Atomic layer deposition (ALD) is an important tool for the research and fabrication of thin-films, used across a wide variety of applications, including the creation of thin metal-oxides, used in the fabrication of high-k semiconductor devices. This scope of this study was to design and build a ‘home-made’ ALD chamber, with a coupled in-situ X-ray Photoelectron Spectroscopy (XPS) tool, in order to be able to characterise the chemical components of thermally grown ALD films before exposing them to atmospheric contamination. Thermally grown films of aluminium oxide were grown using trimethylaluminium (TMA) as a precursor and H2O as a co-reactant. These films were grown at differing temperatures and initial surface conditions, in order to test which conditions led to the most ideal films. Titanium oxide films were also grown using a similar method, (employing titanium isopropoxide (TTIP) as the precursor and H2O as the co-reactant) to ensure the chamber was compatible with a variety of different ALD techniques. While some degree of aluminosilicate growth was observed for all aluminium oxide samples, the growth rates and film compositions for both the TMA and TTIP films were similar to those observed in other studies. These findings show that the system designed works as intended and shows its potential to be used as a process characterisation tool for ALD thin-film processes.