Surface studies in ultra high vacuum

An ultra high vacuum system capable of attaining pressures of 10-12 mm Hg was used for thermal desorption experiments. The metal chosen for these experiments was tantalum because of its suitability for thermal desorption experiments and because relatively little work has been done using this metal. The gases investigated were carbon monoxide, hydrogen and ethylene. The kinetic and thermodynamic parameters relating to the desorption reaction were calculated and the values obtained related to the reaction on the surface. The thermal desorption reaction was not capable of supplying all the information necessary to form a complete picture of the desorption reaction. Further information was obtained by using a quadrupole mass spectrometer to analyse the desorbed species. The identification of the desorbed species combined with the value of the desorption parameters meant that possible adatom structures could be postulated. A combination of these two techniques proved to be a very powerful tool when investigating gas-metal surface reactions and gave realistic values for the measured parameters such as the surface coverage, order of reaction, the activation energy and pre-exponential function for desorption. Electron microscopy and X-ray diffraction were also used to investigate the effect of the gases on the metal surface.

The characterisation of clean metal surfaces

The most perfectly structured metal surface observed in practice is that of a field evaporated field-ion microscope specimen. This surface has been characterised by adopting various optical analogue techniques. Hence a relationship has been determined between the structure of a single plane on the surface of a field-ion emitter and the geometry of a binary zone plate. By relating the known focussing properties of such a zone plate to those obtained from the projected images of such planes in a field-ion micrograph, it is possible to extract new information regarding the local magnification of the image. Further to this, it has been shown that the entire system of planes comprising the field-ion imaging surface may be regarded as a moire pattern formed between over-lapping zone plates. The properties of such moire zone plates are first established in an analysis of the moire pattern formed between zone plates on a flat surface. When these ideas are applied to the field-ion image it becomes possible to deduce further information regarding the precise topography of the emitter. It has also become possible to simulate differently proJected field-ion images by overlapping suitably aberrated zone plates. Low-energy ion bombardment is an essential preliminary to much surface research as a means of producing chemically clean surfaces. Hence it is important to know the nature and distribution of the resultant lattice damage, and the extent to which it may be removed by annealing. The field-ion microscope has been used to investigate such damage because its characterisation lies on the atomic scale. The present study is concerned with the in situ sputtering of tungsten emitters using helium, neon, argon and xenon ions with energies in the range 100eV to 1keV, together with observations of the effect of annealing. The relevance of these results to surface cleaning schedules is discussed.

Heat transfer from molten materials to liquids

An apparatus was designed and constructed which enabled material to be melted and heated to a maximum temperature of 1000C and then flooded with a pre-heated liquid. A series of experiments to investigate the thermal interaction between molten metals (aluminium, lead and tin) and sub-cooled water were conducted. The cooling rates of the molten materials under conditions of flooding were measured with a high speed-thermocouple and recorded with a transient recorder. A simplified model for calculating heat fluxes and metal surface temperatures was developed and used. Experimental results yielded boiling heat transfer in the transition film and stable film regions of the classic boiling curve. Maximum and minimum heat fluxes were observed at nucleate boiling crisis and the Leidenfrost point respectively. Results indicate that heat transfer from molten metals to sub-cooled water is a function of temperature and coolant depth and not a direct function of the physical properties of the metals. Heat transfer in the unstable transition film boiling region suggests that boiling dynamics in this region where a stationary molten metal is under pool boiling conditions at atmospheric pressure would not initiate a fuel-coolant interaction. Low heat fluxes around the Leidenfrost point would provide efficient fuel-coolant decoupling by a stable vapour blanket to enable coarse mixing of the fuel and coolant to occur without appreciable loss of thermal energy from the fuel. The research was conducted by Gareph Boxley and was submitted for the degree of PhD at the University of Aston in Birmingham in 1980.

Some aspects of the dynamic performance of machine tool structural joints

The work presented in this thesis is concerned with the dynamic behaviour of structural joints which are both loaded, and excited, normal to the joint interface. Since the forces on joints are transmitted through their interface, the surface texture of joints was carefully examined. A computerised surface measuring system was developed and computer programs were written. Surface flatness was functionally defined, measured and quantised into a form suitable for the theoretical calculation of the joint stiffness. Dynamic stiffness and damping were measured at various preloads for a range of joints with different surface textures. Dry clean and lubricated joints were tested and the results indicated an increase in damping for the lubricated joints of between 30 to 100 times. A theoretical model for the computation of the stiffness of dry clean joints was built. The model is based on the theory that the elastic recovery of joints is due to the recovery of the material behind the loaded asperities. It takes into account, in a quantitative manner, the flatness deviations present on the surfaces of the joint. The theoretical results were found to be in good agreement with those measured experimentally. It was also found that theoretical assessment of the joint stiffness could be carried out using a different model based on the recovery of loaded asperities into a spherical form. Stepwise procedures are given in order to design a joint having a particular stiffness. A theoretical model for the loss factor of dry clean joints was built. The theoretical results are in reasonable agreement with those experimentally measured. The theoretical models for the stiffness and loss factor were employed to evaluate the second natural frequency of the test rig. The results are in good agreement with the experimentally measured natural frequencies.

Do ‘passive’ medical titanium surfaces deteriorate in service in the absence of wear?

Globally, more than 1000 tonnes of titanium (Ti) is implanted into patients in the form of biomedical devices on an annual basis. Ti is perceived to be ‘biocompatible’ owing to the presence of a robust passive oxide film (approx. 4 nm thick) at the metal surface. However, surface deterioration can lead to the release of Ti ions, and particles can arise as the result of wear and/or corrosion processes. This surface deterioration can result in peri-implant inflammation, leading to the premature loss of the implanted device or the requirement for surgical revision. Soft tissues surrounding commercially pure cranial anchorage devices (bone-anchored hearing aid) were investigated using synchrotron X-ray micro-fluorescence spectroscopy and X-ray absorption near edge structure. Here, we present the first experimental evidence that minimal load-bearing Ti implants, which are not subjected to macroscopic wear processes, can release Ti debris into the surrounding soft tissue. As such debris has been shown to be pro-inflammatory, we propose that such distributions of Ti are likely to effect to the service life of the device.

Within-site variation in lichen growth rates and its implications for direct lichenometry

Variation in lichen growth rates poses a significant challenge for the application of direct lichenometry, i.e. the construction of lichen dating curves from direct measurement of growth rates. To examine the magnitude and possible causes of within-site growth variation, radial growth rates (RaGRs) of thalli of the fast-growing foliose lichen Melanelia fuliginosa ssp. fuliginosa (Fr. ex Duby) Essl. and the slow-growing crustose lichen Rhizocarpon geographicum (L.) DC. were studied on two S-facing slate rock surfaces in north Wales, UK using digital photography and an image analysis system (Image-J). RaGRs of M. fuliginosa ssp. fuliginosa varied from 0.44 to 2.63 mmyr-1 and R. geographicum from 0.10 to 1.50 mmyr-1.5. Analysis of variance suggested no significant variation in RaGRs with vertical or horizontal location on the rock, thallus diameter, aspect, slope, light intensity, rock porosity, rock surface texture, distance to nearest lichen neighbour or distance to vegetation on the rock surface. The frequency distribution of RaGR did not deviate from a normal distribution. It was concluded that despite considerable growth rate variation in both species studied, growth curves could be constructed with sufficient precision to be useful for direct lichenometry. © 2014 Swedish Society for Anthropology and Geography.

Gravity spun polycaprolactone fibres for soft tissue engineering:interaction with fibroblasts and myoblasts in cell culture

Poly(ε-caprolactone) (PCL) fibres were produced by wet spinning from solutions in acetone under low shear (gravity flow) conditions. As-spun PCL fibres exhibited a mean strength and stiffness of 7.9 MPa and 0.1 GPa, respectively and a rough, porous surface morphology. Cold drawing to an extension of 500% resulted in increases in fibre strength (43 MPa) and stiffness (0.3 GPa) and development of an oriented, fibrillar surface texture. The proliferation rate of Swiss 3T3 mouse fibroblasts and C2C12 mouse myoblasts on as-spun, 500% cold-drawn and gelatin-modified PCL fibres was determined in cell culture to provide a basic measure of the biocompatibility of the fibres. Proliferation of both cell types was consistently higher on gelatin-coated fibres relative to as-spun fibres at time points below 7 days. Fibroblast growth rates on cold-drawn PCL fibres exceeded those on as-spun fibres but myoblast proliferation was similar on both substrates. After 1 day in culture, both cell types had spread and coalesced on the fibres to form a cell layer, which conformed closely to the underlying topography. The high fibre compliance combined with a potential for modifying the fibre surface chemistry with cell adhesion molecules and the surface architecture by cold drawing to enhance proliferation of fibroblasts and myoblasts, recommends further investigation of gravity-spun PCL fibres for 3-D scaffold production in soft tissue engineering. © 2005 Elsevier Ltd. All rights reserved.

Selective oxidation of cyclohexene through gold functionalized silica monolith microreactors

Two simple, reproducible methods of preparing evenly distributed Au nanoparticle containing mesoporous silica monoliths are investigated. These Au nanoparticle containing monoliths are subsequently investigated as flow reactors for the selective oxidation of cyclohexene. In the first strategy, the silica monolith was directly impregnated with Au nanoparticles during the formation of the monolith. The second approach was to pre-functionalize the monolith with thiol groups tethered within the silica mesostructure. These can act as evenly distributed anchors for the Au nanoparticles to be incorporated by flowing a Au nanoparticle solution through the thiol functionalized monolith. Both methods led to successfully achieving even distribution of Au nanoparticles along the length of the monolith as demonstrated by ICP-OES. However, the impregnation method led to strong agglomeration of the Au nanoparticles during subsequent heating steps while the thiol anchoring procedure maintained the nanoparticles in the range of 6.8 ± 1.4 nm. Both Au nanoparticle containing monoliths as well as samples with no Au incorporated were tested for the selective oxidation of cyclohexene under constant flow at 30 °C. The Au free materials were found to be catalytically inactive with Au being the minimum necessary requirement for the reaction to proceed. The impregnated Au-containing monolith was found to be less active than the thiol functionalized Au-containing material, attributable to the low metal surface area of the Au nanoparticles. The reaction on the thiol functionalized Au-containing monolith was found to depend strongly on the type of oxidant used: tert-butyl hydroperoxide (TBHP) was more active than H2O2, likely due to the thiol induced hydrophobicity in the monolith.

The interaction of luminance and texture amplitude in surface depth perception

Previous studies have suggested separate channels for detection of first-order luminance modulations (LM) and second-order modulations of the local amplitude (AM) of a texture. Mixtures of LM and AM with different phase relationships appear very different: in-phase compounds (LM + AM) look like 3-D corrugated surfaces, while out-of-phase compounds (LM - AM) appear flat and/or transparent. This difference may arise because the in-phase compounds are consistent with multiplicative shading, while the out-of-phase compounds are not. We investigated the role of these modulation components in surface depth perception. We used a textured background with thin bars formed by local changes in luminance and/or texture amplitude. These stimuli appear as embossed surfaces with wide and narrow regions. Keeping the AM modulation depth fixed at a suprathreshold level, we determined the amount of luminance contrast required for observers to correctly indicate the width (narrow or wide) of 'raised' regions in the display. Performance (compared to the LM-only case) was facilitated by the presence of AM, but, unexpectedly, performance for LM - AM was as good as for LM + AM. Thus, these results suggest that there is an interaction between first-order and second-order mechanisms during depth perception based on shading cues, but the phase dependence is not yet understood.

Wear resistance of surface treated metal-working tools

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An ultra-sensitive localised surface plasmon resonance fibre device for environmental sensing based upon a structured bi-metal coating

We demonstrate a bi-metal coating (platinum and gold or silver) localised surface plasmon resonance fibre device that produces an index spectral sensitivity of over 11,000 nm/RIU, yielding an index resolution of 5×10-6in the aqueous index regime, consisting of a structured multi-layered thin film on D-shaped fibre. © 2014 SPIE.

Nanoindentation measurement of surface residual stresses in particle-reinforced metal matrix composites

The surface residual stresses in SiC particle-reinforced Al matrix composites are measured using a recently developed nanoindentation technique. The tensile biaxial residual stress in Al is found to increase with the particle concentration. The stress magnitudes are in reasonable agreement with those from numerical modeling.

Highly sensitive, localized surface plasmon resonance fiber device for environmental sensing, based upon a structured bi-metal array of nano-wires

We demonstrate a bi-metal coated (platinum and gold or silver), localized surface plasmon resonance fiber sensor with an index sensitivity exceeding 11,900 nm/RIU, yielding an index resolution of 2 × 10-5 in the aqueous index regime. This is one of the highest index sensitivities achieved with an optical fiber sensor. The coatings consist of arrays of bi-metal nano-wires (typically 36 nm in radius and 20 μm in length), supported by a silicon dioxide thin film on a thin substrate of germanium, the nano-wires being perpendicular to the longitudinal axis of the D-shaped fiber.