Influence of an InGaN superlattice pre-layer on the performance of semi-polar (11-22) green LEDs grown on silicon.

It is well-known that it is crucial to insert either a single InGaN underlayer or an InGaN superlattice (SLS) structure (both with low InN content) as a pre-layer prior to the growth of InGaN/GaN multiple quantum wells (MQWs) served as an active region for a light-emitting diode (LED). So far, this growth scheme has achieved a great success in the growth of III-nitride LEDs on c-plane substrates, but has not yet been applied in the growth of any other orientated III-nitride LEDs. In this paper, we have applied this growth scheme in the growth of semi-polar (11-22) green LEDs, and have investigated the impact of the SLS pre-layer on the optical performance of semi-polar (11-22) green LEDs grown on patterned (113) silicon substrates. Our results demonstrate that the semi-polar LEDs with the SLS pre-layer exhibit an improvement in both internal quantum efficiency and light output, which is similar to their c-plane counterparts. However, the performance improvement is not so significant as in the c-plane case. This is because the SLS pre-layer also introduces extra misfit dislocations for the semi-polar, but not the c-plane case, which act as non-radiative recombination centres.

Metrology of crystal defects through intensity variations in secondary electrons from the diffraction of primary electrons in a scanning electron microscope.

Understanding defects and their roles in plastic deformation and device reliability is important for the development of a wide range of novel materials for the next generation of electronic and optoelectronic devices. We introduce the use of gaseous secondary electron detectors in a variable pressure scanning electron microscope for non-destructive imaging of extended defects using electron channelling contrast imaging. We demonstrate that all scattered electrons, including the secondary electrons, can provide diffraction contrast as long as the sample is positioned appropriately with respect to the incident electron beam. Extracting diffraction information through monitoring the modulation of the intensity of secondary electrons as a result of diffraction of the incident electron beam, opens up the possibility of performing low energy electron channelling contrast imaging to characterise low atomic weight and ultra-thin film materials. Our methodology can be adopted for large area, nanoscale structural characterisation of a wide range of crystalline materials including metals and semiconductors, and we illustrate this using the examples of aluminium nitride and gallium nitride. The capability of performing electron channelling contrast imaging, using the variable pressure mode, extends the application of this technique to insulators, which usually require conducting coatings on the sample surface for traditional scanning electron microscope based microstructural characterisation.

Improving EBSD precision by orientation refinement with full pattern matching.

We present a comparison of the precision of different approaches for orientation imaging using electron backscatter diffraction (EBSD) in the scanning electron microscope. We have used EBSD to image the internal structure of WC grains, which contain features due to dislocations and subgrains. We compare the conventional, Hough-transform based orientation results from the EBSD system software with results of a high-precision orientation refinement using simulated pattern matching at the full available detector resolution of 640 × 480 pixels. Electron channelling contrast imaging (ECCI) is used to verify the correspondence of qualitative ECCI features with the quantitative orientation data from pattern matching. For the investigated sample, this leads to an estimated pattern matching sensitivity of about 0.5 mrad (0.03°) and a spatial feature resolution of about 100 nm. In order to investigate the alternative approach of postprocessing noisy orientation data, we analyse the effects of two different types of orientation filters. Using reference features in the high-precision pattern matching results for comparison, we find that denoising of orientation data can reduce the spatial resolution, and can lead to the creation of orientation artefacts for crystallographic features near the spatial and orientational resolution limits of EBSD.

Determining GaN Nanowire Polarity and its Influence on Light Emission in the Scanning Electron Microscope.

The crystal polarity of noncentrosymmetric wurtzite GaN nanowires is determined nondestructively in the scanning electron microscope using electron backscatter diffraction (EBSD). The impact of the nanowire polarity on light emission is then investigated using cathodoluminescence (CL) spectroscopy. EBSD can determine polarity of noncentrosymmetric crystals by interrogating differences in the intensity distribution of bands of the EBSD pattern associated with semipolar planes. Experimental EBSD patterns from an array of GaN nanowires are compared with theoretical patterns produced using dynamical electron simulations to reveal whether they are Ga- or N-polar or, as in several cases, of mixed polarity. CL spectroscopy demonstrates the effect of the polarity on light emission, with spectra obtained from nanowires of known polarity revealing a small but measurable shift (≈28 meV) in the GaN near band edge emission energy between those with Ga and N polarity. We attributed this energy shift to a difference in impurity incorporation in nanowires of different crystal polarity. This approach can be employed to nondestructively identify polarity in a wide range of noncentrosymmetric nanoscale material systems and provide direct comparison with their luminescence.

Practical application of direct electron detectors to EBSD mapping in 2D and 3D.

The use of a direct electron detector for the simple acquisition of 2D electron backscatter diffraction (EBSD) maps and 3D EBSD datasets with a static sample geometry has been demonstrated in a focused ion beam scanning electron microscope. The small size and flexible connection of the Medipix direct electron detector enabled the mounting of sample and detector on the same stage at the short working distance required for the FIB. Comparison of 3D EBSD datasets acquired by this means and with conventional phosphor based EBSD detectors requiring sample movement showed that the former method with a static sample gave improved slice registration. However, for this sample detector configuration, significant heating by the detector caused sample drift. This drift and ion beam reheating both necessitated the use of fiducial marks to maintain stability during data acquisition.

Quantitative imaging of anti-phase domains by polarity sensitive orientation mapping using electron backscatter diffraction.

Advanced structural characterisation techniques which are rapid to use, non-destructive and structurally definitive on the nanoscale are in demand, especially for a detailed understanding of extended-defects and their influence on the properties of materials. We have applied the electron backscatter diffraction (EBSD) technique in a scanning electron microscope to non-destructively characterise and quantify antiphase domains (APDs) in GaP thin films grown on different (001) Si substrates with different offcuts. We were able to image and quantify APDs by relating the asymmetrical intensity distributions observed in the EBSD patterns acquired experimentally and comparing the same with the dynamical electron diffraction simulations. Additionally mean angular error maps were also plotted using automated cross-correlation based approaches to image APDs. Samples grown on substrates with a 4° offcut from the [110] do not show any APDs, whereas samples grown on the exactly oriented substrates contain APDs. The procedures described in our work can be adopted for characterising a wide range of other material systems possessing non-centrosymmetric point groups.

Diffraction effects and inelastic electron transport in angle-resolved microscopic imaging applications.

We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations.

Rapid nondestructive analysis of threading dislocations in wurtzite materials using the scanning electron microscope.

We describe the use of electron channeling contrast imaging in the scanning electron microscope to rapidly and reliably image and identify threading dislocations (TDs) in materials with the wurtzite crystal structure. In electron channeling contrast imaging, vertical TDs are revealed as spots with black-white contrast. We have developed a simple geometric procedure which exploits the differences observed in the direction of this black-white contrast for screw, edge, and mixed dislocations for two electron channeling contrast images acquired from two symmetrically equivalent crystal planes whose g vectors are at 120° to each other. Our approach allows unambiguous identification of all TDs without the need to compare results with dynamical simulations of channeling contrast.

Characterization of nitride thin films by electron backscatter diffraction.

Thin films incorporating GaN, InGaN and AlGaN are presently arousing considerable excitement because of their suitability for UV and visible light-emitting diodes and laser diodes. However, because of the lattice mismatch between presently used substrates and epitaxial nitride thin films, the films are of variable quality In this paper we describe our preliminary studies of nitride thin films using electron backscattered diffraction (EBSD). We show that the EBSD technique may be used to reveal the relative orientation of an epitaxial thin film with respect to its substrate (a 90 degrees rotation between a GaN epitaxial thin film and its sapphire substrate is observed) and to determine its tilt (a GaN thin film was found to be tiltedby 13 +/- 1 degrees towards [1010]GaN), where the tilt is due to the inclination of the sapphire substrate (cut off-axis by 10 degrees from (0001)sapphire towards (1010)sapphire). We compare EBSD patterns obtained from As-doped GaN films grown by plasma-assisted molecular beam epitaxy (PA-MBE) with low and high As4 flux, respectively. Higher As4 flux results in sharper, better defined patterns, this observation is consistent with the improved surface morphology observed in AFM studies. Finally, we show that more detail can be discerned in EBSD patterns from GaN thin films when samples are cooled.