Polarity control in MBE growth of III-nitrides,and its device application

Until recently, molecular beam epitaxy (MBE) has been behind metalorganic chemical vapor deposition (MOCVD) as a growth technique for III-nitride thin films, due to the lack of nitrogen source powerful enough for the growth in vacuum and the understanding of growth mechanism. We have clarified that the quality of GaN epilayers on sapphire substrates grown by N2 plasma-assisted MBE can be much improved by realizing Ga-polarity growth mode, which enables us to fabricate HFETs using the MBE-grown AIGaN/GaN 2DEG structures. The Ga-polarity growth mode was found to be achieved by Al high temperature buffer process, In flux exposure etc., and directly confirmed by coaxial impact collision ion scattering spectroscopy (CAICISS) technique. The relation between the surface reconstruction structure of GaN epilayers and the lattice polarity of the epilayers is also shown.     

Carrier recombination under one-photon and two-photon excitation in GaN epilayers

Luminescence properties of 100-mum thick GaN epilayers grown by hydride vapor phase epitaxy (HVPE) over three different substrates: high-pressure grown n-type bulk GaN (HP-n-GaN), high-pressure bulk GaN doped with magnesium (HP-GaN:Mg), and free-standing HVPE lifted-off from sapphire (FS-HVPE-GaN), were compared by means of one-photon and two-photon excitations. The contribution of carrier capture to nonradiative traps was estimated by the analysis of luminescence transients with carrier diffusion taken into account. The estimated values of carrier lifetime of about 3ns and diffusion coefficient of 1cm(2)/s indicate the highest quality of GaN epilayers on FS-HVPE-GaN substrates.     

GaN外延层中的缺陷对光学性质的影响

用金属有机化合物气相外延（ＭＯＶＥＰ）方法生长具有不同表面形貌的非掺杂ＧａＮ，并对部分样品的外延层表面进行镜面加工．用阴极射线发光、光散射和拉曼散射方法观察ＧａＮ中深能级发光、缺陷散射光分布和拉曼散射光频移．结果表明，缺陷不但影响ＧａＮ的发光和光散射，而且影响拉曼频移     

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.     

高质量氮化镓材料的光致发光研究

利用氨气源分子束外延（GSMBE）技术,在改型Ⅳ型分子束外延设备上生长高质量GaN单晶外延材料,并对样品进行了光致发光测量。分析室温和低温光致发光谱,系统地研究GaN的发光峰及其起源,并对常见的黄色发光带现象及其微结构起因进行探讨。     

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.     

Properties comparison of GaN epilayers deposited under different growth temperatures

Undoped GaN epilayers were grown on c-plane sapphire substrates under different growth temperatures by metalorganic chemical vapour deposition (MOCVD). The optical and structural characteristics of these grown samples were studied and compared. It was found that the crystalline quality of GaN film deposited at 1050°C was better that of other samples. Photoluminescence spectra showed that the intensities of yellow luminescence band of the samples decreased as the growth temperature increased. All above test results demonstrate that high temperature deposition can serve as a good method for high-quality GaN epilayer growth and there exists an optimal growth temperature.     

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.     

Effect of Reactor Pressure on Qualities of GaN Layers Grown by Hydride Vapour Phase Epitaxy

The influence of reactor pressure on GaN layers grown by hydride vapour phase epitaxy （HVPE） is investigated. By decreasing the reactor pressure from0. 7 to 0.5 mm, the GaN layer growth mode changes from the island-like one to the step flow. The improvements in structural and optical properties and surface morphology of GaN layers are observed in the step flow growth mode. The results clearly indicate that the reactor pressure, similarly to the growth temperature, is One of the important parameters to influence the qualities of GaN epilayers grown by HVPE, due to the change of growth mode.     

Structural and optical properties of GaN thin films grown on Al2O3 substrates by MOCVD at different reactor pressures

GaN thin films grown by MOCVD on (0 0 0 1) Al₂O₃ substrates at different growth pressures were characterized by field-emission scanning electron microscopy, atomic force microscopy, micro-Raman, and photoluminescence at room temperature. It was found that there is an optimum pressure of 76 Torr at which the structural and optical properties of the GaN samples are superior. On the other hand samples grown at higher pressure exhibited hexagonal surface pits and surface spirals. The results showed that the growth pressure strongly influences the morphology, and significantly affects the structural and optical properties of the GaN epilayers.     

Comparative study of different properties of GaN films grown on(0001) sapphire using high and low temperature AlN interlayers

Comparative study of high and low temperature AlN interlayers and their roles in the properties of GaN epilayers prepared by means of metal organic chemical vapour deposition on (0001) plane sapphire substrates is carried out by high resolution x-ray diffraction, photoluminescence and Raman spectroscopy. It is found that the crystalline quality of GaN epilayers is improved significantly by using the high temperature AlN interlayers, which prevent the threading dislocations from extending, especially for the edge type dislocation. The analysis results based on photoluminescence and Raman measurements demonstrate that there exist more compressive stress in GaN epilayers with high temperature AlN interlayers. The band edge emission energy increases from 3.423~eV to 3.438~eV and the frequency of Raman shift of $E_{2 }$(TO) moves from 571.3~cm$^{ - 1}$ to 572.9~cm$^{ - 1}$ when the temperature of AlN interlayers increases from 700~$^{\circ}$C to 1050~$^{\circ}$C. It is believed that the temperature of AlN interlayers effectively determines the size, the density and the coalescence rate of the islands, and the high temperature AlN interlayers provide large size and low density islands for GaN epilayer growth and the threading dislocations are bent and interactive easily. Due to the threading dislocation reduction in GaN epilayers with high temperature AlN interlayers, the approaches of strain relaxation reduce drastically, and thus the compressive stress in GaN epilayers with high temperature AlN interlayers is high compared with that in GaN epilayers with low temperature AlN interlayers.     

Raman spectroscopy of optical phonons as a probe of GaN epitaxial layer structural quality

We report on Raman scattering measurements of all Raman-active phonons in wurtzite and zinc blende structure GaN epilayers grown on GaAs (001), GaAs (111)A, and GaAs (111)B oriented substrates by means of molecular beam epitaxy (MBE). Raman spectra are taken from these epilayers at room temperature and 77 K in backscattering geometry. The measured values of the phonon frequencies are in agreement with other studies and with lattice dynamic calculations of phonon modes in GaN zinc blende and wurtzite structures. We show that crystal quality is much better in samples grown on GaAs (111) substrates than in samples grown on GaAs (001) substrates. The observation of disorder-activated modes gives information about sample quality. Comparison of the spectra from different thickness epilayers shows that the GaN is more highly disordered close to the substrate, particularly for the (001) substrates. Received 16 July 1999     

The oxidation of gallium nitride epilayers in dry oxygen

The oxidation of GaN epilayers in dry oxygen has been investigated. The GaN epilayers, about 1 7m thick, were grown on (0001) sapphire substrates by rapid thermal process/low pressure metalorganic chemical vapor deposition. Bulk /-2/ X-ray diffraction (XRD) data showed that the slight oxidation of GaN began to occur at 800 °C for 6 h. The oxide was identified as the monoclinic #-Ga₂O₃. The GaN epilayers were completely oxidized at 1050 °C for 4 h or at 1100 °C for 1 h. For all samples, the strongest oxide's peak is (11-3), and (30-6) followed. There is a rapid oxidation process in the initial stage of oxidation, and a relatively slow process followed when the temperature was over 1000 °C. The oxidation of two stages was limited by the rate of an interfacial reaction mechanism and by the diffusion mechanism, respectively. When the temperature reaches 1100 °C, the oxidation rate is very fast, which is considered as the results of the GaN decomposition at high temperature under atmosphere. The oxide layers were also observed by a scanning electron microscope, which shows a rough oxide surface and an expansion of the volume of 40%. The photoluminescence (PL) seriously influenced by the oxidation is also discussed.     

Surface kinetics of GaN evaporation and growth by molecular-beam epitaxy

The kinetics of surface processes during the growth of GaN by molecular-beam epitaxy (MBE) with ammonia as the source of reactive nitrogen is studied theoretically and experimentally. A model of surface processes is developed taking into account specific effects of the blocking of NH₃ adsorption sites by Group III and Group V surface species. Parameters of the model (respective kinetic rate constants) are determined from comparison with experimental data. It is shown that the evaporation rate of GaN in ammonia atmosphere is much lower than that in vacuum. Kinetics of GaN growth under gallium-rich and nitrogen-rich conditions are compared. Under nitrogen-rich conditions the GaN surface is predicted to be enriched by NH_x surface radicals, in contrast to the case of growth under gallium-rich conditions or of free evaporation in vacuum. It is shown that use of the nitrogen-rich conditions allows one to increase the growth temperature by 80–90°C compared with the case of gallium-rich conditions or plasma-activated MBE. The increased growth temperature is favorable in improving the optical and electrical properties of the material grown.     

初始化生长条件对a-GaN中应变的影响

利用高分辨X射线衍射(HRXRD)与拉曼散射光谱(Raman scattering spectra)研究了氮化处理与低温AlN缓冲层对低压金属有机化学气相沉积(LP-MOCVD)在r面蓝宝石衬底上外延的a面GaN薄膜中的残余应变的影响。实验结果表明:与氮化处理后生长的a-GaN相比,使用低温AlN缓冲层后生长的a-GaN具有较小的摇摆曲线的半高宽和较低的残余应变,而且其结构各向异性和残余应变各向异性也均有一定程度的降低。因此,与氮化处理相比,低温AlN缓冲层更有利于a-GaN的生长。     

Possible origin of room-temperature ferromagnetism in undoped GaN epilayers implanted with Mn ions

Manganese ions were implanted into unintentionally doped GaN epilayers grown by metal organic chemical vapor deposition (MOCVD). The (Ga,Mn)N and Ga_xMn_y phases were formed after Mn-implanted undoped GaN epilayers annealed at 700 and 800 °C. The samples showed ferromagnetic behavior at room temperature with the highest magnetization obtained in the sample annealed at 800 °C. Ferromagnetic signal reduces as annealing temperature increased above 900 °C. It is believed that the room-temperature ferromagnetic property of Mn-implanted undoped GaN epilayers are mainly from (Ga_,Mn)N. The Ga_xMn_y phases play a critical role in providing holes and also contribute to increasing the ferromagnetic property.     

Thermal characterization of GaN heteroepitaxies using ultraviolet transient thermoreflectance

Thermal transport properties of GaN heteroepitaxial structures are of critical importance for the thermal management of high-power GaN electronic and optoelectronic devices. Ultraviolet(UV) lasers are employed to directly heat and sense the GaN epilayers in the transient thermoreflectance(TTR) measurement, obtaining important thermal transport properties in different GaN heterostructures, which include a diamond thin film heat spreader grown on GaN. The UV TTR technique enables rapid and non-contact thermal characterization for GaN wafers.     

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.     

Si基GaN的微结构表征

采用快速辐射加热/低压-金属有机化学气相淀积(RTP/LP-MOCVD)方法分别以AlN和阳极氧化铝为缓冲层材料在Si衬底上外延生长GaN薄膜,通过X射线衍射谱(XRD)、光荧光谱(PL)、拉曼散射谱(RamanScattering)等手段对它们的微结构进行了表征和分析,结果指出AlN是优良的缓冲层材料。     

The study of hydrogenation effect for the deep levels in GaN epilayers

After the undoped GaN epilayers were grown on (0 0 0 1) sapphire substrates by plasma-assisted molecular beam epitaxy (PAMBE), the photoconductivity (PC) and thermally stimulated current (TSC) measurements have been carried out so as to investigate the hydrogenation and annealing effect of the deep levels. These results indicate that the values of concentrations of the deep levels in the GaN epilayers decrease by the passivation of hydrogenation in both PC and TSC measurements. After hydrogenation, the PC intensity for the hydrogenated GaN epilayer decreased remarkably in comparison with that for the as-grown sample and the TSC peak near 150 K drastically decreased.In the case of PC measurement, the PC intensity for the hydrogenated and annealed GaN epilayer was approximately half that for the hydrogenated only GaN epilayer when the hydrogenated epilayer was annealed at 700°C. This result reveals that the passivation of the deep levels due to the hydrogenation is still effective at the annealing temperature of 700°C. In the case of TSC measurement, the deep levels changed slightly in comparison with that of hydrogenated GaN epilayer when the hydrogenated GaN epilayer was annealed at 600°C for 30 s. This result also shows that the passivation of deep levels due to the hydrogenation is still effective at the annealing temperature of 600°C for 30 s. In considering the above circumstances, these TSC results are in reasonable agreement with the PC results.