Engineering topics

Benz, K. W.

Publications and source records attributed to Benz, K. W..

At least 19 records

NASA NTRS2003

Reduction of Defects in Germanium-Silicon

Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in the crystals. In addition to float-zone processing, detached Bridgman growth, although not a completely crucible-free method, is a promising tool to improve crystal quality. It does not suffer from the size limitations of float zoning and the impact of thermocapillary convection on heat and mass transport is expected to be negligible. Detached growth has been observed frequently during g experiments. Considerable improvements in crystalline quality have been reported for these cases. However, neither a thorough understanding of the process nor a quantitative assessment of the quality of these improvements exists. This project will determine the means to reproducibly grow GeSi alloys in a detached mode and seeks to compare processing-induced defects in Bridgman, detached-Bridgman, and floating-zone growth configurations in GeSi crystals (Si less than or equal to 10 at%) up to 20mm in diameter. Specific objectives include: measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; determination of the mechanism of detached growth including the role of convection; quantitative determination of the differences in defects and impurities for crystals grown using normal Bridgman, detached Bridgman, and floating zone (FZ) methods; investigation of the influence of a defined flow imposed by a rotating magnetic field on the characteristics of detached growth; control of time-dependent Marangoni convection in the case of FZ growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and growth of benchmark quality GeSi-single crystals.

Szofran, Frank R.↗

NASA NTRS2001

Reduction of Defects in Germanium-Silicon

Szofran, Frank R.↗

NASA NTRS2001

Wetting Angle and Surface Tension of Germanium Melts on Different Substrate Materials

The sessile drop technique has been used to measure the wetting angle and the surface tension of molten germanium (Ge) on various substrate materials. Sapphire, fused silica, glassy carbon, graphite, SiC, carbon-based aerogel, pyrolytic boron nitride (pBN), AlN, Si3N4, and CVD diamond were used as substrate materials. In addition, the effects of different cleaning procedures and surface treatments on the wetting behavior were investigated. The highest wetting angles with values around 170 deg. were found for pBN substrates under active vacuum or with a slight overpressure of 5N Argon or forming gas (2% Hydrogen in 5N Argon). The measurement of the surface tension and its temperature dependence for Ge under a forming gas atmosphere resulted in gamma(T) = 591 - 0.077 (T-T(sub m).

Kaiser, N.↗

NASA NTRS2001

Float Zone Growth of Alloy Semiconductor Crystals: Influence of Solutocapillary Convection

Growth techniques with large free melt surfaces are affected by convective flows induced by gradients of the surface tension. In the case of dilute semiconductor alloys (in our case: germanium-silicon), the impact of solutocapillary convection (due to the concentration dependence of the surface tension) has to be taken into account in addition to the "normal" thermocapillary convection (due to the temperature dependence of the surface tension). Theoretical considerations, based on experimental temperature profiles, growth geometry, segregation coefficient, and measured values for the temperature and concentration coefficients of the surface tension, lead to the conclusion that for the germanium rich side of the Ge(1-x)Si(x) system, the contribution of solutocapillary convection is, at least in front of the solid-liquid interface, the dominant factor. It results in an additional flow roll with a flow direction opposite to the thermocapillary flow, similar to the ones reported for metal alloys or high Prandtl-number fluids.

Dold, P.↗

NASA NTRS2001

Measurement of Microscopic Growth Rates in Float-Zone Silicon Crystals

Time dependent convective flows during crystal growth of doped semiconductors lead to fluctuations of the composition, so called dopant striations. In general, it is difficult to decide which is the main mechanism for the generation of these striations, it might be either the fluctuation of the concentration field in the melt and the extent of the solute boundary layer ahead of the solid-liquid interface or a variation of the growth velocity. Direct access to the concentration field is rather complicated to achieve, especially considering the high process temperature and the chemical activity of liquid silicon. The contribution of growth rate fluctuations to the formation of compositional fluctuations can be determined by measuring microscopic growth rates. The classical method of current pulses requires electrical feed-throughs and good electrical contacts, both are critical issues for the growth of high purity silicon crystals. Using a radiation based heating system, the heating power can be modulated very fast and effectively. We added to the normal heater power a sinusoidal off-set in the frequency range of 1 to 10 Hz, generating a narrow spaced weak rippling in the grown crystals which are superposed to the dopant striations caused by natural and by thermocapillary convection. The pulling speed was varied between 1 and 4mm/min. The microscope images of etched crystals slices have been analyzed by peak-search algorithms (measuring the spacing between each artificially induced marker) and by FFT. Performing growth experiments under a time-dependent flow regime, fluctuations of the microscopic growth velocity of Delta(v)/v(sub average) up to 50% have been measured. Damping the time-dependent convection by the use of an axial, static magnetic field of 500mT, the microscopic growth rate became constant within the resolution limit of this method. The results will be discussed using analytical methods for the calculation of microscopic growth velocity and by comparing them with measurements of temperature fluctuations in the melt during growth experiments itself.

Dold, P.↗

NASA NTRS2000

Float-Zone Growth of Gel-xSix (x ? 10 at .%) Single Crystals: Influence of Thermocapillary and Solutocapillary Convection

Gel-xSix (x ? 10 at.%) single crystals have been grown with the float-zone technique applied within a monoellipsoid mirror furnace. The feed crystal consisted of synthesized GeO.95siO.05 polycrystalline material. Two Boron-doped (much much more than 1-2 (raised dot) 1017 at/cm3) crystals were grown under identical conditions using <100> Ge seeds. One Ge:Ga-doped (much much more than 1018 at/cm3) reference crystal was also grown in the same furnace. Compositional profiles were measured with an energy dispersive analysis by X-ray (EDAX). The maximum silicon concentration attained was 10 at.%. Micrographs of the etched crystals show sharp changes in interface curvature at the crystal edges. These are considered to be caused by solutal Marangoni convection, whose strength is assumed to be a direct function of silicon concentration, Theoretical considerations show that the flow direction, velocity, and strength varies significantly from a solutal Marangoni convection regime directly in front of the solid-liquid interface to a thermal Marangoni convection regime within the bulk melt.

Campbell, Tom 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 NTRS2000

Detached and Floating-Zone Growth of Semiconductor Crystals on the ISS

Understanding the mechanism of detached Bridgman growth and establishing the growth of large scale germanium-silicon crystals by the float-zone technique are the key points of the project "RDGS - Reduction of Defects in Germanium-Silicon". The contact angle of the melt and the growth angle of the crystal are essential parameters which allow a controlled use of detached growth. The contact angle was determined for a variety of different substrates and melt compositions; pBN showed the highest value for pure germanium as well as for germanium-rich GeSi melts. The growth angle of Ge(sub 0.95) Si(sub 0.05) was measured to be 8.5-10.5 degrees which concurs with the values of pure germanium and silicon, respectively. The temperature dependence and the concentration dependence of the surface tension were determined for concentrations up to 10at% silicon (partial derivative (gamma)/partial derivative T=-0.08 (raised dot) 10(exp -3)N/m (raised dot) K, partial derivative (gamma)/partial derivative (C)=2.2 (raised dot) 10(exp -3)N/m (raised dot) at%). Using these values, the critical Marangoni number indicating the transition to time-dependent thermocapillary flow will be exceeded for the growth of large scale float-zone crystals onboard the ISS. Therefore, suitable tools for flow control are required.

Dold, P.↗

NASA NTRS1999

Reduction of Defects in Germanium-Silicon

It is well established that 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 often cited as a promising tool to improve crystal quality, without the limitations of float zoning. Detached growth has been found to occur quite often during microgravity 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 will determine the means to reproducibly grow Ge-Si alloys in the detached mode. Specific objectives include: (1) measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; (2) determination of the mechanism of detached growth including the role of convection; (3) quantitative determination of the differences of defects and impurities among normal Bridgman, detached Bridgman, and floating zone (FZ) growth; (4) investigation of the influence of defined azimuthal or meridional flow due to rotating magnetic fields on the characteristics of detached growth; (5) control time-dependent Marangoni convection in the case of FZ-growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and (6) grow high quality GeSi-single crystals with Si-concentration up to 10 at% and diameters up to 20 mm.

Szofran, Frank R.↗

NASA NTRS1999

Magnetic Damping of Solid Solution Semiconductor Alloys

The objective of this study is to: (1) experimentally test the validity of the modeling predictions applicable to the magnetic damping of convective flows in electrically conductive melts as this applies to the bulk growth of solid solution semiconducting materials; and (2) assess the effectiveness of steady magnetic fields in reducing the fluid flows occurring in these materials during processing. To achieve the objectives of this investigation, we are carrying out a comprehensive program in the Bridgman and floating-zone configurations using the solid solution alloy system Ge-Si. This alloy system has been studied extensively in environments that have not simultaneously included both low gravity and an applied magnetic field. Also, all compositions have a high electrical conductivity, and the materials parameters permit reasonable growth rates. An important supporting investigation is determining the role, if any, that thermoelectromagnetic convection (TEMC) plays during growth of these materials in a magnetic field. TEMC has significant implications for the deployment of a Magnetic Damping Furnace in space. This effect will be especially important in solid solutions where the growth interface is, in general, neither isothermal nor isoconcentrational. It could be important in single melting point materials, also, if faceting takes place producing a non-isothermal interface. In conclusion, magnetic fields up to 5 Tesla are sufficient to eliminate time-dependent convection in silicon floating zones and possibly Bridgman growth of Ge-Si alloys. In both cases, steady convection appears to be more significant for mass transport than diffusion, even at 5 Tesla in the geometries used here. These results are corroborated in both growth configurations by calculations.

Szofran, Frank R.↗

NASA NTRS1999

Measurement of Temperature Fluctuations and Microscopic Growth Rates in a Silicon Floating Zone Under Microgravity

USA Several microgravity experiments on sounding rockets and the Space Shuttle have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed during the TEXUS36 flight (February 7, 1998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3 Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4 mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. They were characterized by Spreading Resistance measurements and Differential Interference Contrast microscopy. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Marangoni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies ? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.

Croell, Arne↗

NASA NTRS1999

The Role of Marangoni Convection for the FZ-Growth of Silicon

Growing crystals by the floating zone (FZ) technique under microgravity avoids the size restriction we have under earth conditions due to hydrostatic pressure. Further, buoyancy related convection is eliminated to a great degree. But in the case of silicon, the gravity independent thermocapillary (Marangoni) convection is time-dependent even for small zone geometries. This has been demonstrated in several Technische Experimente unter Schwerelosigkeit (TEXUS) technical experiments under reduced gravity flights. Thus, to really take advantage of microgravity with respect to improved crystal quality, tools are required to control Marangoni convection in space facilities. With the application of magnetic fields, convection can be influenced; fluid flow can either be damped (static magnetic fields) or overlaid by a regular flow regime (rotating magnetic fields). In floating zones of 8-10 mm diameter and height (i.e., Ma is much greater than 6X 10(exp 3), a static magnetic field of about 2OOmT is sufficient to suppress time-dependent Marangoni convection to a high degree, but in dependence on the kind and the concentration of the added dopant, a new type of strongly pronounced dopant inhomogeneities have been detected. They are originated by thermoelectromagnetic convection. This can be avoided as well as detrimental effects on the radial dopant distribution by using rotating magnetic fields instead of static ones. Applying 7.5mT/5OHz to the FZ, the intensity of the dopant fluctuations is reduced to a high degree. Considering the rather low power consumption of rotating magnetic fields, this will be a useful tool for control or elimination of time-dependent Marangoni convection under microgravity. The strong time-dependent character of thermocapillary flow and its influence on the temperature field has been measured in silicon half-zones for Marangoni numbers of Ma is much greater than l - 1.5 X 10(exp 4): temperature fluctuations up to 4C have been determined, their frequency range was 0.4 and 0.4Hz. Between certain thermocouple or sensor pairs, strong correlation has been detected.

Dold, P.↗

NASA NTRS1999

Determination of the Wetting Angle of Germanium and Germanium-Silicon Melts on Different Substrate Materials

During Bridgman growth of semiconductors detachment of the crystal and the melt meniscus has occasionally been observed, mainly under microgravity (microg) conditions. An important factor for detached growth is the wetting angle of the melt with the crucible material. High contact angles are more likely to result in detachment of the growing crystal from the ampoule wall. In order to achieve detached growth of germanium (Ge) and germanium-silicon (GeSi) crystals under 1g and microg conditions, sessile drop measurements were performed to determine the most suitable ampoule material as well as temperature dependence of the surface tension for GeSi. Sapphire, fused quartz, glassy carbon, graphite, SiC, pyrolytic Boron Nitride (pBN), AIN, and diamond were used as substrates. Furthermore, different cleaning procedures and surface treatments (etching, sandblasting, etc.) of the same substrate material and their effect on the wetting behavior were studied during these experiments. pBN and AIN substrates exhibited the highest contact angles with values around 170 deg.

Kaiser, Natalie↗

NASA NTRS1999

The Influence of Static and Rotating Magnetic Fields on Heat and Mass Transfer in Silicon Floating Zones

Hear and mass transfer in float-zone processing are strongly influenced by convective flows in the zone. They are caused by buoyancy convection, thermocapillary (Marangoni) convection, or artificial sources such as rotation and radio frequency heating. Flows in conducting melts can be controlled by the use of magnetic fields, either by damping fluid motion with static fields or by generating a def@ned flow with rotating fields. The possibilities of using static and rotating magnetic fields in silicon floating-zone growth have been investigated by experiments in axial static fields up to ST and in transverse rotating magnetic fields up to 7.S mT. Static fields of a few 100 MT already suppress most striations but are detrimental to the radial segregation by introducing a coring effect. A complete suppression of dopant striations caused by time-dependent thermocapillary convection and a reduction of the coring to insignificant values, combined with a shift of the axial segregation profile towards a more diffusion-limited case, is possible with static fields ? 1T. However, under certain conditions the use of high axial magnetic fields can lead to the appearance of a new type of pronounced dopant striations, caused by thermoelec:romagnetic convection. The use of a transverse rotating magnetic field influences the microscopic segregation at quite low inductions, of the order of a few mT. The field shifts time-dependent flows and the resulting striation patterns from a broad range of low frequencies at high amplitudes to a few high frequencies at low amplitudes

Croell, Arne↗

NASA NTRS1999

Static Magnetic Fields in Semiconductor Floating-Zone Growth

Heat and mass transfer in semiconductor float-zone processing are strongly influenced by convective flows in the zone, originating from sources such as buoyancy convection, thermocapillary (Marangoni) convection, differential rotation, or radio frequency heating. Because semiconductor melts are conducting, flows can be damped by the use of static magnetic fields to influence the interface shape and the segregation of dopants and impurities. An important objective is often the suppression of time-dependent flows and the ensuing dopant striations. In RF-heated Si-FZ - crystals, fields up to O.STesla show some flattening of the interface curvature and a reduction of striation amplitudes. In radiation-heated (small-scale) SI-FZ crystals, fields of 0.2 - 0.5 Tesla already suppress the majority of the dopant striations. The uniformity of the radial segregation is often compromised by using a magnetic field, due to the directional nature of the damping. Transverse fields lead to an asymmetric interface shape and thus require crystal rotation (resulting in rotational dopant striations) to achieve a radially symmetric interface, whereas axial fields introduce a coring effect. A complete suppression of dopant striations and a reduction of the coring to insignificant values, combined with a shift of the axial segregation profile towards a more diffusion-limited case, are possible with axial static fields in excess of 1 Tesla. Strong static magnetic fields, however, can also lead to the appearance of thermoelectromagnetic convection, caused by the interaction of thermoelectric currents with the magnetic field.

Croll, Arne↗

NASA NTRS1999

Measurement of Temperature Fluctuations and Microscopic Growth Rates in a Silicon Floating Zone on TEXUS36

Several pg experiments on sounding rockets and the Space Shuttle have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed during the TEXUS36 flight (February 7, 1 998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. They were characterized by Spreading Resistance measurements and Differential Interference Contrast microscopy. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Marangoni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.

Croell, Arne↗

NASA NTRS1999

Detached Growth of Germanium and Germaniumsilicon

Up to now, detached growth was observed mainly under microgravity, i.e. under the absence of hydrostatic pressure that hinders the formation of a free melt meniscus. the detached growth of germanium doped with gallium was obtained under 1 g conditions, the growth was performed in quartz-glass ampoule. Part of the crystal grew without wall contact, the detached growth was observed in-situ with a CCD-camera as well as after the growth process in form of growth lines and the formation of <111> facets on the crystal surface. GeSi crystal (oriientation: <111>, maximum silicon content: 4 at%, seed material: Ge) was grown in a pBN crucible (excluding the possibility of in-situ monitoring of the growth process). The grown crystal exhibits three growth facets, indicating also wall free growth. Surface analysis of the crystals (NDIC, SEM) and characterization of crystal segregation (EDAX, resistivity measurement) and defect structure (EPD, x-ray diffraction measurements) will be presented.

Dold, P.↗

NASA NTRS1999

Measurement of Temperature Fluctuations and Microscopic Growth Rates in a Silicon Floating Zone on TEXUS36

Several earlier (micro)g experiments have shown that time-dependent thermocapillary (Marangoni) convection is the major cause for the formation of dopant striations in floating-zone grown semiconductor crystals, at least in small-scale systems not employing RF heating. To quantify this correlation, a silicon floating-zone experiment was performed on the TEXUS36 flight (February 7, 1 998) in the monoellipsoid mirror furnace TEM02-ELLI. During the experiment, temperature fluctuations in the silicon melt zone and the microscopic growth rate were simultaneously measured. Temperature fluctuations of 0.5 C - 0.7 C with main frequencies between 0.1 Hz and 0.3 Hz were detectable. The microscopic growth rate fluctuated considerably around the average growth rate of 1 mm/min: rates from 4mm/min to negative values (backmelting) were observed. Dopant striations are clearly visible in the Sb-doped crystal. The frequencies associated with the dopant inhomogeneities correspond quite well with those of the temperature fluctuations and microscopic growth rates. 3D numerical simulations were performed to predict the optimum position of the temperature sensor, to evaluate characteristic temperature amplitudes and frequencies, and to give insight into the instability mechanisms of Maran-goni convection in this configuration. The simulations were in good agreement with the experimental values, showing temperature fluctuations with frequencies f? 0.25 Hz and amplitudes up to 1.8 C at a position equivalent to that of the sensor tip in the experiment.

Croell, Arne↗