Group-III nitride materials are increasingly important, because of their semiconducting properties and bandgaps tuneable across a wide range from the infrared to ultraviolet. They are of particular interest for optoelectronic and power electronic applications. The studies on nitride materials are comprehensive, and one way to categorise them is based on the scale of the material, namely: (a) 3D bulk materials, for example the development of 3D bulk nitride substrate; (b) epitaxial layers, for example GaN/InGaN 2D quantum well based light emitting diodes (LEDs); (c) 1D nitride nanowires and (d) 0D quantum dots, for example InGaN quantum dot based single photon sources.

This thesis uses a multimicroscopy concept to investigate various group-III nitride nanowires and hillocks. Multiple different microscopy techniques were applied to the same specific nanostructure or defect. This allows the properties of the materials of interest to be linked directly to the nanostructures or defects, providing a more complete picture of the samples that have been studied. The multiple microscopy techniques used to conduct the work in this thesis include (scanning) transmission electron microscopy ((S)TEM), cathodoluminescence (CL), focused ion beam (FIB) and atomic force microscopy (AFM). Specifically, AFM was used to characterise the morphology of the sample on a sub-nanometer scale. The crystalline structures were characterised using (S)TEM, and the in-situ energy dispersive X-ray spectroscopy (EDS) was used to conduct compositional analysis of the selected sites. CL was used to reveal the optoelectronic properties by analysing the emission wavelengths of the materials, excited by the electron beam. FIB was the technique used to prepare site-specific samples to be measured in (S)TEM. A detailed explanation of these characterisation techniques was also included.

In the context of the studies on nitride materials, nitride nanowires and their heterostructures are a particular research focus. They combine the unique properties of III-nitride materials together with the advantages induced by the nanowire geometry. This thesis explores three different nanowire systems: a GaN nanowire structure incorporating a GaN/ScGaN axial heterostructure grown by molecular beam epitaxy (MBE); GaN/InGaN core-shell nanowires fabricated by a hybrid approach combining metalorganic vapour phase epitaxy (MOVPE) and dry etching techniques; and AlGaN nanowires on free standing AlGaN substrates fabricated by MBE and inductively coupled plasma (ICP) etching. The optoelectronic properties, compositions and structures of these nanowires were studied in detail. Moreover, a comprehensive review on the properties, growth methods and applications of group-III nitride nanowires is also included in this thesis.

Apart from nanowires, a lot of effort has been focusing on the improvement of the quality of epitaxial layers of GaN and its alloys, and they currently have an even wider perspective than nitride nanowires. The understanding of defects within the epitaxial layers is crucial in order to mitigate the their adverse effects, leading to the increased emphasis on defect analysis. Hillocks are a type of defects found on GaN epilayers, which are less well studied than other defects such as dislocations and stacking faults. As a consequence, the formation mechanisms of hillocks remain controversial. In this context, after a review on the past studies on GaN hillocks, this thesis also investigates two types of hillocks, i.e. hillocks on GaN p-i-n diodes and hillocks on GaN grown on patterned sapphire substrates (PSS). Their nanoscale structures, properties and formation mechanisms are studied.