In this work, the influence of thermal treatment on the structure of Kankara kaolinite was studied for the first time, using X-ray diffractogram (XRD), EDX, NanoSEM, FTIR-Attenuated Total Reflectance, DTA/TGA and BET surface area measurements. The treatment temperatures applied represents the peak of the transformation stages. The results show that surface area decreases with increase in temperature of treatment, while its crystal structure was transformed from the native kaolinite structure via the amorphous metakaolin to the typical mullite/crystobalite structure though with some unidentifiable peaks. The morphological studies showed that Kankara kaolinite is composed of nano-platelets of about 30nm thickness and in bundles of between 1 – 3 µm thicknesses with some marked variations/reductions as the treatment temperatures increases. The DTA/TGA result shows that the kaolinite undergoes dehydroxylation at 528.560C while been converted to metakaolin with a weight loss of about 14.4%. The presence of the characteristic OH, Al-OH, Si-OH and Si-O-Al bands were confirmed with the ATR studies which also showed the disappearance and subsequent appearance of new bands as the treatment temperature increased, this also affected the surface area and pore sizes of the transformation products
