低温MOCVD法沉积的GaN/GaAs(001)薄膜中的孪晶现象

采用同步辐射XRD极图法对低温MOCVD生长的GaN缓冲层薄膜进行了研究.极图研究表明,低温GaN薄膜中除有正常结晶外还存在一次孪晶和二次孪晶.在χ固定为55°时的{111}ψ扫描中发现了异常的Bragg衍射峰,表明GaN/GaAs(001)低温生长中孪晶现象非常明显.GaAs(001)表面上出现的{111}小面极性会在生长初期影响孪晶成核,实验结果表明孪晶更易在{111}B面即N面上成核.     

Twinning in Low-Temperature MOCVD Grown GaN on (001) GaAs Substrate

GaN buffer layers (thickness ～60nm) grown on GaAs(001) by low-temperature MOCVD are investigated by X-ray diffraction pole figure measurements using synchrotron radiation in order to understand the heteroepitaxial growth features of GaN on GaAs(001) substrates.In addition to the epitaxially aligned crystallites,their corresponding twins of the first and the second order are found in the Xray diffraction pole figures.Moreover,{111} φ scans with χ at 55°reveal the abnormal distribution of Bragg diffractions.The extra intensity maxima in the pole figures shows that the process of twinning plays a dominating role during the growth process.It is suggested that the polarity of {111} facets emerged on (001) surface will affect the growth twin nucleation at the initial stages of GaN growth on GaAs(001) substrates.It is proposed that twinning is prone to occurring on {111}B,Nterminated facets.     

AlGaN缓冲层结构对Si基GaN材料性能的影响

Si衬底与GaN之间较大的晶格失配和热失配引起的张应力使GaN外延层极易产生裂纹,如何补偿GaN所受到的张应力是进行Si基GaN外延生长面临的首要问题.采用金属有机化合物化学气相沉积(MOCVD)技术在4英寸(1英寸=2.54 cm)Si (111)衬底上制备了GaN外延材料并研究了不同AlGaN缓冲层结构对Si基GaN外延材料性能的影响,并采用高分辨X射线衍射仪(HRXRD)、原子力显微镜(AFM)、喇曼光谱以及光学显微镜对制备的GaN材料的性能进行了表征.采用3层A1GaN缓冲层结构制备了表面光亮、无裂纹的GaN外延材料,其(002)晶面半高宽为428 arcsec,表面粗糙度为0.194 nm.结果表明,采用3层A1GaN缓冲层结构可以有效地降低GaN材料的张应力和位错密度,进而遏制表面裂纹的出现,提高晶体质量.     

The role of the low temperature buffer layer and layer thickness in the optimization of OMVPE growth of GaN on sapphire

In agreement with previous work,¹² a thin, low temperature GaN buffer layer, that is used to initiate OMVPE growth of GaN growth on sapphire, is shown to play a critical role in determining the surface morphology of the main GaN epilayer. X-ray analysis shows that the mosaicity of the main GaN epilayer continues to improve even after several μm of epitaxy. This continuing improvement in crystal perfection correlates with an improvement in Hall mobility for thicker samples. So far, we have obtained a maximum mobility of 600 cm²/V-s in a 6 μm GaN epilayer. Atomic force microscopy (AFM) analysis of the buffer layer and x-ray analysis of the main epilayer lead us to conclude that the both of these effects reflect the degree of coherence in the main GaN epitaxial layer. These results are consistent with the growth model presented by Hiramatsu et al., however, our AFM data indicates that for GaN buffer layers partial coherence can be achieved during the low temperature growth stage.     

Comparative Study on MOCVD Growth of a-Plane GaN Films on r-Plane Sapphire Substrates Using GaN, AlGaN, and AlN Buffer Layers

In this work, we have comparatively investigated the effects of the GaN, AlGaN, and AlN low-temperature buffer layers (BL) on the crystal quality of a-plane GaN thin films grown on r-plane sapphire substrates. Scanning electron microscopy images of the a-plane GaN epilayers show that using an AlGaN BL can significantly reduce the density of surface pits. The full-width at half-maximum values of the x-ray rocking curve (XRC) are 0.19°, 0.36°, and 0.48° for the films grown using Al_0.15Ga_0.85N, GaN, and AlN BLs, respectively, indicating that an AlGaN BL can effectively reduce the mosaicity of the films. Room-temperature photoluminescence shows that the AlGaN BL results in lower impurity incorporation in the subsequent a-plane GaN films, as compared with the case of GaN and AlN BLs. The higher crystal quality of a-plane GaN films produced by the Al_0.15Ga_0.85N BL could be due to improvement of BL quality by reducing the lattice mismatch between the BL and r-sapphire substrates, while still keeping the lattice mismatch between the BL and epitaxial a-plane GaN films relatively small.     

Metalorganic chemical vapor deposition growth of high optical quality and high mobility GaN

Hall mobilities as high as 702 and 1230 cm²/Vs at 300 and 160K along with low dislocation densities of 4.0 × 10⁸ cm^-2 have been achieved in GaN films grown on sapphire by metalorganic chemical vapor deposition. High growth temperatures have been established to be crucial for optimal GaN film quality. Photoluminescence measurements revealed a low intensity of the deep defect band around 550 nm in films grown under optimized conditions.     

SiC衬底AlN缓冲层的应变对GaN外延层质量的影响

在3英寸(1英寸=2.54 cm)SiC衬底上采用金属有机物化学气相沉积(MOCVD)法生长GaN外延材料。研究了AlN缓冲层的应变状态对GaN外延层应变状态和质量的影响。使用原子力显微镜和高分辨率X射线双晶衍射仪观察样品表面形貌,表征外延材料质量的变化,使用高分辨喇曼光谱仪观察外延材料应力的变化,提出了基于外延生长的应变变化模型。实验表明,GaN外延层的张应变随着AlN缓冲层应变状态的由压变张逐渐减小,随着GaN张应力的逐渐减小,GaN位错密度也大大减少,表面形貌也逐渐变好。     

High-Quality GaN heteroepitaxial films grown by metalorganic chemical vapor deposition

In this paper, we describe the growth and characterization of high-quality GaN heteroepitaxial films grown on basal-plane sapphire substrates using metalorganic chemical vapor deposition. The quality of these films is analyzed by a variety of methods, including high-resolution x-ray diffraction, optical transmission spectroscopy, transmission electron microscopy (TEM), room temperature photoluminescence, and room-temperature Hall measurements. The x-ray diffraction full width at half maximum value of ΔΘ ～37 arc s is the narrowest reported to date for any III-V nitride film on any substrate. The x-ray rocking curves for ～0.48 μm thick GaN/Al₂O₃ heteroepitaxial layers exhibit Pendellösung fringes, indicating that even relatively thin films can be of high quality. High-resolution TEM lattice images further attest to the excellent structural quality, showing the films to be completely free of stacking faults. Furthermore, no evidence of columnar growth is observed.     

Direct growth of CdTe on (100), (211), and (111) Si by metalorganic chemical vapor deposition

CdTe epilayers were grown directly on (100), (211), and (111) silicon substrates by metalorganic chemical vapor deposition (MOCVD). The crystallinity and the growth orientation of the CdTe film were dependent on the surface treatment of the Si substrate. The surface treatment consisted of exposure of the Si surface to diethyltelluride (DETe) at temperatures over 600°C prior to CdTe growth. Direct growth of CdTe on (100) Si produced polycrystalline films whereas (lll)B single crystals grew when Si was exposed to DETe prior to CdTe growth. On (211) Si, single crystal films with (133)A orientation was obtained when grown directly; but produced films with (211)A orientation when the Si surface was exposed to DETe. On the other hand, only (lll)A CdTe films were possible on (111) Si, both with and without Te source exposure, although twinning was increased after exposure. The results indicate that the exposure to a Te-source changes the initial growth stage significantly, except for the growth on (111) Si. We propose a model in which a Te atom replaces a Si atom that is bound to two Si atoms.     

Nucleation and growth behavior for GaN grown on (0001) sapphire via multistep growth approach

Formation and coalescence of GaN truncated three dimensional islands (TTIs) on (0001) sapphire are observed during growth of GaN using a close spaced metalorganic chemical vapor deposition reactor. To encourage formation of TTIs to occur uniformly over the buffer layer, growth conditions are chosen under which thermal desorption and/or mass transport of the buffer layer can be suppressed. During coalescence of TTIs, growth conditions that favor higher desorption of species on the GaN (0001) surface and incorporation on other planes are beneficial. Therefore, changing the growth conditions as the growth mode changes is effective to obtain both good crystallinity and flat surface morphology.     

Si基GaN薄膜的制备方法及结构表征

分别采用射频磁控溅射、热壁化学气相沉积(CVD)、电泳沉积法制备GaN薄膜。利用扫描电镜(SEM)、荧光光谱仪对样品进行结构、形貌和发光特性的分析比较。射频磁控溅射方法中,把SiC中间层沉淀到Si衬底上,目的是为了缓冲由GaN外延层和Si衬底的晶格失配造成的应力。结果证实了SiC中间层提高了GaN薄膜的质量。热壁化学气相沉积法制备GaN晶体膜时,选择H2作反应气体兼载体,有利于GaN膜的形成。电泳沉积法显示所得样品为六方纤锌矿结构的GaN多晶薄膜。结果表明:溅射法制备的GaN薄膜结晶效果好;CVD法制备时GaN薄膜应用范围广;电泳沉积法操作方便、简单易行。     

Structural study of GaN grown on (001) GaAs by organometallic vapor phase epitaxy

Detailed transmission electron microscope (TEM) and transmission electron diffraction (TED) examination has been performed on organometallic vapor phase epitaxial GaN layers grown on (001) GaAs substrate to investigate microstructures and phase stability. TED and TEM results exhibit the occurrence of a mixed phase of GaN. The wurtzite (α) phase grains are embedded in the zinc-blende (β) phase matrix. It is shown that there are two types of the wurtzite GaN phase, namely, the epitaxial wurtzite and the tilted wurtzite. The tilted wurtzite grains are rotated some degrees ranging from ∼5° to ∼35° regarding the GaAs substrate. A simple model is presented to describe the occurrence of the mixed phases and the two types of the wurtzite phase.     

Structural and Optical Properties of ZnO Nanotips Grown on GaN Using Metalorganic Chemical Vapor Deposition

ZnO nanotips are grown on epitaxial GaN/c-sapphire templates by metalorganic chemical vapor deposition. X-ray diffraction (XRD) studies indicate that the epitaxial relationship between ZnO nanotips and the GaN layer is (0002)ZnO||(0002)GaN and (101̄0)ZnO||(101̄0)GaN. Temperature-dependent photoluminescence (PL) spectra have been measured. Sharp free exciton and donor-bound exciton peaks are observed at 4.4 K with photon energies of 3.380 eV, 3.369 eV, and 3.364 eV, confirming high optical quality of ZnO nanotips. Free exciton emission dominates at temperatures above 50 K. The thermal dissociation of these bound excitons forms free excitons and neutral donors. The thermal activation energies of the bound excitons at 3.369 eV and 3.364 eV are 11 meV and 16 meV, respectively. Temperature-dependent free A exciton peak emission is fitted to the Varshni’s equation to study the variation of energy bandgap versus temperature.     

Epitaxial growth of cubic gan on (111) GaAs by metalorganic chemical vapor deposition

We are reporting the first comprehensive investigation of the structural properties of cubic GaN grown on (111) GaAs substrates by low-pressure metalorganic chemical vapor deposition. The minimum full width at half maximum (FWHM) of the x-ray diffraction (XRD) peak of (111) GaN was found to be ∼12 min. The use of low temperature GaN buffers helps to reduce the FWHM of the XRD. Cross-sectional transmission electron microscopy (XTEM) revealed the presence of columnar structures in the GaN film with widths of the order of 500A. Selected area electron diffraction (SAD) patterns at the interface confirmed that cubic (111) GaN was grown in-plane with the (111) GaAs substrate. Highresolution transmission electron microscopy (HRTEM) showed that the interface characteristics of GaN on (111)A GaAs substrate were better than those of the GaN on (lll)B GaAs substrate.     

Mass spectroscopy study of GaN metalorganic chemical vapor deposition

Metalorganic chemical vapor phase deposition of GaN on (100) GaAs has been studied using mass spectroscopy. With increasing substrate temperature, the amount of decomposed trimethylgallium (TMGa) was observed to increase exponentially with a characteristic energy of 1.5 eV. The presence of NH₃ was found to suppress the production of CH₃ in the gas phase. This implies that CH₃ of TMGa reacts with the hydrogen atom of NH₃, forming CH₄ as a main gas product. Studies of nitrogen evaporation from the growth surface when TMGa flow was off lead to the conclusion that increased growth rate could result in decreased background electron concentration due to nitrogen vacancy. The presence of NH₃ significantly promotes the decomposition of TMGa. Desorption of excess Ga atoms from the growth surface at low NH₃ flow rates takes place as suggested by the increased ratio of peak intensity of Ga (m/e = 69) to that of DMGa ((CH₃)₂Ga, m/e- 99) with decreasing NH₃ flow rate.     

Effect of Growth Time on Properties of GaN Micro-grains Grown by Hot-wall CVD Method

GaN microcrystalline grains were grown by hot- wall chemical vapor deposition on Si (111) substrate. These grains with diameters of 2- 4 tim were detected by scanning electron microscopy. X-ray diffraction, Fourier transformation infrared transmission spectroscopy and photoluminescence were used to analyze the structure, composition and the optical properties of the samples. The results show that the microcrystalline grains are hexagonal wurtzite GaN, and the property of the grains was greatly affected by the growth time.     

Properties of GaN epitaxial layers grown at high growth rates by metalorganic chemical vapor deposition

GaN epitaxial layers were grown at high growth rates by increasing the input trimethylgallium (TMG) flow rate while keeping the NH₃ flow rate constant in metalorganic chemical vapor deposition. The electrical and optical properties of the grown layers have been investigated. With the increasing TMG flow rate, the electron concentration tends to decrease gradually and the Hall mobility decreases significantly. Considering the temperature dependence of the Hall mobility and the correlation between the Hall mobility and the electron concentration, it has been indicated that the more acceptors are incorporated and consequently the compensation ratio becomes higher with increasing the TMG flow rate. Photoluminescence measurements have revealed that the intensity ratio of the bound exciton emission to the 2.2 eV band emission, which is assumed to correlate to carbon or Ga vacancies, was decreased with increasing the TMG flow rate. It might be reasonable to take a lot of acceptor incorporation to explain the degradation of the electrical and optical properties in the samples grown at high growth rates by increasing the TMG flow rate.     

退火对Ge掺杂SiO2薄膜的影响

用等离子体增强化学气相淀积制备了Ge掺杂SiO2薄膜,并对薄膜进行了不同温度的退火处理。采用棱镜耦合仪、原子力显微镜和傅里叶变换红外光谱分析技术研究了不同退火温度对Ge掺杂SiO2薄膜性质的影响。通过1 100℃退火处理后,正的折射率变化量和负的体积变化量随着GeH4流量增加而增大,Ge-O-Ge键增多;而通过900℃退火处理后,折射率没有随着GeH4流量增加而增大;薄膜的表面粗糙度随着退火温度升高而降低。研究结果表明,SiO2薄膜中Ge掺杂过量,其折射率反常下降;通过1 100℃退火处理后,折射率随着GeH4流量增加而增大,折射率的增大主要是由于薄膜密实化和Ge-O-Ge键的形成。     

Poly- and single-crystalline h-GaN grown on SiCN/Si(100) and SiCN/Si(111) substrates by MOCVD

This paper reports the growth of polycrystalline GaN on Si(100) and single-crystalline h-GaN on Si(111) substrates with a single-crystalline SiCN burffer layer by metalorganic chemical vapor deposition (MOCVD). From high-resolution x-ray diffraction (HRXRD) and scanning election microscopy (SEM) analyses, GaN on SiCN/Si(100) is polycrystalline and GaN on SiCN/Si(111) is single-crystalline. From photoluminescence analysis, the energy gaps of h-GaN/SiCN/Si(100) and c-GaN/SiCN/Si(100) are ∼3.4 and ∼3.2 eV at 300 K but shift to 3.5 and 3.3 eV at 15 K, respectively. A model to explain the growth mechanism is also proposed.     

红橙光InGaN/GaN量子阱的结构与光学性质研究

采用金属有机物化学气相沉积(MOCVD)技术生长了具有高In组分InGaN阱层的InGaN/GaN多量子阱(MQW)结构,高分辨X射线衍射(HRXRD)ω-2θ扫描拟合得到阱层In含量28%。比较大的表面粗糙度表明有很大的位错密度。室温下光致荧光(PL)研究发现该量子阱发射可见的红橙光,峰位波长在610 nm附近。变温PL(15～300 K)进一步揭示量子阱在低温下有两个发光机制,对应的发射峰波长分别为538 nm和610 nm。由于In分凝和载流子的局域化导致的载流子动力改变,使得量子阱PL发光峰值随温度增加呈明显的"S"变化趋势。