Diffusion and phase change characterization by mass spectrometry

The high temperature diffusion of trace elements in metals and alloys was investigated. Measurements were made by high sensitivity mass spectrometry in which individual atoms were detected, and quantitative data was obtained for zircaloy-2, 304 stainless steel, and tantalum. Additionally, a mass spectrometer was also an analytical tool for determining an allotropic phase change for stainless steel at 955 C, and a phase transition region between 772 C and 1072 C existing for zircaloy-2. Diffusion rates were measured in thin (0.001" (0.0025 cm) and 0.0005" (0.0013 cm)) ribbons which were designed as high temperature thermal ion sources, with the alkali metals as naturally occurring impurities. In the temperature and pressure regime where diffusion measurements were made, the solute atoms evaporated from the ribbon filaments when the impurities diffused to the surface, with a fraction of these impurity atoms ionized according to the Langmuir-Saha relation. The techniques developed can be applied to many other alloys important to space vehicles and supersonic transports; and, with appropriate modifications, to the diffusion of impurities in composites.