Röntgentopographische Untersuchung von KDP-Kristallen

The dislocation configuration arising in KDP crystals grown from the solution has been studied by X-ray diffraction topography method (Lang-method). The space orientation of dislocations and their Burgersvektor directions are determinated. The dislocations density did not exceed 10³ cm⁻², and there are areas which were free form dislocations. The sources of dislocations were classified as inclusions of mother liquor and foreign particles respectively.     

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.     

Effects of the Crystal Diameter on the Dislocation Density in KCl Crystals Grown by the Czochralski Method

The dependence of dislocation density on the crystal diameter of the Czochralski grown KCl crystals (both pure and Sr doped) was investigated by the method of the etch pit and X-ray topograph. (1) The dislocation density drastically decreased with the decrease in diameter (D) for small D (D < 2 mm, Fig. 2). (2) The dislocation density in the Sr doped crystal was lower than that of pure component in the diameter examined. (3) Many helical dislocations and dislocation loops were observed in the thin crystals (D ∼ 0.5 mm) of the pure KCl and Sr doped one, respectively, by X-ray projection topography. These results were discussed in connection with the dislocation generation mechanisms due to thermal stresses or supersaturated point defects.     

Antistructure disorder and its relation to dislocations in III–V semiconductors

Intimate relationship between antistructure defects and dislocations occurs in GaAs which manifests itself as: (i) appearing of spatial correlation between grown-in dislocations and the EL2 defects (component of the latter are As_Ga antisites), (ii) similar suppression of the concentration of EL2 and dislocation density due to the doping with donor impurities, (iii) generation of As_Ga antisites during the plastic deformation of a crystal. Al these effects can be understood in terms of the dislocation-mediated generation of As_Ga antisites via absorption of As_i interstitials at dislocation jogs. Large anion (cation) precipitates appearing at dislocations are pointed out to be important for both antisite and dislocation generation under certain conditions.     

Plastische Verformung von Siliziumeinkristallen unterschiedlicher Ausgangsversetzungsdichte im Streckgrenzenbereich

Floating-zoned Silicon crystals orientated for single slip both dislocation-free and with grown-in dislocations (EPD₀ = 6,5 · 10⁴ cm⁻²) were dynamically deformed in compression in the temperature range 1120 … 1300 K up to the lower yield point. The dislocation structure of plastically deformed crystals (T = 1138 K; a₀ = 1,45 · 10⁻⁴ s⁻¹) was examined by etching and high-voltage electron microscopy. The crystals exhibit essential differences in deformation behaviour and in the resulting dislocation structure. Typical for the dislocation-free basic material are (i) an inhomogeneous deformation in the range of the upper yield point (ii) a greater portion of sessile lomer dislocations at the lower yield point in relation to the crystal with grown-in dislocations. The measured stresses were related to those values calculated from structure data by employing plasticity theory of diamond-like semiconductors.     

TEM-Untersuchungen von Gitterfehlern in ZnSiP2-Einkristallen

Results are dealt with concerning TEM investigations of lattice defects in ZnSiP₂ single crystals. After the crystal growth dislocations or stacking faults were found in a few cases only. More frequently twins were present in the microstructure. The crystallographic elements of twinning are {112} 〈111〉. After plastic deformation by bending at 900 °C local dislocation arrangements with high defect density (N_v ≈ 10⁶…︁ 10⁷ cm⁻²) were observed. By means of the diffraction contrast one Burgers vector b = 1/2 〈111〉 could be identified. In some cases the crystals also contained wide deformation stacking faults, which were limited by partial dislocations. The density of twins was not increased under the conditions of deformation reported here. As it can be concluded from investigations of Oettel et al. and from the results of the twin analysis, slip and generation of stacking faults take place on {112}-planes in ZnSiP₂ crystals. Crystallographic considerations on both processes are dealt with.     

Effects of doping of Ca and Ba on the dislocation distribution in melt grown KCl crystals

The effects of doping of Ca and Ba (∼ 0.02 at %) upon the dislocation distribution in melt grown KCl crystals without cellular segregation were studied by an etch pit method in connection with the dispersion state of the dopants, which was examined by the dark field illumination. – (1) In the Ca-doped crystal, in which the dopants were distributed uniformly, the formation of subboundaries was completely suppressed and dislocations were distributed at random. (2) In the Ba-doped crystal, however, the dopants were non-uniformly distributed and the dislocations tended to form subboundaries. The dislocations within the subgrains were distributed in a non-uniform manner. (3) The dislocation density in the Ba doped crystal was higher than that of undoped or Ca-doped crystal. This was explained by the mechanism similar to the Tiller's prediction. – Finally, the stress distribution due to the concentration fluctuation was examined by the birefringence patterns.     

On the delay of thermally activated motion of pyramidal dislocations in zinc

The effect of shear stress and temperature on the delay time, t_i, of thermally activated motion of dislocations in the {112 2} 〈112 3〉 slip system in Zn single crystals is studied. The delay is associated with a higher density of crystal defects at the initial path of dislocation motion.     

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.     

Finite element analysis of dislocation density during bulk single crystal growth (effect of doping atoms in InP single crystal)

A computer code for simulation of dislocation density in a bulk single crystal during liquid encapsulated Czochralski (LEC) or Czochralski (CZ) growth process. In this computer code, the shape of crystal–melt interface and the temperature in a crystal at an arbitrary time were determined by linear interpolation of the results that were discretely obtained by heat conduction analysis of a CZ single crystal growth system. A dislocation kinetics model called Haasen–Sumino model was used as a constitutive equation. In this model, creep strain rate is related to dislocation density, and this model extended to multiaxial stress state was incorporated into a finite element elastic creep analysis program for axisymmetric bodies. Dislocation density simulations were performed using this computer code for InP bulk single crystals with about 8″ in diameter. In the analysis, the effect of dopant atoms on the dislocation density was examined. In the case of a low doped InP single crystal, dislocations are distributed in the whole of the crystal. On the other hand, in the case of a highly doped InP single crystal, dislocations are localized at both the central and peripheral regions of the crystal.     

TEM and X-ray investigations of defect structure of PbSnTe crystal

The Pb_0.8Sn_0.2Te single crystal grown by the Bridgman technique was examined by X-ray and TEM methods. The X-ray reflection topography revealed that the PbSnTe crystal consisted of monocrystallinic blocks with linear dimensions of 1–5 mm separated by low angle boundaries of tilt-twist character. “As grown” defects observed by TEM method have been identified as single perfect dislocations and dislocation pairs. A mean density of dislocations inside the crystal blocks was no more than 10³ cm⁻². Except “as grown” defects rows of mobile dislocations were observed. All of dislocations lines were characterized by the same type of Burgers vector, i.e. b = 1/2a〈110〉.     

Defects in LEC-grown Indium Phosphide Crystals Doped with Tin

Crystalline defects in Sn-doped LEC indium phosphide have been revealed by chemical etching and analyzed by TEM. Grown-in dislocations, various kinds of defect clusters and colonies of microdefects were found. The symmetrical defect clusters are shown to equate mostly with larger dislocation loops exhibiting shear components and/or other dislocation arrangements generated by a stress source which is positioned in the centre of the dislocation cluster. Those centres are often formed by a plate-like agglomeration composited of tiny inclusions and very small faulted dislocation loops. Such planarly arranged accumulations of microdefects lie on {111} planes. The direct vicinity of single threading grown-in dislocations is always enriched with tiny perfect dislocation loops and precipitates. Additionally, very large isolated interstitial-type perfect dislocation loops with b = a₀/2 〈110〉 have been found by TEM experiments. Mostly, the {110} habit plane of such loops is decorated with an high number of small dislocation loops and precipitates as a consequence of dislocation climb.     

4H碳化硅单晶中的位错

4H碳化硅(4H-SiC)单晶具有禁带宽度大、载流子迁移率高、热导率高和稳定性良好等优异特性,在高功率电力电子、射频/微波电子和量子信息等领域具有广阔的应用前景。经过多年的发展,6英寸(1英寸=2.54 cm)4H-SiC单晶衬底和同质外延薄膜已得到了产业化应用。然而,4H-SiC单晶中的总位错密度仍高达10³~10⁴ cm^-2,阻碍了4H-SiC单晶潜力的充分发挥。本文介绍了4H-SiC单晶中位错的主要类型,重点讲述4H-SiC单晶生长、衬底晶圆加工以及同质外延过程中位错的产生、转变和湮灭机理,并概述4H-SiC单晶中位错的表征方法,最后讲述了位错对4H-SiC单晶衬底和外延薄膜的性质,以及4H-SiC基功率器件性质的影响。     

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)     

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.     

Formation of Dislocations and Twins As a Result of Uniaxial Compression of Magnesium Single Crystals: Molecular Dynamics Simulation

An atomistic simulation of the deformation of ideal magnesium crystal along the \([11\bar 20]\) crystallographic axis has been performed. The evolution of structural defects under load at T = 300–350 K is considered in detail. It is established that the nucleation of dislocations in an ideal crystal occurs when the stress reaches a level of 0.1G (G is the shear modulus). The acting deformation modes are found to be prismatic slip of a dislocations and \(\{ 10\bar 13\} \) twinning. The formation of dislocation networks and dislocation sites in the twinning plane is observed. Some reactions are proposed to describe the dislocation evolution in the \((\bar 3034)\) plane.     

Dislocations in magnetic garnet crystals

1. Dislocations in magnetic flux-grown garnet crystals (Y₃Fe₅O₁₂ and others) have been observed. As a rule, {110} growth pyramids have more defects than {211} ones. 2. The highest content of defects (dislocation density 10³–10⁴ cm⁻²) is observed in Y₃Fe₅O₁₂ that grows on crucible walls adjacent to the free surface of the solution where the flow of heat is not uniform to the greatest degree. Bottom grown crystals usually have less dislocations. Far fewer dislocations are in wall grown crystals, least of all dislocations are contained in crystals that grow inside the solution. The solution pouring off at the end of the crystallization period increases dislocation density by some dozens. 3. Heat treatment decreases dislocation density. The less dislocation content and the lower ordering are in the initial crystal, the higher heat treatment effectiveness.     

半导体单晶生长过程中的位错研究

阐述了现有的半导体单晶位错模型,即临界切应力模型和粘塑性模型的基本理论及应用状况.分析了熔体法单晶生长过程中影响位错产生、增殖的各种因素,以及抑制位错增殖的措施.与熔体不润湿、与晶体热膨胀系数相近的坩埚材料,低位错密度的籽晶可有效地抑制生长晶体的位错密度;固液界面的形状及晶体内的温度梯度是降低位错密度的关键控制因素,而两因素又受到炉膛温度梯度、长晶速率、气体和熔体对流等晶体生长工艺参数的影响.最后,对熔体单晶生长过程的位错研究进行了展望.     

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)