Optical properties of laterally overgrown GaN pyramids grown on (1 1 1) silicon substrate

Optical properties of laterally overgrown GaN hexagonal pyramids on (1 1 1) Si substrates are studied by cathodoluminescence (CL) spectroscopy and mapping techniques. The results are compared with structural properties obtained by scanning and transmission electron microscopic techniques. To clarify the origin of the bandedge and yellow-band emissions from the GaN pyramids, wavelength-resolved CL properties of normal and cleaved GaN pyramids are investigated in the top and/or cross-sectional view configurations. The cross-sectional view CL images for cleaved GaN pyramid samples show significant differences between the overgrown areas on top of the mask and the coherently grown regions over the windows. A precise reverse (identical) contrast between bandedge (yellow-band) emission intensity and threading dislocation density is observed by comparing the cross-sectional view CL and transmission electron microscopic images. It is demonstrated that a strong correlation exists between structural defects and optical properties in laterally overgrown GaN hexagonal pyramids.     

GaN纳米柱发光特性

用自组装的Ni纳米岛做掩模通过ICP刻蚀得到GaN纳米柱,采用扫描电子显微镜(SEM)观测其形貌,室温下光致发光(PL)谱测量研究样品发光特性。结果表明,室温下GaN 纳米柱的发光强度是体材料的2.6倍。为了修复刻蚀损伤,用KOH对样品进行湿法处理,发现经KOH处理的纳米柱与处理前相比变得更直,且其发光较处理之前进一步增强。为了研究其原因,分别对KOH处理前后的样品进行变温PL谱的测量,发现湿法处理后发光增强是由于内量子效率的提高引起的。     

光致电化学法提高垂直结构发光二极管出光效率的研究

研究了在垂直结构发光二极管(VLED)器件中, 光致电化学法(PEC)刻蚀N极性n-GaN的速率受不同刻蚀条件(刻蚀浓度、刻蚀时间和光照强度)的影响. 并选择N极性n-GaN表面含有较理想六角金字塔结构(侧壁角为31°)的样品制成器件, 研究PEC刻蚀对VLED的欧姆接触和光电性能的影响. 结果表明, 与未粗化样品相比, PEC刻蚀后的样品接触电阻率明显降低, 形成更好的欧姆接触; 其电学特性有较好的改善, 光输出功率有明显提高, 在20 mA电流下光输出功率增强了86.1%. 对不同金字塔侧壁角度的光提取效率用时域有限差分法(FDTD)模拟, 结果显示光提取效率在侧壁角度为20°– 40°有显著提高, 在23.6° (GaN-空气界面的全反射角)时达到最大.     

Investigation of structural and optical properties of nanoporous GaN film

The structural and optical characteristics of porous GaN prepared by Pt-assisted electroless etching under different etching durations are reported. The porous GaN samples were investigated by scanning electron microscopy (SEM), high-resolution X-ray diffraction (HR-XRD), photoluminescence (PL) and Raman scattering. SEM images indicated that the density of the pores increased with the etching duration; however, the etching duration has no significant effect on the size and shape of the pores. XRD measurements showed that the (0 0 0 2) diffraction plane peak width of porous samples was slightly broader than the as-grown sample, and it increased with the etching duration. PL measurements revealed that the near band edge peak of all the porous samples were red-shifted; however, the porosity-induced PL intensity enhancement was only observed in the porous samples; apart from that, two additional strain-induced structural defect-related PL peaks observed in as-grown sample were absent in porous samples. Raman spectra showed that the shift of E₂ (high) to lower frequency was only found in samples with high density of pores. On the contrary, the absence of two forbidden TO modes in the as-grown sample was observed in some of porous samples.     

Atomic structure of defects in GaN:Mg grown with Ga polarity

The atomic structure of characteristic defects (Mg-rich hexagonal pyramids and truncated pyramids) in GaN:Mg thin films grown with Ga polarity was determined at atomic resolution by reconstruction of the scattered electron wave in a transmission electron microscope. Small cavities within the defects have inside walls covered by GaN of reverse polarity. We propose that lateral overgrowth of the cavities restores matrix polarity on the defect base. From matrix to defect, exchange of Ga and N sublattices leads to a 0.6+/-0.2 A displacement of Ga sublattices. We observe a [1100]/3 shift from matrix AB stacking to BC stacking for the entire pyramid. Electron energy loss spectroscopy detected changes in N edge and presence of oxygen on the defect walls. Our results explain commonly observed decrease of acceptor concentration in heavily doped GaN:Mg.     

Optimized ICP etching process for fabrication of oblique GaN sidewall and its application in LED

Inductively coupled plasma (ICP) etching of GaN is systemically investigated by changing ICP power/RF bias power, operating pressure, and Cl₂/BCl₃ gas mixing ratio. The hexagonal etch pits related to screw dislocation existing along GaN epitaxial layer were observed on the etched GaN surface after ICP etching. The intensity of band-edge emission is significantly reduced from the etched n-GaN surface, which reveals that plasma-induced damage are generated after ICP etching. The oblique sidewall is transferred into GaN using a combination of Cl₂/BCl₃ plasma chemistry and hard mask SiO₂. By adjusting ICP etching process parameters, oblique sidewalls with various oblique angles can be formed, allowing for conformal metal lines coverage across the mesa structures, which can play an important role in the interconnection of multiple microchips for light emitting diodes (LEDs) fabrication.     

Synthesis of flower-shape clustering GaN nanorods by ammoniating Ga2O3 films

Flower-shape clustering GaN nanorods are successfully synthesized on Si（111） substrates through ammoniating Ga2O3/ZnO films at 950℃. The as-grown products are characterized by x-ray diffraction （XRD）, scanning electron microscope （SEM）, field-emission transmission electron microscope （FETEM）, Fourier transform infrared spectrum （FTIR） and fluorescence spectrophotometer. The SEM images demonstrate that the products consist of flower-shape clustering GaN nanorods. The XRD indicates that the reflections of the samples can be indexed to the hexagonal GaN phase and HRTEM shows that the nanorods are of pure hexagonal GaN single crystal. The photoluminescence （PL） spectrum indicates that the GaN nanorods have a good emission property. The growth mechanism is also briefly discussed.     

Investigation of yellow luminescence intensity of N-polar unintentionally doped GaN

This paper reports that the yellow luminescence intensity of N-polar GaN Epi-layers is much lower than that of Ga-polar ones due to the inverse polarity,and reduces drastically in the N-polar unintentionally-doped GaN after etching in KOH solution.The ratio of yellow luminescence intensity to band-edge emission intensity decreases sharply with the etching time.The full width at half maximum of x-ray diffraction of(10-12) plane falls sharply after etching,and the surface morphology characterized by scanning electron microscope shows a rough surface that changes with the etching time.The mechanism for the generation of the yellow luminescence are explained in details.     

全息技术制作二维光子晶体蓝宝石衬底提高发光二极管外量子效率

为了提高GaN基发光二极管(LED)的外量子效率,在蓝宝石衬底制作了二维光子晶体.衬底上的二维光子晶体结构采用激光全息技术和感应耦合等离子体(ICP)干法刻蚀技术制作,然后采用金属氧化物化学气相沉积(MOCVD)技术在图形蓝宝石衬底(PSS)上生长2μm厚的n型GaN层,4层量子阱和200nm厚的p型GaN层,形成LED结构.衬底上制作的二维光子晶体为六角晶格结构,晶格常数为3.8μm,刻蚀深度为800nm.LED器件光强输出测试结果显示,在PSS上制作的LED(PSS-LED)的发光强度普遍高于蓝宝石平 关键词： 全息 发光二极管 图形蓝宝石衬底 外量子效率     

单晶硅表面金字塔生长过程的实验研究

在普通碱液中添加一种特殊的添加剂,在不同时间下对单晶硅表面进行刻蚀.用扫描电子显微镜观察样品表面形貌,结果显示：单晶硅片放入加入添加剂2 mL的刻蚀液中,经过10 min刻蚀后晶体表面零星出现大小不一的金字塔,并有大面积的平滑区|刻蚀15 min后金字塔大小趋向一致,平滑区面积缩小|刻蚀20 min硅片表面形成平均尺寸为2～4 μm金字塔绒面结构,并且均匀性好、覆盖率高|刻蚀25 min后,进入过腐蚀阶段,金字塔出现变大的现象.研究表明：与传统碱腐蚀相比,添加剂可以缩短单晶硅刻蚀时间,并获得较为理想的绒面结构,在工业上应用可以降低生产成本和生产时间,提高生产率.     

Selective growth of GaInN quantum dot structures

In this work, we present an approach to fabricate GaInN quantum dots. The idea is to have a complete control of the position of the quantum dot during the growth and to use this positioned dot for future functioning. For this purpose we have prepared templates with selectively grown GaN pyramids by MOVPE. After proper adjustment of the GaN growth we have overgrown these templates with InGaN to form the quantum dots on top of the pyramids. Finally the structures were capped with GaN and photoluminescence measurements were performed.     

单晶硅表面金字塔生长过程的实验研究

在普通碱液中添加一种特殊的添加剂,在不同时间下对单晶硅表面进行刻蚀.用扫描电子显微镜观察样品表面形貌,结果显示:单晶硅片放入加入添加剂2 mL的刻蚀液中,经过10 min刻蚀后晶体表面零星出现大小不一的金字塔,并有大面积的平滑区;刻蚀15 min后金字塔大小趋向一致,平滑区面积缩小;刻蚀20 min硅片表面形成平均尺寸...     

CVD法制备硅基氮化镓薄膜

利用化学气相沉积法(CVD),分别以三氧化二镓(Ga₂O₃)和氨气(NH₃)为镓源和氮源在硅衬底合成了一种由片状微晶构成的氮化镓(GaN)薄膜,实验中没有使用缓冲层。通过场发射扫描电子显微镜(FESEM)、电子能量散射谱(EDS)、X射线衍射(XRD)、高分辨电镜(HRTEM)和光致发光谱(PL)对样品进行分析,生成物为质量较好的富镓的纯氮化镓薄膜。片状氮化镓微晶表面大小约数百纳米,厚度数十纳米,薄膜表面平整、致密,没有裂纹或龟裂现象,与Si衬底结合紧密。氮化镓薄膜的带边峰位于367nm处,同时出现了黄光发射峰。并对此种氮化镓薄膜的生长机理进行了探讨。     

Optimization of inductively coupled plasma deep etching of GaN and etching damage analysis

Inductively coupled plasma (ICP) etching of GaN with an etching depth up to 4 μm is systemically studied by varying ICP power, RF power and chamber pressure, respectively, which results in etch rates ranging from ∼370 nm/min to 900 nm/min. The surface morphology and damages of the etched surface are characterized by optical microscope, scanning electron microscope, atomic force microscopy, cathodoluminescence mapping and photoluminescence (PL) spectroscopy. Sub-micrometer-scale hexagonal pits and pillars originating from part of the structural defects within the original GaN layer are observed on the etched surface. The density of these surface features varies with etching conditions. Considerable reduction of PL band-edge emission from the etched GaN surface indicates that high-density non-radiative recombination centers are created by ICP etching. The density of these non-radiative recombination centers is found largely dependent on the degree of physical bombardments, which is a strong function of the RF power applied. Finally, a low-surface-damage etch recipe with high ICP power, low RF power, high chamber pressure is suggested.     

Self-formation of GaN hollow nanocolumns by inductively coupled plasma etching

GaN hollow nanocolumns were formed by inductively coupled plasma etching. It was found that the tops of the GaN nanocolumns were hexagonal with the c axis perpendicular to the substrate surface. It was also found that the density of the GaN nanocolumns depends strongly on etching parameters, which suggests that the formation of these GaN nanocolumns was not related to the dislocation density in the original GaN epitaxial layers. With an Ar concentration of 42.86%, it was found that the diameter of the whole nanocolumns was around 80 nm and the diameter of the nanocavities inside these nanocolumns was around 40 nm, while the density of the nanocolumns was around 4.4×10⁹ cm^-2. PACS 68.65.-K; 61.70.+w; 81.10.BK     

Optimization of the preparation of GaN-based specimens with low-energy ion milling for (S)TEM

We report on optimization of electron transparent GaN based specimens for transmission electron microscopy (TEM) and scanning TEM (STEM) studies by combining focused ion beam thinning and low-energy (≤500 eV) Ar-ion milling. Energy dependent ion milling effects on GaN based structures are investigated and the quality of ion milled samples is compared with that of specimens prepared by wet chemical etching. Defects formed during ion milling lead to amorphization of the specimen. The experimental results are compared with Monte-Carlo simulations using the SRIM (stopping and range of ions in matter) software. Specimen thickness was deduced from high-angle annular dark field STEM images by normalization of measured intensities with respect to the intensity of the scanning electron probe and comparison with multislice simulations in the frozen lattice approach. The results show that the thickness of the amorphous surface layer can be successfully reduced below 1 nm by low energy ion milling, leading to a homogeneous image contrast in TEM and STEM, so that good conditions for quantitative analysis can be achieved. For an ion energy of 400 eV the thickness measurements resulted in an etching rate of about 6-8 nm/min.     

石英衬底上GaN薄膜沉积及其光学性能的研究

GaN薄膜材料广泛应用于发光二极管(LED),激光二极管(LD)等光电器件。但是GaN基器件的制备与应用以及器件推广很大一部分取决于其器件的价格,常用的方式是在单晶蓝宝石衬底上沉积制备GaN薄膜样品,单晶蓝宝石衬底晶向择优,可以制备出高质量的GaN薄膜样品,但是单晶蓝宝石衬底价格昂贵,一定程度上限制了其GaN基器件推广使用。如何在廉价衬底上直接沉积高质量的GaN薄膜,满足器件的要求成为研究热点。石英玻璃价格廉价,但是属于非晶体,没有择优晶向取向,很难制备出高质量薄膜样品。本研究采用等离子体增强金属有机物化学气相沉积系统在非晶普通石英衬底上改变氮气反应源流量低温制备GaN薄膜材料。制备之后采用反射高能电子衍射谱、X射线衍射光谱、室温透射光谱和光致光谱对制备的薄膜进行系统的测试分析。其结果表明：在氮气流量适当的沉积参数条件下,所制备的薄膜具有高C轴的择优取向,良好的结晶质量以及优异的光学性能。     

Deep etching of epitaxial gallium nitride film by multiwavelength excitation process using F2 and KrF excimer lasers

The deep etching of GaN(0001) thin films epitaxially grown on Al₂O₃(0001) has been investigated by laser ablation using F₂ and KrF excimer lasers. The simultaneous irradiation with F₂ and KrF excimer lasers markedly improves etching quality compared with single-KrF excimer laser ablation and provides almost the same quality as that in the case of single-F₂ laser ablation with a high etching rate. Additionally, the present method achieves the deep etching of a GaN film of more than 5 μm in depth with steep side walls at an angle of 87° by changing the laser incidence angle. PACS 52.38.Mf; 61.82.Fk; 81.65.Cf     

在双热舟化学气相沉积系统中通过掺In技术生长GaN纳米线和纳米锥

在现有的一台蒸发镀膜机基础上，设计加工了一个双热舟化学气相沉积系统.该系统具有真空度高、升温速度快、源和衬底温度可分别控制等优点，有利于化合物半导体纳米材料的生长.利用该生长系统，通过在生长过程中掺入等电子杂质In作为表面活性剂，分别在Si衬底和3C-SiC/Si衬底上生长出高质量的具有纤锌矿结构的单晶GaN纳米线和纳米尖三棱锥.所得产物通过场发射扫描电子显微镜、高分辨透射电子显微镜、能量色散x射线谱仪、x射线衍射仪，和荧光谱仪进行表征.这里所用的生长方法新颖，生长出的GaN纳米尖三棱锥在场发射和激光方面有潜在的应用价值. 关键词： GaN 纳米结构 透射电子显微镜 光致荧光谱     

GaAs pyramids on GaAs/AlAs Bragg reflectors as alternative microcavities

Pyramidal microcavities are a new class of optical resonators with potentially small mode volume and high quality factor. Our GaAs pyramids with embedded InGaAs quantum dots are placed on top of GaAs/AlAs distributed Bragg reflectors to increase the optical confinement at the base of the pyramids. The pyramidal shape is achieved by a wet-chemical etching process using an AlAs sacrificial layer. Temperature-dependent micro-photoluminescence measurements are used to verify optical modes.