-Centered Cubic metals. However, there has been little investigation of nanocrystalline Mg alloys. In this study, bulk coarse-grained and nanocrystalline Mg alloys were fabricated by a mechanical alloying method. The mixed powder of Mg chips and Al powder was mechanically milled under argon atmosphere for different durations of 0 hours (MA0), 10 hours (MA10), 20 hours (MA20), 30 hours (MA30) and 40 hours (MA40), followed by compaction and sintering. Then the sintered billets were hot-extruded into metallic rods with a 7 mm diameter. The obtained Mg alloys have a nominal composition of Mg–5wt% Al, with grain sizes ranging from 13 μm down to 50 nm, depending on the milling durations. The microstructure characterization and evolution after deformation were carried out by means of Optical microscopy, X-Ray Diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy, Scanning Probe Microscopy and Neutron Diffraction techniques. Nanoindentaion, compression and micro-compression tests on micro-pillars were used to study the size effects on the mechanical behaviour of the Mg alloys. Two kinds of size effects on the mechanical behaviours and deformation mechanisms were investigated: grain size effect and sample size effect. The nanoindentation tests were composed of constant strain rate, constant loading rate and indentation creep tests. The normally reported indentation size effect in single crystal and coarse-grained crystals was observed in both the coarse-grained and nanocrystalline Mg alloys. Since the indentation size effect is correlated to the Geometrically Necessary Dislocations under the indenter to accommodate the plastic deformation, the good agreement between the experimental results and the Indentation Size Effect model indicated that, in the current nanocrystalline MA20 and MA30, the dislocation plasticity was still the dominant deformation mechanism. Significant hardness enhancement with decreasing grain size, down to 58 nm, was found in the nanocrystalline Mg alloys. Further reduction of grain size would lead to a drop in the hardness values. The failure of grain refinement strengthening with the relatively high strain rate sensitivity of nanocrystalline Mg alloys suggested a change in the deformation mechanism. Indentation creep tests showed that the stress exponent was dependent on the loading rate during the loading section of the indentation, which was related to the dislocation structures before the creep starts. The influence of grain size on the mechanical behaviour and strength of extruded coarse-grained and nanocrystalline Mg alloys were investigated using uniaxial compression tests. The macroscopic response of the Mg alloys transited from strain hardening to strain softening behaviour, with grain size reduced from 13 ìm to 50 nm. The strain hardening was related to the twinning induced hardening and dislocation hardening effect, while the strain softening was attributed to the localized deformation in the nanocrystalline grains. The tension–compression yield asymmetry was noticed in the nanocrystalline region, demonstrating the twinning effect in the ultra-fine-grained and nanocrystalline region. The relationship k tensions < k compression failed in the nanocrystalline Mg alloys; this was attributed to the twofold effect of grain size on twinning. The nanocrystalline Mg alloys were found to exhibit increased strain rate sensitivity with decreasing grain size, with strain rate ranging from 0.0001/s to 0.01/s. Strain rate sensitivity of coarse-grained MA0 was increased by more than 10 times in MA40. The Hall-Petch relationship broke down at a critical grain size in the nanocrystalline region. The breakdown of the Hall-Petch relationship and the increased strain rate sensitivity were due to the localized dislocation activities (generalization and annihilation at grain boundaries) and the more significant contribution from grain boundary mediated mechanisms. In the micro-compression tests, the sample size effects on the mechanical behaviours were studied on MA0, MA20 and MA40 micro-pillars. In contrast to the bulk samples under compression, the stress-strain curves of MA0 and MA20 micro-pillars were characterized with a number of discrete strain burst events separated by nearly elastic strain segments. Unlike MA0 and MA20, the stress-strain curves of MA40 micro-pillars were smooth, without obvious strain bursts. The deformation mechanisms of the MA0 and MA20 micro-pillars under micro-compression tests were considered to be initially dominated by deformation twinning, followed by dislocation mechanisms. For MA40 pillars, the deformation mechanisms were believed to be localized dislocation activities and grain boundary related mechanisms. The strain hardening behaviours of the micro-pillars suggested that the grain boundaries in the nanocrystalline micro-pillars would reduce the source (nucleation sources for twins/dislocations) starvation hardening effect. The power law relationship of the yield strength on pillar dimensions in MA0, MA20 supported the fact that the twinning mechanism was correlated to the pre-existing defects, which can promote the nucleation of the twins. Then, we provided a latitudinal comparison of the results and conclusions derived from the different techniques used for testing the coarse-grained and nanocrystalline Mg alloy; this helps to better understand the deformation mechanisms of the Mg alloys as a whole. At the end, we summarized the thesis and highlighted the conclusions, contributions, innovations and outcomes of the research. Finally, it outlined recommendations for future work.

Fusing loop detector and probe vehicle data to estimate travel time statistics on signalized urban networks

This article presents a methodology that integrates cumulative plots with probe vehicle data for estimation of travel time statistics (average, quartile) on urban networks. The integration reduces relative deviation among the cumulative plots so that the classical analytical procedure of defining the area between the plots as the total travel time can be applied. For quartile estimation, a slicing technique is proposed. The methodology is validated with real data from Lucerne, Switzerland and it is concluded that the travel time estimates from the proposed methodology are statistically equivalent to the observed values.

Distinguishing new science from calibration effects in the electron-volt neutron spectrometer VESUVIO at ISIS

The "standard" procedure for calibrating the Vesuvio eV neutron spectrometer at the ISIS neutron source, forming the basis for data analysis over at least the last decade, was recently documented in considerable detail by the instrument’s scientists. Additionally, we recently derived analytic expressions of the sensitivity of recoil peak positions with respect to fight-path parameters and presented neutron–proton scattering results that together called in to question the validity of the "standard" calibration. These investigations should contribute significantly to the assessment of the experimental results obtained with Vesuvio. Here we present new results of neutron–deuteron scattering from D2 in the backscattering angular range (theata > 90 degrees) which are accompanied by a striking energy increase that violates the Impulse Approximation, thus leading unequivocally the following dilemma: (A) either the "standard" calibration is correct and then the experimental results represent a novel quantum dynamical effect of D which stands in blatant contradiction of conventional theoretical expectations; (B) or the present "standard" calibration procedure is seriously deficient and leads to artificial outcomes. For Case(A), we allude to the topic of attosecond quantumdynamical phenomena and our recent neutron scattering experiments from H2 molecules. For Case(B),some suggestions as to how the "standard" calibration could be considerably improved are made.

Sensitivity of peak positions to flight-path parameters in a deep-inelastic scattering neutron TOF spectrometer

The effects of small changes in flight-path parameters (primary and secondary flight paths, detector angles), and of displacement of the sample along the beam axis away from its ideal position, are examined for an inelastic time-of-flight (TOF) neutron spectrometer, emphasising the deep-inelastic regime. The aim was to develop a rational basis for deciding what measured shifts in the positions of spectral peaks could be regarded as reliable in the light of the uncertainties in the calibrated flight-path parameters. Uncertainty in the length of the primary or secondary flight path has the least effect on the positions of the peaks of H, D and He, which are dominated by the accuracy of the calibration of the detector angles. This aspect of the calibration of a TOF spectrometer therefore demands close attention to achieve reliable outcomes where the position of the peaks is of significant scientific interest and is discussed in detail. The corresponding sensitivities of the position of peak of the Compton profile, J(y), to flight-path parameters and sample position are also examined, focusing on the comparability across experiments of results for H, D and He. We show that positioning the sample to within a few mm of the ideal position is required to ensure good comparability between experiments if data from detectors at high forward angles are to be reliably interpreted.

The Use of a Nitroxide Probe in DMSO to Capture Radicals in Particulate Pollution

A profluorescent nitroxide was used to evaluate the oxidative potential of pollution derived from a compression ignition engine fuelled with biodiesel. The reaction products responsible for the observed fluorescence increase when a DMSO solution of nitroxide was exposed to biodiesel exhaust were determined by using HPLC/MS. The main fluorescent species was identified as a methanesulfonamide adduct arising from the reaction of the nitroxide with DMSO-derived sulfoxyl radicals.

Measurement of anisotropies of the kinetic energy and anharmonicity in pyrolytic graphite by neutron Compton scattering

Neutron Compton scattering (NCS) measurements of the anisotropy of the momentum distribution and the mean Laplacian of the interatomic potential ∇2V have been performed using electron volt neutrons, with wave vector transfers between 24 Å−1 and 98 Å−1. The measured momentum distribution of the atoms displays significantly more anisotropy than a calculation using a model density of states. We have observed anisotropies in ∇2V for the first time. The results suggest that the atomic potential is harmonic within the graphite planes, but anharmonic for vibrations perpendicular to the planes.

Neutron Compton scattering from selectively deuterated acetanilide

With the aim of developing the application of neutron Compton scattering (NCS) to molecular systems of biophysical interest, we are using the Compton spectrometer EVS at ISIS to characterize the momentum distribution of protons in peptide groups. In this contribution we present NCS measurements of the recoil peak (Compton profile) due to the amide proton in otherwise fully deuterated acetanilide (ACN), a widely studied model system for H-bonding and energy transfer in biomolecules. We obtain values for the average width of the potential well of the amide proton and its mean kinetic energy. Deviations from the Gaussian form of the Compton profile, analyzed on the basis of an expansion due to Sears, provide data relating to the Laplacian of the proton potential. (C) 1998 Elsevier Science B.V. All rights reserved.

Multiple scattering in deep inelastic neutron scattering : Monte Carlo simulations and experiments at the ISIS eVS inverse geometry spectrometer

A procedure for the evaluation of multiple scattering contributions is described, for deep inelastic neutron scattering (DINS) studies using an inverse geometry time-of-flight spectrometer. The accuracy of a Monte Carlo code DINSMS, used to calculate the multiple scattering, is tested by comparison with analytic expressions and with experimental data collected from polythene, polycrystalline graphite and tin samples. It is shown that the Monte Carlo code gives an accurate representation of the measured data and can therefore be used to reliably correct DINS data.

Calibration of the electron volt spectrometer, a deep inelastic neutron scattering spectrometer at the ISIS pulsed neutron spallation source

The electron Volt Spectrometer (eVS) is an inverse geometry filter difference spectrometer that has been optimised to measure the single atom properties of condensed matter systems using a technique known as Neutron Compton Scattering (NCS) or Deep Inelastic Neutron Scattering (DINS). The spectrometer utilises the high flux of epithermal neutrons that are produced by the ISIS neutron spallation source enabling the direct measurement of atomic momentum distributions and ground state kinetic energies. In this paper the procedure that is used to calibrate the spectrometer is described. This includes details of the method used to determine detector positions and neutron flight path lengths as well as the determination of the instrument resolution. Examples of measurements on 3 different samples are shown, ZrH2, 4He and Sn which show the self-consistency of the calibration procedure.

The temperature dependence of the momentum distribution of beryllium measured by neutron Compton scattering

In this paper we report a new neutron Compton scattering (NCS) measurement of the ground state single atom kinetic energy of polycrystalline beryllium at momentum transfers in the range 27}104 As ~1 and temperatures in the range 110}1150 K. The measurements have been made with the electron Volt spectrometer (eVS) at the ISIS facility and the measured kinetic energies are shown to be &10% higher than calculations made in the harmonic approximation.