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Rosenberger, Franz

Publications and source records attributed to Rosenberger, Franz.

At least 55 records · Page 3

Vapor crystal growth technology development: Application to cadmium telluride

Growth of bulk crystals by physical vapor transport was developed and applied to cadmium telluride. The technology makes use of effusive ampoules, in which part of the vapor contents escapes to a vacuum shroud through defined leaks during the growth process. This approach has the advantage over traditional sealed ampoule techniques that impurity vapors and excess vapor constituents are continuously removed from the vicinity of the growing crystal. Thus, growth rates are obtained routinely at magnitudes that are rather difficult to achieve in closed ampoules. Other advantages of this effusive ampoule physical vapor transport (EAPVT) technique include the predetermination of transport rates based on simple fluid dynamics and engineering considerations, and the growth of the crystal from close to congruent vapors, which largely alleviates the compositional nonuniformities resulting from buoyancy driven convective transport. After concisely reviewing earlier work on improving transport rates, nucleation control, and minimization of crystal wall interactions in vapor crystal growth, a detail account is given of the largely computer controlled EAPVT experimentation.

Rosenberger, Franz↗

CBr4 vapor growth morphologies near the polymorphic transition point. I - Single crystals. II - Crystals with large-angle grain boundaries

High-resolution microscopy and image processing were used to investigate morphological changes in CBr4 single crystals during growth from the vapor at various levels of supersaturation and at temperatures below the compound's polymorphic phase transition. It was found that, as the temperature increased at fixed supersaturations, the corners of the crystals became rounded as a result of thermal roughening; the rounding temperatures were different for crystallographically different corners. A study of CBr4 crystals with large-angle grain boundaries or twin boundaries (extended macrodefects), conducted at the temperature of polymorphic phase transition showed that the phase transition temperature, T(tr) and crystal surface morphology of these crystals depended on the presence or absence of extended macrodefects. Unlike the case of a perfect single crystal, where the T(tr) was about 46.75 C, the phase transition in crystals with extended macrodefects occurred significantly below 46.75.

Xiao, Rong-Fu↗

Growth morphologies of crystal surfaces

A previously proposed Monte Carlo model (Xiao et al., 1988, 1990) is extended to three dimensions, and reevaporation after accommodation and growth on dislocation-induced steps are included. It is found again that, for a given set of growth parameters, the critical size beyond which a crystal cannot retain its macroscopically faceted shape scales linearly with the mean free path in the vapor. However, the three-dimensional systems show increased shape stability as compared with the corresponding two-dimensional cases. The experimental observation that the critical size of a growing crystal depends on the prevailing growth mechanism is confirmed, and detailed insight into the processes leading to the loss of face and facet stability is obtained.

Xiao, Rong-Fu↗

Fluid dynamics and low gravity effects of chemical vapor deposition

Based on the comparison between experimental data and numerical results for the growth of GaAs from TMGa, it was shown that 3D simulations are necessary to simulate rectangular CVD reactors even when operated under subcritical (Ra) conditions. The important points found are summarized in the three attached reprints. The experimental studies of mixed convection in horizontal channels have shown three regimes of high Ra (22,220) number flows. At Re = 18.5, the rolls develop very quickly, significantly modulating the axial velocity even before it reaches the beginning of the hot plate. A few centimeters downstream, the velocities become asymmetric about the vertical centerplane and at x = 12 cm, become unsteady. These asymmetries were predicted theoretically, but experimental evidence has not been published prior to this work. At Re = 36, the axial velocity is only slightly modified at x = 0. Although the flow remains steady and symmetric about the vertical centerplane, there is a small spatial oscillation in the velocities over the length of the channel. The period of this oscillation was around 5 cm. At Re = 54, the longitudinal rolls developed smoothly over a length of 30 cm, with no asymmetries, unsteadiness, or spatial oscillations. Comparison of numerical simulations of these flows to experiments has revealed the importance and difficulty of setting proper thermal boundary conditions on the sidewalls. Calculated flows and experimentally measured flows showed very similar profiles, but at different axial locations, with the rolls developing more rapidly in the experiments. This is directly attributable to partially conducting sidewalls of the apparatus being hotter in the entrance section than the adiabatic walls of the simulations. A thorough comparison of the experimental data and numerical results for a variety of sidewall boundary conditions is in preparation.

Nyce, Thomas A.↗

Process modelling for Space Station experiments

Examined here is the sensitivity of a variety of space experiments to residual accelerations. In all the cases discussed the sensitivity is related to the dynamic response of a fluid. In some cases the sensitivity can be defined by the magnitude of the response of the velocity field. This response may involve motion of the fluid associated with internal density gradients, or the motion of a free liquid surface. For fluids with internal density gradients, the type of acceleration to which the experiment is sensitive will depend on whether buoyancy driven convection must be small in comparison to other types of fluid motion, or fluid motion must be suppressed or eliminated. In the latter case, the experiments are sensitive to steady and low frequency accelerations. For experiments such as the directional solidification of melts with two or more components, determination of the velocity response alone is insufficient to assess the sensitivity. The effect of the velocity on the composition and temperature field must be considered, particularly in the vicinity of the melt-crystal interface. As far as the response to transient disturbances is concerned, the sensitivity is determined by both the magnitude and frequency of the acceleration and the characteristic momentum and solute diffusion times. The microgravity environment, a numerical analysis of low gravity tolerance of the Bridgman-Stockbarger technique, and modeling crystal growth by physical vapor transport in closed ampoules are discussed.

Alexander, J. Iwan D.↗

Definition study for temperature control in advanced protein crystal growth

Some of the technical requirements for an expedient application of temperature control to advanced protein crystal growth activities are defined. Lysozome was used to study the effects of temperature ramping and temperature gradients for nucleation/dissolution and consecutive growth of sizable crystals and, to determine a prototype temperature program. The solubility study was conducted using equine serum albumin (ESA) which is an extremely stable, clinically important protein due to its capability to bind and transport many different small ions and molecules.

Nyce, Thomas A.↗

Nucleation and growth control in protein crystallization

The five topics summarized in this final report are as follows: (1) a technique for the expedient, semi-automated determination of protein solubilities as a function of temperature and application of this technique to proteins other than lysozyme; (2) a small solution cell with adjustable temperature gradients for the growth of proteins at a predetermined location through temperature programming; (3) a microscopy system with image storage and processing capability for high resolution optical studies of temperature controlled protein growth and etching kinetics; (4) growth experiments with lysozyme in thermosyphon flow ; and (5) a mathematical model for the evolution of evaporation/diffusion induced concentration gradients in the hanging drop protein crystallization technique.

Rosenberger, Franz↗

Modelling crystal growth: Convection in an asymmetrically heated ampoule

The objective was to develop and implement a numerical method capable of solving the nonlinear partial differential equations governing heat, mass, and momentum transfer in a 3-D cylindrical geometry in order to examine the character of convection in an asymmetrically heated cylindrical ampoule. The details of the numerical method, including verification tests involving comparison with results obtained from other methods, are presented. The results of the study of 3-D convection in an asymmetrically heated cylinder are described.

Alexander, J. Iwan D.↗

Morphological stability and kinetics in crystal growth from vapors

The following topics are discussed: (1) microscopy image storage and processing system; (2) growth kinetics and morphology study with carbon tetrabromide; (3) photothermal deflection vapor growth setup; (4) bridgman growth of iodine single crystals; (5) vapor concentration distribution measurement during growth; and (6) Monte Carlo modeling of anisotropic growth kinetics and morphology. A collection of presentations and publications of these results are presented.

Rosenberger, Franz↗

Modelling the solution growth of TGS crystals in low gravity

The experimental growth of triglycine sulfate (TGS) crystals from aqueous solution is modeled here in two dimensions using the PHOENICS finite volume code. Simulations are carried out for steady, impulsive, and periodic accelerations in order to determine tolerable acceleration levels. Scaling arguments are used to estimate the times required for thermal and solutal variations from the initial equilibrium state to be diffusively transported throughout the system, and to obtain order of magnitude information on the relative magnitudes of diffusive and convective transport. The computed concentration fields reflect the features of the concentration distributions found experimentally during experiments conducted aboard Spacelab 3 in 1985.

Nadarajah, Arunan↗

Growth morphology with anisotropic surface kinetics

The morphological evolution of crystals growing from an incongruent vapor phase is studied using a Monte Carlo model, and the full range of growth morphologies is recovered. The diffusion in the bulk nutrient and the anisotropy in the interface kinetics are morphologically destabilizing and stabilizing, respectively. For a given set of simulation parameters and lattice symmetries there is a critical size, which scales linearly with the mean free path in the vapor, beyond which a crystal cannot retain its stable, macroscopically faceted growth shape. Surface diffusion stabilizes faceted growth on the shorter scale of the mean surface diffusion length. In simulations with a uniform drift superimposed on the random walk nutrient transport, crystal faces oriented toward the drift show enhanced morphological stability compared to the purely diffusive situation. Rotational drifts with periodic reversal of direction are morphologically stabilizing for all crystal facets.

Xiao, Rong-Fu↗

Three-dimensional modelling of horizontal chemical vapor deposition. I - MOCVD at atmospheric pressure

A systematic numerical study of the MOCVD of GaAs from trimethylgallium and arsine in hydrogen or nitrogen carrier gas at atmospheric pressure is reported. Three-dimensional effects are explored for CVD reactors with large and small cross-sectional aspect ratios, and the effects on growth rate uniformity of tilting the susceptor are investigated for various input flow rates. It is found that, for light carrier gases, thermal diffusion must be included in the model. Buoyancy-driven three-dimensional flow effects can greatly influence the growth rate distribution through the reactor. The importance of the proper design of the lateral thermal boundary conditions for obtaining layers of uniform thickness is emphasized.

Ouazzani, Jalil↗

Three-dimensional numerical modelling of transport in horizontal MOCVD reactors

A systematic three-dimensional study for the MOCVD of gallium arsenide is presented. Numerical solutions, obtained for the system of equations governing the steady state heat, momentum, and mass transfer in horizontal reactors with large and small aspect ratio, are compared with experimental growth rate distributions. The effects on layer thickness uniformity of lateral thermal boundary conditions and susceptor tilt are explored. The validity of a parabolic flow approximation of the equations is also investigated by comparison with the complete three-dimensional treatment.

Ouazzani, Jalil↗

Bridgman crystal growth in low gravity - A scaling analysis

The results of an order-of-magnitude or scaling analysis are compared with those of numerical simulations of the effects of steady low gravity on compositional nonuniformity in crystals grown by the Bridgman-Stockbarger technique. In particular, the results are examined of numerical simulations of the effect of steady residual acceleration on the transport of solute in a gallium-doped germanium melt during directional solidification under low-gravity conditions. The results are interpreted in terms of the relevant dimensionless groups associated with the process, and scaling techniques are evaluated by comparing their predictions with the numerical results. It is demonstrated that, when convective transport is comparable with diffusive transport, some specific knowledge of the behavior of the system is required before scaling arguments can be used to make reasonable predictions.

Alexander, J. I. D.↗

Analysis of the low gravity tolerance of Bridgman-Stockbarger crystal growth. I - Steady and impulse accelerations

The effects of steady and impulse-type residual accelerations on dopant distributions during directional solidification in 2D and 3D 'generic' models of the Bridgman-Stockbarger technique are investigated using numerical methods. The calculations are based on the thermophysical properties of molten germanium doped with a low concentration of gallium. A Chebyshev collocation pseudospectral method is used for the solution of the governing momentum-, mass-, species-, and heat-transfer equations. Only convection caused by temperature gradients is considered. It is found that lateral nonuniformity in composition is very sensitive to the orientation of the steady component of the residual gravity vector and to the particular operating conditions under consideration. It is also found that laterally or radially averaged composition profiles are alone insufficient to describe the extent of residual convection in a spacecraft environment. The effects of impulse-type disturbances can be severe and can extend for times on the order of 1000 sec after the termination of the impulse.

Alexander, J. Iwan D.↗

Novel protein crystal growth technology: Proof of concept

A technology for crystal growth, which overcomes certain shortcomings of other techniques, is developed and its applicability to proteins is examined. There were several unknowns to be determined: the design of the apparatus for suspension of crystals of varying (growing) diameter, control of the temperature and supersaturation, the methods for seeding and/or controlling nucleation, the effect on protein solutions of the temperature oscillations arising from the circulation, and the effect of the fluid shear on the suspended crystals. Extensive effort was put forth to grow lysozyme crystals. Under conditions favorable to the growth of tetragonal lysozyme, spontaneous nucleation could be produced but the number of nuclei could not be controlled. Seed transfer techniques were developed and implemented. When conditions for the orthorhombic form were tried, a single crystal 1.5 x 0.5 x 0.2 mm was grown (after in situ nucleation) and successfully extracted. A mathematical model was developed to predict the flow velocity as a function of the geometry and the operating temperatures. The model can also be used to scaleup the apparatus for growing larger crystals of other materials such as water soluble non-linear optical materials. This crystal suspension technology also shows promise for high quality solution growth of optical materials such as TGS and KDP.

Nyce, Thomas A.↗

Analysis of models for two solution crystal growth problems

Two diffusive solution crystal growth models are considered which are characterized by two phases separated by an interface, a lack of convective mixing in either phase, and the presence of diffusion components differing widely in diffusivity. The first model describes precipitant-driven solution crystal growth and the second model describes a hanging drop evaporation problem. It is shown that for certain proteins sharp concentration gradients may develop in the drop during evaporation, while under the same conditions the concentrations of other proteins remain uniform.

Fehribach, Joseph D.↗

Viscosity measurements at high temperature and high pressure: A novel technique

The extensive numerical modelling of transport phenomena was performed for the melt growth of mercury cadmium telluride. To increase the fidelity of modelling the kinematic viscosity of liquid Hg(1-x)Cd(x)Te was determined at various compositions in the range of x between 0 and 0.2 and at temperatures around and below the respective melting point. The phase diagram of Hg(1-x)Cd(x)Te shows that for this range the melting point varies from 670 C for pure HgTe to 790 C at x=0.2. The vapor pressure above the melt varies correspondingly from 15 to about 40 atm. Hence, the measurement of viscosities in this system requires a technique that allows for combinations of high temperatures and pressures. In addition, a closed isothermal system is required. The high pressure melt container must also be inert to molten Hg(1-x)Cd(x)Te to avoid possible errors from contamination of the liquid. A novel technique that largely circumvents the above experimental problems is described. Its theory is also presented.

Jin, Wei-Qing↗