We develop a reciprocal-space model that describes the (hkl) dependence of the broadened Bragg peakwidths produced by x-ray diffraction from a dislocated epilayer. We compare the model to experiments and find that it accurately describes the peakwidths of 16 different Bragg reflections in the [010] zone of both GaN and AlN heterolayers. Using lattice-distortion parameters determined by fitting the model to selected reflections, we estimate threading-dislocation densities for seven different GaN and AlGaN samples and find improved agreement with transmission electron microscopy measurements.

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Procedures have been developed based on finite-element modeling of nanoindentation data to obtain the mechanical properties of thin films and ion-beam-modified layers independently of the properties of the underlying substrates. These procedures accurately deduce the yield strength, Young’s elastic modulus, and layer hardness from indentations as deep as 50% of the layer thickness or more. We have used these procedures to evaluate materials ranging from ion implanted metals to deposited, diamond-like carbon layers. The technique increases the applicability of indentation testing to very thin layers, composite layers, and modulated compositions. This article presents an overview of the procedures involved and illustrates them with selected examples.

We have developed a process for making thick, stress-free, amorphous-tetrahedrally bonded carbon (a-tC) films with hardness and stiffness near that of diamond. Using pulsed-laser deposition, thin a-tC films (0.1–0.2 μm) were deposited at room temperature. The intrinsic stress in these films (6–8 GPa) was relieved by a short (2 min) anneal at 600 °C. Raman and electron energy-loss spectra from single-layer annealed specimens show only subtle changes from as-grown films. Subsequent deposition and annealing steps were used to build up thick layers. Films up to 1.2 μm thick have been grown that are adherent to the substrate and have low residual compressive stress (<0.2 GPa). The values of hardness and modulus determined directly from an Oliver–Pharr analysis of nanoindentation experimental data were 80.2 and 552 GPa, respectively. We used finite-element modeling of the experimental nanoindentation curves to separate the “intrinsic” film response from the measured substrate/film response. We found a hardness of 88 GPa and Young’s modulus of 1100 GPa. From these fits, a lower bound on the compressive yield stress of diamond (∼100 GPa) was determined.

To examine further the strain relaxation produced by inclined threading dislocations in AlGaN, a heterostructure with three AlGaN layers having successively increasing Ga contents and compressive strains was grown on an AlN template layer by metalorganic vapor-phase epitaxy. The strain state of the layers was determined by x-ray diffraction (XRD) and the dislocation microstructure was characterized with transmission electron microscopy (TEM). As the GaN mole fraction of the heterostructure increased from 0.15 to 0.48, the increased epitaxial strain produced inclined dislocations with successively greater bend angles. Using the observed bend angles, which ranged from 6.7° to 17.8°, the measured strain relaxation within each layer was modeled and found to be accounted for by threading-dislocation densities of 6–7×109/cm2, in reasonable agreement with densities determined by TEM and XRD. In addition to the influence of lattice-mismatch strain on the average bend angle, we found evidence that local strain inhomogeneities due to neighboring dislocations influence the specific bend angles of individual dislocations. This interaction with local strain fields may contribute to the large spread in the bend angles observed within each layer. A detailed TEM examination found that the initial bending of threading dislocations away from vertical often occurs at positions within <15 nm of the AlGaN/AlN heterointerface. Under the assumption that dislocation climb mediated by bulk-defect diffusion is effectively suppressed at the growth temperature, this result implies that inclination is established by processes occurring at the dynamic growth surface. We describe a mechanism where dislocation bending occurs by means of dislocation-line jogs created when surface steps overgrow vacancies that attach to threading-dislocation cores at their intersection with the growth surface.