Characterization of dislocations in a LiNbO3 single crystal grown by micro pulling down method

LiNbO₃ single crystals grown by the micro pulling down (μ-PD) method have been revealed to be as free of dislocations and subgrain boundaries up to 500 μm in diameter. On the other hand, μ-PD LiNbO₃ single crystals grown along the x-axis in diameter of 800 μm were observed to be dislocated due to the size effect of crystal. The Burgers vectors of dislocations were determined to be [22 01], [101 1], and [01 11] by X-ray topography.     

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.     

Melt nonstoichiometry and defect structure of ZnGeP<Subscript>2</Subscript> crystals

The defect structure of ZnGeP₂ crystals grown from a melt by the vertical Bridgman method has been investigated. A deviation of the melt composition from stoichiometric leads to the formation of striations and the inclusions of other phases which are observed as structures (chains) oriented parallel to the growth axis. According to the microanalysis data, the inclusion composition corresponds to a mixture of ZnGeP₂, Zn₃P₂, and Ge. Nanoinclusions of germanium phosphide are detected by transmission electron microscopy. X-ray topography reveals defects of four types. The main defects in the central part of an ingot are related to the composition fluctuations, and the newly formed dislocations are basically single ones. Most dislocations are formed at the crystal periphery.     

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.     

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.     

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.     

Investigation of PbTiO3 crystal lattice defects by transmission electron microscopy

The investigation of PbTiO₃ single crystal structure was carried out by the method of transmission electron microscopy (TEM). It is shown that the following types of defects are observed: ferroelectric 90°-and 180°-domain boundaries, dislocations and their complexes, and planar defects.     

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.     

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.     

Single‐crystal sapphire microstructure for high‐resolution synchrotron X‐ray monochromators

We report on the growth and characterization of sapphire single crystals for X‐ray optics applications. Structural defects were studied by means of laboratory double‐crystal X‐ray diffractometry and white‐beam synchrotron‐radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique. Therein the dislocation density was 10²–10³ cm⁻² and a small area with approximately 2*2 mm² did not show dislocation contrast in many reflections. This crystal has suitable quality for application as a backscattering monochromator. A clear correlation between growth rate and dislocation density is observed, though growth rate is not the only parameter impacting the quality.     

Characterization of large‐sized Nd:YAG single crystals grown by horizontal directional solidification

Nd³⁺‐doped Y₃Al₅O₁₂ single crystals have been grown by the horizontal directional solidification (HDS) method in different thermal zone. The Grashof (G_r), Prandtl (P_r), Marangoni (M_a) and Rayleigh (R_a) numbers of melt in HDS system have been discussed for our experimental system to understand the mechanism of melt flow patterns and concentration gradient of dopant. The concentration gradient of Nd³⁺ ions was explained with melt flow processes during crystal growth in different thermal zone, and results indicated that high growth temperature will be helpful for uniformity of dopant in HDS‐grown single crystal. The main microscopic growth defects such as bubbles and irregular inclusions in HDS‐grown Nd:YAG crystals were observed, and the causes were discussed as well. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Dislocations of salol crystals grown by the Czochralski method

Crystals of salol were grown by the Czochralski method in three different pulling directions to examine the crystallographic orientation effect of the seed. They were characterized by the etch pit method and X-ray projection topography. It was found that the dislocation density was 2 × 10³−1 × 10⁴/cm² and that the configuration of dislocations was straight. The running directions of dislocations strongly depend on the pulling directions; i.e., [11 0] and [1 10] for the crystal grown in [100] axis, [11 0], [1 10] and [110] for the crystal pulled along [112] axis and [010] for [010] axis crystal.     

Epitaxial growth of silicon carbide layers by sublimation “Sandwich method” (II) structural defects and growth mechanism

Structural defects of α-SiC epitaxial layers grown by sublimation “sandwich-method” in vacuum at the temperatures ranging from 1600 to 2100 °C have been investigated by X-ray topography and optical microscopy methods. It was shown, that perfect SiC layers with the homogeneous polytype structure and small dislocation density (≦ 10² cm⁻²) may be obtained on the substrates with any crystallographic orientation at the conditions close to quasi-equilibrium one. The presence of impurities and silicon deficiency in the vapour phase, lead usually to the deterioration of morphological and structural perfection of SiC layers. There are the following structural defects: uncoherent polytype inclusions (mainly β-SiC), pores, dislocations, specific stacking faults. Morphological peculiarities of the SiC epitaxial layers and possible growth mechanisms are discussed.     

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.     

Czochralski-growth of germanium crystals containing high concentrations of oxygen impurities

Oxygen-containing germanium (Ge) single crystals with low density of grown-in dislocations were grown by the Czochralski (CZ) technique from a Ge melt, both with and without a covering by boron oxide (B₂O₃) liquid. Interstitially dissolved oxygen concentrations in the crystals were determined by the absorption peak at 855 cm⁻¹ in the infrared absorption spectra at room temperature. It was found that oxygen concentration in a Ge crystal grown from melt partially or fully covered with B₂O₃ liquid was about 10¹⁶ cm⁻³ and was almost the same as that in a Ge crystal grown without B₂O₃. Oxygen concentration in a Ge crystal was enhanced to be greater than 10¹⁷ cm⁻³ by growing a crystal from a melt fully covered with B₂O₃; with the addition of germanium oxide powder, the maximum oxygen concentration achieved was 5.5×10¹⁷ cm⁻³. The effective segregation coefficients of oxygen in the present Ge crystal growth were roughly estimated to be between 1.0 and 1.4.     

Zur Lumineszenz von Zinksiliziumphosphid

Results of cathodoluminescene measurements of ZnSiP₂-single crystals grown by different techniques are reported. The luminescence excited in the various samples showed considerable differences in intensity and spectral position. These differences are apparently caused by the irregular incorporation of recombination centres in the present stage of crystal growth. Samples grown by “vapour phase technique with ZnCl₂” and by “spontaneous crystallisation from Sn or zn melt” showed line spectra typical for the special method of crystal growing. This relation between a typical line spectrum and the method of crystal growing chosen is attributed to the participation of intrinsic defects in the recombination processes. The detection of doping elements by means of luminescence measurements is discussed for ZnSiP₂ crystals doped by adding Te, Se, Ga. or In to the Zn melt.     

KDP single crystal growth via three‐dimensional motion growth method

A novel system for rapid crystal growth, namely three‐dimensional motion growth method (“3D MGM”) was proposed. Using this system, a potassium dihydrogen phosphate (KDP) seed was grown to a single crystal with a final size of 50×55×85 mm³. The KDP crystal was characterized by Raman spectroscopy, UV‐vis‐NIR spectroscopy, extinction ratio, laser damage threshold, and etching studies. Raman spectrum shows KDP crystal grown by “3D MGM” maintains good crystallinity as that grown by rotating‐crystal method (“RCM”). The “3D MGM” grown KDP crystal has much better transmittance, higher extinction ratio, higher damage threshold and less dislocation density, compared to “RCM” grown crystal.     

Growth of several quantum crystals: CD4, 4He and 3He

Large single crystals of CD₄, ⁴He, and ³He have been grown from the melt at low temperatures. These “quantum” crystals were characterized with X-ray diffraction techniques which allow excellent determinations of crystal quality. The crystal CD₄ was grown from its melt at saturated vapor pressure. Over 100 helium crystals were grown at constant pressures between 2.9 and 13.8 MPa. It has been found that the hcp and bcc crystals grow in preferred directions, and that growth rates of about 0.3 mm/ min are appropriate for hcp ⁴He, while bcc ³He requires the slower rate of 0.06 mm/min for good quality crystals. There is some indication that it is the isotope, and not the crystal structure, which is the cause of the fact that the hcp ⁴He crystals are much more stable than the bcc ³He crystals. Comparison of several theoretical crystal growth parameters for many substances leads to the conclusion that methane is basically a normal material, while helium is abnormal, having very different growth parameters from most substances. Helium is interesting in that its crystal growth parameters can be changed by very large amounts while keeping the chemistry constant.     

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.     

X-ray Topographic Assessment of Defects in Pure and Substituted Hexaferrite Crystals

Results of X-ray diffraction topography, in reflection and transmission scanning geometry, of flux grown single crystals of substituted and unsubstituted hexaferrites bearing composition SrGa_xIn_yFe_12-(x+y)O₁₉ (where x = 0, 5, 7, 9; y = 0, 0.8, 1.3, 1.0) are presented. Diffraction topographs reveal defects like misoriented grains, dislocations, cavities, inclusions, and the strain patterns in these crystals. The unsubstituted hexaferrites exhibit better perfection when compared to the substituted ones. The study is reported to support the results obtained by chemical etching and fractography, besides yielding additional information covering defects.