MBE growth and properties of GaN and AlxGa1−xN on GaN/SiC substrates

The growth of GaN and AlGaN by molecular beam epitaxy (MBE) has been studied using GaN/SiC substrates. The GaN/SiC substrates consisted of ∼3 μm thick GaN buffer layers grown on 6H-SiC wafers by metalorganic vapor phase epitaxy (MOVPE) at Crée Research, Inc. The MBE-grown GaN films exhibit excellent structural and optical properties—comparable to the best GaN grown by MOVPE. Al_xGa_1−xN films (x ∼ 0.06-0.08) and Al_xGa_1−xN/GaN multi-quantum-well structures which display good optical properties were also grown by MBE on GaN/SiC substrates.     

可用于Ⅲ族氮化物生长的50mm 3C-SiC/Si(111)衬底的制备

利用新研制出的垂直式低压CVD(LPCVD)SiC生长系统,获得了高质量的50mm 3C-SiC/Si(111)衬底材料.系统研究了3C-SiC的n型和p型原位掺杂技术,获得了生长速率和表面形貌对反应气体中SiH4流量和C/Si原子比率的依赖关系.利用Hall测试技术、非接触式方块电阻测试方法和SIMS,分别研究了3C-SiC的电学特性、均匀性和故意调制掺杂的N浓度纵向分布.利用MBE方法,在原生长的50mm 3C-SiC/Si(111)衬底上进行了GaN的外延生长,并研究了GaN材料的表面、结构和光学特性.结果表明3C-SiC是一种适合于高质量无裂纹GaN外延生长的衬底或缓冲材料.     

P- and N-type doping of GaN and AlGaN epitaxial layers grown by metalorganic chemical vapor deposition

Mg- and Si-doped GaN and AlGaN films were grown by metalorganic chemical vapor deposition and characterized by room-temperature photoluminescence and Hall-effect measurements. We show that the p-type carrier concentration resulting from Mg incorporation in GaN:Mg films exhibits a nonlinear dependence both on growth temperature and growth pressure. For GaN and AlGaN, n-type doping due to Si incorporation was found to be a linear function of the silane molar flow. Mg-doped GaN layers with 300K hole concentrations p ∼2×10¹⁸ cm⁻³ and Si-doped GaN films with electron concentrations n∼1×10¹⁹ cm⁻³ have been grown. N-type Al_0.10Ga_0.90N:Si films with resistivities as low as p ∼6.6×10⁻³ Ω-cm have been measured.     

Characterization of AlGaN/GaN structures on various substrates grown by radio frequency-plasma assisted molecular beam epitaxy

The structural properties and surface morphology of AlGaN/GaN structures grown on LiGaO₂ (LGO), sapphire, and hydride vapor phase epitaxy (HVPE)-grown GaN templates are compared. AlGaN grown on LGO substrates shows the narrowest x-ray full width at half maximum (FWHM) for both symmetric 〈00.4〉 and asymmetric 〈10.5〉 reflections. Atomic force microscopy (AFM) analysis on AlGaN surfaces on LGO substrates also show the smoothest morphology as determined by grain size and rms roughness. The small lattice mismatch of LGO to nitrides and easily achievable Ga-polarity of the grown films are the primary reasons for the smoother surface of AlGaN/GaN structure on this alternative substrate. Optimizations of growth conditions and substrate preparation results in step flow growth for an AlGaN/GaN structure with 300 Å thick Al_0.25Ga_0.75N on 2.4 μm thick GaN. A high III/V flux ratio during growth and recently improved polishing of LGO substrates aids in promoting two dimensional step flow growth. The GaN nucleation layer directly on the LGO substrate showed no evidence of mixed phase cubic and hexagonal structure that is typically observed in the nucleation buffer on sapphire substrates. Cross-sectional high-resolution transmission electron microscopy (HRTEM) was performed on an AlGaN/GaN heterostructure grown on LGO. The atomic arrangement at the AlGaN/GaN interface was sharp and regular, with locally observed monolayer and bilayer steps.     

Optical and electrical characterization of GaN layers grown on silicon and sapphire substrates

Characterization of the structural, optical and electrical properties of GaN layers grown by two epitaxial techniques (ECR-MBE and MOCVD) using different substrates (vicinal Si111 and sapphire) has been performed. The quality of the samples grown by MOCVD seems to be influenced by the nitrogen source used for the growth. Unintentionally doped MBE samples with n-type concentrations around 10¹⁸ cm⁻³ and Hall mobility of 15 cm² (V s)⁻¹ were studied. GaN films doped with Mg and grown using AlN buffer layers have also been analyzed to study the influence of the thickness of the buffer layer on the optical properties of the GaN epilayer. In the samples with low Mg doping, a thin AlN buffer layer improved the optical quality of the film. In general, all the MBE samples doped with Mg were highly resistive, probably due to a low activation or high ionization energy of the Mg acceptors. Technological issues related to the formation of ohmic contacts on GaN layers are also presented.     

AlGaN中Mg掺杂对蓝光发光二极管光电性质的影响

采用金属有机化学气相沉积技术生长了GaN基多量子阱(MQW)蓝光发光二极管外延片,并采用高分辨率X射线衍射仪(HRXRD)和光致光谱仪(PL)表征晶体质量和光学性能,其他的光电性能由制成芯片后测试获得,目的是研究外延片p型AlGaN电子阻挡层Mg掺杂的优化条件.结果表明,在生长p型AlGaN电子阻挡层的Cp2Mg流量为300 cm3/min时,蓝光发光二极管获得最小正向电压VF,而且在此掺杂流量下的多量子阱蓝光发光二极管芯片发光强度明显高于其他流量的样品.因此可以通过优化AlGaN电子阻挡层的掺杂浓度,来显著提高多量子阱蓝光发光二极管的电学性能和光学性能.     

Influence of crystalline defects on transport properties of GaN grown by ammonia-molecular beam epitaxy and magnetron sputter epitaxy

GaN layers have been grown using an MBE/MSE (molecular beam epitaxy/magnetron sputter epitaxy) dual-mode system. The layers grown by the two techniques exhibited a large difference in crystalline quality and presented a broad spectrum of structural, optical, and transport properties that are useful for an analysis of the role of crystalline defects in GaN epilayers. The model of electron scattering by charged threading dislocations was applied in a theoretical fit of the mobility data. The theoretical fit in combination with x-ray diffraction and photoluminescence studies reveal the correlation between dislocation density, electron mobility, doping characteristics and yellow luminescence.     

Si衬底和Si-SiO_2-Si柔性衬底上的GaN生长

使用MBE方法在Si(111)衬底和Si SiO2 Si柔性衬底上生长了GaN外延层 ,并对在两种衬底上生长的样品进行了对比分析 .在柔性衬底上获得了无裂纹的外延层 ,其表面粗糙度为 0 6nm .研究了GaN外延层中的应力及其光学性质 ,光致发光测试结果表明柔性衬底上生长的外延层中应力和杂质浓度明显低于直接生长在Si衬底上的样品的值 .研究结果显示了所用柔性衬底有助于改善GaN外延膜的质量     

Surface morphology and electronic properties of dislocations in AlGaN/GaN heterostructures

Scanning force microscopy was used to examine the surfaces of AlGaN/GaN heterostructures grown by molecular beam epitaxy (MBE) on GaN templates prepared by hydride vapor phase epitaxy (HVPE). Away from dislocations, the MBE growth replicates the surface morphology of the HVPE film, with monolayer steps clarly visible in topographic images. However, the surface morphology near dislocations depends strongly on the MBE growth conditions. Under Ga rich growth the dislocations appear as hillocks, while under stoichiometric growth they appear as pits. A dependence on Al concentration is also observed. Surface contact potential variation near dislocations is consistent with excess negative charges surrounding by a depletion region, but this was observed only for the film grown under stoichiometric conditions.     

Growth and characterization of ZnO thin films on GaN epilayers

Dense ZnO(0001) films formed at 500°C via coalescence of islands grown via metalorganic vapor phase epitaxy (MOVPE) either on GaN/AlN/SiC(0001) substrates or on initial, coherent ZnO layers. Conical crystallites formed due to thermal expansion-induced stresses between the ZnO and the substrate. Interfaces between the ZnO films on GaN epilayers exposed either simultaneously to diethylzinc and oxygen or only to diethylzinc at the initiation of growth were sharp and epitaxial. Interfaces formed after the exposure of the GaN to O₂ were less coherent, though an interfacial oxide was not observed by cross-sectional transmission electron microscopy (TEM). Threading dislocations and stacking faults were observed in all films.     

Near-Infrared Absorption in Lattice-Matched AlInN/GaN and Strained AlGaN/GaN Heterostructures Grown by MBE on Low-Defect GaN Substrates

We have investigated near-infrared absorption and photocurrent in lattice-matched AlInN/GaN and strained AlGaN/GaN heterostructures grown by molecular-beam epitaxy (MBE) on low-defect GaN substrates for infrared device applications. The AlGaN/GaN heterostructures were grown under Ga-rich conditions at 745°C. Material characterization via atomic force microscopy and high-resolution x-ray diffraction indicates that the AlGaN/GaN heterostructures have smooth and well-defined interfaces. A minimum full-width at half-maximum of 92 meV was obtained for the width of the intersubband absorption peak at 675 meV of a 13.7 Å GaN/27.5 Å Al_0.47Ga_0.53N superlattice. The variation of the intersubband absorption energy across a 1 cm × 1 cm wafer was ±1%. An AlGaN/GaN-based electromodulated absorption device and a quantum well infrared detector were also fabricated. Using electromodulated absorption spectroscopy, the full-width at half-maximum of the absorption peak was reduced by 33% compared with the direct absorption measurement. This demonstrates the suitability of the electromodulated absorption technique for determining the intrinsic width of intersubband transitions. The detector displayed a peak responsivity of 195 μA/W at 614 meV (2.02 μm) without bias. Optimal MBE growth conditions for lattice-matched AlInN on low-defect GaN substrates were also studied as a function of total metal flux and growth temperature. A maximum growth rate of 3.8 nm/min was achieved while maintaining a high level of material quality. Intersubband absorption in AlInN/GaN superlattices was observed at 430 meV with full-width at half-maximum of 142 meV. Theoretical calculations of the intersubband absorption energies were found to be in agreement with the experimental results for both AlGaN/GaN and AlInN/GaN heterostructures.     

用侧向外延生长法降低立方相GaN中的层错密度

尝试用侧向外延(ELOG)方法来降低立方相GaN中的层错密度.侧向外延是在SiO2/GaN/GaAs图形衬底上进行的,对生长所得的立方相GaN外延层用扫描电子显微镜(SEM)和透射电子显微镜(TEM)进行了观察和分析,TEM的平面像表明经过ELOG方法生长后,立方相GaN外延层中的层错密度由侧向外延生长前的5×109cm-2降低至生长后的6×108cm-2.双晶X射线衍射(DCXRD)测量给出侧向外延前后外延层ω扫描(002)衍射摇摆曲线的半高宽(FWHM)分别为33′和17.8′,表明晶体质量有了较大改善.对立方相GaN侧向外延过程中层错减少的机制进行了讨论.     

Catalyst-free growth of GaN nanowires

We have grown GaN and AlGaN nanowires on Si (111) substrates with gassource molecular beam epitaxy (MBE). No metal catalysts were used. The nanowires displayed a number of interesting materials properties, including room-temperature luminescence intensity greater than that of free-standing HVPE-grown GaN, relaxed lattice parameters, and the tendency of nanowires dispersed in solvents to align in response to electric fields. The wires were well separated, 50–250 nm in diameter, and grew to lengths ranging from 2 μm to 7 μm. Transmission electron microscopy indicated that the wires were free of defects, unlike the surrounding matrix layer.     

不同AlGaN层厚度的AlGaN/GaN高电子迁移率晶体管的静态特性

利用金属有机化合物气相外延技术研究了AlGaN/GaN高电子迁移率晶体管(HEMT)结构的外延生长及器件制作,重点比较了具有不同AlGaN层厚度的HEMT器件的静态特性.实验发现具有较薄AlGaN隔离层的结构表现出较好的器件特性.栅长为1μm的器件获得了650mA/mm的最大饱和电流密度和100mS/mm的最大跨导.     

Spontaneous growth of GaN nanowire nuclei on N- and Al-polar AlN: A piezoresponse force microscopy study of crystallographic polarity

The polarity of gallium nitride (GaN) nanowire nuclei grown on AlN layers was studied by piezoresponse force microscopy (PFM). N- or Al-polar AlN layers were grown by molecular beam epitaxy (MBE) on Si (111) substrates by use of Al- or N-rich growth conditions, respectively. Short and low density GaN nanowires were then grown on each AlN polarity type. PFM measurements verified the expected AlN layer polarity and further indicated that predominantly N-polar nanowires are produced for growth on both AlN polarity types. Cross-section scanning transmission electron microscopy (STEM) images further reveal that the nanowires on Al-polar AlN films are nucleated on regions in the AlN layer that contain inversion domains, which propagate into the GaN nanowire nuclei. PFM measurements were found to be a convenient technique for mapping the polarity of a statistically significant number of individual GaN nanowires.     

Gradual tilting of crystallographic orientation and configuration of dislocations in GaN selectively grown by vapour phase epitaxy methods

Cross-sectional transmission electron microscope (TEM) observation was performed for selectively grown gallium nitride (GaN) in order to examine the dependence of GaN microstructure on the growth conditions. The GaN films were grown by hydride vapour phase epitaxy (HVPE) or metalorganic vapour phase epitaxy (MOVPE) on GaN covered with a patterned mask. Thin foil specimens for TEM observation were prepared with focused ion beam (FIB) machining apparatus. It was demonstrated that the c-axis of GaN grown over the terrace of the mask tilts towards the centre of the terrace when the GaN is grown in a carrier gas of N2. The wider terrace results in a larger tilting angle if other growth conditions are identical. The tilting is attributed to 'horizontal dislocations' (HDs) generated during the overgrowth of GaN on the mask terrace. The HDs in HVPE-GaN have a semi-loop shape and are tangled with one another, while those in MOVPE-GaN are straight and lined up to form low-angle grain boundaries.     

利用混合极性制备多孔缓冲层及其在GaN厚膜外延中的应用

使用分子束外延(MBE)技术在(0001)面蓝宝石衬底上生长混合极性的氮化镓(GaN)薄膜,利用不同极性面的GaN薄膜在强碱溶液中腐蚀特性的差异,混和极性样品经腐蚀处理后,得到了一层具有多孔结构的GaN层.以多孔结构的GaN作为缓冲层,用卤化物气相外延(HVPE)方法生长GaN厚膜.X射线双晶衍射和光致发光等测试结果表明,多孔结构的GaN缓冲层可以有效地释放GaN厚膜和衬底之间因热膨胀系数失配产生的应力,使GaN厚膜晶体的质量得到很大提高.     

Residual impurities in GaN/Al2O3 grown by metalorganic vapor phase epitaxy

Residual impurities in GaN films on sapphire (A1₂O₃) substrates grown by two-step metalorganic vapor phase epitaxy (MOVPE) have been investigated. We have mainly investigated the incorporation of carbon into the GaN films with GaN buffer layers on A1₂O₃ during MOVPE growth, comparing trimethygallium (TMGa) and triethygallium (TEGa) as the typical gallium precursors. The films were characterized by secondary ion mass spectroscopy analysis, photolu-minescence, and Hall measurements. The carbon, hydrogen, and oxygen concentrations increase with decreasing growth temperature in using TMGa. Especially the carbon concentration increases with decreasing a V/III ratio, for both TMGa and TEGa. There is about two times more carbon in the GaN films grown using TEGa than those using TMGa. The carbon from TMGa mainly enhances the D-A pair emission (∼378 nm), which shows the carbon makes an acceptor level at nitrogen sites in GaN. On the other hand, the carbon from TEGa enhances a deep emission (∼550 nm), which shows the carbon makes not only an acceptor level but deep levels at interstitial sites in GaN. The carbon impurities originate from methyl radicals for TMGa, or ethyl radicals for TEGa. It is supposed that, in the case of TEGa, the carbon impurities are not always located at nitrogen sites, but are also located at interstitial sites because of the C-C bonding in ethyl radicals.     

Influence of arsenic incorporation on surface morphology and Si doping in GaAs(110) homoepitaxy

We have studied the relationship between the arsenic incorporation kinetics and the surface morphology and Si doping behaviour in GaAs(110) films grown by molecular beam epitaxy (MBE). The homoepitaxial growth of GaAs(110) requires low substrate temperatures and high As/Ga flux ratios to obtain films with good surface morphology, and under these conditions Si doped layers exhibit n-type behaviour. At higher growth temperatures and lower As/Ga flux ratios, the epitaxial films are highly faceted and the Si doped layers are p-type. We show that this growth related site switching behaviour and variation in surface morphology is due to a decrease in the As coverage arising from a small and temperature dependent incorporation coefficient of arsenic on this surface.     

High-Temperature Growth of GaN and Al<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Ga<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>N via Ammonia-Based Metalorganic Molecular-Beam Epitaxy

The effect of high-temperature growth on the crystalline quality and surface morphology of GaN and Al _x Ga_1?x N grown by ammonia-based metalorganic molecular-beam epitaxy (NH₃-MOMBE) has been investigated as a means of producing atomically smooth films suitable for device structures. The effects of V/III ratio on the growth rate and surface morphology are described herein. The crystalline quality of both GaN and AlGaN was found to mimic that of the GaN templates, with (002) x-ray diffraction (XRD) full-widths at half- maximum (FWHMs) of ~350 arcsec. Nitrogen-rich growth conditions have been found to provide optimal surface morphologies with a root-mean-square (RMS) roughness of ~0.8 nm, yet excessive N-rich environments have been found to reduce the growth rate and result in the formation of faceted surface pitting. AlGaN exhibits a decreased growth rate, as compared with GaN, due to increased N recombination as a result of the increased pyrolysis of NH₃ in the presence of Al. AlGaN films grown directly on GaN templates exhibited Pendellösung x-ray fringes, indicating an abrupt interface and a planar AlGaN film. AlGaN films grown for this study resulted in an optimal RMS roughness of ~0.85 nm with visible atomic steps.