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.     

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.     

X-Ray study of the defect structure of PbTe single crystals

PbTe single crystals grown by different methods were thinned electrolytically and examined by X-ray transmission topography. The transmission topographs, first obtained of this material, reveal substructure, slip lines and single dislocations. The samples exhibit different structural perfection in dependence on the growth method. In crystals of relatively high perfection, slip lines are the striking feature of defect structure, caused by surface damage during mechanical preparation. The most perfect sample has a dislocation density of 10² to 2 ṁ 10³ cm⁻². No slip occurs, probably due to small dopant contents.     

Dislocation etching in V3Si

Dislocations in as-grown and in plastically deformed V₃Si single crystals have been studied by chemical etching. In as-grown crystals dislocations are partly arranged in small-angle boundaries parallel to {001}, {011}, and {112} planes. The total dislocation density amounted to (10⁵−10⁶) cm⁻². After plastic deformation at elevated temperatures indications for slip and climb processes were observed. The dislocation density increased to 10⁷ cm⁻².     

Dislocation densities in copper single crystals after thermal treatment

Copper crystals of high purity and doped with nickel were subjected to a long time thermal treatment at 1050°C, in order to reduce the as-grown dislocation density of about 10⁷ cm⁻². A dissolution of the dislocations during their motion to the crystal surface was observed. Regions of different dislocation densities arose. Finally the crystals exhibited constant dislocation densities of 10² cm⁻². Such a perfection or a better one of the crystals is reached only by a long time treatment, since the dislocation velocity without external stresses cannot exceed 1 · 10⁻⁷ cm · s⁻¹ in copper single crystals of high purity.     

Deformation mechanism and dislocation structure of high-purity molybdenum single crystals at low temperatures

High purity molybdenum single crystals were deformed in tension and compression along the symmetric double slip orientation [110] in the temperature range from 300 K down to 0.5 K with strain rates between 10⁻³ and 10⁻⁵ s⁻¹. The activation volume was measured by stress relaxation tests. The dislocation structure of the deformed crystals (T → 1.85 K) was examined by high voltage electron microscopy. It was established that the low temperature increase of the critical shear stress exhibits three distinct temperature regimes with different temperature dependences. These non-uniformities are discussed in terms of recently developed theories of kink-pair formation and kink-kink interactions on screw dislocations in bcc metals. The HVEM observations suggest that the mobility of screw dislocations at very low temperatures should be determined by the combined effects of the PEIERLS barriers and the jog dragging.     

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.     

Structure sensitivity of relaxation phenomena in NaCl and KCl crystals doped with some divalent impurities (II) effect of plastic deformation

By studying: 1/the role of dislocations in the origin of the C-ITC-peak in undeformed crystals, 2/ the effect of plastic deformation upon the behaviour of this peak, and 3/ the recovery of the deformation-induced changes of the basic characteristics of this peak (H^C, T_M^C) it has been confirmed that dislocation lines surrounded by the Cottrell-like atmospheres can be considered as polarizable entities related with the high-temperature dielectrical response of as cleaved NaCl and KCl crystals doped with divalent impurities. The Maxwell/Wagner model of polarization effects in heterogeneous dielectrics satisfactory accounts for the majority of the experimental data. The quantitative analysis of the results obtained yields some additional informations concerning the interaction- and motion-parameters of the defects considered.     

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.     

Correlation between Light Microscopical and Electron Microscopical Images of Crystal Defects in GaP

Ultramicroscopy and dark-field-illumination basing on the scattering of photons are easily available, they are nondestructive light microscopical methods for real structure investigations of semiconducting materials. The observation of dislocations is possible because of photon scattering at precipitations adherent to the dislocation line. This work gives a direct correlation between light microscopical and electron microscopical images of dislocations and in this way some hints on the nature of scattering centres. The light scattering takes place at precipitations caused due to gettering of impurity atoms by the dislocation line. Besides elongated dislocations prismatic loops were observed. The loop density was found to be in the order of magnitude of about 10¹² cm⁻³ which corresponds to a concentration of about 10¹⁷ atoms contained in the loops in good agreement with the concentration of impurities in the crystals.     

Effect of the defect structure character in calcite single crystals on X-ray diffraction

The paper presents experimental results for the dependence of the integral intensity of anomalous transmission T_i and Laue reflection R_i of X-rays on the structural quality of calcite single crystals as obtained by a two-crystal spectrometer. The relation between X-ray dynamic and kinetic scattering as a function of the sample thickness, densities of perfect dislocations in perfect CaCO₃ crystals and of atom-vacancy complexes in calcite crystals with „background”︁ has been found. Distortions due to perfect grown-in dislocations in calcite are shown to exceed those produced in crystals with „background”︁. The latter appear to be more X-ray transparent. A comparison with results of twin layer thickening experiments on CaCO₃ crystals of different qualities again points to the different nature of these distortions. In CaCO₃ crystals with the dislocation density of up to 2 × × 10³ cm⁻², the X-ray scattering, in our experiments, was consistent with the dynamic diffraction theory, while at higher dislocation densities, the X-ray scattering markedly differs from it.     

Influence of Dislocations in KDP Crystals on Laser Damage Threshold

The dislocation density in KDP crystals has been determined by X-ray diffraction topography (LANG method). A method for determining the laser damage thresholds in dependence on dislocation density is described. It is found that dislocations with a density about 10³ cm⁻² reduce the laser damage threshold up to a factor of two compared with perfect regions. It is shown that experimentally measured damage results can be explained theoretically.     

Observation of individual dislocations in 6H and 4H SiC by means of back‐reflection methods of X‐ray diffraction topography

SiC crystals of high structural perfection were investigated with several methods of X‐ray diffraction topography in Bragg‐case geometry. The methods included section and projection synchrotron white beam topography and monochromatic beam topography. The investigated 6H and 4H samples contained in large regions dislocations of density not exceeding 10³ cm^‐2. Most of them cannot be interpreted as hollow core dislocations (micro‐ or nano‐pipes). The concentration of the latter was lower than 10² cm^‐2. The present investigation confirmed the possibility of revealing dislocations with all used methods. The quality of presently obtained Bragg‐case multi‐crystal and section images of dislocation enabled analysis based on comparison with numerically simulated images. The analysis confirmed the domination of screw‐type dislocations in the investigated crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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.     

The factors affecting the polarization transformations of X-rays in Laue diffraction from crystals with dislocations

The transformations of X-ray polarization with coherent σ-and π-components have been studied for the Laue diffraction from LiF crystals with a high dislocation density (10⁴–10⁵ mm^?2). The dependence of the parameter characterizing the diffraction-induced birefringence and the degree of coherence of the transmitted beam on the squared reciprocal-lattice vector (H ² = 4sin²θ/λ²) is determined. It is shown that the parameter characterizing the diffraction-induced birefringence in crystals with dislocations is determined by the static Debye-Waller factor (exp(-L)) and the effective thickness Δ of the crystal. The exponent L increases and the parameter Δ decreases with the dislocation density.     

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〉.     

Real structure investigations of LiNbO3 single crystals grown by the flux method

The real structure of flux grown LiNbO₃ crystals is investigated by etching technique, X-ray topography, and optical polariscopic method. The main defects are microdomains, dislocations and minor impurities of V³⁺−ions. The crystals do not contain growth striations. The mean dislocation density is in the order of 10³ cm⁻². The main origin of the defects seems to be post-growth mechanical stress. The results are discussed in comparison to the real structure typically found in the case of Czochralski crystals.     

The defect structure of ammonium sulphate single crystals

The defect structure of larger ammonium sulphate crystals, grown from aqueous solutions, has been studied by means of X-ray diffraction topography after Lang's method. Several types of dislocations were identified. Moreover it was found that no relationship exists between growth rate and dislocation density, which implies that crystal growth proceeds via two-dimensional nucleation. No difference was found in the defect structure of crystals grown from pure water solutions and from aqueous solutions with 10 – 20% glycerine as additive: In both cases neither growth bands nor sector boundaries were found. On the other hand, crystals grown in aqueous solutions contaminated with Mn²⁺ and Fe³⁺ revealed growth bands and for Fe³⁺ a mosaic-like structure.     

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.     

Dislocation activity in single crystals of stannic iodide

Single crystals of stannic iodide (SnI₄) have been grown employing the controlled-reaction between SnCl₂ and KI solutions by diffusion process in silica gels. As-grown (111) surfaces of the crystals have been optically studied. Characteristic growth spirals and hopper growth patterns have been observed on them. By successively etching (111) surfaces in a 0.2 N HCl solution, it is established that the pits indicate the sites of dislocations in the crystals. This is further confirmed by comparing the etch patterns before and after chemically polishing (111) surfaces. The average dislocation in the SnI₄ crystals have been determined and found to be 7.3 × 10² cm⁻². Observations of polygonisations are described and the implications are discussed.