Characterisation of dispersions within annealed HVOLF thermally sprayed AlSnCu coatings

High velocity oxy-liquid fuel (HVOLF) AlSnCu coatings are characterised following annealing for up to 5 hours at 300°C. A combination of statistical analysis of BSE images and TEM observations demonstrate the decrease in the number of sub-micron and nanoscale Sn particles with annealing, commensurate with a decrease in the coating microhardness. TEM evidence further suggests the coarsening of nanoscale Sn through a mechanism of a liquid phase migration within the Al matrix. EELS and EFTEM additionally allow the identification of the precipitation of theta'

Progress towards a methodology for high throughput 3D reconstruction of soot nanoparticles via electron tomography

The aim of this work is to make progress towards the development of 3D reconstruction as a legitimate alternative to traditional 2D characterisation of soot. Time constraints are the greatest opposition to its implementation, as currently reconstruction of a single soot particle takes around 5-6 hours to complete. As such, the accuracy and detail gains are currently insufficient to challenge 2D characterisation of a representative sample (e.g. 200 particles). This work is a consideration of the optimisation of the steps included within the computational reconstruction and manual segmentation of soot particles. Our optimal process reduced the time required by over 70% in comparison to a typical procedure, whilst producing models with no appreciable decrease in quality

Microstructural characterisation of TiAlTiAu and TiAlPdAu ohmic contacts to AlGaN/GaN

Ti/Al/Ti/Au and Ti/Al/Pd/Au contacts to AlGaN/GaN have been investigated to ascertain the effect of annealing temperature on the structural evolution of the contacts. Ti/Al/Ti/Au contacts become ohmic after rapid thermal annealing at 750°C or higher, corresponding to the formation of an interfacial TiN phase, with inclusions penetrating through the AlGaN layer observed after annealing at 950°C. The Pd layer is shown to be more efficient at inhibiting diffusion of Au to the interface than Ti. Ohmic behaviour was not seen with the Ti/Al/Pd/Au scheme. Either the presence of Au at the interface may improve ohmic behaviour, or the Ti:Al ratio is insufficient in this scheme

Morphological characterisation of diesel soot in oil and the associated extraction dependence

The size and morphology of soot particles and agglomerates extracted from lubricating oil drawn from the sump of a diesel engine have been investigated and compared using Transmission Electron Microscopy (TEM) and Nanoparticle Tracking Analysis (NTA). Samples were prepared for electron microscopy imaging by both centrifugation and solvent extraction to investigate the impact of these procedures on the morphological characteristics, such as skeleton length and width and circularity, of the obtained soot. It was shown that centrifugation increases the extent of agglomeration within the sample, with 15% of the agglomerates above 200 nm compared to only 11% in the solvent extracted soot. It was also observed that the width of centrifugation extracted soot was typically 10 nm to 20 nm larger than that of solvent extracted soot, suggesting that centrifugation forces the individual agglomerate chains together. Moreover, centrifugation fails to extract a large percentage of particles below 50 nm, with only 4% of the agglomerates smaller than 50 nm in the centrifugation extracted soot, whereas agglomerates in this size range accounted for 19 % using solvent extraction. As TEM represents a comparatively time and cost expensive characterisation tool, unsuitable for high throughput testing required by industry, NTA was explored as a low cost, rapid alternative method for measuring particle size. It was found that results generated by NTA, within the limits of detection, correlated well with those obtained using TEM. This correlative electron microscopy and light scattering approach was further used to appraise the morphological characteristics of two commercial sources of carbon black (CB), enabling the selection of the most suitable soot surrogate, essential for the further development of oils with optimised functional properties

Formation of hollow carbon nanoshells from thiol stabilised silver nanoparticles via heat treatment

Uniform, less 10 nm sized, hollow carbon nano-shells (HCNS) have been prepared via a single-step, thermal treatment of alkanethiol stabilised Ag nanoparticles (TS-AgNP). Direct evidence for the formation of spherical HCNS from TS-AgNP is provided by in situ MEMS heating on Si3N4 supports within a TEM, and ex situ thermal processing of TS-AgNP on carbon nanotube supports. A mechanism is proposed for the thermally driven, templated formation of HCNS from the TS-AgNP stabilising layer, with Ag catalysing the graphitisation of carbon in advance of thermally induced AgNP template removal. This facile processing route provides for excellent size control of the HCNS product via appropriate AgNP template selection. However, a rapid rate of heating was found to be crucial for the formation of well-defined HCNS, whilst a slow heating rate gave a much more disrupted product, comprising predominantly lacy carbon with decreased levels of graphitic ordering, reflecting a competition between the thermal transformation of the TS-layer and the rate of removal of the AgNP template

Microstructural characterisation of TiAlTiAu and TiAlPdAu ohmic contacts to AlGaN/GaN

Ti/Al/Ti/Au and Ti/Al/Pd/Au contacts to AlGaN/GaN have been investigated to ascertain the effect of annealing temperature on the structural evolution of the contacts. Ti/Al/Ti/Au contacts become ohmic after rapid thermal annealing at 750°C or higher, corresponding to the formation of an interfacial TiN phase, with inclusions penetrating through the AlGaN layer observed after annealing at 950°C. The Pd layer is shown to be more efficient at inhibiting diffusion of Au to the interface than Ti. Ohmic behaviour was not seen with the Ti/Al/Pd/Au scheme. Either the presence of Au at the interface may improve ohmic behaviour, or the Ti:Al ratio is insufficient in this scheme

Toward mid-infrared, subdiffraction, spectral-mapping of human cells and tissue: SNIM (scanning near-field infrared microscopy) tip fabrication

Scanning near-field infrared microscopy (SNIM) potentially enables subdiffraction, broadband mid-infrared (MIR:3–25-μm wavelength range) spectral-mapping of human cells and tissue for real-time molecular sensing, with prospective use in disease diagnosis. SNIM requires an MIR-transmitting tip of small aperture for photon collection. Here, chalcogenide-glass optical fibers are reproducibly tapered at one end to form a MIR transmitting tip for SNIM. A wet-etching method is used to form the tip. The tapering sides of the tip are Al-coated. These Al-coated tapered-tips exhibit near-field power-confinement when acting either as the launch-end or exit-end of the MIR optical fiber. We report first time optimal cleaving of the end of the tapered tip using focused ion beam milling. A flat aperture is produced at the end of the tip, which is orthogonal to the fiber-axis and of controlled diameter. A FIB-cleaved aperture is used to collect MIR spectra of cells mounted on a transflection plate, under illumination of a synchrotron- generated wideband MIR beam

Structural characterisation of MBE grown zinc-blende Ga1-xMnxN/GaAs(001) as a function of Ga flux

Ga1-xMnxN films grown on semi-insulating GaAs(001) substrates at 680°C with fixed Mn flux and varied Ga flux demonstrated a transition from zinc-blende/wurtzite mixed phase growth for low Ga flux (N-rich conditions) to zinc-blende single phase growth with surface Ga droplets for high Ga flux (Ga-rich conditions). N-rich conditions were found favourable for Mn incorporation in GaN lattice. α-MnAs inclusions were identified extending into the GaAs buffer layer