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At least 289 records · Page 16

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.↗

Development of Advanced Multizone Facilities for Microgravity Processing

NASA has been interested in experimental ground based study to investigate the fundamental processes involved in phase transformation processes during growth of metallic, nonmetallic and electronic materials. Solidification, vapor growth and solution growth techniques of growing crystals are of special interest because of the inherent importance of convection in the nutrient solution. Convection enhances the mass transport through the nutrient and results in faster growth rates. Availability of low gravity environment of space has provided scientists a new variable to control the extent of convection and thus isolate the diffusive phenomena for their better understanding. The thermal gradient at the liquid-solid interface is determined by the alloy characteristics, the hot zone temperature, cold zone temperature and the width of the insulating zone. The thermal profiles get established by the existing material and geometrical constraints of the experimental set up. The major effort under this research was devoted to designing a programmable furnace which can be used to obtain thermal profiles along the length of the sample as per the demands of the scientists. The furnace did not have active cooling of the zones. Only active heating and passive cooling were utilized.

Source record↗

Study of Magnetic Damping Effect on Convection and Solidification Under G-Jitter Conditions

As shown by NASA resources dedicated to measuring residual gravity (SAMS and OARE systems), g-jitter is a critical issue affecting space experiments on solidification processing of materials. This study aims to provide, through extensive numerical simulations and ground based experiments, an assessment of the use of magnetic fields in combination with microgravity to reduce the g-jitter induced convective flows in space processing systems. We have so far completed asymptotic analyses based on the analytical solutions for g-jitter driven flow and magnetic field damping effects for a simple one-dimensional parallel plate configuration, and developed both 2-D and 3-D numerical models for g-jitter driven flows in simple solidification systems with and without presence of an applied magnetic field. Numerical models have been checked with the analytical solutions and have been applied to simulate the convective flows and mass transfer using both synthetic g-jitter functions and the g-jitter data taken from space flight. Some useful findings have been obtained from the analyses and the modeling results. Some key points may be summarized as follows: (1) the amplitude of the oscillating velocity decreases at a rate inversely proportional to the g-jitter frequency and with an increase in the applied magnetic field; (2) the induced flow approximately oscillates at the same frequency as the affecting g-jitter, but out of a phase angle; (3) the phase angle is a complicated function of geometry, applied magnetic field, temperature gradient and frequency; (4) g-jitter driven flows exhibit a complex fluid flow pattern evolving in time; (5) the damping effect is more effective for low frequency flows; and (6) the applied magnetic field helps to reduce the variation of solutal distribution along the solid-liquid interface. Work in progress includes numerical simulations and ground-based measurements. Both 2-D and 3-D numerical simulations are being continued to obtain further information on g-jitter driven flows and magnetic field effects. A physical model for ground-based measurements is completed and some measurements of the oscillating convection are being taken on the physical model. The comparison of the measurements with numerical simulations is in progress. Additional work planned in the project will also involve extending the 2-D numerical model to include the solidification phenomena with the presence of both g-jitter and magnetic fields.

Li, Ben Q.↗

Potential Flow Interactions With Directional Solidification

The effect of convective melt motion on the growth of morphological instabilities in crystal growth has been the focus of many studies in the past decade. While most of the efforts have been directed towards investigating the linear stability aspects, relatively little attention has been devoted to experimental and numerical studies. In a pure morphological case, when there is no flow, morphological changes in the solid-liquid interface are governed by heat conduction and solute distribution. Under the influence of a convective motion, both heat and solute are redistributed, thereby affecting the intrinsic morphological phenomenon. The overall effect of the convective motion could be either stabilizing or destabilizing. Recent investigations have predicted stabilization by a flow parallel to the interface. In the case of non-parallel flows, e.g., stagnation point flow, Brattkus and Davis have found a new flow-induced morphological instability that occurs at long wavelengths and also consists of waves propagating against the flow. Other studies have addressed the nonlinear aspects (Konstantinos and Brown, Wollkind and Segel)). In contrast to the earlier studies, our present investigation focuses on the effects of the potential flow fields typically encountered in Hele-Shaw cells. Such a Hele-Shaw cell can simulate a gravity-free environment in the sense that buoyancy-driven convection is largely suppressed, and hence negligible. Our interest lies both in analyzing the linear stability of the solidification process in the presence of potential flow fields, as well as in performing high-accuracy nonlinear simulations. Linear stability analysis can be performed for the flow configuration mentioned above. It is observed that a parallel potential flow is stabilizing and gives rise to waves traveling downstream. We have built a highly accurate numerical scheme which is validated at small amplitudes by comparing with the analytically predicted results for the pure morphological case. We have been able to observe nonlinear effects at larger times. Preliminary results for the case when flow is imposed also provide good validation at small amplitudes.

Buddhavarapu, Sudhir S.↗

Flight Experiment to Study Double-Diffusive Instabilities in Silver-Doped Lead Bromide Crystals

A detailed study on the effect of convection on crystal quality was carried out by growing lead bromide crystals in transparent Bridgman furnace. Direct observations were made on the solid-liquid interface and a new kind of instability was observed. This could be explained on the basis of toroidal flow in the AgBr-doped lead bromide sample. With the increasing translation velocity, the interface changed from flat to depressed, and then formed a cavity in the center of the growth tube. The crystal grown at the lowest thermal Rayleigh number showed the highest quality and crystal grown at the largest thermal Rayleigh number showed the worst quality. Numerical studies were carried out to provide a framework for interpreting the observed convective and morphological instabilities, and to determine the critical (limiting) concentration of dopant for a particular growth velocity and gravity level. Theoretical instability diagrams were compared with data obtained from the experimental studies. These studies provided basic data on convective behavior in doped lead bromide crystals grown by the commercially important Bridgman process.

Singh, N. B.↗

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.↗

Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

Ritter, T. M.↗

Microstructural Development of Directionally Solidified Hg(1-x)Zn(x)Se Alloys

Hg(1-x)Zn(x)Se alloys have been studied as an alternative to HgCdTe for the detection of electromagnetic radiation, because the shorter ZnSe and HgSe bonds were predicted to improve lattice stability. Previous studies showed that optical properties were stable with time and that the microhardness was higher than for HgTe based alloys. However, for this material to be commercially viable, compositional variations must be reduced, and the distribution of defects induced by the growth process must be understood. The basic structural properties of bulk materials were characterized, and dislocation etch pit densities were measured to determine whether the addition of Zn to the HgSe lattice reduced the potential for dislocation formation. Hg(0.9)Zn(0.1)Se alloys were directionally solidified using a modified Bridgman-Stockbarger method and in an applied magnetic field. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. The combination of a convex liquid-solid interface shape and a method for reduced wetting produced boules that were a single crystal after reaching full diameter. Observed surface features indicated ampoule wetting could be eliminated using a graphite getter. Microstructural characteristics were greatly improved over HgCdTe alloys, In six boules, a total of only one twin was observed, and no inclusions were found. A method for polishing and producing dislocation etch pits was developed for these alloys, revealing dislocation etch pit densities one to two orders of magnitude less than HgTe based alloys. A kink in the thermal profile during processing of one boule generated more dislocations than did lattice mismatch due to compositional variations. The results of this investigation indicate this alloy has improved microstructural properties and resistance to dislocation formation compared with similar II-VI alloys, and should be further investigated for the detection of electromagnetic radiation.

Cobb, S. D.↗

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.↗

Microstructural Development of Directionally Solidified Hg(1-x)Zn(x)Se Alloys

Hg(1-x)Zn(x)Se alloys have been studied as an alternative to Hg(1-x)Cd(x)Te for the detection of electromagnetic radiation, because the shorter ZnSe and HgSe bonds have been predicted to improve lattice stability. Several ingots with x = 0.1 were directionally solidified using a modified Bridgman-Stockbarger method; one was grown in an applied magnetic field, which greatly reduced radial compositional variations. A method was developed to reduce wetting. This, combined with the convex liquid-solid interface shape, produced boules that were single crystalline after growing about 3.5 cm. Observed surface features indicated ampoule wetting was eliminated using a graphite getter. Microstructural characteristics were greatly improved over HgCdTe alloys. In six boules, a total of only one twin was observed. A method for polishing and producing dislocation etch pits was developed for these alloys, revealing dislocation etch pit densities one to two orders of magnitude less than HgTe-based alloys. A kink in the thermal profile during processing of one boule generated more dislocations than did lattice mismatch due to compositional variations. This alloy has improved microstructural properties and resistance to dislocation formation compared with similar II-VI alloys.

Cobb, S. D.↗

Particle Engulfment and Pushing Micro-Gravity Experiments and Mathematical Modeling

The phenomenon of interaction of particles with solid-liquid interfaces that results in particle engulfment or pushing (PEP) has been Studied since mid 1960's. While the original interest stemmed from geology applications (frost heaving in soil), it was recognized early that understanding particle behavior at solidifying interfaces mi ht yield 9 practical benefits in other fields. In metallurgical applications the issue is the location of particles with respect to grain boundaries at the end of solidification. Considerable amount of experimental and theoretical research was lately focused on applications to metal matrix composites produced by casting; or spray forming techniques. Another application of PEP is in the growing of Y1Ba2CU3O7-delta(123) superconductor crystals from an undercooled liquid. The oxide melt contains Y2Ba1CU1O5 (211) precipitates, which act as flux pinning sites. The paper presents results of PEP micro-gravity research performed by the authors on two shuttle missions using metallic and polymeric materials. In addition. a discussion on the theoretical aspects of the physics of PEP is offered. Analytical and numerical models for planar solidification interfaces developed by the authors are used to explain the experimental results. Shortcomings of steady-state models are emphasized. A numerical model that includes the effect of the solutal field and of natural convection is introduced. A discussion of phenomena associated with dendritic solidification based on experimental observations is also offered. A mechanism of engulfment is proposed.

Stefanescu, Doru M.↗

Model of ASTM Flammability Test in Microgravity: Iron Rods

There is extensive qualitative results from burning metallic materials in a NASA/ASTM flammability test system in normal gravity. However, this data was shown to be inconclusive for applications involving oxygen-enriched atmospheres under microgravity conditions by conducting tests using the 2.2-second Lewis Research Center (LeRC) Drop Tower. Data from neither type of test has been reduced to fundamental kinetic and dynamic systems parameters. This paper reports the initial model analysis for burning iron rods under microgravity conditions using data obtained at the LERC tower and modeling the burning system after ignition. Under the conditions of the test the burning mass regresses up the rod to be detached upon deceleration at the end of the drop. The model describes the burning system as a semi-batch, well-mixed reactor with product accumulation only. This model is consistent with the 2.0-second duration of the test. Transient temperature and pressure measurements are made on the chamber volume. The rod solid-liquid interface melting rate is obtained from film records. The model consists of a set of 17 non-linear, first-order differential equations which are solved using MATLAB. This analysis confirms that a first-order rate, in oxygen concentration, is consistent for the iron-oxygen kinetic reaction. An apparent activation energy of 246.8 kJ/mol is consistent for this model.

Steinberg, Theodore A↗

Study of Magnetic Damping Effect on Convection and Solidification Under G-Jitter Conditions

As shown in space flight experiments, g-jitter is a critical issue affecting solidification processing of materials in microgravity. This study aims to provide, through extensive numerical simulations and ground based experiments, an assessment of the use of magnetic fields in combination with microgravity to reduce the g-jitter induced convective flows in space processing systems. Analytical solutions and 2-D and 3-D numerical models for g-jitter driven flows in simple solidification systems with and without the presence of an applied magnetic field have been developed and extensive analyses were carried out. A physical model was also constructed and PIV measurements compared reasonably well with predictions from numerical models. Some key points may be summarized as follows: (1) the amplitude of the oscillating velocity decreases at a rate inversely proportional to the g-jitter frequency and with an increase in the applied magnetic field; (2) the induced flow oscillates at approximately the same frequency as the affecting g-jitter, but out of a phase angle; (3) the phase angle is a complicated function of geometry, applied magnetic field, temperature gradient and frequency; (4) g-jitter driven flows exhibit a complex fluid flow pattern evolving in time; (5) the damping effect is more effective for low frequency flows; and (6) the applied magnetic field helps to reduce the variation of solutal distribution along the solid-liquid interface. Work in progress includes developing numerical models for solidification phenomena with the presence of both g-jitter and magnetic fields and developing a ground-based physical model to verify numerical predictions.

Li, Ben Q.↗

Space- and Ground-Based Crystal Growth Using a Baffle (CGB)

The composition of semiconductor crystals produced in space by conventional melt-growth processes (directional solidification and zone melting) is affected by minute levels of residual micro-acceleration, which causes natural convection. The residual acceleration has random magnitude, direction and frequency. Therefore, the velocity field in the melt is apriori unpredictable. As a result, the composition of the crystals grown in space can not be predicted and reproduced. The method for directional solidification with a submerged heater or a baffle was developed under NASA sponsorship. The disk-shaped baffle acts as a partition, creating a small melt zone at the solid-liquid interface. As a result, in ground based experiment the level of buoyancy-driven convection at the interface is significantly reduced. In several experiments with Te-doped GaSb, nearly diffusion controlled segregation was achieved.

Ostrogorsky, A. G.↗

Float Zone Growth of Alloy Semiconductor Crystals: Influence of Solutocapillary Convection

Growth techniques with large free melt surfaces are affected by convective flows induced by gradients of the surface tension. In the case of dilute semiconductor alloys (in our case: germanium-silicon), the impact of solutocapillary convection (due to the concentration dependence of the surface tension) has to be taken into account in addition to the "normal" thermocapillary convection (due to the temperature dependence of the surface tension). Theoretical considerations, based on experimental temperature profiles, growth geometry, segregation coefficient, and measured values for the temperature and concentration coefficients of the surface tension, lead to the conclusion that for the germanium rich side of the Ge(1-x)Si(x) system, the contribution of solutocapillary convection is, at least in front of the solid-liquid interface, the dominant factor. It results in an additional flow roll with a flow direction opposite to the thermocapillary flow, similar to the ones reported for metal alloys or high Prandtl-number fluids.

Dold, P.↗

Measurement of Microscopic Growth Rates in Float-Zone Silicon Crystals

Time dependent convective flows during crystal growth of doped semiconductors lead to fluctuations of the composition, so called dopant striations. In general, it is difficult to decide which is the main mechanism for the generation of these striations, it might be either the fluctuation of the concentration field in the melt and the extent of the solute boundary layer ahead of the solid-liquid interface or a variation of the growth velocity. Direct access to the concentration field is rather complicated to achieve, especially considering the high process temperature and the chemical activity of liquid silicon. The contribution of growth rate fluctuations to the formation of compositional fluctuations can be determined by measuring microscopic growth rates. The classical method of current pulses requires electrical feed-throughs and good electrical contacts, both are critical issues for the growth of high purity silicon crystals. Using a radiation based heating system, the heating power can be modulated very fast and effectively. We added to the normal heater power a sinusoidal off-set in the frequency range of 1 to 10 Hz, generating a narrow spaced weak rippling in the grown crystals which are superposed to the dopant striations caused by natural and by thermocapillary convection. The pulling speed was varied between 1 and 4mm/min. The microscope images of etched crystals slices have been analyzed by peak-search algorithms (measuring the spacing between each artificially induced marker) and by FFT. Performing growth experiments under a time-dependent flow regime, fluctuations of the microscopic growth velocity of Delta(v)/v(sub average) up to 50% have been measured. Damping the time-dependent convection by the use of an axial, static magnetic field of 500mT, the microscopic growth rate became constant within the resolution limit of this method. The results will be discussed using analytical methods for the calculation of microscopic growth velocity and by comparing them with measurements of temperature fluctuations in the melt during growth experiments itself.

Dold, P.↗

Particle Engulfment and Pushing (PEP): Past Micro-Gravity Experiments and Future Experimental Plan on the International Space Station (ISS)

The interaction of an insoluble particle with a growing solid-liquid interface (SLI) has been a subject of investigation for the four decades. For a metallurgist or a material scientist understanding the fundamental physics of such an interaction is relevant for applications that include distribution of reinforcement particles in metal matrix composites, inclusion management in castings, and distribution of Y2Ba1Cu1O5 (211) precipitates (flux pinning sites) in Y1Ba2Cu3O7 (123) superconducting crystals. The same physics is also applicable to other areas including geological applications (frost heaving in soils) and preservation of biological cells. Experimentally this interaction can be quantified in terms of a critical growth velocity, Vcr, of the SLI below which particles are pushed ahead of the advancing interface, and above which the particles are engulfed. Past experimental evidence suggests that this Vcr is an inverse function of the particle radius, R. In order to isolate the fundamental physics that governs such a relationship it is necessary to minimize natural convection at the SLI that is inherent in ground based experiments. Hence for the purpose of producing benchmark data (Vcr vs. R) PEP is a natural candidate for micro-gravity experimentation. Accordingly, experiments with pure Al containing a dispersion of ZrO2 particles and an organic analogue, succinonitrile (SCN) containing polystyrene particles have been performed on the LMS and USMP-4 mission respectively. In this paper we will summarize the experimental data that was obtained during these two micro-gravity missions and show that the results differ compared to terrestrial experiments. We will also discuss the basic elements of our analytical and numerical model and present a comparison of the predictions of these models against micro-gravity experimental data. Finally. we will discuss our future experimental plan that includes the ISS glovebox and MSRRl.

Sen, Subhayu↗

Microgravity Science Glovebox Investigations SUBSA

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is a Microgravity Science Glovebox Investigation manifested for the UF2 flight, on the U.S. Orbiter 111, to the International Space Station (ISS). SUBSA complements the "parent" flight investigation CG13 (Space-and Groundbased Crystal Growth Using a Baffle). During directional solidification, the disk-shaped baffle acts as a partition, creating a small melt zone at the solid-liquid interface. As a result, the level of buoyancy-driven convection at the interface is significantly reduced. In space, the baffle will reduce convection driven by residual micro acceleration. The baffle reduces the Rayleigh number (Ra) of the melt by a factor of 103. The combined effect of the baffle and microgravity will yield a reduction in Ra by a factor of 107 to 109 approaching effectively the acceleration conditions in "nanogravity". The results of ground based tests and numerical modeling will be presented. The furnace for directional solidification (flight hardware and the ground unit) was developed by Tec-Masters Inc. The flight ampoules were produced jointly at Rensselaer, Tec-Masters Inc. and Crystallod Inc.

Ostrogorsky, A.↗