Growth of boron doped diamond by vapor deposition
Growth of p-type semiconducting diamond by vapor phase deposition using methane-diborane doping gas mixture in presence of diamond seed crystals
Poferl, D. J.↗
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Controlled in situ etch-back
A controlled in situ etch-back technique is disclosed in which an etch melt and a growth melt are first saturated by a source-seed crystal and thereafter etch-back of a substrate takes place by the slightly undersaturated etch melt, followed by LPE growth of a layer by the growth melt, which is slightly supersaturated.
Mattauch, R. J.↗
Growth of GaAs from a free surface melt under controlled arsenic pressure in a partially confined configuration
A partially confined configuration for the growth of GaAs from melt in space was developed, consisting of a triangular prism containing the seed crystal and source material in the form of a rod. It is suggested that the configuration overcomes two obstacles in the growth of GaAs in space: total confinement in a quartz crucible and lack of arsenic pressure control. Ground tests of the configuration show that it is capable of crystal growth in space and is useful for studying the growth of GaAs from a free-surface melt on earth. The resulting chemical composition, electrical property variations, and phenomenological models to account for the results are presented.
Gatos, H. C.↗
Grain orientation in high Tc superconductors by molten salt powder synthesis
The molten salt or the flux method is used to fabricate a grain oriented YBa2Cu3O(7-x) (123) superconductor. Here we suggest a two-stage approach in using the 'green phase', Y2BaCuO5 (211), as seed crystals in the formation of YBa2Cu3O(7-x). The process uses Y2BaCuO5 formed by molten salt synthesis. The Y2BaCuO5 phase was observed to be stable in water and in most of the salt systems. Salt processing can form a small quantity of anisotropic particles of Y2BaCuO5. This material can form the 123 phase when tape cast and sintered in the presence of the required levels of Ba and Cu.
Gopalakrishnan, Sudhakar↗
Controlling nucleation in protein solutions
A simple one-step technique for controlling the nucleation stage in protein solutions without the use of a seed crystal was developed using a specially designed apparatus in which the nucleation and growth processes can be separated. The method can be applied only to species that have a temperature-dependent solubility. The effectiveness of this 'thermonucleating' device was demonstrated with the nucleation and growth of ice, Rochelle salt, and lysozyme.
Demattei, R. C.↗
Microstructure and Macrosegregation Study of Directionally Solidified Al-7Si Samples Processed Terrestrially and Aboard the International Space Station
This talk reports research that has been carried out under the aegis of NASA as part of a collaboration between ESA and NASA for solidification experiments on the International Space Station (ISS). The focus has been on the effect of convection on the microstructural evolution and macrosegregation in hypoeutectic Al‐Si alloys during directional solidification (DS). The DS‐experiments have been carried out under 1‐g at Cleveland State University (CSU) and under low‐g on the International Space Station (ISS). The thermal processing‐history of the experiments is well defined for both the terrestrially‐processed samples and the ISS‐processed samples. We have observed that the primary dendrite arm spacings of two samples grown in the low‐g environment of the ISS show good agreement with a dendrite‐growth model based on diffusion controlled growth. The gravity‐driven convection (i.e., thermosolutal convection) in terrestrially grown samples has the effect of decreasing the primary dendrite arm spacings and causes macrosgregation. In order to process DS‐samples aboard the ISS, dendritic‐seed crystals have to partially remelted in a stationary thermal gradient before the DS is carried out. Microstructural changes and macrosegregation effects during this period are described.
Angart, Samuel↗
Comparison of Directionally Solidified Samples Solidified Terrestrially and Aboard the International Space Station
This article reports research that has been carried out under the aegis of NASA as part of a collaboration between ESA and NASA for solidification experiments on the International Space Station (ISS). The focus has been on the effect of convection on the microstructural evolution and macrosegregation in hypoeutectic Al-Si alloys during directional solidification (DS). Terrestrial DS-experiments have been carried out at Cleveland State University (CSU) and under microgravity on the International Space Station (ISS). The thermal processing-history of the experiments is well defined for both the terrestrially processed samples and the ISS-processed samples. As of this writing, two dendritic metrics was measured: primary dendrite arm spacings and primary dendrite trunk diameters. We have observed that these dendrite-metrics of two samples grown in the microgravity environment show good agreements with models based on diffusion controlled growth and diffusion controlled ripening, respectively. The gravity-driven convection (i.e., thermosolutal convection) in terrestrially grown samples has the effect of decreasing the primary dendrite arm spacings and causes macrosegregation. Dendrite trunk diameters also show differences between the earth- and space-grown samples. In order to process DS-samples aboard the ISS, the dendritic seed crystals were partially remelted in a stationary thermal gradient before the DS was carried out. Microstructural changes and macrosegregation effects during this period are described and have modeled.
Angart, S.↗
Characterization of Semi-Insulating CdTe Crystals Grown by Horizontal Seeded Physical Vapor Transport
CdTe crystals were grown by horizontal seeded physical vapor transport technique in uncoated and boron nitride coated fused silica ampoules with the source materials near the congruent sublimation condition. The grown crystals were characterized by current-voltage measurements, low temperature photoluminescence spectroscopy, near IR transmission optical microscopy, spark source mass spectroscopy and chemical etching. The measured resistivities of the crystals were in the high-10(exp 8) ohm-cm range. Although the crystal grown in the boron nitride coating was contaminated with boron from the photoluminescence measurements, the coating yielded a single crystal with no inclusions or precipitates.
Chattopadhyay, K.↗
In-Situ Partial Pressure Measurements and Visual Observation during Crystal Growth of ZnSe by Seeded Physical Vapor Transport
An in-situ monitoring furnace was constructed with side windows to perform partial pressure measurements by optical absorption and visual observation of the growing crystal. A fused silica -rowth ampoule with a 4.5 cm long square tube between the source and the seed was prepared for the optical absorption measurements. A ZnSe crystal was grown by the seeded physical vapor transport (PVT) technique in the horizontal configuration. The growth temperature was 1120 C and the furnace translation rate was 3nmVday. Partial pressures of Se2, P(sub Se2), at three locations along the length of the growth ampoule were measured at 90 min intervals during the growth process. The measured P (sub Se2) were in the range of 2.0 to 6.5 x 10(exp -3) atm. The P(sub Se2) results indicated that the partial pressure profile was inconsistent with the results of the one-dimensional diffusion mass transport model and that the source composition shifted toward Se-rich during the run, i.e. the grown crystal was more Zn-rich than the source. The visual observation showed that the seed crystal first etched back, with greater thermal etching occurring along the edges of the seed crystal. Once the growth started, the crystal crew in a predominately contactless mode and facets were evident during growth. The crystal did not grow symmetrically which is believed to be due to the unintentional asymmetry of the radial thermal profile in the furnace.
Su, Ching-Hua↗
Laser-Heated Floating Zone Production of Single-Crystal Fibers
This report describes how a laser-heated floating zone apparatus can be used to investigate single-crystal fibers of various compositions. A feedrod with a stoichiometric composition of high-purity powders was connected to a pedestal and fed into a laser scan where it combined with a single-crystal fiber seed. A molten zone was formed at this junction. As the feedrod was continuously fed into the laser scan, a single-crystal fiber of a prescribed orientation was withdrawn from the melt. The resultant fibers, whose diameters ranged from 100 to 250 gm, could then be evaluated on the basis of their growth behavior, physical properties, mechanical properties, and fiber perfection.
Ritzert, Frank↗
Vapor Growth of ZnSe-based Compound Semiconductors in Low Gravity environment on International Space Station
Six low-gravity experiments of crystal growth of ZnSe-based compound semiconductors by physical vapor transport (PVT) are scheduled to be processed inside Low Gradient Furnace (LGF) on Materials Science Research Rack (MSRR) in Material Science Laboratory (MSL) on International Space Station (ISS) starting from February 27th, 2023. The flight samples consist of three unseeded growths of ZnSe, Cr-doped ZnSe and ZnSeTe as well as growth of ZnSe on top of three single crystal ZnSe seeds with orientation of (100), (110) and (111). The main scientific objective of the flight experiments is to establish the effects of gravity-driven fluid flows on Earth to (i) the non-uniform incorporation of impurities and defects and (ii) the deviation from stoichiometry observed in the grown crystals caused by growth interface fluctuations and evolution as the results of buoyancy-driven convection and irregular fluid-flows. The investigation will also evaluate the effects of gravity on the PVT process by examining (i) the growth kinetics on various seed orientations, (ii) the dopant segregation and distribution in the Cr doped ZnSe, and (iii) the compositional segregation and distribution in the ternary ZnSeTe crystal grown by PVT. Additionally, from X-ray diffraction/topography and by measuring the density and distribution of various crystalline defects it will assess the self-induced strain effects developed during processing at elevated temperatures caused by the weight of the crystals. During the ground-based preparations, the following tasks have been accomplished: • Establish the thermodynamic properties of the ZnSe binary and related ternary systems by measuring the partial pressures of the vapor phase coexisting with the condensed phases and perform phase diagram calculations for comparison. • Evaluate the effects of gravity-driven convection in the growth process by performing experiments under various vapor transport orientations relative to gravity vector, i.e., horizontal, vertically stabilized and destabilized configurations. • Establish a quantitative correlation between growth parameters and the characteristics and properties of the grown crystals by characterizing the crystals using a variety of techniques. • Evaluate the fundamentals of the current theories on vapor transport and crystal growth kinetics by performing in-situ and real-time monitoring techniques during growth. • Develop a one-dimensional diffusion limited theory of mass transport and two- and three-dimensional numerical simulations of both mass transport and heat transfer and thus establish the microgravity requirements for the flight experiments and to predict the characteristics of the grown crystals such as the solid-vapor interface shapes… etc. and establish a fundamental understanding of the crystal growth process from the comparison with experimental results.
ZnSe↗
Binodal Colloidal Aggregation Test - 4: Polydispersion
Binodal Colloidal Aggregation Test - 4: Polydispersion (BCAT-4-Poly) will use model hard-spheres to explore seeded colloidal crystal nucleation and the effects of polydispersity, providing insight into how nature brings order out of disorder. Crewmembers photograph samples of polymer and colloidal particles (tiny nanoscale spheres suspended in liquid) that model liquid/gas phase changes. Results will help scientists develop fundamental physics concepts previously cloaked by the effects of gravity.
Chaikin, Paul M.↗
The Feasibility of Bulk Crystallization as an Industrial Purification and Production Technique for Proteins
Bulk crystallization in stirred vessels is used industrially for the recovery and purification of many inorganic and organic materials. Although much has been written on the crystallization of proteins for X-ray diffraction analysis, very little has been reported on the application of bulk crystallization in stirred vessels. In this study, a 1-liter, seeded, stirred, batch crystallizer was used with ovalbumin as a model protein to test the feasibility of this crystallization method as a recovery and purification process for proteins. Results were obtained for ovalbumin solubility, nucleation thresholds, crystal breakage and crystal growth kinetics in bulk solution under a range of operating conditions of pH and ammonium sulphate concentration (Judge et al., 1996). Experiments were also performed to determine the degree of purification that can be achieved by the crystallization of ovalbumin from a mixture of proteins. The effect of the presence of these proteins upon the ovalbumin crystal growth kinetics was also investigated (Judge et al., 1995). All of these aspects are essential for the design of bulk crystallization processes which have not previously been reported for proteins. Results from a second study that investigated the effect of structurally different proteins on the solubility, crystal growth rates and crystal purity of chicken egg white lysozyme are also presented (Judge et al., 1997). In this case face growth rates were measured using lysozyme purified by liquid chromatography and the effect of the addition of specific protein impurities were observed on the (110) and (101) crystal faces. In these two studies the results are presented to show the feasibility and purifying ability of crystallization as a production process for proteins.
Judge, Russell A.↗
Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors
Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.
Larson, D. J., Jr.↗
Crystallization of Chicken Egg White Lysozyme from Assorted Sulfate Salts
Chicken egg white lysozyme has been found to crystallize from ammonium, sodium, potassium, rubidium, magnesium, and manganese sulfates at acidic and basic pH, with protein concentrations from 60 to 190 mg/ml. Four different crystal morphologies have been obtained, depending upon the temperature, protein concentration, and precipitating salt employed, Crystals grown at 15 C were generally tetragonal, with space group P43212. Crystallization at 20 C typically resulted in the formation of orthorhombic crystals, space group P21212 1. The tetragonal much less than orthorhombic morphology transition appeared to be a function of both the temperature and protein concentration, occurring between 15 and 20 C and between 100 and 125 mg/ml protein concentration. Crystallization from 0.8 -1.2M magnesium sulfate at pH 7.6 - 8.0 gave a hexagonal (trigonal) crystal form, space group P3121, which diffracted to 2.8 A. Ammonium sulfate was also found to result in a monoclinic form, space group C2. Small twinned monoclinic crystals of approx. 0.2 mm on edge were grown by dialysis followed by seeded sitting drop crystallization.
Forsythe, Elizabeth L.↗
Te-and Zn-Doped InSb Crystals Grown in Microgravity
In 2002, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation, seven doped InSb crystals were grown in microgravity at the International Space Station. The key goals of the SUBSA investigation are: (a) to clarify the origin of the melt convection in space laboratories; (b) to reduce melt convection to the level which allows reproducible diffusion-controlled segregation; (e) to explore the submerged baffle process and liquid encapsulation in microgravity. 30 crystal growth experiments were conducted in the ground unit, to optimize the design of flight ampoules and to test the transparent SUBSA furnace developed by TecMasters Inc. The specially designed furnace, allowed observation of the crystal growth process (melting, seeding, motion of the solid-liquid interface, etc.). In the summer of 2002, eight crystal growth experiments were conducted in the Microgravity Science Glovebox (MSG) facility at the ISS. Four Te-doped (k = 0.5) and three Zn-doped (k2.9) crystals were grown on undoped seeds. In one experiment, we were not able to seed and grow. The seven grown crystals were sectioned and analyzed using SIMS. The design of the SUBSA ampoules, the segregation data and the video images obtained during the SUBSA flight experiments will be presented and discussed.
Ostrogorsky, A. G.↗
Novel Electric Nucleation Technique for Growing Large Single Crystal in Space
We present, herein, an electrical model for growing crystals without a seed which might not be free of defects and thereby still hinder the growth of a perfect crystal in space. The system is designed to confine nucleation to a single site automatically in an under saturated solution to avoid multiple nucleation. The technique is based on the effect of electrostriction, which is the tendency of a material to become more compressed in the presence of an electric field. The system is designed to create an electrical potential well between two hyperboloid electrodes with applied voltage at low frequency. The induced potential well between the electrodes oscillates at low frequency and attracts the solute and condenses it into the region of maximum field intensity. The alternating voltage prevents molecules with intrinsic charge from being attracted to the electrodes. The continuous presence of the electric field during the duration of the experiment, provides a continuous migration of the molecules toward the trapping site. This will eliminate the creation of a depletion region around the nucleation center and will enhance the crystal growth rate. Aside from the above mentioned advantages, the system is compact, safe to operate, and inexpensive to build.
Abdeldayem, Hossin↗
Project Explorer takes its second step: GAS-608 in engineering development
An a continuation of its Project Explorer series, the Alabama Space and Rocket Center is sponsoring the development of two additional Get Away Special payloads. Details are given of GAS-608, including descriptions of its six experiments in organic crystal growth, roach eggs, yeast, radish seeds, bacterial morphology, and silicon crystals. A brief summary is also presented of GAS-105 and the Space Camp program for stimulating student first hand participation in space flight studies. GAS-608 will carry six student experiments, which will involve biology, crystal growth, and biochemistry in addition to a centralized package for electronics and power supply.
Kitchens, Philip H.↗