Präparation und Charakterisierung von Granateinkristalloberflächen

The preparation of single crystal substrates of gadolinium gallium garnet as a typical example of a brittle material is described. The mechanical polishing with iron oxide and diamond as well as a mechano-chemical polishing procedure basing on SiO₂/H₃PO₄ are investigated. Working damage is investigated by X-ray topography, double crystal spectrometry and selective etching. Results are discussed in the frame of a brittle fracture model of the abrasion process.     

A study of the morphology and magnetic properties of silicon whiskers

Methods of growing Si whiskers are considered and the results of studying their magnetic susceptibility χ are reported. Silicon whiskers are grown using the method of chemical transport reactions in a closed bromide system. The crystals studied were divided into four groups: (i) crystals 0.1–0.9 μm in diameter, (ii) twinned crystals 1–2 μm in diameter, (iii) needle-like crystals from 5 to 1500 μm in diameter, and (iv) isometric crystals (the latter were not measured). With an increase in diameter, the whiskers of the first group changed their state from paramagnetic to diamagnetic, while the crystals of the third group showed a transition from a diamagnetic to a paramagnetic state. All these crystals show a nonlinear dependence of χ on the strength of an external magnetic field H; the nonlinearity increases with increasing the sample paramagnetism. The susceptibility of twinned samples is diamagnetic and close to the value of χ for bulk silicon, and the nonlinearity of the dependence χ (H) is insignificant. The measured values of χ of Si whiskers are explained by features of their crystal structure and chemical composition.     

Über die Zerfallsstruktur des Ni-Katalysators und die Ni(C)-Phase des Diamanten bei der Diamantsynthese

The nature of intermediate phases in the Ni C system is discussed and the concentration dependence of the specific atomic volume is determined. Decomposition structures of Ni C samples exposed to high pressures and temperatures are studied metallographically and by X-ray diffraction. The specific atomic volume of Ni(C) decomposition phase and of Ni(C) satellite phase of Diamond is measured by the asymmetric powder method and from this the concentration of carbon is ascertained. It is stated that the Ni(C_y) satellite phase of diamond — the terminal solid solution of carbon in nickel approximately contains 3 at.% of carbon. It is concluded from this that this phase is the result of the last stage of decomposition of carbon supersaturated catalyst. Thus, the intermediate phase is playing no important role in diamond nucleation.     

Geometric modeling of homoepitaxial CVD diamond growth: I. The {1 0 0}{1 1 1}{1 1 0}{1 1 3} system

Plasma-assisted CVD homoepitaxial diamond growth is a process that must satisfy many stringent requirements to meet industrial applications, particularly in high-power electronics. Purity control and crystalline quality of the obtained samples are of paramount importance and their optimization is a subject of active research. In the process of such studies, we have obtained high purity CVD diamond monocrystals with unusual morphologies, namely with apparent {1 1 3} stable faces. This phenomenon has led us to examine the process of CVD diamond growth and build up a 3D geometrical model, presented here, describing the film growth as a function of time. The model has been able to successfully describe the morphology of our obtained crystals and can be used as a predictive tool to predetermine the shape and size of a diamond crystal grown in a given process configuration. This renders accessible control of desirable properties such as largest usable diamond surface area and/or film thickness, before the cutting and polishing manufacture steps take place. The two latter steps are more sensitive to the geometry of the growth sectors, which will be addressed in a companion paper.Our model, applicable to the growth of any cubic lattice material, establishes a complete mapping of the final morphology state of growing diamond, as a function of the growth rates of the crystalline planes considered, namely {1 0 0}, {1 1 1}, {1 1 0}, and {1 1 3} planes, all of which have been observed experimentally in diamond films. The model makes no claim as to the stability of the obtained faces, such as the occurrence of non-epitaxial crystallites or twinning. It is also possible to deduce transient behavior of the crystal morphology as growth time is increased. The model conclusions are presented in the form of a series of diagrams, which trace the existence (and dominance) boundaries of each face type, in presence of the others, and where each boundary crossing represent a topology change in terms of number of faces, edges and vertices. We validate the model by matching it against crystals published in the literature and illustrate its predictive value by suggesting ways to increase usable surface area of the diamond film.     

Erosivität und Mechanolumineszenz

One of the complicated properties of solids is also their erosivity. An exact and simple definition makes the erosivity as an easy measurable property of solids. The erosion which is the reason of erosivity has two aspects: 1. technological as an working procedure, 2. methodical as a method for the measuring of erosivity. Because with the erosion there are two objects in interaction, the abrasive particles and the material to be machined — with their collision deformations occurs. It is possible in some cases to observe mechanoluminescence. The mechanoluminescence can be used as to the interpretation of the erosionsmechanism as to the regulation of the experimental collisions.     

Oberflächenmorphologie und Gleitverhalten trikliner Einkristalle von TCNQ-Komplexsalzen

The electron microskopic investigation of the most important crystal faces of the TCNQ-complex salts with triphenylmethylphosphonium and with triphenylmethylarsonium showed growth accessories and etch pits but also slide steps which could be provocated intentionally as by local deformations with a needle point as by axial pressure deformation. The orientation of the slide steps in different crystal faces leads to (010) as the slide plain. Axial pressure normal to the (010) faces caused unexpected strong shear deformation, which could serve for the estimation of the slide directions parallel to [101] or [101]. The sliding and cleaving parallel to (010) is favoured by the crystal structure, for (010) being parallel to a „smooth”︁ net-plain not crossed by overlapping molecules.     

Leitfähigkeits- und Halleffektmessungen an Tellur-Epitaxieschichten auf KCl

The temperature dependence of resistivity of epitactixial thin tellurium films grown on (110) KCl is contrary to the results well known from single crystals. For interpretation of this discrepancy a model is proposed which makes use of piezoresistance effects. This model is in qualitative and quantitative agreement with measurements.     

Synthetic Diamond — Basic Research and Applications

Non-equilibrium growth of synthetic diamond layers by chemical vapour deposition (CVD) techniques on heterosubstrates has largely been improved over the past decade. On silicon substrates highly textured and oriented diamond films can be grown with optical transparencies and thermal conductivities suitable for broad-band optical windows and heat spreaders. Boron pulse-doping of homoepitaxial diamond layers leads to high p-conductivity at room temperature allowing the fabrication of Schottky diodes and field effect transistors operating at temperatures up to 1000 K. Other devices such as sensors and detectors are being successfully fabricated. At the same time many basic questions remain to be solved including efficient n-type doping.     

Versetzungsätzungen und Mikrohärtemessungen an druckverformten Reinsteiseneinkristallen

The dislocation occurring at single or repeated loading in metals is mainly explained by the dislocation process. The results of investigation available are a contribution to the detection of the connection between dislocation density and work-hardening.     

金刚石单晶高温高压合成中氮对硫的影响

为了研究在金刚石大单晶生长过程中氮对硫的影响,在6.5 GPa高压条件下采用温度梯度法分别研究了两种不同合成体系中金刚石的合成.利用傅里叶显微红外光谱(FTIR)仪对所合成的金刚石进行了测试,测试结果表明:晶体中(a)中不含有氮,晶体中(b)中氮的浓度为280 ppm.此外,对所合成的样品进行了X射线光电子能谱测试,测试结果表明:在Ib型金刚石中有硫元素存在,而硫未进入到IIa型金刚石中.因此,金刚石中氮的存在对金刚石中硫的进入有促进作用.     

Structure of autoepitaxial diamond films

A reflection high energy electron diffraction (RHEED) method has been used to investigate the structural peculiarities of synthetic diamond autoepitaxial films, deposited from a gaseous phase onto natural diamond seed crystal. The diamond films on the (111) and (110) faces usually have internal stresses, which cause the (111) plane microtwinning process at thicknesses of about 1000 Å. The thickness of twin lamellas is about 0.01?1μm. On the (100) face the diamond films do not undergo twinning and have a high structural perfection.     

GaN grown on (1 1 1) single crystal diamond substrate by molecular beam epitaxy

GaN epilayers are grown on (1 1 1) oriented single crystal diamond substrate by ammonia-source molecular beam epitaxy. Each step of the growth is monitored in situ by reflection high energy electron diffraction. It is found that a two-dimensional epitaxial wurtzite GaN film is obtained. The surface morphology is smooth: the rms roughness is as low as 1.3 nm for 2×2 μm² scan. Photoluminescence measurements reveal pretty good optical properties. The GaN band edge is centred at 3.469 eV with a linewidth of 5 meV. These results demonstrate that GaN heteroepitaxially grown on diamond opens new rooms for high power electronic applications.     

化学气相沉积(CVD)金刚石研究现状和发展趋势

化学气相沉积(CVD)技术的发展使得金刚石优异的综合性能得以充分发挥,在诸多领域获得应用,并有可能实现跨越式的发展。色心使得金刚石量子加速器初步显示了巨大可行性,包括紫外激光写入窗口等诸多应用场景将金刚石的光、电、热和力学综合优势发挥到了极致,超宽禁带金刚石半导体应用将很快实现,金刚石的散热应用也在不断拓展。本文在总结CVD金刚石的制备方法和性能特点的基础上,根据金刚石的本征特点和应用领域,将其分为量子级、电子级、光学级、热学级和力学级五类,对各类金刚石的研究和应用状况进行了详细阐述,进一步明晰CVD金刚石目前的发展状态,对研判其未来发展趋势有重要意义。     

高温高压与CVD金刚石单晶衬底质量对比研究

本文通过高分辨X射线衍射(HRXRD)、激光拉曼光谱(Raman)、晶格畸变检测等测试分析方法对多组高温高压(HTHP) Ⅰb、HTHP Ⅱa和化学气相沉积(CVD)型(100)面金刚石单晶样品进行对比研究。HRXRD和Raman的检测结果均表明HTHP Ⅱa型金刚石单晶的结晶质量接近天然金刚石,其XRD摇摆曲线半峰全宽和Raman半峰全宽分别为0.015°~0.018° 和1.45~1.85 cm^-1。晶格畸变检测仪的检测结果表明,HTHP Ⅱa型金刚石单晶的应力分布主要有两种:一种几乎无明显应力分布,另一种沿<110>方向呈对称的放射状分布,其他区域无晶格畸变。HTHP Ⅰb和CVD型金刚石单晶应力分布均相对分散,晶格畸变复杂,与其HRXRD和Raman的检测结果相符。进一步利用等离子体刻蚀法对三种类型金刚石单晶(100)面位错缺陷进行对比分析,结果表明,HTHP Ⅱa型金刚石位错密度为三者中最低,仅为1×10³ cm^-2。本研究为制备高质量大尺寸CVD金刚石单晶的衬底选择提供了实验依据。     

NiMnCo粉末触媒合成金刚石特征的研究

本文采用扫描电子显微镜(SEM)、图象分析仪和金刚石性能测试仪分别对粉末状和片状NiMnCo触媒合成的金刚石形貌、(111)、(100)结晶面的微形貌、包裹体分布及其力学性能进行分析.研究结果表明:与片状触媒合成的金刚石相比,NiMnCo粉末触媒合成的金刚石呈典型的六-八面体,晶型完整率高;(111)、(100)结晶面完整无缺陷,透明度高、包裹体少且细小分散.因此,NiMnCo粉末触媒合成的金刚石具有较高的静压强度和热稳定性.     

离子轰击增强金刚石膜与Si衬底结合力的进一步研究

由于金刚石与Si有较大的表面能差,利用化学气相沉积(CVD)制备金刚石膜时,金刚石在镜面光滑的Si表面上成核困难,而负衬底偏压能够增强金刚石在镜面光滑Si表面上的成核,表明金刚石核与Si表面的结合力也得到增强.本文分析衬底负偏压引起的离子轰击对Si表面产生的影响之后,基于离子轰击使得Si衬底表面产生了微缺陷(凹坑)增大了金刚石膜与Si衬底结合的面积,理论研究了离子轰击对金刚石膜与Si衬底结合力的影响.     

大尺寸单晶金刚石磨抛一体化加工研究

金刚石因其优异的物理性质被视为下一代半导体材料,然而其极高的硬度、脆性和耐腐蚀性导致其加工困难,尤其是对于大尺寸的化学气相沉积(chemical vapor deposition, CVD)单晶金刚石(SCD)晶片而言,目前还缺乏一种高效、低成本的磨抛加工方法。本文提出一种基于工件自旋转的同心双砂轮磨抛一体化加工技术,在一次装夹中,先采用金刚石磨料的陶瓷内圈砂轮磨削单晶金刚石晶片表面,将单晶金刚石表面迅速平坦化,后采用金刚石与CuO混合磨料的外圈溶胶-凝胶(sol-gel,SG)抛光轮抛光单晶金刚石晶片表面,使其在较短时间内完成从原始生长面(Sa约46 nm)到原子级表面精度(Sa＜0.3 nm)的加工。磨削加工中,硬质金刚石磨料的陶瓷砂轮高速划擦金刚石晶片表面,在强机械作用下获得较大的材料去除以及纳米级的光滑单晶金刚石表面,同时引起进一步的表面非晶化;SG抛光加工中,硬质金刚石磨料高速划擦单晶金刚石表面形成高温高压环境,进一步诱导CuO粉末与单晶金刚石表面的非晶碳发生氧化还原反应,实现反应抛光。磨抛一体化的加工技术为晶圆级的单晶、多晶金刚石的工业化生产提供借鉴。     

磨料形貌及分散介质对4H碳化硅晶片研磨质量的影响研究

研磨作为4H碳化硅(4H-SiC)晶片加工的重要工序之一,对4H-SiC衬底晶圆的质量具有重要影响。本文研究了金刚石磨料形貌和分散介质对4H-SiC晶片研磨过程中材料去除速率和面型参数的影响,基于研磨过程中金刚石磨料与4H-SiC晶片表面的接触情况,推导出简易的晶片材料去除速率模型。研究结果表明,磨料形貌显著影响4H-SiC晶片的材料去除速率,材料去除速率越高,晶片的总厚度变化(TTV)越小。由于4H-SiC中C面和Si面的各向异性,4H-SiC晶片研磨过程中C面的材料去除速率高于Si面。在分散介质的影响方面：水基体系研磨液的Zeta电位绝对值较高,磨料分散均匀,水的高导热系数有利于控制研磨过程中的盘面温度;乙二醇体系研磨液的Zeta电位绝对值小,磨料易发生团聚,增大研磨过程的磨料切入深度,晶片的材料去除速率提高,晶片最大划痕深度随之增大。     

Anisotrope Längenänderungen bei spannungs- und verformungsinduzierter martensitischer Gitterumwandlung kubisch-flächenzentriert → hexagonal

With the elastic and plastic deformation of the steel X8Mn16, respectively, a stress or deformation induced transformation of the fcc γ-matrix lattice into the hex. ϵ-martensite occurs, being connected with anisotropic changes in length, and leading to a decrease of the apparent elastic modulus of the alloy. A further investigation shows it is obviously the question of the result of the strain-memory effect, until now not yet being observed with iron alloys. Similar anisotropic changes in length can be taken into account with all pure metals and alloys, the martensitic transformation of which turns out under the influence of an outer uniaxial stress.