Periodic formation of cracks in isomorphously mixed crystals with a continuously varying composition during their growth

Original data on the periodic formation of crack systems in growing crystals are obtained in experiments on growing isomorphously mixed potassium-rubidium biphthalate crystals with a continuously varying impurity concentration during crystal growth. The origin and conditions of the periodic formation of growth cracks in crystals are explained using the previously developed computer model for calculating heterometry-induced internal stresses in isomorphously mixed crystals during their growth.     

Growth dislocations in zonal isomorphously mixed crystals

The orientation, distribution, and density of dislocations in isomorphously mixed potassium-rubidium biphthalate crystals composed of two zones with different concentrations of isomorphous rubidium impurity are experimentally studied. A model for the formation of growth dislocations in the external zone, which compensate internal heterometry-induced stresses at the interface between the zones, is proposed.     

PVT法生长SiC过程生长界面形状对热应力的影响

PVT法生长SiC过程中晶体内部的热应力是其位错产生的主要原因,而生长界面的形状对晶体热应力及缺陷的产生都有一定影响.本文对不同生长界面晶体的温场及应力场进行了数值分析,结果显示相对于凸出及平整界面的晶体,微凹界面晶体的轴向温差最小,同时产生缺陷的切应力Τrz及引起开裂的径向正应力σrr值都为最小.     

Optical defects in barium—strontium niobate single crystals

The distributions of edge dislocations and residual mechanical stresses in Ba_xSr_1-xNb₂O₆ (BSN) crystals are investigated and the explanation of the nature of the “growth column” is proposed. The “growth column” is a defect zone going through all of the crystal and usually repeating in its cross-section the contour of the seed crystal. The “growth column” boundary is the closed contour with extremely high edge dislocation density. These dislocations are connected with thermal stresses due to seed-melt contact or abrupt crystal widening. Under proper crystal seeding and widening conditions one can obtain the BSN crystals with dislocation densities less than 10 cm⁻² and without the “growth column”. The method of chemico-mechanical polishing of BSN crystals not forming a defect layer on the surface of the crystals have been developed. The high temperature diffusion annealing is shown to eliminate the growth striae in BSN crystals.     

The role of dislocations in the formation of mechanical stresses during annealing of gallium arsenide single crystals

The effect of dislocations on the change of mechanical stresses in undoped semi-insulating gallium arsenide single crystals has been studied during their annealing in vacuum and in the arsenic atmosphere. The phenomena observed are explained by the effect of dislocations playing the role of channels for arsenic diffusion on the concentration of intrinsic point defects in the crystal regions surrounding dislocations. The mechanism of arsenic diffusion over dislocations allows one to consider dislocations as sources and sinks of arsenic without the translational and twinning processes and, thus, makes the well-known data on the reactions of dislocation interaction with point defects and the experimental structural data for single crystals more consistent.     

Solid mechanics and material strength studies on the melt growth of bulk single crystals

Microdefects such as dislocations and macrocracking should be controlled during the crystal growth process to obtain high-quality bulk single crystals. Solid mechanics and material strength studies on the single crystals are of importance to solve the problems related to the generation and multiplication of dislocations and the cracking of single crystals. The present paper reviews such research activities that comprise the thermal stress analysis during crystal growth process, the dislocation density estimation during crystal growth process, and the cracking of single crystal due to thermal stress.     

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.     

Propagation behavior of threading dislocations during physical vapor transport growth of silicon carbide (SiC) single crystals

The dislocation formation and propagation processes in physical vapor transport (PVT) grown 4H silicon carbide (4H–SiC) single crystals have been investigated using defect selective etching and transmission electron microscopy (TEM). It was found that while the growth initiation process generally increased the density of threading dislocations in the grown crystal, for certain areas of the crystal, threading dislocations were terminated at the growth initiation. Foreign polytype inclusions also introduced a high density of dislocations at the polytype boundary. In the polytype-transformed areas of the crystal, almost no medium size hexagonal etch pits due to threading screw dislocations were observed, indicating that the foreign polytype inclusions had ceased the propagation of threading screw dislocations. Based on these results, we argued the formation and propagation of the threading dislocations in PVT grown SiC crystals, and proposed the dislocation conversion process as a plausible cause of the density reduction of threading dislocations during the PVT growth of SiC single crystals.     

Defect generation on mechanically surface defects before and after the oxidation (II). Dislocation generation at cracks

The generation of crystal defects at residual cracks due to a wet oxidation of chemically mechanically polished silicon wafers at 1100 °C was investigated. It was found that the nucleation of oxidation stacking faults at these elastic cracks is impeded as compared to the regions between the cracks. However, extended dislocations, dislocation dipoles, certain stacking faults, and precipitates are generated at such cracks. These crystal defects and the crack itself impede the nucleation of oxidation stacking faults at the crack, as they locally reduce the excess interstitials at the oxidation front.     

Atomic force microscopy studies on liquid inclusions and induced defects of cadmium mercury thiocyanate crystal

Liquid inclusions and various defects accordingly induced on a nonlinear optical material of CMTC crystal were investigated by atomic force microscopy. Liquid inclusions are chiefly caused by formation of macrosteps, which result from impurity‐induced inhibiting of step growth and meeting of step trains advancing along different directions. Liquid inclusions induce generation of dislocations and even cracks within the crystal by three‐dimensional nucleation growth. Liquid inclusions also provide screw dislocation growth sources, leading to formation of spiral hillock trains with ridged tails. Etching experiments reveal circular hollow cores, indicative of screw dislocation growth, and negative crystals resulting from further crystallization in the liquid inclusions. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

大尺寸KDP晶体切削开裂效应数值模拟分析研究

大尺寸KDP(KH2PO4)晶体在切割过程中容易出现开裂现象,为了研究大尺寸KDP晶体切割过程中开裂机制并提出合理切割方案,本文对大尺寸KDP晶体切削效应进行了研究.大尺寸KDP晶体切削过程中刀片与晶体之间的接触应力和切割引起的热应力是晶体切削过程中主要致裂因素,因此本文采用有限元计算方法对KDP晶体切削过程进行热力耦合数值仿真模拟.结果表明切割过程中KDP晶体与刀片之间的压力应小于4.1 MPa,切口处温差应控制在4.2℃之内,同时本文还得到了切削过程可控参数(车床推进力和刀片的线速度)的安全取值范围,该范围的提出对KDP晶体的切割技术具有十分重要的意义.     

Dislocations and dislocation reduction in space grown GaSb

The behaviour of dislocations in GaSb crystals grown in space both from a stoichiometric melt (floating zone method, FZ) and a Bi solution (floating solution zone, FSZ) respectively, is studied. Predominantly straight 60° dislocations with Burgers vectors of the type b = a/2 <110> in (111) glide planes are identified. In the 20 mm long FZ single crystal the linear growing out of the dislocations is observed which reduces the dislocation density in the centre of the crystal to values below 300 cm^–2. The Bi incorporation in the FSZ crystal results in a misfit between seed and grown crystal and in a network of misfit dislocations at the interface. Thermocapillary convection during growth as well as the surface tension may be the reasons for the presence of curved dislocations and the higher dislocation density within a 1 – 2 mm border region at the edges of both of the crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

晶格畸变检测仪研究碳化硅晶片中位错缺陷分布

利用晶格畸变检测仪研究了SiC晶片位错分布情况,通过对熔融KOH腐蚀后的SiC晶片进行全片或局部扫描,从而得到完整SiC晶片或局部区域的位错分布.与LEXT OLS40003D激光共聚焦显微镜扫描腐蚀图进行比较,晶格畸变检测仪扫描腐蚀图可以将晶片上位错腐蚀坑信息完全呈现出来,且根据腐蚀坑呈现的颜色及尺寸大小,可以分辨出...     

Mechanism of condensation of heteroepitaxial A3B5 layers pulse of moderate power

The mechanism of condensation of heteroepitaxial layers in laser deposition was studied on GaAs films on NaCl. Films were deposited in a superhigh vacuum using laser pulses of moderate power. Pulsed deposition proved to be more suitable for nucleation and growth than continuous deposition. However in this case it is important to compare the number of atoms deposited per pulse and the number of preferential adsorption centres in the substrate temperature of 310 °C. The density of dislocations in the films was about 10⁹ cm⁻². The main reasons for the dislocations are the excess of low volatile component and thermal stresses. Using a laser with quantum energy higher than the energy gap of the deposited semiconductor GaAs, which provides congruent evaporation, and making an additional deposition of As, we could reduce dislocations to 10⁷ cm⁻². A mechanism is proposed to explain the reduction of temperature in single crystal growth under laser deposition: high energy ion component of laser plasma gives rise to orienting defects on the substrate surface, and these defects determine epitaxial growth.     

Nucleation of Cracks in CdS during Ultrasonic Treatment

High amplitude ultrasonic vibrations with frequencies f_r ∼ 90 kHz and vibration amplitudes ε ⩽ 3.4. 10⁻⁴ were used to obtain oscillatory stresses σ ⩽ 14 MPa in CdS single crystals. Such treatment leads to the nucleation of cracks in annealed samples and to the formation of dislocations in as-grown samples. The different behaviour can be explained by the reduction of the free dislocation segment lengths due to the diffusion of point defects towards the dislocation lines during the annealing treatment.     

Sub-boundaries on (002) cleavages of Li2CO3 single crystals

Linear arrays of dislocations (straight, terminating and curved) are observed on etching with 2% citric acid (002) cleavages of lithium carbonate (Li₂CO₃) single crystals, grown by zone melting technique. As the dislocations are non-uniformly spaced and disappear on successive etching, they may not be revealing low-angle grain boundary, nor slip traces as they are terminating and curved meaning crystallographically non-oriented. On the observation of experiments on successive etching and etching of matched pairs, it is concluded that the arrays of etch pits reveal dislocation walls (dislocation density 1.1 × 10⁶ — 1.5 × 10⁷ pits cm⁻²) probably created due to the localized thermal stresses released as a result of high temperature annealing of the crystal during growth. The implications are discussed.     

Dislocation Multiplication in the Flexoelectric Distortion Grid with an Increase in Electric Field Amplitude

It is shown that a plane one-dimensional flexoelectric grid well simulates the processes of the nucleation of defects (dislocations) and an increase in their number in crystals under increasing mechanical stresses in the crystal lattice. The latter rise with an increase in electric field above the instability threshold and the corresponding growth of the modulations of the flexoelectric-grid spatial structure. Parameters of these modulations are obtained for various boundary conditions at the surface of a nematic film oriented in one direction. The previous data on the dislocation patterns in strong fields are explained. The applicability of the dislocation theory to the planar one-dimensional grid is shown.     

碲锌镉晶体晶格畸变的测定与分析

在高分辨X射线衍射仪上,利用不对称布拉格衍射STD技术与单晶摇摆曲线技术相结合的方法,对碲锌镉单晶材料的晶格畸变进行了分析测定.此方法实现了一次装样,多角度、多次测定晶体的摇摆曲线,从而利用多组实验数据完成多元线性回归方程组的求解,避开了一般应变测定方法中难以确定无应力状态下衍射角的问题.所测定的生长态碲锌镉晶片晶格畸变量为10-3～10-2数量级,该畸变量是碲锌镉晶片存在成份偏析、位错和空位等缺陷以及晶片受到的应力综合作用的结果.     

Peculiarities of the melt growth of metal single crystals with specified crystal-geometric and structural parameters

This paper describes the authors' modifications of Kapitza and Bridgman apparatus and growth methods of metal single crystals with specified crystal geometric and structural parameters. The effects associated with defect formation are discussed. The features of the effects in their relation to the crystal lattice types and crystallographic orientation are indicated. It is concluded that one of the main factors responsible for the defect formation during single crystal growth in the mould is strain. This is due to thermomechanical stresses arising during the crystal growth and cooling to room temperature, from the difference in thermal expansion coefficients of the crystal and mould materials.     

Three-dimensional global analysis of thermal stress and dislocations in a silicon ingot during a unidirectional solidification process with a square crucible

A three-dimensional global model was used to obtain the solution of a thermal field within the entire furnace during a unidirectional solidification process of multicrystalline silicon with a square crucible. Then the thermal stress distribution in the silicon ingot was solved. Based on the solution of thermal stress, relaxation of stress and multiplication of dislocations were performed by using the Haasen–Alexander–Sumino model (HAS model). The influence of crucible constraint on stress levels and dislocations was investigated. It was found that the crucible constraint had significant influence on the thermal stresses and dislocations in the ingot. The results indicated that it is important to reduce the crucible constraint in order to relax thermal stresses and reduce dislocations in a silicon ingot during the solidification process.