Timothy L. Burnett

Mapping of Local Electrical Properties in Epitaxial Graphene Using Electrostatic Force Microscopy

Local electrical characterization of epitaxial graphene grown on 4H-SiC(0001) using electrostatic force microscopy (EFM) in ambient conditions and at elevated temperatures is presented. EFM provides a straightforward identification of graphene with different numbers of layers on the substrate where topographical determination is hindered by adsorbates. Novel EFM spectroscopy has been developed measuring the EFM phase as a function of the electrical DC bias, establishing a rigorous way to distinguish graphene domains and facilitating optimization of EFM imaging.

Large volume serial section tomography by Xe Plasma FIB dual beam microscopy

Ga(+) Focused Ion Beam-Scanning Electron Microscopes (FIB-SEM) have revolutionised the level of microstructural information that can be recovered in 3D by block face serial section tomography (SST), as well as enabling the site-specific removal of smaller regions for subsequent transmission electron microscope (TEM) examination. However, Ga(+) FIB material removal rates limit the volumes and depths that can be probed to dimensions in the tens of microns range. Emerging Xe(+) Plasma Focused Ion Beam-Scanning Electron Microscope (PFIB-SEM) systems promise faster removal rates. Here we examine the potential of the method for large volume serial section tomography as applied to bainitic steel and WC-Co hard metals. Our studies demonstrate that with careful control of milling parameters precise automated serial sectioning can be achieved with low levels of milling artefacts at removal rates some 60× faster. Volumes that are hundreds of microns in dimension have been collected using fully automated SST routines in feasible timescales (<24h) showing good grain orientation contrast and capturing microstructural features at the tens of nanometres to the tens of microns scale. Accompanying electron back scattered diffraction (EBSD) maps show high indexing rates suggesting low levels of surface damage. Further, under high current Ga(+) FIB milling WC-Co is prone to amorphisation of WC surface layers and phase transformation of the Co phase, neither of which have been observed at PFIB currents as high as 60nA at 30kV. Xe(+) PFIB dual beam microscopes promise to radically extend our capability for 3D tomography, 3D EDX, 3D EBSD as well as correlative tomography.

Identification of epitaxial graphene domains and adsorbed species in ambient conditions using quantified topography measurements

We discuss general limitations of topographical studies of epitaxial graphene in ambient conditions, in particular, when an accurate determination of the layers thickness is required. We demonstrat ...

Epitaxial graphene on SiC(

Surface potential distribution, V(CPD), and evolution of atmospheric adsorbates on few and multiple layers (FLG and MLG) of graphene grown on SiC(0001) substrate have been investigated by electrostatic and Kelvin force microscopy techniques at T = 20-120 °C. The change of the surface potential distribution, ΔV(CPD), between FLG and MLG is shown to be temperature dependent. The enhanced ΔV(CPD) value at 120 °C is associated with desorption of adsorbates at high temperatures and the corresponding change of the carrier balance. The nature of the adsorbates and their evolution with temperature are considered to be related to the process of adsorption and desorption of the atmospheric water on MLG domains. We demonstrate that both the nano- and microscale wettability of the material are strongly dependent on the number of graphene layers.

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Abstract A sample of AISI type 316 stainless steel from a power station steam header, showing reheat cracking, was removed from service and has been examined by a combination of microscale X-ray computed tomography (CT), nanoscale serial section focused ion beam–scanning electron microscopy (FIB-SEM), energy dispersive X-ray (EDX) spectrum imaging and transmission electron microscopy (TEM). Multiscale three-dimensional analysis using correlative tomography allowed key regions to be found and analysed with high resolution techniques. The grain boundary analysed was decorated with micrometre sized, facetted cavities, M23C6 carbides, ferrite and G phase but no σ phase. Smaller intragranular M23C6 particles were also observed, close to the grain boundaries. This intimate coexistence suggests that the secondary phases will control the nucleation and growth of the cavities. Current models of cavitation, based on isolated idealised grain boundary cavities, are oversimplified.

): functional electrical microscopy studies and effect of atmosphere

Plasma electrolytic oxidation (PEO) is of increasing interest for the formation of ceramic coatings on metals for applications that require diverse coating properties, such as wear and corrosion resistance, low thermal conductivity, and biocompatibility. Porosity in the coatings can have an important impact on the coating performance. However, the quantification of the porosity in coatings can be difficult due to the wide range of pore sizes and the complexity of the coating morphology. In this work, a PEO coating formed on titanium is examined using high resolution X-ray computed tomography (X-ray CT). The observations are validated by comparisons of surface views and cross-sectional views of specific coating features obtained using X-ray CT and scanning electron microscopy. The X-ray CT technique is shown to be capable of resolving pores with volumes of at least 6 μm(3). Furthermore, the shapes of large pores are revealed and a correlation is demonstrated between the locations of the pores, nodules on the coating surface, and depressions in the titanium substrate. The locations and morphologies of the pores, which constitute 5.7% of the coating volume, indicate that they are generated by release of oxygen gas from the molten coating.

Multiscale 3D analysis of creep cavities in AISI type 316 stainless steel

Abstract Stress corrosion cracks of all types are characterised by extensive crack branching, and this is frequently used as the key failure analysis characteristic to identify this type of cracking. For aluminium alloys, stress corrosion cracking (SCC) is almost exclusively an intergranular failure mechanism. For plate and extruded components, this had led to the development of test procedures using double cantilever beam and compact tension precracked specimens that rely on the pancake grain shape to constrain cracking, so that fracture mechanics can be applied to the analysis of stress intensity and crack velocity and the evolution of a characteristic performance curve. We have used X-ray computed tomography to examine in detail SCC in aluminium alloys in three dimensions for the first time. We have found that crack branching limits the stress intensity at the crack tip as the applied stress is shared amongst a number of cracks that are held together by uncracked ligaments. We propose that the plateau region observed in the v-K curve is an artefact due to crack branching, and at the crack tips of the many crack branches, cracking essentially occurs at constant K almost irrespective of the crack length. We have amplified the crack branching effect by examining a sample where the long axis of the pancake grains was inclined to the applied stressing direction. Our results have profound implications for the future use of precracked specimens for SCC susceptibility testing and the interpretation of results from these tests.

X-ray Computed Tomographic Investigation of the Porosity and Morphology of Plasma Electrolytic Oxidation Coatings.

Electrostatic Force Spectroscopy and Scanning Kelvin Probe Microscopy techniques are used to study the performance of side-gated Hall devices made of epitaxial graphene on 4H-SiC(0001). Electrostatic Force Spectroscopy is a novel method which allows quantitative surface potential measurements with high spatial resolution. Using these techniques, we calibrate work function of the metal coated tip and define the work functions for single and double-layer graphene. We also show that the use of moderate strength electrical fields in the side-gate geometry does not notably change the performance of the device.

The role of crack branching in stress corrosion cracking of aluminium alloys

An experimental protocol (workflow) has been developed for time‐lapse x‐ray nanotomography (nano‐CT) imaging of environmentally driven morphological changes to materials. Two case studies are presented. First, the leaching of nanoparticle corrosion inhibitor pigment from a polymer coating was followed over 14 days, while in the second case the corrosion damage to an AA2099 aluminium alloy was imaged over 12 hours. The protocol includes several novel aspects relevant to nano‐CT with the use of a combination of x‐ray absorption and phase contrast data to provide enhanced morphological and composition information, and hence reveal the best information to provide new insights into the changes of different phases over time. For the pigmented polymer coating containing nominally strontium aluminium polyphosphate, the strontium‐rich components within the materials are observed to leach extensively whereas the aluminium‐rich components are more resistant to dissolution. In the case of AA2099 it is found that the initial grain boundary corrosion is driven by the presence of copper‐rich phases and is then followed by the corrosion of grains of specific orientation.

Surface potential variations in epitaxial graphene devices investigated by Electrostatic Force Spectroscopy

The surface oxidation of aluminum is still poorly understood despite its vital role as an insulator in electronics, in aluminum-air batteries, and in protecting the metal against corrosion. Here we use atomic resolution imaging in an environmental transmission electron microscope (TEM) to investigate the mechanism of aluminum oxide formation. Harnessing electron beam sputtering we prepare a pristine, oxide-free metal surface in the TEM. This allows us to study, as a function of crystallographic orientation and oxygen gas pressure, the full oxide growth regime from the first oxide nucleation to a complete saturated, few-nanometers-thick surface film.