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

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

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

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

Structural characterization of B-doped diamond nanoindentation tips

Copyright © Materials Research Society 2011. We report on the electrical and structural properties of boron-doped diamond tips commonly used for in-situ electromechanical testing during nanoindentation. The boron dopant environment, as evidenced by cathodoluminescence (CL) microscopy, revealed significantly different boron states within each tip. Characteristic emission bands of both electrically activated and nonelectrically activated boron centers were identified in all boron-doped tips. Surface CL mapping also revealed vastly different surface properties, confirming a high amount of nonelectrically activated boron clusters at the tip surface. Raman microspectroscopy analysis showed that structural characteristics at the atomic scale for boron-doped tips also differ significantly when compared to an undoped diamond tip. Furthermore, the active boron concentration, as inferred via the Raman analysis, varied greatly from tip-to-tip. It was found that tips (or tip areas) with low overall boron concentration have a higher number of electrically inactive boron, and thus non-Ohmic contacts were made when these tips contacted metallic substrates. Conversely, tips that have higher boron concentrations and a higher number of electrically active boron centers display Ohmic-like contacts. Our results demonstrate the necessity to understand and fully characterize the boron environments, boron concentrations, and atomic structure of the tips prior to performing in situ electromechanical experiments, particularly if quantitative electrical data are required

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 samples studied for loads of up to 250 mN. © 2002 American Institute of Physics

Nitrogen-rich indium nitride

Elastic recoil detection analysis, using an incident beam of 200 MeV Au ions, has been used to measure indium nitride films grown by radio-frequency sputtering. It is shown that the films have nitrogen-rich stoichiometry. Nitrogen vacancies are therefore unlikely to be responsible for the commonly observed high background carrier concentration. Ultraviolet Raman and secondary ion mass spectroscopy measurements are used to probe the state of the excess nitrogen. The nitrogen on indium anti-site defect is implicated, though other possibilities for the site of the excess nitrogen, such as molecular nitrogen, or di-nitrogen interstitials cannot be excluded. It is further shown that a shift in the (0002) x-ray diffraction peak correlates with the excess nitrogen, but not with the oxygen observed in some samples.5 page(s