Single-crystal germanium is a semiconductor material which shows complicated phase transformation under high pressure. In this study, new insight into the phase transformation of diamond-cubic germanium (dc-Ge) was attempted by controlled cyclic nanoindentation combined with Raman spectroscopic analysis. Phase transformation from dc-Ge to rhombohedral phase (r8-Ge) was experimentally confirmed for both single and cyclic nanoindentation under high loading/unloading rates. However, compared to single indentation, double cyclic indentation with a low holding load between the cycles caused more frequent phase transformation events. Double cyclic indentation caused more stress in Ge than single indentation and increased the possibility of phase transformation. With increase in the holding load, the number of phase transformation events decreased and finally became less than that under single indentation. This phenomenon was possibly caused by defect nucleation and shear accumulation during the holding process, which were promoted by a high holding load. The defect nucleation suppressed the phase transformation from dc-Ge to r8-Ge, and shear accumulation led to another phase transformation pathway, respectively. A high holding load promoted these two phenomena, and thus decreased the possibility of phase transformation from dc-Ge to r8-Ge.
Fused silica is an important optical material with important applications, where the surface must be precisely machined without subsurface damage. In this study, multi-cyclic indentations under incremental loads were performed on fused silica using two kinds of indenters to clarify the mechanisms of crack generation and propagation induced by precision grinding. It was found that incremental loading cyclic nanoindentation induced various patterns of subsurface cracking and surface spalling. Four kinds of surface spalling were identified at different locations around an indent, the temporal formation mechanisms of which were clarified by microscopic observation and topographical measurement. Load–displacement curve analysis demonstrated that incremental propagation of lateral cracks during early indentation cycles caused large-scale brittle fractures during later cycles. Compared with a Berkovich indenter, a cube-corner indenter caused more significant brittle fractures and surface spalling. The findings in this study will deepen the understanding of subsurface damaging mechanism of fused silica and other brittle solids caused by cyclic tool-workpiece interactions in grinding and other mechanical machining processes.
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