Effect of phase transformations on the shape of the unloading curve in the nanoindentation of silicon

Silicon wafers subject to depth-sensing indentation tests have been studied using Raman microspectroscopy. We report a strong correlation between the shape of the load-displacement curve and the phase transformations occurring within a nanoindentation. The results of Raman microanalysis of nanoindentations in silicon suggest that sudden volume change in the unloading part of the load-displacement curve (“pop-out” or “kink-back” effect) corresponds to the formation of Si–XII and Si–III phases, whereas the gradual slope change of the unloading curve (“elbow”) is due to the amorphization of silicon on pressure release. The transformation pressures obtained in nanoindentation tests are in agreement with the results of high pressure cell experiments.