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At least 415 records · Page 23

Improved opportunities for the investigation of crystal growth phenomena on Space Station Freedom

Space Station Freedom is intended to provide long-duration access to a microgravity environment crewed by a team of well-trained astronaut scientists. To illustrate the benefits afforded by such a facility, a general review of crystal growth (CG) from liquids is given, concentrating on the basic elements of the underlying physics and chemistry. Two examples of CG techniques illustrating the effect of mass transport limitations on growth rate and thus experiment duration are presented. Thermodynamic and thermophysical properties and suggested thermal boundary and growth conditions are used to estimate the experiment duration of two mass-transport-limited CG scenarios. A hypothetical study that probes a large processing space via a number of short-duration experiments is described.

Wargo, M. J.↗

Concentration Dependence of Solution Shear Viscosity and Solute Mass Diffusivity in Crystal Growth from Solutions

The physical properties of a supersaturated binary solution such as its density rho, shear viscosity eta, and solute mass diffusivity D are dependent on the solute concentration c: rho = rho(c), eta = eta(c), and D = D(c). The diffusion boundary layer equations related to crystal growth from solution are derived for the case of natural convection with a solution density, a shear viscosity, and a solute diffusivity that are all depen- dent on solute concentration. The solution of these equations has demonstrated the following. (1) At the vicinity of the saturation concentration c(sub s) the solution shear viscosity eta depends on rho as eta(sub s) = eta(rho(sub s))varies as square root of rho(c(sub s)). This theoretically derived result has been verified in experiments with several aqueous solutions of inorganic and organic salts. (2) The maximum solute mass transfer towards the growing crystal surface can be achieved for values of c where the ratio of d ln(D(c)/dc) to d ln(eta(c)/dc) is a maximum.

Izmailov, Alexander F.↗

Simulation of triglycine sulfate crystal growth in space

Consideration is given to the numerical simulation of the solution growth of triglycine sulfate in space, with heat transfer, mass transfer, buoyancy-driven convection, the dependence of solubility on temperature, and finite interface kinetics taken into account. In the bulk solution, weak thermal convection was established quickly. The thermal convection then becomes dominated by solutionally driven motion. The convection due to the steady background g is predicted to influence both the growth rate and the crystal morphology. The time required for buoyancy-driven convection to influence the growth rate depends on the magnitude of g, i.e., more time for smaller g. Under the same cooling condition, the average growth rate increases as the magnitude of g increases. A steady average growth rate of 1.0 mm/d can be obtained when a properly designed cooling rate is applied to the sting. The most uniform growth is obtained when the g vector is aligned such that the solution flows normal towards the center of the crystal surface.

Sun, Jianhua↗

Crystal growth of ZnSe and related ternary compound semiconductors by physical vapor transport

The materials to be investigated are ZnSe and related ternary semiconducting alloys (e.g., ZnS(x)Se(1-x), ZnTe(x)Se(1-x), and Zn(1-x)Cd(x)Se). These materials are useful for opto-electronic applications such as high efficient light emitting diodes and low power threshold and high temperature lasers in the blue-green region of the visible spectrum. The recent demonstration of its optical bistable properties also makes ZnSe a possible candidate material for digital optical computers. The investigation consists of an extensive ground-based study followed by flight experimentation, and involves both experimental and theoretical work. The objectives of the ground-based work are to establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low gravity environment and to obtain the experimental data and perform the analyses required to define the optimum parameters for the flight experiments. During the six months of the Preliminary Definition Phase, the research efforts were concentrated on the binary compound ZnSe - the purification of starting materials of Se by zone refining, the synthesis of ZnSe starting materials, the heat treatments of the starting materials, the vapor transport rate measurements, the vapor partial pressure measurements of ZnSe, the crystal growth of ZnSe by physical vapor transport, and various characterization on the grown ZnSe crystals.

Su, Ching-Hua↗

A preliminary study of numerical simulation of thermosolutal convection of interest to crystal growth

Calculations were performed with computer models using three types of finite difference methods of thermosolutal convection: horizontal heating of a container filled with a stably stratified solution, finger convection in a container, and finger convection in a horizontally infinite channel. The importance of including thermosolutal convection in models of crystal growth is emphasized, and the difficulties in doing so are demonstrated. It is pointed out that these difficulties, due primarily to the fine structure of the convection, may be partly overcome by the use of fine grids and implicit time stepping methods.

Miller, T. L.↗

Lack of Evidence for Prenucleation Aggregate Formation in Lysozyme Crystal Growth Solutions

There have been numerous claims of large concentrations of prenucleation aggregates in supersaturated as well as undersaturated lysozyme solutions at high salt concentrations. The presence of these aggregates was derived from measurements of the light or neutron scattering intensity, ultracentrifugation and dialysis behavior, as well as over-simplified crystal growth kinetics considerations. In all these interpretations it has been assumed that lysozyme solutions are either ideal or that protein interactions are independent of salt concentration. Contrary to these presumptions, our static and dynamic light scattering experiments provide evidence that lysozyme forms highly non-ideal, strongly interacting solutions. At low salt concentrations, the scattering intensities fall well below the values expected for an ideal, monomeric solution at the same protein concentration, while diffusivities increase with increasing protein concentration. Upon increase in salt concentration, these trends are eventually reversed. This enhancement in scattering intensity and decrease in diffusivity was widely interpreted as sign of aggregate formation. Yet, a quantitative interpretation of the scattering behavior over the whole salt concentration range can only be given in terms of a transition from net repulsion to net attraction between lysozyme monomers. Increased salt screening of the electrostatic repulsion among the protein macro-ions, together with attractive protein interactions, such as van der Waals, hydrophobic and hydration forces, provide an unambiguous mechanism for the observed transition and a more physical interpretation of the various observations.

Muschol, Martin↗

Crystal growth and magnetic structure of ternary silicide Eu Pd 3 Si 2

The hexagonal CaCu 5 –type structure (P6/mmm) is the prototype for more than 100 ternary borides, gallides, and silicides, with general stoichiometry of RTM 3 X 2 (R=lanthanide/alkaline earth; TM=transition metal; X=B, Ga, Si, Ge). Here we report the synthesis, crystal structure, and bulk magnetic properties of polycrystalline and single crystal samples of EuPd 3 Si 2 and its nonmagnetic analog SrPd 3 Si 2 . Both compounds crystallize in the orthorhombic space group symmetry Imma (no. 74, Z = 2, oI12) displaying pseudohexagonal symmetry. Ferromagnetic (FM) order of Eu 2+ at T C1 =78K and a spin-reorientation transition at T C2 =5K appear as distinctive features in bulk magnetization, specific heat, and resistivity/resistance measurements. Neutron powder diffraction measurements on EuPd 3 Si 2 confirm FM order of the Eu 2+ spins below T C1 , with the spins aligned along the a axis below T C2 . Electronic band structure calculations corroborate the crystal structure and the FM state for EuPd 3 Si 2 , with a Pd d–band polarization in the same direction as the Eu 4f polarization, enhancing the observed spin moment.

36 MATERIALS SCIENCE↗

Floating zone crystal growth, structure, and properties of a cubic Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 garnet-type lithium-ion conductor

As a promising candidate for solid-state electrolytes in Li-ion batteries, the garnet-type Li-ion conductor series Li 5+x La 3 Nb 2-x Zr x O 12 (LLNZO) (0 ≤ x ≤ 2) exhibits high ionic conductivity at room temperature. However, no previous single-crystal growth or characterization has been reported for LLNZO compositions 0 ≤ x ≤ 1. To obtain a complete understanding of the trend in the structure–property relationship in this class of materials, we used the floating zone (FZ) method to grow a single crystal of Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 that was 4 mm in diameter and 10 mm in length. Using Laue neutron single-crystal diffraction, two distinct Li sites were observed: tetrahedral 24d and octahedral 96h sites. The maximum entropy method (MEM) based on neutron single-crystal diffraction data was used to map Li nuclear density and estimate that the bottleneck of Li transport exists between neighboring tetrahedral and octahedral sites, and that Li is delocalized between split octahedral sites. Room-temperature Li-ion conductivity in Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 measured with electrochemical impedance spectroscopy (EIS) was 1.37 × 10 -4 S cm -1 . The Li migration activation energy was estimated to be 0.50 eV from EIS and 0.47 eV from dielectric relaxation measurements. The Li-ion jump attempt rate was estimated to be 1.47 × 10 12 Hz while the time scale of successful migration is 10 -7 to 10 -6 s.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigation of Vibrational Control of the Bridgman Crystal Growth Technique

The objectives are: Conduct a parametric theoretical and numerical investigation of vibro-convective buoyancy-driven flow in differentially heated cylindrical containers. Investigate buoyant vibro-convective transport regimes in Bridgman-type systems with a focus on the use of vibration to suppress, or control, convection in order to achieve transport control during crystal growth. Assess the feasibility of vibro-convective control as a means of offsetting "g-jitter" effects under microgravity conditions, Exchange information with the experimental group at the General Physics Institute (GPI) of the Russian Academy of Science who are undertaking a complementary experimental program.

Fedoseyev, Alexandre I.↗

Non-linear resonance of fluids in a crystal growth cavity

In the microgravity environment, the effect of gravity on fluid motion is much reduced. Hence, secondary effects such as vibrations, jitters, surface tension, capillary effects, and electromagnetic forces become the dominant mechanism of fluid convection. Numerous studies have been conducted to investigate fluid behavior in microgravity with the ultimate goal of developing processes with minimal influence from convection. Industrial applications such as crystal growth from solidification of melt and protein growth for pharmatheutical application are just a few examples of the vast potential benefit that can be reaped from material processing in space. However, a space laboratory is not immune from all undesirable disturbances and it is imperative that such disturbances be well understood, quantifiable, and controlled. Non-uniform and transient accelerations such as vibrations, jitters, and impulsive accelerations exist as a result of crew activities, space vehicle maneuvering, and the operations of on-board equipment. Measurements conducted on-board a U.S. Spacelab showed the existence of vibrations in the frequency range of 1 to 100 Hz with a dominant mode of 17 Hz and harmonics of 54 Hz. The observed vibration is not limited to any coordinate plane but exists in all directions. Similar situation exists on-board the Russian MIR space station. Due to the large structure of its design, the future International Space Station will have its own characteristic vibration spectrum. It is well known that vibration can exert substantial influence on heat and mass transfer processes, thus hindering any attempts to achieve a diffusion-limited process. Experiments on vibration convection for a liquid-filled enclosure under one-g environment showed the existence of different flow regimes as vibration frequency and intensity changes. Results showed the existence of a resonant frequency, near which the enhancement is the strongest, and the existence of a high frequency asymptote. Numerical simulations of vibration convection have been conducted by Yurkov, Fu and Shieh, and by Wang. These analyses considered a two-dimensional air-filled cell under weightlessness condition and showed results similar to those of the experiments. It is not yet known whether resonance convection can be triggered by jitter alone or whether it requires the interaction of jitter with other convective forces in low gravity. An order of magnitude analysis, however, can be used to show the dependence of the resonance frequency on the fluid Prandtl number. Even though the onset of resonance convection may depend on other factors, results indicates that fluids with low Prandtl numbers are more susceptible to resonance than those with high Prandtl numbers. The current study is aimed at gaining additional insights to this problem using germanium as working fluid. Germanium was chosen for this analysis because of its common usage in solidification process and its relatively low Prandtl number (Pr = 0.02).

Wang, Francis C.↗

Unsteady Crystal Growth Due to Step-Bunch Cascading

Based on our experimental findings of growth rate fluctuations during the crystallization of the protein lysozym, we have developed a numerical model that combines diffusion in the bulk of a solution with diffusive transport to microscopic growth steps that propagate on a finite crystal facet. Nonlinearities in layer growth kinetics arising from step interaction by bulk and surface diffusion, and from step generation by surface nucleation, are taken into account. On evaluation of the model with properties characteristic for the solute transport, and the generation and propagation of steps in the lysozyme system, growth rate fluctuations of the same magnitude and characteristic time, as in the experiments, are obtained. The fluctuation time scale is large compared to that of step generation. Variations of the governing parameters of the model reveal that both the nonlinearity in step kinetics and mixed transport-kinetics control of the crystallization process are necessary conditions for the fluctuations. On a microscopic scale, the fluctuations are associated with a morphological instability of the vicinal face, in which a step bunch triggers a cascade of new step bunches through the microscopic interfacial supersaturation distribution.

Vekilov, Peter G.↗

Follow up on the crystal growth experiments of the LDEF

The results of the 4 solution growth experiments on the LDEF have been published elsewhere. Both the crystals of CaCO3, which were large and well shaped, and the much smaller TTF-TCNQ crystals showed unusual morphological behavior. The follow up on these experiments was begun in 1981, when ESA initiated a 'Concept Definition Study' on a large, 150 kg, Solution Growth Facility (SGF) to be included in the payload of EURECA-1, the European Retrievable Carrier. This carrier was a continuation of the European Spacelab and at that time planned for launch in 1987. The long delay of the LDEF retrieval and of subsequent missions brought about reflections both on the concept of crystal growth in space and on the choice of crystallization materials that had been made for the LDEF. Already before the LDEF retrieval, research on TTF-TCNQ had been stopped, and a planned growth experiment with TTF-TCNQ on the SGF/EURECA had been cancelled. The target of the SGF investigation is now more fundamental in nature. None of the crystals to be grown here are, like TTF-TCNQ, in particular demand by science or industry, and the crystals only serve the purpose of model crystals. The real purpose of the investigation is to study the growth behavior. One of the experiments, the Soret Coefficient Measurement experiment is not growing crystals at all, but has it as its sole purpose to obtain accurate information on thermal diffusion, a process of importance in crystal growth from solution.

Nielsen, K. F.↗

Tetragonal Lysozyme Nucleation and Crystal Growth: The Role of the Solution Phase

Lysozyme, and most particularly the tetragonal form of the protein, has become the default standard protein for use in macromolecule crystal nucleation and growth studies. There is a substantial body of experimental evidence, from this and other laboratories, that strongly suggests this proteins crystal nucleation and growth is by addition of associated species that are preformed by standard reversible concentration-driven self association processes in the bulk solution. The evidence includes high resolution AFM studies of the surface packing and of growth unit size at incorporation, fluorescence resonance energy transfer measurements of intermolecular distances in dilute solution, dialysis kinetics, and modeling of the growth rate data. We have developed a selfassociation model for the proteins crystal nucleation and growth. The model accounts for the obtained crystal symmetry, explains the observed surface structures, and shows the importance of the symmetry obtained by self-association in solution to the process as a whole. Further, it indicates that nucleation and crystal growth are not distinct mechanistically, but identical, with the primary difference being the probability that the particle will continue to grow or dissolve. This model also offers a possible mechanism for fluid flow effects on the growth process and how microgravity may affect it. While a single lysozyme molecule is relatively small (M.W. = 14,400), a structured octamer in the 4(sub 3) helix configuration (the proposed average sized growth unit) would have a M.W. = 115,000 and dimensions of 5.6 x 5.6 x 7.6 nm. Direct AFM measurements of growth unit incorporation indicate that units as wide as 11.2 nm and as long as 11.4 nm commonly attach to the crystal. These measurements were made at approximately saturation conditions, and they reflect the sizes of species that both added or desorbed from the crystal surface. The larger and less isotropic the associated species the more likely that it will be oriented to some degree in a flowing boundary layer, even at the low flow velocities measured about macromolecule crystals. Flow-driven effects resulting in misorientation upon addition to and incorporation into the crystal need only be a small fraction of a percentage to significantly affect the resulting crystal. One Earth, concentration gradient driven flow will maintain a high interfacial concentration, i.e., a high level (essentially that of the bulk solution) of solute association at the interface and higher growth rate. Higher growth rates mean an increased probability that misaligned growth units are trapped by subsequent growth layers before they can be desorbed and try again, or that the desorbing species will be smaller than the adsorbing species. In microgravity the extended diffusive boundary layer will lower the interfacial concentration. This results in a net dissociation of aggregated species that diffuse in from the bulk solution, i.e., smaller associated species, which are more likely able to make multiple attempts to correctly bind, yielding higher quality crystals.

Pusey, Marc L.↗

A Mechanistic Understanding of Nonclassical Crystal Growth in Hydrothermally Synthesized Sodium Yttrium Fluoride Nanowires

Sodium yttrium fluoride (NaYF 4 ) is an important upconverting material with many potential uses in chemistry, materials science, and biology, which can be synthesized hydrothermally in both cubic (α) and hexagonal (β) crystallographic polymorphs. Understanding the mechanisms underlying the phase conversion between the cubic and hexagonal polymorphs is of great interest to help inform future synthetic efforts, for example in the design of atomically precise quantum materials with well-defined sizes and morphologies. In this work, we use a combination of analytical transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), powder X-ray diffraction (XRD), in situ liquid cell TEM, atom probe tomography (APT), and extended X-ray absorption fine structure (EXAFS) measurements to show that the hexagonal NaYF 4 nanowires form through a nonclassical crystal growth mechanism involving the formation and subsequent oriented attachment of mesocrystals consisting of cubic (α) phase units. Additionally, EXAFS measurements suggest that substitutional Yb 3+ point defects within NaYF 4 are distributed evenly throughout the crystal lattice without clustering and also that they may exhibit selective substitution into one of the two possible trivalent yttrium sites in the unit cell for hydrothermally synthesized β-NaYF 4 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Optimized in situ crystal growth and disordered quasi-one-dimensional magnetism in Li 2 Mn 2 ( MoO 4 ) 3

We present that the quasi-one-dimensional structure of Li 2 Mn 2 ( MoO 4 ) 3 consists of three mutually distinct chains of Li 1 - x Mn x -centered polyhedra in which Mn ostensibly adopts a J = 5 / 2 Mn 2 + configuration. In situ x-ray scattering experiments carried out as crystallites emerge from a molten oxide solution facilitate the synthesis of large single crystals. Ex situ x-ray diffraction finds no evidence of long-range Li/Mn occupancy ordering, suggesting that the structure is effectively composed of finite chains of Mn moments of statistically varying lengths. UV/visible diffuse reflectance spectroscopy measurements establish a wide 3.43(12)-eV direct charge gap consistent with the local polyhedral coordination of the nominally Mn 2 + species. The temperature T dependence of the DC magnetic susceptibility χ reveals a fluctuating moment of only 2.74 μ B ± 0.01 μ B /Mn, dramatically reduced from the 5.9 μ B /Mn expected for Mn 2 + . Meanwhile, the Weiss temperature Θ W = - 89 ± 1 K reveals antiferromagnetic fluctuations that are stymied from reaching an ordered state apparently by the chemical disorder intrinsic to the polyhedral chains. Measurements of magnetization vs field H at T ≤ 10 K are far from saturation even at H = 5 T and are strongly non-Brillouin-like, instead scaling as H / T 0.24 ( 3 ) and suggesting the presence of quantum fluctuations associated with an eventual quasi-one-dimensional, disordered magnetic phase.

1-dimensional systems↗

Real time quantitative imaging for semiconductor crystal growth, control and characterization

A quantitative real time image processing system has been developed which can be software-reconfigured for semiconductor processing and characterization tasks. In thermal imager mode, 2D temperature distributions of semiconductor melt surfaces (900-1600 C) can be obtained with temperature and spatial resolutions better than 0.5 C and 0.5 mm, respectively, as demonstrated by analysis of melt surface thermal distributions. Temporal and spatial image processing techniques and multitasking computational capabilities convert such thermal imaging into a multimode sensor for crystal growth control. A second configuration of the image processing engine in conjunction with bright and dark field transmission optics is used to nonintrusively determine the microdistribution of free charge carriers and submicron sized crystalline defects in semiconductors. The IR absorption characteristics of wafers are determined with 10-micron spatial resolution and, after calibration, are converted into charge carrier density.

Wargo, Michael J.↗

Models of Mass Transport During Microgravity Crystal Growth of Alloyed Semiconductors in a Magnetic Field

Alloyed semiconductor crystals, such as germanium-silicon (GeSi) and various II-VI alloyed crystals, are extremely important for optoelectronic devices. Currently, high-quality crystals of GeSi and of II-VI alloys can be grown by epitaxial processes, but the time required to grow a certain amount of single crystal is roughly 1,000 times longer than the time required for Bridgman growth from a melt. Recent rapid advances in optoelectronics have led to a great demand for more and larger crystals with fewer dislocations and other microdefects and with more uniform and controllable compositions. Currently, alloyed crystals grown by bulk methods have unacceptable levels of segregation in the composition of the crystal. Alloyed crystals are being grown by the Bridgman process in space in order to develop successful bulk-growth methods, with the hope that the technology will be equally successful on earth. Unfortunately some crystals grown in space still have unacceptable segregation, for example, due to residual accelerations. The application of a weak magnetic field during crystal growth in space may eliminate the undesirable segregation. Understanding and improving the bulk growth of alloyed semiconductors in microgravity is critically important. The purpose of this grant to to develop models of the unsteady species transport during the bulk growth of alloyed semiconductor crystals in the presence of a magnetic field in microgravity. The research supports experiments being conducted in the High Magnetic Field Solidification Facility at Marshall Space Flight Center (MSFC) and future experiments on the International Space Station.

Ma, Nancy↗

Influence of non steady gravity on natural convection during micro-gravity solidification of semiconductors. I - Time scale analysis. II - Implications for crystal growth experiments

Consideration is given to the influence of temporal variations in the magnitude of gravity on natural convection during unidirectional solidification of semiconductors. It is shown that the response time to step changes in g at low Rayleigh numbers is controlled by the momentum diffusive time scale. At higher Rayleigh numbers, the response time to increases in g is reduced because of inertial effects. The degree of perturbation of flow fields by transients in the gravitational acceleration on the Space Shuttle and the Space Station is determined. The analysis is used to derive the requirements for crystal growth experiments conducted on low duration low-g vehicles. Also, the effectiveness of sounding rockets and KC-135 aircraft for microgravity experiments is examined.

Griffin, P. R.↗