The aim of this research project was to synthesise both the normal and inverse cobalt aluminate spinels by various methods and characterise them mainly by Raman spectroscopy with the support of X-ray powder diffraction (XRD), Fourier transform infra-red spectroscopy (FT-IR), energy disperse spectroscopy (EDS), and scanning electron microscopy (SEM). Four different synthesis methods (glycine-gel, citrate-gel, polyol and solid-state) were used to synthesise the cobalt aluminate powders with the general formula CoIICoIIIxAl2-xO4 (where x = 0-2). The gel or powder precursors were annealed at various temperatures ranging from 350ºC - 1000ºC. The properties of the intermediate and final products, influenced by the synthesis method, processing temperature, processing time and particle size, were compared. Raman spectra and XRD patterns indicating the presence of both normal and inverse cobalt aluminate spinel were observed. The inverse spinel was identified both as a transitional phase as well as a final phase, depending on the synthesis method and annealing temperature used. The various synthesis methods were also used to gain further insight into the crystal chemistry of cobalt aluminate. The solid-state method is the more traditional synthesis method. Solution techniques (glycine-gel, citrate-gel and polyol) were used in an attempt to synthesise blue cobalt aluminate at relatively low temperatures and processing times in order to obtain homogeneous, nanosized crystals with broad applicability. The polyol method was found to be most favourable for the synthesis of blue cobalt aluminate with regard to processing temperature and processing time. The various characterisation methods used, show that the intensity of the colour of the powders produced are strongly related to the degree of material crystallinity as well as Al/Co ratio. Inverse (Co2AlO4) and Co3O4 spinels are formed at lower temperatures or when the Co/Al ratio is greater than 0.5. The normal spinel (CoAl2O4) is produced at higher temperatures or when the Co/Al ratio is 0.5. The XRD patterns of CoAl2O4, Co2AlO4 and Co3O4, are very similar because they share the same spinel cubic structure (space group Fd3m) differing only slightly in the lattice size. It has been demonstrated that Raman and XRD can be used to distinguish between inverse and normal spinels while FT-IR and EDS are useful for assessing the purity of the powders produced. As predicted by group theory, five Raman and four IR active vibrations were evident in the results. / Dissertation (MSc)--University of Pretoria, 2009. / Chemistry / unrestricted