Spatially resolved X‐ray diffraction as a tool for strain analysis in laterally modulated epitaxial structures

Spatially resolved X‐ray diffraction (SRXRD) is applied for micro‐imaging of strain in laterally modulated epitaxial structures. In GaAs layers grown by liquid phase epitaxial lateral overgrowth (ELO) on SiO₂‐masked GaAs substrates a downward tilt of ELO wings caused by their interaction with the mask is observed. The distribution of the tilt magnitude across the wings width is determined with μm‐scale spatial resolution. This allows measuring of the shape of the lattice planes in individual ELO stripes. If a large area of the sample is studied the X‐ray imaging provides precise information on the tilt of an individual wing and its distribution. In heteroepitaxial GaSb/GaAs ELO layers local mosaicity in the wing area is found. By the SRXRD the size of microblocks and their relative misorientation were analyzed. Finally, the SRXRD technique was applied to study distribution of localized strain in AlGaN epilayers grown by MOVPE on bulk GaN substrates with AlN mask. X‐ray mapping proves that by mask patterning strain in AlGaN layer can be easily engineered, which opens a way to produce thicker, crack‐free AlGaN layers with a higher Al content needed in GaN‐based laser diodes. All these examples show that high spatial and angular resolutions offered by SRXRD makes the technique a powerful tool to study local lattice distortions in semiconductor microstructures. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Molecular beam epitaxy of GaN/AlxGa1−xN superlattices for 1.52 – 4.2 μm intersubband transitions

High-quality superlattice structures of GaN/AlGaN were grown on (0 0 0 1) sapphire substrates by molecular beam epitaxy. The threading dislocation density was reduced by growing low-temperature AlN layers in between the high-temperature GaN. In addition, in situ monitoring of the growth rate was achieved using pyrometric interferometry. Cross-sectional transmission electron microscopy of the superlattice structures revealed abrupt interfaces between GaN/AlGaN and excellent layer uniformity. We observed intersubband absorption at wavelengths as short as 1.52 μm in the GaN/AlGaN material system. A range of intersubband absorption peaks was observed between 1.52 and 4.2 μm by varying the well thickness and barrier Al content. In addition, the distribution of the built-in electric field between the well and barrier layers was also found to affect the intersubband transition wavelength.     

Thick GaN layers on sapphire with various buffer layers

Thick GaN layers deposited in HVPE system on composite substrates made on sapphire substrates in Metalorganic Vapour Phase Epitaxy (MOVPE) system have been investigated. The following substrates were used: (00.1) sapphire substrates with AlN, AlN/GaN and GaN thin layers. The crystallographic structure and the quality of the epitaxial thick GaN layers were determined. Comparison of the three types of thick layers was performed. Significant differences were observed. It was found that thick GaN deposited on the simplest MOVPE‐GaN/sapphire composite substrate has comparable structure's properties as the other, more complicated. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Growth Kinetics and Surface Morphology of GaN Epitaxial Layers on Sapphire

The growth kinetics of GaN on Sapphire was analyed on the base of some experimental data such as: the growth rate temperature depandence, on the base of some experimental data such as: the growth rate temperature dependence, the grwoth rate dependence on the gas flow velocity, the growth rate depandence on the crystallographic and spatial orientation of the substrate. The limiting stage of the epitaxy process was established at different growth conditions. The morphology of GaN epitaxial layers obtained at these conditions is described.     

AlGaN epitaxial lateral overgrowth on Ti-evaporated GaN/sapphire substrate

AlGaN growth using epitaxial lateral overgrowth (ELO) by metalorganic chemical vapor deposition on striped Ti, evaporated GaN on sapphire, has been investigated. AlGaN/AlN films growth on GaN/AlGaN superlattices (SLs) structure on the Ti masks, with various SLs growth temperature (1030, 1060 and 1090 °C) were grown. With increasing the growth temperature, AlGaN surface became flat. The AlGaN film had a cathodoluminescence peak around 345 nm. However, in secondary ion mass spectrometry (SIMS) measurement, Ti signal was detected on the top of AlGaN surface when GaN/AlGaN SLs was grown on Ti striped masks. By inserting the AlN blocking layer on SLs, Ti diffusion was stopped at the AlN layer, and the AlGaN crystalline quality was improved.     

Ammonothermal epitaxy of wurtzite GaN using an NH4I mineralizer

Purely wurtzite phase needle crystals and epitaxial layers of GaN were grown by the ammonothermal method using an NH₄I mineralizer. The inclusion of zincblende phase GaN was effectively eliminated by increasing the growth temperature higher than 500 °C. Accordingly, an approximately 20-μm-thick GaN epitaxial layer was achieved on the Ga-polar face of a c-plane GaN seed wafer at 520 °C. Although the characteristic deep state emission band dominated the room temperature photoluminescence spectrum, the near-band-edge emission of GaN was observed for both the needle crystals and the epitaxial layers. These results encourage one to grow better quality GaN crystals at a high growth rate under high-temperature growth conditions.     

Triple axis diffractometric investigations of the microstructure of thin AlxGa1‐xN epitaxial films

Al_xGa_1‐xN/GaN (Si doped or undoped) with the Al content in the composition range of 0.046 ≤ x ≤ 0.164 grown on the c sapphire face by atmospheric pressure MOCVD method were studied by high resolution x‐ray diffraction including symmetrical and asymmetrical ω/2θ scans and reciprocal space maps. A high sensitivity to small inhomogeneities of the layer thickness and lattice mismatch between AlGaN and GaN is reported, recognised as changes in the interference pattern of the diffraction peak observed across the sample. They are very well correlated with optical properties derived from independent photoreflectivity measurements. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Investigation of metal–GaN and metal–AlGaN contacts by XPS depth profiles and by electrical measurements

Metal/GaN Schottky contacts have been studied by X-ray photoelectron spectroscopy (XPS). Au/GaN, Pt/GaN, Pd/GaN are sharp while Ti/GaN is diffuse with the following composition, starting from the surface: Ti+TiN, Ti+Ti_xGa_yN, Ti+Ti_xGa_yN+Ga, GaN+Ga. Au/AlGaN and Ni/AlGaN contacts are much broader than Au/GaN: Al and Ga are found more than 100 Å away from the interface. Schottky barrier height was measured for the Au/GaN, Pd/GaN, Pt/GaN, Au/AlGaN and Ni/AlGaN contacts.     

Epitaxial growth of silicon carbide layers by sublimation “Sandwich method” (II) structural defects and growth mechanism

Structural defects of α-SiC epitaxial layers grown by sublimation “sandwich-method” in vacuum at the temperatures ranging from 1600 to 2100 °C have been investigated by X-ray topography and optical microscopy methods. It was shown, that perfect SiC layers with the homogeneous polytype structure and small dislocation density (≦ 10² cm⁻²) may be obtained on the substrates with any crystallographic orientation at the conditions close to quasi-equilibrium one. The presence of impurities and silicon deficiency in the vapour phase, lead usually to the deterioration of morphological and structural perfection of SiC layers. There are the following structural defects: uncoherent polytype inclusions (mainly β-SiC), pores, dislocations, specific stacking faults. Morphological peculiarities of the SiC epitaxial layers and possible growth mechanisms are discussed.     

Molecular beam epitaxy (MBE) growth and structural properties of GaN and AlN on 3C-SiC(0 0 1) substrates

AlN and GaN was deposited by molecular beam epitaxy (MBE) on 3C-SiC(0 0 1) substrates on low-temperature (LT) GaN and AlN buffer layers. It is shown that not only GaN but also epitaxial AlN can be stabilized in the metastable zincblende phase. The zincblende AlN is only obtained on a zincblende LT-GaN buffer layer; on the other hand, AlN crystallizes in the wurtzite phase if it is grown directly on a 3C-SiC(0 0 1) substrate or on a LT-AlN buffer layer. The structural properties of the layers and in particular the orientation relationship of the wurtzite AlN on the 3C-SiC(0 0 1) were analyzed by conventional and high-resolution transmission electron microscopy.     

Investigation on the origin of crystallographic tilt in lateral epitaxial overgrown GaN using selective etching

The crystallographic tilt of the lateral epitaxial overgrown (LEO) GaN on sapphire substrate with SiN_x mask is investigated by double crystal X-ray diffraction. Two wing peaks beside the GaN 0002 peak can be observed for the as-grown LEO GaN. During the selective etching of SiN_x mask, each wing peak splits into two peaks, one of which disappears as the mask is removed, while the other remains unchanged. This indicates that the crystallographic tilt of the overgrown region is caused not only by the plastic deformation resulted from the bending of threading dislocations, but by the non-uniformity elastic deformation related with the GaN/SiN_x interfacial forces. The widths of these two peaks are also studied in this paper.     

Two‐ and three‐dimensional growth modes of nitride layers

Heteroepitaxial three dimensional (3D) and two dimensional (2D) growth modes of nitride layers on sapphire substrates are discussed. It is shown that the 3D or 2D growth mode of AlGaN layers depends predominantly on the growth conditions of the underneath low temperature (LT) nucleation layer. Commonly described in literature 3D growth mode is achieved on LT GaN or AlN nucleation layer grown relatively fast. Successive growth of secondary layer at high temperature begins from separated sites, where individual 3D crystallites are formed. Threading dislocations present in crystallites bend on their facets, which reduces the quantity of dislocations. However, slight crystallographic misorientations between crystallites lead to the creation of new dislocations during coalescence of the crystallites. As a result, edge and mix dislocations appear at similar densities of about 10⁹ cm^‐2. Modification of growth conditions of LT AlN nucleation layer, especially reduction of their growth rate, leads to drastic changes in properties of the layer. Successive growth of secondary AlGaN layer at high temperature starts evenly on whole surface retaining atomic flatness. Thus growth at high temperature occurs only by 2D mode. Therefore, it is possible to grow a very thin AlGaN layers directly on top of LT nucleation layer. Such layers contain large number (10¹⁰ cm^‐2) of edge dislocations, and relatively small number (less then 10⁸ cm^‐2) of mix dislocations. It is also shown that the decisive factor determining the growth mode of AlN nucleation layer is a growth of the first few atomic layers on substrate surface. The slow growth of these few first atomic layers decide about the 2D growth mode, and the fast one about the 3D one. The model explaining this difference is presented as well. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

MOVPE of AlN-free hexagonal GaN/cubic SiC/Si heterostructures for vertical devices

The heterostructures of GaN/SiC/Si were prepared without using AlN or AlGaN buffer layers (AlN buffers) in the metalorganic vapor phase epitaxy of GaN on SiC. GaN (0 0 0 1) with specular surface was obtained. The AlN buffers are usually used in the conventional growth of GaN on SiC due to the poor nucleation of GaN on SiC. Instead, the nucleation of GaN was controlled by varying the partial pressure of H₂ in the carrier gas, the mixture of H₂ and N₂, during the low-temperature (600 °C) growth of GaN (LT-GaN). After the LT-GaN, the high-temperature (1000 °C) growth of GaN was performed using pure H₂ as the carrier gas. The epitaxial film of cubic SiC (1 1 1) on a Si (1 1 1) substrate was used as the SiC template. Increasing the partial pressure of H₂ in the carrier gas decreased the coverage of SiC surface by LT-GaN. It is suggested that the hydrogen atoms adsorbed on the surface of SiC is preventing the nucleation of GaN.     

MOVPE growth of nonpolar a-plane GaN with low oxygen contamination and specular surface on a freestanding GaN substrate

We investigated unintentionally doped nonpolar a- and m-plane GaN layers grown by metalorganic vapor phase epitaxy under several sets of conditions on freestanding a- and m-plane GaN substrates. Oxygen contamination in a-plane GaN is greatly reduced by increasing the V/III ratio during growth. As a result, a high-resistivity GaN buffer layer for an AlGaN/GaN heterostructure field-effect transistor was realized.     

Cross‐sectional and surface Raman mapping of thick GaN layers

Raman scattering spectroscopy was utilized for investigation of the structural properties of thick GaN layers. These layers with thickness ∼ 40 μm have been grown by HVPE technique on the sapphire substrates. The investigations have been focused on the strain distribution in GaN layer cross‐section as a function of distance from an interface sapphire/GaN and mapping of the surface and of the inner layer, near the sapphire/GaN interface. From the observed phonon shifts in the Raman spectra strain differences lower than 6.4×10^–4 corresponding to stress differences of 240 MPa were estimated across the thick GaN epitaxial layer. The measurements exhibit that strain in the layer causes changes in the Raman spectra and allow determining the relaxation process in the crystal. The obtained results confirmed, that the mode frequencies in the measured Raman spectra in both directions (parallel or perpendicular to the growth direction) for layer thicknesses over 30 µm are comparable with typical values for bulk material and match the low strain in the structure due to relaxation processes. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Stress control by micropits density variation in strained AlGaN/GaN/SiN/AlN/Si(111) heterostructures

AlGaN/GaN heterostructures were deposited on Si utilizing in‐situ SiN masking layer as a mean to decrease stress present in the final heterostructures. Structures were grown under different V/III ratio using metalorganic vapour phase epitaxy (MOVPE). Additional approach was applied to obtain crack‐free heterostructures which was deposition of 15 nm low temperature AlN interlayer. Each of the heterostructure contained GaN layer of 2.4 μm total thickness. In‐situ SiN masking layer were obtained via introduction of SiH4 precursor into reactor under high temperature growth conditions for 100 s. In that manner, few monolayers of SixNx masking layer were deposited, which due to the partial coverage of AlN, played role of a mask leading to initial 3D growth mode enhancing longer coalescence of GaN buffer layer. To study surface morphology AFM images were observed. Three methods were used in order to obtain basal plane stress present in multilayer structures ‐ MicroRaman spectroscopy, XRD studies and optical profilometry. It was found that varying V/III precursors ratio during GaN layer growth characteristic for structures with the SiN mask approach formation of triangular micropits can be minimized. Outcomes for three different methods turned out to be coherent. It was found that certain amount of micropits on the surface can be advantageous lowering stress introduced during cooling after process to the AlGaN/GaN/SiN/AlN/Si(111) structure.     

In situ optical monitoring of AlGaN thickness and composition during MOVPE growth of AlGaN/GaN microwave HFETs

Real-time spectral reflectometry has been implemented to monitor the MOVPE growth of AlGaN/GaN microwave HFET structures. The aim is to monitor and control the thickness and composition of the thin AlGaN layer during growth. In order to extract useful information from the in situ spectra the optical constants of AlGaN as a function of alloy composition are required at the growth temperature (1050°C). As the first step to obtaining the high temperature optical constants, a room temperature spectroscopic ellipsometry study (energy range 1.65–4.95 eV) has been carried out on thin AlGaN films of various thickness (30 and 100 nm) and aluminium content (0.15 and 0.25). The multilayer model of each sample from the ellipsometry study is used to generate a reflectance spectrum which is compared with the in situ spectral reflectometry spectrum of the same sample acquired at room temperature to verify the technique. Further work is in progress to model the bandgap and optical constants of GaN and AlGaN at growth temperature.     

石墨烯上外延GaN薄膜的取向演变研究

本文研究了在石墨烯上生长GaN薄膜时晶体取向的变化。采用AlN成核层辅助生长,GaN由取向相差较大的小晶粒,逐渐合并为与石墨烯取向一致的晶粒,最终形成了约4.6μm厚的GaN薄膜。通过EBSD和XRD证实了GaN晶体取向一致性的提高,拉曼光谱也表明GaN晶体的高质量。     

Untersuchung von GaN-Epitaxieschichten mit ionometrischen Methoden

The crystalline quality of epitaxial {0001} GaN layers of thickness between 2 and 11 μm on spinel or sapphire substrates has been investigated using proton channeling and blocking. Backscattering spectra of 1 MeV-protons indicate that the perfection of the GaN layers for GaN/sapphire is essential higher than for GaN/spinel. It has been shown that for GaN on spinel the density of imperfections decreases with increasing layer thickness. Blocking patterns give additional informations on perfection and crystal structure of the layers.     

First III–V-nitride-based violet laser diodes

InGaN multi-quantum-well (MQW) structure laser diodes (LDs) were grown by metalorganic chemical vapor deposition on a sapphire substrate with (11 0) orientation (A face). The mirror facet for a laser cavity was formed by cleaving the substrate along the (1 02) orientation (R-face). The structure of the LDs was an InGaN MQW/GaN/AlGaN separate confinement heterostructure (SCH). As an active layer, the InGaN MQW structure was used. The InGaN MQW LDs showed strong stimulated emission at a wavelength of 415.3 nm under pulsed current injection above 360 mA at room temperature. The laser threshold current density was 6 kA/cm². As a maximum characteristic temperature of the threshold current, T₀ = 313 K was obtained for the InGaN MQW/GaN/AlGaN SCH LDs.