Size-strain separation in diffraction line profile analysis.

Separation of size and strain effects on diffraction line profiles has been studied in a round robin involving laboratory instruments and synchrotron radiation beamlines operating with different radiation, optics, detectors and experimental configurations. The studied sample, an extensively ball milled iron alloy powder, provides an ideal test case, as domain size broadening and strain broadening are of comparable size. The high energy available at some synchrotron radiation beamlines provides the best conditions for an accurate analysis of the line profiles, as the size-strain separation clearly benefits from a large number of Bragg peaks in the pattern; high counts, reliable intensity values in low-absorption conditions, smooth background and data collection at different temperatures also support the possibility to include diffuse scattering in the analysis, for the most reliable assessment of the line broadening effect. However, results of the round robin show that good quality information on domain size distribution and microstrain can also be obtained using standard laboratory equipment, even when patterns include relatively few Bragg peaks, provided that the data are of good quality in terms of high counts and low and smooth background.

Coupling of strain, stress, and oxygen non-stoichiometry in thin film Pr0.1Ce0.9O2-δ.

Stress and strain in thin films of Pr0.1Ce0.9O2-δ, supported on yttria stabilized zirconia (YSZ) and sapphire substrates, induced by large deviations from oxygen stoichiometry (δ = 0) were investigated by in situ high temperature X-ray diffraction and wafer curvature studies. The measured stresses and strains were correlated with change in δ, measured in situ using optical transmission spectroscopy of defect centers in the films and compared with prior chemical capacitance studies. The coefficient of chemical expansion and elastic modulus values for the films were found to be 18% less than, and 16% greater than in the bulk, respectively. Irreproducible stress and strain during cycling on YSZ substrates was observed and related to microstructural changes as observed by TEM. The enthalpy of defect formation was found to be similar for films supported on sapphire and YSZ, and appeared to decrease with tensile stress, and increase with compressive stress. Larger stresses observed for YSZ supported films as compared to sapphire supported films were found and accounted for by the difference in film orientations.

Investigating the structure and biocompatibility of niobium and titanium oxides as coatings for orthopedic metallic implants.

Applying sol gel based coatings to orthopedic metallic implant materials can significantly improve their properties and lifespan in vivo. For this work, niobium (Nb2O5) and titanium (TiO2) oxides were prepared via solution processing in order to determine the effect of atomic arrangement (amorphous/crystalline) on bioactivity. Thermal evaluation on the synthesized materials identified an endotherm for Nb2O5 at 75 °C with 40% weight loss below 400 °C, and minimal weight loss between 400 and 850 °C. Regarding TiO2 an endotherm was present at 92 °C with 25% weight loss below 400 °C, and 4% between 400 and 850 °C. Phase evolution was determined using High Temperature X-ray Diffraction (HT-XRD) where amorphous-Nb2O5 (450 °C), hexagonal-Nb2O5 (525 °C), orthorhombic-Nb2O5 (650 °C), amorphous-TiO2 (275 °C) and tetragonal TiO2 (500 °C) structures were produced. Simulated body fluid (SBF) testing was conducted over 1, 7 and 30 days and resulted in positive chemical and morphological changes for crystalline Nb2O5 (525 °C) and TiO2 (500 °C) after 30 days of incubation. Rod-like CaP deposits were observed on the surfaces using Scanning Electron Microscopy (FE-SEM) and Grazing Incidence-X-ray Diffraction (GI-XRD) shows that the deposits were X-ray amorphous. Cell viability was higher with the TiO2 (122%) samples when compared to the growing cell population while Nb2O5 samples exhibited a range of viability (64-105%), partially dependent on materials atomic structure.

Fabrication of CaO-NaO-SiO(2)/TiO (2) scaffolds for surgical applications.

A series of titanium (Ti) based glasses were formulated (0.62 SiO(2)-0.14 Na(2)O-0.24 CaO, with 0.05 mol% TiO(2) substitutions for SiO(2)) to develop glass/ceramic scaffolds for bone augmentation. Glasses were initially characterised using X-ray diffraction (XRD) and particle size analysis, where the starting materials were amorphous with 4.5 µm particles. Hot stage microscopy and high temperature XRD were used to determine the sintering temperature (~700 °C) and any crystalline phases present in this region (Na(2)Ca(3)Si(6)O(16), combeite and quartz). Hardness testing revealed that the Ti-free control (ScC-2.4 GPa) had a significantly lower hardness than the Ti-containing materials (Sc1 and Sc2 ~6.6 GPa). Optical microscopy determined pore sizes ranging from 544 to 955 µm. X-ray microtomography calculated porosity from 87 to 93 % and surface area measurements ranging from 2.5 to 3.3 SA/mm(3). Cytotoxicity testing (using mesenchymal stem cells) revealed that all materials encouraged cell proliferation, particularly the higher Ti-containing scaffolds over 24-72 h.