Structure of selenium and tellurium clusters in cavities of NaX zeolite

The structure of NaX zeolite crystals with the Se and Te atoms incorporated into the structure from their vapors has been studied. It is shown that selenium atoms form clusters in the shape of six-and four-membered rings located in the cuboctahedral cavities of the structure framework. Single Se₂ molecules are located in large cavities, whereas Te atoms form four-membered rings located in cuboctahedra. Large cavities are occupied by two alternating configurations of Te atoms forming either a chain consisting of 16 links or an eight-membered ring.     

Growth parameters for large diameter float zone silicon crystals

Factors that directly affect the ability to grow dislocation free float zone silicon crystals up to 80 mm in diameter have been experimentally determined. The highest yield is obtained for 80 mm diameter crystals by starting with 68 mm to 74 mm diameter poly crystal rod stock. Lower transport speeds for crystal growth of (111) orientation crystals were 3 to 4 mm/min and for (100), 2 to 3 mm/min. Rotation rates of both upper and lower shafts were found to have an effect on growth at the solid-liquid interface. Rates established for lower shaft were 6 to 8 rpm for the (111) crystals and 3 to 4 rpm for (100), counter-clock-wise. Upper rotation rates were 2 rpm on (111) crystals and 3 to 5 rpm on (100), clockwise. Seed orientation, which is critical, was held to within plus or minus $\text{1}\text{2}\text{°}$ of perfect orientation. The minimum seed growth length was 50 to 70 mm. To assist in reducing the side lobes on (111) dislocation free crystals, a cooling ring with a flow or argon was used. For best (100) growth the shape of the lower side of a one turn copper rf work coil was made conical. Six to ten dislocation free crystals in each orientation group were produced using these parameters.     

Hydrodynamic conditions for growth of large KDP crystals

Three-dimensional mass transfer is simulated. The factors determining the hydrodynamic conditions for efficient mass transfer in growth of large KDP single crystals (cross sections up to 45 × 45 cm²) from solutions in a real 300-l-crystallizer are established. The conditions for the motion of the supersaturated solution to the surface of a growing crystal in the direction opposite to that of gravitation are attained. The growth mode developed provides growth rates that are five times higher of large high-quality optical KDP crystals.     

Investigations on the crystallization of larger NaA and NaX zeolite crystals in the presence of triethanolamine (I). The influence of Na2O and SiO2 content

Sodium silicate-aluminate aqueous systems with various contents of Na₂O and SiO₂ containing triethanolamine were crystallized. Optimum Na₂O and SiO₂ contents have been observed to give NaA and NaX zeolite crystals with dimensions up to 80 μm. For NaA crystals the values are: ∼ 3.5 mass% Na₂O, ∼ 1.65 mass% SiO₂; for NaX crystals ∼ 2.5 mass% Na₂O, ∼ 1.5 mass% SiO₂. – The effect of other additives on crystal size is proved. – The results are discussed in terms of nucleation and growth, reaction rate, and supersaturation. Supposition are made to gain larger crystals by maintaining the excess of solute over a longer period of time.     

Vertical Bridgman growth and characterization of large ZnGeP2 single crystals

The growth of ZnGeP₂ crystals by seeded Vertical Bridgman method was studied. High-quality near-stoichiometric ZnGeP₂ single crystals obtained were of 20–30 mm in diameter and 90–120 mm in length. By selection of the seed crystallographic orientation the single crystal ingots without cracks and twins were grown, as shown by X-ray diffraction. The infrared transmission property of the ZnGeP₂ crystals was studied by the calculated optical absorption coefficient spectra. The results showed that after thermal annealing of the crystals the optical absorption coefficient was ～0.10 cm^?1 at 2.05 μm, and ～0.01 cm^?1 at 3–8 μm. The rocking curves patterns of the (4 0 0) reflection demonstrated that the as-grown single crystals possessed a good structural quality. The composition of the crystals was close to the ideal stoichiometry ratio of 1:1:2. The low-loss typical ZnGeP₂ samples of 6 mm×6 mm×15 mm in sizes were cut from the annealed ingots for optical parametric oscillation experiments. The output power of 3.2 W was obtained at 3–5 μm when the incident pumping power of 2.05 μm laser was 9.4 W, and the corresponding slope efficiency and the conversion efficiency were 44% and 34%, respectively.     

Flux process for growth of large crystals with application to beryllia

A procedure is described for flux-growth of beryllia crystals, applicable to other crystals. Growth is promoted in a solvent flux by continuous transport of BeO solute in a steady-state thermal gradient. Prepared seeds are mounted on a support structure, submerged in the flux at thermal equilibrium, and rotated during the growth period. The character of growth depends on multi-parameter growth conditions including proper seed crystal structure and preparation, flux composition and impurities, temperature, and operational procedures.     

Analysis of the dopant segregation effects at the floating zone growth of large silicon crystals

A computer simulation is carried out to study the dopant concentration fields in the molten zone and in the growing crystal for the floating zone (FZ) growth of large (> 100 mm) Si crystals with the needle-eye technique and with feed/crystal rotation. The mathematical model developed in the previous work is used to calculate the shape of the molten zone and the velocity field in the melt. The influence of melt convection on the dopant concentration field is considered. The significance of the rotation scheme of the feed rod and crystal on the dopant distribution is investigated. The calculated dopant concentration directly at the growth interface is used to determine the normalized lateral resistivity distribution in the single crystal. The calculated resistivity distributions are compared with lateral spreading resistivity measurements in the single crystal.     

3D simulation of the effects of growth parameters on the growth of sapphire crystals using heat exchanger method

3D simulations using the commercial CFDRC and FIDAP code, which are based on finite element techniques, were performed to investigate the effects of anisotropic conductivity on the convexity of the melt–crystal interface and the hot spots of sapphire crystal in a heat‐exchanger‐method crystal growth system. The convection boundary conditions of both the energy input to the crucible by the radiation as well as convection inside the furnace and the energy output through the heat exchanger are modeled. The cross‐sectional flow pattern and the shape of the melt–crystal interface are confirmed by comparing the 3‐D modeling results with previous 2D simulation results. In the 3D model, the “hot spots” in the corners of the crucible are donut shaped, and the shape changes with the value of the conductivity of anisotropic crystal. The outline of the crystal becomes more convex as the conductivity in the z direction (k_sz) increases. The outline of melt–crystal interface is elliptical when the anisotropic conductivity is moving in the radial direction (k_sx and k_sy). The portion at the outline touching the bottom of the crucible is smaller than the maximum outline of the crystal, meaning that the shape at the “hot spot”, changes with the value of the conductivities of anisotropic crystal. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Oriented growth of large size calcium fluoride single crystals for optical lithography

We report (1 1 1), (1 1 0) and (1 0 0) growth of CaF₂ by the vertical Bridgman method. Crystals up to 250 mm diameter were grown and various growth parameters such as growth rate, temperature gradient and post-growth cooling rate were studied. It was found that the growth rate and the cooling rate are slower for the larger diameter crystals with a fixed temperature gradient. These growth parameters were optimized for growing the crystals along specific orientation after realizing that CaF₂ has a tendency to grow along an orientation close to 1 1 0. Degradation in optical transmittance was evaluated by irradiating the crystal to γ-rays up to a dose of 10⁵ rad. Optimized scavenger addition resulted in crystals with better radiation resistance and excellent VUV transmittance.     

Surface growth mechanisms and structural faulting in the growth of large single and spherulitic titanosilicate ETS-4 crystals

Morphological, surface and crystallographic analyses of titanosilicate ETS-4 products, with diverse habits ranging from spherulitic particles composed of submicron crystallites to large single crystals, are presented. Pole figures revealed that crystal surfaces with a-, b- and c- axes corresponded to 110, 010 and 001 directions, respectively. Thus, technologically important 8-membered ring pores and titania chains in ETS-4 run along the b-axis of single crystals and terminate at the smallest crystal face. Height of the spiral growth steps observed on 1 0 0 and 0 0 1 surfaces corresponded to the interplanar spacings associated with their crystallographic orientation, and is equivalent to the thickness of building units that form the ETS-4 framework. Data suggest that the more viscous synthesis mixtures, with a large driving force for growth, increased the two- and three-dimensional nucleation, while limiting the transport of nutrients to the growth surface. These conditions increase the tendency for stacking fault formation on 1 0 0 surfaces and small angle branching, which eventually results in spherulitic growth. The growth of high quality ETS-4 single crystals (from less viscous synthesis mixtures) occurred at lower surface nucleation rates. Data suggest that these high quality, large crystals grew due to one-dimensional nucleation at spiral hillocks, and indicate that under these conditions un-faulted growth is preferred.     

Analysis of the static method of the growth of cadmium sulphide crystals with large temperature gradients

The paper gives an analysis of the thermodynamical conditions of crystallization of cadmium sulphide from the gaseous phase with the use of large temperature gradients in the course of crystal growth. From the achieved results there follows that large temperature gradients with the static method of crystal growth favourably influences the formation of crystallization nuclei and the growth of single crystals. The crystals cultivated under such conditions are comparatively large, their volume being several cm³ and their weight ranging from 40–60 g. These crystals are suitable for photoelectrical and electroacoustical measurements and various technical applications.     

Peculiarities of the melt growth of metal single crystals with specified crystal-geometric and structural parameters

This paper describes the authors' modifications of Kapitza and Bridgman apparatus and growth methods of metal single crystals with specified crystal geometric and structural parameters. The effects associated with defect formation are discussed. The features of the effects in their relation to the crystal lattice types and crystallographic orientation are indicated. It is concluded that one of the main factors responsible for the defect formation during single crystal growth in the mould is strain. This is due to thermomechanical stresses arising during the crystal growth and cooling to room temperature, from the difference in thermal expansion coefficients of the crystal and mould materials.     

Synthesis and characterization of ZSM-8-type zeolite crystals

Procedure for hydrothermal synthesis of ZSM-8-type zeolite crystals, using TEA—OH as a template, in the system having molar composition 16.2 (Na₂O) — Al₂O₃ — 117 (SiO₂) — 4.8 (TEA)₂O — 3887 H₂O at 170 °C is described. Results of characterization of these crystals by XRD, IR, EDAX, SEM, TGA, and adsorption studies are described and discussed. X-ray diffraction studies establish that the crystals are ZSM-8-type with structure similar to that of ZSM-5-type crystals. Crystals have prismatic bipyramidal morphology with average size 18–25 microns. Degased calcined samples adsorb xylenes in the order p > m > 0. Pore length per unit cell, estimated from n-hexane adsorption studies, is 46 Å.     

Optical parameters of paratellurite crystals

Refractive indices and transmittances of paratellurite single crystals have been measured. The specific optical rotation is determined and the Verdet constants are calculated for a radiation wavelength of 355 nm.     

Investigations on nucleation,thermodynamical parameters and growth of Benzimidazole crystals from low temperature solution

Metastable zonewidth and induction period measurements of Benzimidazole (BMZ) are presented. The nucleation parameters such as interfacial tension, radius of the critical nucleus and critical free energy change have been calculated for the solution grown Benzimidazole (BMZ) single crystals at different supersaturation ratios. The grown BMZ crystals were characterized by the differential scanning calorimetric studies for analysis of thermal properties. The dielectric behaviour of the crystal was studied at different temperature and frequency. The laser damage threshold studies show that BMZ crystal has higher laser damage threshold. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Modeling of the shape of polyethylene oxide single crystals and determination of the kinetic crystallization parameters: Theoretical and experimental approaches

The curvature of faces of polymer single crystals is described by the system of Mansfield equations, which is based on the Frank-Seto growth model. This model assumes the velocity of nucleus steps to be the same for their propagation to the right and left and is valid only for symmetric crystallographic planes. To describe the shape of polyethylene oxide single crystals grown from melt and limited by the {100} and {120} folding planes, it is assumed that the layer velocities to the right and left are different on {120} faces. This approach allows modeling, with a high accuracy, of the observed shapes of polymer single crystals grown at different temperatures, which makes it possible to determine unambiguously the fundamental crystallization parameters: the dimensionless ratio of the secondary homogeneous nucleation rate to the average velocities of nuclei along the crystallization planes and the ratio of nucleus velocities to the right and left. In addition, it was found that a known macroscopic single-crystal growth rate can be used to determine the absolute values of the secondary homogeneous nucleation rate and the velocities of nuclei along the growth plane.