Search NASA⌕ Search

SEARCH · Search NASA

Results for “crystal zoning”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Numerical simulations of inductive-heated float-zone growth

The present work provides an improved fluid flow and heat-transfer modeling of float-zone growth by introducing a RF heating model so that an ad hoc heating temperature profile is not necessary. Numerical simulations were carried out to study the high-temperature float-zone growth of titanium carbide single crystal. The numerical results showed that the thermocapillary convection occurring inside the molten zone tends to increase the convexity of the melt-crystal interface and decrease the maximum temperature of the molten zone, while the natural convection tends to reduce the stability of the molten zone by increasing its height. It was found that the increase of induced heating due to the increase of applied RF voltage is reduced by the decrease of zone diameter. Surface tension plays an important role in controlling the amount of induced heating. Finally, a comparison of the computed shape of the free surface with a digital image obtained during a growth run showed adequate agreement.

Chan, Y. T.↗
NASA NTRS1991

Quantitative determination of the mineral distribution in different collagen zones of calcifying tendon using high voltage electron microscopic tomography

High voltage electron microscopic tomography was used to make the first quantitative determination of the distribution of mineral between different regions of collagen fibrils undergoing early calcification in normal leg tendons of the domestic turkey, Meleagris gallopavo. The tomographic 3-D reconstruction was computed from a tilt series of 61 different views spanning an angular range of +/- 60 degrees in 2 degrees intervals. Successive applications of an interactive computer operation were used to mask the collagen banding pattern of either hole or overlap zones into separate versions of the reconstruction. In such 3-D volumes, regions specified by the mask retained their original image density while the remaining volume was set to background levels. This approach was also applied to the mineral crystals present in the same volumes to yield versions of the 3-D reconstructions that were masked for both the crystal mass and the respective collagen zones. Density profiles from these volumes contained a distinct peak corresponding only to the crystal mass. A comparison of the integrated density of this peak from each profile established that 64% of the crystals observed were located in the collagen hole zones and 36% were found in the overlap zones. If no changes in crystal stability occur once crystals are formed, this result suggests the possibilities that nucleation of mineral is preferentially and initially associated with the hole zones, nucleation occurs more frequently in the hole zones, the rate of crystal growth is more rapid in the hole zones, or a combination of these alternatives. All lead to the conclusion that the overall accumulation of mineral mass is predominant in the collagen hole zones compared to overlap zones during early collagen fibril calcification.

NASA Program Space Biology↗
NASA NTRS2001

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 (micro)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 Pepsi alloys in a detached mode and seeks to compare processing-induced defects in Bridgman, detached-Bridgman, and floating-zone growth configurations in Pepsi crystals (Si less or = 10 at%) up to 20mm in diameter.

Szofran, Frank R.↗
NASA NTRS1998

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

In growing crystals by the floating zone (FZ) technique under microgravity, the size restriction we have under earth conditions because of the hydrostatic pressure are avoided. Further, buoyancy related convection is eliminated to a high 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 improve crystal quality, tools are required to control Marangoni convection in space facilities. Applying 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 8-10mm diameter and height (Ma approximately equals 6 x 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 75mT/50Hz 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 approximately equal to 1-1.5 x 10(exp 4): temperature fluctuations up to 4C have been determined. Their frequency range was 0.1 and 0.4 Hz. Between certain thermocouple or sensor pairs, strong correlation has been detected.

Dold, P.↗
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.↗
DOE OSTI2024

Magnetic properties of the quasi-XY Shastry-Sutherland magnet ER 2 Be 2 SiO 7

Polycrystalline and single-crystal samples of the insulating Shastry-Sutherland compound Er 2 ⁢Be 2 ⁢SiO 7 were synthesized via a solid-state reaction and the floating zone method, respectively. The crystal structure, Er single-ion anisotropy, zero-field magnetic ground state, and magnetic phase diagrams along high-symmetry crystallographic directions were investigated with bulk measurement techniques, x-ray and neutron diffraction, and neutron spectroscopy. Here, we establish that Er 2 ⁢Be 2 ⁢SiO 7 crystallizes in a tetragonal space group with planes of orthogonal Er dimers and a strong preference for the Er moments to lie in the local plane perpendicular to each dimer bond. We also find that this system has a noncollinear ordered ground state in zero field with a transition temperature of 0.841 K consisting of antiferromagnetic dimers and in-plane moments. Finally, we mapped out the H-T phase diagrams for Er 2 ⁢Be 2 ⁢SiO 7 along the directions H ∥ [001], [100], and [110]. While an increasing in-plane field simply induces a phase transition to a field-polarized phase, we identify three metamagnetic transitions in the H ∥ [001] case. Single-crystal neutron diffraction results reveal that the H ∥ [001] phase diagram can be explained predominantly by the expected field-induced behavior of classical, anisotropic moments, although the microscopic origin of one phase requires further investigation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure based modeling of friction stir welded joint of dissimilar metals using crystal plasticity

We report the friction stir welding (FSW) process shows promising results in joining dissimilar metals which are otherwise almost impossible to join using traditional welding techniques. Being a new technique, the deformation and the failure mechanism of the joints made by the FSW process needs to be investigated. In this work, a joint between AZ31 Mg alloy and DP590 steel is modeled using phenomenological crystal plasticity formulation on the mesoscale in the form of a representative volume element (RVE). The interface of the two materials is modeled using a cohesive zone model. A parametric study has been performed to understand the effect of grain size and interface fracture toughness as well as strength on the mechanical performance of the joint. It was found that the grain size of AZ31 Mg alloy, as well as DP590 steel, has little effect on the overall joint performance. On the other hand, interface fracture toughness and strength have a significant impact on the mechanical properties of the joint

36 MATERIALS SCIENCE↗
DOE OSTI2021

Concentrating rare earth elements to phosphate in molten coal ash by a temperature gradient approach

Synthetic coal ash bearing 560 ppm europium oxide, blended with aluminum phosphate, was heat treated above its melting temperature and crystal evolutions with respect to europium concentration under controlled cooling were studied. The sample in a boat crucible was subjected to a temperature gradient of 100 °C across it to cause zone refining effects on crystallization behaviors in the melt (slag). Post analysis found six mineral phases formed from the melt while europium was only present in calcium phosphate, implying the majority of europium was segregated to the calcium phosphate. Europium concentrations in the calcium phosphate phase tended to be higher at zones with higher temperatures: as high as 7200 ppm, a 13-fold increase from the initial concentration.

01 COAL, LIGNITE, AND PEAT↗
NASA NTRS1990

Growth and characterization of CdS crystals

A growth method for the physical vapor transport of compound semiconductors in closed ampoules is described. With the unique techniques applied in the heat treatment of the starting materials and the temperature profiles provided by the three-zone translational furnace, large crystals of CdS have been grown successfully by the method at lower temperatures than previously used. Both unseeded and seeded growth have been investigated. The CdS crystals were examined using optical and scanning electron microscopies (SEM) to study the microstructure and the dislocation etch-pits. The crystals were further characterized by infrared (IR) and ultraviolet (UV) transmission measurements.

Su, Ching-Hua↗
NASA NTRS1984

Float zone experiments in space

The molten zone/freezing crystal interface system and all the mechanisms were examined. If Marangoni convection produces oscillatory flows in the float zone of semiconductor materials, such as silicon, then it is unlikely that superior quality crystals can be grown in space using this process. The major goals were: (1) to determine the conditions for the onset of Marangoni flows in molten tin, a model system for low Prandtl number molten semiconductor materials; (2) to determine whether the flows can be suppressed by a thin oxide layer; and (3) based on experimental and mathematical analysis, to predict whether oscillatory flows will occur in the float zone silicon geometry in space, and if so, could it be suppressed by thin oxide or nitride films. Techniques were developed to analyze molten tin surfaces in a UHV system in a disk float zone geometry to minimize buoyancy flows. The critical Marangoni number for onset of oscillatory flows was determined to be greater than 4300 on atomically clean molten tin surfaces.

Verhoeven, J. D.↗
NASA NTRS2013

Can Supersaturation Affect Protein Crystal Quality?

In quiescent environments (microgravity, capillary tubes, gels) formation of a depletion zone is to be expected, due either to limited sedimentation, density driven convection or a combination of both. The formation of a depletion zone can: Modify solution supersaturation near crystal; Give rise to impurity partitioning. It is conjectured that both supersaturation and impurity partitioning affect protein crystal quality and size. Further detailed investigations on various proteins are needed to assess above hypothesis.

Gorti, Sridhar↗
NASA NTRS1981

Modeling of the float zone process

The interaction of heat, mass, and momentum transport in the floating zone method for growing single crystals from the melt is examined. Methods for detailed numerical simulation of the transport phenomena in a floating zone are developed. Results of the calculations are combined with experiments to determine the effects of solidification induced, surface tension driven, and buoyancy driven convection in establishing dopant redistribution in the melt and the roles of heat transfer in crystal and melt and melt/solid interface shape in determining crystal quality. State of the art finite element techniques were developed for calculating the influence of natural convection in the melt on the shape of a melt/crystal interface and dopant segregation in the crystal. These techniques are demonstrated for solidification by the Bridgman technique. Numerical techniques are developed that calculate the shapes of both the melt/solid and melt/gas interfaces simultaneously with the thermal fields in melt and solid. Models for the fluid flows due to the rotation of the feed and crystal rods are completed and the effects of these flows on dopant segregation are studied, especially in the case of zones longer than can be achieved on Earth.

Brown, R. A.↗
NASA NTRS1996

Structural relations between collagen and mineral in bone as determined by high voltage electron microscopic tomography

Aspects of the ultrastructural interaction between collagen and mineral crystals in embryonic chick bone have been examined by the novel technique of high voltage electron microscopic tomography to obtain three-dimensional information concerning extracellular calcification in this tissue. Newly mineralizing osteoid along periosteal surfaces of mid-diaphyseal regions from normal chick tibiae was embedded, cut into 0.25 microns thick sections, and documented at 1.0 MV in the Albany AEI-EM7 high voltage electron microscope. The areas of the tissue studied contained electron dense mineral crystals associated with collagen fibrils, some marked by crystals disposed along their cylindrically shaped lengths. Tomographic reconstructions of one site with two mineralizing fibrils were computed from a 5 degrees tilt series of micrographs over a +/- 60 degrees range. Reconstructions showed that the mineral crystals were platelets of irregular shape. Their sizes were variable, measured here up to 80 x 30 x 8 nm in length, width, and thickness, respectively. The longest crystal dimension, corresponding to the c-axis crystallographically, was generally parallel to the collagen fibril long axis. Individual crystals were oriented parallel to one another in each fibril examined. They were also parallel in the neighboring but apparently spatially separate fibrils. Crystals were periodically (approximately 67 nm repeat distance) arranged along the fibrils and their location appeared to correspond to collagen hole and overlap zones defined by geometrical imaging techniques. The crystals appeared to be continuously distributed along a fibril, their size and number increasing in a tapered fashion from a relatively narrow tip containing smaller and infrequent crystals to wider regions having more densely packed and larger crystals. Defined for the first time by direct visual 3D imaging, these data describe the size, shape, location, orientation, and development of early crystals in normal bone collagen. The results suggest that platelet-shaped crystals are arranged in channels or grooves which are formed by collagen hole zones in register and that crystal sizes may exceed the dimensions of hole zones. Such data agree with those from mineral-matrix interaction in normally calcifying avian tendon obtained by similar high voltage tomographic means, but in addition they indicate a possible gradual and continuous deposition of crystals in collagen of bone unlike tendon and imply that individual collagen fibrils in local regions of osteoid are organized such that they all may be aligned in a coherent manner.

NASA Discipline Number 40-40↗
NASA NTRS1976

Float-zone processing in a weightless environment

The results were reported of investigations to: (1) test the validity of analyses which set maximum practical diameters for Si crystals that can be processed by the float zone method in a near weightless environment, (2) determine the convective flow patterns induced in a typical float zone, Si melt under conditions perceived to be advantageous to the crystal growth process using flow visualization techniques applied to a dimensionally scaled model of the Si melt, (3) revise the estimates of the economic impact of space produced Si crystal by the float zone method on the U.S. electronics industry, and (4) devise a rational plan for future work related to crystal growth phenomena wherein low gravity conditions available in a space site can be used to maximum benefit to the U.S. electronics industry.

Fowle, A. A.↗
NASA NTRS1979

Programs for calculating cell parameters in electron and X-ray diffraction

Ten programs for calculating cell parameters from single crystal electron diffraction patterns are presented. Most of the programs, written for use with a programmable desk calculator, are also applicable to X-ray diffraction work. The programs can be used to calculate d-spacings from electron diffraction plate measurements, and to determine cell data (including interplanar angles and zone angles) for all crystal systems. A program for rhombohedral-hexagonal conversions and one for matching crystal data from standards with apparent crystal parameters found in diffraction patterns are included. Because they allow rapid determination of data not present in X-ray listings or elsewhere in the literature, the programs facilitate identification of unknowns.

Polkowski, G.↗
NASA NTRS1989

An ion microprobe study of the intra-crystalline behavior of REE and selected trace elements in pyroxene from mare basalts with different cooling and crystallization histories

The effects of crystallization interaction on the trace element zoning characteristics of pyroxenes are analyzed using electron and ion microprobe techniques. Four pigeonite basalts with similar isochemical composition, but different cooling rates and crystallization histories are studied. Pyroxene quadrilaterals displaying crystallization trends are presented. The crystal chemical rationalization of REE zoning, pattern shapes, and abundances are examined. The data reveal that the trace element zoning characteristics in pyroxene and the partitioning of trace elements between pyroxene and the melt are related to the interaction between the efficiency of the crystallization process, the kinetics at the crystal-melt interface, the kinetics of plagioclase nucleation and the characteristics of the crystal chemical substitutions in the pyroxene and the associated crystallizing phase.

Shearer, C. K.↗
DOE OSTI2026

Small Co-doping induced magnetic and electrical transitions in single crystal CaF⁢e 0.95 ⁢C⁢o 0.05 ⁢O 3

CaFe⁢O 3 and CaF⁢e 0.95 ⁢C⁢o 0.05 ⁢O 3 single crystals were grown by combing floating-zone method with high oxygen pressure treatment. Both crystals show charge disproportionation of Fe (F⁡e 4+ → F⁡e 3+ + F⁡e 5+ ) accompanied by a metal-to-insulator transition as well as a crystal structural transformation from Pbnm to 𝑃⁢2 1 /𝑛. However, the slight introduction of Co significantly suppresses the critical temperature of charge disproportionation from 290 K in CaFe⁢O 3 to 260 K in CaF⁢e 0.95 ⁢C⁢o 0.05 ⁢O 3 . Different from the single antiferromagnetic phase transition as observed in the polycrystalline CaFe⁢O 3 , two sequential antiferromagnetic transitions are found to occur in these two single crystals with the Néel temperatures around 119 and 112 K for CaFe⁢O 3 crystal and 109 and 98 K for CaF⁢e 0.95 ⁢C⁢o 0.05 ⁢O 3 crystal, respectively. Neutron diffraction illustrates the formation of a spiral antiferromagnetic structure. Moreover, as the temperature further decreases to 65 K, a third magnetic transition accompanied by a second electrical transition is observed in the slightly Co-doped CaF⁢e 0.95 ⁢C⁢o 0.05 ⁢O 3 crystal. In conclusion, first-principles calculations suggest that the introduction of a moderate amount of Co and the peculiar spiral spin texture play an important role in the presence of such new magnetic and electrical transitions.

Xia, Hailiang [Chinese Academy of Sciences (CAS), ↗
DOE OSTI2023

Influence of Light Atoms on Quantification of Atomic Column Positions in Distorted Perovskites with HAADF-STEM

Measurement of picometer-scale atomic displacements by aberration-corrected STEM has become invaluable in the study of crystalline materials, where it can elucidate ordering mechanisms and local heterogeneities. HAADF-STEM imaging, often used for such measurements due to its atomic number contrast, is generally considered insensitive to light atoms such as oxygen. Light atoms, however, still affect the propagation of the electron beam in the sample and, therefore, the collected signal. In this work, we demonstrate experimentally and through simulations that cation sites in distorted perovskites can appear to be displaced by several picometers from their true positions in shared cation-anion columns. The effect can be decreased through careful choice of sample thickness and beam voltage or can be entirely avoided if the experiment allows reorientation of the crystal along a more favorable zone axis. Therefore, it is crucial to consider the possible effects of light atoms and crystal symmetry and orientation when measuring atomic positions.

36 MATERIALS SCIENCE↗