Engineering topics

Volz, M. P.

Publications and source records attributed to Volz, M. P..

At least 73 records · Page 4

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

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

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

Toward Understanding Pore Formation And Mobility During Controlled Directional Solidification In A Microgravity Environment Investigation (PFMI)

The generation and inclusion of detrimental porosity, e.g., "pipes" and "rattails" can occur during controlled directional solidification processing. The origin of these defects is generally attributed to gas evolution and entrapment during solidification of the melt. On Earth, owing to buoyancy, an initiated bubble can rapidly rise through the liquid melt and "pop" at the surface; this is obviously not ensured in a low gravity or microgravity environment. Clearly, porosity generation and inclusion is detrimental to conducting any meaningful solidification-science studies in microgravity. Thus it is essential that model experiments be conducted in microgravity, to understand the details of the generation and mobility of porosity, so that methods can be found to eliminate it. In hindsight, this is particularly relevant given the results of the previous directional solidification experiments conducted in Space. The current International Space Station (ISS) Microgravity Science Glovebox (MSG) investigation addresses the central issue of porosity formation and mobility during controlled directional solidification processing in microgravity. The study will be done using a transparent metal-analogue material, succinonitrile (SCN) and succinonitrile-water "alloys", so that direct observation and recording of pore generation and mobility can be made during the experiments. Succinonitrile is particularly well suited for the proposed investigation because it is transparent, it solidifies in a manner analogous to most metals, it has a convenient melting point, its material properties are well characterized and, it has been successfully used in previous microgravity experiments. The PFMI experiment will be launched on the UF-2, STS-111 flight. Highlighting the porosity development problem in metal alloys during microgravity processing, the poster will describe: (i) the intent of the proposed experiments, (ii) the theoretical rationale behind using SCN as the study material for porosity generation and migration and, (iii) the experimental protocol for the investigation of the effects of the processing parameters. Photographs of the flight experimental hardware, and the novel sample ampoule, will be exhibited. The experimental apparatus will be described in detail and a summary of the scientific objectives will be presented.

Grugel, R. N.↗

NASA NTRS2002

Pore Formation and Mobility (PFMI): An International Space Station Glovebox Investigation

Porosity in the form of "bubbles and pipes" can occur during controlled directional solidification processing of metal alloys. It is detrimental to material properties and precludes obtaining meaningful scientific results. On Earth, density differences allow an initiated bubble can rise through the liquid and "pop" at the surface resulting in a sound casting. This is not likely to occur in a microgravity environment and, unfortunately, a number of experiments conducted in microgravity have suffered from porosity effects. The current investigation is a systematic effort towards understanding porosity formation and mobility during controlled directional solidification in a microgravity environment. This will be investigated by utilizing a transparent material, succinonitrile (SCN), in conjunction with a translating temperature gradient stage so that direct observation and recording of pore generation and mobility can be made. The talk will cover the porosity problem, the details of the proposed experiments and the experimental hardware, and the expectations from the microgravity experiments.

Grugel, R. N.↗

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

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 NTRS2001

The Science of Detached Bridgman Growth and Solutocapillary Convection in Solid Solution Crystals

Bridgman and Float-zone crystal growth experiments are planned for NASA's First Materials Science Research Rack using the European Space Agency's Materials Science Laboratory with the Low Gradient Furnace (LGF) and Float Zone Furnace with Rotating Magnetic Field (FMF) inserts, respectively. Samples will include germanium and germanium-silicon alloys with up to 10 atomic percent silicon. The Bridgman part of the investigation includes detached growth samples and so there will be a solid-liquid-gas tri-junction in those experiments just as there will be in all float-zone experiments. There are other similarities as well as significant differences between the types of growth that will be discussed. The presentation will call attention to the reasons that experiments in microgravity will provide information unattainable from Earth-based experiments.

Szofran, F. R.↗

NASA NTRS2001

Investigation of Vibrational Control of the Bridgman Crystal Growth Technique

The character of natural buoyant convection in rigidly contained inhomogeneous fluids can be drastically altered by vibrating the container. Vibrations are expected to play a crucial influence on heat and mass transfer onboard the International Space Station (ISS). It is becoming evident that substantial vibrations will exist on the ISS in the wide frequency spectrum. In general, vibrational flows are very complex and governed by many parameters. In many terrestrial crystal growth situations, convective transport of heat and constituent components is dominated by buoyancy driven convection arising from compositional and thermal gradients. Thus, it may be concluded that vibro-convective flow can potentially be used to influence and even control transport in some crystal growth situations.

Fedoseyev, Alexandre I.↗

NASA NTRS2001

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 (2at% Si average composition) in preparation for a series of experiments aboard the International Space Station (ISS) to differentiate among proposed mechanisms contributing to detachment. Sessile drop measurements were first carried out for a large number of substrates made of potential ampoule materials to determine the contact angles and the surface tension as a function of temperature and composition. The process atmosphere and duration of the experiment (for some cases) were also found to have significant influence on the wetting angle. 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 to an equilibrium value with duration of measurement ranging from 150 to 117 deg (Ge), 129 to 100 deg (GeSi). Forming gas (Ar + 2% H2) and vacuum have been used in the growth ampoules. With gas in the ampoule, a variation of the temperature profile during growth has been used to control the pressure difference between the top of the melt and the volume below the melt caused by detachment of the growing crystal. The stability of detachment has been modeled and substantial insight has been gained into the reasons that detachment has most often been observed in reduced gravity but nonetheless has occurred randomly even there. An empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed and will be presented. Methods for determining the nature and extent of detachment include profilometry and optical and electron microscopy. This surface study is the subject of another presentation at this Congress. Results in this presentation will show that we have established the effects of different ampoule materials, temperature profiles, pressure differences, and silicon concentrations and that samples that are nearly completely detached can be grown repeatedly.

Szofran, F. R.↗

NASA NTRS2001

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 Congress. 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 in general and others to processing events or conditions. These results will be compared with observations of surface features on detached regions of microgravity grown crystals.

Cobb, S. D.↗

NASA NTRS2001

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 micrometers, 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 0.5 mm were observed around the whole circumference. The maximum fluctuation of the gap thickness is in the range of 5-10 micrometers. 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 NTRS2001

Toward Understanding Pore Formation and Mobility During Controlled Directional Solidification in a Microgravity Environment Investigation (PFMI)

Grugel, R. N.↗

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

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.↗