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At least 55 records · Page 3

Thermal-capillary analysis of small-scale floating zones Steady-state calculations

Galerkin finite element analysis of a thermal-capillary model of the floating zone crystal growth process is used to predict the dependence of molten zone shape on operating conditions for the growth of small silicon boules. The model accounts for conduction-dominated heat transport in the melt, feed rod and growing crystal and for radiation between these phases, the ambient and a heater. Surface tension acting on the shape of the melt/gas meniscus counteracts gravity to set the shape of the molten zone. The maximum diameter of the growing crystal is set by the dewetting of the melt from the feed rod when the crystal radius is large. Calculations with small Bond number show the increased zone lengths possible for growth in a microgravity environment. The sensitivity of the method to the shape and intensity of the applied heating distribution is demonstrated. The calculations are compared with experimental observations.

Duranceau, J. L.↗

Microgravity Silicon Zoning Investigation

This research program is directed toward the understanding of the float zone crystal growth process, the melt interactions which lead to crystal inhomogeneities, and the influence of microgravity on reducing these inhomogeneities. Silicon was selected as the model crystal because its inhomogeneities lead to known variations in device performance, and because the mechanisms involved in its growth are understood better than for other high temperature crystals. The objective of the program is to understand the growth mechanisms in float zone growth and thereby determine the feasibility and advantages of float zone growth of silicon under microgravity conditions. This will be done by characterizing the growth at g = 1, projecting the changes in melt flows due to microgravity, observing these in space growth and determining the effects on defective inhomogeneities. A Thin Rod Zoner was constructed as a laboratory prototype for flight growth of 5 mm diameter silicon crystals, which can be done within the power and cooling capabilities of shuttle flights. A new method of zoning silicon, using resistance heating, has resulted in melting 5 mm diameter ingots.

E L Kern↗

Thermocapillary convection instability in microgravity crystal growth

Energy and linear stability theories are applied to study the stability properties of thermocapillary convection in a half zone model of the float zone crystal growth process. The analyses yield results which provide sufficient conditions for both stability and instability, respectively, and therefore, lower and upper bounds for the Marangoni numbers at which oscillatory thermocapillary convection will appear. The results of the analyses are compared with available experimental and numerical data.

Neitzel, G. P.↗

Toward In Situ Synchrotron Mapping of Crystal Selection Processes during Crystal Growth

In this work, we present an automated and rapid method for non-destructive mapping of crystal grains in a rod-shaped sample. The approach was designed for application to in situ float-zone crystal growth experiments at an x-ray synchrotron source, but could be useful in other applications. The methods have been tested on a TiO 2 boule grown in an optical float zone furnace. The approach applies a statistical filter to polycrystalline diffraction patterns on 2D detectors to rapidly determine the degree of powder-quality 1of the signal. When larger crystals emerge in the growth, their position, size and shape can be tracked using an automated blob-tracking algorithm that follows individual Bragg peaks as a function of position in a grid-scan, even when multiple crystals are contributing spots to diffraction images. This method is found to be robust as the same crystal shape can be independently reconstructed using different sets of Bragg reflections. Image segmentation methods are then used to map out the polycrystalline grains. We also note that other information about crystal quality, such as mosaicity or strain state, may be inferred and mapped from the intensity variation of the Bragg peaks at different locations within the sample.

36 MATERIALS SCIENCE↗

Modelling of the MEA float zone using accelerometer data

During a floating zone experiment involving the growth of indium on a recent orbiter mission, (STS 32) oscillation of the zone shapes were observed to occur in response to the background acceleration. An understanding of the nature of the response of the zone shape to forced (g-jitter) oscillations and predictions of its impact on future experiments is of great interest not only to the PI's but to other commercial and academic investigators who plan to fly similar experiments in the orbiter and on space station. Motivated by this, a 15 month study was undertaken to analyze the nature of the g-sensitivity of the STS 32 floating zone crystal growth experiment. Numerical models were used to describe the time-dependent free surface motion of the zone as it responds to the spacecraft residual acceleration. Relevant experimental data concerning the acceleration environment was obtained from the Honeywell in Space Accelerometer (HISA) investigators through MSFC's ACAP program and processed and analyzed. For the indium floating zone experiment, a series of calculations were made using time-dependent axial accelerations g(t). The form of g(t) included simple sinusoidal disturbances as well as actual data (subject to appropriate filtering) measured on the STS 32 mission. Focus was on the calculation of the response of the free surface of the zone as well as the internal flows and internal heat transfer. The influence of solidification on the response of the zone shape was also examined but found to be negligible.

Alexander, J. Iwan D.↗

The control of float zone interfaces by the use of selected boundary conditions

The main goal of the float zone crystal growth project of NASA's Materials Processing in Space Program is to thoroughly understand the molten zone/freezing crystal system and all the mechanisms that govern this system. The surface boundary conditions required to give flat float zone solid melt interfaces were studied and computed. The results provide float zone furnace designers with better methods for controlling solid melt interface shapes and for computing thermal profiles and gradients. Documentation and a user's guide were provided for the computer software.

Foster, L. M.↗

Power requirements for space crystal growth

The need for power to grow silicon of a size suitable to make into devices is addressed. The expected results are tied to available power. The projection of the size of float zone crystals as a function of time is discussed. An accompanying graph shows that 4 in. will be the normally used diameter by 1985 and 5 in. by 1990. Material to be tested in device lines in this time frame should be 4 in. or more. The various power losses, 25 kW with a 50% power efficiency, which is much improved over present RF heating efficiencies.

Kern, E. L.↗

Solar energy concentrator system for crystal growth and zone refining in space

The technological feasibility of using solar concentrators for crystal growth and zone refining in space has been performed. Previous studies of space-deployed solar concentrators were reviewed for their applicability to materials processing and a new state-of-the-art concentrator-receiver radiation analysis was developed. The radiation analysis is in the form of a general purpose computer program. It was concluded from this effort that the technology for fabricating, orbiting and deploying large solar concentrators has been developed. It was also concluded that the technological feasibility of space processing materials in the focal region of a solar concentrator depends primarily on two factors: (1) the ability of a solar concentrator to provide sufficient thermal energy for the process and (2) the ability of a solar concentrator to provide a thermal environment that is conductive to the processes of interest. The analysis indicate that solar concentrators can satisfactorily provide both of these factors.

Mcdermit, J. H.↗

Potential productivity benefits of float-zone versus Czochralski crystal growth

Efficient mass production of single-crystal silicon is necessary for the efficient silicon solar arrays needed in the coming decade. However, it is anticipated that there will be difficulty growing such volumes of crystals using conventional Czochralski (Cz) methods. While the productivity of single crystals might increase with a crystal diameter increase, there are two obstacles to the mass production of large diameter Czochralski crystals, the long production cycle due to slow growth rate and the high heat requirements of the furnaces. Also counterproductive would be the large resistivity gradient along the growth direction of the crystals due to impurity concentration. Comparison between Float zone (FZ) and Cz crystal growth on the basis of a crystal 150 mm in diameter is on an order of two to four times in favor of the FZ method. This advantage results from high growth rates and steady-state growth while maintaining a dislocation-free condition and impurity segregation.

Abe, T.↗

Sensitivity of liquid bridges subject to axial residual acceleration

It has become evident that the float zone crystal growth method and isothermal liquid bridges may be very sensitive to the residual acceleration environment of a spacelab. Using a slender-body approximation, the problem of determining the axisymmetric response of the shape of the free surface of a cylindrical liquid column bounded by two solid regions is modeled by a one-dimensional system of nonlinear equations. It is found that the sensitivity of the zone shape depends on the static Bond number, BO, aspect ratio, and viscosity, as well as the amplitude and frequency of the disturbance. The general trend is an increase in tolerable residual gravity with increasing frequency. At the eigenfrequencies of the zone, however, there are dramatic deviations from this trend. At these frequencies the tolerable residual gravity level can be two orders of magnitude lower at this frequency.

Zhang, Yiqiang↗

Growth of a single crystal ribbon in space

Three critical technological areas associated with adapting the method of pulling signal crystal silicon ribbon to a space environment were investigated. Basic parameters such as the magnitude of the forces required and the coupling between thermal and force are discussed. The design of a ribbon puller is described, and the problems encountered are also discussed. The force fields in the vicinity of a coil were characterized and results of attempts to pull ribbon are described. The results of the one experiment to grow a conventional float zone crystal in an external static magnetic field are presented.

Padovani, F. A.↗

Control of Meridional Flow by a Non-Uniform Rotational Magnetic Field

The diffusive mass transfer of species during crystal growth in vertical ampoules is significantly affected by fluid flow in the liquid mother phase (melt). For electrically conductive melts, an elegant way of remotely inducing and controlling this flow is by utilizing a uniform rotational magnetic field (RMF) in the transverse direction. It induces an azimuthal flow which tends to homogenize the thermal and solutal fields. The rotating field also reduces the diffusion boundary layer, stabilizes temperature fluctuations, and promotes better overall crystal growth. For moderate strengths of the applied magnetic field (2-20 m Tesla) with frequencies of up to 400 Hz, the induced secondary meridional flow becomes significant. It typically consists of one roll at the bottom of the liquid column and a second roll (vortex) at the top. The flow along the centerline (ampoule axis) is directed from the growing solid (interface) towards the liquid (melt). In case of convex interfaces (e.g. in floating zone crystal growth) such flow behavior is beneficial since it suppresses diffusion at the center. However, for concave interfaces (e.g. vertical Bridgman crystal growth) such a flow tends to exacerbate the situation in making the interface shape more concave. It would be beneficial to have some control of this meridional flow- for example, a single recirculating cell with controllable direction and flow magnitude will make this technique even more attractive for crystal growth. Such flow control is a possibility if a non-uniform PNE field is utilized for this purpose. Although this idea has been proposed earlier, it has not been conclusively demonstrated so far. In this work, we derive the governing equations for the fluid dynamics for such a system and obtain solutions for a few important cases. Results from parallel experimental measurements of fluid flow in a mercury column subjected to non-uniform RMF will also be presented.

Mazuruk, Konstantin↗

Interface velocity dependent solute trapping and phase selection during rapid solidification of laser melted hypo-eutectic Al-11at.%Cu alloy

Microstructure formation of a hypo-eutectic Al-11Cu (atom percent) alloy during solidification after laser melting has been studied by transmission electron microscopy (TEM). The evolution of the solid-liquid-interface velocity, V SL , during the solidification process has been determined from direct observation by in-situ TEM. This enabled correlating V SL with development of four distinct microstructure zones. Crystal growth mode transitions from planar to cellular, cellular to dendritic, dendritic to cellular, and cellular to planar, have been observed for the accelerating solid-liquid-interface. The transition from coupled two-phase growth to the single-phase growth occurred for V SL = V a = (0.80±0.05) m/s, where V a is the velocity of absolute stability, at the onset of banded morphology grain formation. The in-situ and post-mortem TEM uniquely permitted determination of the non-equilibrium solidus for the rapidly solidifying Al-11Cu alloy. Experimental evidence for solute clustering and chemical ordering tendencies at length scales on the order of ≤ 5nm has been detected in the single-phase regions of the banded grains. The structural features of the single-phase bands have been interpreted as signatures of ‘frozen in’ configurations present in the liquid boundary layer adjacent to the growing crystal, which has a width of about 3nm. Finally, the nano-scale spatiotemporal resolution experimental TEM studies performed here provided quantitative metrics, e.g. the solidification interface velocity dependent solute concentration of the α-Al phase and the near-atomic scale structure in the single-phase bands, that are uniquely suitable for comparison with theory and model predictions for solidification microstructure development in multicomponent alloys after laser melting.

36 MATERIALS SCIENCE↗

Atomic Resolution Imaging of Light Elements in a Crystalline Environment using Dynamic Hollow-Cone Illumination Transmission Electron Microscopy

Multiple electron scattering and the nonintuitive nature of image formation with coherent radiation complicate the interpretation of conventional transmission electron microscopy images. Precession of the illuminating beam in transmission electron microscopy (TEM) can lead to more robust and interpretable images with some penalty to image contrast, a technique known as dynamic hollow-cone illumination TEM. Here, we demonstrate direct and robust imaging of light and heavy atoms in a crystalline environment with this technique. This method is similar to the annular bright-field technique in scanning transmission electron microscopy, via the principle of reciprocity. Dynamic hollow-cone illumination TEM is challenging in practice due to sensitivity to the misalignment of the precession axis, microscope objective aperture, and crystal zone axis.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

U redox state tracked in mineralized hydrothermal carbonate with implications for U-Pb geochronology

U-Pb carbonate geochronology can directly constrain the timing and rates of important geological processes. However, the mechanisms and controls on U incorporation, distribution, and retention in carbonate minerals remain unclear, limiting geological interpretations. Here X-ray absorption spectroscopy (µXAS) and in-situ U-Pb carbonate geochronology are combined to temporally track U distribution and redox state in a porphyry-epithermal system. In this setting, multiple generations of carbonate minerals record fluid conditions and processes which control the solubility and deposition of metals, including U. This novel approach provides the first evidence of both oxidized UO 2 2+ and reduced U 4+ species in temporally distinct generations of carbonate within a single sample. Preservation of two different U oxidation states during discrete precipitation events requires U retentivity within older domains, demonstrating that the U-Pb carbonate geochronometer is robust under hydrothermal conditions. Furthermore, crystal zones with abundant fluid/vapour inclusions linked to boiling processes coincide with relatively high levels of U and favourable U/Pb. Targeting carbonate domains with these textures may therefore increase success in U-Pb geochronology. U-Pb carbonate dating combined with µXAS can track the temporal evolution of processes critical for metal deposition in long-lived and multistage hydrothermal-magmatic ore deposit settings.

58 GEOSCIENCES↗

Experimental study of pyroxene-liquid interaction in quartz-normative basalt 15597

Equilibrium and controlled cooling rate experiments on a synthetic analog of Apollo 15 quartz normative basalt 15597 are reported. While the partitioning of the major elements Ca, Mg, and Fe between pyroxene and liquid is rate independent, the K sub D parameter for Fe/Mg, which is calculated for low-Ca pyroxene, is temperature dependent. It is suggested that chemical trends observed in lunar pyroxenes are a consequence of three rate processes. The processes are (1) rate-dependent suppression of crystallization of other phases until lower temperature alters liquid composition and, therefore, the composition of the pyroxene that crystallizes; (2) the efficiency of fractional crystallization and the extent of crystal zoning are rate dependent; and (3) the partitioning of Al2O3, TiO2, and Cr2O3 between pyroxene and liquid depends on cooling rate.

Grove, T. L.↗

Characterization of the effects of metallic impurities on silicon solar cell performance

The effects of controlled concentrations of secondary impurities (Al, C, Ca, Cr, Cu, Fe, Mg, Mn, Mo, Ta, Ti, V, Zn, and Zr), incorporated alone or in combinations into Czochralski and float zone crystals, on the performance of silicon solar cells were investigated. Impurity concentrations ranged from 10 to the 11th to 10 to the 17th/cu cm. Solar cells were fabricated by a conventional diffusion process and characterized by computer reduction of current-voltage data. The data suggest that performance loss primarily results from reduction of the base diffusion length. On the basis of this assumption, a first order analytic model which predicts cell performance as a function of impurity concentrations is developed. Calculated performance parameters are in good agreement with observation, except for some impurities, such as Fe, Cu and Ni, which degrade cells via recombination and defects in the junction space-charge region. N-base devices are less affected by impurities, although degradation mechanisms appear to be the same as in p-devices. There seems to be very limited interaction between impurities in multiply-doped cells.

Davis, J. R.↗