Preferred Growth of Antimony Single Crystals

Single Crystals of antimony were grown by the Chalmer's method from the melt. The crystals were grown under different temperature gradients of 92 °C/cm, 75 °C/cm and 52 °C per cm. The growth velocities were varied from 1.5 cm/hr to 9 cm/hr. At low growth velocities antimony exhibits a preferred orientation in the range 1 cm/hr to 6 cm/hr. No effect of temperature gradient is observed. The results are compared with those of bismuth, cadmium and zinc which are contradictory to what has been observed.     

Direct melt crystal growth of isotactic polybutene‐1 trigonal phase

The morphology, crystalline structure and crystal growth kinetics of melt‐crystallized thin isotactic polybutene‐1 films have been studied with transmission electron microscopy, electron diffraction and optical microscopy. It is demonstrated that a bypass of tetragonal phase crystallization and direct melt crystal growth of the trigonal phase can be achieved via self‐seeding at atmospheric pressure using solution‐grown trigonal crystals as nuclei. Electron microscopy and optical microscopy observations show that melt‐crystallized isotactic polybutene‐1 single crystals of the trigonal phase have rounded or hexagonal morphologies around 75°C. The growth rate of trigonal crystals in the melt has been obtained by in‐situ optical microscopy. The growth rate of trigonal crystals in the melt is 1/100 and 1/1000 that of tetragonal crystals in the melt around 70 and 90°C, respectively. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Interface Dynamics during Indium Antimonide Crystal Growth

Experiments with a stoichiometric InSb compound were first performed at small temperature gradient across the crystal/melt interface of 3 °C/cm and furnace translation velocity, V_frn, of 2 μ/sec. Known growth requirements for quality crystals were confirmed. They are, (1) the interface temperature must be close to the congruent melting temperature and, (2) the interface must be located within the adiabatic zone. These requirements can be obtained only through specific settings of the heater temperatures. An X-ray radioscopic system has been modified to accommodate real-time visualization of the crystal/melt interface during vertical Bridgman-Stockbarger growth of InSb. It is shown that asymmetric temperature settings of the heaters can be advantageously used to minimize defect formation. The interface temperature was assessed indirectly with calibrated outside thermocouples. Optical microscopy and electron microprobe analyses provided feedback on crystalline homogeneity.     

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)     

Influence of annealing on nanocrystal formation in Ni amorphous alloy

An amorphous Ni alloy has been obtained as a ribbon by plasma-arc melt spinning in a copper water-cooled lining slag crucible. Ribbon samples have been annealed in a special cylindrical furnace at temperatures from 200 to 400°C for 1 h in Ar. It is established that nanocrystals in the alloy samples increase in size with increasing annealing temperature. The rise of resistivity upon annealing at temperatures below 300°C and its significant decrease at higher temperatures is consistent with the change in the amorphous alloy microstructure.     

Growth and characterization of SSD InP crystals used as substrates for infra-red LED's

Bulk indium phosphide crystals have been grown by the synthesis, solute diffusion (SSD) method. Various growth temperatures and temperature gradients in the indium melt were investigated. The growth temperature of about 850–900°C and the temperature gradient of about 10–15°C cm⁻¹ were found as the most suitable growth conditions. All grown crystals were of the n-type either undoped or doped with Te or Sn. Infrared light-emitting junctions were grown by single LPE process. Characteristic surface structures of InP epitaxial layers as a function of the growth temperature and cooling rate were observed. Efficiencies of LED's have been typically 0.8%. Single LPE process on LEC InP substrates has given LED's with substantially lower efficiencies.     

A crystallizer for the investigation of conditions of growth of single crystals from solutions

The crystallizer of the Walker-Kohman type for isotherm growing of single crystals from solutions is described which has been designed to provide the maintenance of constant conditions of crystallization chosen in advance and the investigation of the influence of these conditions on the resulting structural regularity of the crystals as grown. The temperature of the solution can be kept inside the interval from 30 to 60°C, with an accuracy ±0.002°C. The equipment allows the setting and keeping the requested value of supersaturation, hydrodynamic conditions, thermal stabilization of the crystallization solution and enables the optic and gravimetric observing of the single crystal during its growth. The total function of the described equipment was tested by growing single crystals of triglycine sulphate at 52°C.     

Electical,Magnetic, and Thermal Properties of Cadmium Hydrogen Phosphate Hydrate Crystals

The d.c. electrical conductivity of pelletized samples of cadmium hydrogen phosphate hydrate (CHP) crystals have been studied in the temperature range 50 °C to 250 °C. It has been observed that CHP crystals exhibit ionic conductivity at 140 °C and possess semiconducting property. At room temperature CHP has stable crystal structure. From thermal analysis it is concluded that CHP crystals possess water of crystallization and the material to be diamagnetic.     

Preparation and some properties of synthetic proustite single crystals

Conditions for the preparation of proustite single crystals are reported. For selecting these conditions temperature gradients in the crystallisation zone and in the melt, the rate of moving of the crystallisation front, the radial gradient, tube geometry, stabilisation of temperature, mechanisms of zone travelling, partial pressures were changed. – Differential-thermal, X-ray, and spectral-chemical analysis were applied to initial substances and final crystal bodies. To decrease the influence of spontaneous crystallisation an optimal temperature gradient was applied approaching maximum undercooling at the liquid-solid interface. – Optically transparent proustite crystals resulted. In the range from 1 to 12 μm they show 80% transparency. Microhardness was measured along the growth direction which deviated from the c-axis about 25°.     

Dielectric and thermal behaviour of holmium tartrate trihydrate crystals

Measurements on dielectric constant of holmium tartrate trihydrate crystals at frequencies of the applied a.c. in the range 1 kHz to 1 MHz and at temperature in the range 30°C to 330°C are reported. The dielectric constant ε′ increases with temperature at all frequencies, attains a peak near 250°C, and then decreases as the temperature goes beyond 250°C. The anomalous dielectric behaviour at near about 250°C is attributed to be as a result of crystallographic/polymorphic phase transition brought about in the material. The results on the dielectric behaviour of the material are supplemented by results of thermal analysis viz., TG and DTA. Thermogravimetric and differential thermal analytic techniques have been used to study thermal behaviour of the material. It is shown that the material is thermally stable up to 220°C beyond which it decomposes through three stages till the formation of holmium oxide at 1200°C. The non‐isothermal kinetic parameters e.g., activation energy and the frequency factor have been evaluated for first two stages of thermal decomposition by using the integral method of Coats and Redfern. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization of Sulphides in KSCN Melts

The melt of potassium thiocyanate can be used as solvent and as supplier of sulphur for the preparation of crystals of sulphides and complex sulphosalts. The solubilities of some sulphides in the KSCN melt were determined at 250°C. Small crystals of sulphides of Cu, Ag, Tl, Hg, Pb, Ni and of ternary As- and Sb-sulphosalts of these metals could be obtained from this flux in a temperature gradient. Moreover, crystals of sulphides were formed by a direct slow reaction of metals with molten KSCN.     

Synthesis,structural and thermal studies of tetrathioureacopper(I) chloride crystals

Tetrathioureacopper(I) chloride, hereafter abbreviated as TCC, was synthesised and single crystals were obtained from saturated aqueous solution by slow evaporation (solution growth) method at room temperature. The crystals obtained are bright, colourless and transparent having well defined external faces. The grown crystals were characterized through elemental analysis, single crystal X‐ray diffraction study, thermal analysis, electron spin resonance spectroscopy and Fourier Transform infrared spectroscopy. The elemental analysis confirms the stoichiometry of the compound. The single crystal diffraction studies indicate that TCC crystallises in the tetragonal lattice and the unit cell parameters are a = b = 13.4082 Å, c = 13.8074 Å, V = 2482.29 ų, α = β = γ = 90°. Space group and the number of molecules per unit cell (Z) are found to be P4₁2₁2 and 8 respectively. The TG curve of the sample shows a prolonged decomposition from 210 to 628.3 °C, from which the decomposition pattern has been formulated. The endothermic peaks in the DTA curve indicate melting and decomposition of the compound at 165.2 and 633.8 °C respectively. An exothermic peak in high temperature DSC indicates a phase transition in the compound at 274.8 °C. Thermal anomalies observed in the low temperature DSC at –163.3, –152.0, –141.5, –108.3, 1.0 and 12.1 °C in the heating run and –157.1 and –153.9 °C in the cooling run reveal first order phase transitions in the crystal. The peaks observed at –146.2 °C in both the heating and cooling runs suggest occurrence of a second order phase transition in this compound. The IR spectroscopic data were used to assign the characteristic vibrational frequencies of various groups present in the compound. The ESR study confirms that the copper is in the +1 oxidation state in the complex. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Ionic conductivity studies in KCl–NaCl mixed crystals

Single crystals of KCl and a few compositions of KCl-NaCl mixed crystals were grown from melt by Kyropoulos technique. Ionic conductivity measurements have been carried in these crystals in the temperature range 100 to 400 °C. The activation energy for the migration of charge carriers have been calculated from the conductivity-temperature plots of these crystals and the results obtained were discussed.     

Growth and Dislocation Etching of InBi0.8Sb0.2 Single Crystal

InBi_0.8Sb_0.2 single crystals have been grown by zone melting method. The freezing interface temperature gradient of 3 °C/cm has been found to yield the best quality crystals obtainable at growth velocity 1.0 cm/hr. Traingular features have been obtained on the free surface of the as grown crystal. A new dislocation etchant based on nitric acid has been found to give reproducible etch-pitting on the cleavage surface. Standard tests for a dislocation etchant have been carried out and results are reported.     

Single crystal growth from the melt and magnetic properties of hexaferrites–aluminates

Single crystals of aluminum substituted barium hexaferrite were grown by the floating zone method with optical heating. Single crystals were produced from a melt of stoichiometric composition. The process was carried out under a pressure of 50 atm of oxygen. In the system BaO–(x)Al₂O₃–(6?x)Fe₂O₃ the region of single phase crystal growth from the melt is limited by the value x=3. For higher substitutions single-phase crystallization is not observed. The grown single crystals are cylindrical boules with a diameter of 4–5 mm and with lengths up to 50 mm. To avert cracking the crystals have been annealed during the process of growth at 1100 °C. The content of FeO in the composition of single crystals of barium hexaferrite, grown by zone melting under an oxygen pressure of 50 atm, is approximately 0.3 wt%. In the system of hexaferrite–aluminates the macroscopic magnetic moment of the material disappears at x=3.     

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.     

Crystal growth of ZrW2O8 and its optical and mechanical characterization

ZrW₂O₈ is known for its isotropic negative thermal expansion over a wide of range of temperature from ?272 to 777 °C. However, ZrW₂O₈ melts incongruently at 1257 °C and is stable only over a short temperature interval between 1105 and 1257 °C. This makes the growth of single crystals a formidable challenge. In order to study the intrinsic properties of this compound, a repeatable, viable single crystal growth strategy is required. Here we report a simple, self-seeding, self-fluxing single crystal growth process which resulted in single crystals of ZrW₂O₈ up to about 4 mm in size. Grown crystals were characterized by X-ray diffraction (XRD), Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. Mechanical properties of the crystals were studied using nanoindentation.     

Thermodynamic feasibility study for chemical vapour deposition of some ternary crystals using iodine and hydrogen iodide

Thermodynamic feasibility of transition metal dichalcogenide (TMDC) single crystals of Cu Al S₂, Cu Al Se₂, Cu Al Te₂, Cu Ga S₂, Cu Ga Se₂, Cu Ga Te₂, Cu In S₂, Cu In Se₂, Cu In Te₂, Ag Ga S₂, Ag Ga Se₂, Ag Ga Te₂, Ag In Se₂, Ag In Te₂, using iodine and hydrogen iodide as transporting agents has been reported in this paper. Results give range of temperature for the iodide transport and prevention of starting material formation (elemental transport) in the growth zone. From the range of temperature for the growth of crystals, selected source zone and growth zone temperatures with a differential of 100 °C are also listed. Referring the data listed in the tables can grow good quality crystals. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Influence of reduced working frequencies on the floating‐zone growth of silicon single crystals

Lowering the working frequency in the inductively heated floating zone growth of Si Single crystals will reduce the risk of arcing at the induction coil. This is of particular interest in the growth of large diameter crystals. In the current paper we present results from growth experiments at lower frequencies, 2 MHz and 1.7 MHz. It is found that the growth of dislocation‐free crystals is possible at these frequencies and cause distinct changes in the interface deflection and radial resistivity profiles. Results from numerical simulation of the melt flow at different frequencies are presented. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Experimental investigation of different configurations for the seeded growth of SiC crystals via a VLS mechanism

The growth of SiC crystals or epilayers from the liquid phase has already been reported for many years. Even if the resulting material can be of very high structural quality and the possibility to close micropipes was demonstrated, handling the liquid phase still is a challenge. Moreover, it is highly difficult to stabilize the C dissolution front and then to stabilize the growth front over a long growth time. Based on the Vapour‐Liquid‐Solid (VLS) mechanism, we present a new configuration for the growth of SiC single crystal which should allow first to simplify the liquid handling at high temperature and second to precisely control the crystal growth front. The process consists in a modified top and bottom seeded solution growth method, in which the liquid is held under electromagnetic levitation and fed from the gas phase. 3C‐SiC crystals exhibiting well‐faceted morphology were successfully obtained at 1100‐1200 °C with exceptional growth rates, varying from 1 to 1.5 mm/h in Ti‐Si melt. It was shown that the nucleation density decreases simultaneously with increasing propane partial pressure. At 1200‐1400 °C, thick homoepitaxial 6H‐SiC layers were successfully obtained in Co‐Si and Ti‐Si melts, with growth rate up to 200 µm/h. Large terraces with smooth surfaces are observed suggesting a layer by layer growth mode, and the influence of the system pressure was demonstrated. It was shown that the terrace size decrease simultaneously with increasing propane partial pressure which suggests the beginning of a two dimensional to three dimensional growth mode transition. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)