Growth of high-purity ZnTe single crystals by the sublimation travelling heater method

A travelling heater method (THM) was developed to grow high-purity ZnTe from the vapor phase. This crystal growth method is called the “sublimation THM”. The temperature of the sublimation interface was set at 815°C and the temperature of the growth interface was varied from 785 to 800°C. The growth rate was 3 mm/day. Under these conditions, it was found that the growth process was mainly due to surface nucleation. Characteristics of the crystals were compared with those of solution-THM and vapor phase epitaxially grown crystals. The free-exciton line at 2.381 eV strongly appears and a doublet structure in neutral- acceptor bound exciton at 2.375 eV is clearly resolved with splitting energy of about 0.7 meV. We thus conclude that the THM from the vapor phase is suitable for preparing ZnTe single crystals which have excellent luminescent properties.     

Numerical optimization of thermal field in CdTe crystal growth by travelling heater method

Cadmium telluride (CdTe) and his compounds play a leading role in X‐ray and γ‐ray detector technology. One of the most used methods for growing these crystals is the travelling heater method (THM). The ingots obtained by using this technique show excellent composition uniformity, but the structural quality is affected by the presence of large grains which appear because of large curvatures of the solid‐liquid interface during the solidification process. This numerical work investigate the thermal field and melt convection in CdTe processing by THM in order to elucidate the mechanism of growing these crystals. The influence of the furnace geometry on the interface shape and temperature gradient in liquid is analyzed for samples with small (1 cm) and large (5 cm) diameters. The computations include flow effects on thermal field in the melted zone. The thermal conditions are optimized for THM growth of CdTe crystals at high solidification temperatures. A new multi‐zone furnace configuration for growing crystals of large diameter and flattened interface is proposed in this work.     

Double crystal topographic investigations of PbTe grown by the travelling heater method (THM)

THM-grown PbTe and PbTe: Tl were examined near the (n, —n)-position by means of X-ray double crystal arrangement. The half-width of the rocking curves of Tl doped PbTe is larger than that of undoped PbTe by factor two. Long range and local lattice plane distortions, as well as disturbances induced during preparation, in the from of dislocation slip lines and greatly disoriented areas were observed.     

Experimental measurement of temperature distribution across a loop-like heater

A new method for in situ measuring the temperature distribution of small loop-like heater for crystal growth in space is proposed. The existence of thermocouple and other attachment may cause the non-uniformity of the heater temperature distribution.     

Crystal growth by the travelling heater method using tapered crucibles and applied rotating magnetic field

Crystal growth experiments were carried out by the Travelling Heater Method using tapered growth ampoules with and without the application of a rotating magnetic field. The objective was to enhance its commercial potential by reducing the size of required seed crystals and increasing the growth rate. To this end, a number of GaSb crystals were grown using either 25 mm diameter straight, or 10 mm to 25 mm tapered growth ampoules. Growth rates of 2 mm/day and 5 mm/day were employed. The effect of rotating magnetic fields of several strengths and frequencies was examined. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The numerical simulation of heat and mass transfer during growth of a binary system by the travelling heater method

The influence of convection and heat and mass transfer on the shape and position of melt/solid interfaces and on radial composition segregation is analysed numerically for the travelling heater method growth of a binary alloy in a vertical transparent ampoule. Results are presented for crystal and melt with thermophysical properties similar to Cd_xHg_1−xTe with the assumption that the pseudobinary CdTe-HgTe phase diagram is true. The two-dimensional axisymmetric heat transfer equation, hydrodynamical equation and convective diffusion equation are included in the mathematical model. The rates of crystal growth and dissolution are supposed to be proportional to the compositional supercooling in the melt near the interfaces. It is shown for the conditions when convection is absent that the interfaces are asymmetrically positioned respectively to the heater centre line. Intensive convection makes their position more symmetrical but the length of the liquid zone greater. The flow pattern in the melt appears to be greatly influenced by solutal gravitational convection. The nonlinear dependence of the melt density on the temperature and composition are used in the model. The cases when speed of the heater is antiparallel (stable density stratification) or parallel (unstable stratification) to the vector of gravitational acceleration are considered.     

Diffusion-controlled distribution of solute in Sn-1% Bi specimens solidified by the submerged heater method

Two 1.35 kg, 5.8 cm diameter Sn-1% Bi specimens were solidified using the submerged heater method (SHM). The distribution of solute was found to be uniform axially, indicating that diffusion-controlled steady-state segregation, though to be unattainable on earth because of the gravity induced interference, was achieved.     

Influence of gravitation on the processes of heat and mass transfer in solution crystal growth by the travelling heater method (THM) (III)

The effect of the natural and thermocapillary convection on the vortex configuration in solution during growth of PbTe crystal by the travelling heater method is considered. The estimation of the parameters of growth process (i. e. axial temperature gradients, gravitational acceleration, degree of the solution's surface contact with ampoule), when the vortex configuration undergoes qualitative variation, is given. In terms of the one-dimensional thermodiffusive problem solution the effect produced by the convective stirring on the position of growing and dissolving interfaces is described.     

Calculation of temperature fields in a cylindrical heater system

A model for calculation of time dependent temperature fields in a cylindrical furnace used for crystal growth experiments is described. The comparison of the calculated and the experimental temperature profiles shows good agreement in the stationary case and the suitability of the model for the prediction of static temperature fields on the basis of given heating power distributions, and vice versa.     

Controlling the axial temperature gradient in inductively heated Czochralski systems

A heating system is described that allows to increase the temperature gradients in rf‐heated Czochralski setups during the growth. This system applies an active afterheater, operated by a separate induction coil parallel to that heating the crucible. By changing the inductivity of an additional coil located outside the growth chamber, the ratio of the rf currents flowing through the crucible and afterheater and, consequently, the geometry of the heat input to the setup can be altered. The efficiency of the heating systems has been demonstrated in various experiments.     

Simple calculation of the axial temperature characteristics of a unidirectionally solidified sample

The model described in this paper treats the numerical solution of a heat transfer problem in a one-dimensional way determining the axial temperature characteristics. The physical quantities are considered as values depending on temperature and the real wall temperature profile of the heating-cooling system is included. The sample shape corresponds to the numerous cases of long and thin cylinders. The calculation were carried out by a medium desk computer. The results of the calculation are in good line with the experimental data.     

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)     

Comparison of cadmium manganese telluride crystals grown by traveling heater method and vertical Bridgman method

In this paper, the CdMnTe crystals were grown by the Travelling Heater Method (THM) and the Vertical Bridgman (VB) method, respectively. The crystal properties, including the Mn axial distribution, impurity concentrations, resistivity, Hall effects and energy response spectra, were characterized and compared. The results shown that the CdMnTe crystal grown by the THM had more uniform Mn distribution and lower impurity concentrations compared to the crystal grown by VB method. The resistivity of CdMnTe grown by THM was (1.5 ∼ 8) × 10¹⁰ Ω.cm, while the resistivity of CdMnTe grown by VB was 10⁷∼10⁸ Ω.cm. The In dopant distributed uniformly throughout the crystal ingot grown by THM with the doping concentration of 0.6–0.7 ppm, while the In dopant concentration throughout the crystal grown by VB method is in the range of 1.31–2.4 ppm. Hall measurements revealed that the conductivity of the THM grown crystal was weak n‐type conductivity and the VB grown crystal was p‐type conductivity. A planar CdMnTe detector from the THM grown crystal showed a resolution of 8% of the ²⁴¹Am radiation at 59.5 keV peak, however, no energy response was revealed with the CdMnTe detector by the VB method. The results demonstrate that CdMnTe crystal grown by THM have better crystal quality and detector properties compared to that by VB method.     

Optimization of surface temperature distribution for control of point defects in the silicon single crystal

Optimization of crystal surface temperature distribution is performed for the control of point defects in a silicon single crystal grown by the Czochralski process. In the optimization problem, we seek an optimal solution that minimizes the level of point defects while the radial uniformity of temperature is maximized. In order to solve the optimization problem with the equality constraints described by partial differential equations, the variational principle is used. Based on the calculus of variations and the method of Lagrange multiplier, the Euler–Lagrange equations are derived and solved by the finite difference method. In order to handle inequality constraints, the penalty function method is also applied. The optimal distribution of the crystal surface temperature is expected to provide an insight for the design of thermal surroundings such as the thermal shield configuration and the heater/cooler position.     

Heat and mass transfer problems in solution growth of GaP crystals by the travelling solvent method (TSM)

The influence of the natural convection on the heat and mass transfer process during growth of GaP crystals from the solution is considered. The two-dimensional quasi-stationary thermodiffusive hydrodynamic problem for the GaP growth system by travelling solvent method (TSM), as a model, has been solved. Computation is given for the temperature and concentration field distribution in the solution. The picture of vortex configuration for different lengths of the liquid zone, the shape of the growing and dissolving interfaces and also the boundary layers thickness are obtained. The experimental dependence of the growth rate on the convection intensity observed mostly confirmed the calculation results.     

A novel method of temperature control for a crystal growth puller

A facile method to control the contracting rate of the thermal expansible bars for pulling crystal is first suggested. The thermal expansible bars, set in a modified Dewar flask whose vacuum degree is controlled, are heated to designed temperature and then switch off the power to let it cool down at a desired rate, which depends largely on the changeable vacuum degree. This new approach is expected to completely eliminate the effects, which possibly reduces the smooth extent of thermal expansion, caused by the minor temperature fluctuations during crystal growth process and to realize the utmost smooth and slow pulling rate. It is expected to install this apparatus in optical floating zone furnace, instead of traditional motor, to grow peritectic crystal, such as crystal Bi‐2223, since for the peritectic reaction, in principle, the extremely slow growing rate is considerably essential.     

Numerical study of radial temperature distribution in the AlN sublimation growth system

A large radial temperature gradient in the AlN sublimation growth system would lead to non‐uniform growth rate along the radial direction and introduce thermal stress in the as grown crystal. In this paper, we have numerically studied the radial thermal uniformity in the crucible of a AlN sublimation growth system. The temperature difference on the source top surface is insignificant while the radial temperature gradient on the lid surface is too large to be neglected. The simulation results showed that the crucible material with a large thermal conductivity is beneficial to obtain a uniform temperature distribution on the lid surface. Moreover, it was found that the temperature gradient on the lid surface decreases with increased lid thickness and decreased top window size.     

Axial temperature distribution in Silicon-Germanium grown by the RF-heated float zone technique

The RF-heated float zone method has been used to study the segregation behaviour of silicongermanium solid solutions in the concentration range from 0 to 25 at% germanium. Completely dislocation free crystals up to 8 at% germanium could be obtained. Since constitutional supercooling is the main reason preventing single crystalline growth, pyrometric temperature measurements have been performed to reveal the temperature slope at the interface and to determine the critical growth rate. The temperature gradient ΔT/Δz was found to increase with increasing germanium concentration.