Engineering topics

Szofran, F. R.

Publications and source records attributed to Szofran, F. R..

At least 19 records

NASA NTRS2005

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

A series of (100)-oriented gallium-doped germanium crystals has been grown by the vertical Bridgman method and under the influence of a rotating magnetic field (RMF). Time-dependent flow instabilities occur when the critical magnetic Taylor number (Tm(sup c)) is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. Tm(sup c) decreases as the aspect ratio of the melt increases, and approaches the theoretical limit expected for an infinite cylinder. Intentional interface demarcations are introduced by pulsing the RMF on and off The RMF has a marked affect on the interface shape, changing it from concave to nearly flat as the RMF strength is increased.

Volz, M. P.↗

NASA NTRS2005

X-ray Characterization of Detached-Grown Germanium Crystals

Germanium (111)-oriented crystals have been grown by the vertical Bridgman technique, in both detached and attached configurations. Microstructural characterization of these crystals has been performed using synchrotron white beam x-ray topography (SWBXT) and double axis x-ray diffraction. Dislocation densities were measured from x-ray topographs obtained using the reflection geometry. For detached-grown crystals, the dislocation density is 4-6 x 10(exp 4) per square centimeter in the seed region, and decreases in the direction of growth to less than 10(exp 3) per square centimeter, and in some crystals reaches less than 10(exp 2) per square centimeter. For crystals grown in the attached configuration, dislocation densities were on the order of 10(exp 4) per square centimeter in the middle of the crystals, increasing to greater than 10(exp 5) per square centimeter near the edge. The measured dislocation densities are in excellent agreement with etch pit density results. The rocking curve linewidths were relatively insensitive to the dislocation densities. However, broadening and splitting of the rocking curves were observed in the vicinity of subgrain boundaries identified by x-ray topography in some of the attached-grown crystals.

Volz, M. P.↗

NASA NTRS2004

Detached Growth of Germanium by Directional Solidification

Detached crystal growth technique (dewetting) offers improvement in the quality of the grown crystals by preventing sticking to the walls of the crucible and thus reducing the possibility of parasitic nucleation and formation of lattice defects upon cooling. One of the factors relevant for the phenomena is the pressure differential across the meniscus at the crystal-melt interface. We investigated this effect experimentally. The growth took place in closed ampoules under the pressure of an inert gas (forming gas: 96% Ar + 4% H2). The pressure above the melt was adjustable and allowed for a control of the pressure difference between the top and bottom menisci. The crystals were characterized, particularly by taking profilometer measurements along the grown crystals surface. The effects of the experimental conditions on the detachment were compared with those predicted based on the theory of Duffar et al.

Palosz, W.↗

NASA NTRS2004

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

A series of (100)-oriented gallium-doped germanium crystals have been grown by the Bridgman method and under the influence of a rotating magnetic field (RMF). Time-dependent flow instabilities occur when the critical magnetic Taylor number (Tm(sup c) is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. The experimental data indicate that Tm(sup c) increases as the aspect ratio of the melt decreases. Modeling calculations predicting Tm(sup c) as a function of aspect ratio are in reasonable agreement with the experimental data. The RMF has a marked affect on the interface shape, changing it from concave to nearly flat as the RMF strength is increased. Also, by pulsing the RMF on and off, it is shown that intentional interface demarcations can be introduced.

Volz, M. P.↗

NASA NTRS2004

Detached Growth of Germanium by Directional Solidification

The conditions of detached solidification under controlled pressure differential across the meniscus were investigated. Uncoated and graphite- or BN-coated silica and pBN crucibles were used. Detached and partly detached growth was achieved in pBN and BN-coated crucibles, respectively. The results of the experiments are discussed based on the theory of Duffar et al.

Palosz, W.↗

NASA NTRS2003

Melt-Crucible Wetting Behavior in Semiconductor Melt Growth Systems

The wetting angles of several semiconductor-substrate combinations that are of practical importance for crystal growth have been measured: Ga-GaSb-Sb on fused quartz; Ge on fused quartz and carbon-based substrates, each with different roughness; Si on fused quartz plates and on plates coated with fused quartz, Si3N4, and BN powders. The Ga-GaSb-Sb system showed no significant dependence of the wetting angle on the composition despite a large composition dependence of the surface tension. For Ge, the effect of the roughness on the angle could initially be seen on both types of substrates, but for the fused quartz substrates an equilibrium value independent of the surface treatment was reached after several hours of contact time. For Si, total wetting was found for Si3N4 powders. A reduction of the angle over time was found for both fused quartz and BN powders, with the BN powder showing the highest angle at 150-120 deg.

Croell, A.↗

NASA NTRS2003

In-Situ Pressure Measurements During the Detached Growth of Germanium

Crystal growth by the vertical Bridgman method in which there is little or no contact between the wall and the crystal has been termed detached solidification. Detachment has been observed frequently in previous microgravity experiments, and has been reported under some terrestrial conditions as well. It is expected that detachment can be conditioned by establishing an appropriate pressure difference below and above the melt. To test this hypothesis, an experimental technique has been developed to measure this pressure difference during the growth of germanium by the vertical Bridgman method. The apparatus allows for both monitoring the pressures and actively controlling them during growth. For a given melt height, there is a maximum pressure difference attainable before gas bubbles up through the melt. This maximum pressure increases with increasing melt height. As the melt height approaches zero, the maximum pressure difference, about 20 mbar in these experiments, is determined by the surface tension and gap width of the meniscus at the bottom of the melt.

Volz, M. P.↗

NASA NTRS2003

Analysis of Radial Segregation in Directionally Solidified Hg(0.89)Mn(0.11)Te

Bridgman growth experiments were performed on Hg(0.89)Mn(0.11)Te (MMT) to determine the extent of radial Manganese segregation during directional solidification. MMT crystals were directionally solidified at rates of 0.09 and 0.18 p d s and in axial thermal gradients of 83 and 68"C/cm. Wavelength Dispersive Spectroscopy (WDS) and Fourier Transform Infra-Red (FTIR) analytical techniques were used to determine the radial homogeneity in all boules and the deflection of the solid-liquid interface (SLI) in two boules that were rapidly quenched after 5 to 6 cm of directional solidification. For all growth runs, the measured radial coinpositional variations were on the order of 0.01 molar percent MnTe in the steady state region of growth. Comparison of the measured radial compositional results of the crystals to predicted values in the diffusion-limited regime indicate a strong influence of convection near the solid-liquid interface. This conclusion is supported by the weak influence of the translation rates and axial thermal gradients utilized in this study upon radial compositional homogeneity.

Price, M. W.↗

NASA NTRS2002

Stability of Detached Grown Germanium Single Crystals

Detachment of the melt meniscus from the crucible during semiconductor Bridgman growth experiments has been observed in recent years especially, under microgravity experiments. Under earth conditions, the hydrostatic pressure counteracts the mechanism, whereby it is more difficult to achieve detached Bridgman growth. Attempts to get stable detached growth under terrestrial conditions have been discussed in the literature and have been the subject of recent experiments in our own group. The advantage of crystals grown without wall contact is obvious: In general, they possess a higher crystal quality than conventional Bridgman grown crystals with wall contact. However, due to the interaction of different parameters such as the wetting behavior of the melt with the crucible, and the dependence of the growth angle with the shape of the melt meniscus, the mechanism leading to detachment is very complicated and not completely understood. We have grown several doped and undoped Germanium crystals with the detached Bridgman and the normal Bridgman growth technique. Pyrolytic boron nitride containers were used for all growth experiments. In the detached grown crystals the typical gap thickness between the pBN crucible and the crystal is in the range of 10 to 100 microns, which was determined by performing profilometer measurements. Etch pit density measurements were also performed and a comparison between detached and attached grown crystals will be given. An interesting feature was detected on the surface of a detached grown crystal. Strong surface striations with an average axial distance of 0.5mm were observed around the whole circumference. The maximum fluctuation of the gap thickness is in the range of 5-10 microns. These variations of the detached gap along the crystal axis can be explained by a kind of stiction of the melt/crucible interface and thus by a variation of the meniscus shape. This phenomenon leading to the fluctuation of the gap thickness will be discussed in detail.

Schweizer, M.↗

NASA NTRS2002

Solutocapillary Convection in the Float-Zone Process with a Strong Magnetic Field

This paper treats the axisymmetric flow and mass transport in a cylindrical liquid bridge between the melting end of a feed rod and the solidifying end of an alloyed semiconductor crystal. There is a strong, uniform, steady, axial magnetic field. The surface tension depends on the temperature and the concentration of the species, while variations of the concentration occur because one species is rejected into the liquid during solidification. The thermocapillary and solutocapillary convections tend to cancel- over part of the liquid bridge. For certain parameter ranges, there are two different stable steady solutions: one where the concentration gradient along the free surface leads to dominance by the solutocapillary convection and one where the mass transport due to the thermocapillary convection makes the concentration gradient along the free surface small, so that the thermocapillary convection is dominant.

Walker, J. S.↗

NASA NTRS2002

Wetting Angles and Surface Tension of Ge(1-x)Si(x) Melts on Different Substrate Materials

The wetting angles and the surface tension of Ge(1-x)Si(x) melts (0.02 less than x less than 0.13) have been measured on various substrate materials using the sessile drop technique. Fused quartz, sapphire, SiC, glassy carbon, pBN, AIN, and Si3N4 have been used as substrates. The highest and most stable wetting angles were found for pBN substrates with 164 +/- 8 deg., either under forming gas with an additional carbon getter in the system or under active vacuum. The surface tension measurements resulted in a value of +2.2 x 10(exp -3) N/m.at%Si for the concentration dependence delta(gamma)/(delta)C. For the composition range measured, the temperature dependence (delt)gamma/(delta)T showed values similar to those of pure Ge, on average -0.07 x 10(exp -3) N/mK.

Croell, A.↗

NASA NTRS2002

The Detached Bridgman Process: Application for the Growth of Low-Defect Germanium Crystals

During crystal growth in the vertical Bridgman process, both the melt and the growing crystal are in contact with the ampoule wall. The different thermal coefficients of expansion of the crystal and the ampoule wall can lead to stresses, crystal defects, and not rarely to cracks and/or polycrystalline growth in the crystal. The detached Bridgman process is characterized by the fact that the melt meniscus frees itself from the ampoule wall and the crystal can be grown without wall contact with the ampoule. After the effect of detachment was observed due to the reduced force of gravity during the early experiments under microgravity conditions, in the past few years the Bridgman process likewise has been successfully used to grow at least partially detached under 1g-condition. If the requirements for detaching the melt meniscus from the ampoule wall are not fulfilled by the material-specific parameters (like e.g. wetting behavior between ampoule and melt and the growth angle of the crystal), detachment can be obtained also by the imposition of suitable pressure ratios in the growth ampoule. In the context of this paper, the growth of germanium by the detached and vertical Bridgman processes in pyrolytic boron nitride crucibles will be reported, Typical gap widths between ampoule wall and detached grown crystals are approximately 10-50 microns. Compared to the crystals grown with wall contact, a reduction of the etch pit density of approximately two orders of magnitude could be obtained by growing with the detached process.

Schweizer, M.↗

NASA NTRS2002

Detached Bridgman Growth of Germanium and Germanium-Silicon Alloy Crystals

Earth based experiments on the science of detached crystal growth are being conducted on germanium and germanium-silicon alloys (2 at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS). The purpose of the microgravity experiments includes differentiating among proposed mechanisms contributing to detachment, and confirming or refining our understanding of the detachment mechanism. Because large contact angle are critical to detachment, sessile drop measurements were used to determine the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. The contact angles were 173 deg (Ge) and 165 deg (GeSi) for pBN. For fused silica, the contact angle decreases from 150 deg to an equilibrium value of 117 deg (Ge) or from 129 deg to an equilibrium value of 100 deg (GeSi) over the duration of the experiment. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. Results in this presentation will show that we have established the effects on detachment of ampoule material, pressure difference above and below the melt, and silicon concentration; samples that are nearly completely detached can be grown repeatedly in pBN.

Szofran, F. R.↗

NASA NTRS2002

Effect of Residual Accelerations on the Crystal Growth of II-VI Semiconductors in Low Earth Orbit

The paper compares and summarizes the effects of residual acceleration during crystal growth on the compositional variation of two II-VI solid solution binary alloys (Hg(0.8)Cd(0.2)Te and Hg(0.84)Zn(0.16)Te). The crystals were grown by directional solidification on the second United States Microgravity Payload (USMP-2) and the first United States Microgravity Laboratory (USML-1) missions, respectively. For both alloys, changes in the direction and magnitude of the quasisteady acceleration vector (approximately 0.4- 1 mu g) caused large changes in the radial compositional distribution that demonstrates the importance of residual accelerations, even in the submicrogravity range, for large density gradients in the melt and slow solidification rates. The observed compositional variations will be correlated to changes in the radial flow velocities ahead of the solidification interface.

Gillies, D. C.↗

NASA NTRS2002

Characterization of Surface Features in Detached Grown 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. At present, the mechanisms contributing to the detachment are not completely understood and until recently detachment has not been reproducibly obtained. It is commonly understood that the main factors that promote the occurrence of detached growth include: high contact angle between the melt and the crucible material, high growth angle, and a pressure difference between the annular gap around the solid below the melt and the volume above the melt along the meniscus. These parameters were varied in Bridgman growth experiments to determine the conditions required to achieve detached growth terrestrially in Ge and GeSi alloys. These experiments are in preparation for experiments on the International Space Station (ISS). The detailed objectives of the flight experiments and a description of the growth methods employed are the subject of another presentation at this Conference. Detached crystals were achieved repeatedly in pyrolytic boron nitride ampoules when a pressure difference was employed. All crystals, except for those grown in fused silica ampoules, were easily removed from their containers, however, this fact alone is not sufficient to infer detached growth. Detachment was verified by comparing profilometer measurements of the radius of the samples with observations of the sample surfaces using optical and electron microscopy. The surfaces of the attached areas of the crystals had the same shape and surface texture as the interior crucible wall. Regions of detached growth contained many unique features and crystal facets could usually be observed. Several of these surface features have been correlated with mechanisms of detachment or free-surface growth and others to processing events or conditions.

Cobb, S. D.↗

NASA NTRS2002

Bridgman Growth of Detached GeSi Crystals

Ge(1-x)Si(x) (0 less than x less than 0.12) has been grown by the vertical Bridgman technique using adjustments in the applied temperature profile to control the pressure difference between the bottom and top of the melt. Using this technique. a pressure difference is created by decreasing the temperature in the gas volume above the melt while the sample is molten but prior to growth. A maximum pressure difference approximately equal to the hydrostatic pressure of the molten sample can thus be obtained. Several GeSi crystals were grown in pyrolitic boron nitride ampoules. 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 flow 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 surface roughness of the samples with a profilometer and by observations of the sample surfaces with optical and electron microscopy.

Volz, M. P.↗

NASA NTRS2002

Bridgman Growth of Germanium Crystals in a Rotating Magnetic Field

A series of (100)-oriented gallium-doped germanium crystals have been grown by the Bridgman method and under the influence of a rotating magnetic field (RMF). The RMF has a marked affect on the interface shape, changing it from concave to nearly flat. The onset of time-dependent flow instabilities occurs when the critical magnetic Taylor number is exceeded, and this can be observed by noting the appearance of striations in the grown crystals. The critical magnetic Taylor number is a sensitive function of the aspect ratio and, as the crystal grows under a constant applied magnetic field, the induced striations change from nonperiodic to periodic, undergo a period-doubling transition, and then cease to exist. Also, by pulsing the RMF on and off, it is shown that intentional interface demarcations can be introduced.

Volz, M. P.↗

NASA NTRS2002

Crystal Growth of HgZnTe Alloy by Directional Solidification in Low Gravity Environment

An Hg(0.84)Zn(0.16)Te alloy crystal was back-melted and partially re-solidified during the first United States Microgravity Laboratory 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 a HgZnTe alloy ingot partially grown and quenched on the ground can be back-melted and re-grown in space under nearly steady-state growth conditions. An identical "ground-truth" experiment was performed following the mission and a comparison between the properties of the crystals is described. The results indicate the importance of residual microgravity acceleration (less than or approx. equal to 0.4 micro-grams) even in the sub-microgravity range for the slow solidification velocities and large density gradients.

Su, Ching-Hua↗