Formation of titanium nitride layers on titanium metal: Results of XPS and AES investigations

The reaction of titanium metal with gaseous nitrogen and ammonia at temperatures of 8900C leads to the formation of nitridic overlayers on the metallic substrate. The thicknesses of the overlayers increase with increasing reaction time. Under comparable conditions ammonia reacts much slower than nitrogen. XPS and AES depth profile analyses show continuous changes of the in-depth compositions of the overlayers. This can be interpreted in terms of a very irregular thickness of the overlayers, an assumption which is substantiated by local AES analyses and by the observation of a pronounced crystalline structure of the substrate after annealing pretreatment, which can give rise to locally different reaction rates. The depth profile is also influenced by the broad ranges of stability of the titanium nitride phases formed during the reaction. The quantitative analysis of the titanium/nitrogen overlayers by AES is difficult because of the overlap of titanium and nitrogen Auger peaks. In quantitative XPS analysis problems arise due to difficulties in defining Ti 2p peak areas. This work presents practical procedures for the quantitative evaluation by XPS and AES of nitridic overlayers with sufficient accuracy. (orig.)