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Understanding the growth mechanisms of III-nitride nanowires is of great importance to realise their full potential. We present a systematic study of silane-assisted GaN nanowire growth on c-sapphire substrates by investigating the surface evolution of the sapphire substrates during the high temperature annealing, nitridation and nucleation steps, and the growth of GaN nanowires. The nucleation step - which transforms the AlN layer formed during the nitridation step to AlGaN - is critical for subsequent silane-assisted GaN nanowire growth. Both Ga-polar and N-polar GaN nanowires were grown with N-polar nanowires growing much faster than the Ga-polar nanowires. On the top surface of the N-polar GaN nanowires protuberance structures were found, which relates to the presence of Ga-polar domains within the nanowires. Detailed morphology studies revealed ring-like features concentric with the protuberance structures, indicating energetically favourable nucleation sites at inversion domain boundaries. Cathodoluminescence studies showed quenching of emission intensity at the protuberance structures, but the impact is limited to the protuberance structure area only and does not extend to the surrounding areas. Hence it should minimally affect the performance of devices whose functions are based on radial heterostructures, suggesting that radial heterostructures remain a promising device structure.

Herein, the use of cathodoluminescence (CL) hyperspectral mapping in the quantification of the AlGaN alloy composition in graded buffer structures is explored. The quantification takes advantage of the known parabolic dependence of the AlGaN bandgap on the alloy composition allowing the AlGaN near‐band‐edge (NBE) emission energy recorded from CL to be converted to a composition. The proposed quantification method is first applied to cleaved cross‐sections of two nominally step‐graded AlGaN buffer structures each containing five AlGaN layers with different compositions. By comparing the compositions obtained from CL to those calculated using X‐ray diffraction, a close agreement between values from both techniques is observed. However, due to a change in the bowing parameter, some deviation is observed for layers with compositions near 75%. The method is then applied to cleaved cross‐sections of an AlGaN buffer whose group III precursor flow molar ratio is varied linearly throughout the growth. Herein, the hyperspectral nature of the CL datasets is exploited such as to produce composition maps by converting the relevant AlGaN‐NBE emission energy at each pixel of the CL data to a composition.

Time-resolved cathodoluminescence offers new possibilities for the study of semiconductor nanostructures - including defects. The versatile combination of time, spatial, and spectral resolution of the technique can provide new insights into the physics of carrier recombination at the nanoscale. Here, we used power-dependent cathodoluminescence and temperature-dependent time-resolved cathodoluminescence to study the carrier dynamics at trench defects in InGaN quantum wells - a defect commonly found in III-nitride structures. The measurements show that the emission properties of trench defects closely relate to the depth of the related basal plane stacking fault within the quantum well stack. The study of the variation of carrier decay time with detection energy across the emission spectrum provides strong evidence supporting the hypothesis that strain relaxation of the quantum wells enclosed within the trench promotes efficient radiative recombination even in the presence of an increased indium content. This result shines light on previously reported peculiar emission properties of the defect, and illustrates the use of cathodoluminescence as a powerful adaptable tool for the study of defects in semiconductors.

Spectral diffusion can lead to considerable broadening of the line width of nitride quantum dots. Here, InGaN quantum dots grown on a nonpolar plane were shown to exhibit a decreased spectral diffusion rate compared to polar nitride dots. A robust intensity correlation method was used to measure the spectral diffusion rate of six quantum dots. A maximum spectral diffusion time of 1170 ± 50 ns was found. An increase of the rate with increasing power was observed. The decreased internal field leads to a lifetime for the nonpolar dots that is shorter than that for polar dots; the important ratio of spectral diffusion time to lifetime is more favorable for nonpolar quantum dots, thereby increasing the chances of generating indistinguishable photons.

Bright and efficient deep-red light-emitting diodes (LEDs) are important for applications in medical therapy and biological imaging due to the high penetration of deep-red photons into human tissues. Metal-halide perovskites have potential to achieve bright and efficient electroluminescence due to their favorable optoelectronic properties. However, efficient and bright perovskite-based deep-red LEDs have not been achieved yet, due to either Auger recombination in low-dimensional perovskites or trap-assisted nonradiative recombination in three-dimensional perovskites. Here, we demonstrate a lateral Cs

The diffuse scattering from basal plane stacking faults (BSF) of (112) GaN layers was observed by laboratory X-ray diffraction (XRD) systems. To observe the diffuse scattering, the (112) GaN samples were oriented in the [20] zone for 10l and 20l series of reflections or in the [50] zone for 21l series. The profiles of the characteristic diffuse intensity streaks (parallel to [0001]) were fitted with a linear combination of area normalised Gauss and Lorentz functions. The area of the Lorentzian contribution correlated with the BSF density measured by cathodoluminescence, electron channeling contrast imaging, and transmission electron microscopy for densities between 103 cm−1 to mid 105 cm−1, and hence allows for the quantification of the BSF density. The diffuse X-ray scattering of different reflections also suggests that the I1 type BSFs dominate in our samples. This makes XRD a strong method to quantify BSF densities over the whole range, with the added advantage of being non-destructive.

2H-Benzotriazol-2-ylethylammonium bromide and iodide and its difluorinated derivatives are synthesized and employed as interlayers for passivation of formamidinium lead triiodide (FAPbI3) solar cells. In combination with PbI2 and PbBr2, these benzotriazole derivatives form two-dimensional (2D) Ruddlesden-Popper perovskites (RPPs) as evidenced by their crystal structures and thin film characteristics. When used to passivate n-i-p FAPbI3 solar cells, the power conversion efficiency improves from 20% to close to 22% by enhancing the open-circuit voltage. Quasi-Fermi level splitting experiments and scanning electron microscopy cathodoluminescence hyperspectral imaging reveal that passivation provides a reduced nonradiative recombi-nation at the interface between the perovskite and hole transport layer. Photoluminescence spectroscopy, angle-resolved grazing-incidence wide-angle X-ray scattering, and depth profiling X-ray photoelectron spectroscopy studies of the 2D/three-dimensional (3D) interface between the benzotriazole RPP and FAPbI3 show that a nonuniform layer of 2D perovskites is enough to passivate defects, enhance charge extraction, and decrease nonradiative recombination. The research has received funding from the Ministry of Education, Culture, and Science (Gravity program 024.001.035) and the Netherlands Organization for Scientific Research via a Spinoza grant. This work of B.T.v.G. is part of the Advanced Research Center for Chemical Building Blocks, ARC CBBC, which is cofounded and cofinanced by the Netherlands Organization for Scientific Research (NWO) and the Netherlands Ministry of Economic Affairs (project 2016.03.Tue). W.T.M.v.G., K.V.H., L.L., and D.V. acknowledge the Research Foundation Flanders (FWO) for the funding of the SBO project PROCEED (S002019N) and the senior FWO research projects G043320N and G0A8723N. A.M. acknowledges the FWO for the funding of his FWO fundamental research PhD grant (1115721N). This study was supported by the Special Research Fund (BOF) of Hasselt University (BOF22PD01). J.F.O. acknowledges funding from the Engineering and Physical Sciences Research Council (EPSRC) Nano Doctoral Training Centre (EP/L015978/1).

Summary The progress of Cu(In,Ga)S2 remains significantly limited mainly due to photovoltage (Voc) losses in the bulk and at the interfaces. Here, via a combination of photoluminescence, cathodoluminescence, electrical measurements, and ab initio modeling, we address the bulk and interface losses to improve ∼1.6-eV-band-gap (Eg) Cu(In,Ga)S2. The optoelectronic quality of the absorber improves upon reducing the [Cu]/[Ga+In] (CGI) ratio, as manifested by the suppression of deep defects, higher quasi-Fermi level splitting (QFLS), improved charge-carrier lifetime, and higher Voc. We identify antisite CuIn/CuGa as a major performance-limiting deep defect by comparing the formation energies of various intrinsic defects. Interface recombination is suppressed using a Zn(O,S) buffer layer in Cu-poor devices, which leads to the activation energy of recombination equal to the Eg. We demonstrate an efficiency of 15.2% with Voc of 902 mV from a H2S-free, Cd-free, and KCN-free process.

The use of pulsed mode scanning electron microscopy cathodoluminescence (CL) for both hyperspectral mapping and time-resolved measurements is found to be useful for the study of hybrid perovskite films, a class of ionic semiconductors that have been shown to be beam sensitive. A range of acquisition parameters is analysed, including beam current and beam mode (either continuous or pulsed operation), and their effect on the CL emission is discussed. Under optimized acquisition conditions, using a pulsed electron beam, the heterogeneity of the emission properties of hybrid perovskite films can be resolved via the acquisition of CL hyperspectral maps. These optimized parameters also enable the acquisition of time-resolved CL of polycrystalline films, showing significantly shorter lived charge carriers dynamics compared to the photoluminescence analogue, hinting at additional electron beam-specimen interactions to be further investigated. This work represents a promising step to investigate hybrid perovskite semiconductors at the nanoscale with CL.

With a view to supporting the development of ultra-violet light-emitting diodes and related devices, the compositional, emission and morphology properties of Si-doped n-type Al x Ga1-x N alloys are extensively compared. This study has been designed to determine how the different Al x Ga1-x N crystal orientations (polar (0001) and semipolar (11–22)) affect group-III composition and Si incorporation. Wavelength dispersive x-ray (WDX) spectroscopy was used to determine the AlN mole fraction (x ≈ 0.57–0.85) and dopant concentration (3 × 1018–1 × 1019 cm−3) in various series of Al x Ga1-x N layers grown on (0001) and (11–22) AlN/sapphire templates by metalorganic chemical vapor deposition. The polar samples exhibit hexagonal surface features with Ga-rich boundaries confirmed by WDX mapping. Surface morphology was examined by atomic force microscopy for samples grown with different disilane flow rates and the semipolar samples were shown to have smoother surfaces than their polar counterparts, with an approximate 15% reduction in roughness. Optical characterization using cathodoluminescence (CL) spectroscopy allowed analysis of near-band edge emission in the range 4.0–5.4 eV as well as various deep impurity transition peaks in the range 2.7–4.8 eV. The combination of spatially-resolved characterization techniques, including CL and WDX, has provided detailed information on how the crystal growth direction affects the alloy and dopant concentrations.

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.

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.

The impact of high energy proton radiation, as would be encountered in highly eccentric and Europa orbits, on ultra-thin GaAs solar cells was studied. The cells were irradiated with 68 MeV protons at fluences of 2 × 1012 cm−2 and 1 × 1013cm−2. Cathodoluminescence and dark I-V were used to evaluate the variation of defect density and J 02 with fluence, respectively. The applicability of cathodoluminescence to the study of radiation damage in photovoltaic devices is discussed.

During the epitaxy of AlGaN on sapphire for deep UV emitters, significant lattice mismatch leads to highly strained heterojunctions and the formation of threading dislocations. Combining cathodoluminescence, electron beam induced current and x-ray microanalysis reveal that dislocations with a screw component permeate through a state-of-the-art UVC LED heterostructure into the active region and perturb their local environment in each layer as growth progresses. In addition to acting as non-radiative recombination centers, these dislocations encourage high point defect densities and three-dimensional growth within their vicinity. We find that these point defects can add parasitic recombination pathways and compensate intentional dopants.

Advances in obtaining untwinned (10[Formula: see text]3)-oriented semi-polar GaN enable a new crystal orientation for the growth of green and red LED structures. We present a scanning electron microscopy study that combines the structural characterization of electron channeling contrast imaging with the optical characterization of cathodoluminescence hyperspectral imaging on a [Formula: see text] GaN layer. An extensive defect analysis revealed that the dominant defects consist of basal plane stacking faults (BSFs), prismatic stacking faults, partial dislocations, and threading dislocations. With a defect density of about an order of magnitude lower than in comparable. The optical properties of the defects have been characterized from 10 to 320 K, showing BSF luminescence at room temperature indicating a reduced density of non-radiative recombination centers in the as-grown samples compared to established semi- and non-polar orientations. Our findings suggest that growth along (10[Formula: see text]3) has the potential for higher radiative efficiency than established semi-polar orientations.

Zincblende GaN has the potential to bridge the “green gap” due to the absence of internal electric fields with respect to wurtzite GaN. However, at present, the quality of zincblende GaN light emitting diodes (LEDs) is not yet sufficient for useful efficient green devices. One of the major challenges is the poor spectral purity of the emitted light. A multimicroscopy approach, combining scanning electron microscopy-cathodoluminescence (SEM-CL), scanning transmission electron microscopy (STEM), and scanning electron diffraction (SED), is applied on a single feature to enable cross correlation between techniques and to investigate the possible causes for the broad optical emission of a zincblende GaN LED structure. This investigation demonstrates that SEM-CL on a site-specific TEM cross section prepared by focused ion beam (FIB) microscope can provide access to nanoscale light emission variations that can be directly related to structural differences seen in STEM. We demonstrate that the general large quantum well (QW) emission peak width relates to quantum well thickness and In content fluctuations. Multiple low-energy QW emission peaks are found to be linked with stacking fault bunches that intersect the QWs. Splitting of the QW emission peak is also found to be caused by the formation of wurtzite-phase inclusions associated with twins formed within the zincblende matrix. Our characterization also illustrates the quantum well structure within such wurtzite inclusions and their impact on the optical emission.

Halide double perovskites have gained significant attention, owing to their composition of low-toxicity elements, stability in air, and recent demonstrations of long charge-carrier lifetimes that can exceed 1 s. In particular, Cs2AgBiBr6 has been the subject of many investigations in photovoltaic devices. However, the efficiencies of solar cells based on this double perovskite are still far from the theoretical efficiency limit of the material. Here, we investigate the role of grain size on the optoelectronic properties of Cs2AgBiBr6 thin films. We show through cathodoluminescence measurements that grain boundaries are the dominant non-radiative recombination sites. We also demonstrate through field-effect transistor and temperature-dependent transient current measurements that grain boundaries act as the main channels for ion transport. Interestingly, we find a positive correlation between carrier mobility and temperature, which resembles the hopping mechanism often seen in organic semiconductors. These findings explain the discrepancy between the long diffusion lengths >1 m found in Cs2AgBiBr6 single crystals versus the limited performance achieved in their thin film counterparts. Our work shows that mitigating the impact of grain boundaries will be critical for these double perovskite thin films to reach the performance achievable based on their intrinsic single-crystal properties.

The application of quaternary In x Al y Ga1−x− y N active regions is a promising path towards high efficiency UVB-light emitting diodes (LEDs). For the utilization of In x Al y Ga1−x−y N, detailed knowledge of the interplay between growth parameters, adatom incorporation, optical and structural properties is crucial. We investigated the influence of the trimethylaluminium (TMAl) and trimethylindium (TMIn) flux on the composition and luminescence properties of In x Al y Ga1−x−y N layers by multi-mode scanning electron microscopy. We found that varying the molar TMIn flow from 0 to 17.3 μmol min−1 led to an InN concentration between 0% and 3.2% and an emission energy between 4.17 and 3.75 eV. The variation of the molar TMAl flow from 3.5 to 35.4 μmol min−1 resulted in a AlN composition between 7.8% and 30.7% with an emission energy variation between 3.6 and 4.1 eV. Cathodoluminescence hyperspectral imaging provided evidence for the formation of nanoscale InN-rich regions. Analyzing the emission properties of these InN-rich regions showed that their emission energy is inhomogeneous and varies by ≈150 meV. We provide evidence that the formation of these InN-rich regions is highly dependent on the AlN and InN composition of the layer and that their formation will strongly affect the performance of In x Al y Ga1−x−y N LEDs.

Consistent studies of the quaternary composition are rare as it is impossible to fully determine the quaternary composition by X-ray diffraction or deduce it from that of ternary alloys. In this paper we determined the quaternary composition by wavelength dispersive X-ray spectroscopy of Inx Aly layers grown by metal organic vapor phase epitaxy. Further insights explaining the peculiarities of Inx Aly Ga1-x-yN growth in a showerhead reactor were gained by simulations of the precursor decomposition, gas phase adduct formation and indium incorporation including desorption. The measurements and simulations agree very well showing that the indium incorporation in a range from 0% to 2% is limited by desorption which is enhanced by the compressive strain to the relaxed Al0.5Ga0.5N buffer layer as well as indium incorporation into AlN particles forming in the gas phase. Utilizing Inx Aly Ga1-x-yN layers containing 2% of indium for multiple quantum wells (MQWs), it was possible to show an almost five times higher photoluminescence intensity of InAlGaN MQWs in comparison to AlGaN MQWs.

Zincblende InGaN/GaN quantum wells offer a potential improvement to the efficiency of green light emission by removing the strong electric fields present in similar structures. However, a high density of stacking faults may have an impact on the recombination in these systems. In this work, scanning transmission electron microscopy and energy-dispersive x-ray measurements demonstrate that one-dimensional nanostructures form due to indium segregation adjacent to stacking faults. In photoluminescence experiments, these structures emit visible light, which is optically polarized up to 86% at 10 K and up to 75% at room temperature. The emission redshifts and broadens as the well width increases from 2 nm to 8 nm. Photoluminescence excitation measurements indicate that carriers are captured by these structures from the rest of the quantum wells and recombine to emit light polarized along the length of these nanostructures.

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.

Three-dimensional core-shell nanostructures could resolve key problems existing in conventional planar deep UV light-emitting diode (LED) technology due to their high structural quality, high-quality nonpolar growth leading to a reduced quantum-confined Stark effect and their ability to improve light extraction. Currently, a major hurdle to their implementation in UV LEDs is the difficulty of growing such nanostructures from Al

While the use of electron probe microanalysis (EPMA) is widespread in the geological and metallurgical sciences, it remains less prevalent in the field of semiconductor research. For these materials, trace element (i.e. dopant) levels typically lie near or beneath the detection limit of wavelength-dispersive Xray (WDX) spectrometers, while alloy compositions of ternary mixtures and multilayer structures can more readily be determined using X-ray diffraction techniques. The electron beam measurements more commonly applied to semiconductors remain transmission electron microscopy (for structural characterization), and scanning electron microscopy (topographic, optical and electrical information). Despite this, there are many aspects of the EPMA that make it an attractive platform for all of thesetypes of semiconductor characterization, particularly when combining compositional information fromWDX with complementary and simultaneously-acquired signals. These advantages include: built-inlight optics; a stable, quantified and high-current beam; and a combined large-area and high-resolutionmapping capability. This allows the measurement of cathodoluminescence (CL), electron beam-inducedcurrent (EBIC) and electron channelling contrast imaging (ECCI) signals alongside WDX, which weapply to the investigation of visible and UV AlxInyGa1-x-yN materials, devices and nanostructures.

As a route to the formation of regular arrays of AlN nanorods, in contrast to other III-V materials, the use of selective area growth via metal organic vapor phase epitaxy (MOVPE) has so far not been successful. Therefore, in this work we report the fabrication of a highly uniform and ordered AlN nanorod scaffold using an alternative hybrid top-down etching and bottom-up regrowth approach. The nanorods are created across a full 2-inch AlN template by combining Displacement Talbot Lithography and lift-off to create a Ni nanodot mask, followed by chlorine-based dry etching. Additional KOH-based wet etching is used to tune the morphology and the diameter of the nanorods. The resulting smooth and straight morphology of the nanorods after the two-step dry-wet etching process is used as a template to recover the AlN facets of the nanorods via MOVPE regrowth. The facet recovery is performed for various growth times to investigate the growth mechanism and the change in morphology of the AlN nanorods. Structural characterization highlights, first, an efficient dislocation filtering resulting from the ~130 nm diameter nanorods achieved after the two-step dry-wet etching process, and second, a dislocation bending induced by the AlN facet regrowth. A strong AlN near band edge emission is observed from the nanorods both before and after regrowth. The achievement of a highly uniform and organized faceted AlN nanorod scaffold having smooth and straight non-polar facets and improved structural and optical quality is a major stepping stone toward the fabrication of deep UV core-shell-based AlN or AlxGa1-xN templates.

Core–shell nanostructures are predicted to highly improve the efficiency of deep-UV light emitting diodes (LEDs), owing to their low defect density, reduced quantum-confined Stark effect, high-quality non-polar growth and improved extraction efficiency. In this paper, we report on the nanofabrication of high-quality AlN nanorod arrays using a hybrid top-down/bottom-up approach for use as a scaffold for UV LED structures. We describe the use of Displacement Talbot Lithography to fabricate a metallic hard etch mask to allow AlN nanorod arrays to be dry etched from a planar AlN template. In particular, we investigate the impact of etching parameters on the nanorod etch rate, tapering profile and mask selectivity in order to achieve vertical-sided nanorod arrays with high aspect ratios. AlN facet recovery is subsequently explored by means of regrowth using Metal Organic Vapor Phase Epitaxy. Low pressure and high V/III ratio promote straight and smooth sidewall faceting, which results in an improvement of the optical quality compared to the initial AlN template. The promising results open new perspectives for the fabrication of high-efficiency deep-UV-emitting core–shell LEDs.

Microcavities based on group-III nitride material offer a notable platform for the investigation of light-matter interactions as well as the development of devices such as high efficiency light emitting diodes (LEDs) and low-threshold nanolasers. Disk or tube geometries in particular are attractive for low-threshold lasing applications due to their ability to support high finesse whispering gallery modes (WGMs) and small modal volumes. In this article we present the fabrication of homogenous and dense arrays of axial InGaN/GaN nanotubes via a combination of displacement Talbot lithography (DTL) for patterning and inductively coupled plasma top-down dry-etching. Optical characterization highlights the homogeneous emission from nanotube structures. Power-dependent continuous excitation reveals a non-uniform light distribution within a single nanotube, with vertical confinement between the bottom and top facets, and radial confinement within the active region. Finite-difference time-domain simulations, taking into account the particular shape of the outer diameter, indicate that the cavity mode of a single nanotube has a mixed WGM-vertical Fabry-Perot mode (FPM) nature. Additional simulations demonstrate that the improvement of the shape symmetry and dimensions primarily influence the Q-factor of the WGMs whereas the position of the active region impacts the coupling efficiency with one or a family of vertical FPMs. These results show that regular arrays of axial InGaN/GaN nanotubes can be achieved via a low-cost, fast and large-scale process based on DTL and top-down etching. These techniques open a new perspective for cost effective fabrication of nano-LED and nano-laser structures along with bio-chemical sensing applications.

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 µm crack-free and fully coalesced AlN was grown on such substrates. Extended defect analysis comparing X-ray 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° 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° 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 %).

In this paper we describe the scanning electron microscopy techniques of electron backscatter diffraction, electron channeling contrast imaging, wavelength dispersive X-ray spectroscopy, and cathodoluminescence hyperspectral imaging. We present our recent results on the use of these non-destructive techniques to obtain information on the topography, crystal misorientation, defect distributions, composition, doping, and light emission from a range of UV-emitting nitride semiconductor structures. We aim to illustrate the developing capability of each of these techniques for understanding the properties of UV-emitting nitride semiconductors, and the benefits were appropriate, in combining the techniques.

Detailed knowledge of the dopant concentration and composition of wide band gap AlxGa1−xN layers is of crucial importance for the fabrication of ultra violet (UV) light emitting diodes (LEDs). This paper demonstrates the capabilities of wavelength dispersive X-ray (WDX) spectroscopy in accurately determining these parameters and compares the results with those from high resolution X-ray diffraction (HR-XRD) and secondary ion mass spectrometry (SIMS). WDX spectroscopy has been carried out on different silicon-doped wide bandgap AlxGa1−xN samples (x between 0.80 and 1). This study found a linear increase in the Si concentration with the SiH4/group-III ratio, measuring Si concentrations between 3×1018 cm−3 and 2.8×1019 cm−3, while no direct correlation between the AlN composition and the Si incorporation ratio was found. Comparison between the composition obtained by WDX and by HR-XRD showed very good agreement in the range investigated, while comparison of the donor concentration between WDX and SIMS found only partial agreement, which we attribute to a number of effects.

With advances in nanolithography and dry etching, top-down methods of nanostructuring have become a widely used tool for improving the efficiency of optoelectronics. These nano dimensions can offer various benefits to the device performance in terms of light extraction and efficiency, but often at the expense of emission color quality. Broadening of the target emission peak and unwanted yellow luminescence are characteristic defect-related effects due to the ion beam etching damage, particularly for III–N based materials. In this article we focus on GaN based nanorods, showing that through thermal annealing the surface roughness and deformities of the crystal structure can be “self-healed”. Correlative electron microscopy and atomic force microscopy show the change from spherical nanorods to faceted hexagonal structures, revealing the temperature-dependent surface morphology faceting evolution. The faceted nanorods were shown to be strain- and defect-free by cathodoluminescence hyperspectral imaging, micro-Raman, and transmission electron microscopy (TEM). In-situ TEM thermal annealing experiments allowed for real time observation of dislocation movements and surface restructuring observed in ex-situ annealing TEM sampling. This thermal annealing investigation gives new insight into the redistribution path of GaN material and dislocation movement post growth, allowing for improved understanding and in turn advances in optoelectronic device processing of compound semiconductors.

Correction for 'Site controlled red-yellow-green light emitting InGaN quantum discs on nano-tipped GaN rods' by M. Conroy et al., Nanoscale, 2016, 8 , 11019-11026.

We report a method of growing site controlled InGaN multiple quantum discs (QDs) at uniform wafer scale on coalescence free ultra-high density (>80%) nanorod templates by metal organic chemical vapour deposition (MOCVD). The dislocation and coalescence free nature of the GaN space filling nanorod arrays eliminates the well-known emission problems seen in InGaN based visible light sources that these types of crystallographic defects cause. Correlative scanning transmission electron microscopy (STEM), energy-dispersive X-ray (EDX) mapping and cathodoluminescence (CL) hyperspectral imaging illustrates the controlled site selection of the red, yellow and green (RYG) emission at these nano tips. This article reveals that the nanorod tips’ broad emission in the RYG visible range is in fact achieved by manipulating the InGaN QD's confinement dimensions, rather than significantly increasing the In%. This article details the easily controlled method of manipulating the QDs dimensions producing high crystal quality InGaN without complicated growth conditions needed for strain relaxation and alloy compositional changes seen for bulk planar GaN templates.

A series of Si-doped AlN-rich AlGaN layers with low resistivities was characterized by a combination of nanoscale imaging techniques. Utilizing the capability of scanning electron microscopy to reliably investigate the same sample area with different techniques, it was possible to determine the effect of doping concentration, defect distribution, and morphology on the luminescence properties of these layers. Cathodoluminescence shows that the dominant defect luminescence depends on the Si-doping concentration. For lower doped samples, the most intense peak was centered between 3.36 eV and 3.39 eV, while an additional, stronger peak appears at 3 eV for the highest doped sample. These peaks were attributed to the (VIII-ON)2− complex and the VIII3− vacancy, respectively. Multimode imaging using cathodoluminescence, secondary electrons, electron channeling contrast, and atomic force microscopy demonstrates that the luminescence intensity of these peaks is not homogeneously distributed but shows a strong dependence on the topography and on the distribution of screw dislocations.

The influence of substrate miscut on Al0.5Ga0.5N layers was investigated using cathodoluminescence (CL) hyperspectral imaging and secondary electron imaging in an environmental scanning electron microscope. The samples were also characterized using atomic force microscopy and high resolution X-ray diffraction. It was found that small changes in substrate miscut have a strong influence on the morphology and luminescence properties of the AlGaN layers. Two different types are resolved. For low miscut angle, a crack-free morphology consisting of randomly sized domains is observed, between which there are notable shifts in the AlGaN near band edge emission energy. For high miscut angle, a morphology with step bunches and compositional inhomogeneities along the step bunches, evidenced by an additional CL peak along the step bunches, are observed. (C) 2014 Author(s).

Cathodoluminescence (CL) hyperspectral imaging—the acquisition of a full optical emission spectrum at each pixel of an image—has become firmly established as a measurement mode in scanning electron microscopy (SEM) [1]. CL is sensitive to the structural, compositional and electrical properties of a sample, and the inherent multimode nature of SEM makes it possible to combine CL with other techniques which are also sensitive to one or more of these properties. For example, combining CL hyperspectral imaging with simultaneous X-ray microanalysis has been used to probe composition variations within semiconductors [2] and minerals [3]. In this work we present recent results combining CL hyperspectral imaging with other SEM modes, and also demonstrate the benefits of introducing additional measurement parameters, such as sample applied bias and microscope chamber pressure. Structural defects are central in determining the performance of electrical and optical devices based on III-nitride semiconductors. To better understand the effect of threading dislocations on carrier recombination in such materials, we have carried out CL imaging together with electron channeling contrast imaging (ECCI), which is sensitive to the lattice distortions associated with such defects. Using this combination of techniques we have shown that both pure edge dislocations and mixed (combination of edge + screw) dislocations act as nonradiative recombination centers in GaN epilayers [4]. Since CL provides information only about radiative recombination, it needs to be coupled with other techniques to provide a fuller picture of the different carrier loss mechanisms which limit device performance, an objective we achieved by measuring CL together with electron beam induced current (EBIC). This signal originates within the junction of an electrically contacted device (measured via an external circuit) and is dependent on the total (i.e. radiative + nonradiative) recombination. By carrying out both techniques simultaneously on InxGa1-xN/GaN light-emitting diodes (LEDs), we have separated out nonradiative recombination from other loss mechanisms, such as light extraction or electrical contacting issues [5]. These CL/EBIC measurements on contacted LEDs have opened up the possibility of introducing an additional variable into CL imaging: applied bias voltage. Figure 1 shows an example of such measurements for an InGaN/GaN LED device. This capability allows the emission to be imaged under conditions closer to those of a device in normal operation. It also allows us—by imaging at several bias values—to differentiate between the drift and diffusion components of the current, and to probe the influence of the quantum-confined Stark effect in the active region of the LED. Furthermore, comparison with electroluminescence (EL) hyperspectral images yields additional information: for example, in some areas of the LED we see correlations between contrast features in EL and EBIC images which are not present in the CL, implying that they originate in the diode junction or contacts rather than in the active layer itself [5]. Finally, we have demonstrated CL hyperspectral imaging in an environmental SEM operating with a variable pressure of water vapor. This has allowed us to measure for the first time such insulating

Light-emitting diodes based on halide perovskites have recently reached external quantum efficiencies of over 20%. However, the performance of visible perovskite light-emitting diodes has been hindered by non-radiative recombination losses and limited options for charge-transport materials that are compatible with perovskite deposition. Here, we report efficient, green electroluminescence from mixed-dimensional perovskites deposited on a thin (~1 nm) lithium fluoride layer on an organic semiconductor hole-transport layer. The highly polar dielectric interface acts as an effective template for forming high-quality bromide perovskites on otherwise incompatible hydrophobic charge-transport layers. The control of crystallinity and dimensionality of the perovskite layer is achieved by using tetraphenylphosphonium chloride as an additive, leading to external photoluminescence quantum efficiencies of around 65%. With this approach, we obtain light-emitting diodes with external quantum efficiencies of up to 19.1% at high brightness (>1,500 cd m−2). Green perovskite light-emitting diodes with external quantum efficiencies of up to 19.1% at high brightness can be created by depositing an ultrathin layer of strongly polar lithium fluoride between the perovskite and hole-transport layers.