Published online by Cambridge University Press: 21 February 2011
We have examined grain boundaries in both undoped and boron doped Ni0.76Al0.24 using electron energy loss spectroscopy (EELS), x-ray fluorescence (EDX) and annular dark field (ADF) imaging in a UHV STEM. A detailed study of a high angle grain boundary in nickel rich Ni3Al doped with 1000 ppm boron shows nickel enrichment occurring in a 5Å wide region. Boron segregation to the boundary is observed with EELS and is seen to vary along the boundary, coinciding with ADF contrast changes in the surrounding grains that may be due to local strain fields. Spatially resolved EELS of the Ni L2,3 core edge, which is sensitive to changes in the hole density in the nickel d band, shows boron rich regions of the grain boundary to have a bonding similar to that of the bulk material. Boundary regions without boron have an electronic structure similar to that of the undoped grain boundaries where the Fermi level lies deeper in the nickel d band. In addition to studying boron segregation, EELS provides a unique opportunity to examine the changes in bonding that control the local properties of the material.