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White beam synchrotron radiation X-ray topography (SR-XRT) and X-ray diffraction (XRD) measurements were used to non-destructively study the defect structure of a bulk GaN wafer, grown by the ammonothermal method. SR-XRT topographs revealed high crystal quality with threading dislocation density 8.8×10 4 cm −2 and granular structure consisting of large, slightly misaligned grains. The threading dislocations within grains were identified as mixed and screw type, while no pure threading edge dislocations were observed. [ABSTRACT FROM AUTHOR]

• Aluminum nitride thin films deposited on vertical Si(1 1 1) surfaces using MOCVD. • The films have high quality wurtzite structure and c-axis orientation. • Full width at half maximum of the 0002 in-plane X-ray rocking curve is 1.70°–3.44°. • The film thickness reduces at a rate of 0.8–1.2 nm/μm down the vertical surfaces. • Reducing the deposition pressure improves the film conformality and morphology. Metalorganic chemical vapor deposited (MOCVD) aluminum nitride (AlN) on vertical sidewalls can be used to implement piezoelectric in-plane actuation and sensing in microelectromechanical system (MEMS) sensors. The AlN films should optimally cover conformally the sidewalls and have good crystal quality with c -axis oriented microstructure for optimal piezoelectric properties. Previous MOCVD AlN research has focused on using AlN as a buffer layer for other III-nitrides and so far, AlN growth has not been studied on large vertical surfaces. In this study, AlN thin films were grown using MOCVD on vertical sidewalls of fabricated templates and the conformality and crystal quality was characterized. The growth template fabrication was optimized with respect to surface roughness, the conformal coverage was analyzed by measuring the thickness profiles of the films, and the crystal quality was investigated using in-plane XRD and TEM. The AlN films have good crystal quality (FWHM 1.70°–3.44°) and c -axis orientation on vertical Si(1 1 1) sidewalls. However, the thicknesses of the films reduce approximately at a rate of 0.8–1.2 nm/ μ m down the sidewall. Lowering the reactor pressure improved the conformal coverage while changing the growth mode from columnar to step-flow, which also improved the film morphology. [ABSTRACT FROM AUTHOR]

Though several methods exist to produce bulk crystals of gallium nitride (GaN), none have been commercialized on a large scale. The sodium flux method, which involves precipitation of GaN from a sodium–gallium melt supersaturated with nitrogen, offers potentially lower cost production due to relatively mild process conditions while maintaining high crystal quality. We successfully developed a novel apparatus for conducting crystal growth of bulk GaN using the sodium flux method which has advantages with respect to prior reports. A key task was to prevent sodium loss or migration from the growth environment while permitting N 2 to access the growing crystal. We accomplished this by implementing a reflux condensing stem along with a reusable capsule containing a hermetic seal. The reflux condensing stem also enabled direct monitoring of the melt temperature, which has not been previously reported for the sodium flux method. Furthermore, we identified and utilized molybdenum and the molybdenum alloy TZM as a material capable of directly containing the corrosive sodium–gallium melt. This allowed implementation of a crucible-free system, which may improve process control and potentially lower crystal impurity levels. Nucleation and growth of parasitic GaN (“PolyGaN”) on non-seed surfaces occurred in early designs. However, the addition of carbon in later designs suppressed PolyGaN formation and allowed growth of single crystal GaN. Growth rates for the (0001) Ga face (+ c -plane) were up to 14 µm/h while X-ray omega rocking (ω-XRC) curve full width half-max values were 731″ for crystals grown using a later system design. Oxygen levels were high, >10 19 atoms/cm 3 , possibly due to reactor cleaning and handling procedures. [ABSTRACT FROM AUTHOR]

Ammonothermally grown GaN is a promising substrate for high-power optoelectronics and electronics thanks to its scalability and high structural perfection. Despite extensive research, ammonothermal GaN still suffers from significant concentrations of impurities. This article discusses the evolution of impurity incorporation during growth of basic ammonothermal GaN, in specific whether the impurity concentration changes temporally along the growth direction and how the autoclave influences the impurity concentration. The effect of the impurities on the structural, electrical and optical properties of the grown crystal is also discussed. The chemical analysis is carried out by time of flight secondary ion mass spectroscopy (ToF-SIMS) and laser-ablation inductively-coupled plasma mass spectroscopy (LA-ICP-MS). Strain and dislocation generation caused by impurity concentration gradients and steps are studied by synchrotron radiation x-ray topography (SR-XRT). Fourier transform infrared (FTIR) reflectivity is used to determine the effect of the impurities on the free carrier concentration, and the luminescent properties are studied by low temperature photoluminescence (PL). The influence of the autoclave is studied by growing a single boule in multiple steps in several autoclaves. LA-ICP-MS and ToF-SIMS ion intensities indicate that the impurity concentrations of several species vary between different autoclaves by over an order of magnitude. SR-XRT measurements reveal strain at the growth interfaces due to impurity concentration gradients and steps. Oxygen is determined to be the most abundant impurity species, resulting in a high free carrier concentration, as determined by FTIR. The large variation in Mn concentration dramatically affects PL intensity. [ABSTRACT FROM AUTHOR]

The ammonothermal method is one of the most promising candidates for large-scale bulk GaN growth due to its scalability and high crystalline quality. However, emphasis needs to be put on understanding the incorporation and effects of impurities during growth. This article discusses how impurities are incorporated in different growth zones in basic ammonothermal GaN, and how they affect the structural, electrical and optical properties of the grown crystal. The influence of growth time on the impurity incorporation is also studied. We measure the oxygen, silicon, and carbon impurity concentrations using secondary ion mass spectrometry, and measure their effect on the lattice constant by high resolution x-ray diffraction (HR-XRD). We determine the resulting free carrier concentration by spatially resolved Fourier transform infrared spectroscopy and study the optical properties by spatially resolved low-temperature photoluminescence. We find that oxygen is incorporated preferentially in different growth regions and its incorporation efficiency depends on the growth direction. The oxygen concentration varies from 6.3×10 20 cm −3 for growth on the { 11 2 ¯ 2 } planes to 2.2×10 19 cm −3 for growth on the ( 0001 ) planes, while silicon and carbon concentration variation is negligible. This results in a large variation in impurity concentration over a small length scale, which causes significant differences in the strain within the boule, as determined by HR-XRD on selected areas. The impurity concentration variation induces large differences in the free carrier concentration, and directly affects the photoluminescence intensity. [ABSTRACT FROM AUTHOR]