The high temperature reaction properties of a metal matrix composite interface have been observed in this research by X-ray reflectivity and X-ray absorption fine structure (XAFS) coupled to Auger electron spectroscopy (AES). This study was taken from the vantage point of the vanadium diffusion barrier interfacial layer in a model aluminum-graphite metal-matrix laminate composite. The interfacial couple of aluminum and vanadium was analysed to ascertain the reaction species at temperatures between 200 and 350 degrees C. X-ray reflectivity and glancing angle XAFS showed that the initial Al-V reaction occurred at 325 degrees C where the aluminum-rich intermetallic Al3V formed. Smart angle XAFS was used to analyse the higher temperature interfacial changes in the temperature range of 300-500 degrees C. Further interactions occurred at 500 degrees C, where interdiffusion of Al, C and O occurred leading to phase formation of the vanadium, dependent on the graphite basal plane orientation. AES, used to determine the initial compositions and those resulting from the high temperature heat treatments, complemented the XAFS results.