In the previous volume,1 we considered a full range of synthetic developments for the preparation of metal oxide nanoparticles from high temperature methods to microwave assisted synthesis to low temperature routes. A more general overview of each preparative route was given. In the current chapter, we will continue our examination of recent reports of traditional and emerging synthetic approaches to nanostructured metal oxides and metal oxide nanocomposites. We will look in detail at a number of examples of composite materials, as well as examine how these materials can be characterised in order to more extensively probe the structure-property relationship. Given the number of potential applications for metal oxide nanomaterials, we will also look at specific examples of composite materials which are under investigation for electronic, energy and catalytic applications. Recent findings have demonstrated that in some cases, carefully constructed hybrid nanostructures can promote a synergetic relationship between the composite constituents.