Bone response is one of the key determining factors in the overall success of biomaterials intended for bone regeneration and osseointegration. Understanding the formation of bone at an implant surface may lead to the improved design of biomaterials for the future. However, due to the inhomogeneity of bone tissue at an interface, two-dimensional images often lack detail on the interfacial complexity. Furthermore, the increasing use of nanotechnology in the design and production of biomaterials demands characterization techniques on a similar nano length scale. While current analysis methods, such as X-ray tomography, transmission electron microscopy, focused ion beam microscopy and scanning electron microscopy, provide a basis for analysing biomaterials and biointerfaces, they are incapable of doing so with both nanometre resolution and three-dimensional clarity. In contrast, electron tomography may be used to characterize the three-dimensional structure of biomaterials and their interfaces to bone with nanometre resolution. In this work, hydroxyapatite scaffolds, and laser-modified titanium and Ti6Al4V implants were studied in contact with human or rabbit bone. Z-contrast electron tomography revealed that the orientation of collagen in bone apposing hydroxyapatite, titanium and Ti6Al4V implants is consistently parallel to the implant surface, where the bioactive layer that precipitates on HA is oriented perpendicular to the implant surface. With this method, complete three-dimensional nanoscale osseointegration of titanium-based implants was also established. The extension of this technique from interfacial analyses to the design of biomaterials provided an understanding of the pore structure of mesoporous titania. In further investigations, the open three-dimensional pore network, as revealed by electron tomography, showed promise as a coating that improves implant osseointegration and enables site-specific drug-delivery from an implant surface. In summary, it was demonstrated that two-dimensional characterization techniques were insufficient for the investigation of nanostructured biomaterials, as well as their interfaces to bone. Visualizing biointerfaces and biomaterials with nanometre precision in three-dimensions can expose new fundamental information on materials properties and bone response, enabling better design of biomaterials for the future.

The deformation mechanisms operating in diamond-like carbon (DLC) coatings on (100) and (111) Si, has been investigated. The effect of coating thickness, indenter geometry, substrate orientation and deposition technique on the deformation of DLC coatings and the underlying substrate was studied by undertaking nanoindentation followed by subsurface microstructural characterization. Uncoated (111) Si was also investigated for comparison. The observed microstructural features were correlated to the indentation response of the coatings and compared with simulation studies, as well as observations on uncoated Si. In uncoated (111) Si, phase transformation was found to be responsible for the discontinuities in the load-displacement curves, similar to (100) Si. However, slip was activated on {311} planes instead of on {111} planes. Moreover, the density of defects was also significantly lower and their distribution asymmetric. The coatings were adherent, uniformly thick and completely amorphous. The load-displacement curves displayed several pop-ins and a pop-out, the indentation loads for the first pop-in and the pop-out depending primarily on the thickness of the coating. The coatings exhibited localized compressive deformation in the direction of loading without any through-thickness cracks. The extent of this localized deformation increased with indentation load. Hardness and thickness of the coatings and the geometry of the indenter influenced the magnitude of compressive strains. Harder and thinner coatings and a blunt indenter exhibited the minimum degree of deformation. Densification by rearrangement of molecules has been suggested as the mechanism responsible for plastic compression. At indentation loads corresponding to the first pop-in, (100) and (111) silicon substrates initially deformed by <111> and <311> slip respectively. Higher indentation loads caused phase transformation. Therefore, unlike in uncoated Si, dislocation nucleation in the Si substrate has been proposed as the mode responsible for the first pop-in. Subsequent pop-ins were attributed to further deformation by slip and twinning, phase transformation and extensive cracking (median and secondary cracks) of the substrate. The pop-out, however, was ascribed to phase transformation. Extensive deformation in the substrate, parallel to the interface, is attributed to the wider distribution of the stress brought about by the DLC coating. Good correlation was obtained between the nanoindentation response, microstructural features and simulation studies.

Copper-alumina composites were developed for testing in abrasive wear applications. The composites featured a porous continuous ceramic-preform network infiltrated by a liquid metal to form the final consolidated composite. The liquid metal phase was pure copper. Six different ceramic preform variants were tested. Ceramic volume fractions of 40, 50 and 60% were used, of two preform types; one pure-alumina, and one with additional 2wt% copper(I) oxide (CU20), functioning as an infiltration aid, the effects of which were determined in a previous study; the copper-oxide reduced infiltration pressure and allowed the use of higher ceramic phase volume fraction in the final composite. Abrasive wear tests against two automotive braking system materials were conducted. Grey cast iron of alloy type GG15 was used to establish a baseline for behaviour of the six different composite samples and compare them. Following this, the three volume fraction variants of samples using the copper-oxide infiltration aid were trialled against a commercially-available European passenger vehicle brake pad friction material; ABEX 6091. Wear tests were conducted on a pin-on-disc tribometer. Hemispherical-headed pins were made from the composite and tested against rotating discs of the grey cast iron and the ABEX friction material. Contact velocity was kept constant at Ims-?? at room temperature in air, and contact loads up to 15N were used. Test loads of 1-4N were used against grey cast iron, and 15N against the ABEX friction material. Optical micrography was used to monitor the wear rate of samples tested against grey cast iron. Scanning electron microscopy (SEM) was used to characterise bulk microstructures and evaluate surface wear features. Transmission electron microscopy (TEM) was used for further microstructural investigation of the sintering and interfacial features of the undamaged pin samples, as well as damage zones and tribofilm compositions. Focussed ion beam (FIB) milling was used to create subsurface cross-sections of wear regions and prepare TEM samples. The wear performance of the different sample types was compared by ceramic content and preform additives. It was found that the wear resistance of pure-alumina preform composites was dependent on ceramic volume fraction. Increasing ceramic content lead to increased wear resistance. The lower sinter temperature of the samples with the copper oxide additive led to reduced wear resistance compared with the monolithic alumina preforms and changes in ceramic volume fractions were not discernable in wear resistance against grey cast iron. This could be further supported by qualitative micrographic observations. All tests against grey cast iron were dominated by tribochemical film formation, which was determined to be oxidation of the iron which formed at the composite pin contact surface. Further testing of the copper-oxide containing samples against the ABEX friction material revealed a mixed result; the 50 and 60% ceramic volume samples produced near-identical wear performance, while the 40% sample suffered poor wear resistance. The dominant wear mechanism of composite pins tested against the ABEX friction material was abrasive wear. Sub-surface analysis of wear pins revealed a prominent damage layer forming at the contact surface of all pin samples which progressively grew into the bulk material. This layer was believed to have an important effect on the wear behaviour of the materials.

This thesis explores the theory describing wavefunctions and images, both elastic and inelastic, formed in scanning transmission electron microscopy. / A method is presented for calculating the elastic wavefunction based upon a new formulation of the boundary conditions which couples the probe to Bloch states within the crystal in a single step. Though this method is fundamentally equivalent to previous approaches based upon the superposition of wavefunctions corresponding to individual plane wave components in the incident probe, it provides new insight into the some of the dynamics, allows for efficient calculations, and proves useful for demonstrating well known results such as reciprocity relations. A formal inversion technique is also presented that uses a collection of diffraction plane data in scanning transmission electron microscopy to reconstruct the object potential, even in the presence of strong multiple scattering. / The new form of the boundary conditions allows for a generalization of a crosssection expression for calculating inelastic images, making use of the theory of mixed dynamic form factors. This enables the simulation of images for a range of inelastic mechanisms, including thermal scattering, used to simulate high-angle annular dark field imaging, and inner-shell ionization, used to simulate electron energy loss spectroscopy images. A multislice form of this expression is given. Selection between the methods can thus be based on the sample of interest: the Bloch wave method is very efficient when the sample is crystalline; the multislice method is more appropriate if the sample lacks periodicity. / The issue of cross-talk, where dynamical probe spreading may result in a signal containing contributions from several columns and therefore confound direct interpretation, is assessed for high-angle annular dark field imaging. Single atom images are simulated to provide an estimate of the localization of signal in electron energy loss spectroscopy, and confirm that the limitations of probe size generally outweigh those of the nature of the ionization interaction. The feasibility of column-by-column spectroscopic identification is demonstrated through a combination of experimental data and supporting calculations. Data demonstrating the location and spectroscopic identification of a single impurity atom in the bulk are supported by simulation and it is demonstrated that a quantitative comparison can offer further useful information: an estimate for the depth of the impurity. / The contribution to electron energy loss spectroscopy images from electrons which have undergone thermal scattering prior to causing an inner-shell ionization event is assessed. It is concluded that this contribution is significant in strongly scattering specimens imaged using fine probes. It will be necessary to include this contribution if quantitative comparisons are to be made.

Copper-alumina composites were developed for testing in abrasive wear applications. The composites featured a porous continuous ceramic-preform network infiltrated by a liquid metal to form the final consolidated composite. The liquid metal phase was pure copper. Six different ceramic preform variants were tested. Ceramic volume fractions of 40, 50 and 60% were used, of two preform types; one pure-alumina, and one with additional 2wt% copper(I) oxide (CU20), functioning as an infiltration aid, the effects of which were determined in a previous study; the copper-oxide reduced infiltration pressure and allowed the use of higher ceramic phase volume fraction in the final composite. Abrasive wear tests against two automotive braking system materials were conducted. Grey cast iron of alloy type GG15 was used to establish a baseline for behaviour of the six different composite samples and compare them. Following this, the three volume fraction variants of samples using the copper-oxide infiltration aid were trialled against a commercially-available European passenger vehicle brake pad friction material; ABEX 6091. Wear tests were conducted on a pin-on-disc tribometer. Hemispherical-headed pins were made from the composite and tested against rotating discs of the grey cast iron and the ABEX friction material. Contact velocity was kept constant at Ims-?? at room temperature in air, and contact loads up to 15N were used. Test loads of 1-4N were used against grey cast iron, and 15N against the ABEX friction material. Optical micrography was used to monitor the wear rate of samples tested against grey cast iron. Scanning electron microscopy (SEM) was used to characterise bulk microstructures and evaluate surface wear features. Transmission electron microscopy (TEM) was used for further microstructural investigation of the sintering and interfacial features of the undamaged pin samples, as well as damage zones and tribofilm compositions. Focussed ion beam (FIB) milling was used to create subsurface cross-sections of wear regions and prepare TEM samples. The wear performance of the different sample types was compared by ceramic content and preform additives. It was found that the wear resistance of pure-alumina preform composites was dependent on ceramic volume fraction. Increasing ceramic content lead to increased wear resistance. The lower sinter temperature of the samples with the copper oxide additive led to reduced wear resistance compared with the monolithic alumina preforms and changes in ceramic volume fractions were not discernable in wear resistance against grey cast iron. This could be further supported by qualitative micrographic observations. All tests against grey cast iron were dominated by tribochemical film formation, which was determined to be oxidation of the iron which formed at the composite pin contact surface. Further testing of the copper-oxide containing samples against the ABEX friction material revealed a mixed result; the 50 and 60% ceramic volume samples produced near-identical wear performance, while the 40% sample suffered poor wear resistance. The dominant wear mechanism of composite pins tested against the ABEX friction material was abrasive wear. Sub-surface analysis of wear pins revealed a prominent damage layer forming at the contact surface of all pin samples which progressively grew into the bulk material. This layer was believed to have an important effect on the wear behaviour of the materials.

Thesis (Ph.D.)--McMaster University, 2005. / Supervisor: G.C. Weatherly and M. Niewczas. Includes bibliographical references (leaves 171-177).

Thesis (M. S. in Interdisciplinary Materials Science)--Vanderbilt University, Aug. 2008. / Title from title screen. Includes bibliographical references.

Thesis (MSc.(Anatomy)--Faculty of Health Sciences)-University of Pretoria, 2007. / Includes bibliographical references.

Thesis (Ph. D.)--Ohio State University, 2005. / Title from first page of PDF file. Document formatted into pages; contains xxii, 212 p.; also includes graphics. Includes bibliographical references (p. 203-212). Available online via OhioLINK's ETD Center

abstract: The research of this dissertation has involved the nanoscale quantitative characterization of patterned magnetic nanostructures and devices using off-axis electron holography and Lorentz microscopy. The investigation focused on different materials of interest, including monolayer Co nanorings, multilayer Co/Cu/Py (Permalloy, Ni81Fe19) spin-valve nanorings, and notched Py nanowires, which were fabricated via a standard electron-beam lithography (EBL) and lift-off process. Magnetization configurations and reversal processes of Co nanorings, with and without slots, were observed. Vortex-controlled switching behavior with stepped hysteresis loops was identified, with clearly defined onion states, vortex states, flux-closure (FC) states, and Omega states. Two distinct switching mechanisms for the slotted nanorings, depending on applied field directions relative to the slot orientations, were attributed to the vortex chirality and shape anisotropy. Micromagnetic simulations were in good agreement with electron holography observations of the Co nanorings, also confirming the switching field of 700-800 Oe. Co/Cu/Py spin-valve slotted nanorings exhibited different remanent states and switching behavior as a function of the different directions of the applied field relative to the slots. At remanent state, the magnetizations of Co and Py layers were preferentially aligned in antiparallel coupled configuration, with predominant configurations in FC or onion states. Two-step and three-step hysteresis loops were quantitatively determined for nanorings with slots perpendicular, or parallel to the applied field direction, respectively, due to the intrinsic coercivity difference and interlayer magnetic coupling between Co and Py layers. The field to reverse both layers was on the order of ~800 Oe. Domain-wall (DW) motion within Py nanowires (NWs) driven by an in situ magnetic field was visualized and quantified. Different aspects of DW behavior, including nucleation, injection, pinning, depinning, relaxation, and annihilation, occurred depending on applied field strength. A unique asymmetrical DW pinning behavior was recognized, depending on DW chirality relative to the sense of rotation around the notch. The transverse DWs relaxed into vortex DWs, followed by annihilation in a reversed field, which was in agreement with micromagnetic simulations. Overall, the success of these studies demonstrated the capability of off-axis electron holography to provide valuable insights for understanding magnetic behavior on the nanoscale. / Dissertation/Thesis / Ph.D. Materials Science and Engineering 2010