The properties of materials change, sometimes catastrophically, as alloying elements and impurities accumulate preferentially at grain boundaries. Studies of bicrystals show that regular atomic patterns often arise as a result of this solute segregation at high-symmetry boundaries, but it is not known whether superstructures exist at general grain boundaries in polycrystals. In bismuth-doped polycrystalline nickel, we found that ordered, segregation-induced grain boundary superstructures occur at randomly selected general grain boundaries, and that these reconstructions are driven by the orientation of the terminating grain surfaces rather than by lattice matching between grains. This discovery shows that adsorbate-induced superstructures are not limited to special grain boundaries but may exist at a variety of general grain boundaries, and hence they can affect the performance of polycrystalline engineering alloys.

The ex situ lift out (EXLO) adhesion forces are reviewed and new applications of EXLO for focused ion beam (FIB)-prepared specimens are described. EXLO is used to manipulate electron transparent specimens on microelectromechanical systems carrier devices designed for in situ electron microscope analysis. A new patented grid design without a support film is described for EXLO. This new slotted grid design provides a surface for holding the specimen in place and also allows for post lift out processing. Specimens may be easily manipulated into a backside orientation to reduce FIB curtaining artifacts with this slotted grid. Large EXLO specimens can be manipulated from Xe+ plasma FIB prepared specimens. Finally, applications of EXLO and manipulation of FIB specimens using a vacuum probe lift out method are shown. The vacuum probe provides more control for placing specimens on the new slotted grids and also allows for easy manipulation into a backside configuration.

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