Extended defects, like threading dislocations, are detrimental to the performance of optoelectronic devices. In the scanning electron microscope, dislocations are traditionally imaged using diodes to monitor changes in backscattered electron intensity as the electron beam is scanned over the sample, with the sample positioned so the electron beam is at, or close to the Bragg angle for a crystal plane/planes. Here, we use a pixelated detector instead of single diodes, specifically an electron backscatter diffraction (EBSD) detector. We present postprocessing techniques to extract images of dislocations and surface steps, for a nitride thin film, from measurements of backscattered electron intensities and intensity distributions in unprocessed EBSD patterns. In virtual diode (VD) imaging, the backscattered electron intensity is monitored for a selected segment of the unprocessed EBSD patterns. In center of mass (COM) imaging, the position of the center of the backscattered electron intensity distribution is monitored. Additionally, both methods can be combined (VDCOM). Using both VD and VDCOM, images of only threading dislocations, or dislocations and surface steps can be produced, with VDCOM images exhibiting better signal-to-noise. The applicability of VDCOM imaging is demonstrated across a range of nitride semiconductor thin films, with varying surface step and dislocation densities.

The structural recovery of AlN grown by reactive sputtering on a sapphire substrate during high-temperature annealing is studied by means of transmission electron microscopy and secondary ion mass spectrometry. The as-grown film shows high-density planar defects, such as basal and prismatic stacking faults, caused by the limited diffusion length of the adatoms and, thus, presents a columnar structure. The presence of high-density nanopipes is associated with the presence of unintentional oxygen impurities. Based on the atomic resolution transmission electron microscopy analysis, we show that basal and prismatic stacking faults vanish in the films via a climb mechanism and describe this process as the nucleation of jogs promoted by the diffusion of vacancies. The nanopipes present in the as-grown film transform into faceted voids and act as a beneficial source of excess vacancies that promote dislocation annihilation by climb. The transformation of nanopipes to faceted voids resembles the transition from open channel pores to close faceted pores, which has been observed in porous silicon and can be described in terms of a classical sintering theory.

AlGaN-based UVC light-emitting diodes (LED) were fabricated on high-quality AlN templates with an engineerable in-plane lattice constant. The controllability of the in-plane strain originated from the vacancy formation in Si-doped AlN (AlN:Si) and their interaction with edge dislocations. The strain state of the Si:AlN top interface could be well depicted by a dislocation-tilt model depending on the buffer strain state, threading dislocation density (TDD), and regrown Si:AlN thickness. The validity of the model was verified by cross-sectional TEM analysis. With a gradually widened lattice constant of regrown Si:AlN layer, strain-induced defects of subsequently grown n-AlGaN was suppressed. Therefore, growing a current spreading layer which possesses a moderate Al content (<65%), decent thickness (>1.5 µm), and a low TDD (<1.0 × 109 cm−2) simultaneously becomes possible. Additionally, the idea of an optimal edge TDD (ρe,opt) in the AlN buffer was revealed for growing high-quality n-AlGaN layers with a targeted thickness. After a deliberate strain-TDD engineering for Si:AlN and n-AlGaN, high-power UVC LEDs (λ = 275 nm, P > 200 mW) with a low forward voltage (Vf = 5.7 volt) were demonstrated at I = 1.35 A. The low forward voltage under high current injection density was attributed to the success in preparation of a low series resistance and high-quality n-AlGaN current spreading layer.

Growth of Si-doped AlN and of Al0.63Ga0.37N on high quality AlN templates grown by HVPE has been investi-gated. The strain state of Si-doped AlN is thickness-dependent due to the surface-mediated dislocation tilt which induces a tensile strain component. At very low dislocation density in the AlN buffer strain relaxation in micrometer-thick Al0.63Ga0.37N layers is dominated by generation of additional dislocations. As a result, the final threading dislocation density and the surface roughness increase significantly. For a 1.6 mu m Al0.63Ga0.37N on 3.4 mu m Si-doped AlN bi-layer structure, the optimal threading dislocation density (TDD) of the AlN:Si buffer is estimated to be 7 x 108 cm- 2, where the low TDD can be still transferred from the buffer to the thick AlGaN heterostructure without generation of many new dislocations.

In this work, we compare the defect structure in unintentionally doped and Si-doped AlN layers grown by metalorganic vapor phase epitaxy (MOVPE) on high-temperature annealed (HTA) sputtered AlN templates on sapphire substrates. Since the HTA process leads to a reduction of the in-plane lattice constant of the AlN layers, further homoepitaxial overgrowth results in compressively strained AlN layers. With increasing MOVPE-AlN layer thickness, strain relaxation takes place mostly by formation of dislocation half-loops of an irregular shape, which accumulate at the homoepitaxial MOVPE-AlN/HTA-AlN interface. We suggest that these dislocations nucleate at the layer surface and move down to the homoepitaxial interface at high temperatures. The formation of these irregular and hardly controllable defects can be avoided by introduction of Si-doping into the MOVPE-AlN layers. Si-doping enlarges the inclination of threading dislocation lines stemming from the HTA-AlN template, producing an alternative mechanism for strain relaxation.

Driven by a wide range of applications, as shown in Fig. 1(a) , the development of AlGaN-based light emitting diodes in the deep ultraviolet spectral range (DUV-LEDs) has greatly intensified. In contrast to conventional ultraviolet sources UV-LEDs exhibit small form factors, operate at moderate dc voltages, show long lifetimes, and their emission covers the entire UVB and large parts of the UVC wavelength range. Currently, the main driving force are high volume applications like water purification, disinfection of surfaces and appliances, inactivation of germs in air treatment systems as well as sterilization of medical equipment with a focus on UVC-LEDs emitting near the germicidal effectiveness peak around 270 nm [1] . This presentation will provide an overview of state-of-the art in DUV-LED device technologies and present recent advances in the development of high quality AlGaN materials by metalorganic vapour phase epitaxy (MOVPE). We will discuss different approaches to improve the internal quantum efficiency of UV light emitters, including the growth of low defect density AlN layers on sapphire substrates by epitaxial lateral overgrowth (ELO) as well as sputtered and high temperature annealed AlN on sapphire [2] . We will demonstrate AlGaN quantum well (QW) LEDs with output powers of more than 50 mW for single-chip emitters near 265 nm and explore the wavelength limits of deep UV-LEDs with emission as short as 217 nm. These far UV-LEDs are ideally suited for sensing applications like the monitoring of combustion engines, toxic gases, nitrates in water, and may also be utilized for the in-vivo inactivation of multi-drug-resistant germs or viruses without damaging the human skin. Although a strong decline can be observed in the external quantum efficiency (EQE) of UV-LEDs emitting below 250 nm, as shown in Fig 1(b) , considerable advances have been made in the development of 233 nm LEDs with output powers of nearly 1.9 mW at 100 mA corresponding to an EQE of 0.35% [4] . We will discuss the root causes for the EQE decline, including changes in the optical polarization of light emission from deep UV AlGaN QWs and their effects on light extraction as well as changes in internal quantum efficiency and carrier confinement. We will provide an outlook of future progress in DUV-LED performance and demonstrate first applications including a spectrally pure 233 nm irradiation system for the in-vivo inactivation of germs.

Using the example of epitaxial lateral overgrowth of AlN on trench‐patterned AlN/sapphire templates, the impact of introducing a high‐temperature annealing step into the process chain is investigated. Covering the open surfaces of sapphire trench sidewalls with a thin layer of AlN is found to be necessary to preserve the trench shape during annealing. Both the influence of annealing temperature and annealing duration are investigated. To avoid the deformation of the AlN/sapphire interface during annealing, the annealing duration or annealing temperature must be low enough. Annealing for 1 h at 1730 °C is found to allow for the lowest threading dislocation density of 3.5 × 108 cm−2 in the subsequently grown AlN, while maintaining an uncracked smooth surface over the entire 2 in. wafer. Transmission electron microscopy study confirms the defect reduction by high‐temperature annealing and reveals an additional strain relaxation mechanism by accumulation of horizontal dislocation lines at the interface between annealed and nonannealed AlN. By applying a second annealing step, the dislocation density can be further reduced to 2.5 × 108 cm−2.

Recovery of epitaxial AlN films on sapphire at high temperatures is now an established process to produce pseudo-substrates with high crystalline perfection, which can be used to grow epitaxial structures for UV-light-emitting devices. To elucidate the elementary mechanisms taking place during the thermal treatment of MOVPE-grown films, we studied as-grown and annealed samples combining transmission electron microscopy techniques and secondary ion mass spectrometry (SIMS). By using SIMS, we find a temperature-dependent increase in the overall oxygen content of the films, which cannot be explained quantitatively with either simple bulk or pure pipe-diffusion from the sapphire substrate. Instead, we propose a lateral outdiffusion from the dislocation cores to explain qualitatively and quantitatively the presence of observed oxygen concentration plateaus. Based on the formation enthalpy of various atomic defects and complexes found in literature, we conclude that the di-oxygen/aluminum vacancy complex (VAl–2ON) is the dominant point defect controlling the annealing process. The formation of this defect at high temperatures promotes a dislocation core climb process, which causes the annihilation/fusion of the threading dislocation segments.

The scanning electron microscopy techniques of electron backscatter diffraction (EBSD), electron channelling contrast imaging (ECCI) and cathodoluminescence (CL) hyperspectral imaging provide complementary information on the structural and luminescence properties of materials rapidly and non-destructively, with a spatial resolution of tens of nanometres. EBSD provides crystal orientation, crystal phase and strain analysis, whilst ECCI is used to determine the planar distribution of extended defects over a large area of a given sample. CL reveals the influence of crystal structure, composition and strain on intrinsic luminescence and/or reveals defect-related luminescence. Dark features are also observed in CL images where carrier recombination at defects is non-radiative. The combination of these techniques is a powerful approach to clarifying the role of crystallography and extended defects on a material’s light emission properties. Here we describe the EBSD, ECCI and CL techniques and illustrate their use for investigating the structural and light emitting properties of UV-emitting nitride semiconductor structures. We discuss our investigations of the type, density and distribution of defects in GaN, AlN and AlGaN thin films and also discuss the determination of the polarity of GaN nanowires.

We report on the performance of AlGaN-based deep ultraviolet light-emitting diodes (UV-LEDs) emitting at 265 nm grown on stripe-patterned high-temperature annealed (HTA) epitaxially laterally overgrown (ELO) aluminium nitride (AlN)/sapphire templates. For this purpose, the structural and electro-optical properties of ultraviolet-c light-emitting diodes (UVC-LEDs) on as-grown and on HTA planar AlN/sapphire as well as ELO AlN/sapphire with and without HTA are investigated and compared. Cathodoluminescence measurements reveal dark spot densities of 3.5 × 10 9 cm − 2 , 1.1 × 10 9 cm − 2 , 1.4 × 10 9 cm − 2 , and 0.9 × 10 9 cm − 2 in multiple quantum well samples on as-grown planar AlN/sapphire, HTA planar AlN/sapphire, ELO AlN/sapphire, and HTA ELO AlN/sapphire, respectively, and are consistent with the threading dislocation densities determined by transmission electron microscopy (TEM) and high-resolution X-ray diffraction rocking curve. The UVC-LED performance improves with the reduction of the threading dislocation densities (TDDs). The output powers (measured on-wafer in cw operation at 20 mA) of the UV-LEDs emitting at 265 nm were 0.03 mW (planar AlN/sapphire), 0.8 mW (planar HTA AlN/sapphire), 0.9 mW (ELO AlN/sapphire), and 1.1 mW (HTA ELO AlN/sapphire), respectively. Furthermore, Monte Carlo ray-tracing simulations showed a 15% increase in light-extraction efficiency due to the voids formed in the ELO process. These results demonstrate that HTA ELO AlN/sapphire templates provide a viable approach to increase the efficiency of UV-LEDs, improving both the internal quantum efficiency and the light-extraction efficiency.

Herein, AlN growth by metalorganic vapor‐phase epitaxy on hole‐type nanopatterned sapphire substrates is investigated. Cracking occurs for an unexpectedly thin‐layer thickness, which is associated to altered nucleation conditions caused by the sapphire pattern. To overcome the obstacle of cracking and at the same time to decrease the threading dislocation density by an order of magnitude, high‐temperature annealing (HTA) of a 300 nm‐thick AlN starting layer is successfully introduced. By this method, 800 nm‐thick, fully coalesced and crack‐free AlN is grown on 2 in. nanopatterned sapphire wafers. The usability of such templates as basis for UVC light‐emitting diodes (LEDs) is furthermore proved by subsequent growth of an UVC‐LED heterostructure with single peak emission at 265 nm. Prerequisites for the enhancement of the light extraction efficiency by hole‐type nanopatterned sapphire substrates are discussed.

The influence of compressive strain in high-quality AlN templates on the subsequent growth of AlGaN-based device layers was investigated. The AlN templates showed compressive strain of similar to-0.29% and threading dislocation densities (TDDs) below 6.5 x 10(8) cm(-2). By introducing high Si-doping in MOVPE-grown AlN, the compressive strain was relaxed while preserving the low TDD. By this method, the low TDD was transferred from the AlN template to the micron-thick n-Al0.63Ga0.37N. A 275 nm LED was demonstrated with a similar to 2.5 times power enhancement than the same LED on conventional MOVPE-grown AlN template under low current injection. The maximum external quantum efficiency (EQE) was enhanced from 1.6% to 2.2% with an improved n-AlGaN.

In the past few years, high‐temperature annealing of AlN has become a proven method for providing AlN layers with low dislocation densities. Herein, the example of Al0.77Ga0.23N is used to investigate whether annealing can also improve the material quality of the ternary alloy. A detailed analysis of the influence of annealing temperature on structural and optical material properties is presented. It is found that with increasing annealing temperature, the threading dislocation density can be lowered from an initial value of 6.0 × 109 down to 2.6 × 109 cm−2. Ga depletion at the AlGaN surface and Ga diffusion into the AlN buffer layer are observed. After annealing, the defect luminescence between 3 and 4 eV is increased, accompanied by an increase in the oxygen concentration by about two orders of magnitude. Furthermore, due to annealing optical absorption at 325 nm (3.8 eV) occurs, which increases with increasing annealing temperature. It is assumed that the reason for this decrease in ultraviolet (UV) transmittance is the increasing number of vacancies caused by the removal of group‐III and N atoms from the AlGaN lattice during annealing.

In this article we describe the scanning electron microscopy (SEM) techniques of electron channelling contrast imaging and electron backscatter diffraction. These techniques provide information on crystal structure, crystal misorientation, grain boundaries, strain and structural defects on length scales from tens of nanometres to tens of micrometres. Here we report on the imaging and analysis of dislocations and sub-grains in nitride semiconductor thin films (GaN and AlN) and tungsten carbide-cobalt (WC-Co) hard metals. Our aim is to illustrate the capability of these techniques for investigating structural defects in the SEM and the benefits of combining these diffraction-based imaging techniques.

The impact of different AlN/sapphire template technologies [i.e., planar, epitaxial lateral overgrown (ELO), and high temperature annealed sputtered ELO] is studied with respect to the operation-induced degradation of 265 nm UVC LEDs. UVC LEDs with identical heterostructures were grown on templates providing different threading dislocation densities in the range of 0.8 × 109 cm−2 to 5.8 × 109 cm−2. A long-term stress experiment was performed on batches of LEDs, which were operated at a direct current of 200 mA corresponding to a current density of 60 A/cm2 and at a heat sink temperature of 20 °C. The UVC LEDs on templates with lower threading dislocation densities were found to provide a higher optical power and to degrade slower during 2000 h of operation. The experiment demonstrates an extrapolated L70 lifetime of more than 10 000 h for the high temperature annealed sputtered ELO technology. The results suggest that degradation is caused by operation-induced activation of defects whose density scales with the dislocation density.

Light emitting diodes (LEDs) in the deep ultra-violet (DUV) offer new perspectives for multiple applications ranging from 3D printing to sterilization. However, insufficient light extraction severely limits their efficiency. Nanostructured sapphire substrates in aluminum nitride based LED devices have recently shown to improve crystal growth properties, while their impact on light extraction has not been fully verified. We present a model for understanding the impact of nanostructures on the light extraction capability of DUV-LEDs. The model assumes an isotropic light source in the semiconductor layer stack and combines rigorously computed scattering matrices with a multilayer solver. We find that the optical benefit of using a nanopatterned as opposed to a planar sapphire substrate to be negligible, if parasitic absorption in the p-side of the LED is dominant. If losses in the p-side are reduced to 20%, then for a wavelength of 265 nm an increase of light extraction efficiency from 7.8% to 25.0% is possible due to nanostructuring. We introduce a concept using a diffuse ('Lambertian') reflector as p-contact, further increasing the light extraction efficiency to 34.2%. The results underline that transparent p-sides and reflective p-contacts in DUV-LEDs are indispensable for enhanced light extraction regardless of the interface texture between semiconductor and sapphire substrate. The optical design guidelines presented in this study will accelerate the development of high-efficiency DUV-LEDs. The model can be extended to other multilayer opto-electronic nanostructured devices such as photovoltaics or photodetectors.

Herein, the scope is to provide an overview on the current status of AlN/sapphire templates for ultraviolet B (UVB) and ultraviolet C (UVC) light‐emitting diodes (LEDs) with focus on the work done previously. Furthermore, approaches to improve the properties of such AlN/sapphire templates by the combination of high‐temperature annealing (HTA) and patterned AlN/sapphire interfaces are discussed. While the beneficial effect of HTA is demonstrated for UVC LEDs, the growth of relaxed AlGaN buffer layers on HTA AlN is a challenge. To achieve relaxed AlGaN with a low dislocation density, the applicability of HTA for AlGaN is investigated.

Strain relaxation mechanisms in AlGaN based light emitting diodes emitting in the ultraviolet B spectral range (UVB‐LEDs) grown on different AlN/sapphire templates are analyzed by combining in situ reflectivity and curvature data with transmission electron microscopy. In particular, the impact of dislocation density, surface morphology, and lattice constant of the AlN/sapphire templates is studied. For nonannealed AlN/templates with threading dislocation densities (TDDs) of 4 × 109 and 3 × 109 cm−2 and different surface morphologies strain relaxation takes place mostly by conventional ways, such as inclination of threading dislocation lines and formation of horizontal dislocation bands. In contrast, a TDD reduction down to 1 × 109 cm−2 as well as a reduction of the lattice constant of high temperature annealed AlN template leads to drastic changes in the structure of subsequently grown AlGaN layers, e.g., to transformation to helical dislocations and enhanced surface enlargement by formation of macrofacets. For the growth of strongly compressively strained AlGaN layers for UVB‐LEDs the relaxation mechanism is strongly influenced by the absolute values of TDD and the lattice constant of the AlN templates and is less influenced by their surface morphology.

We present overgrowth of nano-patterned sapphire with different offcut angles by metalorganic vapor phase epitaxy. Hexagonal arrays of nano-pillars were prepared via Displacement Talbot Lithography and dry-etching. 6.6 mu m crack-free and fully coalesced AlN was grown on such substrates. Extended defect analysis comparing Xray diffraction, electron channeling contrast imaging and selective defect etching revealed a threading dislocation density of about 109 cm(-2). However, for c-plane sapphire offcut of 0.2 degrees towards m direction the AlN surface shows step bunches with a height of 10 nm. The detrimental impact of these step bunches on subsequently grown AlGaN multi-quantum-wells is investigated by cathodoluminescence and transmission electron microscopy. By reducing the sapphire offcut to 0.1 degrees the formation of step bunches is successfully suppressed. On top of such a sample an AlGaN-based UVC LED heterostructure is realized emitting at 265 nm and showing an emission power of 0.81 mW at 20 mA (corresponds to an external quantum efficiency of 0.86%).