Surfaces and interfaces in nano-scale and nano-structured materials

Abstract

In this thesis, advanced characterisation methods, including atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) were employed to study surface and interfaces in a range of nano-scale and nano-structured materials. These techniques were used to measure solute segregation towards grain boundaries and to explore the relationship between grain boundary segregation and grain boundary mobility. APT was also used to characterise the structure of nanoparticles used as catalysts, and the adsorption behaviour of sulphur on catalytic surfaces, to gain more information about the structure-activity relationships, and deactivation processes. This research included the development and improvement of new and existing APT sample preparation techniques, conducting the experiments, and data analysis. The first part of this thesis is concerned with nanocrystalline alloys processed by severe plastic deformation. In the second part the exceptional hardening of an 316L austenitic steel during annealing was also investigated using APT. This thesis also concentrated on the study of nanoparticles for catalysis via APT. Systematic investigations of different APT sample preparation techniques were performed in order to find a way of producing reproducible and reliable specimens. Different acquisition parameters, substrates and coatings were tested to improve the APT data quality. Experiments were conducted in which needles were dipped in thiophene. Here the aim was to investigate the phenomenon of sulphur poisoning by using APT to investigate how thiophene bonds with different metal substrates. A glovebag setup was designed for the transfer of APT samples in a controlled environment, to avoid oxidation of the samples. This allowed the comparison of oxidised and un-oxidised specimen states. In the last part of this thesis, the accuracy of crystallographic information contained within APT datasets was verified for the first time by comparing the datasets to TKD measurements.