Dry etching characteristics of GaN for blue/green light-emitting diode fabrication

The etch rates, surface morphology and sidewall profiles of features formed in GaN/InGaN/AlGaN multiple quantum well light-emitting diodes by Cl₂-based dry etching are reported. The chlorine provides an enhancement in etch rate of over a factor of 40 relative to the physical etching provided by Ar and the etching is reactant-limited until chlorine gas flow rates of at least 50 standard cubic centimeters per minute. Mesa sidewall profile angle control is possible using a combination of Cl₂/Ar plasma chemistry and SiO₂ mask. N-face GaN is found to etch faster than Ga-face surfaces under the same conditions. Patterning of the sapphire substrate for improved light extraction is also possible using the same plasma chemistry.     

Effects of the ultrasonic flexural vibration on the interaction between the abrasive particles; pad and sapphire substrate during chemical mechanical polishing (CMP)

In this paper, the technique of ultrasonic flexural vibration assisted chemical mechanical polishing (UFV-CMP) was used for sapphire substrate CMP. The functions of the polishing pad, the silica abrasive particles, and the chemical additives of the slurry such as pH value regulator and dispersant during the sapphire's UFV-CMP were investigated. The results showed that the actions of the ultrasonic and silica abrasive particles were the main factors in the sapphire material removal rate (MMR) and the chemical additives were helpful to decrease the roughness of sapphire. Then the effects of the flexural vibration on the interaction between the silica abrasive particles, pad and sapphire substrate from the kinematics and dynamics were investigated to explain why the MRR of UFV-CMP was bigger than that of the traditional CMP. It indicated that such functions improved the sapphire's MRR: the increasing of the contact silica particles’ motion path lengths on the sapphire's surface, the enhancement of the contact force between the contact silica particles and the sapphire's surface, and the impaction of the suspending silica particles to the sapphire's surface.     

Self assembled micro masking effect in the fabrication of SiC nanopillars by ICP-RIE dry etching

This report presents the results of the novel fabrication of 4H-SiC pillars with nanopores using ICP-RIE dry etching. Cl₂/Ar gas plasma with various mass flow rates was used in this etching process to produce SiC nanopillars without using patterned etch mask. Cylindrical pillars of 300 nm diameter and 500 nm height with smooth side walls were etched on SiC wafer. The etching condition for the optimized fabrication of SiC nanopillars is presented in this report. Each nanopillar has been produced with a nanosize pore at the center along its length and up to the middle of the cylindrical nanopillar; it is a unique feature has not ever been reported in case of SiC. Inclusion of oxygen was found influence the formation of nanopillars by the effect of SiO₂ micro masking. The formation of self assembled SiO₂ layer and its micro masking effect in the fabrication of this unique nanostructure has been investigated using TEM, STEM and EDAX measurements.     

Multiform structures with silicon nanopillars by cesium chloride self-assembly and dry etching

We develop a novel method to fabricate multiform structures of Si nanopillars (diameters > 40 nm, aspect ratio > 10, coverage ratio > 35%) by dry etch with self-assembled cesium chloride (CsCl) nanoislands as mask. The pillars can cover structures of lateral size 1 μm and unpolished Si wafer, enabling uneven surface to be textured by nanopillars without complex process or expensive polishing. Planar micro-patterns and tridimensional localization of nanopillars have been easily realized, useful for integrating nanopillars to devices. By figuring out substrate influences, fast formation of CsCl islands within 1 min has been achieved for the first time, making CsCl process flow to be possibly controlled within 30 min. Based on the deliquescence of salt, CsCl self-assembly is simple, widely tunable and compatible, which endows the approaches great practical potential.     

Ultrasonic flexural vibration assisted chemical mechanical polishing for sapphire substrate

The sapphire substrates are polished by traditional chemical mechanical polishing (CMP) and ultrasonic flexural vibration (UFV) assisted CMP (UFV-CMP) respectively with different pressures. UFV-CMP combines the functions of traditional CMP and ultrasonic machining (USM) and has special characteristics, which is that ultrasonic vibrations of the rotating polishing head are in both horizontal and vertical directions. The material removal rates (MRRs) and the polished surface morphology of CMP and UFV-CMP are compared. The MRR of UFV-CMP is two times larger than that of traditional CMP. The surface roughness (root mean square, RMS) of the polished sapphire substrate of UFV-CMP is 0.83 Å measured by the atomic force microscopy (AFM), which is much better than 2.12 Å obtained using the traditional CMP. And the surface flatness of UFV-CMP is 0.12 μm, which is also better than 0.23 μm of the traditional CMP. The results show that UFV-CMP is able to improve the MRR and finished surface quality of the sapphire substrates greatly. The material removal and surface polishing mechanisms of sapphire in UFV-CMP are discussed too.     

Dry etching of MgCaO gate dielectric and passivation layers on GaN

MgCaO films grown by rf plasma-assisted molecular beam epitaxy and capped with Sc₂O₃ are promising candidates as surface passivation layers and gate dielectrics on GaN-based high electron mobility transistors (HEMTs) and metal-oxide semiconductor HEMTs (MOS-HEMTs), respectively. Two different plasma chemistries were examined for etching these thin films on GaN. Inductively coupled plasmas of CH₄/H₂/Ar produced etch rates only in the range 20-70 Å/min, comparable to the Ar sputter rates under the same conditions. Similarly slow MgCaO etch rates (∼100 Å/min) were obtained with Cl₂/Ar discharges under the same conditions, but GaN showed rates almost an order of magnitude higher. The MgCaO removal rates are limited by the low volatilities of the respective etch products. The CH₄/H₂/Ar plasma chemistry produced a selectivity of around 2 for etching the MgCaO with respect to GaN.     

离子束平动刻蚀工艺衍射光学元件的设计及制作

提出了一种用于制作二维光束整形衍射光学元件的新方法———离子束平动刻蚀工艺。分别介绍了利用这种新方法设计衍射光学元件的原理、设计过程以及刻蚀工艺系统的构成和掩模板的设计方法。结果表明 ,这种新的工艺方法不拘泥于圆对称系统 ,不但继承了离子束旋转刻蚀工艺的位相真正连续分布的优势 ,而且所制作出的衍射光学元件 ,即使对于半导体激光器所产生的两个方向发散角不同的激光束来说也仍然可以进行整形 ,并最终能得到矩形焦斑。这种工艺方法的理论设计也可以从二维化简为两个一维的设计 ,从而大大简化了设计计算的复杂程度     

Investigation of chlorine-based etchants in wet and dry etching technology for an InP planar Gunn diode

Mesa etching technology is considerably important in the Gunn diode fabrication process. In this paper we fabricate InP Gunn diodes with two different kinds of chlorine-based etchants for the mesa etching for comparative study. We use two chlorine-based etchants, one is HCl-based solution (HCl/H 3 PO 4 ), and the other is Cl 2 -based gas mixture by utilizing inductively coupled plasma system (ICP). The results show that the wet etching (HCl-based) offers low cost and approximately vertical sidewall, whilst ICP system (Cl 2 -based) offers an excellent and uniform vertical sidewall, and the over-etching is tiny on the top and the bottom of mesa. And the fabricated mesas of Gunn diodes have average etching rates of ～ 0.6 μm/min and ～ 1.2 μm/min, respectively. The measured data show that the current of Gunn diode by wet etching is lower than that by ICP, and the former has a higher threshold voltage. It provides a low-cost and reliable method which is potentially applied to the fabrication of chip terahertz sources.     

Influence on the laser induced backside dry etching of thickness and material of the absorber, laser spot size and multipulse irradiation

Laser induced backside dry etching method (LIBDE) was developed - analogously to the well-known laser induced backside wet etching (LIBWE) technique - for the micromachining of transparent materials. In this procedure, the absorbing liquid applied during LIBWE was replaced with solid metal layers. Fused silica plates were used as transparent targets. These were coated with 15-120 nm thick layers of different metals (silver, aluminium and copper). The absorbing films were irradiated by a nanosecond KrF excimer laser beam through the quartz plate. The applied fluence was varied in the 150-2000 mJ/cm² range, while the irradiated area was between 0.35 and 3.6 mm². At fluences above the threshold values, it was found that the metal layers were removed from the irradiated spots and the fused silica was etched at the same time. In our experiments, we investigated the dependence of the main parameters (etch rate and threshold) of LIBDE on the absorption of the different metal layers (silver, copper, aluminium), on the size of the irradiated area, on the film thickness and on the number of processing laser pulses.     

蓝宝石基片上制备双面Tl_2Ba_2CaCu_2O_8超导薄膜

在蓝宝石基片上,以CeO2为缓冲层制备了高质量的双面Tl2Ba2CaCu2O8(Tl-2212)超导薄膜。以金属铈靶作为溅射源生长了c轴取向的CeO2缓冲薄膜,并对CeO2薄膜进行了高温处理,有效改善了其结晶质量和表面形貌。采用两步法制备了双面的Tl-2212超导薄膜。XRD测试显示,薄膜为纯的Tl-2212相,且其晶格c轴垂直于衬底表面。超导薄膜的Tc为106K,Jc(77K,0T)为3.5MA/cm2,微波表面电阻Rs(77K,10GHz)为390μΩ。     

Buffer design for nitrogen polarity GaN on sapphire by RF-MBE and application to the nanostructure formation using KOH etching

GaN films were grown by radiofrequency plasma-assisted molecular beam epitaxy on a variety of sapphire substrates with different buffer layer and/or preparation processes, to show the controllability of lattice-polarity selection as well as their applicability to the nanostructure fabrication. Film polarities, which have been checked by reflection high-energy electron diffraction reconstructions and etched morphologies in KOH aqueous solution, were very sensitive to these preparation processes. Ga-polarity GaN could be obtained by an introduction of a high-temperature nitridation and an AlN interlayer deposition, and the N-polarity film with a flat surface and large grains could be grown on a low-temperature-nitrided sapphire in combination with a use of nitrogen-flux modulation sequence, while other pretreatment resulted in the mixed polarities. The resultant morphology of N-polarity GaN after KOH etching clearly reflects crystallographic orientation and the highly anisotropic-etching behavior show the usefulness of the low-temperature-nitrided sapphire for obtaining large-domain N-polarity GaN and the feasibility of nanostructure fabrication without the use of an expensive dry-etching process.     

半球蓝宝石整流罩制造技术研究

整流罩在高速飞行中既要对空气进行整流,同时又起光学窗口的作用。蓝宝石材料硬度高,加工非常困难。分别从精磨模、精磨磨料、抛光膜层、抛光辅料、机床速度和压力等方面介绍了一种加工蓝宝石整流罩的工艺方法。     

干冻磨削用低温冷风发生系统的设计

低温冷风发生系统是研究和应用低温冷风磨削的前提,低温冷风磨削是绿色磨削技术的重要分支之一。采用以单级蒸汽压缩制冷系统为核心,设计了一套干冻磨削用低温冷风发生系统,对该系统流程做了详细的描述及各个系统装置进行了详细的介绍。该低温冷风发生系统设计合理、结构简单、易于控制和操作。     

Generation and removal of pits during chemical mechanical polishing process for MgO single crystal substrate

Magnesium oxide (MgO) single crystal is an important substrate for high temperature superconductor, ferroelectric and photoelectric applications. The function and reliability of these devices are directly affected by the quality of polished MgO surface because any defect on the substrate, such as pit or scratch, may be propagated onto device level. In this paper, chemical mechanical polishing (CMP) experiments were conducted on MgO (1 0 0) substrate using slurry mainly comprised of 1-hydroxy ethylidene-11-diphosphonic acid (HEDP) and silica or ceria particles. Through monitoring the variations of the pits topography on substrate surface, generation and removal mechanism of the pits were investigated. The experimental results indicate that the pits were first generated by an indentation or scratch caused by particles in the slurry. If the rate of chemical etching in the defect area is higher than the material removal rate, the pits will grow. If chemical reaction in the defect area is slower than the material removal rate, the pits will become smaller and eventually disappear. Consequently, these findings may provide insight into strategies for minimizing pits during CMP process.     

Structural and optical properties of SrCu2O2 films deposited on sapphire substrates by pulsed laser deposition

We deposited SrCu₂O₂ (SCO) films on sapphire (Al₂O₃) (0 0 0 1) substrates by pulsed laser deposition. The crystallographic orientation of the SCO thin film showed clear dependence on the growth temperature. X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis showed that the film deposited at 400 °C was mainly oriented in the SCO [2 0 0] direction, whereas when the growth temperature was increased to 600 °C, the SCO film showed a dominant orientation of SCO [1 1 2]. The SCO film deposited at 500 °C was obvious polycrystalline, showing multi peaks from (2 0 0), (1 1 2), and (2 1 1) diffraction in the XRD spectrum. The SCO film deposited at 600 °C showed a band gap energy of 3.3 eV and transparency up to 80% around 500 nm. The photoluminescence (PL) spectra of the SCO films grown at 500 °C and 600 °C mainly showed blue-green emission, which was attributed to the intra-band transition of the isolated Cu⁺ and Cu⁺–Cu⁺ pairs according to the temperature dependent-PL analysis.     

Comparative study on BIS thiourea cadmium acetate crystals using HRXRD, etching, microhardness, UV-visible and dielectric characterizations

〈1 1 1〉 oriented bis thiourea cadmium acetate (BTCA) crystal of diameter 15 mm and length 45 mm was grown for the first time by the unidirectional Sankaranarayanan-Ramasamy (SR) method. The conventional and SR method grown BTCA crystals were characterized by using high-resolution X-ray diffraction (HRXRD), chemical etching, Vickers microhardness, UV-vis, dielectric studies and differential scanning calorimetry. The HRXRD analysis indicates that the crystalline perfection of SR method grown crystal is good without having any low angle internal structural grain boundaries. The transmittance of SR method grown BTCA is 14% higher than that of conventional grown crystal. The dielectric constant was higher and the dielectric loss was less in SR method grown crystal. The crystals grown by SR method possess less dislocation density and higher microhardness.     

XRD与SEM的钢渣尾渣物理激发机理研究

钢渣是冶金工业中产生的主要固体废弃物,其产量约为每年粗钢产量的15%~20%。由于技术的局限,导致我国钢渣利用率较低,仅为年钢渣产量的10%;同时加之管理制度的不健全,导致钢渣大量露天堆放,对土地资源、地下水源,以及空气质量造成严重影响。固体废弃物再利用是资源可持续发展的重要途径之一,由于钢渣的主要化学成分(CaO,SiO₂,A1₂O₃,MgO,Fe₂O₃,MnO,f-CaO等)、主要矿物组成(硅酸三钙、硅酸二钙、钙镁橄榄石、钙镁蔷薇辉石、铁酸二钙等)与水泥熟料的主要化学成分、主要矿物组成极为相似,是一种具有潜在胶凝活性的胶凝材料。以钢渣尾渣作为研究对象,采用机械研磨的方式对钢渣尾渣处理,即物理激发,获得不同粒径钢渣尾渣微粉。依据《用于水泥和混凝土中的钢渣粉》(GB/T 20491-2006)与《水泥胶砂强度检验方法(ISO法)》(GB/T 17671-1999)制备一系列钢渣尾渣胶砂试块(分别标记为A₄₀,A₆₀,A₈₀,A₁₀₀和A₁₂₀)。研究对钢渣尾渣胶凝活性的影响,以及不同水化时间对钢渣尾渣胶凝活性的影响,即3 d钢渣尾渣胶砂强度、7 d钢渣尾渣胶砂强度与28 d钢渣尾渣胶砂强度。利用激光粒度分析仪(LPSA)对钢渣尾渣微粉的粒径分布进行测试与分析,X射线衍射仪(XRD)对钢渣尾渣微粉与钢渣尾渣胶砂的矿物组成进行测试与分析,扫描电子显微镜(SEM)进行微观形貌测试与分析,从而获得钢渣尾渣的物理激发机理。结果表明,随着钢渣尾渣微粉粒径的减小,其胶凝活性呈现先增加后降低的趋势,当研磨时间为80 min时,A₈₀钢渣尾渣微粉的胶凝活性最高,即3 d活性指数为67.55%、7 d活性指数为71.96%和28 d活性指数为73.61%。随着钢渣尾渣微粉粒径的减小,钢渣尾渣微粉中RO相的XRD特征峰强度稳定,Ca₂SiO₄与Ca₃SiO₅的XRD特征峰强度呈现先增加后降低的趋势,Ca₃SiO₅与Ca₂SiO₄参与水化反应,生成一定量的Ca(OH)₂与C-S-H凝胶,具有良好的胶凝活性。A₈₀钢渣尾渣微粉中Ca₂SiO₄含量较少,而Ca₃SiO₅含量较多,均可以生成一定量的Ca(OH)₂与C-S-H凝胶,小幅提高A₈₀钢渣尾渣胶砂的早期(3~7 d)力学性能,大幅提高A₈₀钢渣尾渣胶砂的中、后期(7 d~28 d)力学性能。当水化时间3 d时,A₈₀钢渣尾渣胶砂中存在少量水化产物且大量分散小颗粒;当水化时间7 d时,A₈₀钢渣尾渣胶砂中水化产物大幅增加且形成较大颗粒;当水化时间28 d时,A₈₀钢渣尾渣胶砂中形成大量水化产物且几乎不存在分散小颗粒。从而进一步实现固体废弃物的资源化再利用,达到钢铁企业增加效益,环境缓解压力的目的。     

Wavelength dispersive X-ray analysis and cathodoluminescence techniques for monitoring the chemical removal of AlInN on an N-face GaN surface

This paper shows the selective etching process of an AlInN sacrificial layer, lattice-matched to GaN, on N-face GaN by an aqueous solution of 1,2-diaminoethane. Using the wavelength dispersive X-ray (WDX) spectrometers on an electron probe micro-analyser, together with an optical spectrometer and silicon CCD array added to the light microscope, and sharing the same focus as the electron microscope, cathodoluminescence spectra are collected from exactly the same spot as sampled by the WDX spectrometers. This technique allows the compositional properties of the etched AlInN layer and the optical properties of the semiconductor layers underlying the sacrificial layer to be scrutinised, verifying the etching selectivity and the efficiency of the process.     

微晶硅薄膜沉积过程中的等离子体光学与电学特性研究

采用空间分辨光发射谱和傅里叶变换功率阻抗分析仪研究了衬底偏压和辉光功率对微晶硅薄膜沉积过程中的等离子体光学与电学特性的影响.研究表明：在交流偏压(AC)、悬浮(floating)、负直流加交流(-DC＋AC)偏压下,Hα发射强度空间分布规律相似,平均鞘层长度相等;正直流加交流(＋DC＋AC)偏压和接地(grounded)时Hα发射强度显著增强,并存在双峰(double layers)现象.增大功率,Hα发射强度也随着增大,并在17W与22W之间产生跳变.电学测试发现功率增大,等离子体电阻降低,电抗降低,电 关键词： 等离子体 光发射谱 衬底偏压 辉光功率     

Study on the relationships between Raman shifts and temperature range for a-plane GaN using temperature-dependent Raman scattering

In this paper, Raman shifts of a-plane GaN layers grown on r-plane sapphire substrates by low-pressure metal-organic chemical vapor deposition (LPMOCVD) are investigated. We compare the crystal qualities and study the relationships between Raman shift and temperature for conventional a-plane GaN epilayer and insertion AlN/AlGaN superlattice layers for a-plane GaN epilayer using temperature-dependent Raman scattering in a temperature range from 83 K to 503 K. The temperature-dependences of GaN phonon modes (A₁ (TO), E₂ (high), and E₁ (TO)) and the linewidths of E₂ (high) phonon peak are studied. The results indicate that there exist two mechanisms between phonon peaks in the whole temperature range, and the relationship can be fitted to the pseudo-Voigt function. From analytic results we find a critical temperature existing in the relationship, which can characterize the anharmonic effects of a-plane GaN in different temperature ranges. In the range of higher temperature, the relationship exhibits an approximately linear behavior, which is consistent with the analyzed results theoretically.