高阻GaN的MOCVD外延生长

利用金属有机化合物气相沉积(MOCVD)在蓝宝石衬底上生长了高阻GaN薄膜。对GaN成核层生长的反应室压力、生长时间和载气类型对GaN缓冲层电学特性的影响进行了分析。实验结果表明,延长GaN成核层的生长时间,降低成核层生长时的反应室压力,载气由H₂换为N₂都会得到高阻的GaN缓冲层。样品的方块电阻R_s最高为2.49×10¹¹ Ω/□。以高阻GaN样品为衬底制备了AlGaN/AlN/GaN结构HEMT器件,迁移率最高达1 230 cm²/(V·s)。     

GaN基异质结缓冲层漏电分析

通过对GaN基异质结材料C-V特性中耗尽电容的比较,得出AlGaN/GaN异质结缓冲层漏电与成核层的关系.实验结果表明,基于蓝宝石衬底低温GaN成核层和SiC衬底高温AlN成核层的异质结材料比基于蓝宝石衬底低温AlN成核层异质结材料漏电小、背景载流子浓度低.深入分析发现,基于薄成核层的异质结材料在近衬底的GaN缓冲层中具有高浓度的n型GaN导电层,而基于厚成核层的异质结材料的GaN缓冲层则呈高阻特性.GaN缓冲层中的n型导电层是导致器件漏电主要因素之一,适当提高成核层的质量和厚度可有效降低GaN缓冲层的背景载流子浓度,提高GaN缓冲层的高阻特性,抑制缓冲层漏电. 关键词： AlGaN/GaN异质结 GaN缓冲层 漏电 成核层     

Characterization of the N-polar GaN film grown on C-plane sapphire and misoriented C-plane sapphire substrates by MOCVD

Gallium nitride (GaN) thin film of the nitrogen polarity (N-polar) was grown on C-plane sapphire and misoriented C-plane sapphire substrates respectively by metal-organic chemical vapor deposition (MOCVD). The misorientation angle is off-axis from C-plane toward M-plane of the substrates, and the angle is 2° and 4° respectively. The nitrogen polarity was confirmed by examining the images of the scanning electron microscope before and after the wet etching in potassium hydroxide (KOH) solution. The morphology was studied by the optical microscope and atomic force microscope. The crystalline quality was characterized by the x-ray diffraction. The lateral coherence length, the tilt angle, the vertical coherence length, and the vertical lattice-strain were acquired using the pseudo-Voigt function to fit the x-ray diffraction curves and then calculating with four empirical formulae. The lateral coherence length increases with the misorientation angle, because higher step density and shorter distance between adjacent steps can lead to larger lateral coherence length. The tilt angle increases with the misorientation angle, which means that the misoriented substrate can degrade the identity of crystal orientation of the N-polar GaN film. The vertical lattice-strain decreases with the misorientation angle. The vertical coherence length does not change a lot as the misorientation angle increases and this value of all samples is close to the nominal thickness of the N-polar GaN layer. This study helps to understand the influence of the misorientation angle of misoriented C-plane sapphire on the morphology, the crystalline quality, and the microstructure of N-polar GaN films.     

表面预处理对石墨烯上范德瓦耳斯外延生长GaN材料的影响

基于范德瓦耳斯外延生长的氮化镓/石墨烯材料异质生长界面仅靠较弱的范德瓦耳斯力束缚,具有低位错、易剥离等优势,近年来引起了人们的广泛关注.采用NH_3/H_2混合气体对石墨烯表面进行预处理,研究了不同NH_3/H_2比对石墨烯表面形貌、拉曼散射的影响,探讨了石墨烯在NH_3和H_2混合气氛下的表面预处理机制,最后在石墨烯上外延生长了1.6μm厚的GaN薄膜材料.实验结果表明:石墨烯中褶皱处的C原子更容易与气体发生刻蚀反应,刻蚀方向沿着褶皱进行;适当NH_3/H_2比的混合气体对石墨烯进行表面预处理可有效改善石墨烯上GaN材料的晶体质量.本研究提供了一种可有效提高GaN晶体质量的石墨烯表面预处理方法,可为进一步研究二维材料上高质量的GaN外延生长提供参考.     

Optical and structural investigation of a-plane GaN layers on r-plane sapphire with nucleation layer optimization

Nonpolar a-plane GaN epilayers are grown on several r-plane sapphire substrates by metal organic chemical vapour deposition using different nucleation layers:(A) a GaN nucleation layer deposited at low temperature(LT);(B) an AlN nucleation layer deposited at high temperature;or(C) an LT thin AlN nucleation layer with an AlN layer and an AlN/AlGaN superlattice both subsequently deposited at high temperature.The samples have been characterized by Xray diffraction(XRD),atomic force microscopy and photoluminescence.The GaN layers grown using nucleation layers B and C show narrower XRD rocking curves than that using nucleation layer A,indicating a reduction in crystal defect density.Furthermore,the GaN layer grown using nucleation layer C exhibits a surface morphology with triangular defect pits eliminated completely.The improved optical property,corresponding to the enhanced crystal quality,is also confirmed by temperature-dependent and excitation power-dependent photoluminescence measurements.     

The effects of sapphire nitridation on GaN growth by metalorganic chemical vapour deposition

In situ optical reflectivity measurements are employed to monitor the GaN epilayer growth process above a low-temperature GaN buffer layer on a c-plane sapphire substrate by metalorganic chemical vapour deposition. It is found that the lateral growth of the GaN islands and their coalescence are promoted in the initial growth stage if optimized nitridation time and temperature are selected when the substrate is pre-exposed to ammonia. As confirmed by atomic force microscopy observations, the quality of the GaN epilayers is closely dependent on the surface morphology of the nitridated buffer layer, especially grain size and nucleation density.     

界面形核时间对GaN薄膜晶体质量的影响

利用金属有机化学气相沉积技术系统研究了界面形核时间对c面蓝宝石衬底上外延生长GaN薄膜晶体质量的影响机理. 用原子力显微镜、扫描电子显微镜、高分辨X射线衍射仪以及光致发光光谱仪表征材料的晶体质量以及光学性质. 随着形核时间的延长, 退火后形成的形核岛密度减小、尺寸增大、均匀性变差, 使得形核岛合并过程中产生的界面数量先减小后增大, 导致GaN外延层的螺位错和刃位错密度先减小后增大, 这与室温光致发光光谱中得到的带边发光峰与黄带发光峰的比值先增大后降低一致. 研究结果表明, 外延生长过程中, 界面形核时间会对GaN薄膜中的位错演变施加巨大影响, 从而导致GaN外延层的晶体质量以及光学性质的差异.     

Polar Dependence of Threading Dislocation Density in GaN Films Grown by Metal-Organic Chemical Vapor Deposition

We investigate the threading dislocation(TD) density in N-polar and Ga-polar GaN films grown on sapphire substrates by metal-organic chemical vapor deposition.X-ray diffraction results reveal that the proportion of screw type TDs in N-polar GaN is much larger and the proportion of edge type TDs is much smaller than that in Ga-polar.Transmission electron microscope results show that the interface between the AlN nucleation layer and the GaN layer in N-polar films is smoother than that in Ga-polar films,which suggests different growth modes of GaN.This observation explains the encountered difference in screw and edge TD density.A model is proposed to explain this phenomenon.     

N极性GaN薄膜的MOCVD外延生长

采用MOCVD技术在c面蓝宝石衬底上外延制备了N极性GaN薄膜。通过KOH腐蚀的方法判定了GaN外延薄膜的极性。通过X射线双晶衍射(XRD)摇摆曲线和光致荧光(PL)谱测试研究了成核层生长时间对N极性GaN薄膜晶体质量和发光性能的影响。研究结果表明,成核层生长时间为300 s时,N极性GaN薄膜样品的位错密度最低,发光性能最好。采用拉曼(Raman)光谱对样品的应变状态进行了分析。     

Effects of AlN nucleation layer thickness on crystal quality of AlN grown by plasma-assisted molecular beam epitaxy

In this paper,the effects of thickness of AlN nucleation layer grown at high temperature on AlN epi-layer crystalline quality are investigated.Crack-free AlN samples with various nucleation thicknesses are grown on sapphire substrates by plasma-assisted molecular beam epitaxy.The AlN crystalline quality is analysed by transmission electron microscope and x-ray diffraction (XRD) rocking curves in both (002) and (102) planes.The surface profiles of nucleation layer with different thicknesses after in-situ annealing are also analysed by atomic force microscope.A critical nucleation thickness for realising high quality AlN films is found.When the nucleation thickness is above a certain value,the (102) XRD full width at half maximum (FWHM) of AlN bulk increases with nucleation thickness increasing,whereas the (002) XRD FWHM shows an opposite trend.These phenomena can be attributed to the characteristics of nucleation islands and the evolution of crystal grains during AlN main layer growth.     

Investigation of GaN layer grown on different low misoriented sapphire by MOCVD

GaN layer on c-plane misoriented sapphire, grown by metal organic chemical vapor deposition, has been studied. It was observed that the random and non-uniform distribution of the step was caused by the step reconstruction for GaN grown on 0° sapphire by atomic force microscopy. The image quality parameter analysis of electron back-scatter diffraction indicated that the strains were reduced for GaN grown on 0.2° and 0.3° sapphire, and optical and electrical properties were improved. The electroluminescence intensity of LED grown on 0.2° and 0.3° sapphire was 2 times as that of 0° sapphire.     

一种外延生长高质量GaN薄膜的新方法

采用化学方法腐蚀c-面蓝宝石衬底，以形成一定的图案；利用LP-MOCVD在经过表面处理的蓝宝石衬底上以及常规c-面蓝宝石衬底上外延生长GaN薄膜.采用高分辨率双晶X射线衍射(DCXRD)、三维视频光学显微镜(OM)、扫描电子显微镜(SEM)和原子力显微镜(AFM)进行分析，结果表明，在经过表面处理形成一定图案的蓝宝石衬底上外延生长的GaN薄膜明显优于在常规蓝宝石衬底上外延生长的GaN薄膜，其(0002)面上的XRD FWHM为208.80弧秒，(1012)面上的为320.76弧秒.同时，此方法也克服了传统 关键词： 表面处理 MOCVD 横向外延生长 GaN薄膜     

Growth of nonpolar a-plane GaN on nano-patterned r-plane sapphire substrates

Sapphire substrates were nano-patterned by inductive coupled plasma etching process. Nonpolar a-plane GaN films were grown on planar and nano-patterned r-plane sapphire substrates by metal organic chemical vapor deposition. The anisotropic characteristic and the crystalline quality of the a-plane GaN films were studied through XRD rocking curves. The cross section and surface morphologies of the a-plane GaN films were studied using SEM and AFM measurements, respectively. The crystal quality and surface flatness of the nonpolar a-plane GaN were greatly improved through the usage of the nano-patterned r-plane sapphire substrates.     

Performance improvement of InGaN/GaN multiple quantum well visible-light photodiodes by optimizing TEGa flow

The performance of an InGaN/GaN multiple quantum well(MQW) based visible-light Schottky photodiode(PD)is improved by optimizing the source flow of TEGa during In Ga N QW growth. The samples with five-pair InGaN/GaN MQWs are grown on sapphire substrates by metal organic chemical vapor deposition. From the fabricated Schottky-barrier PDs, it is found that the smaller the TEGa flow, the lower the reverse-bias leakage is. The photocurrent can also be enhanced by depositing the In GaN QWs with using lower TEGa flow. A high responsivity of 1.94 A/W is obtained at 470 nm and -3-V bias in the PD grown with optimized TEGa flow. Analysis results show that the lower TEGa flow used for depositing In Ga N may lead to superior crystalline quality with improved InGaN/GaN interface, and less structural defects related non-radiative recombination centers formed in the MQWs.     

GaP layers grown on GaN with and without buffer layers

The growth of GaP layer on GaN with and without buffer layers by metal-organic chemical vapour deposition (MOCVD) has been studied. Results indicate that the GaP low temperature buffer layer can provide a high density of nucleation sites for high temperature (HT) GaP growth. These sites can promote the two-dimensional (2D) growth of HT GaP and reduce the surface roughness. A GaP single crystal layer grown at 680°C is obtained using a 40-nm thick GaP buffer layer. The full-width at half-maximum (FWHM) of the (111) plane of GaP layer, measured by DCXRD, is 560 arcsec. The GaP layer grown on GaN without low temperature GaP buffer layer shows a rougher surface. However, the FWHM of the (111) plane is 408 arcsec, which is the indication of better crystal quality for the GaP layer grown on GaN without a low temperature buffer layer. Because it provides less nucleation sites grown at high growth temperature, the three-dimensional (3D) growth is prolonged. The crystalline quality of GaP is lightly improved when the surface of GaN substrate is pretreated by PH3 , while it turned to be polycrystalline when the substrate is pretreated by TEGa.     

Effect of growth pressure on the morphology evolution and doping characteristics in nonpolar a-plane GaN

Nonpolar a-plane GaN layers grown on r-plane sapphire substrates were examined by using a two-step growth process. The higher initial growth pressure for the nucleation layer resulted in the improved crystalline quality with lower density of both threading dislocations and basal stacking faults. This was attributed to the higher degree of initial roughening and recovery time via a growth mode transition from three-dimensional (3D) to quasi two-dimensional (2D) lateral growth. Using Hall-effect measurements, the overgrown Si doped GaN layers grown with higher initial growth pressure were found to have higher mobility. The scattering mechanism due to the dislocations was dominant especially at low temperature (<200 K) for the lower initial growth pressure, which was insignificant for the higher initial growth pressure. The temperature-dependent Hall-effect measurements for the Mg doped GaN with a higher initial growth pressure yielded the activation energy and the acceptor concentration to be 128 meV and 1.2 × 10¹⁹ cm⁻³, respectively, corresponding to about 3.6% of activation at room temperature. Two-step growth scheme with a higher initial growth pressure is suggested as a potential method to improve the performance of nonpolar a-plane GaN based devices.     

Characterization of free-standing GaN substrate grown through hydride vapor phase epitaxy with a TiN interlayer

Large-scale GaN free-standing substrate was obtained by hydride vapor phase epitaxy directly on sapphire with porous network interlayer. The bottom surface N-face and top surface Ga-face showed great difference in anti-etching and optical properties. The variation of optical and structure characteristics were also microscopically identified using spatially resolved cathodoluminescence and micro-Raman spectroscopy in cross-section of the GaN substrate. Three different regions were separated according to luminescent intensity along the film growth orientation. Some tapered inversion domains with high free carrier concentration of 5 × 10¹⁹ cm⁻³ protruded up to the surface forming the hexagonal pits. The dark region of upper layer showed good crystalline quality with narrow donor bound exciton peak and low free carrier concentration. Unlike the exponential dependence of the strain distribution, the free-standing GaN substrate revealed a gradual increase of the strain mainly within the near N-polar side region with a thickness of about 50 μm, then almost kept constant to the top surface.     

The influence of nitridation time on the structural properties of GaN grown on Si (111) substrate

In the present paper, the effect of in-situ substrate nitridation time on crystalline quality of GaN films grown on Si (111) substrates by metal organic chemical vapor deposition (MOCVD) were investigated. A thin buffer layer of silicon nitride (SiN _x ) with various thicknesses was achieved through the nitridation of substrate at different nitiridation times ranging from 0 to 660 s. The structural characteristics, such as dislocation densities, correlation lengths of columnar crystallites, the tilt and twist of the mosaic structure, and the angles of rotational disorder, were all studied in detail by using a planar and cross-sectional view of high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (HRXRD) performed at different scattering geometries. It was found that the dislocation densities, lateral coherence lengths, vertical coherence lengths, and the tilt and twist of mosaic blocks in GaN films monotonically varies with the nitridation time. The experimental findings showed that the nitridation times had more influence on edge dislocation densities than the screw type.     

磁控反应溅射AlN缓冲层对GaN基LED器件性能的影响

以直流磁控反应溅射法(RMS)在图形化蓝宝石衬底上制备的AlN薄膜作为缓冲层,采用金属有机化学气相沉积法(MOCVD)外延生长了GaN基LED。与MOCVD生长的低温GaN缓冲层相比,RMS制备的AlN缓冲层具有表面更平整、颗粒更小的形核岛,有利于促进GaN外延的横向生长,减少了形核岛合并时的界面数量和高度差异,降低了缺陷和位错产生的几率。研究结果表明,溅射AlN缓冲层取代传统低温GaN缓冲层后,外延生长的GaN材料具有更高的晶体质量,LED器件在亮度、漏电和抗静电能力等光电特性上均有明显提升。     

Properties of GaN on different polarity buffer layers by hydride vapour phase epitaxy

This paper reports on N-, mixed-, and Ga-polarity buffer layers are grown by molecular beam epitaxy (MBE) on sapphire (0001) substrates, with the GaN thicker films grown on the buffer layer with different polarity by hydride vapour epitaxy technique (HVPE). The surface morphology, structural and optical properties of these HVPE-GaN epilayers are characterized by wet chemical etching, scanning electron microscope, x-ray diffraction, and photoluminescence spectrum respectively. It finds that the N-polarity film is unstable against the higher growth temperature and wet chemical etching, while that of GaN polarity one is stable. The results indicate that the crystalline quality of HVPE-GaN epilayers depends on the polarity of buffer layers.