AlN/蓝宝石模板上生长的GaN研究

研究了在分子束外延制备的AlN/蓝宝石模板上采用金属有机物化学气相外延生长的非故意掺杂GaN的材料性质.采用X射线衍射(XRD)、透射电镜(TEM)和原子力显微镜研究了AlN模板的晶体质量和表面相貌对GaN的影响.结果表明,当AlN的表面粗糙度较小时,尽管AlN模板的位错密度较高((102)面XRD ω扫描半高全宽900—1500 arcsec),但生长得到的GaN依然具有和在蓝宝石衬底上采用"二步法"生长的GaN可比拟的晶体质量((002)面XRD ω扫描半高全宽200—30 关键词： 氮化镓 氮化铝 金属有机物化学气相外延     

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.     

氮化铝单晶薄膜的ECR PEMOCVD低温生长研究

采用电子回旋共振等离子体增强金属有机物化学气相沉积（ECR－PEMOCVD）技术，在c轴取向的蓝宝石即α Al2O3（0001）衬底上，以氮化镓（GaN）缓冲层和外延层作为初始层，分别以高纯氮气（N2）和三甲基铝(TMAl)为氮源和铝源低温生长氮化铝（AlN）薄膜.并利用反射高能电子衍射（RHEED）、原子力显微镜（AFM）和x射线衍射（XRD）等测量结果，研究了氢等离子体清洗、氮化和GaN初始层对六方AlN外延层质量的影响，从而获得解理性与α Al2O3衬底一致的六方相AlN单晶薄膜，其XRD半高宽为1 关键词： AlN 氢等离子体清洗 氮化 GaN     

Effect of high-temperature buffer thickness on quality of AlN epilayer grown on sapphire substrate by metalorganic chemical vapor deposition

The effect of an initially grown high-temperature AlN buffer (HT-AlN) layer's thickness on the quality of an AlN epilayer grown on sapphire substrate by metalorganic chemical vapor deposition (MOCVD) in a two-step growth process is investigated. The characteristics of AlN epilayers are analyzed by using triple-axis crystal X-ray diffraction (XRD) and atomic force microscopy (AFM). It is shown that the crystal quality of the AlN epilayer is closely related to its correlation length. The correlation length is determined by the thickness of the initially grown HT-AlN buffer layer. We find that the optimal HT-AlN buffer thickness for obtaining a high-quality AlN epilayer grown on sapphire substrate is about 20 nm.     

国产SiC衬底上利用AIN缓冲层生长高质量GaN外延薄膜

采用高温AlN作为缓冲层在国产SiC衬底上利用金属有机物化学气相外延技术生长GaN外延薄膜.通过优化AlN缓冲层的生长参数得到了高质量的GaN外延薄膜,其对称(0002)面和非对称(1012)面X射线衍射摇摆曲线的半峰宽分别达到130 arcsec和252 arcsec,这是目前报道的在国产SiC衬底上生长GaN最好的...     

MOCVD生长Si衬底上HT-AlN缓冲层低生长压力对GaN薄膜的影响

采用金属有机化学气相沉积（MOCVD）技术在Si（111）衬底上外延GaN薄膜,对高温AlN（HT-AlN）缓冲层在小范围内低生长压力（6.7~16.6 kPa）条件下对GaN薄膜特性的影响进行了研究。研究结果表明GaN外延层的表面形貌、结构和光学性质对HT-AlN缓冲层的生长压力有很强的的依赖关系。增加HT-AlN缓冲层的生长压力,GaN薄膜的光学和形貌特性均有明显改善,当HT-AlN缓冲层的生长压力为13.3 kPa时,得到无裂纹的GaN薄膜,其（002）和（102）面的X射线衍射峰值半高宽分别为735 arcsec和778 arcsec,由拉曼光谱计算得到的张应力为0.437 GPa,原子力显微镜（AFM）观测到表面粗糙度为1.57 nm。     

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.     

Fabrication of piezoelectric AlN thin film for FBARs

This paper focuses on the fabrication of film bulk acoustic-wave resonator (FBAR) comprising an aluminum nitride (AlN) piezoelectric thin film sandwiched between two metal electrodes and located on a silicon substrate with a low-stress silicon nitride (Si₃N₄) support membrane for high frequency wireless applications, and analyzes the optimization of the thin AlN film deposition parameters on Mo electrodes using the reactive RF magnetron sputter system. Several critical parameters of the sputtering process such as RF power and Ar/N₂ flow rate ratio were studied to clarify their effects on different electrodes characteristics of the AlN films. The experiment indicated that the process for Mo electrode was easier compared with that of the Pt/Ti or Au/Cr bi-layer electrode as it entailed only one photo resist and metal deposition step. Besides, Pt/Ti or Au/Cr electrodes reduced the resonance frequency due to their high mass density and low bulk acoustic velocity. Compared with the case of the Al bottom electrode, there is no evident amorphous layer between the Mo bottom electrode and the deposited AlN film. The characteristics of the FBAR devices depend not only upon the thickness and quality of the AlN film, but also upon the thickness of the top electrode and the materials used. The results indicate that decreasing the thickness of either the AlN film or the top electrode increases the resonance frequency. This suggests the potential of tuning the performance of the FBAR device by carefully controlling AlN film thickness. Besides, increasing either the thickness of the AlN film or higher RF power has improved a stronger c-axis orientation and tended to promote a narrower rocking curve full-width at half-maximum (FWHM), but increased both the grain size and the surface roughness. An FBAR device fabricated under optimal AlN deposition parameters has demonstrated the effective electromechanical coupling coefficient (k _eff²) and the quality factor (Q _{f x} ) are about 1.5% and 332, respectively.     

The effect of low temperature AlN interlayers on the growth of GaN epilayer on Si (111) by MOCVD

Low temperature (LT) AlN interlayers were used to effectively reduce the tension stress and micro-cracks on the surface of the GaN epilayer grown on Si (111) substrate. Optical Microscopy (OM), Atomic Force Microscopy (AFM), Surface Electron Microscopy (SEM) and X-Ray Diffraction (XRD) were employed to characterize these samples grown by metal-organic chemical vapor deposition (MOCVD). In addition, wet etching method was used to evaluate the defect of the GaN epilayer. The results demonstrate that the morphology and crystalline properties of the GaN epilayer strongly depend on the thickness, interlayer number and growth temperature of the LT AlN interlayer. With the optimized LT AlN interlayer structures, high quality GaN epilayers with a low crack density can be obtained.     

Growth of preferentially-oriented AlN films on amorphous substrate by pulsed laser deposition

Preferentially-oriented aluminum nitride (AlN) films are grown directly on natively-oxidized Si (100) substrate by pulsed laser deposition (PLD) in nitrogen (N₂) environment. The AlN preferential orientation changes from (002) to (100) with increasing N₂ pressure. Such different behaviors are discussed in terms of deposition-rate-dependent preferential orientation, kinetic energy of depositing species and confinement of laser plume. Finally, sample deposited at 0.9 Pa is proved to have the highest (002) peak intensity, the lowest FWHM value, the highest deposition rate and a relatively low RMS roughness (1.138 nm), showing the optimal growth condition for c-axis-oriented AlN growth at this N₂ pressure.     

On the Growth of High-Temperature Epitaxial AlN (AlGaN) Layers on Sapphire Substrates by Ammonia Molecular Beam Epitaxy

The growth of high-temperature AlN and AlGaN layers on (0001) sapphire substrates by ammonia based molecular-beam epitaxy is studied. Factors affecting the formation of inverted domains in high-temperature AlN films are examined. The density of inverted domains is found to correlate with the density of nucleation islands during the initial stages of growth. The denser coverage of a surface by nucleation islands suppresses the formation of inverted domains. It is possible to increase the density of surface coating at the nucleation growth stage by increasing the degree of substrate nitriding, reducing the deposition temperature, and using intense ammonia fluxes during deposition of the initial layers. The kinetic model in the mean field approximation is developed to explain the observed effects of growth parameters on the density of nucleation islands. The growth features of AlN and its structure are taken into account. The obtained results are used to grow AlN/AlGaN layers with improved structural quality. The grown films have a root-mean-square surface roughness of 2 Å and 120 arc s FWHM of X-ray diffraction peaks for the AlN 0002 reflection. The density of inverted domains is decreased to below 10⁵ cm^-2. Improvement in the quality of the AlN films is achieved by using two-step growth and by the application of gallium as a surfactant.     

Influence of AlN Buffer Thickness on GaN Grown on Si(111) by Gas Source Molecular Beam Epitaxy with Ammonia

Hexagonal GaN is grown on a Si(111) substrate with AlN as a buffer layer by gas source molecular beam epitaxy (GSMBE) with ammonia. The thickness of AlN buffer is changed from 9 to 72nm. When the thickness of AlN buffer is 36nm, the surface morphology and crystal quality of GaN is optimal. The in-situ reflection high energy electron diffraction (RHEED) reveals that the transition to a two-dimensional growth mode of AlN is the key to the quality of GaN. However, the thickness of AlN buffer is not so critical to the residual in-plane tensile stress in GaN grown on Si(111) by GSMBE for AlN thickness between 9 to 72nm.     

Engineering of nearly strain-free ZnO films on Si(1 1 1) by tuning AlN buffer thickness

ZnO properties were investigated as a function of AlN buffer layer thickness (0–100 nm) in ZnO/AlN/Si(1 1 1) structures grown by metal organic vapor phase epitaxy. A significant improvement of ZnO film crystallinity by tuning AlN buffer thickness was confirmed by x-ray diffraction, topography and photoluminescence measurements. An optimal AlN buffer layer thickness of 50 nm is defined, which allows for growth of nearly strain-free ZnO films. The presence of free excitons at 10 K suggests high crystal quality for all ZnO samples grown on AlN/Si(1 1 1) templates. The intensities of neutral and ionized donor bound exciton lines are found to correlate with the in-plane and out-of-plane strain in the films, respectively.     

ZnO／AlN／Si（111）薄膜的外延生长和性能研究

用常压金属化学气相沉积法(MOCVD)在Si(111)衬底上制备了马赛克结构ZnO单晶薄膜。引入低温Al N缓冲层以阻止衬底氧化、缓解热失配和晶格失配。薄膜双晶X射线衍射2θ/ω联动扫描只出现了Si(111)、ZnO(000l)及Al N(000l)的衍射峰。ZnO/Al N/Si(111)薄膜C方向晶格常量为0.5195nm,表明在面方向处于张应力状态;其对称(0002)面和斜对称(1012)面的双晶X射线衍ω摇摆曲线半峰全宽分别为460″和1105″;干涉显微镜观察其表面有微裂纹,裂纹密度为20cm-1;3μm×3μm范围的原子力显微镜均方根粗糙度为1.5nm;激光实时监测曲线表明薄膜为准二维生长,生长速率4.3μm/h。低温10K光致发光光谱观察到了薄膜的自由激子、束缚激子发射及它们的声子伴线。所有结果表明,采用金属化学气相沉积法并引入Al N为缓冲层能有效提高Si(111)衬底上ZnO薄膜的质量。     

低温缓冲层对氧化锌薄膜质量的影响

利用金属有机化学气相沉积(MOCVD)法,在Si衬底上外延生长ZnO薄膜。为了改善氧化锌薄膜的质量,首先在Si衬底上生长低温ZnO缓冲层,然后再生长高质量的ZnO薄膜。通过XRD、SEM、光致发光(PL)光谱的实验研究,发现低温ZnO缓冲层可有效降低ZnO薄膜和Si衬底之间的晶格失配以及因热膨胀系数不同引起的晶格畸变。利用低温缓冲层生长的ZnO薄膜的(002)面衍射峰的强度要比直接在Si上生长的ZnO薄膜样品的高,并且衍射峰的半高宽也由0.21°减小到0.18°,同时有低温缓冲层的样品室温下的光致发光峰也有了明显的增高。这说明利用低温缓冲层生长的ZnO薄膜的结晶质量和光学性质都得到了明显改善。     

Structure and mechanical properties of Al/AlN multilayer with different AlN layer thickness

Nanometer scale Al/AlN multilayers have been prepared by dc magnetron sputtering technique with a columnar target. A set of Al/AlN multilayers with the Al layer thickness of 2.9 nm and the AlN layer thickness variation from 1.13 to 6.81 nm were determined. Low angle X-ray diffraction (LAXRD) was used to analyze the layered structure of multilayers. The phase structure of the coatings was investigated with grazing angle XRD (GAXRD). Mechanical properties of these multilayers were thoroughly studied using a nanoindentation and ball-on-disk micro-tribometer. It was found that the multilayer hardness and reduced modulus showed no strong dependence on the AlN layer thickness. Al2.9 nm/AlN1.13 nm multilayer had more excellent tribological properties than single layers and other proportion multilayers with a lowest friction coefficient of 0.15. And the tribological properties of all the multilayers are superior to the AlN single layer.     

Low‐temperature growth of high quality AlN films on carbon face 6H‐SiC

AlN films have been grown on atomically flat carbon face 6H‐SiC (000 ) substrates by pulsed laser deposition and their structural properties have been investigated. In‐situ reflection high‐energy electron diffraction observations have revealed that growth of AlN at 710 °C proceeds in a Stranski–Krastanov mode, while typical layer‐by‐layer growth occurs at room temperature (RT) with atomically flat surfaces. It has been revealed that the crystalline quality of the AlN film is dramatically improved by the reduction in growth temperature down to RT and the full width at half maximum values in the X‐ray rocking curves for 0004 and 10 2 diffractions of the RT‐grown AlN film are 0.05° and 0.07°, respectively. X‐ray reciprocal space mapping has revealed that the introduction of misfit dislocations is suppressed in the case of RT growth, which is probably responsible for the improvement in crystalline quality. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characterization of thick HVPE GaN films

The morphology of the top surface for HVPE GaN layers grown on a MOCVD GaN template with a thin LT-AlN interlayer was investigated. This surface is characterized by the formation of numerous hillocks associated with screw dislocations or nanopipes. Their size is large and may reach more than 1 mm. The rocking curves of the 002 and 102 reflections correspond to a relaxed layer. The HREM images of the as-deposited and annealed interlayers show a perfect atomic structure with a very abrupt AlN/HVPE GaN interface. Thus, the deposition of the LT-AlN layer has promoted the growth of an HVPE layer with an excellent crystalline quality.     

Effect of double AlN buffer layer on the qualities of GaN films grown by radio-frequency molecular beam epitaxy

This paper reports that the GaN thin films with Ga-polarity and high quality were grown by radio-frequency molecular beam epitaxy on sapphire （0001） substrate with a double A1N buffer layer. The buffer layer consists of a high-temperature （HT） A1N layer and a low-temperature （LT） A1N layer grown at 800℃ and 600℃, respectively. It is demonstrated that the HT-A1N layer can result in the growth of GaN epilayer in Ga-polarity and the LT-A1N layer is helpful for the improvement of the epilayer quality. It is observed that the carrier mobility of the GaN epilayer increases from 458 to 858cm^2/V.s at room temperature when the thickness of LT-A1N layer varies from 0 to 20nm. The full width at half maximum of x-ray rocking curves also demonstrates a substantial improvement in the quality of GaN epilavers by the utilization of LT-A1N layer.     

Characteristics of GaN epilayer grown on Al2O3 with AlN buffer layer by molecular beam epitaxy

Double crystal rocking curve (DCRC), atomic force microscopy (AFM), scanning electron microscopy (SEM), and photoluminescence (PL) measurements on GaN epilayers grown with various thicknesses (3.4, 8.5, 17, 34, and 51 nm) of the AlN buffer layer were carried out to investigate the surface, the structural, and the optical properties of the GaN epilayers. The results of the DCRC, AFM, SEM, and PL measurements showed that the GaN epilayer grown on a 3.4 nm AlN buffer layer had the best quality. These results indicate that GaN active layers grown on 3.4 nm AlN buffer layers hold promise for potential applications in optoelectronic devices.