Phase separation of InxGa1−xN into Ga-rich and In-rich regions has been studied by electron energy-loss spectroscopy (EELS) in a monochromated, aberration corrected scanning transmission electron microscope (STEM). We analyze the full spectral information contained in EELS of InGaN, combining for the first time studies of high-energy and low-energy ionization edges, plasmon, and valence losses. Elemental maps of the N K, In M4,5 and Ga L2,3 edges recorded by spectrum imaging at 100 kV reveal sub-nm fluctuations of the local indium content. The low energetic edges of Ga M4,5 and In N4,5 partially overlap with the plasmon peaks. Both have been fitted iteratively to a linear superimposition of reference spectra for GaN, InN, and InGaN, providing a direct measurement of phase separation at the nm-scale. Bandgap measurements are limited in real space by scattering delocalization rather than the electron beam size to ∼10 nm for small bandgaps, and their energetic accuracy by the method of fitting the onset of the joint density of states rather than energy resolution. For an In0.62Ga0.38N thin film we show that phase separation occurs on several length scales.

Phase separation of InxGa1-xN alloys into Ga-rich and In-rich regions was observed by a number of research groups for samples grown with high indium content, x. Due to the radiation sensitivity of InGaN to beam damage by fast electrons, high-resolution imaging in transmission electron microscopy (TEM) or core-loss electron energy-loss spectroscopy (EELS) may lead to erroneous results. Low-loss EELS can yield spectra of the plasmon loss regions at much lower electron fluxes. Unfortunately, due to their delayed edge onset, the low energetic core losses of Ga and In partially overlap with the plasmon peaks, all of which shift with indium content.

Here we demonstrate a method to quantify phase separation in InGaN thin films from the low-loss region in EELS by simultaneously fitting both plasmon and core losses over the energy range of 13-30eV. Phase separation is shown to lead to a broadening of the plasmon peak and the overlapping core losses, resulting in an unreliable determination of the indium concentration from analyzing the plasmon peak position alone if phase separation is present. For x=0.3 and x=0.59, the relative contributions of the binary compounds are negligibly small and indicate random alloys. For xnom.=0.62 we observed strong broadening, indicating phase separation.

In this work, we carry out structural analysis of ferromagnetic Mn-doped ZnO thin films deposited by radio frequency magnetron sputtering, using transmission electron microscopy (TEM) and high resolution x-ray diffraction. On top of sapphire (0001) substrates, Mn rich precipitates and an interface reaction layer are observed following the deposition of Zn(Mn)O layers above 500°C. The crystalline quality of ZnO layers deposited by magnetron sputtering is highly improved at 500°C as well as the measured ferromagnetic response.

ZnO nanorods were grown by catalyst-assisted vapor phase transport on Si(001), GaN(0001)/c-Al2O3, and bulk ZnO(0001) substrates. Morphology studies showed that ZnO nanorods grew mostly perpendicularly to the GaN substrate surface, whereas a more random directional distribution was found for nanorods on Si. Optical properties of fabricated nanorods were studied by steady-state photoluminescence and time-resolved photoluminescence. Stimulated emission was observed from ZnO nanorods on GaN substrates. Raman spectroscopy revealed biaxial strain in the nanorod samples grown on Si. Conductive atomic force microscopy was applied to study I-V spectra of individual nanorods.

The energy of coincidence grain boundaries in wurtzite structure was investigated with the Stillinger-Weber potential after modification for GaN. A boundary can have two interfaces with a different period corresponding to the edge and diagonal of the unit cell of coincidence site lattices for rotations around [0001] in the range 0–60°. Their energy depends mainly on the atomic structure of the dislocation cores used for the boundary plane reconstruction. As a function of the structure units in the period, the energy of the edge and diagonal shows two minima which are observed for the edge boundaries.

An investigation of 1–5 nm in diameter indium rich clusters in MOCVD InxGa1-xN/GaN quantum well is carried out. To this end, quantitative High Resolution Transmission Electron Microscopy (HRTEM) is coupled with the Finite Element Method (FEM) for the calculation of thin foil relaxation and for image simulation. The measurement of the tetragonal distortion from HRTEM images is a useful tool for the determination of chemical composition in heterostructures. However, for a correct interpretation of the measured lattice distortion on HRTEM images, one needs to take into account the strain averaging across TEM sample and inhomogeneous relaxation of the sample. As a first step, 3D FEM simulation of the relaxation process as a function of the position of indium rich cluster relative to the foil surface is performed. Next, the calculated 3D displacement field is used to simulate the HRTEM images. The results clearly show that the magnitude of the strain field depends on the cluster position. It is concluded that the HRTEM images of indium rich clusters can differ even for the same indium content due to different positions of the clusters.

Epitaxial layers of GaN contain a very high density of threading dislocations. In the first stage of growth they may form low and high angle grain boundaries. Energetic calculations of <0001> tilt grain boundaries have been performed with the Stillinger-Weber potential modified to take into account the wrong bonds Ga-Ga and N-N. The variation of the energy has been calculated as a function of the rotation angle. Two minima exist with special atomic structures based on a limited number of structural units. They are used to describe the other misorientations in terms of dislocation cores.

We investigated the structural behavior of the Ni/Au contact on GaN(000l) during annealing in N2, using in-situ x-ray diffraction, anomalous x-ray scattering, and high resolution electron microscopy. Thermally activated atomic mobility caused the two metal atoms, Au and Ni, to interdiffuse during annealing and form solid solutions. At temperature higher than 500°C, GaN decomposition and reactions occurred mostly along GaN dislocations. By decomposed nitrogen reacted with Ni, interestingly, epitaxial Ni4N phase was formed. The epitaxial relationship of the Ni4N, Au, and Ni was identified as M(111)//GaN(0002) and M[0 1 1]//GaN[0211] (M= Ni4N, Au, and Ni).

The interaction of growth intrinsic stacking faults with inversion domain boundaries in GaN epitaxial layers is studied by high resolution electron microscopy. It is observed that stacking faults may mediate a structural transformation of inversion domain boundaries, from the low energy types, known as IDB boundaries, to the high energy ones, known as Holt-type boundaries. Such interactions may be attributed to the different growth rates of adjacent domains of inverse polarity.

The influence of the variation of the Ga/N flux ratio during deposition and of the different substrate nitridation temperatures on the microstructure of 2H-GaN films grown on (0001) sapphire, by RF plasma MBE, is investigated by conventional and high resolution Transmission Electron Microscopy (TEM-HREM). The different growth rates of the inverse polarity domains in Ga-rich and N-rich specimens result in film surfaces of different roughness, whereas the stacking fault (SF) content is significantly higher in samples grown under N-rich conditions. Low temperature nitridation of the substrate results in a low density of defects in GaN film. Cubic GaN “pockets”, near the substrate/GaN interface that are present in low temperature nitridated samples are not observed in high temperature nitridated samples.

The growth of InGaN layers was carried out by molecular beam epitaxy (MBE). The nitrogen precursor was ammonia. The optical and structural properties of the InGaN layers have been investigated by transmission electron microscopy (TEM), x-ray diffraction (XRD) and photoluminescence (PL). For optimized growth conditions, the PL spectrum of InGaN (x=0.1) alloy is narrow (FWHM ≤ 50 meV) and the Stokes shift measured by PL excitation is weak (<50 meV), i.e. near band edge transitions are observed. Under these conditions, flat surfaces can be obtained, and InGaN/GaN quantum wells (QWs) with sharp interfaces can be grown. On the other hand, when growth conditions depart from a narrow optimum window, the structural quality of the samples strongly degrade, whereas the luminescence spectra are dominated by deep levels, exhibiting a strong Stokes shift. MBE grown light emitting diodes (LEDs) using InGaN/GaN QWs have been fabricated. Their electroluminescence (EL) peaks at 440 nm at 300K.

The growth of InGaN layers was carried out by molecular beam epitaxy (MBE). The nitrogen precursor was ammonia. The optical and structural properties of the InGaN layers have been investigated by transmission electron microscopy (TEM), x-ray diffraction (XRD) and photoluminescence (PL). For optimized growth conditions, the PL spectrum of InGaN (x=0.1) alloy is narrow (FWHM ≤ 50 meV) and the Stokes shift measured by PL excitation is weak (<50 meV), i.e. near band edge transitions are observed. Under these conditions, flat surfaces can be obtained, and InGaN/GaN quantum wells (QWs) with sharp interfaces can be grown. On the other hand, when growth conditions depart from a narrow optimum window, the structural quality of the samples strongly degrade, whereas the luminescence spectra are dominated by deep levels, exhibiting a strong Stokes shift. MBE grown light emitting diodes (LEDs) using InGaN/GaN QWs have been fabricated. Their electroluminescence (EL) peaks at 440 nm at 300K.