Imaging Threading Dislocations and Surface Steps in Nitride Thin Films Using Electron Backscatter Diffraction.

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.

Core-Shell Nanorods as Ultraviolet Light-Emitting Diodes.

Existing barriers to efficient deep ultraviolet (UV) light-emitting diodes (LEDs) may be reduced or overcome by moving away from conventional planar growth and toward three-dimensional nanostructuring. Nanorods have the potential for enhanced doping, reduced dislocation densities, improved light extraction efficiency, and quantum wells free from the quantum-confined Stark effect. Here, we demonstrate a hybrid top-down/bottom-up approach to creating highly uniform AlGaN core-shell nanorods on sapphire repeatable on wafer scales. Our GaN-free design avoids self-absorption of the quantum well emission while preserving electrical functionality. The effective junctions formed by doping of both the n-type cores and p-type caps were studied using nanoprobing experiments, where we find low turn-on voltages, strongly rectifying behaviors and significant electron-beam-induced currents. Time-resolved cathodoluminescence measurements find short carrier liftetimes consistent with reduced polarization fields. Our results show nanostructuring to be a promising route to deep-UV-emitting LEDs, achievable using commercially compatible methods.

Employing Cathodoluminescence for Nanothermometry and Thermal Transport Measurements in Semiconductor Nanowires.

Thermal properties have an outsized impact on efficiency and sensitivity of devices with nanoscale structures, such as in integrated electronic circuits. A number of thermal conductivity measurements for semiconductor nanostructures exist, but are hindered by the diffraction limit of light, the need for transducer layers, the slow scan rate of probes, ultrathin sample requirements, or extensive fabrication. Here, we overcome these limitations by extracting nanoscale temperature maps from measurements of bandgap cathodoluminescence in GaN nanowires of <300 nm diameter with spatial resolution limited by the electron cascade. We use this thermometry method in three ways to determine the thermal conductivities of the nanowires in the range of 19-68 W/m·K, well below that of bulk GaN. The electron beam acts simultaneously as a temperature probe and as a controlled delta-function-like heat source to measure thermal conductivities using steady-state methods, and we introduce a frequency-domain method using pulsed electron beam excitation. The different thermal conductivity measurements we explore agree within error in uniformly doped wires. We show feasible methods for rapid, in situ, high-resolution thermal property measurements of integrated circuits and semiconductor nanodevices and enable electron-beam-based nanoscale phonon transport studies.

Influence of the reactor environment on the selective area thermal etching of GaN nanohole arrays.

Selective area thermal etching (SATE) of gallium nitride is a simple subtractive process for creating novel device architectures and improving the structural and optical quality of III-nitride-based devices. In contrast to plasma etching, it allows, for example, the creation of enclosed features with extremely high aspect ratios without introducing ion-related etch damage. We report how SATE can create uniform and organized GaN nanohole arrays from c-plane and (11-22) semi-polar GaN in a conventional MOVPE reactor. The morphology, etching anisotropy and etch depth of the nanoholes were investigated by scanning electron microscopy for a broad range of etching parameters, including the temperature, the pressure, the NH3 flow rate and the carrier gas mixture. The supply of NH3 during SATE plays a crucial role in obtaining a highly anisotropic thermal etching process with the formation of hexagonal non-polar-faceted nanoholes. Changing other parameters affects the formation, or not, of non-polar sidewalls, the uniformity of the nanohole diameter, and the etch rate, which reaches 6 µm per hour. Finally, the paper discusses the SATE mechanism within a MOVPE environment, which can be applied to other mask configurations, such as dots, rings or lines, along with other crystallographic orientations.

Impact of Inductively Coupled Plasma Etching Conditions on the Formation of Semi-Polar ( 11 2 ¯ 2 ) and Non-Polar ( 11 2 ¯ 0 ) GaN Nanorods.

The formation of gallium nitride (GaN) semi-polar and non-polar nanostructures is of importance for improving light extraction/absorption of optoelectronic devices, creating optical resonant cavities or reducing the defect density. However, very limited studies of nanotexturing via dry etching have been performed, in comparison to wet etching. In this paper, we investigate the formation and morphology of semi-polar (112¯2) and non-polar (112¯0) GaN nanorods using inductively coupled plasma (ICP) etching. The impact of gas chemistry, pressure, temperature, radio-frequency (RF) and ICP power and time are explored. A dominant chemical component is found to have a significant impact on the morphology, being impacted by the polarity of the planes. In contrast, increasing the physical component enables the impact of crystal orientation to be minimized to achieve a circular nanorod profile with inclined sidewalls. These conditions were obtained for a small percentage of chlorine (Cl2) within the Cl2 + argon (Ar) plasma combined with a low pressure. Damage to the crystal was reduced by lowering the direct current (DC) bias through a reduction of the RF power and an increase of the ICP power.

Displacement Talbot lithography for nano-engineering of III-nitride materials.

Nano-engineering III-nitride semiconductors offers a route to further control the optoelectronic properties, enabling novel functionalities and applications. Although a variety of lithography techniques are currently employed to nano-engineer these materials, the scalability and cost of the fabrication process can be an obstacle for large-scale manufacturing. In this paper, we report on the use of a fast, robust and flexible emerging patterning technique called Displacement Talbot lithography (DTL), to successfully nano-engineer III-nitride materials. DTL, along with its novel and unique combination with a lateral planar displacement (D2TL), allow the fabrication of a variety of periodic nanopatterns with a broad range of filling factors such as nanoholes, nanodots, nanorings and nanolines; all these features being achievable from one single mask. To illustrate the enormous possibilities opened by DTL/D2TL, dielectric and metal masks with a number of nanopatterns have been generated, allowing for the selective area growth of InGaN/GaN core-shell nanorods, the top-down plasma etching of III-nitride nanostructures, the top-down sublimation of GaN nanostructures, the hybrid top-down/bottom-up growth of AlN nanorods and GaN nanotubes, and the fabrication of nanopatterned sapphire substrates for AlN growth. Compared with their planar counterparts, these 3D nanostructures enable the reduction or filtering of structural defects and/or the enhancement of the light extraction, therefore improving the efficiency of the final device. These results, achieved on a wafer scale via DTL and upscalable to larger surfaces, have the potential to unlock the manufacturing of nano-engineered III-nitride materials.

"Double" displacement Talbot lithography: fast, wafer-scale, direct-writing of complex periodic nanopatterns.

We describe a new low-cost nanolithographic tool for creating periodic arrays of complex, nano-motifs, across large areas within minutes. Displacement Talbot lithography is combined with lateral nanopositioning to enable large-area patterning with the flexibility of a direct-write system. In this way, we can create different periodic patterns in short timescales using a single mask with no mask degradation. We demonstrate multiple exposures, combined with discrete lateral displacements, and single exposures, with continuous displacements, to achieve image inversion, pitch reduction, and nanogaps between metal nanoparticles. Our approach provides a flexible route to create large-area nanopatterned materials and devices in high volumes.

Deep UV Emission from Highly Ordered AlGaN/AlN Core-Shell Nanorods.

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 xGa1- xN materials with a bottom-up approach. In this paper, we report the successful fabrication of an AlN/Al xGa1- xN/AlN core-shell structure using an original hybrid top-down/bottom-up approach, thus representing a breakthrough in applying core-shell architecture to deep UV emission. Various AlN/Al xGa1- xN/AlN core-shell structures were grown on optimized AlN nanorod arrays. These were created using displacement Talbot lithography (DTL), a two-step dry-wet etching process, and optimized AlN metal organic vapor phase epitaxy regrowth conditions to achieve the facet recovery of straight and smooth AlN nonpolar facets, a necessary requirement for subsequent growth. Cathodoluminescence hyperspectral imaging of the emission characteristics revealed that 229 nm deep UV emission was achieved from the highly uniform array of core-shell AlN/Al xGa1- xN/AlN structures, which represents the shortest wavelength achieved so far with a core-shell architecture. This hybrid top-down/bottom-up approach represents a major advance for the fabrication of deep UV LEDs based on core-shell nanostructures.

Hybrid Top-Down/Bottom-Up Fabrication of a Highly Uniform and Organized Faceted AlN Nanorod Scaffold.

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.