Engineering topics

Regel, Liya L.

Publications and source records attributed to Regel, Liya L..

At least 19 records

NASA NTRS2004

Residual Gas Effects on Detached Solidification in Microgravity

Our long term goal has been to make detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Thus, the objective of the current project was to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. Our focus was on the influence of oxygen on indium antimonide on clean silica ("quartz"). The research was performed by three chemical engineering graduate students, the third of whom will complete his research in the summer of 2005. Originally, we had planned to use a sealed silica cell containing a zirconia electrochemical element to control the oxygen partial pressure. However, zirconia requires an operating temperature above the 530 C melting point of InSb and is difficult to form a gas-tight seal with silica. Thus, we decided instead to flow an oxygen-containing gas through the cell. A special apparatus was designed, built and perfected. A piece of InSb was placed on a horizontal silica plate in a quartz cell. High purity argon, helium or hydrogen-containing gas is passed continuously through the cell while the oxygen concentration in the effluent gas is measured. The shape of the resulting drop was used to determine contact angle and surface tension of Ga-doped and high purity InSb. Oxygen appeared to decrease the contact angle, and definitely did not increase it. The following section gives the background for the research. Section 2 summarizes the results obtained on Ga-doped InSb with relatively high oxygen concentrations. Section 3 describes recent improvements made to the apparatus and methods of analysis. Section 4 gives recent results for high-purity InSb at low oxygen concentrations. Final results will be obtained only this summer (2005). Each section has its own references.

Wilcox, William R.↗

NASA NTRS2003

Microgravity Effects on Materials Processing: A Review

Materials processing in space has been studied both theoretically and experimentally for over 1/4 of a century. In the beginning, we naively spoke of zero gravity, elimination of convection, growth of perfect crystals, and eventual manufacturing in space. All of these appear to have fallen by the wayside. On the other hand, we have learned an unprecedented amount about the influences of gravity on materials processing. We have had many surprises, and not all experimental results have yet been satisfactorily explained. Gravity was found to influence processes that were thought to be gravity-independent. One consequence is that materials processing on earth has often been improved. And it is difficult to imagine how the materials-processing industries could have flourished without the engineers and scientists who received their training by working on microgravity materials processing.

Wilcox, William R.↗

NASA NTRS2003

Improved Crystal Quality By Detached Solidification in Microgravity

Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long term goals have been: (1) To develop a complete understanding of all of the phenomena of detached solidification.; (2) To make it possible to achieve detached solidification reproducibly; (3) To increase crystallographic perfection through detached solidification. We have three major achievements to report here: (1) We obtained a new material balance solution for the Moving Meniscus Model of detached solidification. This solution greatly clarifies the physics as well as the roles of the parameters in the system; (2) We achieved detached solidification of InSb growing on earth in BN-coated ampoules; (3) We performed an extensive series of experiments on freezing water that showed how to form multiple gas bubbles or tubes on the ampoule wall. However, these did not propagate around the wall and lead to fully detached solidification unless the ampoule wall was extremely rough and non-wetted.

Regel, Liya L.↗

NASA NTRS2003

Residual Gas Effects on Detached Solidification in Microgravity

Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long-term goal is to make such detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Detached solidification is more likely when the contact angle for the melt on the ampoule wall is high, i.e. non-wetting. It has been claimed that impurities increase the contact angle. The objective of the current project is to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. We are focusing on determining the influence of oxygen on the contact angle of molten InSb on clean silica ('quartz'), including the advancing and retreating contact angles in addition to the usual equilibrium contact angle. We have created a gas flow system that allows us to control the oxygen partial pressure over a sessile drop of InSb on a horizontal quartz surface. The cell is slowly tilted while videotaping to reveal the contact angles on the two sides of the drop just prior to it rolling down the surface. Thus far, we have learned the following: (1) Molten InSb readily forms an oxide layer in the presence of the trace amounts of oxygen found in high purity argon; (2) This oxide contains a substantial amount of Ga, which presumably is a trace contaminant that is not detectable in the starting material; (3) The addition of 10% hydrogen to the argon gas is sufficient to reduce the oxide and produce a clean drop; (4) An infrared filter must precede the video camera in order to produce a sharp image of the drop for later image analysis; (5) Tilting the surface on which the drop rests causes the two sides of the drop to display different contact angles, reflecting contact line sticking; (6) Vibration strongly accelerates the approach of the drop to its final shape on a horizontal surface by helping to overcome sticking of the contact line; (7) Oscillation of the drop surface due to vibration appears to increase as the surface is inclined from horizontal. Presumably, the angle at which the drop rolls down the surface is also reduced by vibration. This observation is particularly significant, as the meniscus must move along the ampoule wall during detached solidification.

Regel, Liya L.↗

NASA NTRS2003

Improved Crystal Quality by Detached Solidification in Microgravity

The goals of our work on detached solidification have been to: 1) Develop a complete understanding of all of the phenomena of detached solidification; 2) Make it possible to achieve detached solidification reproducibly; and 3) Increase crystallographic perfection through detached solidification. Specifically, we aimed in this project to: 1) Identify a system and develop methods that would allow viewing of the melt surface and convection in the melt during detached solidification in microgravity; 2) Improve understanding of the origination and evolution of detachment through experiments and theoretical treatments; and 3) Achieve detachment on earth. The project resulted in 14 publications, 15 presentations, completion of 2 Ph.D. theses, and completion of 2 M.S. theses. Two additional papers are currently being reviewed for publication. Copies of most of the papers are included as appendices.

Regel, Liya L.↗

NASA NTRS2003

Detached Solidification of InSb on Earth

Detached solidification of lightly gallium-doped indium antimonide was achieved in the laboratory only when the ampoule was coated with hexagonal boron nitride and when the material appeared to be oxide-free. A furnace was constructed with the temperature increasing with height in order to minimize bouyancy-driven convection, so as to maximize transport of segregated dissolved gases into the gap between the growing solid and the ampoule wall. There appeared to be no difference in results with freezing rates of 5 mmh and 10 mm/h. Best results were obtained when the ampoule was backfilled with 20 kPa of Ar-10%H2 prior to sealing. The detached portions were depressed by several pm from adjacent attached regions, were rough, and sometimes had microfacets and steps.

Wang, Jianbin↗

NASA NTRS2003

Improved Crystal Quality by Detached Solidification in Microgravity

The goals of our work on detached solidification have been to: Develop a complete understanding of all of the phenomena of detached solidification; Make it possible to achieve detached solidification reproducibly; Increase crystallographic perfection through detached solidification. Specifically, we aimed in this project to: Identify a system and develop methods that would allow viewing of the melt surface and convection in the melt during detached solidification in microgravity; Improve understanding of the origination and evolution of detachment through experiments and theoretical treatments; Achieve detachment on earth. The project resulted in 14 publications, 15 presentations, completion of 2 Ph.D. theses, and completion of 2 M.S. theses. Two additional papers are currently being reviewed for publication. Copies of most of the papers are attached as appendices. Among the accomplishments are: Achievement of detached solidification of InSb on earth and determination of the conditions favoring detachment on earth. Development of a new method for coating the interior of silica growth ampoules with transparent boron nitride, which yields the high contact angles for semiconductor melts that favor detachment. Development of a new coating for the interior of Pyrex ampoules yielding very high contact angles for water and molten organic compounds. Development of a material-balance model for steady detached solidification that provides greatly improved insight into the process, both in microgravity and on earth. Dimensionless parameters were found that clarify the role of operating conditions and physical properties. The reason for the occurrence of two steady states was clarified, along with their relative stability. Observation of periodic gas tubes during directional solidification of water and organic compounds. Gas bubbles did not propagate around the periphery to yield full detachment. Failure to obtain detachment is attributed to the ready plastic deformation of these materials, so that the frozen material continues to adhere to the ampoule wall during cooling.

Regel, Liya L.↗

NASA NTRS2003

Inexpensive Method for Coating the Interior of Silica Growth Ampoules with Pyrolytic Boron Nitride

An inexpensive method was developed for coating the interior of silica ampoules with hexagonal boron nitride. An aqueous solution of boric acid was used to coat the ampoule prior to drying in a vacuum at 200 C. This coating was converted to transparent boron nitride by heating in ammonia at 1000 C. Coated ampoules were used to achieve detached solidification of indium antimonide on earth.

Wang, Jianbin↗

NASA NTRS2000

Influence of Contact Angle, Growth Angle and Melt Surface Tension on Detached Solidification of InSb

We extended the previous analysis of detached solidification of InSb based on the moving meniscus model. We found that for steady detached solidification to occur in a sealed ampoule in zero gravity, it is necessary for the growth angle to exceed a critical value, the contact angle for the melt on the ampoule wall to exceed a critical value, and the melt-gas surface tension to be below a critical value. These critical values would depend on the material properties and the growth parameters. For the conditions examined here, the sum of the growth angle and the contact angle must exceed approximately 130, which is significantly less than required if both ends of the ampoule are open.

Wang, Yazhen↗

NASA NTRS1999

Improved Crystal Quality by Detached Solidification in Microgravity

Directional solidification in microgravity has often led to ingots that grew with little or no contact with the ampoule wall. When this occurred, crystallographic perfection was usually greatly improved -- often by several orders of magnitude. Unfortunately, until recently the true mechanisms underlying detached solidification were unknown. As a consequence, flight experiments yielded erratic results. Within the past four years, we have developed a new theoretical model that explains many of the flight results. This model gives rise to predictions of the conditions required to yield detached solidification, both in microgravity and on earth. A discussion of models of detachment, the meniscus models and results of theoretical modeling, and future plans are presented.

Regel, Liya L.↗

NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

The long term goal of this project is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. Prior experimental results on the influence of microgravity on the microstructure of fibrous eutectics have been contradictory. Theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in the melt sufficiently to cause a measurable change in microstructure when the eutectic grows at minimum supercooling. Currently, there are four other hypotheses that might explain the observed changes in microstructure of fibrous eutectics caused by convection: (1) Disturbance of the concentration boundary layer arising from an off-eutectic melt composition and growth at the extremum; (2) Disturbance of the concentration boundary layer of a habit-modifying impurity; (3) Disturbance of the concentration boundary layer arising from an off-eutectic interfacial composition due to non-extremum growth; and (4) A fluctuating freezing rate combined with differences in the kinetics of fiber termination and fiber formation. We favor the last of these hypotheses. Thus, the primary objective of the present grant is to determine experimentally and theoretically the influence of a periodically varying freezing rate on eutectic solidification. A secondary objective is to determine the influence of convection on the microstructure of at least one other eutectic alloy that might be suitable for flight experiments.

Wilcox, William R.↗

NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the projects in the present grant is to test hypotheses for the reported influence of microgravity on the microstructure of eutectics. The prior experimental results on the influence of microgravity on the microstructure of eutectics have been contradictory. With lamellar eutectics, microgravity had a negligible effect on the microstructure. Microgravity experiments with fibrous eutectics sometimes showed a finer microstructure and sometimes a coarser microstructure. Most research has been done on the MnBi/Bi rod-like eutectic. Larson and Pirich obtained a two-fold finer microstructure both from microgravity and by use of a magnetic field to quench buoyancy-driven convection. Smith, on the other hand, observed no change in microgravity. Prior theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in front of a growing eutectic sufficiently to cause a measurable change in microstructure. We assumed that the bulk melt was at the eutectic composition and that freezing occurred at the extremum, i.e. with minimum total undercooling at the freezing interface. There have been four hypotheses attempting to explain the observed changes in microstructure of fibrous eutectics caused by convection: I .A fluctuating freezing rate, combined with unequal kinetics for fiber termination and branching. 2. Off-eutectic composition, either in the bulk melt due to an off-eutectic feed or at the freezing interface because of departure from the extremum condition. 3. Presence of a strong habit modifying impurity whose concentration at the freezing interface would be altered by convection. At the beginning of the present grant, we favored the first of these hypotheses and set out to test it both experimentally and theoretically. We planned the following approaches: I .Pass electric current pulses through the MnBi/Bi eutectic during directional solidification in order to produce an oscillatory freezing rate. 2. Directionally solidify the MnBi/Bi eutectic on Mir using the QUELD II gradient freeze furnace developed by Professor Smith at Queen's University. 3. Select another fibrous eutectic system for investigation using the Accelerated Crucible Rotation Technique to introduce convection. 4. Develop theoretical models for eutectic solidification with an oscillatory freezing rate. Because of the problems with Mir, we substituted ground-based experiments at Queen's University with QUELD II vertical and horizontal, with and without vibration of the furnace. The Al-Si system was chosen for the ACRT experiments. Three related approaches were used to model eutectic solidification with an oscillatory freezing rate. A sharp interface model was used to calculate composition oscillations at the freezing interface in response to imposed freezing rate oscillations.

Wilcox. William R.↗

NASA NTRS1998

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the present projects is to test hypotheses for the reported influence of microgravity on the microstructure of three fibrous eutectics (MnBi-Bi, InSb-NiSb, Al3Ni-Al). A secondary objective is to determine the influence of convection on the microstructure of other eutectic alloys. Two doctoral students and a masters student supported as a teaching assistant were recruited for this research. Techniques were developed for directional solidification of MnBi-Bi eutectics with periodic application of current pulses to produce an oscillatory freezing rate. Image analysis techniques were developed to obtain the variation in MnBi fiber spacing, which was found to be normally distributed. The mean and standard deviation of fiber spacing were obtained for several freezing conditions. Eighteen ampoules were prepared for use in the gradient freeze furnace QUELD developed at Queen's University for use in microgravity. Nine of these ampoules will be solidified soon at Queen's in a ground-based model. We hope to solidify the other nine in the QUELD that is mounted on the Canadian Microgravity Isolation Mount on MIR. Techniques are being developed for directional solidification of the Al-Si eutectic at different freezing rates, with and without application of accelerated crucible rotation to induce convection. For the first time, theoretical methods are being developed to analyze eutectic solidification with an oscillatory freezing rate. In a classical sharp-interface model, we found that an oscillatory freezing rate increases the deviation of the average interfacial composition from the eutectic, and increases the undercooling of the two phases by different amounts. This would be expected to change the volume fraction solidifying and the fiber spacing. Because of difficulties in tracking the freezing interfaces of the two solid phases, a phase-field model is also being developed. A paper demonstrating application of phase field methods to periodic structures has been submitted for publication.

Wilcox, William R.↗

NASA NTRS1997

Modeling of Detached Solidification

Our long term goal is to develop techniques to achieve detached solidification reliably and reproducibly, in order to produce crystals with fewer defects. To achieve this goal it is necessary to understand thoroughly the physics of detached solidification. It was the primary objective of the current project to make progress toward this complete understanding. 'Me products of this grant are attached. These include 4 papers and a preliminary survey of the observations of detached solidification in space. We have successfully modeled steady state detached solidification, examined the stability of detachment, and determined the influence of buoyancy-driven convection under different conditions. Directional solidification in microgravity has often led to ingots that grew with little or no contact with the ampoule wall. When this occurred, crystallographic perfection was usually greatly improved -- often by several orders of magnitude. Indeed, under the Soviet microgravity program the major objective was to achieve detached solidification with its resulting improvement in perfection and properties. Unfortunately, until recently the true mechanisms underlying detached solidification were unknown. As a consequence, flight experiments yielded erratic results. Within the past three years, we have developed a new theoretical model that explains many of the flight results. This model gives rise to predictions of the conditions required to yield detached solidification.

Regel, Liya L.↗

NASA NTRS1994

Modelling directional solidification

This grant, NAG8-831, was a continuation of a previous grant, NAG8-541. The long range goal of this program has been to develop an improved understanding of phenomena of importance to directional solidification, in order to enable explanation and prediction of differences in behavior between solidification on Earth and in space. Emphasis in the recently completed grant was on determining the influence of perturbations on directional solidification of InSb and InSb-GaSb alloys. In particular, the objective was to determine the influence of spin-up/spin-down (ACRT), electric current pulses and vibrations on compositional homogeneity and grain size.

Wilcox, William R.↗

NASA NTRS1994

Influence of convection on microstructure

The primary motivation for this research was to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Four primary hypotheses were to be tested under this current grant: (1) A fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment. (2) An interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment. (3) The Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results. (4) The microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. These hypotheses were tested. It was concluded that none of these can explain the Grumman flight results. Experiments also were performed on the influence of current pulses on MnBi-Bi microstructure. A thorough review was made of all experimental results on the influence of convection on the fiber spacing in rod eutectics, including results from solidification in space or at high gravity, and use of mechanical stirring or a magnetic field. Contradictory results were noted. The predictions of models for convective influences were compared with the experimental results. Vigorous mechanical stirring appears to coarsen the microstructure by altering the concentration field in front of the freezing interface. Gentle convection is believed to alter the microstructure of a fibrous eutectic only when it causes a fluctuating freezing rate with a system for which the kinetics of fiber branching differs from that for fiber termination. These fluctuations may cause the microstructure to coarsen or to become finer, depending on the relative kinetics of these processes. The microstructure of lamellar eutectics is less sensitive to freezing rate fluctuations and to gentle convection.

Wilcox, William R.↗

NASA NTRS1993

Centrifuge in space fluid flow visualization experiment

A prototype flow visualization system is constructed to examine buoyancy driven flows during centrifugation in space. An axial density gradient is formed by imposing a thermal gradient between the two ends of the test cell. Numerical computations for this geometry showed that the Prandtl number plays a limited part in determining the flow.

Arnold, William A.↗

NASA NTRS1992

Modelling Directional Solidification

The long range goal of this program has been to develop an improved understanding of phenomena of importance to directional solidification, in order to enable explanation and prediction of differences in behavior between solidification on Earth and in space. Current emphasis is on determining the influence of perturbations on directional solidification.

Wilcox, William R.↗