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All sourcesNASA NTRSDOE OSTI
NASA NTRS1993

Growth of Si spherical crystals and the surface oxidation (M-9)

Nearly 90 percent of semiconductor devices are produced with Si single crystals as the starting materials. For instance, the integrated circuits (IC), which are used in almost all electronic equipments such as TV, tape recorders, audio amplifiers, etc., are made after various processings of Si single crystal wafers. In these wafers, the same controlled amounts of impurities are added and the uniformities in their distributions are extremely important. Growth under microgravity makes it possible to eliminate the buoyancy-driven convection in the melt, which is one of the main origins of convections which results in non-uniformity of the impurity. Another source of convection is known as Marangoni convection which is driven on the free surface when a temperature gradient occurs. One of the merits of microgravity experimentation is that the detailed study of this convection becomes possible. Another important advantage of microgravity is that growth of crystals without a crucible is possible. This makes it possible to study melt growth without the strain which is usually introduced on the ground. Nevertheless, we should repeat and analyze many growth experiments in space to get reliable results. However, since in the FMPT, the time for the experiment is limited, we plan to carry out two kinds of very simple and basic experiments as the first step for the semiconductor growth experiment. In the first experiment, we use single crystal Si sphere as the starting material and as shown, this sphere is heated in the furnace at a slightly higher temperature than the melting point. After the melting front moves nearly half way to its center, the temperature is decreased to stop the melting and to start the growth from the seed for which we use the unmelted solid party of the sphere. The sphere is centered by quartz protuberances inside of the quartz crucible. There exists the possibility of temperature fluctuations being introduced when the molten sphere occasionally touches the protuberances. The total time needed for the melting and the growth processes is estimated to be 30 minutes. Infrared emission from the sphere is monitored in order to prevent the accidental loss of the central solid core. The schematical illustration of the second experient is shown. A single crystal, Si rod is used as the starting material. In the first stage, the rod is melted from one end to obtain a liquid sphere. In the second stage, the single crystal is grown by decreasing the temperature from the unmelted part of the rod which is used as the seed. The second experient somewhat resembles the Czochralski method used on the ground; however, in the space experiment, no crucible is employed and the temperature uniformity is much superior. In both experiments, phosphorous is doped to allow observation of the change in the shape of the liquid solid interface during crystal growth and the impurity striations, if any.

Nishinaga, Tatau↗
NASA NTRS2002

Length Scale and Gravity Effects on Microgravity Boiling Heat Transfer

Boiling is a complex phenomenon where hydrodynamics, heat transfer, mass transfer, and interfacial phenomena are tightly interwoven. An understanding of boiling and critical heat flux in microgravity environments is of importance to space based hardware and processes such as heat exchange, cryogenic fuel storage and transportation, electronic cooling, and material processing due to the large amounts of heat that can be removed with relatively little increase in temperature. Although research in this area has been performed in the past four decades, the mechanisms by which heat is removed from surfaces in microgravity are still unclear. In earth gravity, buoyancy is an important parameter that affects boiling heat transfer through the rate at which bubbles are removed from the surface. A simple model describing the bubble departure size based on a quasistatic force balance between buoyancy and surface tension is given by the Fritz [I] relation: Bo(exp 1/2) = 0.0208 theta where Bo is the ratio between buoyancy and surface tension forces. For small, rapidly growing bubbles, inertia associated with the induced liquid motion can also cause bubble departure. In microgravity, the magnitude of effects related to natural convection and buoyancy are small and physical mechanisms normally masked by natural convection in earth gravity such as Marangoni convection can substantially influence the boiling and vapor bubble dynamics. CHF (critical heat transfer) is also substantially affected by microgravity. In 1 g environments, Bo has been used as a correlating parameter for CHF. Zuber's CHF model for an infinite horizontal surface assumes that vapor columns formed by the merger of bubbles become unstable due to a Helmholtz instability blocking the supply of liquid to the surface. The jets are spaced lambda(sub D) apart, where lambda(sub D) = 2pi square root of 3[(sigma)/(g(rho(sub l) - rho(sub v)](exp 1/2) = 2pi square root of 3 L Bo(exp -1/2) = square root of 3 lambda(sub c) and is the wavelength that amplifies most rapidly. The critical wavelength, lambda(sub c), is the wavelength below which a vapor layer underneath a liquid layer is stable. For heaters with Bo smaller than about 3 (heaters smaller than lambda(sub D)), the above model is not applicable, and surface tension effects dominate. Bubble coalescence is thought to be the mechanism for CHF under these conditions. Small Bo can result by decreasing the size of a heater in earth gravity, or by operating a large heater in a lower gravity environment. In the microgravity of space, even large heaters can have low Bo, and models based on Helmholtz instability should not be applicable. The macrolayer model of Haramura and Katto is dimensionally equivalent to Zuber's model and has the same dependence on gravity, so it should not be applicable as well. The goal of this work is to determine how boiling heat transfer mechanisms in a low-g environment are altered from those at higher gravity levels. Boiling data using a microheater array was obtained under gravity environments ranging from 1.8 g to 0.02 g with heater sizes ranging from 2.7 mm to 1 mm. The boiling behavior for 2.7 mm at 0.02 g looked quite similar to boiling on the 1 mm heater at 1 g-the formation of a large primary bubble surrounded by smaller satellite bubbles was observed under both conditions. The similarity suggests that for heaters smaller than some fraction of I(sub c), coalescence and surface tension dominate boiling heat transfer. It also suggests that microgravity boiling can be studied by studying boiling on very small heaters.

Kim, Jungho↗
DOE OSTI2020

Deposit geometry and oxygen concentration spatial variations due to composition change in printed functionally graded components

Functionally graded materials (FGMs) with site specific chemical composition are commonly manufactured by directed energy deposition (DED). Although previous work fabricated an FGM with a compositional variation between a ferritic and austenitic alloy, difficulties arose due to variations in deposit shape with composition change. This problem also occurs for FGMs in literature; however, unlike other cases, the thermophysical properties of these two alloys were similar throughout the build. Here, we investigate the role of chemical composition and surface-active elements on deposit geometry during the manufacture of FGMs by laser DED. Single-track experiments for the relevant FGM compositions are analyzed with results from a well-tested, three-dimensional, transient numerical heat transfer and fluid flow model and thermodynamic calculations. Experiments showed deposit shape varied as a function of composition for constant laser power and scan speed. Thermodynamic analysis indicated that the oxygen solubility in the fusion zone varied significantly for each composition used for the FGM. Numerical modeling revealed that the change in fluid flow caused by Marangoni convection due to dissolved oxygen in the fusion zone were mainly responsible for the changes in deposit shape observed in experiments. Finally, because oxygen can be introduced into the fusion zone through the feedstock as well as the surrounding atmosphere, these findings elucidate a previously unconsidered aspect of process control during DED fabrication of FGMs.

36 MATERIALS SCIENCE↗
NASA NTRS1996

Studies in Thermocapillary Convection of the Marangoni-Benard Type

The effects of imposed nonlinear oscillatory shear upon the onset of Marangoni-Bernard convection, as predicted by linear theory, in a layer of liquid with a deformable free surface were reported upon by Or and Kelly for small amplitude oscillations. Depending on the operating conditions, either stabilization or destabilization might occur. The aim of the current paper is to report the results for finite amplitude imposed oscillations so that the actual amount of stabilization or destabilization can be determined for prescribed operating conditions.

Kelly, Robert E.↗
NASA NTRS1999

Studies in Thermocapillary Convection of the Marangoni-Benard Type

A nonlinear feedback control strategy for delaying the onset and eliminating the subcritical nature of long-wavelength Marangoni-Benard convection is investigated based on an evolution equation. A control temperature is applied to the lower wall in a gas-liquid layer otherwise heated uniformly from below. It is shown that, if the interface deflection is assumed to be known via sensing as a function of both horizontal coordinates and time, a control temperature with a cubic-order polynomial dependence on the deflection is capable of delaying the onset as well as eliminating the subcritical instability altogether, at least on the basis of a weakly nonlinear analysis. The control coefficients required for stabilization are O(1) for both delaying onset indefinitely and eliminating subcritical instability.

Kelly, R. E.↗
NASA NTRS1996

Bubble Dynamics on a Heated Surface

In this work, we study the combined thermocapillary and natural convective flow generated by a bubble on a heated solid surface. The interaction between gas and vapor bubbles with the surrounding fluid is of interest for both space and ground-based processing. On earth, the volumetric forces are dominant, especially, in apparatuses with large volume to surface ratio. But in the reduced gravity environment of orbiting spacecraft, surface forces become more important and the effects of Marangoni convection are easily unmasked. In order to delineate the roles of the various interacting phenomena, a combined numerical-experimental approach is adopted. The temperature field is visualized using Mach-Zehnder interferometry and the flow field is observed by a laser sheet flow visualization technique. A finite element numerical model is developed which solves the two-dimensional momentum and energy equations and includes the effects of bubble surface deformation. Steady state temperature and velocity fields predicted by the finite element model are in excellent qualitative agreement with the experimental results. A parametric study of the interaction between Marangoni and natural convective flows including conditions pertinent to microgravity space experiments is presented. Numerical simulations clearly indicate that there is a considerable difference between 1-g and low-g temperature and flow fields induced by the bubble.

Kassemi, Mohammad↗
NASA NTRS2011

Prospects for Interdisciplinary Science Aboard the International Space Station

The assembly of the International Space Station was completed in early 2011, and is now embarking on its first year of the coming decade of use as a laboratory. Two key types of physical science research are enabled by ISS: studies of processes that are normally masked by gravity, and instruments that take advantage of its position as a powerful platform in orbit. The absence of buoyancy-driven convection enables experiments in diverse areas such as fluids near the critical point, Marangoni convection, combustion, and coarsening of metal alloys. The positioning of such a powerful platform in orbit with robotic transfer and instrument support also provides a unique alternative platform for astronomy and physics instruments. Some of the operating or planned instruments related to fundamental physics on the International Space Station include MAXI (Monitoring all-sky X-ray Instrument for ISS), the Alpha Magnetic Spectrometer, CALET (Calorimetric Electron Telescope), and ACES (Atomic Clock Experiment in Space). The presentation will conclude with an overview of pathways for funding different types of experiments from NASA funding to the ISS National Laboratory, and highlights of the streamlining of services to help scientists implement their experiments on ISS.

Robinson, Julie A.↗
NASA NTRS1999

Long-Wavelength Rupturing Instability in Surface-Tension-Driven Benard Convection

A liquid layer with a free upper surface and heated from below is subject to thermocapillary-induced convective instabilities. We use very thin liquid layers (0.01 cm) to significantly reduce buoyancy effects and simulate Marangoni convection in microgravity. We observe thermocapillary-driven convection in two qualitatively different modes, short-wavelength Benard hexagonal convection cells and a long-wavelength interfacial rupturing mode. We focus on the long-wavelength mode and present experimental observations and theoretical analyses of the long-wavelength instability. Depending on the depths and thermal conductivities of the liquid and the gas above it, the interface can rupture downwards and form a dry spot or rupture upwards and form a high spot. Linear stability theory gives good agreement to the experimental measurements of onset as long as sidewall effects are taken into account. Nonlinear theory correctly predicts the subcritical nature of the bifurcation and the selection between the dry spot and high spots.

Swift, J. B.↗
NASA NTRS1998

Oscillatory/Chaotic Thermocapillary Flow Induced by Radiant Heating

There is a continuing need to understand the fluid physics occurring under low gravity conditions in processes such as crystal growth, materials processing, and the movement of bubbles or droplets. The fluid flow in such situations is often caused by a gradient in interfacial tension. If a temperature gradient is created due to a heat source, the resulting flow is called thermocapillary flow, a special case of Marangoni Convection. In this study, an experimental investigation was conducted using silicone oil in cylindrical containers with a laser heat source at the free surface. It was desired to determine the conditions under which steady, axisymmetrical thermocapillary flow becomes unstable and oscillatory three-dimensional flow states develop. The critical Marangoni number for each observed oscillatory state was measured as a function of the container aspect ratio and the dynamic Bond number, a measure of buoyant force versus ii thermocapillary force. Various oscillatory modes were observed during three- dimensional convection, and chaotic flow was reached in one test condition. The critical Marangoni numbers are compared with those measured in previous studies, and the power spectra and phase trajectories of the instantaneous surface temperature distributions are used to characterize the routes of transitions to the chaotic flow state. Results show that only superharmonic modes appear in the routes to chaos while infinite number of subharmonic modes occur in flow transitions for pure Rayleigh convection.

DeWitt, Kenneth J.↗
NASA NTRS2006

Heat Transfer of Thermocapillary Convection in a Two-Layered Fluid System Under the Influence of Magnetic Field

Heat transfer of a two-layer fluid system has been of great importance in a variety of industrial applications. For example, the phenomena of immiscible fluids can be found in materials processing and heat exchangers. Typically in solidification from a melt, the convective motion is the dominant factor that affects the uniformity of material properties. In the layered flow, thermocapillary forces can come into an important play, which was first emphasized by a previous investigator in 1958. Under extraterrestrial environments without gravity, thermocapillary effects can be a more dominant factor, which alters material properties in processing. Control and optimization of heat transfer in an immiscible fluid system need complete understanding of the flow phenomena that can be induced by surface tension at a fluid interface. The present work is focused on understanding of the magnetic field effects on thermocapillary convection, in order to optimize material processing. That is, it involves the study of the complicated phenomena to alter the flow motion in crystal growth. In this effort, the Marangoni convection in a cavity with differentially heated sidewalls is investigated with and without the influence of a magnetic field. As a first step, numerical analyses are performed, by thoroughly investigating influences of all pertinent physical parameters. Experiments are then conducted, with preliminary results, for comparison with the numerical analyses.

Ramachandran, N.↗
NASA NTRS2003

Control of Thermal Convection in Layered Fluids Using Magnetic fields

Immiscible fluid layers are found in a host of applications ranging from materials processing, for example the use of encapsulants in float zone crystal growth technique and a buffer layer in industrial Czochralski growth of crystals to prevent Marangoni convection, to heat transfer phenomena in day-to-day processes like the presence of air pockets in heat exchangers. In the microgravity and space processing realm, the exploration of other planets requires the development of enabling technologies in several fronts. The reduction in the gravity level poses unique challenges for fluid handling and heat transfer applications. The present work investigates the efficacy of controlling thermal convective flow using magnetic fluids and magnetic fields. The setup is a two-layer immiscible liquids system with one of the fluids being a diluted ferrofluid (super paramagnetic nano particles dispersed in carrier fluid). Using an external magnetic field one can essentially dial in a volumetric force - gravity level, on the magnetic fluid and thereby affect the system thermo-fluid behavior. The paper will describe the experimental and numerical modeling approach to the problem and discuss results obtained to date.

Ramachandran, N.↗
NASA NTRS1991

Convection in a two-layer fluid system

Experimental results are presented, and preliminary computations are performed on a system of two immiscible liquid layers with a temperature gradient applied parallel to the interface. The experiments reflect the combined contribution of buoyancy and surface-tension-induced (Marangoni) convection. It is concluded that buoyancy effects appear to be dominant and mask any surface-tension-induced convection present. Numerical computations show significant modification of pure buoyant convection by surface-tension gradients. The results are of interest in connection with the liquid encapsulation of GaAs melts in a microgravity environment.

Prakash, A.↗
NASA NTRS1984

Float zone experiments in space

The molten zone/freezing crystal interface system and all the mechanisms were examined. If Marangoni convection produces oscillatory flows in the float zone of semiconductor materials, such as silicon, then it is unlikely that superior quality crystals can be grown in space using this process. The major goals were: (1) to determine the conditions for the onset of Marangoni flows in molten tin, a model system for low Prandtl number molten semiconductor materials; (2) to determine whether the flows can be suppressed by a thin oxide layer; and (3) based on experimental and mathematical analysis, to predict whether oscillatory flows will occur in the float zone silicon geometry in space, and if so, could it be suppressed by thin oxide or nitride films. Techniques were developed to analyze molten tin surfaces in a UHV system in a disk float zone geometry to minimize buoyancy flows. The critical Marangoni number for onset of oscillatory flows was determined to be greater than 4300 on atomically clean molten tin surfaces.

Verhoeven, J. D.↗
NASA NTRS1999

Reduction of Defects in Germanium-Silicon

It is well established that crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached-Bridgman growth is often cited as a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur quite often during microgravity experiments and considerable improvements of crystal quality have been reported for those cases. However, no thorough understanding of the process or quantitative assessment of the quality improvements exists so far. This project will determine the means to reproducibly grow Ge-Si alloys in the detached mode. Specific objectives include: (1) measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; (2) determination of the mechanism of detached growth including the role of convection; (3) quantitative determination of the differences of defects and impurities among normal Bridgman, detached Bridgman, and floating zone (FZ) growth; (4) investigation of the influence of defined azimuthal or meridional flow due to rotating magnetic fields on the characteristics of detached growth; (5) control time-dependent Marangoni convection in the case of FZ-growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and (6) grow high quality GeSi-single crystals with Si-concentration up to 10 at% and diameters up to 20 mm.

Szofran, Frank R.↗
NASA NTRS1998

Reduction of Defects in Germanium-Silicon

It is well established that crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float- zone processing, detached-Bridgman growth is often cited as a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur quite often during micro-g experiments and considerable improvements of crystal quality have been reported for those cases. However, no thorough understanding of the process or quantitative assessment of the quality improvements exists so far. This project will determine the means to reproducibly grow Ge-Si alloys in the detached mode. Specific objectives include: (1) measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; (2) determination of the mechanism of detached growth including the role of convection; (3) quantitative determination of the differences of defects and impurities among normal Bridgman, detached Bridgman, and Floating Zone (FZ) growth; (4) investigation of the influence of defined azimuthal or meridional flow due to rotating magnetic fields on the characteristics of detached growth; (5) control time-dependent Marangoni convection in the case of FZ-growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and (6) grow high quality GeSi-single crystals with Si-concentration up to 10 at% and diameters up to 20 mm.

Szofran, Frank R.↗
NASA NTRS2003

Reduction of Defects in Germanium-Silicon

Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in the crystals. In addition to float-zone processing, detached Bridgman growth, although not a completely crucible-free method, is a promising tool to improve crystal quality. It does not suffer from the size limitations of float zoning and the impact of thermocapillary convection on heat and mass transport is expected to be negligible. Detached growth has been observed frequently during g experiments. Considerable improvements in crystalline quality have been reported for these cases. However, neither a thorough understanding of the process nor a quantitative assessment of the quality of these improvements exists. This project will determine the means to reproducibly grow GeSi alloys in a detached mode and seeks to compare processing-induced defects in Bridgman, detached-Bridgman, and floating-zone growth configurations in GeSi crystals (Si less than or equal to 10 at%) up to 20mm in diameter. Specific objectives include: measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; determination of the mechanism of detached growth including the role of convection; quantitative determination of the differences in defects and impurities for crystals grown using normal Bridgman, detached Bridgman, and floating zone (FZ) methods; investigation of the influence of a defined flow imposed by a rotating magnetic field on the characteristics of detached growth; control of time-dependent Marangoni convection in the case of FZ growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and growth of benchmark quality GeSi-single crystals.

Szofran, Frank R.↗
NASA NTRS2000

Fluid Physics and Macromolecular Crystal Growth in Microgravity

The molecular structure of biological macromolecules is important in understanding how these molecules work and has direct application to rational drug design for new medicines and for the improvement and development of industrial enzymes. In order to obtain the molecular structure, large, well formed, single macromolecule crystals are required. The growth of macromolecule crystals is a difficult task and is often hampered on the ground by fluid flows that result from the interaction of gravity with the crystal growth process. One such effect is the bulk movement of the crystal through the fluid due to sedimentation. A second is buoyancy driven convection close to the crystal surface. On the ground the crystallization process itself induces both of these flows. Buoyancy driven convection results from density differences between the bulk solution and fluid close to the crystal surface which has been depleted of macromolecules due to crystal growth. Schlieren photograph of a growing lysozyme crystal illustrating a 'growth plume' resulting from buoyancy driven convection. Both sedimentation and buoyancy driven convection have a negative effect on crystal growth and microgravity is seen as a way to both greatly reduce sedimentation and provide greater stability for 'depletion zones' around growing crystals. Some current crystal growth hardware however such as those based on a vapor diffusion techniques, may also be introducing unwanted Marangoni convection which becomes more pronounced in microgravity. Negative effects of g-jitter on crystal growth have also been observed. To study the magnitude of fluid flows around growing crystals we have attached a number of different fluorescent probes to lysozyme molecules. At low concentrations, less than 40% of the total protein, the probes do not appear to effect the crystal growth process. By using these probes we expect to determine not only the effect of induced flows due to crystal growth hardware design but also hope to optimize crystallization hardware so that destructive flows are minimized both on the ground and in microgravity.

Pusey, M.↗
NASA NTRS1993

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗