Vapour phase growth of epitaxial silicon carbide layers

After a brief overview of different epitaxial layer growth techniques, the homoepitaxial chemical vapour deposition (CVD) of SiC with a focus on hot-wall CVD is reviewed. Step-controlled epitaxy and site competition epitaxy have been utilized to grow polytype stable layers more than 50 μm in thickness and of high purity and crystalline perfection for power devices. The influence of growth parameters including gas flow, C/Si ratio, growth temperature and pressure on growth rate and layer uniformity in thickness and doping are discussed. Background doping levels as low as 10¹⁴ cm⁻³ have been achieved as well as layers doped over a wide n-type (nitrogen) and p-type (aluminium) range.

Furthermore the status of numerical process simulation is mentioned and SiC substrate preparation is described. In order to get flat and damage free epi-ready surfaces, they are prepared by different methods and characterised by atomic force microscopy and by scanning electron microscope using channelling patterns. For the investigation of defects in SiC high purity CVD layers are grown. The improvement of the quality of bulk crystal substrates by micropipe healing and so-called dislocation stop layers can further decrease the defect density and thus increase the yield and performance of devices. Due to its high growth rate functionality and scope for the use of multi-wafer equipment hot-wall CVD has become a well-established method in SiC-technology and has therefore great industrial potential.     

The texture of GaSb ingots grown by the bridgman method

Crystallographic features of GaSb grown by the Bridgman procedure were investigated by scanning electron microscopy. Chemical etching and the electron channelling method were used to determine the position and crystallographic orientation of crystallites. A pronounced 〈110〉 texture was detected which was misaligned by 5÷28° with respect to the main axes of the ingots. Boundaries were categorized according to the orientation change accross them. Results were compared. The majority of small angle boundaries are probably caused by thermal stresses induced dislocation migration.     

Structural characterization of heteroepitaxial films of CdSe and ZnTe

The effects of composition, orientation and temperature of substrate on the structure and morphology of epitaxial CdSe and ZnTe films are analyzed. Single crystal wafers of zinc telluride and zinc selenide oriented along (110) and natural cleaved mica were used as substrates. This paper presents a complex investigation of the growth mechanism and crystal perfection of the films by optical microscopy, X-ray and electron diffraction, and by electron microscopy. The structure of the transient region of the film substrate interface was studied by X-ray microanalyzer and by scanning electron microscope. Cadmium selenide layers grown on mica had hexagonal structure and were oriented in the (0001) plane, those grown on zinc telluride crystals had cubic structure and orientation along (110). Zinc telluride layers were cubic and were oriented parallel the (111) plane when deposited on mica, and parallel to (110) when deposited on zinc selenide substrates. It is shown that the layers grew by a layer mechanism. Epitaxial growth of cubic cadmium selenide layers on zinc telluride single crystals, as well as of ZnTe layers on ZnSe substrates, made it possible to grow heterojunctions with a low density of misfit dislocations at the interface; this gave rise to intensive injection electroluminescence and effective separation of non-equilibrium charge carriers in such structures.     

Investigation on growth,optical, thermal,mechanical and dielectric studies of Benzimidazolium L-aspartate NLO crystal

The organic salt of Benzimidazolium L-aspartate (BLA) has been synthesised and single crystals were grown by slow evaporation solution growth technique at room temperature using water as the solvent. The grown crystal was subjected to single crystal X-ray diffraction analysis and confirmed it belongs to monoclinic crystal system with space group P2₁/c. The crystalline perfection was studied using High resolution X-ray diffraction (HRXRD). The functional groups were analysed by FT-IR analysis. The optical transmittance and the lower cut-off wavelength of the BLA crystal have been identified by UV-Vis study. The thermal stability of the title crystal was investigated by TGA/DTA analyses. The Vickers microhardness analysis was carried out to study the mechanical strength of the crystal. The dielectric response of the crystal was studied in the frequency range 100 to 5 MHz at different temperatures. The surface morphology of the grown BLA crystal was studied by scanning electron microscopy (SEM). The second harmonic generation efficiency was measured in comparison with KDP by employing Kurtz Perry Powder method.     

Determination of the crystallographic parameters of a fcc metal by means of electron channelling patterns

Indexing and mapping of selected area electron channelling patterns (SAECPs) of an Al‐Zn‐Mg alloy have been performed. Although, channelling patterns are similar for crystals having the same system, since the interplanar spacing and the angular band width depend on lattice parameter, the details of the map will differ for every material. Angles between the poles and the angular separations of channelling bands were measured on the micrographs and calculated with the well known equations and found to be well in agreement within the error limits. Also the channelling line widths were calculated with the help of extinction distances of the reflecting planes. Structure factors and atomic scattering factors for selected reflections were also calculated for the present alloy whose a = 4.054 Å.     

Zur Struktur von organischen Mischkristallschichten

The structure of organic mixed crystal films is investigated by means of a appropriated model - copper phthalocyanine/vanadyl phthalocyanine. These films are polycrystalline and contain mixed crystal grains, the size being smaller than that which can be detected by X-ray methods. By infrared spectroscopy and scanning electron microscopy or after recrystallisation by texture goniometer investigations the orientations of microcrystals on the substrate was obtained.     

Helldunkel-Struktur der Kossel-Interferenzlinien und Kristallstruktur-Analyse (II). Theoretische Linienprofil-Ausläufer und Vergleich mit experimentellen Ergebnissen

As shown in part I of this paper, from a Kossel-line profile the tails are best suited for crystal structure analysis. In this part a general theoretical expression has been derived for the tails of line profile in case of different examples often observed. The theoretical results have been compared with experimental ones. As a consequence two possibilities of application in crystal structure analysis can be recommended: at first the proof of proposals of structure by the use of tails of the profiles including phase information, and secondly the direct evaluation of structure amplitudes in favourable cases. – The dark and bright fields in Kossel patterns can be explained by taking into consideration the long ranging tails of profiles. The physical similarities and differences between Kossel interferences, divergent beam interferences, Kikuchi lines and channelling patterns are considered.     

Synthesis of ZnO nanorods by the thermal reduction process of a mixture of ZnO and Al powder

Single‐crystalline Zinc oxide (ZnO) nanorods were firstly synthesized on gold‐coated Si substrate via a simple thermal reduction method from the mixture of ZnO and Al powder. The growth process was carried out in a quartz tube at different temperature (550‐700 °C) and at different oxygen partial pressure. Their structure properties were investigated by X‐ray diffraction (XRD), scanning electron microscope (SEM), X‐ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The length of the as‐prepared ZnO nanorods was up to several micrometers and their diameters were about 130 nm. The X‐ray diffraction patterns, transmission electron microscopic images, and selective area electron diffraction patterns indicate that the one‐dimensional ZnO nanorods are a pure Single‐crystal and preferentially oriented in the [0001] direction. The reaction mechanism of ZnO nanorods was proposed on the basis of experimental data. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Observations on the growth of NiMoO4 crystals in Silica gel media

Growth of NiMoO₄ crystals by gel method has been described. By manipulating the condition of growth parameters, crystals of fairly large dimensions have been obtained at ambient temperature. The crystal faces are examined by optical and scanning electron microscopy and thus a two-dimensional layer growth mechanism for the development of the faces have been proposed.     

Channeling‐enhanced EDX for polarity resolved crystal orientation determination

Using channeling‐enhanced energy‐dispersive X‐ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non‐centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling‐enhanced, angle‐dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non‐centrosymmetric point group. The method shown here overcomes the limitation of a reduced point‐group sensitivity of electron backscatter diffraction patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections.     

Assembling ultra-thick and crack-free colloidal crystals via an isothermal heating evaporation induced self-assembly method

Ultra-thick and crack-free colloidal crystals have many advantages in a number of existing and emerging applications. In this work, such systems are fabricated by a simple and reproducible method based on assembly of monodisperse silica particles by a crystalline layer assembly technique (CLAT). We find that high quality of colloidal crystals is obtained by using two simple processes: sintering of silica particles and thermal treatment of colloidal crystals. The crack-free colloidal crystal with a thickness of 100 μm is fabricated. The morphologies and microstructures of colloidal crystals are identified by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The reflection spectra are measured by UV-VIS spectrum measurement. The reflection spectra of the colloidal crystal with different thicknesses are calculated by using multiple scattering methods. When the thickness of the colloidal crystal is smaller than 60 μm, the reflection spectra of experimental measurements agree very well with that of theoretical calculations.     

KMnO4与醇类有机物制备MnOOH的研究

在140℃的条件下,用KMnO4分别与甲醇、乙醇、丙醇、丁醇、乙二醇、1,3-丙二醇以及1,4-丁二醇进行水热反应24 h。采用X射线粉末衍射(XRD)与环境扫描电子显微镜(SEM)对反应产物进行表征。结果表明,KMnO4与乙醇、丙醇、丁醇以及1,4-丁二醇反应均可以得到较纯的棒状MnOOH晶体。KMnO4与甲醇、1,3-丙二醇反应不仅得到了MnOOH晶体并且也得到Mn3O4晶体,而与乙二醇的反应只得到了Mn3O4晶体。并简单探讨了形成这种规律的原因。     

OM- and SEM investigations on the laser damage of tellurium dioxide single crystals

By means of optical (OM) and scanning electron microscopy (SEM) the morphological changes involved by intensive laser pulses in tellurium dioxide single crystals, were investigated. The typical morphological characteristics of the damaged crystal regions will be described and discussed.     

Investigation of the Microstructure of Crystals Surfaces by the Method of Self-decoration during Ion Bombardment

A method is developed for self-decoration with ion bombardment by which the surface structure of crystal samples is investigated. The existing surface structure of the objects, as well as the additionally developed structure after prolonged ion bombardment are visualized by this method. When using scanning electron microscopy the method allows multiple investigation of the sample or of one and the same parts of it respectively. The mechanism of the method is revealed by the results obtained in the performed experiments. It is proved that the crystal surface and its decoration depend on the peculiarities of the crystal structure and on the conditions of bombardment. By varying the conditions of ion bombardment the sensitivity of the method is considerably changed.     

Investigation of crystal lattice defects of PbZrO3 single crystals by transmission electron microscopy

The investigation of PbZrO₃ single crystal structure was carried out by the method of transmission electron microscopy (TEM). It is shown that extended planar defects, slip lines, twins, and morié patterns are observed in PbZrO₃.     

TEM investigation of precipitates in VCz GaAs crystals

Bulk GaAs crystals were grown from various Ga‐rich melts by the vapour‐pressure controlled Czochralski method in order to reduce As precipitates. The correlation of the melt composition with both, structural perfection and solid composition was examined by various methods of transmission electron microscopy (TEM). From transmission electron diffraction and diffraction contrast imaging a direct correlation between melt composition and sample properties is missing. High‐resolution TEM imaging hints to inhomogeneities only for the sample grown from a melt with a mole fraction of y = 0.492. Strain analysis of a selected defect reveals a strained crystal lattice in the surrounding of the defect. For the same sample, high angle annular dark‐field imaging and energy dispersive X‐ray spectroscopy verify the formation of precipitates. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

烧结法制备高炉渣CMAS系统微晶玻璃的研究

利用高炉渣及其它辅助原料制备基础玻璃,采用一步烧结法制备主晶相为辉石的CaO-MgO-Al2O3-SiO2(CMAS)微晶玻璃.综合运用DSC,XRD以及场发射扫描电子显微镜等测试手段,分析热处理制度对高炉渣CMAS微晶玻璃的析晶行为及性能的影响.结果表明:随着热处理温度上升,微晶玻璃的主晶相均为辉石,次晶相均为长石,晶相析出量增加,微晶玻璃的体积密度及抗折强度均呈现先增后减趋势.随着热处理时间增加,微晶玻璃的体积密度及抗折强度均呈现下降趋势.当热处理温度为1020 ℃,晶化时间30 min时,样品的机械性能最好,体积密度为2.690 g·cm-3,抗折强度为67.00 MPa.     

Peculiarities of the growth of KDP single crystals with incorporated aluminium oxyhydroxide nanoparticles

Grown for the first time are KH₂PO₄ (KDP) crystals with incorporated aluminium oxyhydroxide Al₂O₃·nH₂O nanoparticles (n=3.5–3.6). The influence of the nanoparticles on the structure perfection and the growth kinetics of the crystal faces are studied. The presence of the nanoparticles in the crystal matrix is confirmed by the results of chemical analysis, X-ray diffraction (XRD) analysis and transmission electron microscopy (TEM). The most essential inhibiting effect of the nanoparticles is observed for the {100} faces. The mechanism of influence of the nanoparticles on the {100} faces growth is explained on the base of the Cabrera–Vermilyea (C–V) model using Langmuir adsorption isotherm.     

六钛酸钾晶须的制备及生长机理的研究

通过KDC方法成功制备了六钛酸钾(K2Ti6O13)晶须,并进行了热重分析和差热分析,研究烧结时间和烧结温度对K2Ti6O13晶须结晶过程的影响,通过X射线衍射分析了K2Ti6O13晶须的相组成和晶体指数.此外,通过扫描电子显微镜和透射电子显微镜研究晶须的微观结构,揭示了K2Ti6O13晶须的生长机理.     

Emissionsmikroskopische Untersuchungen zur Änderung der Sekundärelektronenemission bei der plastischen Verformung

Both the electron optical image contrast and the electron current density of all crystal grains decrease by plastic deformation of polycrystalline samples in a secondary electron emission microscope with conventional high vacuum. As a presumption both the sample temperature and the vacuum must be so high that the secondary electron yield does not change during the variation of these parameters. After recrystallisation the electron current densities of the crystallites with preserved orientation return to those of the initial stage. From these results it follows that a connection exists between secondary electron yield and crystal lattice perfection. A qualitative explanation of this connection is tried.