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NASA NTRS1997

Thermal Problems in Material processing of High-Temperature Materials

In this final report axial segregation in unsteady diffusion dominated directional solidification of a binary alloy with a planar solid-liquid interface profile is considered. The analysis is an extension of the work of Smith et al. to account for an arbitrary initial axial concentration profile. This situation is important in the experimental studies of growth of crystals in a microgravity environment in which the growth is from melts formed by re-melting crystals that have a known axial impurity profile. Three situations are discussed. There are the initial transient, a re-solidified crystal, and multipass solidification.

Korpela, Seppo A.↗

NASA NTRS1998

Buckets: Aggregative, Intelligent Agents for Publishing

Buckets are an aggregative, intelligent construct for publishing in digital libraries. The goal of research projects is to produce information. This information is often instantiated in several forms, differentiated by semantic types (report, software, video, datasets, etc.). A given semantic type can be further differentiated by syntactic representations as well (PostScript version, PDF version, Word version, etc.). Although the information was created together and subtle relationships can exist between them, different semantic instantiations are generally segregated along currently obsolete media boundaries. Reports are placed in report archives, software might go into a software archive, but most of the data and supporting materials are likely to be kept in informal personal archives or discarded altogether. Buckets provide an archive-independent container construct in which all related semantic and syntactic data types and objects can be logically grouped together, archived, and manipulated as a single object. Furthermore, buckets are active archival objects and can communicate with each other, people, or arbitrary network services.

Nelson, Michael L.↗

NASA NTRS1998

Gravitational Role in Liquid Phase Sintering

To comprehensively understand the gravitational effects on the evolution of both the microstructure and the macrostructure during liquid phase sintering, W-Ni-Fe alloys with W content varying from 35 to 98 wt.% were sintered in microgravity. Compositions that slump during ground-based sintering also distort when sintered under microgravity. In ground-based sintering, low solid content alloys distort with a typical elephant-foot profile, while in microgravity, the compacts tend to spheroidize. This study shows that microstructural segregation occurs in both ground-based as well as microgravity sintering. In ground-based experiments, because of the density difference between the solid and the liquid phase, the solid content increases from top to the bottom of the sample. In microgravity, the solid content increases from periphery to the center of the samples. This study also shows that the pores during microgravity sintering act as a stable phase and attain anomalous shapes.

Upadhyaya, Anish↗

NASA NTRS1998

Toward Optimum Scale and TBC Adhesion on Single Crystal Superalloys

Single crystal superalloys exhibit excellent cyclic oxidation resistance if their sulfur content is reduced from typical impurity levels of approximately 5 ppmw to below 0.5 ppmw. Excellent alumina scale adhesion was documented for PWA 1480 and PWA 1484 without yttrium additions. Hydrogen annealing produced effective desulfurization of PWA 1480 to less than 0.2 ppmw and was also used to achieve controlled intermediate levels. The direct relationship between cyclic oxidation behavior and sulfur content was shown. An adhesion criterion was proposed based on the total amount of sulfur available for interfacial segregation, e.g., less than or equal to 0.2 ppmw S will maximize adhesion for a 1 mm thick sample. PWA 1484, melt desulfurized to 0.3 ppmw S, also exhibited excellent cyclic oxidation resistance and encouraging TBC lives (10 mils of 8YSZ, plasma sprayed without a bond coat) in 1100 C cyclic oxidation tests.

Smialek, James L.↗

NASA NTRS1999

Fundamental Studies of Solidification in Microgravity Using Real-Time X-Ray Microscopy

This research applies a state of the art X-ray Transmission Microscope, XTM, to image (with resolutions up to 3 micrometers) the solidification of metallic or semiconductor alloys in real-time. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. During this study, the growth of secondary phase fibers and lamellae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Current high resolution X-ray sources and high contrast X-ray detectors have advanced to allow systematic study of solidification dynamics and the resulting microstructure. We have employed a state-of-the-art sub-micron source with acceleration voltages of 10-100 kV to image solidification of metals. One useful strength of the XTM stems from the manner an image is formed. The radiographic image is a shadow formed by x-ray photons that are not absorbed as they pass through the specimen. Composition gradients within the specimen cause variations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). The ability to image these features in real-time enables more fundamental and detailed understanding of solidification dynamics than has previously been possible. Hence, application of this technique towards microgravity experiments will allow rigorous testing of critical solidification models.

Curreri, Peter A.↗

NASA NTRS1999

Melt Stabilization of PbSnTe in a Magnetic Field

Both the experimental observation and numerical simulation indicate that the Bridgman growth of PbSnTe under the microgravity environment in space is still greatly influenced by buoyancy-induced convection. The application of a magnetic field during the semiconductor growth can dampen the convective flow in the metal-like melt. However, for Bridgman growth of PbSnTe on earth (with either vertical or horizontal configuration), both experimental observation and numerical modeling suggest that even with a strong magnetic furnace (5-Tesla constant axial magnetic field), the convective flow in the melt still cannot be sufficiently suppressed to reach the diffusion-controlled level. In order to completely dampen the buoyancy-induced convection on earth, estimates based on scaling analysis indicate that for common experimental conditions, an extremely high magnetic field is required, far beyond the capacity of the experimental apparatus currently available. Therefore, it is proposed that only the combination of microgravity environment and magnetic damping will produce the desired diffusion-controlled growth state for this particular material. The primary objectives of this study are to provide a quantitative understanding of the complex transport phenomena during solidification of non-dilute binarys, to furnish a numerical tool for furnace design and growth condition optimization, to provide estimates of the required magnetic field strength for low gravity growth, and to assess the role of magnetic damping for space and earth control of the double-diffusive convection. As an integral part of a NASA research program, our numerical simulation supports both the flight and ground-based experiments in an effort to bring together a complete picture of the complex physical phenomena involved in the crystal growth process. For Bridgman growth of PbSnTe under microgravity (with both vertical and horizontal configurations), the simulations suggest that a moderate axial magnetic field of only a few kilo-Gauss in strength could effectively eliminate buoyancy-induced convection in the melt and control solute segregation. Therefore, this work confirms the idea that the combination of microgravity environment and the magnetic damping will indeed be sufficient to produce the desired diffusion-controlled growth state for PbSnTe.

Fripp, Archibald L.↗

NASA NTRS1999

Crystal Growth of II-VI Semiconducting Alloys by Directional Solidification

This research study is investigating the effects of a microgravity environment during the crystal growth of selected II-VI semiconducting alloys on their compositional, metallurgical, electrical and optical properties. The on-going work includes both Bridgman-Stockbarger and solvent growth methods, as well as growth in a magnetic field. The materials investigated are II-VI, Hg(1-x)Zn(x)Te, and Hg(1-x)Zn(x)Se, where x is between 0 and 1 inclusive, with particular emphasis on x-values appropriate for infrared detection and imaging in the 5 to 30 micron wavelength region. Wide separation between the liquidus and solidus of the phase diagrams with consequent segregation during solidification and problems associated with the high volatility of one of the components (Hg), make the preparation of homogeneous, high-quality, bulk crystals of the alloys an extremely difficult nearly an impossible task in a gravitational environment. The three-fold objectives of the on-going investigation are as follows: (1) To determine the relative contributions of gravitationally-driven fluid flows to the compositional redistribution observed during the unidirectional crystal growth of selected semiconducting solid solution alloys having large separation between the liquidus and solidus of the constitutional phase diagram; (2) To ascertain the potential role of irregular fluid flows and hydrostatic pressure effects in generation of extended crystal defects and second-phase inclusions in the crystals; and, (3) To obtain a limited amount of "high quality" materials needed for bulk crystal property characterizations and for the fabrication of various device structures needed to establish ultimate material performance limits. The flight portion of the study was to be accomplished by performing growth experiments using the Crystal Growth Furnace (CGF) manifested to fly on various Spacelab missions.

Lehoczky, Sandor L.↗

NASA NTRS1999

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport

Complete and systematic ground-based experimental and theoretical analyses on the Physical Vapor Transport (PVT) of ZnSe and related ternary compound semiconductors have been performed. The analyses included thermodynamics, mass flux, heat treatment of starting material, crystal growth, partial pressure measurements, optical interferometry, chemical analyses, photoluminescence, microscopy, x-ray diffraction and topography as well as theoretical, analytical and numerical analyses. The experimental results showed the influence of gravity orientation on the characteristics of: (1) the morphology of the as-grown crystals as well as the as-grown surface morphology of ZnSe and Cr doped ZnSe crystals; (2) the distribution of impurities and defects in ZnSe grown crystals; and (3) the axial segregation in ZnSeTe grown crystals.

Su, Ching-Hua↗

NASA NTRS1998

Melt Convection Effects in the Bridgman Crystal Growth of an Alloy Under Microgravity Conditions

The solidification of a dilute bismuth-tin alloy under Bridgman crystal growth conditions is investigated in support of NASA's MEPHISTO space shuttle flight experiment. Computations are performed in two-dimensions with a uniform grid. The simulation includes the species-concentration, temperature and flow fields, as well as conduction in the ampoule. Fully transient simulations have been performed; no simplifying steady state approximations are used. Results are obtained under microgravity conditions for pure bismuth, and Bismuth-0.1 at.% Sn and Bi-1.0 at.% Sn alloys. The concentration dependence of the melting temperature is neglected; the solid/liquid interface temperature is assumed to be the melting temperature of pure bismuth for all cases studied. For the Bi-1.0 at.% Sn case the results indicate that a secondary convective cell, driven by solutal gradients, forms near the interface. The magnitude of the velocities in this cell increases with time; this causes increasing solute segregation at the liquid/solid interface.

Simpson James E.↗

NASA NTRS1996

Repartitioning of NaCl and Protein Impurities in Lysozyme Crystallization

Nonuniform precipitant and impurity incorporation in protein crystals can cause lattice strain and, thus, possibly decrease the X-ray diffraction resolution. To address this issue, a series of crystallization experiments were carried out, in which initial supersaturation, NaCl concentration, protein purity level and crystallized fraction were varied. Lysozyme and protein impurities, as well as sodium and chloride were independently determined in the initial solution, supernatant and crystals. The segregation coefficients for Na(+) and Cl(-) were found to be independent of supersaturation and NaCl concentration, and decreased with crystallized fraction/crystal size. Numerical evaluation of the extensive body of data, based on a nucleation-growth- repartitioning model, suggests a core of approx. 40 microns in which salt is incorporated in much greater concentrations than during later growth. Small crystals containing higher amounts of incorporated NaCl also had higher protein impurity contents. This suggests that the excess salt is associated with the protein impurities in the core. X-ray topography revealed strain fields in the center of the crystals comparable in size to the inferred core. The growth rates of crystals smaller than 30-40 pm in size were consistently 1.5-2 times lower than those of larger crystals, presumably due to higher chemical potentials in the core.

Vekilov, Peter G.↗

NASA NTRS1999

Effects of G-Jitter on Directional Solidification of a Binary Alloy

A study of directional solidification of a weak binary alloy (specifically, Bi - 1 at% Sn) based on the fixed grid single domain approach is being undertaken. The enthalpy method is used to solve for the temperature field over the computational domain including both the solid and liquid phases; latent heat evolution is treated with the aid of an effective specific heat coefficient. A source term accounting for the release of solute into the liquid during solidification has been incorporated into the solute transport equation. The vorticity-stream function formulation is used to describe thermo-solutal convection in the liquid region. In this paper we present a numerical simulation of g-jitter. A background gravity of 1 microgram has been assumed, and new results for the effects of periodic disturbances over a range of amplitudes and frequencies on solute field and segregation have been presented.

Benjapiyaporn, C.↗

NASA NTRS1999

In-Situ X-Ray Microscopy of Phase and Composition Distributions in Metal Alloys During Solidification

This research applies a state of the art X-ray Transmission Microscope, to image the solidification of metallic or semiconductor alloys in real-time. By employing a hard x-ray source with sub-micron dimensions, resolutions of up to 3 gm can be obtained with magnifications of over 800 X. Specimen growth conditions were optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid inter-face. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. Composition gradients within the specimen cause vafiations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). During this study, the growth of secondary phase fibers and lameilae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Keywords: x-ray, microscope, solidification, microfocus, real-time, microstructure

Kaukler, William F.↗

NASA NTRS1999

Real-Time Investigation of Solidification of Metal Matrix Composites

Casting of metal matrix composites can develop imperfections either as non- uniform distributions of the reinforcement phases or as outright defects such as porosity. The solidification process itself initiates these problems. To identify or rectify the problems, one must be able to detect and to study how they form. Until, recently this was only possible by experiments that employed transparent metal model organic materials with glass beads to simulate the reinforcing phases. Recent results obtained from a Space Shuttle experiment (using transparent materials) will be used to illustrate the fundamental physics that dictates the final distribution of agglomerates in a casting. We have further extended this real time investigation to aluminum alloys using X-ray microscopy. A variety of interface-particle interactions will be discussed and how they alter the final properties of the composite. A demonstration of how a solid-liquid interface is distorted by nearby voids or particles, particle pushing or engulfment by the interface, formations of wormholes, Aggregation of particles, and particle-induced segregation of alloying elements will be presented.

Kaukler, William↗

NASA NTRS1999

Low Temperature Photoluminescence of PVT Grown ZnSe and ZnSeTe

ZnSe and ZnSeTe single crystals were grown by physical vapor transport (PVT) technique horizontally and vertically. The grown ZnSe and ZnSeTe single crystals were characterized by low temperature photoluminescence at 5 to 10 K using the 3.4 eV emission of an argon laser. The intensity of the sharp near band edge defect lines at 2.799, 2.783 eV and the intrinsic free exciton line at 2.802 eV were mapped on various crystal surfaces with different orientations to the gravitational field. The results show the effects of gravity vector orientation on the defect segregation. Comparison of the photoluminescence spectra of the ZeSe crystal before and after annealing in the Zn vapor shows that the 2.783 eV line of ZnSe crystal is related to the zinc vacancy. The photoluminescence spectra of the ternary ZnSeTe crystal were characterized by a single broad band from 2.2 to 2.4 eV, with a Full Width at Half Maximum (FWHM) of about 100 meV. The temperature dependence of the peak position and intensity were determined from 7 to 150 K.

Wang, Ling Jun↗

NASA NTRS1998

The Role of Marangoni Convection for the FZ-Growth of Silicon

Fluctuations of the electrical resistivity due to inhomogeneous dopant distribution are still a serious problem for the industrial processing yield of doped silicon crystals. In the case of silicon floating-zone growth, the main sources of these inhomogeneities are time- dependent flows in the liquid phase during the growth process. Excluding radio frequency (RF) induced convection, buoyancy and thermocapillary (Marangoni) convection are the two natural reasons for fluid flow. Both originate from temperature/concentration gradients in the melt, buoyancy convection through thermal/concentrational volume expansion, and thermocapillary convection through the temperature/concentration dependence of the surface tension. To improve the properties of grown crystals, knowledge of the strength, the characteristic, and the relation of these two flow mechanisms is essential. By the use of microgravity, the effect and the strength of buoyancy (gravity dependent) and thermocapillary (gravity independent) convection can be separated and clarified. Applying magnetic fields, both convective modes can be influenced: fluid flow can either be damped (static magnetic fields) or overlaid by a regular flow regime (rotating magnetic fields). Two complementary approaches have been pursued: Silicon full zones (experiments on the German sounding rockets TEXUS 7, 12, 22, 29, and 36) with the maximum temperature at half of the zone height and silicon half zones (experiments on the Japanese sounding rockets TR-IA4 and 6) with the maximum temperature at the top of the melt. With the full zone arrangement, the intensity and the frequency of the dopant striations could be determined and the critical Marangoni number could be identified. The half zone configuration is suited to classify the flow pattern and to measure the amplitude and the frequency of temperature fluctuations in the melt by inserting thermocouples or temperature sensors into the melt. All experiments have been carried out in monoellipsoid mirror furnaces. Typical zone geometries are approx. 8 to 14 mm in diameter and height. The crystals grown under microgravity are compared to crystals grown in static axial magnetic fields (B<5 tesla) and in transversal rotating magnetic fields (B<7.5 mT / f=50 Hz). Experimental results are completed by 3D numerical simulations: the obtained temperature and concentration distribution in the melt confirm the damping effect of rotating magnetic fields and explain the change in the radial segregation under static magnetic fields.

Dold, P.↗

NASA NTRS1999

Double Diffusive Convection in Materials Processing

A great number of crystals grown in space are plagued by convective motions which contribute to structural flaws. The character of these instabilities is not well understood but is associated with density variations in the presence of residual gravity (g-jitter). As a specific example, past HgCdTe crystal growth space experiments by Lehoczky and co-workers indicate radial compositional asymmetry in the grown crystals. In the case of HgCdTe the rejected component into the melt upon solidification is HgTe which is denser than the melt. The space grown crystals indicate the presence of three dimensional flow with the heavier HgTe-rich material clearly aligned with the residual gravity (0.55-1.55 micro g) vector. This flow stems from double-diffusive convection, namely, thermal and solutal buoyancy driven flow in the melt. The study of double-diffusive convection is multi-faceted and rather vast. In our investigation, we seek to focus on one specific aspect of this discipline that is of direct relevance to materials processing especially crystal growth, namely, the side ways heating regime. This problem has been widely studied, both experimentally and numerically, in the context of solar ponds wherein the system is characterized by a linear salt (solutal) gradient with an imposed lateral temperature gradient. The induced flow instabilities arise from the wide disparity between the fluid thermal diffusivity and the solute diffusivity. The extension of the analysis to practical crystal growth applications has however not been rigorously made and understood. One subtle but important difference in crystal growth systems is the fact that die system solute gradient is non-linear (typically exponential). Besides, the crystal growth problem has the added complexities of solidification, both lateral and longitudinal thermal gradients and segregation phenomena in systems where binary and ternary compounds are being grown. This paper treats the side ways heating problem alone in a model fluid system. Results from detailed numerical calculations, mainly two dimensional are provided. The interactions between a non-linear solute gradient and an imposed transverse thermal gradient are investigated. The buoyancy effects are treated in the traditional Boussinesq approximation and also in a more complete density formulation to address recent concerns of the first approach especially in simulations of the system response in a reduced gravity environment. Detailed flow, temperature and solute field plots along with heat and mass transfer results are presented in the paper. Implications to practical crystal growth systems as discerned from the modeling results are also explored and reported.

Ramachandra, Narayanan↗

NASA NTRS1998

Directional Solidification and Characterization of Hg(0.89) Mn(0.11)Te

Two boules of Hg(0.89)Mn(0.11)Te(MMT) were solidified using the vertical Bridgman-Stockbarger method. Translation rates of 0.09 and 0. 18 microns/s were used. The influence of growth rate on axial compositional homogeneity in the MMT boules was evaluated experimentally by conducting precision density measurements on radial slices taken from each boule. In addition, Plane Front Solidification theory and segregation coefficient (k) data for the Hg(1-x)Mn(x)Te system were used to fit theoretical composition profiles to the measured MMT axial composition profiles. The strong correlation between the measured and calculated MMT axial composition profiles indicates diffusion dominated axial solute redistribution in the boules under the applied growth conditions. The analysis of the MMT axial composition profiles by Plane Front Solidification theory allowed the calculation of the effective diffusion coefficient (D(eff) = 3.5 x l0(exp -5) sq cm/s). The k-values for the Hg(1-x)Mn(x)Te system and the D(sub eff) - value were then used to verify that both boules were solidified under conditions which did not exceed the Constitutional Supercooling Criteria under ideal conditions. Finally, a preliminary examination of the radial compositional variation in each MMT was made using Fourier Transform Infra-Red Spectroscopy (FTIR). The radial homogeneity in the MMT boules was found to be comparable for both translation rates.

Price, M. W.↗

NASA NTRS1999

Control of Meridional Flow in Circular Cylinders by a Travelling Axial Magnetic Field

Convective flow in a Bridgman or float zone configuration significantly affects the interface shape and segregation phenomena. While the primary causative factor for this flow is buoyancy induced convection in an enclosed Bridgman melt, the presence of a free surface gives rise to surface tension driven flows in the floating zone processing of melts. It is of interest to curtail these flows in order to realize near quiescent growth conditions that have shown to result in crystals with good longitudinal and radial homogeneity and thereby of better overall quality. While buoyancy effects can be reduced by careful processing in a low gravity (space) environment, the reduction of Marangoni flows due to surface tension variations is not that straight forward. Attempts have been made with some limited success with the use of external fields to affect the melt thermo-fluid behavior. The use of a static magnetic field that reduces convective contamination through the effects of a non-intrusively induced, dissipative Lorentz force in an electrically conducting melt is one such approach. Experiments have shown that axial fields of the order of 5 Tesla can significantly eliminate convection and yield close to diffusion limited crystal growth conditions. The generation and use of such high magnetic fields require substantial hardware and incur significant costs for its operation. Lately, the use of rotating magnetic fields has been tested in semiconductor crystal growth. The method is fairly well known and commonly used in metal processing but its adaptation to crystal growth of semiconductors is fairly recent. The elegance of the technique rests in its low power requirement (typically 10-20 milli-Tesla at 50-400 Hz) and its efficacy in curtailing deleterious temperature fluctuations in the melt. A rotating magnetic field imposes a rotational force and thereby induces a circulation within the melt that tends to dominate other sporadic convective effects. Thus a known low level of convective flow is introduced into the system. A new novel variation of the Lorentz force mechanism is proposed and investigated in this study. Since one of the desired process conditions in melt crystal growth is the minimization of convective effects, this investigation examines the use of an external field of magnetic origin to counteract existing convective flow within the melt. This is accomplished by utilizing a running or traveling axial magnetic wave in the system. The concept is similar to the use of vibrational means in order to induce streaming flows that oppose buoyant or surface tension driven convection in the system. The rotation direction as well as the magnitude (strength) of this circulation can be easily controlled by external inputs thus affording a direct means of controlling the developing shape of the crystallizing front (interface). The theoretical model of this technique is fully developed and presented in this paper. Results from the solution of the developed governing equations and boundary conditions are also presented. An experimental demonstration of the concept is presented through the suppression of natural convective flow in a mercury column. Implications to crystal growth systems will be fully explored in the final manuscript.

Mazuruk, K.↗