The Compelling Case for Indentation as a Functional Exploratory and Characterization Tool

The utility of indentation testing for characterizing a wide range of mechanical properties of brittle materials is highlighted in light of recent articles questioning its validity, specifically in relation to the measurement of toughness. Contrary to assertion by some critics, indentation fracture theory is fundamentally founded in Griffith–Irwin fracture mechanics, based on model crack systems evolving within inhomogeneous but well-documented elastic and elastic–plastic contact stress fields. Notwithstanding some numerical uncertainty in associated stress intensity factor relations, the technique remains an unrivalled quick, convenient and economical means for comparative, site-specific toughness evaluation. Most importantly, indentation patterns are unique fingerprints of mechanical behavior and thereby afford a powerful functional tool for exploring the richness of material diversity. At the same time, it is cautioned that unconditional usage without due attention to the conformation of the indentation patterns can lead to overstated toughness values. Limitations of an alternative, more engineering approach to fracture evaluation, that of propagating a pre-crack through a 'standard' machined specimen, are also outlined. Misconceptions in the critical literature concerning the fundamental nature of crack equilibrium and stability within contact and other inhomogeneous stress fields are discussed.This is the author accepted manuscript. The final version is available from Wiley via http://dx.doi.org/10.1111/jace.1372

Berkovich Nanoindentation on AlN Thin Films

Berkovich nanoindentation-induced mechanical deformation mechanisms of AlN thin films have been investigated by using atomic force microscopy (AFM) and cross-sectional transmission electron microscopy (XTEM) techniques. AlN thin films are deposited on the metal-organic chemical-vapor deposition (MOCVD) derived Si-doped (2 × 1017 cm−3) GaN template by using the helicon sputtering system. The XTEM samples were prepared by means of focused ion beam (FIB) milling to accurately position the cross-section of the nanoindented area. The hardness and Young’s modulus of AlN thin films were measured by a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. The obtained values of the hardness and Young’s modulus are 22 and 332 GPa, respectively. The XTEM images taken in the vicinity regions just underneath the indenter tip revealed that the multiple “pop-ins” observed in the load–displacement curve during loading are due primarily to the activities of dislocation nucleation and propagation. The absence of discontinuities in the unloading segments of load–displacement curve suggests that no pressure-induced phase transition was involved. Results obtained in this study may also have technological implications for estimating possible mechanical damages induced by the fabrication processes of making the AlN-based devices

Exotic silicon phases synthesized through ultrashort laser-induced microexplosion: Characterization with Raman microspectroscopy

Exotic metastable phases of silicon formed under high pressure are expected to have attractive semiconducting properties including narrow band gaps that open up novel technological applications. Confined microexplosions induced by powerful ultrashort laser pulses have been demonstrated as an advanced tool for the creation of new high-pressure phases that cannot be synthesized by other means. Tightly focused laser pulses are used to generate localised modifications inside the material structure, providing the possibility for precise controlled bandgap engineering. In this study, non-invasive Raman spectroscopy was used for analysis of laser-modified zones in silicon and to determine the metastable high- pressure phases contained. Low laser energies induced the formation of amorphous only silicon, while higher energies led to crystalline silicon polymorphs within the modifications, albeit under considerable residual stress up to 4.5 GPa. The presence of the structurally similar r8-Si, bc8-Si and bt8-Si phases is revealed, as well as other yet to be identified phases, and the stacking-related 9R Si polytype is evidenced, presumably stress-induced by the highly compressed laser-modified zone. The ab initio random structure searching approach is used to complementary calculate the Raman signatures and help to identify different Si polymorphs. These findings by Raman spectroscopy from ultrashort laser-induced microexplosion sites may yield novel insights into the local structure and properties of new silicon metastable phases and on the prospect of utilising exotic phases for extending current applications.Royal Society Wolfson Research Merit Awar

Mechanical Deformation Behavior of Nonpolar GaN Thick Films by Berkovich Nanoindentation

In this study, the deformation mechanisms of nonpolar GaN thick films grown on m-sapphire by hydride vapor phase epitaxy (HVPE) are investigated using nanoindentation with a Berkovich indenter, cathodoluminescence (CL), and Raman microscopy. Results show that nonpolar GaN is more susceptible to plastic deformation and has lower hardness thanc-plane GaN. After indentation, lateral cracks emerge on the nonpolar GaN surface and preferentially propagate parallel to the orientation due to anisotropic defect-related stresses. Moreover, the quenching of CL luminescence can be observed to extend exclusively out from the center of the indentations along the orientation, a trend which is consistent with the evolution of cracks. The recrystallization process happens in the indented regions for the load of 500 mN. Raman area mapping indicates that the distribution of strain field coincides well with the profile of defect-expanded dark regions, while the enhanced compressive stress mainly concentrates in the facets of the indentation

Observation of enhanced defect emission and excitonic quenching from spherically indented ZnO

The influence of spherical nanoindentation on the band edge and deep level emission of single crystal c-axis ZnO has been studied by cathodoluminescence (CL) spectroscopy and monochromatic imaging. Excitonic emission is quenched at the indent site and defect emission in the range of 450-720 nm is enhanced. Analysis of CL monochromatic images and spectra suggests that at least two different defect states are responsible for the broad defect emission band. Additionally, the indents result in a strong crystallographic dependence of the defect emission, producing a rosette feature with [112̄0] [21̄1̄0], and [12̄10] orientations that reflect the star-shaped luminescence quenching observed at the excitonic peak (390 nm). © 2006 American Institute of Physics

A quantitative assessment of the mechanical strength of the polar pteropod Limacina helicina antarctica shell

This work directly measures the mechanical properties of pteropod shells collected from the Southern Ocean on the 2007 midsummer Subantarctic Zone Sensitivity to Environmental Change (SAZ-Sense) voyage. Shells from the common Southern Ocean pteropod Limacina helicina antarctica were subjected to mechanical analyses in combination with detailed morphological studies. Average hardness and modulus of 2.30 ± 0.07 GPa and 45.27 ± 0.91 GPa, respectively were calculated from several hundred nanoindentation measurements taken from multiple positions across twelve shells of the same species collected under identical conditions. Quantitative data such as these are critical to establish a reference point for future comparative studies and to both understand and evaluate the implications of further ocean acidification on the structural integrity of these common polar calcifiers, particularly in light of their role in the Southern Ocean carbon cycle and food web

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. © 2002 American Institute of Physics

Microstructural shell strength of the Subantarctic pteropod Limacina helicina antarctica

Anthropogenic inputs of CO2 are changing ocean chemistry and will likely affect calcifying marine organisms, particularly aragonite producers such as pteropods. This work seeks to set a benchmark analysis of pteropod shell properties and variability using nanoindentation and electron microscopy to measure the structural and mechanical properties of Subantarctic pteropod shells (Limacina helicina antarctica) collected in 1998 and 2007. The 1998 shells were collected by a sediment trap deployed at 2000 m, 47°S, 142°E, and the 2007 shells were collected using nets from mixed-layer waters in the region (44°–54°S, 140°–155°E). Transmission electron microscopy revealed that the shells are composed of a polycrystalline structure, and no obvious porosity was visible. The hardness and modulus of the shells were measured using shell cross-section nanoindentation, across various regions of the shell from the inner to outer whorl. No change in mechanical properties was found with respect to the region of the shell cross-section probed. There was no statistically significant difference in the mean modulus or hardness of the shells between the 1998 and 2007 data sets. No major changes in the mechanical properties of these pteropod shells were detected between the 1998 and 2007 data sets, and we discuss the possible biases in the sampling techniques in complicating our analysis. However, quantifying the mechanical properties and microstructure of calcified may still provide insights into the responses of calcification to environmental changes, such as ocean acidification