Characterization of the Induced Plastic Zone in a Single Crystal TiN(001) Film by Nanoindentation and Transmission Electron Microscopy

The slip system of TiN at room temperature has been determined to be {110} 〈110〉 by Burgers vector analysis using transmission electron microscopy and slip trace analysis of indents made on a TiN(001) film deposited on a MgO(001) substrate. Both small indents (0.4 mN maximum load) and large indents (40 mN maximum load) were used to study the dislocation structure in TiN. The nucleation of dislocations was investigated using small indents. Further development of the plastic zone was studied using large indents and microhardness indents (1.6 N). The critical resolved shear stress evaluated at the load when pop-in occurs was estimated to be 3.7 GPa, assuming a Hertzian elastic contact. Indents made with a 0.4 mN maximum load show a complex dislocation pattern with loops and straight segments that belong to the same slip system. Dislocations of mixed screw and edge type are dominant. The cascade of dislocations generated during pop-in is likely to nucleate from loops. For larger indents, the plastic zone extends more than three times the diameter of the imprint. The straight dislocations outside the large imprint are arranged in arrays along the 〈100〉 and 〈110〉 directions. A scanning force microscopy study of the surface outside a microhardness indent revealed a raised surface along 〈110〉 and formation of troughs along 〈100〉.