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Fripp, A. L.

Publications and source records attributed to Fripp, A. L..

At least 19 records

Growth of Compound Semiconductors in a Low Gravity Environment: Microgravity Growth of PbSnTe

The growth of the alloy compound semiconductor lead tin telluride (PbSnTe) was chosen for a microgravity flight experiment in the Advanced Automated Directional Solidification Furnace (AADSF), on the United States Microgravity Payload-3 (USNP-3) in February, 1996 and on USNW- 4 in November, 1997. The objective of these experiments was to determine the effect of the reduction in convection, during the growth process, brought about by the microgravity environment. The properties of devices made from PbSnTe, an alloy of PbTe and SnTe, are dependent on the ratio of the elemental components in the starting crystal. Compositional uniformity in the crystal is only obtained if there is no significant mixing in the liquid during growth. The technological importance of PbSnTe lies in its band gap versus composition diagram which has a zero energy crossing at approximately 40% SnTe. This facilitates the construction of long wavelength (greater than 6 gm) infrared detectors and lasers. The properties and utilization of PbSnTe are the subject of other papers. 1,2 PbSnTe is also interesting from a purely scientific point of view. It is, potentially, both solutally and thermally unstable due to the temperature and density gradients present during growth. Density gradients, through thermal expansion, are imposed in directional solidification because temperature gradients are required to extract heat. Solutal gradients occur in directional solidification of alloys due to segregation at the interface. Usually the gradients vary with both experiment design and inherent materials properties. In a simplified one dimensional analysis with the growth axis parallel to the gravity vector, only one of the two instabilities work at a time. During growth, the temperature in the liquid increases ahead of the interface. Therefore the density, due to thermal expansion, is decreasing in that direction. However, the phase diagram shows that the lighter SnTe is preferentially rejected at the interface. This causes the liquid density to increase with distance away from the interface.

Fripp, A. L.

The Effect of Microgravity Direction on the Growth of PbSnTe

The Space Shuttle Columbia was launched as STS-75 at 2018 GMT (Greenwich Mean Time) on February 22, 1996. One of the two major experiment packages was the Third United States Microgravity Payload (USMP-3), and one of the principal instruments on the USMP was the Advanced Automated Directional Solidification Furnace (AADSF). The AADSF is a multizone directional solidification furnace, and at the time of the USMP-3 flight was capable of processing only one sample per Shuttle mission which, for that flight, was a lead tin telluride (PbSnTe) crystal growth experiment. In the one year since the flight experiment the sample has been retrieved from the spacecraft and analysis has begun. After presenting introductory material on why PbSnTe was chosen as a test material, why microgravity processing was expected to produce desired results, and what we expected to find in conducting these tests, this report discusses the results to date which are far from complete.

Fripp, A. L.

Growth rates and interface shapes in germanium and lead tin telluride observed in-situ, real-time in vertical Bridgman furnaces

Using the advanced technology developed to visualize the melt-solid interface in low Prandtl number materials, crystal growth rates and interface shapes have been measured in germanium and lead tin telluride semiconductors grown in vertical Bridgman furnaces. The experimental importance of using in-situ, real time observations to determine interface shapes, to measure crystal growth rates, and to improve furnace and ampoule designs is demonstrated. The interface shapes observed in-situ, in real-time were verified by quenching and mechanically induced interface demarcation, and they were also confirmed using machined models to ascertain the absence of geometric distortions. Interface shapes depended upon the interface position in the furnace insulation zone, varied with the nature of the crystal being grown, and were dependent on the extent of transition zones at the ends of the ampoule. Actual growth rates varied significantly from the constant translation rate in response to the thermophysical properties of the crystal and its melt and the thermal conditions existing in the furnace at the interface. In the elemental semiconductor germanium the observed rates of crystal growth exceeded the imposed translation rate, but in the compound semiconductor lead tin telluride the observed rates of growth were less than the translation rate. Finally, the extent of ampoule thermal loading influenced the interface positions, the shapes, and the growth rates.

Barber, P. G.

Convection of tin in a Bridgman system. I - Flow characterization by effective diffusivity measurements

An electrochemical titration method was used to investigate the dynamic states in a cylindrical layer of convecting tin. The liquid tin was contained in a cell, with curved boundaries made of quartz and flat boundaries made of a solid state electrolyte - yttria-stabilized zirconia (YSZ). The electrolyte acted as a window through which a trace amount of oxygen could be pumped in or out by the application of a constant voltage. The concentration at the YSZ interface was monitored by operating the electrochemical cell in the galvanic mode. Experimentally determined effective diffusivities of oxygen were compared with the molecular diffusivity. Dynamic states in the convective flow were thus inferred. Temperature measurements were simultaneously made in order to identify the onset of oscillations from a steady convective regime. The experiments were conducted for two different aspect ratios for various imposed temperature gradients and two different orientations with respect to gravity. Transcritical states were identified and comparison to two-dimensional numerical models were made.

Sears, B.

Convection of tin in a Bridgman system. II - An electrochemical method for detecting flow regimes

An ampoule was designed in order to obtain local flow behavior of the flow fields for convection of tin in a vertical Bridgman configuration. Multiple electrochemical cells were located along the periphery of the ampoule. Oxygen was titrated into the ampoule at one of the cell locations using a potentiostat and the concentration of oxygen was monitored at the other cell locations by operating the cells in a galvanic mode. Onset of oscillations were detected by means of thermocouples. We conclude that the flows are generally three dimensional for an aspect ratio of 5. Results on oscillations concurred with those of earlier workers. Suggestions for improved designs were made.

Sears, B.

Thermal calibration and analysis of a Bridgman flight furnace

A combination of computer modeling and experimental measurements is proposed which permits the calibration of the temperature profile for a spacecraft flight furnace. The Fluent code based on the finite difference method uses the furnace set-point temperatures as boundary conditions to model a Bridgman directional solidification furnace. Experimental measurements are employed as a comparison for the numerical analysis, and the radial gradients and wall temperatures are selected when the calculated values are sufficiently close to those from measurements. The calculations are found to agree with experimental data, and some results of the modeling are given which relate to specific furnace parameters. The CFD approach facilitates the transposition of furnace calibration to microgravitational operation in addition to providing precise initial radial temperature gradients and furnace-wall temperatures.

Knuteson, D. J.

Temperature profiles in high gradient furnaces

Accurate temperature measurement of the furnace environment is very important in both the science and technology of crystal growth as well as many other materials processing operations. A high degree of both accuracy and precision is acutely needed in the directional solidification of compound semiconductors in which the temperature profiles control the freezing isotherm which, in turn, affects the composition of the growth with a concomitant feedback perturbation on the temperature profile. Directional solidification requires a furnace configuration that will transport heat through the sample being grown. A common growth procedure is the Bridgman Stockbarger technique which basically consists of a hot zone and a cold zone separated by an insulator. In a normal growth procedure the material, contained in an ampoule, is melted in the hot zone and is then moved relative to the furnace toward the cold zone and solidification occurs in the insulated region. Since the primary path of heat between the hot and cold zones is through the sample, both axial and radial temperature gradients exist in the region of the growth interface. There is a need to know the temperature profile of the growth furnace with the crystal that is to be grown as the thermal load. However it is usually not feasible to insert thermocouples inside an ampoule and thermocouples attached to the outside wall of the ampoule have both a thermal and a mechanical contact problem as well as a view angle problem. The objective is to present a technique of calibrating a furnace with a thermal load that closely matches the sample to be grown and to describe procedures that circumvent both the thermal and mechanical contact problems.

Fripp, A. L.

Effects of supercooling in the initial solidification of PbTe-SnTe solid solutions

Deviations from compositions anticipated by the thermal equilibrium phase diagram have been observed in Bridgman-grown crystals of Pb(1-x)Sn(x)Te, in the first to freeze region of the boule. A set of experiments were conducted to determine the extent of thermal supercooling of Pb(1-x)Sn(x)Te in a Bridgman-like configuration. The results of the compositional profiles and the supercooling measurements are consistent with a diffusionless transformation occurring at the onset of solidification, and the length of uncontrolled growth is inversely related to the temperature gradient of the furnace.

Fripp, A. L.

Preparation for microgravity science investigation of compound semiconductor crystal growth

Preparatory work on Bridgman directional solidification (BDS) of PbSnTe crystals prior to microgravity crystal growth experiments on Shuttle flights are reported. Gravitational effects become important in crystal growth when density gradients are present. The situation is critical in BDS of PbSnTe because of the necessity of obtaining homogeneous compositional distributions, which can be disturbed when convective processes occur. Numerical models have been defined which quantify the effects of convection in the crystal growth solution. The models were verified by earth-based crystal-growth tests in a two-zone furnace using equal concentrations of each of the elements. Data are provided to demonstrate the differences in composition among crystals grown at different orientations to the gravitational field vector.

Fripp, A. L.

Crystal Growth Research in Space

The objectives of this work are to develop growth techniques and theory leading to improved bulk growth of semiconductor single crystals. Ground based experiments will be complemented by experiments carried out in the low-g environment provided by the space shuttle. Analytical studies and laboratory investigations are being conducted to better define the causes of crystalline defects and inhomogeneities. The compound semiconductor lead-tin-telluride is being used as the modeling material. Theoretical techniques are being developed to predict the thermal and solutal fields which are present during bulk growth from a melt. Techniques for measuring the thermophysical properties of semiconductors at high temperatures have been developed. During the past year electrochemical etching techniques have been developed for delineation of inhomogeneous regions in crystals. Thermal diffusivity measurements have been completed for the solid and liquid phases of PbTe and PbSnTe. Preliminary results have been obtained on the effects on crystal morphology of gravity, interface shape and interaction between the melt and the container.

Crouch, R. K.

Reusable thermal cycling clamp

A reusable metal clamp for retaining a fused quartz ampoule during temperature cycling in the range of 20 deg C to 1000 deg C is described. A compressible graphite foil having a high radial coefficient of thermal expansion is interposed between the fused quartz ampoule and metal clamp to maintain a snug fit between these components at all temperature levels in the cycle.

Debnam, W. J., Jr.

Experimental investigation of the effects of gravity on thermosolutal convection and compositional homogeneity in Bridgman grown, compound semiconductors

Lead-tin-telluride has been grown in a thermally stable mode (solutally unstable) and in a solutally stable (thermally unstable) mode in a Bridgman configuration. Significant differences in the crystal morphology and the compositional homogeneity have been found between the two configurations. In addition, for the solutally stable configuration, evidence has been found that the flow characteristics in the melt change drastically during the course of the run.

Crouch, R. K.

Solidification behavior of low and high thermal conductivity materials in a Bridgman-Stockbarger furnace

The solid-liquid interface position and the temperature gradients in both the solid and liquid at the interface have been studied in a modified Bridgman-Stockbarger crystal growth furnace. These crystal growth factors have been studied as a function of ampoule translation rate, materials properties, and the size and temperature of a small auxiliary heater placed at the edge of the furnace hot zone. It has been found that the interface position with respect to a furnace reference point is essentially constant during a run for a low thermal conductivity material whereas the interface position changes continuously during a run with high thermal conductivity material. However, the ampoule translation rate and auxiliary heater conditions produce interface position changes in both high and low thermal conductivity materials.

Ejim, T. I.

Characterization of the general purpose research furnace for low-G directional solidification experiments

Preliminary tests have shown that it is possible to control the temperature settings in NASA's General Purpose Research Furnace in such a manner as to obtain a constant rate of movement of a high temperature isotherm down the length of the furnace. These tests also showed that a temperature gradient on the order of 40 deg cm could be obtained in the furnace while moving the particular isotherm of interest, i.e., 900 C. This provides the possibility of performing directional solidification experiments in the furnace on a MEA flight in the low gravity environment provided by the Shuttle. A functional dependency of growth rate on perturbations during the the growth has been derived and shows the importance of avoiding non-steady growth rates and changing temperature gradients.

Crouch, R. K.

Experiment requirements and implementation plan (Erip) for semiconductor materials growth in low-G environment

The MEA-2 A facility was used to test the effect of the low gravity environment on suppressing convective mixing in the growth of Pb(1-x)Sn(x)Te crystals. The need to eliminate convection, the furnace characteristics and operation that will be required for successful experimental implementation, and to the level that is presently known, the measured physical properties of the Pb(1-x)Sn(x)Te system were discussed. In addition, a brief background of the present and potential utilization of Pb(1-x)Sn(x)Te is given. Additional experiments are anticipated in future MEA-A, improved MEA and other dedicated materials processing in space flight apparatus.

Crouch, R. K.

Solutal diffusion coefficient for liquid PbTe-SnTe

The solutal diffusion coefficient has been determined for liquid lead telluride-tin telluride using a modified shear cell technique. Postdiffusion concentration profiles are presented for several diffusion couples. The best analytical curve fit to the data gives a composition-dependent diffusion coefficient of (/3/7/ to the C power) x 0.00014 sq cm/sec, where C is the PbTe concentration. In addition, data are presented to show the importance of solutal convection in the lead-tin-telluride system.

Clark, I. O.

Optimization studies for the growth of Pb(1-x)Sn(x)Te in space

A study of the effects of convection on the quality of crystals grown by the Bridgman technique has been initiated. This study is to provide a basis for the utilization of the low-gravity environment furnished by the Space Shuttle in the development of crystals with a better quality than obtainable under terrestrial conditions. A series of ground-based studies has been started with the objective to optimize the results of Shuttle experiments. A description is presented of preliminary results of some of these studies. Attention is given to a thermo-solutal convection analysis, the development of a technique for interface demarcation, the growth of Pb(1-x)Sn(x)Te crystals, thermophysical property measurements, and solutal diffusion coefficients.

Crouch, R. K.

Pyroelectric detector arrays

A pryoelectric detector array and the method for making it are described. A series of holes formed through a silicon dioxide layer on the surface of a silicon substrate forms the mounting fixture for the pyroelectric detector array. A series of nontouching strips of indium are formed around the holes to make contact with the backside electrodes and form the output terminals for individual detectors. A pyroelectric detector strip with front and back electrodes, respectively, is mounted over the strip. Biasing resistors are formed on the surface of the silicon dioxide layer and connected to the strips. A metallized pad formed on the surface of the layer is connected to each of the biasing resistors and to the film to provide the ground for the pyroelectric detector array.

Fripp, A. L.