The diffusion coatings were deposited on commercially pure Ti and Ti-6Al-4V alloy at up to 1000 °C for up to 10 h using the pack cementation method. The pack powders consisted of 4 wt% Al (Al reservoir) and 4 wt% NHCl (activator) which were balanced with AlO (inert filler). The growth kinetics of coatings were gravimetrically measured by a high precision balance. The aluminised specimens were characterised by means of scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD). At the early stages of deposition, a TiO (rutile) scale, other than aluminide coating, was developed on both materials at <900 °C. As the experimental temperature arose above 900 °C, the rutile layer became unstable and reduced to the low oxidation state of Ti oxides. When the temperature increased to 1000 °C, the TiO scale dissociated almost completely and the aluminide coating began to develop. After a triple-layered coating was generated, the coating growth was governed by the outward migration of Ti species from the substrates and obeyed the parabolic law. The coating formed consisted of an outer layer of AlTi, a mid-layer of AlTi and an inner layer of AlTi. The outer layer of AlTi dominated the thickness of the aluminide coating.