Engineering topics

Cobb, S. D.

Publications and source records attributed to Cobb, S. D..

34 records · Page 2

NASA NTRS2001

Bridgman Growth of Detached GeSi Crystals

The growth of detached crystals by the Bridgman technique, in which the growing crystal is not in contact with the crucible wall, has been observed both on earth and in microgravity conditions. Such detachment has particularly been in evidence in microgravity experiments, where the pressure head of the molten sample is absent. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. Key parameters which must be considered are the contact angle between the melt and the crucible and the growth angle. Another essential parameter is the pressure difference between the annular gap around the solid below the melt and the volume above the melt. Here we present results of the growth of Ge(0.98)Si(0.02) using adjustments in the applied temperature profile to control the pressure difference between the bottom and top of the melt. The technique is less susceptible to sample contamination than controlling the pressure by connecting the crucible to external gas sources. Using this technique, a pressure difference is created by decreasing the temperature in the volume above the melt while the sample is molten but prior to growth. A maximum pressure difference approximately equal to the pressure head of the molten sample can thus be obtained. Several GeSi crystals were grown in pyrolitic boron nitride crucibles. When a pressure difference was applied, samples were reproducibly grown mostly detached. For comparison, samples were also grown in a configuration in which gas could pass freely between the gap below the melt and the volume above the melt and no pressure difference could be established. These samples were initially attached. Existence of detachment was determined both by measuring the radius of the samples with a profilometer and by observations of the sample surfaces with optical and electron microscopy. The gap thickness between the crucible and detached crystal was on the order of 10 micron. The surfaces of the attached areas of the crystals had the same shape as the interior crucible wall whereas in the detached areas the crystal facets could usually be observed.

Volz, M. P.↗

NASA NTRS2001

Defect Density Characterization of Detached-Grown Germanium Crystals

Several (111)-oriented, Ga-doped germanium crystals were grown in pyrolytic boron nitride (pBN) containers by the Bridgman and the detached Bridgman growth techniques. Growth experiments in closed-bottom pBN containers resulted in nearly completely detached-grown crystals, because the gas pressure below the melt can build up to a higher pressure than above the melt. With open-bottom tubes the gas pressure above and below the melt is balanced during the experiment, and thus no additional force supports the detachment. In this case the crystals grew attached to the wall. Etch pit density (EPD) measurements along the axial growth direction indicated a strong improvement of the crystal quality of the detached-grown samples compared to the attached samples. Starting in the seed with an EPD of 6-8 x 10(exp 3)/square cm it decreased in the detached-grown crystals continuously to about 200-500/square cm . No significant radial difference between the EPD on the edge and the middle of the crystal exists. In the attached grown samples the EPD increases up to a value of about 2-4 x 10(exp 4)/square cm (near the edge) and up to 1 x 10(exp 4)/square cm in the middle of the sample. Thus the difference between the detached- and the attached-grown crystals with respect to the EPD is approximately two orders of magnitude.

Schweizer, M.↗

NASA NTRS2001

Defect Density Comparison of Detached versus Attached Bridgman Grown Germanium Crystals

Semiconductor Bridgman growth without contact between the growing crystal and the growth ampoule has been observed on Earth in the last few years during several experiments. Previously, this so-called detached or dewetted growth phenomenon occurred preferentially under microgravity conditions due to the absence of the hydrostatic pressure. Many theoretical as well as experimental investigations helped to provide a better understanding of the mechanism and to identify the parameters leading to the detachment. Thus, recent attempts to get stable detached growth under terrestrial conditions by Duffar et al. growing III-V compounds and our own group with germanium and germanium-silicon alloys were frequently successful. At this conference we present the results of several germanium growth experiments performed in pyrolytic boron nitride containers. To exert an influence on the pressure ratio above and below the melt we used closed-bottom and open-bottom containers. This resulted in mainly detached-grown single crystals with the closed-bottom crucibles and attached single crystals with the open-bottom tubes. Evidence of detached growth is obtained from the crystal surface with a combination of axial profilometer scans and optical and electron microscopy. Detailed investigations of the defect structure, which is the main focus of this presentation, have shown an improvement of the crystal quality in the detached-grown samples, with a strong reduction of the etch pit density by about two orders of magnitude.

Schweizer, M.↗

NASA NTRS2000

Development Approach for the Accommodation of Materials Science Research for the Materials Science Research Facility on the International Space Station

The Materials Science Research Facility (MSRF) is a modular facility comprised of autonomous Materials Science Research Racks (MSRR's) for research in the microgravity environment afforded by the International Space Station (ISS). The initial MSRF concept consists of three Materials Science Research Racks (MSRR-1, MSRR-2, and MSRR-3) which will be developed for a phased deployment beginning on the third Utilization Flight (UF-3). The facility will house materials processing apparatus and common subsystems required for operating each device. Each MSRR is a stand alone autonomous rack and will be comprised of either on-orbit replaceable Experiment Modules, Module Inserts, investigation unique apparatus, and/or multiuser generic processing apparatus. Each MSRR will support a wide range of materials science themes in the NASA research program and will use the ISS Active Rack Isolation System (ARIS). MSRF is being developed for the United States Laboratory Module and will provide the apparatus for satisfying near-term and long-range Materials Science Discipline goals and objectives.

Schaefer, D. A.↗

NASA NTRS2000

Development of the Materials Science Research Facility (MSRF) and Experiment Apparatus for the International Space Station (ISS)

The Materials Science Research Facility (MSRF) is a modular facility designed to accommodate the current and evolving cadre of peer-reviewed materials science investigations selected to conduct research in the microgravity environment of the International Space Station (ISS). The MSRF concept consists of three Materials Science Research Racks (MSRR-1, MSRR-2, and MSRR-3) which will be developed for phased deployment into the United States Laboratory Module beginning on the third Utilization Flight (UF-3). The facility will house the materials processing apparatus and common subsystems required for operating each device, and will use the ISS Active Rack Isolation System (ARIS). Each MSRR is an autonomous rack and will be comprised of on-orbit replaceable Experiment Modules, Module Inserts, investigation unique apparatus, and/or multi-user generic processing apparatus. The MSRF will be the primary apparatus for satisfying near-term and long-range materials science discipline goals and objectives with each MSRR supporting a wide range of materials science themes in the NASA research program.

Schaefer, D. A.↗

NASA NTRS2000

Reduction of Defects in Germanium-Silicon

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 a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur frequently during microg 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 is determining the means to reproducibly grow Ge-Si alloys in the detached mode.

Szofran, F. R.↗

NASA NTRS1999

Effects of an Applied Magnetic Field on the Directional Solidification of Hg(1-x)Zn(x)Se Alloys

Directionally solidified Hg(0.9)Zn(0.1)Se alloys were studied as an alternative to HgCdTe for the detection of electromagnetic radiation because of predicted improvements in lattice stability. Several boules were grown using a modified Bridgman-Stockbarger method and in an applied magnetic field. Axial compositional profiles showed mass transfer was primarily diffusion controlled. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. Microstructural characteristics and dislocation etch pit densities were greatly improved over HgTe based alloys. The extreme importance of processing conditions on defect generation was illustrated by comparing ampoule configurations and thermal profiles.

Cobb, S. D.↗

NASA NTRS1999

Effect of Interface Shape and Magnetic Field on the Microstructure of Bulk Ge:Ga

Thermal and compositional gradients induced during the growth process contribute significantly to the development of defects in the solidified boule. Thermal gradients and the solid-liquid interface shape can be greatly effected by ampoule material. Compositional gradients are strongly influenced by interface curvature and convective flow in the liquid. Results of this investigation illustrate the combined influences of interface shape and convective fluid flow. An applied magnetic field was used to reduce the effects of convective fluid flow in the electrically conductive melt during directional solidification. Several 8 mm diameter boules of Ga-doped Ge were grown at different field strengths, up to 5 Tesla, in four different ampoule materials. Compositional profiles indicate mass transfer conditions ranged from completely mixed to diffusion controlled. The influence of convection in the melt on the developing crystal microstructure and defect density was investigated as a function of field strength and ampoule material. Chemical etching and electron backscattered electron diffraction were used to map the crystal structure of each boule along the center plane. Dislocation etch pit densities were measured for each boule. Results show the influence of magnetic field strength and ampoule material on overall crystal quality.

Cobb, S. D.↗

NASA NTRS1999

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.↗

NASA NTRS1999

Influence of Applied Thermal Gradients and a Static Magnetic Field on Bridgman-Grown GeSi Alloys

The effect of applied axial and radial thermal gradients and an axial static magnetic field on the macrosegregation profiles of Bridgman-grown GeSi alloy crystals has been assessed. The axial thermal gradients were adjusted by changing the control setpoints of a seven-zone vertical Bridgman furnace. The radial thermal gradients were affected by growing samples in ampoules with different thermal conductivities, namely graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN). 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. All of the samples were grown on Ge seeds. This resulted in a period of free growth until the Si concentration in the solid was in equilibrium with the Si concentration in the liquid. The length of crystal grown during this period was inversely proportional to the applied axial thermal gradient. Several samples were grown in an axial 5 Tesla magnetic field. Measured macroscopic segregation profiles on these samples indicate that the magnetic field did not, in general, reduce the melt flow velocities to below the growth velocities.

Volz, M. P.↗

NASA NTRS1999

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.↗

NASA NTRS1998

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.↗

NASA NTRS1997

Bridgman Growth of Germanium

The high-magnetic-field crystal growth facility at the Marshall Space Flight Center will be briefly described. This facility has been used to grow bulk germanium by the Bridgman technique in magnetic fields up to 5 Tesla. The results of investigations of ampoule material on the interface shape and thermal field applied to the melt on stability against convection will be discussed.

Szofran, F. R.↗

NASA NTRS1994

Crystal growth of selected II-VI semiconducting alloys by directional solidification

A Hg(0.84)Zn(0.16)Te alloy crystal was back-melted and partially resolidified during the first United States Microgravity Laboratory (USML-1) mission in the Marshall Space Flight Center's Crystal Growth Furnace. The experiment was inadvertently terminated at about 30% of planned completion. Nonetheless, it was successfully demonstrated that HgZnTe alloy ingots partially grown and quenched on the ground can be back-melted and regrown in space under nearly steady state growth conditions. An identical 'ground-truth' experiment was performed following the mission. Preliminary results are presented for both crystals, as well as for a series of other crystals grown prior to the mission for the purposes of optimizing in-flight growth conditions.

Lehoczky, Sandor L.↗

NASA NTRS1993

Initial development of a high-pressure crystal growth facility: Center director's discretionary fund

A low-cost, flexible, high-pressure (600 psi) system for crystal growth and related thermophysical properties measurements was designed, assembled, and tested. The furnace system includes a magnetically coupled translation mechanism that eliminates the need for a high-pressure mechanical feedthru. The system is currently being used for continuing crystal growth experiments and thermophysical properties measurements on several material systems including Hg(1-x)Cd(x)Te, Hg(1-x)Zn(x)Te, and Hg(1-x)Zn(x)Se.

Szofran, F. R.↗

NASA NTRS1991

Characterization of directionally solidified Hg(1-x)Zn(x)Se semiconducting alloys

Hg(1-x)Zn(x)Se alloys with composition between x = 0.08 and 0.115 were synthesized from elemental constituents and were resolidified using a Bridgman-Stockbarger growth technique. By performing precision mass-density measurements on selected wafers cut perpendicular to the growth axis, it was shown that the axial compositional profiles fit a numerical solution to the 1D diffusion equation which takes into account the variation of interface velocity with time. Infrared transmission-edge measurements performed on selected transverse slices from each ingot showed that the relative radial variations in composition decreased with decreasing growth rate. Van der Pauw measurements on selected wafers showed that the 10 exp 18/cu cm electron concentration, typical of as-grown crystals, could be reduced by approximately an order of magnitude by annealing in Se vapor.

Cobb, S. D.↗