On the scandium distribution in indium arsenide crystals grown by the Czochralski method

In this paper the behaviour of scandium in n-type monocrystalline indium arsenide grown by Czochralski method in sealed ampoule is studied. The crystals have been grown in [111] direction under different conditions: crystallization rate, As-partial pressure and scandium initial concentration in the melt. The effect of the above factors on the scandium distribution along the crystals have been investigated. Using these results and by means of the equation of normal freezing the effective Sc distribution coefficient (k) in InAs under different technological conditions has been determined. It has been found that k < 1 in all experiments. In order to find the equilibrium coefficient (k₀) at fixed growth conditions the Burton-Prim-Slichter model has been used. On the basis of Hall measurements and atomic absorption analysis of Sc-doped InAs it is concluded that connected with Sc electrically active centers behave as shallow donors, most probably monovalent ones.     

The twisting of LiNbO3 single crystals grown by the Czochralski method

As a result of our experimental work of mainly practical importance we established that for LiNbO₃ single crystals the Mg and Fe dopants promote spirality whereas decreasing of the pulling velocity strongly reduces the propensity of the system to produce spiralshaped crystals.     

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.     

Complex formation and background impurity of Oxygen in the PbTe:Eu doped crystals grown from melt by the Bridgman method

The magnetic field dependence of magnetization M(B) at the temperature 1.72 K in magnetic fields up to 5 T and the temperature dependence of magnetic susceptibility (M_S) χ(T) in the temperature range 1.7–400 K of six PbTe:Eu samples with the concentration of Eu impurity of the order of 1×10¹⁹–1×10²⁰ cm^?3, prepared from the doped crystals grown from the melt by the Bridgman method, have been investigated. It is shown that the dependence of M(B) and χ(T) can be quantitatively explained by the contribution of the single centers of Eu ions, their pairs, and the matrix of the doped crystals using the same set of parameters for each sample. This is true provided we use in our analysis the values of the exchange integrals between Eu ions in EuO normalized with the lattice constant of PbTe, i.e., J₁/k_B=0.056 K for the ferromagnetic interaction of the NN (nearest neighbor) pairs and J₂/k_B=?0.13 K for the antiferromagnetic interaction of the NNN (next nearest neighbor) pairs, as well as different values of the M_S of crystal χ_matrix. It is revealed that the probability of the formation of complexes based on the magnetic impurity pairs is higher in the incipient section of a doped ingot, and it decreases towards the ingot end where the single centers of Eu ions become the only centers of the impurity. We conclude that the pairs of Eu²⁺ ions, which are formed during the growth of the PbTe:Eu ingots from melt by the Bridgman method, are the constituents of the complexes of the magnetic impurities with the background Oxygen impurities in the crystal matrix of the doped lead telluride. It is shown that the formation of the complexes leads to an increase of the M_S of crystal matrix χ_matrix and can even cause the change of its sign from minus to plus, i.e., it can convert the crystal matrix from the diamagnetic to paramagnetic state. The possible causes of this effect are analyzed.     

Haze in sapphire crystals grown by SAPMAC method

Haze defect in SAPMAC method grown sapphire crystal was studied in detail. It is shown that haze is composed by a large number of CO₂ bubbles, and haze always appears in the axis region of the crystal since the bubbles formed in front of the crystallization surface are most always draged to the convection rolls in front of the central part of the crystallizaiton surface by melt and then engulfed by the rolls. Moreover, the effects of pulling rate on the formation of haze were analyzed and means for restraining haze was suggested. (© 2011 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.     

Compositional variation in Si-rich SiGe single crystals grown by multi-component zone melting method using Si seed and source crystals

The effect of the supply of depleted Si solute elements on the compositional variation in the Si-rich SiGe bulk crystals was studied using the method which was used to grow Ge-rich SiGe single crystals with a uniform composition. By selecting the proper pulling rate, we can obtain Si-rich Si_1−xGe_x bulk crystals with uniform composition of x=0.1 without using the supply mechanism of depleted Si solute elements. When the supply mechanism of Si solute elements was used, the initial composition in Si-rich SiGe crystals can be much more easily determined by controlling the growth temperature than that in Ge-rich crystals because the Si seed crystal is not melted down. The supply of Si solute elements is very effective to change the compositional variation even for Si-rich SiGe crystals.     

Cr3+‐doped LiNbO3 crystals grown by the Bridgman method

The growth of LiNbO₃ crystals doped with Cr³⁺ ions in 0.1, 0.2, and 0.5 mol % concentrations by Bridgman method were reported. The Cr³⁺ ion concentrations in crystals were measured by inductively coupled plasma spectrometry. Electron paramagnetic resonance had been used to investigate the sites occupied by the Cr³⁺ ions. Two Cr³⁺ ion centers located at Li⁺ and Nb⁵⁺ sites (Cr_Li³⁺ and Cr_Nb³⁺ centers, respectively) were observed. Optical absorption and temperature‐dependence emission spectra of the Cr³⁺ ions were reported. The crystal‐field parameters and Racah parameters of the Cr³⁺ ion defect sites were reported and compared with those grown by Czochralski technique. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The influence of melt stirring intensity on the axial impurity distribution in proustite single crystals grown by the Stockbarger method using ACRT

The influence of modulated crucible rotation on the axial distribution of Cu, Mg and Si impurities in proustite single crystals grown by the Stockbarger method using ACRT is studied in a wide range of Taylor numbers (1.9·10⁵ < Ta < 7.12·10⁷). The impurity content in the upper part and in the tail portion of the grown crystals is measured using X‐ray‐phase analysis. Micro and macrostriations are observed in the grown crystals. The wavelengths of impurity content fluctuations have been determined. The microfluctuations of axial impurity content are caused by modulated crucible rotation. The studies have revealed that the ACRT provides an effective removal of impurities from the main part of the grown crystal at high intensity of melt stirring, and consequently, the ACRT can be applied validly to decrease the impurity content during the growing of high‐quality proustite single crystals. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

On the shape of crystals grown by Kyropoulos technique

The shape of the crystal grown by Kyropoulos technique has been evaluated on the basis of simple mass transfer approach. For some specific cases we have computed the shapes which are resaonable and generally in conformity with physical requirements. To verify the results crystals of KCl were grown under two specific conditions. The shapes of the resulting crystals agreeing with the calculated shapes within limits of error lend support to the validity of mass transfer approach.     

Twins in CdMnTe single crystals grown by Bridgman method

Cd_1‐xMn_xTe (x =0.2, CdMnTe) crystal was grown by the vertical Bridgman method, which exhibits a pure zincblende structure in the whole ingot. The major defect, twins, which is fatal to CdMnTe crystal, was analyzed with scanning electron microscopy (SEM), X‐ray energy disperse spectroscopy (XEDS) and optic microscopy on the chemical etching surface. The twins observed in the as‐grown ingot are mainly lamellar ones, which lie on the {111} faces from the first‐to‐freeze region of the ingot and run parallel to the growth axis of the ingot. Coherent twins with {115}_t‐{111}_h orientations when indexed with respect to both the twin and host orientations, are often found to be terminated by {110}_t‐{114}_h lateral twins. Te inclusions with about 20 μm in width are observed to preferentially decorate the lamellar twin boundaries. The origin of the twins, relating to the growth twin and the phase transformation twin, is also discussed in this paper. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Morphology and growth mechanism of vapor grown Cd crystals as affected by Bi impurity

The effects of Bi impurity on the morphology and growth mechanism of (physical) vapor-deposited Cd crystals were investigated. Scanning electron microscopic observation revealed, for the first time, hexagonal prismatic Cd crystals which were grown on the Bi contaminated pyrex glass tube wall. This kind of morphology does not appear in the case of pure Cd without the impurity Bi. The top of the hexagonal prismatic crystal was usually rounded hemispherically. X-ray microprobe investigations showed that the tip of the crystals contained about 57 wt% Bi. It was concluded that the Cd hexagonal prismatic crystals grow by the mechanism of vapor-liquid-solid with the impurity Bi.     

The influence of the intensity of melt stirring on the radial impurity distribution in proustite single crystals grown by the Stockbarger method using ACRT

The influence of the intensity of melt stirring on the radial impurity distribution and optical quality of proustite single crystals grown by the Stockbarger method using ACRT is studied by the example of Cu, Sb and Mg impurities. We report results obtained in a wide range of Taylor numbers (1.9×10⁵<Ta<7.12×10⁷). The studies revealed that the ACRT can be applied validly to decrease the impurity content during the growing of high-quality single crystals.     

Homogeneous SiGe crystals grown by using the traveling liquidus-zone method

It is indispensable to estimate a diffusion coefficient in a solution zone in order to grow a homogeneous crystal by using the traveling liquidus-zone (TLZ) method. To estimate the diffusion coefficient of Ge in the SiGe solution zone, result of a two-dimensional numerical simulation is compared with an experimental result. From the comparison, the diffusion coefficient is estimated to be 9.5×10⁻⁵ cm²/s. By using this coefficient, a sample translation rate for obtaining a homogeneous SiGe crystal is determined. By translating samples with appropriate rates, homogeneous Si_0.5Ge_0.5 crystals are successfully grown. The typical Ge composition is 0.496±0.006 for more than 13 mm long. The experimental result shows the homogeneity of ±1.2% in the mole fraction. This deviation corresponds to the variation of less than ±0.03% in the lattice constant. Since this variation is negligibly small, the homogeneity is excellent. Thus it is found that the TLZ method is the universal growth technique, which is applicable to the crystal growth of not only the III–V compounds but also the IV–IV compounds.     

Characterization of bismuth germanate crystals grown by EFG method

Bismuth germanate shaped crystals have been grown by the EFG (Stepanov) method. The correlation between growth rate, shape of crystals, their optical and scintillation parameters has been analysed. Optical and scintillation characteristics of the EFG crystals are similar to those obtained with Czochralski grown crystals, however, growth rate in EFG is by 2.5 times larger. Also we compare the photochromic effect under UV‐irradiation in EFG and Czochralski grown crystals. Material losses at fabrication of plates, pixels, and rods from EFG shaped plates may be reduced by ∼50% compared to large diameter boules.     

Fluctuations of impurity composition and their role in dislocation cross slip in crystals

The influence of impurities on the kinetics of split-dislocation cross slip caused by a change in the stacking-fault energy is studied theoretically. It is shown that the fluctuations in the impurity composition of a crystal make a considerable contribution to the kinetics of dislocation cross slip. The activation-energy spectrum and the average frequency of the processes of dislocation cross slip are calculated for a model of random impurity distribution in a crystal. The calculation shows that the fluctuations in impurity concentration, reducing the stacking-fault energy, play an important role in the low-temperature region.     

A simple method to determine the real composition of LiNbO3 crystals

The shift of the UV-absorption edge was applied to determine the real LiNbO₃ crystal composition. The accuracy of the method is about 10⁻² mole% using a simple commercial UV-spectrophotometer. The effect of various impurities and other error sources are discussed.     

Precipitation and dissolution of KCaCl3 impurity in NaCl crystals

Impurity precipitation in NaCl crystals containing CaCl₂ and KCl in various proportions is studied by means of flotation density measurements. The paper is concerned with the determination and dissolution, the kinetics and activation energy, and the mechanism of nucleation. Two temperature regions for solid solution decomposition were revealed. The characteristic stages in density variation upon isochronal annealing are shown to be correlated with radical changes in the X-ray diffraction patterns. Evidence is given that the nucleation is heterogeneous for the stable phase and homogeneous for the metastable one. – The activation energy in the low-temperature region has been found to be 0.8 ± 0.1 eV, which suggests precipitation to be diffusion-limited. From the kinetics studies it follows that the composition of the metastable phase corresponds to KCaCl₃ and the rate-controlling stage in stoichiometric crystals is a K⁺ diffusion.     

On voids in InxGa1−xSb crystals grown by an ultrasonic- vibration-introduced Czochralski method

The shape and size of voids, and the grown region surrounding a large void were investigated in In_xGa_1–xSb crystals, which were pulled under the introduction of ultrasonic vibrations into the source melt by using a modified Czochralski apparatus. The presence of voids in crystals resulted from (1) atmosphere gas was confined beneath the growth interface of a seed crystal during the seeding procedure, and (2) many bubbles–generated by the cavitation effect due to ultrasonic vibrations–were caught in the growing crystal. Voids were circular, deformed trapezoid, and complex in shape, and were in a range of 20 μm to 3 mm in size. Even in case of a void with the diameter as large as 2 mm, the grown region surrounding it was in the single crystalline state. In this interesting region, the microscopic variation of In concentration and the abrupt change of growth rate were observed.     

Study of microdefects in GaP and GaPZn single crystals grown by the liquid-encapsulation Czochralski method

Microdefects in undoped and zinc-doped GaP single crystals grown by the liquid-encapsulation Czochralski method have been studied by X-ray diffuse scattering. In undoped GaP single crystals, deviation from stoichiometry increases from the beginning to the end of an ingot. The ingot end is characterized by enhanced precipitation of excess gallium with formation of platelike microdefects. With an increase in their size, stress relaxation around microdefects begins to manifest itself. Doping with zinc leads to a significant change in the microdefect formation pattern.