Jodie Bradby

Mechanical deformation of single-crystal ZnO

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.

Mechanical Deformation in Silicon by Micro-indentation

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.

Transmission electron microscopy observation of deformation microstructure under spherical indentation in silicon

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.

Nanoindentation of epitaxial GaN films

Wurtzite GaN films grown on sapphire substrates are studied by nanoindentation with a spherical indenter. No systematic dependence of the mechanical properties of GaN epilayers on the film thickness (at least for thicknesses from 1.8 to 4 μm) as well as on doping type is observed. Slip is identified as one of the physical mechanisms responsible for plastic deformation of GaN and may also contribute to the “pop-in” events observed during loading. No visible material cracking is found even after indentations at high loads (900 mN), but a pronounced elevation of the material surrounding the impression is observed.

Indentation-induced damage in GaN epilayers

The mechanical deformation of wurtzite GaN epilayers grown on sapphire substrates is studied by spherical indentation, cross-sectional transmission electron microscopy (XTEM), and scanning cathodoluminescence (CL) monochromatic imaging. CL imaging of indents which exhibit plastic deformation (based on indentation data) shows an observable “footprint” of deformation-produced defects that result in a strong reduction in the intensity of CL emission. Multiple discontinuities are observed during loading when the maximum load is above the elastic-plastic threshold, and such a behavior can be correlated with multiple slip bands revealed by XTEM. No evidence of pressure-induced phase transformations is found from within the mechanically damaged regions using selected-area diffraction patterns. The main deformation mechanism appears to be the nucleation of slip on the basal planes, with dislocations being nucleated on additional planes on further loading. XTEM reveals no cracking or delamination in any of the sam...

Contact-induced defect propagation in ZnO

Contact-induced damage has been studied in single-crystal (wurtzite) ZnO by cross-sectional transmission electron microscopy (XTEM) and scanning cathodoluminescence (CL) monochromatic imaging. XTEM reveals that the prime deformation mechanism in ZnO is the nucleation of slip on both the basal and pyramidal planes. Some indication of dislocation pinning was observed on the basal slip planes. No evidence of either a phase transformation or cracking was observed by XTEM in samples loaded up to 50 mN with an ∼4.2 μm radius spherical indenter. CL imaging reveals a quenching of near-gap emission by deformation-produced defects. Both XTEM and CL show that this comparatively soft material exhibits extensive deformation damage and that defects can propagate well beyond the deformed volume under contact. Results of this study have significant implications for the extent of contact-induced damage during fabrication of ZnO-based (opto)electronic devices.

Mechanical deformation of InP and GaAs by spherical indentation

The mechanical deformation by spherical indentation of both crystalline InP and GaAs was characterized using cross-sectional transmission electron microscopy (XTEM) and atomic force microscopy. All load–unload curves show a discontinuity (or “pop in”) during loading. Slip bands oriented along {111} planes are visible in XTEM micrographs from residual indentations in both materials and no evidence of any phase transformations was found. Higher load indentations (35 mN for InP and 50 mN for GaAs) also revealed subsurface cracking. In contrast no cracking was found beneath a 25 mN InP indent although the hardness and modulus data are almost identical to those of the cracked sample. The subsurface cracks are thought to be nucleated by high stress concentrations caused by dislocation pileup.

Mechanical properties of ZnO epitaxial layers grown on a- and c-axis sapphire

The University of Sydney, for constructive comments and support. The work at UF is partially supported by the AFOSR under Grant Nos. F49620-03-1-0370 sT.S.d and NSF DMR 0400416.

Nitrogen-rich indium nitride

K.S.A.B. would like to acknowledge the support of an Australian Research Council Fellowship. We would also like to acknowledge the support of the Australian Research Council through a Large grant and a Discovery grant; the support of a Macquarie University Research Development Grant, and the Australian Institute of Nuclear Science and Engineering for SIMS access.

Formation and growth of nanoindentation-induced high pressure phases in crystalline and amorphous silicon

Nanoindentation-induced formation of high pressure crystalline phases (Si-III and Si-XII) during unloading has been studied by Raman micro-spectroscopy, cross-sectional transmission electron microscopy (XTEM), and postindentation electrical measurements. For indentation in crystalline silicon (c-Si), rapid unloading (∼1000 mN∕s) results in the formation of amorphous silicon (a-Si) only; a result we have exploited to quench the formation of high pressure phases at various stages during unloading to study their formation and evolution. This reveals that seed volumes of Si-III and Si-XII form during the early stages of unloading with substantial volumes only forming after the pop-out event that occurs at about 50% of the maximum load. In contrast, high pressure phases form much more readily in an a-Si matrix, with substantial volumes forming without an observable pop-out event with rapid unloading. Postindentation electrical measurements have been used to further investigate the end phases and to identify di...