2,115 research outputs found

    Utilising DualEELS to probe the nanoscale mechanisms of the corrosion of Zircaloy-4 in 350 °C pressurised water

    Get PDF
    Characterisation of materials utilised for fuel cladding in nuclear reactors prior to service is integral in order to understand corrosion mechanisms which would take place in reactor. Zircaloy-4 is one such material of choice for nuclear fuel containment in Pressurised Water Reactors (PWRs). In particular, the metal-oxide interface has been a predominant focus of previous research, however, due to the complex oxidation process of zirconium cladding, there is still no clear understanding of what is present at the interface. Using Scanning Transmission Electron Microscopy (STEM) and Dual Electron Energy Loss Spectroscopy (DualEELS), we have studied the corrosion of this material under conditions similar to those that could be encountered in service. It is shown that under all conditions, whether during faster oxidation in the early stages, slow growth just prior to the transition to a new growth regime, or in the faster growth that happens after this transition, the surface of the metal below the scale is loaded with oxygen up to around 33 at%. Approaching transition, in conditions of slow growth and slow oxygen supply, an additional metastable suboxide is apparent with a thickness of tens of nm. By studying changes in both chemical composition and dielectric function of the material at the oxide scale – metal interface with nanometre resolution, quantitative mapping could be achieved, clearly showing that this is a suboxide composition of ZrO and a Zr oxidation state close to +2

    Measuring assistance to the agricultural industry in Australia using a Production Assistance Index

    Get PDF
    The history of the reforms of the assistance given to Australian agriculture over the past fifty years is a remarkable story, especially when contrasted with the experiences of most other OECD countries. The effects of these reforms have been captured by the Productivity Commission (and its predecessors) and by Lloyd through time series of the nominal rates of assistance to individual agricultural commodities and to the industry as a whole. In this paper the concept of a partial equilibrium production assistance index is developed to obtain a more accurate picture of the implicit welfare consequences of this assistance for the period 1955-59 to 2000-04. This index is a mean of order 2. It is shown that the conventional average, the mean of order 1, substantially underestimates the mean of order 2, which is the correct definition of the average level of assistance.Production Assistance Index, industry assistance, Trade Restrictiveness Index, Australian agricultural policy, Research Methods/ Statistical Methods, Agricultural and Food Policy,

    Spectrum imaging of complex nanostructures using DualEELS: I. digital extraction replicas

    Get PDF
    This paper shows how it is possible to use Dual Electron Energy Loss Spectroscopy (DualEELS) to digitally extract spectrum images for one phase of interest in a complex nanostructured specimen. The specific cases studied here concern Nb or V precipitates, a few nanometres in size, in high manganese steels. The procedures outlined allow the extraction of the precipitate signal from the Fe–Mn matrix, as well as correction for surface oxide and any surface carbon contamination. The resulting precipitate-only spectrum images are then suitable for quantitative analysis of the precipitate chemistry. This procedure results in much improved background shapes under all edges of interest, mainly as a result of the removal of the extended electron loss fine structure (EXELFS) from the elements in the matrix. This allows the reliable extraction of even tiny quantities of elements, such as low levels of nitrogen in some carbide precipitates. As well as being relevant to precipitation in steels, these techniques will be widely applicable to the separation of chemically-distinct phases in complex nanostructured samples, and can be viewed as a digital version of the extraction replica technique

    EELS at very high energy losses

    Get PDF
    Electron energy-loss spectroscopy (EELS) has been investigated in the range from 2 to >10 keV using an optimized optical coupling of the microscope to the spectrometer to improve the high loss performance in EELS. It is found that excellent quality data can now be acquired up until about 5 keV, suitable for both energy loss near edge structure (ELNES) studies of oxidation and local chemistry, and potentially useful for extended energy loss fine structure (EXELFS) studies of local atomic ordering. Examples studied included oxidation in Zr, Mo and Sn, and the ELNES and EXELFS of the Ti-K edge. It is also shown that good quality electron energy-loss spectroscopy can even be performed for losses above 9.2 keV, the energy loss at which the collection angle becomes ‘infinite’, and this is demonstrated using the tungsten L3 edge at about 10.2 keV

    History, Sociology, Modernity : How Connect?

    No full text
    Special Issue on 'The State of Scottish History: Past, Present and Future'Peer reviewedPublisher PD

    Accurate measurement of absolute experimental inelastic mean free paths and EELS differential cross-sections

    Get PDF
    Methods are described for measuring accurate absolute experimental inelastic mean free paths and differential cross-sections using DualEELS. The methods remove the effects of surface layers and give the results for the bulk materials. The materials used are VC0.83,TiC0.98,VN0.97and TiN0.88but the method should be applicable to a wide range of materials. The data were taken at 200 keVusing a probe half angle of 29mradand a collection angle of 36mrad. The background can be subtracted from under the ionisation edges, which can then be separated from each other. This is achieved by scaling Hartree-Slater calculated cross-sections to the edges in the atomic regions well above the threshold. The average scaling factors required are 1.00 for the non-metal K-edges and 1.01 for the metal L-edges (with uncertainties of a few per cent). If preliminary measurements of the chromatic effects in the post-specimen lenses are correct, both drop to 0.99. The inelastic mean free path for TiC0.98 was measured as 103.6±0.5 nm compared to the prediction of 126.9 nm based on the widely used Iakoubovskii parameterisation

    Getting the most out of a post-column EELS spectrometer on a TEM/STEM by optimising the optical coupling

    Get PDF
    Ray tracing is used to find improved set-ups of the projector system of a JEOL ARM 200CF TEM/STEM for use in coupling it to a Gatan 965 Quantum ER EELS system and to explain their performance. The system has a probe aberration corrector but no image corrector. With the latter, the problem would be more challenging. The agreement between the calculated performance and that found experimentally is excellent. At 200kV and using the 2.5mm Quantum entrance aperture, the energy range over which the collection angle changes by a maximum of 5% from that at zero loss has been increased from 1.2keV to 4.7keV. At lower accelerating voltages, these energy ranges are lower e.g. at 80kV they are 0.5keV and 2.0keV respectively. The key factors giving the improvement are an increase in the energy-loss at which the projector cross-over goes to infinity and a reduction of the combination aberrations that occur in a lens stack. As well as improving the energy-loss range, the new set-ups reduce spectrum artefacts and minimise the motion of the diffraction pattern at low STEM magnification for electrons that have lost energy. Even if making the pivot points conjugate with the film plane gives no motion for zero-loss electrons, there will be motion for those electrons that have lost energy, leading to a false sense of security when performing spectrum imaging at low magnifications. De-scanning of the probe after the objective lens is a better way of dealing with this problem
    corecore