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

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

Soot-in-oil 3D volume reconstruction through the use of electron tomography: an introductory study

Understanding soot nanoparticle interaction with oil additives and the causes of soot-induced thickening would assist in lubricant formulation, prolonging engine life and improving engine efficiency. Three-dimensional measurement of soot structures is currently not undertaken as established techniques are limited to two dimensions. While they give valuable information on the structure and reactivity of soot nanoparticles, it is not easy to correlate this to geometry of primary particles and agglomerates. In this work, we investigate the development and application of 3D-TEM for characterisation of soot agglomerates as a new capability to yield information on the volumetric character of fractal nanoparticles. This investigation looks at the feasibility for volume reconstruction of nanometric soot particles in used engine oil from multiple imaging at different tilt angles. Bright-field TEM was used to capture two-dimensional images of soot. Heptane and diethyl ether washes were used to remove volatile contaminants and allowed for images from −60° to +60° tilt with no sign of carbon build-up to be acquired. Tomographic reconstruction from the aligned tilt-series images based on weighted back-projection algorithm has yielded useful information about complex soot nanoparticle size. Estimation of soot mass in oil by nanoparticle tracking analysis (NTA) can be considerably improved by taking into account the three-dimensional shape of the soot agglomerate including the shape factor in the calculations. 3D-TEM measurements were compared with values calculated by using a single-sphere approach when tracking nanoparticles moving under Brownian motion. A shape factor was calculated, dividing the surface area and volume calculated using spherical geometrical estimates, by the respective values calculated using the 3D models. The spherical model of the particle is found on average to overestimate the surface area by sevenfold, and the volume to the actual soot agglomerate by 23 times. Applying the calculated shape factor as a correction reduces the NTA overestimation by one order of magnitude

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

Comparative nanostructure analysis of gasoline turbocharged direct injection and diesel soot-in-oil with carbon black

Two gasoline turbocharged direct injection (GTDI) and two diesel soot-in-oil samples were compared with one flame-generated soot sample. High resolution transmission electron microscopy imaging was employed for the initial qualitative assessment of the soot morphology. Carbon black and diesel soot both exhibit core-shell structures, comprising an amorphous core surrounded by graphene layers; only diesel soot has particles with multiple cores. In addition to such particles, GTDI soot also exhibits entirely amorphous structures, of which some contain crystalline particles only a few nanometers in diameter. Subsequent quantification of the nanostructure by fringe analysis indicates differences between the samples in terms of length, tortuosity, and separation of the graphitic fringes. The shortest fringes are exhibited by the GTDI samples, whilst the diesel soot and carbon black fringes are 9.7% and 15.1% longer, respectively. Fringe tortuosity is similar across the internal combustion engine samples, but lower for the carbon black sample. In contrast, fringe separation varies continuously among the samples. Raman spectroscopy further confirms the observed differences. The GTDI soot samples contain the highest fraction of amorphous carbon and defective graphitic structures, followed by diesel soot and carbon black respectively. The AD1:AG ratios correlate linearly with both the fringe length and fringe separation

TEM studies of multilayer ohmic contacts to n-type AlGaN/GaN

Ti and Pd barrier layers between the Al/Ti diffusion couple and the Au capping layer of multilayer ohmic contacts to n-type AlGaN/GaN field effect transistors were found to be ineffective in preventing the diffusion of Au to the AlGaN following high temperature rapid thermal annealing. The formation of a band of TiN grains at the contact/AlGaN interface is responsible for the activation of the contact. The presence of interfacial Au and threading dislocations are implicated in the formation of additional Ti-nitride inclusions into the AlGaN, although these do not appear to disrupt the Ti-nitride layer at the original contact/nitride interface, nor significantly influence the contact resistance