Deactivation of titanium during temperature-induced hydrogen absorption–desorption cycling

The cyclic stability of metallic titanium during absorption–desorption runs in continuous flow system has been studied in the presence of variable level of impurities such as H ₂O, O ₂ and N ₂ in argon and helium flows. Hydrogen absorption–desorption cycles performed in vacuo were reproducible with respect to the absorption rates and uptakes, while absorption–desorption cycles carried out in the flows of carrier gases in the thermoprogrammed mode resulted in the gradual decrease of hydrogen uptakes followed by a shift of absorption maxima from 800 K to 1000 K. Mass-spectral analysis of the main impurities in a flow of gases revealed that during hydrogen absorption–desorption traces of water, oxygen and nitrogen are consumed by titanium. For the samples subjected to several absorption–desorption cycles in the flow of inert gas XRD revealed the formation of nitrogen-containing titanium compounds, while XPS showed surface enrichment in nitrogen, while oxygen concentration was constant. Nitrogen consumed at higher temperatures during the TPD runs provides better inhibition of hydrogen absorption compared to water and oxygen. Final deactivation state of titanium correlates in general with the overall amount of impurities in the stream. Although deactivation is controlled mostly by the level of toxic impurities in the feed, certain parameters, i.e., hydrogen absorption/desorption rates are dependent on the nature of neutral media—in contrast to helium, noticeable hydrogen desorption occurs even at room temperature in a flow of pure argon.