The mechanical deformation of crystalline silicon induced by micro-indentation has been studied. Indentations were made using a variety of loading conditions. The effects on the final deformation microstructure of the load–unload rates and both spherical and pointed (Berkovich) indenters were investigated at maximum loads of up to 250 mN. The mechanically deformed regions were then examined using cross-sectional transmission electron microscopy (XTEM), Raman spectroscopy, and atomic force microscopy. High-pressure phases (Si-XII and Si-III) and amorphous silicon have been identified in the deformation microstructure of both pointed and spherical indentations. Amorphous Si was observed using XTEM in indentations made by the partial load–unload method, which involves a fast pressure release on final unloading. Loading to the same maximum load using the continuous load cycle, with an approximately four times slower final unloading rate, produced a mixture of Si-XII and Si-III. Slip was observed for all loading conditions, regardless of whether the maximum load exceeded that required to induce “pop-in” and occurs on the {111} planes. Phase transformed material was found in the region directly under the indenter which corresponds to the region of greatest hydrostatic pressure for spherical indentation. Slip is thought to be nucleated from the region of high shear stress under the indenter.

Spherical indentation of crystalline silicon has been studied using cross-sectional transmission electron microscopy (XTEM). Indentation loads were chosen below and above the yield point for silicon to investigate the modes of plastic deformation. Slip planes are visible in the XTEM micrographs in both indentation loads studied. A thin layer of polycrystalline material has been identified (indexed as Si-XII from diffraction patterns) on the low-load indentation. The higher-load indentation revealed a large region of amorphous silicon. The sequence of structural deformation by indentation in silicon has been observed with the initial deformation mechanism being slip until phase transformations can take place.

Ordinary materials can transform into novel phases at extraordinary high pressure and temperature. The recently developed method of ultrashort laser-induced confined microexplosions initiates a non-equilibrium disordered plasma state. Ultra-high quenching rates overcome kinetic barriers to the formation of new metastable phases, which are preserved in the surrounding pristine crystal for subsequent exploitation. Here we demonstrate that confined microexplosions in silicon produce several metastable end phases. Comparison with an ab initio random structure search reveals six energetically competitive potential phases, four tetragonal and two monoclinic structures. We show the presence of bt8 and st12, which have been predicted theoretically previously, but have not been observed in nature or in laboratory experiments. In addition, the presence of the as yet unidentified silicon phase, Si-VIII and two of our other predicted tetragonal phases are highly likely within laser-affected zones. These findings may pave the way for new materials with novel and exotic properties.

The deformation behavior of bulk ZnO single crystals is studied by a combination of spherical nanoindentation and atomic force microscopy. Results show that ZnO exhibits plastic deformation for relatively low loads (≳4–13 mN with an ∼4.2 μm radius spherical indenter). Interestingly, the elastic–plastic deformation transition threshold depends on the loading rate, with faster loading resulting, on average, in larger threshold values. Multiple discontinuities (so called “pop-in” events) in force–displacement curves are observed during indentation loading. No discontinuities are observed on unloading. Slip is identified as the major mode of plastic deformation in ZnO, and pop-in events are attributed to the initiation of slip. An analysis of partial load–unload data reveals values of the hardness and Young’s modulus of 5.0±0.1 and 111.2±4.7 GPa, respectively, for a plastic penetration depth of 300 nm. Physical processes determining deformation behavior of ZnO are discussed.

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