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At least 451 records · Page 25

Process and apparatus for growing a crystal ribbon

A process and apparatus is disclosed for growing a crystal ribbon of a substance of theoretically infinite length from a melt of the substance. A pair of fixedly positioned edge defining members are partially submerged into the melt so as to break the surface of the melt at a predetermined distance from one another. The edge defining members are wettable by the melt and the predetermined distance substantially corresponds to the width of the crystal ribbon to be grown. The crystal ribbon is grown by contacting the surface of the melt with a seed ribbon between the edge defining members whereby a meniscus of the melt is established on the seed ribbon. The meniscus is stabilized by the meniscus of the melt on the edge defining members. Pulling the seed crystal ribbon away from the melt results in continuous growth of the crystal ribbon.

Thornhill, J. W.↗

The use of moments of momentum to account for crystal habits

A three-step theory of crystal growth is proposed which involves first an association of molecules or ions in solution to form an impinging growth unit, then second the orientation of this unit prior to its impact on the surface of a crystal, and finally the attachment of this unit to the crystal face. From this theory the habit of a crystal is dependent upon the moments of momentum of the impinging growth unit. The results of sample calculations are presented or sodium chloride, succinic acid, sucrose, and chromium boride. The faces predicted by this proposed theory are compared with those predicted by other, energy-based calculations and with those experimentally observed. The proposed theory suggests alternative strategies for crystallization and habit modification which may be of technological importance. Listings of the two computer programs that were used are provided.

Barber, P. G.↗

Morphological Stability and Fluid Dynamics of Vapor Crystal Growth

A fundamental understanding of the conditions under which crystals can retain morphological stability, i.e., shape stability of the advancing interface, during growth from vapors was studied. Morphological stability (MS) is a necessary condition for the growth of homogeneous single crystals required for numerous device applications. For crystallization from melts, the MS concepts are well developed and are essentially based on heat and mass transfer conditions about the advancing interface. For crystallization from vapors, the MS requirements are more complex and not well understood. The added complexity arises from the fact that anisotropies in interfacial kinetics are typically stronger in crystallization from vapors than from melts. These pronounced anisotropies root in the distinctly lower atomic roughness of most vapor-solid interfaces.

Rosenberger, F.↗

Low-cost single-crystal turbine blades, volume 2

The overall objectives of Project 3 were to develop the exothermic casting process to produce uncooled single-crystal (SC) HP turbine blades in MAR-M 247 and higher strength derivative alloys and to validate the materials process and components through extensive mechanical property testing, rig testing, and 200 hours of endurance engine testing. These Program objectives were achieved. The exothermic casting process was successfully developed into a low-cost nonproperietary method for producing single-crystal castings. Single-crystal MAR-M 247 and two derivatives DS alloys developed during this project, NASAIR 100 and SC Alloy 3, were fully characterized through mechanical property testing. SC MAR-M 247 shows no significant improvement in strength over directionally solidified (DS) MAR-M 247, but the derivative alloys, NASAIR 100 and Alloy 3, show significant tensile and fatigue improvements. Firtree testing, holography, and strain-gauge rig testing were used to determine the effects of the anisotropic characteristics of single-crystal materials. No undesirable characteristics were found. In general, the single-crystal material behaved similarly to DS MAR-M 247. Two complete engine sets of SC HP turbine blades were cast using the exothermic casting process and fully machined. These blades were successfully engine-tested.

Strangman, T. E.↗

Interface shape in Czochralski grown crystals - Effect of conduction and radiation

A sequential modular computational scheme has been proposed for the calculation of temperature profiles in the melt and crystal including the melt-crystal interface shape and the crystal pulling rate for a fixed crystal radius. The heat transfer in the melt is assumed to occur by conduction only. The shape of melt-gas meniscus, described by Laplace-Young equation, is incorporated in the model and its effects on interface shape and pulling rate are examined. Further, the model incorporates the detailed radiation interaction among the various surfaces in the puller using the Gebhart enclosure theory which accounts for both direct and reflected radiation. The effects of various process parameters on the interface shape and the pulling rate have been investigated. The results of this study indicate that the shape of the melt-gas meniscus has a significant effect on the pulling rate and the interface shape in conformity with earlier studies. Further, it is shown that a simple radiation model (Stefan's model) is inadequate to model the radiation heat exchange in the Czochralski puller apparatus and the detailed Gebhart analysis is necessary for accurate calculation of both the temperature profile in the crystal as well as the interface shape.

Srivastava, R. K.↗

The crystallization of small particles and droplets

A general expression is derived for the volume fraction of material crystallized as a function of time for the situation where boundary effects may be important, and it is applied to a sample consisting of a monodisperse array of small particles. It is assumed that crystallization occurs via homogeneous nucleation followed by crystal growth. The crystallization rate is shown to be controlled by a single dimensionless parameter, beta. Beta exp 1/4 is a dimensionless particle radius which tends to be small when the growth rate is large or when the nucleation rate is small. When beta is large, the general expression for the volume fraction transformed reduces to the standard expression valid for bulk samples. When beta is small, it reduces to the formula used to compute the volume fraction crystallized in droplet undercooling experiments. Hence, the present results are pertinent for the interpretation of some droplet undercooling experiments as well as isothermal DSC and DTA experiments.

Weinberg, M. C.↗

High-purity silicon crystal growth investigations

Information is given on evaporation and segregation contributions to impurity profiles of floating zone crystals (FZ); high-purity silicon float zoning (FZ); minority-carrier lifetime measurement of heavily doped silicon crystals; the effect of some crystal growth parameters on minority-carrier lifetime; and defect investigations by X-ray topography in graphical and tabular form. It was concluded that evaporation contributes substantially to impurity reduction when FZ or cold-crucible growth is conducted in a vacuum; boron and gallium may be more favorable dopants than indium or aluminum for obtaining high minority-carrier lifetimes; minority-carrier lifetimes greater than 100 microseconds are feasible at a 2 times 10 to the 17th power cm-3 doping level; minority-carrier lifetime decreases with increasing crystal cooling rate and also with the presence of dislocations; the method used to clean silicon feed rods affects lifetime; and microdefect densities in dislocation-free FZ crystals appear to be lower with Ga doping than with B doping.

Ciszek, T. F.↗

Preliminary investigations of protein crystal growth using the Space Shuttle

Four preliminary Shuttle experiments are described which have been used to develop prototype hardware for a more advanced system that will evaluate effects of gravity on protein crystal growth. The first phase of these experiments has centered on the development of micromethods for protein crystal growth by vapor-diffusion techniques (using a space version of the hanging-drop method) and on dialysis using microdialysis cells. Results suggest that the elimination of density-driven sedimentation can effect crystal morphology. In the dialysis experiment, space-grown crystals of concanavalin B were three times longer and 1/3 the thickness of earth-grown crystals.

Delucas, L. J.↗

Crystallization of baria-titania-silica glasses

The critical cooling rate for glass formation, Rc, and the crystallization kinetics of the compositions (1/2)(100-x)BaO-(1/2)(100-x)TiO2-(x)SiO2 with x = 20, 25, 30, 33.3, and 40 mol pct were studied using a thermal image furnace. Crystallization was studied under nonisothermal conditions, and the data were analyzed using the Johnson-Mehl-Avrami equation. The Rc and activation energy for crystallization both decrease with increasing silica content. Fresnoite, Ba2TiSi2O8, crystallized from all of the glasses when they were reheated. The infrared absorption spectra of the glasses and crystals show that they both contain (Si2O7) and square pyramidal (TiO5) groups.

Ray, Chandra S.↗

The crystallization of tough thermoplastic resins in the presence of carbon fibers

The presence of carbon fibers increased the crystallization rates of both PEEK and PPS thermoplastic polymers. The effect was most pronounced at higher crystallization temperatures. Isothermal crystallization rates were analyzed by applying classical phenomenological nucleation theory. Unusually high values of the so-called Avrami exponent were found for neat PEEK. Isothermal crystallization of PEEK and PPS polymers produced crystalline samples having a wide variety of melting temperatures. The melting as observed by differential scanning calorimetry occurred as dual endotherms which were called primary (higher temperature) and secondary melting peaks. Each primary peak accounted for most of the crystallinity present. The secondary peaks represented the melting of crystallites formed later than those attributable to the primary endotherms. The presence of carbon fibers increased the thermal stability of both PEEK and PPS crystallites as manifested by higher temperatures for the primary melting peaks. This may be attributable to increased crystallite size, greater crystallite perfection, and/or favorable modification of the crystallite interface. Over the range studied, crystallization temperature strongly influenced the positions of the secondary peaks but not the primary peaks.

Theil, Michael H.↗

A simple apparatus for controlling nucleation and size in protein crystal growth

A simple device is described for controlling vapor equilibrium in macromolecular crystallization as applied to the protein crystal growth technique commonly referred to as the 'hanging drop' method. Crystal growth experiments with hen egg white lysozyme have demonstrated control of the nucleation rate. Nucleation rate and final crystal size have been found to be highly dependent upon the rate at which critical supersaturation is approached. Slower approaches show a marked decrease in the nucleation rate and an increase in crystal size.

Gernert, Kim M.↗

Non-isothermal crystallization of poly(etheretherketone) aromatic polymer composite

The nonisothermal crystallization kinetics of PEEK APC-2 and of 450G neat resin PEEK material were compared using a differential scanning calorimeter to monitor heat flow during crystallization; the effects of cooling rate on the crystallization temperature, the degree of crystallinity, and the conversion rate were investigated. A modified Avrami (1940) analysis was used to describe nonisothermal crystallization kinetics. It was found that, compared with the 450G neat resin PEEK, the nonisothermal crystallization of the PEEK APC-2 composite is characterized by higher initiation temperature, higher heat flow maximum temperature, and greater relative conversion by primary processes.

Cebe, Peggy↗

Protein crystal growth in low gravity

The solubility and growth of the protein canavalin, and the application of the schlieren technique to study fluid flow in protein crystal growth systems were investigated. These studies have resulted in the proposal of a model to describe protein crystal growth and the preliminary plans for a long-term space flight experiment. Canavalin, which may be crystallized from a basic solution by the addition of hydrogen (H+) ions, was shown to have normal solubility characteristics over the range of temperatures (5 to 25 C) and pH (5 to 7.5) studies. The solubility data combined with growth rate data gathered from the seeded growth of canavalin crystals indicated that the growth rate limiting step is a screw dislocation mechanism. A schlieren apparatus was constructed and flow patterns were observed in Rochelle salt (sodium potassium tartrate), lysozyme, and canavalin. The critical parameters were identified as the change in density with concentration (dp/dc) and the change in index of refraction with concentration (dn/dc). Some of these values were measured for the materials listed. The data for lyrozyme showed non-linearities in plots of optical properties and density vs. concentration. In conjunction with with W. A. Tiller, a model based on colloid stability theory was proposed to describe protein crystallization. The model was used to explain observations made by ourselves and others. The results of this research has lead to the development for a preliminary design for a long-term, low-g experiment. The proposed apparatus is univeral and capable of operation under microprocessor control.

Feigelson, Robert S.↗

Dynamic crystallization experiments on chondrule melts in reduced gravity

Chondrules crystallized during the earliest formational history of the solar system; and, if crystal settling and flotation are indicators of crystallization in the presence of gravity, they formed without the influence of gravity. In fact, attempts to duplicate the crystallization history of chondrules in the laboratory have met with limited success, because of the difficulty of comparing objects formed under the influence of gravity with objects that did not. These comparisons are difficult because there are several recognized features introduced by the presence of gravity and no doubt some which are not yet recognized. As a result there are several microscale and macroscale aspects of chondrule petrology which are difficult to understand quantitatively. Most of the features relate to the settling or flotation of early formed crystals. The proposed experiments are briefly described.

Lofgren, Gary↗

The glass transition, crystallization and melting in Au-Pb-Sb alloys

The glass transition, crystallization and melting of Au(55)Pb(22.5)Sb(22.5) alloys have been studied by differential scanning calorimetry DSC. Crystallization on heating above the glass transition temperature Tg (45 C) begins at 64 C. Further crystallization events are observed at 172 C and 205 C. These events were found to correspond to the formation of the intermetallic compounds AuSb2, Au2Pb, and possibly AuPb2, respectively. Isothermal DSC scans of the glassy alloy above Tg were used to monitor the kinetics of crystallization. The solidification behavior and heat capacity in the glass-forming composition range were determined with droplet samples. An undercooling level of 0.3T(L) below the liquidus temperature T(L) was achieved, resulting in crystallization of different stable and metastable phases. The heat capacity C(P) of the undercooled liquid was measured over an undercooling range of 145 C.

Lee, M. C.↗

Solar radiative transfer in cirrus clouds. I - Single-scattering and optical properties of hexagonal ice crystals. II - Theory and computations of multiple scattering in an anisotropic medium

The light scattering and absorption programs of Cai and Liou (1982) and Takano and Jaweera (1985) are extended to include hexagonal ice crystals randomly and horizontally oriented in space. The scattering and polarization results for the ice crystals are calculated. The results are compared with measurement data. The single-scattering properties for horizontally oriented columns and plates are presented and used to explain halos and arcs observed in the atmopshere. In the second section, the theory and computations for multiple scattering in cirrus clouds containing oriented ice crystals are presented. The radiative transfer in clouds composed of horizontally oriented ice crystals is formulated. Also, reflected and transmitted intensities, planetary albedo, and polarization in multiple scattering by ice crystals are discussed.

Takano, Yoshihide↗

Effects of furnace temperature profile on the interface shape during Bridgman crystal growth

The effects of asymmetry in furnace temperature profile and pulling velocity on the crystal interface shape are demonstrated while neglecting the latent heat of solidification. It is concluded that the furnace temperature profile may be varied in order to influence the interface shape of the crystal. An exact thermal analysis is performed on the Bridgman technique by including the latent heat of solidification as a source term. The exact temperature field is obtained for the case of a flat melt-crystal interface. The earlier observation regarding the influence of furnace temperature profile on the crystal interface shape is confirmed and a criterion for a flat crystal interface is obtained. Various furnace temperature profiles are selected and their corresponding results are presented.

Taghavi, K.↗

Human serum albumin crystals and method of preparation

Human serum albumin (HSA) crystals are provided in the form of tetragonal plates having the space groups P42(sub 1)2, the crystals being grown to sizes in excess of 0.5 mm in two dimensions and a thickness of 0.1 mm. Growth of the crystals is carried out by a hanging drop method wherein a precipitant solution containing polyethylene glycol (PEG) and a phosphate buffer is mixed with an HSA solution, and a droplet of mixed solution is suspended over a well of precipitant solution. Crystals grow to the desired size in 3 to 7 days. Concentration of reagents, pH and other parameters are controlled within prescribed limits. The resulting crystals exhibit a size and quality such as to allow performance of x ray diffraction studies and enable the conduct of drug binding studies as well as genetic engineering studies.

Carter, Daniel C.↗