P.Q. Miraglia

Application of Nomarski interference contrast microscopy as a thickness monitor in the preparation of transparent, SiC-based, cross-sectional TEM samples

Reflected light optical microscopy using a Nomarski prism and a differential interference contrast filter have been employed in concert to achieve a technique that provides an accurate color reference for thickness during the dimpling and ion milling of transparent transmission electron microscopy samples of 6H-SiC(000 1) wafers. The samples had thin films of AIN, GaN, and Au deposited on the SiC substrate. A sequence of variously colored primary and secondary interference bands was observed when the SiC was thinner than 20 microm using an optical microscope. The color bands were correlated with the TEM sample thickness as measured via scanning electron microscopy. The interference contrast was used to provide an indication of the dimpling rate, the ion milling rate, and also the most probable location of perforation, which are useful to reduce sample breakage. The application of pressure during the initial cross-sectional preparation reduced the separation of the two halves of the sample sandwich and resulted in increased shielding of the film surface from ion milling damage.

Polarization charges and polarization-induced barriers in AlxGa1−xN/GaN and InyGa1−yN/GaN heterostructures

Polarization charges are measured and the formation of large electrostatic barriers arising primarily as a consequence of the presence of polarization-induced charge densities is deduced from capacitance–voltage analysis of n-type AlxGa1−xN/GaN and InyGa1−yN/GaN heterostructures. In structures consisting of 5–10 nm AlxGa1−xN or InyGa1−yN surrounded by n-GaN, capacitance–voltage profiling studies combined with elementary electrostatic analysis yield experimental estimates of polarization charge densities, which are compared with values expected based on the combined effects of spontaneous and piezoelectric polarization. These results imply the existence of electrostatic barriers that are due primarily to the large polarization charge densities at each heterojunction interface and the resulting potential difference maintained across the thin AlxGa1−xN or InyGa1−yN layers. The electrostatic barriers formed in these structures are large in comparison to the heterojunction conduction-band offsets, demonstratin...

Electrical, structural and microstructural characteristics of as-deposited and annealed Pt and Au contacts on chemical-vapor-cleaned GaN thin films

Schottky contacts of Pt(111) and Au(111) were deposited on chemical-vapor-cleaned, n-type GaN(0001) thin films. The growth mode of the deposition, as determined by x-ray photoelectron spectroscopy analysis, followed the two-dimensional Frank–van der Merwe growth model. The resulting as-deposited metal films were monocrystalline and epitaxial with a (111)//(0002) relationship with the GaN. Selected samples were annealed for three minutes at 400 °C, 600 °C or 800 °C. The rectifying behavior of both contacts degraded at 400 °C; they became ohmic after annealing at 600 °C (Au) or 800 °C (Pt). High-resolution transmission electron micrographs revealed reactions at the metal/GaN interfaces for the higher temperature samples. X-ray diffraction results revealed an unidentified phase in the Pt sample annealed at 800 °C. A decrease in the room temperature in-plane (111) lattice constant for both metals, ranging from −0.1% to −0.5%, was observed as the annealing temperature was increased from 400 to 800 °C. This pla...

Strain and Dislocation Reduction in Maskless Pendeo-Epitaxy GaN Thin Films

Measurement of strain in GaN films grown via pendeo-epitaxy (PE) indicates that the overgrowth, or wing, material is crystallographically relaxed. An increase of 0.02% in the c-axis lattice parameter of the wing material was measured via high-resolution X-ray diffraction (HRXRD); additional evidence for this increase was indicated by an upward shift of the E2 Raman line frequency. Atomic force microscopy studies revealed a reduction in the density of mixed-type dislocations in the wing. A reduction in screw-type dislocations in the wings with respect to the stripes is indicated by a reduction in HRXRD rocking curve FWHM of the (0002) reflections from 646 to 354 arcsec. The off-axis FWHM of the wing area was 126 arcsec compared to 296 arcsec for the stripe indicating reduction in the edge-type dislocations as well. Pendeo-epitaxy growth of wings off the (1120) surface of a GaN stripe produced a material that is crystallographically relaxed, contains fewer defects compared to the stripe and is atomically smooth on the (1120) surface.

Domain structures in 6H-SiC wafers and their effect on the microstructures of GaN films grown on A1N and A10.2Ga0.8N buffer layers

Abstract Silicon carbide wafers contain domains with varying sizes and degrees of tilt. The present research has shown that this microstructure is mimicked in GaN films deposited on AlN-containing buffer layers and that it masks most variations in the FWHM of the X-ray rocking curves of the former. The shape and FWHM in the GaN curves are determined both by domain tilting and dislocation broadening; the latter was dominant in areas of reduced tilt. Analyses of the on- and off-axis X-ray data acquired from these regions of lower tilt revealed the marked effect of the higher density of edge dislocations on broadening. This effect decreased with increasing GaN thickness due to dislocation annihilation. The densities of edge dislocations in GaN films deposited at 1010°C on pitted, less pitted and very smooth AlN layers of the same thickness grown at 1010°C, 1130°C and 1220°C, respectively, were lowest and highest in those films grown on the last two respective layers. Additional studies showed that GaN films grow on Al 0.2 Ga 0.8 N layers via step-flow and possess a lower edge dislocation density than films grown via the Stranski–Krastanov mode on AlN because of the reduced misfit and the absence of boundaries between coalesced islands.

Electron energy distribution during high-field transport in AlN

The energy distribution of electrons transported through intrinsic AlN heteroepitaxial films grown on SiC was directly measured as a function of applied field and AlN film thickness. Following the transport, electrons were extracted into vacuum through a semitransparent Au electrode and their energy distribution was measured using an electron spectrometer. Transport through films thicker than 95 nm at an applied field between 200 and 350 kV/cm occurred as steady-state hot electron transport following a Maxwellian energy distribution with a characteristic carrier temperature. At higher fields (470 kV/cm), intervalley scattering was evidenced by a multicomponent energy distribution featuring a second peak at the energy position of the first satellite valley. Velocity overshoot was observed in films thinner than 95 nm and at fields greater than 550 kV/cm. In this case, a symmetric energy distribution centered at an energy above the conduction band minimum was measured, indicating that the drift component of ...

Removal of 6H-SiC substrate influence when evaluating GaN thin film properties via x-ray

Non-uniformity in GaN thin films deposited on 6H-SiC can make determining the effects of growth variables difficult. Results presented in this work show the effects of the SiC substrates on the GaN films, and how to correct for these effects to obtain meaningful data about the properties of the thin film rather than the substrate underneath. Rocking curve values of GaN thin films are found to track almost 1:1 with the values of the underlying SiC. Plotting rocking curves with respect to the substrate, as well as a variable of importance can therefore yield more meaningful and reliable comparisons instead of plotting the data for the variable alone. This procedure is used to demonstrate the effects of thickness and AlN and AlGaN buffer layers on GaN thin films.

Growth and Characterization of GaN Bulk Crystals via Vapor Phase Transport

Free-standing single crystals of bulk GaN were grown via unseeded vapor phase transport at 1130C on hexagonal BN surfaces via direct reaction of Ga with ammonia. The temperature and stability of the Ga source were critical in terms of uniform nucleation and growth. The source temperature was maintained at 1260C to minimize a rapid reaction leading to the formation of GaN and the subsequent decomposition beneath the surface and consequent spattering of Ga. A maximum crystal growth temperature of 1130C was determined in which the GaN growth kinetics were much greater than decomposition. The number of nucleation events was reduced and the crystal size increased by a novel nucleation technique wherein ammonia was introduced at high temperatures. The resulting crystals were either needles or platelets depending on the process variables employed. Low V/III ratios achieved via ammonia flow rates 75sccm and/or ammonia total pressures 430Torr favored lateral growth. The average lateral growth rate for the platelets was ~50micron/hr; the average vertical growth rate for the needles was ~500micron/hr. Growth rates in all other directions for each of these two morphologies were very low. Seeded growth of both needle and platelet crystals was also achieved; however, the growth rate decreased at longer times and higher pressures due to reaction with hydrogen from the increased decomposition of ammonia. Nitrogen dilution of ammonia reduced the amount of hydrogen generated as a result of ammonia decomposition and increased the kinetic barrier to desorption of reactants from the GaN surface and then alleviated the enhanced decomposition of GaN crystals. A 2mm x 1.5mm needle and a 2.3mm x 1.8mm x 0.3mm platelet of GaN were grown with minimal decomposition in a 66.7% ammonia + 33.3% nitrogen gas mixture. Excellent crystalline quality was confirmed by Raman spectroscopy and Photoluminescence.Crystal growth using a Ga- 5at%Al source was conducted in an attempt to increase growth rate and inhibit decomposition. No notable change in growth rate was observed and hollow crystals were formed, indicating that Al promotes vertical growth under otherwise similar conditions for GaN growth. In addition, fine-grained AlN was formed within the binary Ga-Al source, thus, the supply of Al was progressively reduced. Nucleation control via addition of Si resulted in a slightly reduced number of larger crystals. X-ray Photoelectron Spectroscopy suggested that amorphous silicon nitride was formed on the BN substrate and nucleation rate was slightly reduced. Silicon was not detected within the sensitivity of Energy Dispersive Spectroscopy. Raman spectroscopy revealed insignificant amount of Si present in the crystal. Smoother surface morphology of the crystals grown in the presence of Si was observed by Scanning Electron Microscopy.