Mechanical Deformation Behavior of Nonpolar GaN Thick Films by Berkovich Nanoindentation
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- Wei, T., Hu, Q., Duan, R. et al. Nanoscale Res Lett (2009) 4: 753. doi:10.1007/s11671-009-9310-1
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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 Open image in new window 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 Open image in new window 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.
GaN-related III-nitride materials have drawn much attention over the last decade owing to its highly expected potential in short-wavelength optoelectronic devices, optical detectors, and semiconductor lasers [1, 2]. In order to further improve the performance of these devices, besides the optical and electrical properties of materials, mechanical characteristics and deformation behavior are also crucial for solving the problems of residual stress/strain introduced by heteroepitaxial films and multiple-layer device structures. Furthermore, semiconductor device processing involves extensively with surface contact, cracking, film delamination, and propagation of dislocations, which may degrade the performance of these devices. Consequently, significant interest in determining the mechanical characterizations of GaN materials is motivated, in particular at the nanoscale level, both in basic research and technological applications.
In this respect, nanoindentation has proven to be a powerful technique for probing the information on the mechanical properties of GaN thin films and substrates with characteristic dimensions in the sub-micron regime, such as hardness and elastic modulus, creep resistance, fracture toughness, and adhesion [3–6]. The load–displacement curves also reveal the various structural changes within the indented materials during nanoindentation [7, 8]. However, most of the nanoindentation studies were carried out on c-plane GaN films or bulk single crystals at present. To our knowledge, there are only few reports available on the mechanical deformation behavior of nonpolar GaN epitaxial layers, which have been receiving considerable attention to alleviate the spontaneous and strain-induced piezoelectric polarization effects. Such knowledge is of great importance for realizing better manufacturing processes and device stability of nonpolar GaN. In this study, we investigate the main deformation features of nonpolar m-plane GaN thick films during nanoindentation. Moreover, we also discuss how these features correlate with indentation-produced defect microstructures revealed by Raman scattering and cathodoluminescence (CL) microscopy.
The undoped wurtzite m-plane and c-plane GaN epilayers with a thickness of nearly 50 μm, grown by hydride vapor phase epitaxy (HVPE) method, was used in this study. The detailed growth procedures and structural characterization of the GaN epitaxial layers could be found elsewhere . The nanoindentation tests were performed on MTS Nano Indenter XP system with a continuous contact stiffness measurement (CSM) technique. A diamond pyramid-shaped Berkovich-type indenter tip, whose radius of curvature is approximately 50 nm, was employed for the indentation experiments. All necessary experimental parameters, such as the tip area function and frame compliance, were calibrated prior to each set of experiments using a standard fused silica specimen. A series of continuous load–unload indents were carried out at the load range of 5–500 mN. At least five independent measurements were made for one experimental point. Each indentation was separated by 50 μm to avoid possible interferences between neighboring indents. Here, all indents were performed at room temperature. The analytic method developed by Oliver and Pharr was adopted to determine the hardness (H) and Young’s modulus (E) of GaN films from the load–displacement curves .
After indentation, the contact-induced defect microstructures were analyzed using CL and Raman scattering. The CL observation was performed using a Gatan MonoCL3 plus equipment, installed on a scanning electron microscope (SEM) (FEI Quanta 200FEG) at room temperature. Finally, a LabRam HR800 spectrometer with an automatized XY table of acquisition was used to record the Raman spectra with excitation wavelength of 532 nm of Ar+laser. Raman area mapping was also recorded for the indentation. The laser beam was focused on the sample with a spot diameter of about 1 μm and the spectral resolution was better than 0.1 cm−1. All the Raman spectra were obtained in backscattering geometry.
Results and Discussion
Figure 3 also shows corresponding CL images of the m-plane indented regions at the load of 500 mN. These CL images clearly illustrate the distribution of deformation-induced extended defects which act as efficient nonradiative recombination centers and dramatically suppress CL emission. The quenching of luminescence can be observed to extend exclusively out from the center of the indentations along the Open image in new window orientation, a trend which is consistent with the evolution of cracks as discussed above. Additionally, in the perpendicular and parallel cases toward the surface slates, dark expanded regions obviously differ, as shown in Fig. 3b and e. This is comprehensible since the different distributions of stress near the indentations are produced at the two modes. In contrast, Jian et al. found an indentation pattern called “rosette” by CL emission, with a sixfold structure symmetry reflecting the hexagonal symmetry of c-plane GaN film subjected to Berkovich nanoindentation . The origin of this discrepancy can be ascribed to in-plane anisotropic defects propagation on the nonpolar m-plane GaN surface.
Figure 4b shows a map of the E2 (high) phonon frequency from the region of the indentation in Fig. 3a. In the indentation regions, it is apparent that the enhanced compressive stress mainly concentrates in the facets. The stress at the center is partly released due to the heavily deformed and strain-hardened lattice structure, suffered from the highest pressure under the indenter tip. Therefore, the high defect structure leads to the Raman shift shown in green at the indentation center. Outside the indentation, the formation of cracks does not cause the local stress relaxation as expected and instead leads to the increase of stress. Furthermore, a comparison of CL and Raman mapping clearly illustrates that the size of the dark defect-expanded regions observed in CL images around indentation coincides well with the profile of red regions with high compressive stress. However, in the defect-expanded regions outside the imprint, the E2 (high) mode remains still symmetric and slightly broadened, and no A1 (LO) mode can be observed as shown in Fig. 4c. It is thus deduced that the recrystallization process does not happen in the defect-expanded regions despite the high residual stress.
In order to summarize, details of nanoindentation-induced mechanical deformation of nonpolarm-plane GaN thick films fabricated by HVPE method have been studied by nanoindentation in combination with CL and Raman. In comparison withc-plane GaN, nonpolar GaN has the longer pop-in length and lower hardness, confirming that the orientation of the basal planes plays a key role in defining the mechanical properties of hexagonal GaN. Indentation at high load can produce slip lines and lateral cracks, preferentially propagating along the Open image in new window orientation. The comparison of CL and Raman mapping clearly illustrates that defect-expanded regions observed in CL images are in agreement with the profile of regions with high compressive stress, which represents anisotropic pattern. Finally, the recrystallization behavior is observed in the indented regions of nonpolar GaN at a maximum load up to 500 mN.
This study was supported by the National High Technology Program of China under Grant No. 2006AA03A143, the National Natural Sciences Foundation of China under Grant No. 60806001, and the Knowledge Innovation Program of the Chinese Academy of Sciences under Grant No. ISCAS2008T03. We would also like to thank Professor Li Chen of Peking University for his assistance in the Cathodoluminescence experiments.