Cathodoluminescence imaging for the determination of dislocation density in differently doped HVPE GaN

In this study we report the potential and limitations of the cathodoluminescence dark spot (DS) counting as a method for the determination of dislocation density and distribution in GaN, produced by the hydride vapour phase epitaxy (HVPE). Different GaN sample series (s.i. GaN:Fe and n-type GaN:Si) were used, in order to study the dependence of the results of the DS-counting on the dopant type and concentration. By the direct comparison of these results to classical defect selective etching, the DS-measurements were validated. It could be shown that each of the both methods have their particular restrictions, which must be considered in their application.     

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.     

Thermally induced stress in GaN layers with regard to film coalescence

Thermally induced plane stress in GaN layers of different thicknesses, grown by metalorganic vapour phase epitaxy on sapphire, is investigated. Thin layers, characterized by isolated grains, are found to be stress-free. With increasing layer thickness, however, grains start to coalesce and stress can build up when the samples are cooled down following growth. As soon as the coalescence process is completed and a compact film has been formed, a maximum stress level is reached which does not further increase for still thicker layers. Therefore, it is proposed that grain edges enable non-compact films to elastically relieve in-plane stress.     

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.     

TEM investigations of GaN layers grown on silicon and sintered GaN nano‐ceramic substrates

GaN nano‐ceramics were analyzed using transmission electron microscopy (TEM), showing that these ceramics are characterized by highly disoriented grains of the linear size of 100–150 nm. These GaN ceramics were used as substrates for GaN epitaxy in standard MOVPE conditions. For the comparison, MOVPE GaN layers on silicon substrates were grown using similar conditions. It is shown that MOVPE growth of GaN layers is highly anisotropic for both cases. However, the disorientation of the highly mismatched GaN layer on silicon is different from that characterizing GaN layer deposited on the ceramic substrate. In the latter case the disorientation is much higher, and three dimensional in nature, causing creation of polycrystalline structure having large number of the dislocations. In the case of the GaN layer grown on the silicon substrate the principal disorientation is due to rotation around c‐axis, causing creation of mosaic structure of edge dislocations. Additionally, it is shown that the typical grain size in AlN nucleation layer on Si is smaller, of order of 20 nm. These two factors contribute to pronounced differences in later stage of the growth of GaN layer on the ceramic. Due to high growth anisotropy an appropriately thick GaN layer can, eventually, develop flat surfaces suitable for construction of optoelectronic and electronic structures. As shown by the TEM data, this can be achieved only at the cost of creation of the relatively large density of dislocations and stacking faults. The latter defects were not observed for the GaN growth on Si substrates. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Overgrowth of GaN on Be-doped coalesced GaN nanocolumn layer by rf-plasma-assisted molecular-beam epitaxy—Formation of high-quality GaN microcolumns

GaN crystals were overgrown on GaN nanocolumn platforms with a Be-doped coalesced layer by rf-plasma-assisted molecular-beam epitaxy (rf-MBE). The overgrown GaN included large micrometer-scale hexagonal columnar crystals. These microcrystals were named ‘microcolumns’ and showed high optical properties comparable to those of GaN bulk crystals grown by hydride vapor phase epitaxy (HVPE).     

MOVPE growth and properties of GaN on (1 1 1)Si using an AlInN intermediate layer

Using an AlInN intermediate layer, GaN was grown on (1 1 1)Si substrate by selective metalorganic vapor phase epitaxy. The variation of the surface morphology was investigated as a function of the In composition and thickness of the AlInN layer. It was found that the In composition in the AlInN layer was a function of the growth temperature and thickness. Because of the small band offset at the AlInN/Si hetero-interface, we have achieved a low series resistance of the order of 9 Ω (0.0036 Ω cm²) across the GaN/AlInN/AlN/Si layer structure.     

Growth and properties of semi-polar GaN on a patterned silicon substrate

Adopting anisotropy etching method, a (1 1 1) facet of Si is obtained on a Si substrate and selective area growth (SAG) of GaN is performed with metal-organic vapor phase epitaxy on the facet. The epitaxial lateral overgrowth of (1 1¯ 0 1), (1 1 2¯ 2) GaN is investigated on (0 0 1) and (1 1 3) Si substrate, respectively, and the incorporation properties of Si, C, and Mg elements are discussed in relation to the atomic configuration on the surface. Analyzing the optical and electrical properties of C-doped (1 1¯ 0 1) GaN layer, it is shown that carbon creates a shallow acceptor level. On the thus prepared (1 1¯ 0 1) GaN layer, a light emitting diode (LED) with a C-doped p-type layer is fabricated.     

Transmission electron microscopy study of an AlN nucleation layer for the growth of GaN on a 7-degree off-oriented (0 0 1) Si substrate by metalorganic vapor phase epitaxy

We have investigated the morphology of the high-temperature-grown AlN nucleation layer and its role in the early stage of GaN growth, by means of transmission electron microscopy. The nitride was selectively grown on a 7-degree off-oriented (0 0 1) patterned Si substrate by metalorganic vapor phase epitaxy. AlN was deposited on the inclined unmasked (1 1 1) facet in the form of islands. The size of the islands varied along the slope, which is attributable to the diffusion of the growth species in the vapor phase. The GaN nucleation occurred at the region where rounded AlN islands formed densely. The threading dislocations were observed to generate in the GaN nucleated region.     

Growth of GaN based structures on Si(1 1 0) by molecular beam epitaxy

The growth of GaN based structures on Si(1 1 0) substrates by molecular beam epitaxy using ammonia as the nitrogen precursor is reported. The structural, optical and electrical properties of such structures are assessed and are quite similar to the ones obtained on Si(1 1 1) in-spite of the very different substrate surface symmetry. A threading dislocation density of 3.7×10⁹ cm⁻² is evaluated by transmission electron microscopy, which is in the low range of typical densities obtained on up to 2 μm thick GaN structures grown on Si(1 1 1). To assess the potential of such structure for device realization, AlGaN/GaN high electron mobility transistor and InGaN/GaN light emitting diode heterostructures were grown and their properties are compared with the ones obtained on Si(1 1 1).     

Investigation of GaN crystal quality on silicon substrates using GaN/AlN superlattice structures

The crystal quality of GaN thin film on silicon using GaN/AlN superlattice structures was investigated. The growth was carried out on Si(111) for GaN(0001) in a metal‐organic vapor phase epitaxy system. Various GaN/AlN superlattice intermediate layers have been designed to decrease the dislocation density. The results showed that the etch pit density could be greatly reduced by one order of magnitude. Cross‐sectional transmission electron microscopy (XTEM) study confirmed the efficiency of GaN/AlN superlattice in blocking threading dislocation propagation in GaN crystal. The design of nine period GaN/AlN (20nm/2nm) superlattice has been evidenced to be effective in reducing the dislocation density and improving the crystal quality. In addition, the dislocation bending in GaN/AlN interface and dislocation merging is investigated. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Strain-reduced GaN thick-film grown by hydride vapor phase epitaxy utilizing dot air-bridged structure

A 300 μm GaN thick-film, in diameter 1.5 in, was demonstrated without any crack by hydride vapor phase epitaxy (HVPE) growth. The technique used in relaxing the residual stress caused by differences of thermal expansion coefficients (TEC) and lattice constants between GaN and sapphire substrate to prevent GaN film from crack is called a dot air-bridged structure. After the laser lift-off process, 300-μm-thick freestanding GaN wafer, in diameter 1.5 in, could be fabricated. The compressive stress in the dot air-bridged structure was measured by micro-Raman spectroscopy with the E₂(high) phonon mode. The compressive stress could be reduced to as small as 0.04 GPa, which could prevent the crack during the epitaxial process for GaN growth by HVPE. It is important to obtain a large-area crack-free GaN thick-film, which can be used for fabricating freestanding GaN wafer.     

Metalorganic vapour phase epitaxy of GaN and GaInN/GaN heterostructures and quantum wells

This paper reviews the growth and some characteristics of group III-nitrides by metalorganic vapour phase epitaxy with a particular focus on GaInN layers and heterostructures. We discuss the problems encountered with the low In incorporation efficiency. This can be partly compensated by larger growth rates and higher nitrogen-hydrogen ratios in the carrier gas. However, the grown layers with larger In content show evidence of composition fluctuations and even surface roughening due to problems probably arising from the large lattice mismatch to GaN and from the miscibility gap predicted for essentially the whole composition range. This influences strongly the spectroscopic properties. Consequences on the functionality of optoelectronic devices are also shortly discussed.     

Maskless selective growth of semi-polar (1 12¯ 2) GaN on Si (3 1 1) substrate by metal organic vapor phase epitaxy

Semi-polar (1 1 2¯ 2) GaN layers were selectively grown by metal organic chemical vapor phase epitaxy on patterned Si (3 1 1) substrates without SiO₂ amorphous mask. The (1 1 2¯ 2) GaN layers could be selectively grown only on Si (1 1 1) facets when the stripe mask width was narrower than 1 μm even without SiO₂. Inhomogeneous spatial distribution of donor bound exciton (DBE) peak in low-temperature cathodoluminescence (CL) spectra was explained by the difference of growth mode before and after the coalescence of stripes. It was found that the emission intensity related crystal defects is drastically decreased in case of selective growth without SiO₂ masks as compared to that obtained with SiO₂ masks.     

宽周期掩膜法HVPE侧向外延自支撑GaN的研究

GaN膜在传统生长过程中主要通过异质外延获得,这往往会产生晶格失配和热失配,给GaN带来严重的位错和应力。目前降低位错最广泛的方法是使用侧向外延技术。在这项工作中,首先在蓝宝石基GaN衬底上沉积了一层SiO₂,并用光刻的方法将其制备成高掩膜宽度(窗口宽度20 μm/掩膜宽度280 μm)的宽周期掩膜,再通过氢化物气相外延(HVPE)侧向外延了厚度为325 μm的GaN厚膜,通过胶带可以将其进行剥离形成自支撑衬底。同时通过二维的Wulff结构图研究了GaN生长过程中晶面的变化趋势。宽周期掩膜法对于生长可剥离的低位错密度自支撑GaN有着重大意义。     

Vapor phase growth of GaN using GaN powder sources and thermogravimetric investigations of the evaporating behaviour of the source material

The growth of GaN from the vapor phase is a promising technique for producing both bulk GaN crystals and GaN layers. For establishing a growth method from the vapor phase the source material and reactor setup are of great importance. Highly pure and self synthesized GaN powder was chosen as source material. The evaporation behaviour of the GaN powder was studied by means of thermogravimetry (TG). A vertical growth reactor was set up according to the results of numerical simulations of the temperature distributions and flow patterns. Freely nucleated GaN platelets of some millimetres in length were grown. Furthermore, thin GaN layers were deposited directly on a sapphire substrate. This nucleation layer was successfully overgrown by low pressure solution growth. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

N-type doping of GaN/Si(1 1 1) using Al0.2Ga0.8N/ALN composite buffer layer and Al0.2Ga0.8N/GaN superlattice

The characteristics of Si-doped and undoped GaN/Si(1 1 1) heteroepitaxy with composite buffer layer (CBL) and superlattice are compared and discussed. While as-grown Si-doped GaN/Si(1 1 1) heteroepitaxy shows lower quality compared to undoped GaN, crack-free n-type and undoped GaN with the thickness of 1200 nm were obtained by metalorganic chemical vapor deposition (MOCVD). In order to achieve the crack-free GaN on Si(1 1 1), we have introduced the scheme of multiple buffer layers; composite buffer layer of Al_0.2Ga_0.8N/AlN and superlattice of Al_0.2Ga_0.8N/GaN on 2-in. Si(1 1 1) substrate, simultaneously. The FWHM values of the double-crystal X-ray diffractometry (DCXRD) rocking curves were 823 arcsec and 745 arcsec for n-GaN and undoped GaN/Si(1 1 1) heteroepitaxy, respectively. The average dislocation density on GaN surface was measured as 3.85×10⁹ and 1.32×10⁹ cm⁻² for n-GaN and undoped GaN epitaxy by 2-D images of atomic force microscopy (AFM). Point analysis of photoluminescence (PL) spectra was performed for evaluating the optical properties of the GaN epitaxy. We also implemented PL mapping, which showed the distribution of edge emission peaks onto the 2 inch whole Si(1 1 1) wafers. The average FWHMs of the band edge emission peak was 367.1 and 367.0 nm related with 3.377 and 3.378 eV, respectively, using 325 nm He-Cd laser as an excitation source under room temperature.     

InGaN/GaN微米阵列结构的生长及发光性能研究

采用金属有机化学气相外延技术,在图形化蓝宝石衬底上通过选区外延可控生长了三种不同形貌的InGaN/GaN微米阵列结构,阵列尺寸均为6 μm。其中,六方片状阵列结构以(0001)c面为主,高度为0.6 μm;六棱台状阵列结构包括一个(0001)c面和六个等效的(10-11)半极性面,高度为1.2 μm;六棱锥状阵列结构以(10-11)半极性面为主,高度为5 μm。采用微区光致发光光谱仪对InGaN/GaN微米阵列结构进行发光性能表征,结果表明不同形貌的InGaN/GaN微米阵列结构都可实现多波长发射;阴极荧光光谱结果表明六棱台状InGaN/GaN阵列结构不同晶面位置处发射的波长明显不同,这主要是由于表面迁移效应和横向气相扩散导致各个位置的In组分不同。InGaN/GaN微米阵列结构的成功制备对实现多彩发射和新型光电子器件设计具有重要意义。     

Lateral confined epitaxy of GaN layers on Si substrates

We developed a novel, simple procedure for achieving lateral confined epitaxy (LCE). This procedure enables the growth of uncracked GaN layers on a Si substrate, using a single, continuous metalorganic chemical vapor deposition (MOCVD) run. The epitaxial growth of GaN is confined to mesas, defined by etching into the Si substrate prior to the growth. The LCE-GaN layers exhibit improved morphological and optical properties compared to the plain GaN-on-Si layers grown in the same MOCVD system. By performing a set of LCE growth runs on mesas of varying lateral dimensions, we specified the crack-free range of GaN on Si as 14.0±0.3 μm.     

Selective area growth of GaN nanorods on patterned W/SiO2/Si substrates by RF-MBE

We report on the selective area growth (SAG) of GaN nanorods on Si substrates masked with W or SiO₂ and also on bare Si substrates by RF plasma-assisted molecular beam epitaxy (RF-MBE). The growth of GaN (i.e. irradiation of Ga and RF plasma-activated N₂) on the W mask layer results in the appearance of a ring reflection high-energy electron diffraction (RHEED) pattern coming from α-W. In contrast, broken ring RHEED patterns from GaN nanorods are clearly observed on SiO₂ and Si surfaces. Ex-situ scanning Auger microscopy analysis confirms that no growth of GaN takes place on W. Utilizing this phenomenon, we have demonstrated the SAG of GaN nanorods on Si substrates partly masked with W. We will discuss this phenomenon in terms of the difference in the desorption energy of Ga on W, SiO₂, and Si.