Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likely due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.     

人造金刚石晶体缺陷的同步辐射X射线衍射形貌像浅析

利用同步辐射X射线对人造金刚石晶体缺陷进行了形貌学研究,实验采用了透射(劳埃)形貌术和反射形貌术两种方法.所得的X射线透射劳埃图上大部分斑点分别分布在四条主晶带上,经分析发现,该金刚石晶体主要的晶体缺陷为位错,并推导出晶体内部存在Frank不全位错.该晶体的反射形貌像中位错呈网状分布,说明其表层缺陷多于内部缺陷.此外,由形貌像分析发现该人造金刚石晶体的晶体缺陷明显少于天然金刚石.     

X-ray Topographic Defects' Contrast on Synthetic Quartz

In the present study the linear defects in several synthetic quartz have been surveyed by X-ray topography using Lang method. The grown-in dislocations produced by layers displacement around holes, precipitates or inclusions are discussed. Each growth zone is described with their own defects pattern and some correlations with the external morphology of the crystal are stated. There are also pointed out the asymmetry of the defects for every growth zone and the specific role in the growth mechanism of the s-growth zone. In the final part of the work there are outlined the general and the specific conclusions.     

Crystal growth and dislocation arrangement of Czochralski alexandrite (BeAl2O4:Cr) single crystals

The [001] oriented alexandrite (BeAl₂O₄:Cr) single crystals have been grown by the Czochralski pulling technique. The X-ray topographic investigation indicates that the grown-in dislocations mainly originate from the seed and propagate along the path normal or nearly perpendicular to the growth interface. The dislocation density and arrangement is closely related to the quality of the seed crystal.     

The dependence of anomalous temperature peak of a deforming stress on microstructural parameters

The temperature dependence of a deforming stress (including both low-temperature decreasing branch and an anomalous high-temperature peak) has been calculated on the basis of one mechanism. The theory developed takes into account spontaneous thermally activated processes of dislocation locking and unlocking and describes the transition from conventional dislocation gliding to the jumpwise motion of dislocations with the change of the temperature (in full accordance with the in situelectron microscopy observations). The dependences of the plasticity characteristics (flow stress, strain-rate sensitivity, etc.) on the microstructural parameters such as free dislocation path and the energy barriers that should be overcome by dislocations for transformation of their cores from the “gliding” to the “sessile states” and back have also been determined.     

静压触煤法制备的人造金刚石中的晶体缺陷

本文首次采用透射电子显微术系统地研究了由FeNi触媒制备的金刚石单晶的微观结构,分析了人造金刚石中存在的晶体缺陷,探讨了这些晶体缺陷形成的原因,研究发现金刚石中存在层错,棱柱位错,位错列和位错网络等晶体缺陷,研究结果表明,金刚石中的晶体缺陷与金刚石的高温高压合成过程密不可分,主要起源于金刚石中大量过饱和的空位和观杂质所引起的内应力。     

X-ray diffraction characterization of epitaxial CVD diamond films with natural and isotopically modified compositions

Comparative investigations of homoepitaxial diamond films with natural and modified isotopic compositions, grown by chemical vapor deposition (CVD) on type-Ib diamond substrates, are carried out using double-crystal X-ray diffractometry and topography. The lattice mismatch between the substrate and film is precisely measured. A decrease in the lattice constant on the order of (Δa/a)_relax ～ (1.1–1.2) × 10^–4 is recorded in isotopically modified ¹³С (99.96%) films. The critical thicknesses of pseudomorphic diamond films is calculated. A significant increase in the dislocation density due to the elastic stress relaxation is revealed by X-ray topography.     

DKDP晶体的柱面形貌与缺陷分析

采用原子力显微镜观测全方位生长的DKDP晶体的{100}面形貌,发现有螺旋位错,由此推断DKDP晶体{100}面以螺旋位错机制生长;利用同步辐射X射线白光形貌术观测了DKDP晶体缺陷,探讨了不同生长条件及生长阶段对晶体完整性的影响.     

Dislocation density in heteroepitaxial indium arsenide layers

In As layers have been grown by CVD on (111)B-oriented GaAs substrates. The dislocation density (N_D) distribution through the layer thickness has been studied. N_D is dependent on the mole fraction of AsCl₃ in the gaseous phase and, consequently, on the current carriers concentration. This results in the supposition that the decreasing of N_D in the layers after a “critical” thickness is due to the “pinning” of dislocations at impurity atoms which form stronger bonds with the host In or As atoms than the bond In–As, an effect which is known for bulk GaAs and InP crystals.     

Optimization of the Growth Technology for Crystals with Garnet Structure Based on X-Ray Diffraction Data

High efficiency of the methods of double-crystal X-ray diffractometry (DCXRD) and topography for improving the growth technology of highly homogeneous crystals has been demonstrated on the example of gadolinium gallium garnet (GGG) single crystals. The main types of structural defects observed in Czochralski-grown GGG crystals are found to be macroscopic inhomogeneity of composition distribution, caused by the facet effect manifestation; microinhomogeneous distribution of impurity and main components of the composition in striations; dislocations; and second-phase inclusions. The relationship between the type and density of newly formed defects and the technological conditions for crystal growth are considered. Optimization of the composition of crystals and their growth technology made it possible to obtain high-quality dislocation-free crystals of GGG and complex-substituted garnets on its basis for magneto-optical and microwave devices, elements of solid-state lasers, and other applications.     

金刚石UV-Vis-MIR光谱常见特征综述

金刚石分类体系经过上百年发展已趋于成熟。以光谱为基础的分类依据是紫外可见近红外光谱(UV-Vis-NIR)和中红外光谱(MIR),主要涉及氮、硼杂质元素,所识别的有关晶格缺陷模型已得到较为合理的解释,但大量的晶格缺陷,包括跟氮有关的晶格缺陷研究尚不透彻,这将限制金刚石应用领域的开拓进程。本文汇集了金刚石紫外-可见光-红外光光谱中呈现的部分吸收特征,特别是对金刚石分类系统进行了完整地说明。除此以外,一些在光谱中较易识别的特征,也已经有了较为合理的理论解释和结构模型,总结汇总这些谱学特征以及其对应的结构模型,可以为金刚石材料的进一步研究和应用提供参考。     

Nucleation,Glide Velocity and Blocking of Misfit Dislocations in SiGe/Si

Relaxation of strained layer systems is still not well understood. It is time dependent and changes considerably for samples with different growth history. This has to be discussed in terms of nucleation, glide velocity and blocking of misfit dislocations. We have investigated these phenomena at samples with SiGe layer thicknesses ranging from 60 nm up to 120 nm grown by molecular beam epitaxy (MBE) or chemical vapor deposition (CVD) by means of X-ray topography. The samples were annealed at temperatures between 500° and 600° C. Nucleation of misfit dislocations is heterogeneous and the rate is obviously dependent on layer strain and thickness. A quantified nucleation rate was not yet accessible, mainly due to the preferential formation of dislocation bundles. The propagation velocities of misfit dislocation segments were measured during annealing by means of synchrotron radiation plane wave topography (reflection geometry). The values agree well with theory and there is no evidence that they depend on growth regime. It is shown that the interaction of propagating misfit dislocations with crossing ones may lead to blocking or cross slip in different glide systems. These results are corroborated by investigations with atomic force and transmission electron microscopy.     

Reduction of grown-in dislocation density in Ge Czochralski-grown from the B2O3-partially-covered melt

Germanium (Ge) single crystals with an extremely low density of grown-in dislocations were grown by the Czochralski (CZ) technique with boron oxide (B₂O₃) liquid. Because attachment of particles floating on the melt surface to a growing Ge crystal leads to generation of dislocations during the growth, partial covering of the Ge melt surface with B₂O₃ liquid was attempted. Such attachment of particles was drastically suppressed or the particles were caught by the introduction of B₂O₃ liquid, and a particle-free Ge melt was realized in the central region of the melt surface. Ge single crystals were successfully grown from such melt, the grown-in dislocation density being 0–1×10³ cm⁻², which was remarkably lower than that in Ge crystals grown by a conventional CZ technique. The contaminations by B and O atoms of the grown crystal detected by SIMS analysis were very low. These Ge crystals have the potential for application to be applied as high-quality, dislocation-free substrates of GaAs solar cells for various usages including in space.     

Characterization of the carrot defect in 4H-SiC epitaxial layers

Characterization of the epitaxial defect known as the carrot defect was performed in thick 4H-SiC epilayers. A large number of carrot defects have been studied using different experimental techniques such as Nomarski optical microscopy, KOH etching, cathodoluminescence and synchrotron white beam X-ray topography. This has revealed that carrot defects appear in many different shapes and structures in the epilayers. Our results support the previous assignment of the carrot defect as related to a prismatic stacking fault. However, we have observed carrot defects with and without a visible threading dislocation related etch pit in the head region, after KOH etching. Polishing of epilayers in a few μm steps in combination with etching in molten KOH and imaging using Nomarski optical microscope has been used to find the geometry and origin of the carrot defects in different epilayers. The defects were found to originate both at the epi-substrate interface and during the epitaxial growth. Different sources of the carrot defect have been observed at the epi-substrate interface, which result in different structures and surfaces appearance of the defect in the epilayer. Furthermore, termination of the carrot defect inside the epilayer and the influence of substrate surface damage and growth conditions on the density of carrot defects are studied.     

Bulk and surface components of electric influence on the magnetoplasticity

The influence of weak electric fields on the magnetically induced mobility of individual dislocations in NaCl crystals has been investigated. It is shown that the strong influence of an electric field on the magnetoplasticity, which is caused by the transformation of impurity centers at dislocations from the diamagnetic state (Me ⁺⁺) to the paramagnetic state (Me ⁺), has both bulk and surface components. The surface effect dominates over the bulk one in weak electric fields (E < 0.5 kV/m), which are insufficient for the exciting bulk electromigration of charged defects near dislocations. However, the contribution of the surface effects becomes insignificant in comparison with the bulk processes in stronger fields E. Lacquering crystal faces to block the surface electromigration of defects excludes this stimulation component at any E. It is shown that dislocation motions occurring due to a rapid switching on an electromagnet also disappear in lacquered samples. These effects observed may be related to the same surface electromigration of defects under the vortex electric fields induced by switching on a magnetic field.     

Nature of dislocations promoting growth in liquid phase epitaxy of gallium arsenide

Dislocations promoting growth in the course of liquid phase epitaxy (LPE) of GaAs layers on GaAs substrates are analysed by X-ray topography. The Burgers vectors are determined by comparing double-crystal back-reflection images with calculated misorientations taking into account surface relaxation. Any dislocation which generates a spiral of elementary steps is found to have a Burgers vector component parallel to the macroscopic growth direction. The nature of these growth promoting dislocations may be between pure screw and pure edge type. Defects which might be responsible for the generation of the observed concentric growth step patterns are below the detection limit of current X-ray topography.     

非线性光学晶体BaAlBO3F2的生长与缺陷研究

采用B2O3-LiF-NaF助熔剂体系、中部籽晶法生长出BaAlBO3F2(BABF)晶体,对该晶体的弱吸收性能进行了表征.利用同步辐射白光X射线形貌术和化学腐蚀法研究了BABF晶体的缺陷,观察到BABF晶体中的主要缺陷是生长条纹和位错,并根据形貌和结构特点对生长条纹产生的原因进行了分析讨论,提出了一些减少缺陷和提高晶体质量的措施和方法.     

X-ray Lang Topography and Infrared Spectroscopy in Quartz Crystals Grown Hydrothermally with Intermittent Runs

Growth defects in Y-plates obtained from Y-bar synthetic quartz crystals, grown hydrothermally with intermittent runs, have been studied for the first time by X-ray Lang topography and infrared spectroscopy. To study the effect of interfaces on dislocation structures, the growth runs have been discontinued several (6 to 7) times by switching off the autoclaves from 30 min to 1 h. The dislocations were observed to change their directions at the generated interfaces, sometimes they stop at the in terfaces or move straight through the interfaces depending on the angles of the interfaces which are presumably low-angle grain boundaries. The percentage transmission of infrared beam has also been measured as a function of the distance traversed in the crystal. The inverse anelastic loss (Q) decreases at the interface which is due to the greater accumulation of chemical impurities and H bonded OH⁻ ions at these interfaces. The effect of in-situ electric field on the topographic contrast has also been studied which reveal some interesting results on account of space charge polarization.     

Growth of KDP crystals by splicing “parallel”-seed in aqueous solution and its mechanism

Growth of the habit of a single seed and the special growth of splicing “parallel” seeds were investigated and compared with. Chemical etching and X-ray topography were used to characterize spliced KDP crystals. The kinetic data in different growth stages were measured. It is concluded that secondary capping is the most important stage in the splicing parallel-seed growth, and that the subgrain boundaries emitted from the secondary cap are parallel to or overlap with the splicing boundary and stretch to the prismatic surface about 45° to the z-axis, and that above the twin-crystal regions with subgrain boundaries the real monocrystalline region appears. The growth kinetics of the subgrain boundary approximately corresponds to the growth mechanism of single-spiral dislocation.     

Efficiency of dislocations as sinks of radiation defects in fcc copper crystal

The sink efficiency of perfect dislocations for self-point defects (interstitials and vacancies) in fcc copper crystal has been calculated by the kinetic Monte Carlo method in a temperature range of 293–1000 K and a range of dislocation densities from 1.3 × 10¹² to 3.0 × 10¹⁴ m^?2. Screw, mixed, and edge dislocations with a Burgers vector 1/2<110> in different slip systems are analyzed. The interaction energies of self-point defects with dislocations are calculated using the anisotropic theory of elasticity. Analytical expressions are proposed for the dependences of the calculated values of dislocation sink efficiency on temperature and dislocation density.