This paper characterizes novel “star” defects in GaN films grown with metal–organic vapor phase deposition (MOVPE) on GaN substrates with electron channeling contrast imaging (ECCI) and high-resolution electron backscatter diffraction (HREBSD). These defects are hundreds of microns in size and tend to aggregate threading dislocations at their centers. They are the intersection of six nearly ideal low-angle tilt boundaries composed of $\langle a\rangle$-type pyramidal edge dislocations, each on a unique slip system.

Focused ion beam is a powerful method for cross-sectional transmission electron microscope sample preparation due to being site specific and not limited to certain materials. It has, however, been difficult to apply to many nanostructured materials as they are prone to damage due to extending from the surface. Here we show methods for focused ion beam sample preparation for transmission electron microscopy analysis of such materials, demonstrated on GaAs–GaInP core shell nanowires. We use polymer resin as support and protection and are able to produce cross-sections both perpendicular to and parallel with the substrate surface with minimal damage. Consequently, nanowires grown perpendicular to the substrates could be imaged both in plan and side view, including the nanowire–substrate interface in the latter case. Using the methods presented here we could analyze the faceting and homogeneity of hundreds of adjacent nanowires in a single lamella.

GaN undoped layers of good morphology, good crystallinity and electrical properties were grown on c-plane sapphire substrates by the atmospheric pressure MOVPE technique using a new multi-buffer growth approach. A suitable buffer layer growth technique was worked out which enabled growth of GaN layers with properties superior to those grown in a conventional process scheme. Additional buffer layers, deposited with increasing temperature and increasing V/III molar ratio, were inserted between the low temperature buffer layer and the high temperature GaN layer grown on it. The c and a lattice constants of the high temperature GaN overgrown layer were evaluated from X-ray data. The layer mosaicity and c-lattice parameter variation were determined. The relationship between c and a lattice parameters and the second buffer layer growth scheme has been studied. The effect of second buffer layer growth conditions, buffer layer annealing time as well as the influence of V/III molar ratio during the high temperature GaN deposition on the crystalline and electrical properties of overgrown GaN epitaxial layers are presented. Characterization includes surface morphology examination by SEM and Nomarski optical microscope, X-ray diffraction and C-V measurements.

The wurtzite structure In1−x−yGaxAlyN quaternary system is studied with respect to the unstable region in mixing. The composition in the unstable region is calculated from the free energy of mixing by using the strictly regular solution model. The interaction parameter used in this calculation is obtained by using the delta-lattice-parameter method. Here, the proportionality constant connecting the lattice constants and the band-gap energy is determined by fitting the calculation to the composition data obtained experimentally from InGaN grown by metallorganic vapor phase epitaxy. From this calculation, the ternary alloys of InAlN, InGaN and GaAlN are predicted to always, sometimes, and hardly ever, respectively, have an unstable mixing region. The essential mismatch in thermal equilibrium between the strictly regular solution approximation and the growth conditions in MOVPE is removed by using a fitting calculation and experimental data. Also, the mismatch between the zinc-blende structure and the wurtzite structure is corrected. As a result, this prediction of the phase separation in In1−x−yGaxAlyN becomes more reliable.

InGaN films have been grown on GaN and AlGaN epitaxial layers by metalorganic vapor phase epitaxy. The “composition pulling effect” during the initial InGaN growth stages has been studied as a function of the lattice mismatch between the InGaN and the underlying epitaxial layer. The crystalline quality of the InGaN is good near the InGaN/GaN interface and the composition is close to that of GaN. However, with increasing InGaN film thickness, the crystal quality deteriorates and the indium mole fraction increases. The composition pulling effect becomes stronger with increasing lattice mismatch. It is suggested that indium atoms are excluded from the InGaN lattice during the early growth stages to reduce the deformation energy from the lattice mismatch. TEM observations of the InGaN/GaN structure reveal that the degradation of the crystalline quality of InGaN films grown on GaN is caused by pit formation which arises from edge dislocations propagating through the InGaN film from the underlying GaN.

We present results on the growth of Al-Ga-In-N films in multiwafer reactors with 7×2″ wafer capacity. The design of these reactors allows the combination of high efficiency (TMGa efficiency for GaN around 30%) and excellent uniformity. Results on the growth of all materials from the Al-Ga-In-Nitride family are presented in detail. GaN is grown with an excellent optical quality and very good thickness uniformity below 2% across 2″ wafers. The material quality is shown by electron mobility of more than 500 cm2/Vs at an intentional Si-doping of approximately 1×1017 cm−3. Controlled acceptor doping with Mg yields carrier concentrations between 5×1016 and 1018 cm−3. The layer thickness uniformity of the films are better than 2% over a 2″ wafer area. GaInN is grown with PL emission wavelengths in the visible blue region showing a uniformity better than 1.5 nm standard deviation. The film thickness uniformity represents the same figures as obtained for the binary. The compositional uniformity of AlGaN is in the sub 1% range corresponding to a wavelength variation below 1 nm.

The fabrication of heterostructures from these binary and ternary materials is described as well as results from the characterization of these structures. The results show that reliable and efficient production of Al-Ga-In-Nitride based optoelectronic devices can be performed in multiwafer reactors.

The dependence of the In-incorporation efficiency and the optical properties of MOVPE-grown GaInN/GaN-heterostructures on various growth parameters has been investigated. A significant improvement of the In-incorporation rate could be obtained by increasing the growth rate and reducing the H2-partial pressure in the MOVPE reactor. However, GaInN layers with a high In-content typically show an additional low energy photoluminescence peak, whose distance to the band-edge increases with increasing In-content. For GaInN/GaN quantum wells with an In-content of approximately 12%, an increase of the well thickness is accompanied by a significant line broadening and a large increase of the Stokes shift between the emission peak and the band edge determined by photothermal deflection spectroscopy. With a further increase of the thickness of the GaInN layer, a second GaInN-correlated emission peak emerges. To elucidate the nature of these optical transitions, power-dependent as well as time-resolved photoluminescence measurements have been performed and compared to the results of scanning transmission electron microscopy.

The ternary alloy GaAlN has been grown by low pressure MOVPE (76 Torr) using triethylgallium, trimetylaluminum and ammonia as precursors. The alloy layers were grown on (0001) sapphire substrates using a low temperature AlN buffer. All layers were deposited at a growth temperature of 980°C. Only the aluminum/gallium ratio in the gas phase was changed, keeping the total group III molar flow rate and V/III molar ratio constant.

The aluminum incorporation versus gas phase composition was determined experimentally, using energy dispersive analysis of X-rays (EDAX), and X-ray diffraction. We propose a model, taking into account kinetically limited mass transport of group III species in the gas phase, which describes well the data.

The structural quality of the layers was investigated using X-ray diffraction and TEM experiments.

A degradation of the materials quality is observed with increasing Al content. In this case, growth originate on the buffer grains facets resulting in a “ two directional » growth. This phenomenon, being markedly enhanced when increasing the Al content will be detailed in this paper.

In this paper, we address two different aspects relevant to the growth of GaN. The first part concerns alternative nitrogen source whereas in the second part, we report experimental results on Mg doping. Several nitrogen precursors have been used for the growth of GaN in MOVPE. To produce active species from N2 or NH3, a remote Plasma Enhanced Chemical Vapour Deposition (RPECVD) process has been implemented. In addition, nitrogen organic precursors, triethylamine and t-butylamine were also used. To accurately control the critical parameters of the MOVPE of GaN, we have implemented a laser reflectometry, which allows a real time in situ monitoring of the different steps of the growth. MeCp2Mg was used as Mg precursor for the p doping study. The dependence on the partial pressure of Mg precursor of dopant incorporation, electrical activity and growth rate are reported.