Development of experimental verification techniques for non-linear deformation and fracture.

This project covers three distinct features of thin film fracture and deformation in which the current experimental technique of nanoindentation demonstrates limitations. The first feature is film fracture, which can be generated either by nanoindentation or bulge testing thin films. Examples of both tests will be shown, in particular oxide films on metallic or semiconductor substrates. Nanoindentations were made into oxide films on aluminum and titanium substrates for two cases; one where the metal was a bulk (effectively single crystal) material and the other where the metal was a 1 pm thick film grown on a silica or silicon substrate. In both cases indentation was used to produce discontinuous loading curves, which indicate film fracture after plastic deformation of the metal. The oxides on bulk metals fractures occurred at reproducible loads, and the tensile stress in the films at fracture were approximately 10 and 15 GPa for the aluminum and titanium oxides respectively. Similarly, bulge tests of piezoelectric oxide films have been carried out and demonstrate film fracture at stresses of only 100's of MPa, suggesting the importance of defects and film thickness in evaluating film strength. The second feature of concern is film adhesion. Several qualitative and quantitative tests exist today that measure the adhesion properties of thin films. A relatively new technique that uses stressed overlayers to measure adhesion has been proposed and extensively studied. Delamination of thin films manifests itself in the form of either telephone cord or straight buckles. The buckles are used to calculate the interfacial fracture toughness of the film-substrate system. Nanoindentation can be utilized if more energy is needed to initiate buckling of the film system. Finally, deformation in metallic systems can lead to non-linear deformation due to 'bursts' of dislocation activity during nanoindentation. An experimental study to examine the structure of dislocations around indentations has been carried out to demonstrate the effectiveness in evaluating cross slip and dislocation behavior around nanoindentation impressions in bulk engineering alloys