分子束外延生长GaN薄膜中的一种早期位错结构

利用高分辨电子显微术，对在GaP基体上由分子束外延生长六角GaN晶体薄膜中的晶体缺陷结构进行了研究．实验中发现了GaN薄膜外延生长过程中产生的一种典型早期刃型位错结构．此晶体缺陷位于一大块GaN晶粒内部，其外观类似于一段（1120）晶界．它由一条（1120）高能孤立晶界段及其两端的两个1/6［1120］不完全刃型位错组成．从大晶格失配材料之间分子束外延生长的机理上对这种缺陷结构的形成进行了解释． 关键词：     

常压MOCVD生长ZnO/GaN/Al2O3薄膜及其性能

以去离子水（H2O）和二乙基锌（DEZn）为源材料,生长温度是680℃时,利用常压MOCVD在GaN／Al2O3模板上成功生长了ZnO单晶薄膜,用原子力显微镜（AFM）、X射线双晶衍射（DCXRD）、光致发光谱（PL）对ZnO薄膜的表面形貌、结晶学性质、光学性质作了综合研究。双晶衍射表明,ZnO非对称（1012）面ω扫描的半峰全宽（FWHM）仅为420arcsec,估算所生长ZnO膜的位错密度大约为10^3／cm^2量级,这与具有器件质量的GaN材料的位错密度相当。在ZnO薄膜的低温15K光荧光谱中,观察到很强的自由激子和束缚激子发射以及自由激子与束缚激子的多级声子伴线。     

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)。     

斜切蓝宝石衬底MOCVD生长GaN薄膜的透射电镜研究

利用MOCVD技术在斜切角度为0.3°的c面蓝宝石衬底上生长了非故意掺杂 GaN 薄膜, 并采用透射电子显微镜对材料的质量和材料内部缺陷进行了分析. 研究发现斜切蓝宝石衬底上外延的GaN材料中,位错在距离衬底0.8 μm附近大量湮灭, 同时位错扎堆出现.基于上述现象, 提出了斜切衬底上GaN材料中位错的湮灭机制, 解释了斜切衬底能够提高GaN晶体质量的原因.     

GaN薄膜拉曼散射光谱的研究

利用拉曼散射光谱对在SiC衬底上采用MOCVD异质外延的未故意掺杂GaN薄膜特性进行研究发现E2模式向频率低的方向漂移表明在GaN薄膜中存在张力,由于SiC衬底不平整度增加引起更多位错的出现,从而引起拉曼谱中E2模式的加宽,因此通过选择平整度较好的衬底可以减小缺陷密度,提高薄膜的质量,此外A1(LO)模式的出现与强度可以用来表征未掺杂GaN的薄膜质量。     

SiNx插入层的生长位置对GaN外延薄膜性质的影响

系统研究了纳米量级的多孔 SiNx插入层生长位置对高质量GaN外延薄膜性质的影响.高分辨X射线衍射测量结果表明:SiNx插入层生长在CaN粗糙层上能够得到最好的晶体质量.利用测量结果分别计算出了螺位错和刃位错的密度.此外,GaN薄膜的光学、电学性质分别用Raman散射能谱、低温光致发光能谱和霍尔测量的方法进行了表征.实...     

Si(111)衬底上GaN的MOCVD生长

利用LP-MOCVD在Si（111）衬底上,以高温AIN为缓冲层,分别用低温GaN（LT-GaN）和偏离化学计量比富Ga高温GaN（HT-GaN）为过渡层外延生长六方相GaN薄膜。采用高分辨率双晶X射线衍射（DCXRD）,扫描电子显微镜（SEM）,原子力显微镜（AFM）和室温光致荧光光谱（RT-PL）进行分析。结果表明,有偏离化学计量比富Ga HT-GaN为过渡层生长的GaN薄膜质量和光致荧光特性均明显优于以LT-GaN为过渡层生长的GaN薄膜,得到GaN（0002）和（1012）的DCXRD峰,其半峰全宽（FWHM）分别为698s和842s,室温下的光致荧光光谱在361nm处有一个很强的发光峰,其半峰全宽为44．3meV。     

蓝宝石衬底上RF-MBE生长的GaN中的极性控制和螺旋位错的降低

近年来人们报道了用MBE方法生长GaN的飞速进展,利用RF-MBE方法可以获得高的GAN生长速率和高的电子迁移率.本文讨论了用RF-MBE方法在蓝宝石衬底上生长GaN过程中的极性控制和螺旋位错的降低.在充分氮化的蓝宝石衬底上直接生长GaN,使GaN的极性控制为N-极性,并用高温生长的AlN核化层实现GaN的Ga-极性.对于N-和Ga-极性的GaN这两种情况,高温生长的AlN中间迭层的引入,可以有效地抑制螺旋位错的扩散.位错的降低使GaN的室温电子迁移率得到提高,对于Ga-极性的GaN,其值为332cm²/V·s;而对于N-极性的GaN,其值为688cm²/V·s.     

非故意掺杂GaN薄膜方块电阻与载气中N2比例关系研究

利用金属有机气相外延方法研究了非故意掺杂GaN薄膜的方块电阻与高温GaN体材料生长时载气中N2比例的关系.研究发现,随着载气中N2比例的增加,GaN薄膜方块电阻急剧增加.当载气中N2比例为50%时,GaN薄膜方块电阻达1.1×108Ω/□,且GaN表面平整,均方根粗糙度为0.233 nm.二次离子质谱分析发现,载气中N2比例不同的样品中碳、氧杂质含量无明显差别.随着载气中N2比例的增加,GaN材料中螺型位错相关缺陷密度无明显变化,而刃型位错相关缺陷密度明显增加.结果表明,刃型位错的受主补偿作用是导致GaN薄膜方块电阻变化的主要原因.     

高温预生长对图形化蓝宝石衬底GaN薄膜质量的提高

在图形化蓝宝石衬底生长低温缓冲层之前,通入少量三甲基镓（TMGa）和大量氨气进行短时间的高温预生长,通过改变TMGa流量制备了4个蓝光LED样品。MOCVD外延生长时使用激光干涉仪实时监测薄膜反射率,外延片使用高分辨率X射线衍射（002）面和（102）面摇摆曲线估算位错密度,并使用光致发光谱表征发光性能,制备成芯片后测试了正向电压和输出光功率。结果表明,高温预生长可促进薄膜的横向外延,使得三维岛状GaN晶粒在较小的薄膜厚度内实现岛间合并,有利于降低位错密度,提高外延薄膜质量,LED芯片的输出光功率的增强幅度达29.1%,而电学性能无恶化迹象;但高温预生长工艺中TMGa的流量应适当控制,过量的TMGa导致GaN晶粒过大,将延长岛间合并时间,降低晶体质量。     

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.     

The influence of AlN interlayers on the microstructural and electrical properties of p-type AlGaN/GaN superlattices grown on GaN/sapphire templates

AlN with different thicknesses were grown as interlayers (ILs) between GaN and p-type Al_0.15Ga_0.85N/GaN superlattices (SLs) by metal organic vapor phase epitaxy (MOVPE). It was found that the edge-type threading dislocation density (TDD) increased gradually from the minimum of 2.5×10⁹?cm^?2 without AlN IL to the maximum of 1×10¹⁰?cm^?2 at an AlN thickness of 20 nm, while the screw-type TDD remained almost unchanged due to the interface-related TD suppression and regeneration mechanism. We obtained that the edge-type dislocations acted as acceptors in p-type Al _x Ga_1?x N/GaN SLs, through the comparison of the edge-type TDD and hole concentration with different thicknesses of AlN IL. The Mg activation energy was significantly decreased from 153 to 70?meV with a?10-nm AlN IL, which was attributed to the strain modulation between AlGaN barrier and GaN well. The large activation efficiency, together with the TDs, led to the enhanced hole concentration. The variation trend of Hall mobility was also observed, which originated from the scattering at TDs.     

The effect of nitrogen pressure on the two-step method deposition of GaN films

GaN thin films were deposited on sapphire (0001) substrates at different nitrogen pressures by pulsed laser deposition (PLD) of GaN target in nitrogen atmosphere. Good single crystal GaN thin films were obtained after annealing at 1000 °C for 15 min in a NH₃ atmosphere. An Nd:YAG pulsed laser with a wavelength of 1064 nm was used as the laser source. The influence of nitrogen pressure on the thickness, crystallinity and surface morphology of GaN films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM) and Raman spectroscopy. The results show that at low nitrogen pressure, the surface diffusion of adatoms can be influenced by the collisions between the nitrogen gas molecules and the activated atoms, which can influence the kinetic energy of the activated atoms. However, at high nitrogen pressure, the kinetic energy of adatoms is decided by the annealing temperature. In our experimental conditions, the GaN thin films deposited at 0.75 and 7.5 Pa have a high surface morphology and crystalline quality. PACS 71.55.Eq; 74.62.Fj     

Dislocation Reduction Mechanisms in Gallium Nitride Films Grown by Canti-Bridge Epitaxy Method

By using the special maskless V-grooved c-plane sapphire as the substrate, we previously developed a novel GaN LEO method, or the so-called canti-bridge epitaxy （CBE）, and consequently wing-tilt-free GaN films were obtained with low dislocation densities, with which all the conventional difficulties can be overcome [J. Vacuum Sci. Technol. B 23 （2005） 2476]. Here the evolution manner of dlslocations in the CBE GaN films is investigated using transmission electron microscopy. The mechanisms of dislocation reduction are discussed. Dislocation behaviour is found to be similar to that in the conventional LEO GaN films except the enhanced dislocation-combination at the coalescence boundary that is a major dislocation-reduction mechanism for the bent horizontal-propagating dislocations in the CBE GaN films. The enhancement of this dislocation-combination probability is believed to result from the inclined shape and the undulate morphology of the sidewalls, which can be readily obtained in a wide range of applicable film-growth conditions during the GaN CBE process. Further development of the GaN CBE method and better crystal-quality of the GaN film both are expected.     

蓝宝石衬底上GaN/AlxGa1-xN超晶格插入层对AlxGa1-xN外延薄膜应变及缺陷密度的影响

室温300K下,由于Al_xGa_1-xN的带隙宽度可以从GaN的3.42eV到AlN的6.2eV之间变化,所以Al_xGa_1-xN是紫外光探测器和深紫外LED所必需的外延材料.高质量高铝组分Al_xGa_1-xN材料生长的一大困难就是Al_xGa_1-xN与常用的蓝宝石衬底之间大的晶格失配和热失配.因而采用MOCVD在GaN/蓝宝石上生长的Al_xGa_1-xN薄膜由于受张应力作用非常容易发生龟裂.GaN/Al_xGa_1-xN超晶格插入层技术是释放应力和减少Al_xGa_1-xN薄膜中缺陷的有效方法.研究了GaN/Al_xGa_1-xN超晶格插入层对GaN/蓝宝石上Al_xGa_1-xN外延薄膜应变状态和缺陷密度的影响.通过拉曼散射探测声子频率从而得到材料中的残余应力是一种简便常用的方法,Al_xGa_1-xN外延薄膜的应变状态可通过拉曼光谱测量得到.Al_xGa_1-xN外延薄膜的缺陷密度通过测量X射线衍射得到.对于具有相同阱垒厚度的超晶格,例如4nm/4nm,5nm/5nm,8nm/8nm的GaN/Al_0.3Ga_0.7N超晶格,研究发现随着超晶格周期厚度的增加Al_xGa_1-xN外延薄膜缺陷密度降低,Al_xGa_1-xN外延薄膜处于张应变状态,且5nm/5nmGaN/Al_0.3Ga_0.7N超晶格插入层Al_xGa_1-xN外延薄膜的张应变最小.在保持5nm阱宽不变的情况下,将垒宽增大到8nm,即十个周期的5nm/8nmGaN/Al_0.3Ga_0.7N超晶格插入层使Al_xGa_1-xN外延层应变状态由张应变变为压应变.由X射线衍射结果计算了Al_xGa_1-xN外延薄膜的刃型位错和螺型位错密度,结果表明超晶格插入层对螺型位错和刃型位错都有一定的抑制效果.透射电镜图像表明超晶格插入层使位错发生合并、转向或是使位错终止,且5nm/8nmGaN/Al_0.3Ga_0.7N超晶格插入层导致Al_xGa_1-xN外延薄膜中的刃型位错倾斜30°左右,释放一部分压应变.     

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.     

外延在蓝宝石衬底上的非掺杂GaN研究

采用改变生长条件的方法制备GaN薄膜,在(0001)面蓝宝石衬底上利用金属有机物化学气相沉积技术制备了不同样品,并借助X射线双晶衍射仪(XRD)、PL谱测试仪和光学显微镜对材料进行了分析。XRD(0002)面和(1012)面测试均表明TMGa流量为70 cm3/min时样品位错密度最低。利用该TMGa流量进一步制备了改变生长温度的样品。XRD和PL谱测试结果表明,提高生长温度有利于提高GaN样品的晶体质量和光学性能。最后,利用光学显微镜对样品的表面形貌进行了分析。     

Growth and characterisation of GaN with reduced dislocation density

Two GaN MOVPE growth methods to reduce the threading dislocation (TD) density have been explored. The combined effects of (1) in situ SiN_x masking of the sapphire substrate and (2) starting the epitaxial growth at low V-to-III ratio on the GaN film quality were studied by atomic force microscopy, transmission electron microscopy and high-resolution X-ray diffraction. It was found that the annealing condition of the low-temperature nucleation layer after in situ SiN_x masking is critical in order to decrease the density of nucleation sites and hence increase the average grain size to about 5 μm. However, the coalescence of large grains with vertical side facets results in the formation of dense bundles of TDs at the grain boundaries combined with large numbers of basal-plane dislocation loops throughout the film. The formation of these dislocations can be prevented by starting the epilayer growth at low V-to-III ratio, resulting in the formation of grains with inclined side facets. The interaction of the TDs with the inclined side facets causes the dislocations to bend 90 as the grains grow in size and coalesce. GaN films with dislocation densities as low as 1×10⁸ cm⁻², giving full-width at half-maximum values of 180 and 220 arcsec for respectively (002) and (302) omega scans, were achieved by the combination of in situ masking and low V–III ratio epilayer growth. Hall carrier mobility values in excess of 900 cm² V ⁻¹ s⁻¹ were deduced for Si-doped layers.     

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.     

Thermal stability of SiGe films on an ultra thin Ge buffer layer on Si grown at low temperature

The thermal stability of SiGe films on an ultra thin Ge buffer layer on Si fabricated at low temperature has been studied. The microstructure and morphology of the samples were investigated by high-resolution X-ray diffraction, Raman spectra and atomic force microscopy, and using a diluted Secco etchant to reveal dislocation content. After thermal annealing processing, it is observed that undulated surface, threading dislocations (TDs) and stacking faults (SFs) appeared at the strained SiGe layer, which developed from the propagation of a misfit dislocation (MD) during thermal annealing, and no SFs but only TDs formed in strain-relaxed sample. And it is found that the SiGe films on the Ge layer grown at 300 °C has crosshatch-free surface and is more stable than others, with a root mean square surface roughness of less than 2 nm and the threading dislocation densities as low as ∼10⁵ cm⁻². The results show that the thermal stability of the SiGe films is associated with the Ge buffer layer, the relaxation extent and morphology of the SiGe layer.