A comprehensive, bottoms-up characterization of two of the most widely used biomedical Ti-containing alloys, NiTi and β-Ti, was carried out applying a novel combination of neutron diffraction, neutron prompt-gamma activation, surface morphology, thermal analysis and mechanical tests, to relate composition, microstructure and physical-chemical-mechanical properties to unknown processing history. The commercial specimens studied are rectangular (0.43 × 0.64 mm~0.017 × 0.025 inch) wires, in both pre-formed U-shape and straight extended form. Practical performance was quantitatively linked to the influence of alloying elements, microstructure and thermo-mechanical processing. Results demonstrated that the microstructure and phase composition of β-Ti strongly depended on the composition, phase-stabilizing elements in particular, in that the 10.2 wt.% Mo content in Azdent resulted in 41.2% α phase, while Ormco with 11.6 wt.% Mo contained only β phase. Although the existence of α phase is probable in the meta-stable alloy, the α phase has never been quantified before. Further, the phase transformation behavior of NiTi directly arose from the microstructure, whilst being highly influenced by thermo-mechanical history. A strong correlation (r = 0.878) was established between phase transformation temperature and the force levels observed in bending test at body temperature, reconfirming that structure determines performance, while also being highly influenced by thermo-mechanical history. The novel methodology described is evidenced as generating a predictive profile of the eventual biomechanical properties and practical performance of the commercial materials. Overall, the work encompasses a reproducible and comprehensive approach expected to aid in future optimization and rational design of devices of metallic origin.

Prompt-gamma activation analysis (PGAA) has been extended and validated to measure large and irregularly shaped samples. The detailed sample geometry was implemented in the MCNP-model of the setup and accurate matrix-effect corrections were obtained.

The washing of cathode active materials (CAMs) for lithium-ion batteries (LIBs) to remove unwanted contaminants is of high importance in industrial CAM manufacturing. Nickel-rich NCMs (LiMO₂, M = Ni, Co, Mn), a family of commercial high-energy CAMs, are known for their detrimental reactivity with liquid/gaseous water; yet, insights on the kinetics of the occurring lithium/proton (Li⁺/H⁺) exchange are still lacking. To assess the Li⁺/H⁺ exchange, a set of five independent techniques is developed and employed to quantify its extent for a nickel-rich NCM (LiNi_0.83Co_0.12Mn_0.05O₂) as a function of the washing parameters. Using titration, prompt-gamma activation analysis, thermogravimetric analysis, temperature-dependent X-ray diffraction, and X-ray photoelectron spectroscopy, the proton content of washed NCM samples is determined, exploring the impact of washing time and water-to-CAM mass ratio. Furthermore, a highly protonated NCM (H_0.25Li_0.75Ni_0.83Co_0.12Mn_0.05O₂) is used to investigate the bulk properties, e.g., the change of lattice parameters and the spatial proton distribution, as well as the thermal decomposition of the protonated phase. The gained knowledge on the mechanism and the kinetics of the Li⁺/H⁺ exchange as well as on the decomposition mechanism of the protonated NCM phase is essential for the successful aqueous processing of nickel-rich CAMs, advancing the sustainable production of LIBs.