High-pressure floating-zone growth of perovskite nickelate LaNiO 3 single crystals

DOE PAGES

Zhang, Junjie; Zheng, Hong; Ren, Yang; ...

2017-04-07

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

Numerical simulation of plagioclase rim growth during magma ascent at Bezymianny Volcano, Kamchatka

NASA Astrophysics Data System (ADS)

Gorokhova, N. V.; Melnik, O. E.; Plechov, P. Yu.; Shcherbakov, V. D.

2013-08-01

Slow CaAl-NaSi interdiffusion in plagioclase crystals preserves chemical zoning of plagioclase in detail, which, along with strong dependence of anorthite content in plagioclase on melt composition, pressure, and temperature, make this mineral an important source of information on magma processes. A numerical model of zoned crystal growth is developed in the paper. The model is based on equations of multicomponent diffusion with diagonal cross-component diffusion terms and accounts for mass conservation on the melt-crystal interface and growth rate controlled by undercooling. The model is applied to the data of plagioclase rim zoning from several recent Bezymianny Volcano (Kamchatka) eruptions. We show that an equilibrium growth model cannot explain crystallization of naturally observed plagioclase during magma ascent. The developed non-equilibrium model reproduced natural plagioclase zoning and allowed magma ascent rates to be constrained. Matching of natural and simulated zoning suggests ascent from 100 to 50 MPa during 15-20 days. Magma ascent rate from 50 MPa to the surface varies from eruption to eruption: plagioclase zoning from the December 2006 eruption suggests ascent to the surface in less than 1 day, whereas plagioclase zoning from March 2000 and May 2007 eruptions are better explained by magma ascent over periods of more than 30 days). Based on comparison of diffusion coefficients for individual elements a mechanism of atomic diffusion during plagioclase crystallization is proposed.

Crystal growth and crystallography

NASA Technical Reports Server (NTRS)

Chernov, A. A.

1998-01-01

Selected topics that may be of interest for both crystal-structure and crystal-growth communities are overviewed. The growth of protein crystals, along with that of some other compounds, is one of the topics, and recent insights into related phenomena are considered as examples of applications of general principles. The relationship between crystal growth shape and structure is reviewed and an attempt to introduce semiquantitative characterization of binding for proteins is made. The concept of kinks for complex structures is briefly discussed. Even at sufficiently low supersaturations, the fluctuation of steps may not be sufficient to implement the Gibbs-Thomson law if the kink density is low enough. Subsurface ordering of liquids and growth of rough interfaces from melts is discussed. Crystals growing in microgravity from solution should be more perfect if they preferentially trap stress-inducing impurities, thus creating an impurity-depleted zone around themselves. Evidently, such a zone is developed only around the crystals growing in the absence of convection. Under terrestrial conditions, the self-purified depleted zone is destroyed by convection, the crystal traps more impurity and grows stressed. The stress relief causes mosaicity. In systems containing stress-inducing but poorly trapped impurities, the crystals grown in the absence of convection should be worse than those of their terrestrial counterparts.

Mechanism of abnormally slow crystal growth of CuZr alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, X. Q.; Lü, Y. J., E-mail: yongjunlv@bit.edu.cn; State Key Laboratory of Silicon Materials, Zhejiang University, Hangzhou 310027

2015-10-28

Crystal growth of the glass-forming CuZr alloy is shown to be abnormally slow, which suggests a new method to identify the good glass-forming alloys. The crystal growth of elemental Cu, Pd and binary NiAl, CuZr alloys is systematically studied with the aid of molecular dynamics simulations. The temperature dependence of the growth velocity indicates the different growth mechanisms between the elemental and the alloy systems. The high-speed growth featuring the elemental metals is dominated by the non-activated collision between liquid-like atoms and interface, and the low-speed growth for NiAl and CuZr is determined by the diffusion across the interface. Wemore » find that, in contrast to Cu, Pd, and NiAl, a strong stress layering arisen from the density and the local order layering forms in front of the liquid-crystal interface of CuZr alloy, which causes a slow diffusion zone. The formation of the slow diffusion zone suppresses the interface moving, resulting in much small growth velocity of CuZr alloy. We provide a direct evidence of this explanation by applying the compressive stress normal to the interface. The compression is shown to boost the stress layering in CuZr significantly, correspondingly enhancing the slow diffusion zone, and eventually slowing down the crystal growth of CuZr alloy immediately. In contrast, the growth of Cu, Pd, and NiAl is increased by the compression because the low diffusion zones in them are never well developed.« less

Self-adjusted flux for the traveling solvent floating zone growth of YBaCuFeO5 crystal

NASA Astrophysics Data System (ADS)

Lai, Yen-Chung; Shu, Guo-Jiun; Chen, Wei-Tin; Du, Chao-Hung; Chou, Fang-Cheng

2015-03-01

A modified traveling solvent floating zone (TSFZ) technique was used to successfully grow a large size and high quality single crystal of multiferroic material YBaCuFeO5. This modified TSFZ growth uses a stoichiometric feed rod and pure copper oxide as the initial flux without prior knowledge of the complex phase diagram involving four elements, and the optimal flux for the growth of incongruently melt crystal is self-adjusted after a prolonged stable pulling. The wetting of the feed rod edge that often perturbs the molten zone stability was avoided by adding 2 wt% B2O3. The optimal flux concentration for the YBaCuFeO5 growth can be extracted to be near YBaCuFeO5:CuO=13:87 in molar ratio. The crystal quality was confirmed by the satisfactory refinement of crystal structure of space group P4mm and the two consecutive anisotropic antiferromagnetic phase transitions near 455 K and 170 K.

The study of single crystals for space processing and the effect of zero gravity

NASA Technical Reports Server (NTRS)

Lal, R. B.

1975-01-01

A study was undertaken to analyze different growth techniques affected by a space environment. Literature on crystal growth from melt, vapor phase and float zone was reviewed and the physical phenomena important for crystal growth in zero-gravity environment was analyzed. Recommendations for potential areas of crystal growth feasible for space missions are presented and a bibliography of articles in the area of crystal growth in general is listed.

Coalescence growth mechanism of ultrafine metal particles

NASA Astrophysics Data System (ADS)

Kasukabe, S.

1990-01-01

Ultrafine particles produced by a gas-evaporation technique show clear-cut crystal habits. The convection of an inert gas makes distinct growth zones in a metal smoke. The coalescence stages of hexagonal plates and multiply twinned particles are observed in the outer zone of a smoke. A model of the coalescence growth of particles with different crystal habits is proposed. Size distributions can be calculated by counting the ratio of the number of collisions by using the effective cross section of collisions and the existence probability of the volume of a particle. This simulation model makes clear the effect on the growth rate of coalescence growth derived from crystal habit.

Float-zone processing in a weightless environment

NASA Technical Reports Server (NTRS)

Fowle, A. A.; Haggerty, J. S.; Perron, R. R.; Strong, P. F.; Swanson, J. L.

1976-01-01

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.

Analytics of crystal growth in space

NASA Technical Reports Server (NTRS)

Wilcox, W. R.; Chang, C. E.; Shlichta, P. J.; Chen, P. S.; Kim, C. K.

1974-01-01

Two crystal growth processes considered for spacelab experiments were studied to anticipate and understand phenomena not ordinarily encountered on earth. Computer calculations were performed on transport processes in floating zone melting and on growth of a crystal from solution in a spacecraft environment. Experiments intended to simulate solution growth at micro accelerations were performed.

Thermocapillary convection in zone-melting crystal growth - An open-boat physical simulation

NASA Technical Reports Server (NTRS)

Kim, Y. J.; Kou, Sindo

1989-01-01

Thermocapillary convection in a molten zone of NaNO3 contained in a boat with a free horizontal surface, that is heated from above by a centered wire heater, was studied to simulate flow in zone-melting crystal growth. Using a laser-light-cut technique and fine SiO powder as a tracer, convection in the melt zone was visualized in two different cases. In the first case, the entire melt surface was free, while in the second the melt surface was free only in the immediate vicinity of one vertical wall and was covered elsewhere, this wall being to simulate the melt/crystal interface during crystal growth. It was observed that thermocapillary convection near this wall prevailed in the first case, but was reduced significantly in the second. Since thermocapillary rather than natural convection dominated in the melt, the effect of the partial covering of the melt surface on thermocapillary convection in the melt observed in this study is expected to be similar under microgravity.

Growth Defects in Biomacromolecular Crystals

NASA Technical Reports Server (NTRS)

2003-01-01

NASA's ground based program confirmed close similarity between protein and small molecules crystal growth, but also revealed essential differences. No understanding exists as to why and when crystals grown in space are, in approx. 20 percent of cases, of higher quality. More rationale is needed in flight experiments. Ferritin crystals grown in space are 2.5 times cleaner than their terrestrial counterparts. This may occur because of the existence of a zone depleted with respect to impurities around a crystal growing in stagnant solution. This zone should appear since the distribution coefficient for homologous impurities exceeds unity. This impurity depletion zone hypothesis requires verification and development. Thorough purification from homologous impurities brought about resolution improvement from 2.6 to 1.8 angstroms for ferritin and from 2.6 to 2.0 angstroms for canavalin.

Utilizing Controlled Vibrations in a Microgravity Environment to Understand and Promote Microstructural Homogeneity During Floating-Zone Crystal Growth

NASA Technical Reports Server (NTRS)

Grugel, Richard N.

1999-01-01

It has been demonstrated in floating-zone configurations utilizing silicone oil and nitrate salts that mechanically induced vibration effectively minimizes detrimental, gravity independent, thermocapillary flow. The processing parameters leading to crystal improvement and aspects of the on-going modeling effort are discussed. Plans for applying the crystal growth technique to commercially relevant materials, e.g., silicon, as well as the value of processing in a microgravity environment are presented.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Cobb, Sharon D.; Croell, Anne; Dold, P.; Motafef, S.; Schweizer, M.; Volz, Martin P.; Walker, J. S.

2003-01-01

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.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Cobb, Sharon D.; Croell, Arne; Dold, Peter; Kaiser, Natalie; Motakef, Shariar; Schweizer, Marcus; Volz, Martin P.; Vujisic, Ljubomir

2001-01-01

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.

Controllable Growth of Monolayer MoS2 and MoSe2 Crystals Using Three-temperature-zone Furnace

NASA Astrophysics Data System (ADS)

Zheng, Binjie; Chen, Yuanfu

2017-12-01

Monolayer molybdenum disulfide (MoS2) and molybdenum diselenide (MoSe2) have attracted a great attention for their exceptional electronic and optoelectronic properties among the two dimensional family. However, controllable synthesis of monolayer crystals with high quality needs to be improved urgently. Here we demonstrate a chemical vapor deposition (CVD) growth of monolayer MoS2 and MoSe2 crystals using three-temperature-zone furnace. Systematical study of the effects of growth pressure, temperature and time on the thickness, morphology and grain size of crystals shows the good controllability. The photoluminescence (PL) characterizations indicate that the as-grown monolayer MoS2 and MoSe2 crystals possess excellent optical qualities with very small full-width-half-maximum (FWHM) of 96 me V and 57 me V, respectively. It is comparable to that of exfoliated monolayers and reveals their high crystal quality. It is promising that our strategy should be applicable for the growth of other transition metal dichalcogenides (TMDs) monolayer crystals.

Investigation on the growth and characterization of 4-aminobenzophenone single crystal by the vertical dynamic gradient freeze technique

NASA Astrophysics Data System (ADS)

Prabhakaran, SP.; Ramesh Babu, R.; Sukumar, M.; Bhagavannarayana, G.; Ramamurthi, K.

2014-03-01

Growth of bulk single crystal of 4-Aminobenzophenone (4-ABP) from the vertical dynamic gradient freeze (VDGF) setup designed with eight zone furnace was investigated. The experimental parameters for the growth of 4-ABP single crystal with respect to the design of VDGF setup are discussed. The eight zones were used to generate multiple temperature gradients over the furnace, and video imaging system helped to capture the real time growth and solid-liquid interface. 4-ABP single crystal with the size of 18 mm diameter and 40 mm length was grown from this investigation. Structural and optical quality of grown crystal was examined by high resolution X-ray diffraction and UV-visible spectral analysis, respectively and the blue emission was also confirmed from the photoluminescence spectrum. Microhardness number of the crystal was estimated at different loads using Vicker's microhardness tester. The size and quality of single crystal grown from the present investigation are compared with the vertical Bridgman grown 4-ABP.

Self-tuning multivariable pole placement control of a multizone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, C.; Sharpless, R. B.; Duval, W. M. B.; Rosenthal, B. N.

1992-01-01

This paper presents the design and implementation of a multivariable self-tuning temperature controller for the control of lead bromide crystal growth. The crystal grows inside a multizone transparent furnace. There are eight interacting heating zones shaping the axial temperature distribution inside the furnace. A multi-input, multi-output furnace model is identified on-line by a recursive least squares estimation algorithm. A multivariable pole placement controller based on this model is derived and implemented. Comparison between single-input, single-output and multi-input, multi-output self-tuning controllers demonstrates that the zone-to-zone interactions can be minimized better by a multi-input, multi-output controller design. This directly affects the quality of crystal grown.

Growth of single crystalline delafossite LaCuO2 by the travelling-solvent floating zone method

NASA Astrophysics Data System (ADS)

Mohan, A.; Büchner, B.; Wurmehl, S.; Hess, C.

2014-09-01

Single crystals of LaCuO2 have been grown for the first time using the travelling-solvent floating zone method. The crystal was grown in an Ar-atmosphere by reduction of La2Cu2O5, which was used as the feed rod composition for the growth. The grown crystal has been characterized with regard to phase purity and single crystallinity using powder X-ray diffraction, energy dispersive X-ray analysis, Laue diffraction and scanning electron microscopy.

Growth of CdZnTe Crystals the Bridgman Technique with Controlled Overpressures of Cd

NASA Technical Reports Server (NTRS)

Su, Ching-Hu; Lehoczky, S. L.

2008-01-01

Cd(1-x)Zn(x)Te crystals with x = 0.15 and 0.20, were grown in this study by closed-ampoule directional solidification (Bridgman) technique with a controlled Cd overpressure. The growth ampoule was made of quartz with inner diameter from 20 to 40 mm and a tapered length of 2.5 cm at the growth tip. Both unseeded and seeded growths were performed with total material charges up to 400 g. After the loading of starting CdZnTe material, a typical amount of 2 g of Cd was also loaded inside a Cd reservoir basket, which was attached beneath the seal-off cup. The ampoule was sealed off under a vacuum below lxl0(exp -5) Torr. The sealed ampoule was placed inside a 4-zone Bridgman furnace - a Cd reservoir zone with a heat-pipe furnace liner on the top, followed by a hot zone, a booster heating zone and a cold zone at the bottom. The Cd zone was typically 300 to 400 C below the hot zone setting. High resistivity material has been obtained without any intentional dopants but has been reproducibly obtained with In doping. The crystalline and the electrical properties of the crystals will be reported.

The significance of intergranular diffusion to the mechanisms and kinetics of porphyroblast crystallization

NASA Astrophysics Data System (ADS)

Carlson, William D.

1989-09-01

The spatial disposition, compositional zoning profiles, and size distributions of garnet crystals in 11 specimens of pelitic schist from the Picuris Range of New Mexico (USA) demonstrate that the kinetics of intergranular diffusion controlled the nucleation and growth mechanisms of porphyroblasts in these rocks. An ordered disposition of garnet centers and a significant correlation between crystal radius and near-neighbor distances manifest suppressed nucleation of new crystals in diffusionally depleted zones surrounding pre-existing crystals. Compositional zoning profiles require diffusionally controlled growth, the rate of which increases exponentially as temperature increases with time; an acceleration factor for growth rate can be estimated from a comparison of compositional profiles for crystals of different sizes in each specimen. Crystal size distributions are interpreted as the result of nucleation rates that accelerate exponentially with increasing temperature early in the crystallization process, but decline in the later stages because of suppression effects in the vicinity of earlier-formed nuclei. Simulations of porphyroblast crystallization, based upon thermally accelerated diffusionally influenced nucleation kinetics and diffusionally controlled growth kinetics, quantitatively replicate textural relations in the rocks. The simulations employ only two variable parameters, which are evaluated by fitting of crystal size distributions. Both have physical significance. The first is an acceleration factor for nucleation, with a magnitude reflecting the prograde increase during the nucleation interval of the chemical affinity for the reaction in undepleted regions of the rock. The second is a measure of the relative sizes of the porphyroblast and the diffusionally depleted zone surrounding it. Crystal size distributions for the Picuris Range garnets correspond very closely to those in the literature from a variety of other localities for garnet and other minerals. The same kinetic model accounts quantitatively for crystal size distributions of porphyroblastic garnet, phlogopite, sphene, and pyroxene in rocks from both regional and contact metamorphic occurrences. These commonalities indicate that intergranular diffusion may be the dominant kinetic factor in the crystallization of porphyroblasts in a wide variety of metamorphic environments.

Numerical simulations of inductive-heated float-zone growth

NASA Technical Reports Server (NTRS)

Chan, Y. T.; Choi, S. K.

1992-01-01

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.

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croell, A.

2012-01-01

This investigation involves the comparison of results achieved from three types of crystal growth of germanium and germanium-silicon alloys: (1) Float zone growth (2) Bridgman growth (3) Detached Bridgman growth crystal The fundamental goal of the proposed research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon (GeSi) crystals (silicon concentration in the solid up to 5 at%) for three different growth configurations in order to quantitatively assess the improvements of crystal quality possible by detached growth.

The Universal Multizone Crystallizator (UMC) Furnace: An International Cooperative Agreement

NASA Technical Reports Server (NTRS)

Watring, D. A.; Su, C.-H.; Gillies, D.; Roosz, T.; Babcsan, N.

1996-01-01

The Universal Multizone Crystallizator (UMC) is a special apparatus for crystal growth under terrestrial and microgravity conditions. The use of twenty-five zones allows the UMC to be used for several normal freezing growth techniques. The thermal profile is electronically translated along the stationary sample by systematically reducing the power to the control zones. Elimination of mechanical translation devices increases the systems reliability while simultaneously reducing the size and weight. This paper addresses the UMC furnace design, sample cartridge and typical thermal profiles and corresponding power requirements necessary for the dynamic gradient freeze crystal growth technique. Results from physical vapor transport and traveling heater method crystal growth experiments are also discussed.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Benz, K. W.; Cobb, S. D.; Croell, A.; Dold, P.; Kaiser, N.; Motakel, S.; Walker, J. S.

2000-01-01

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.

The History of a Plutonic-Volcanic System Determined from Compositional and Mineral Inclusion Mapping of Alkali Feldspar Megacrysts

NASA Astrophysics Data System (ADS)

Belfanti, S. A. D.; Gualda, G. A. R.

2017-12-01

Alkali-feldspar megacrysts (2-20 cm long) occur in many granitic rocks, providing extensive records of crystallization within magma bodies. We will use megacrysts from Yosemite National Park's Tuolumne Intrusive Suite to determine if and how megacrysts record recharge and eruption. Preliminary work has focused on 4 crystals. Based on BSE patterns, crystals can be divided into 3 zones: (1) the core, which represents the crystal's first growth and sometimes displays some resorption; (2) the interior, including a series of sub-zones that correspond to different growth periods; and (3) the rim, or outermost growth stage. Common BSE patterns include decreasing brightness from the inner portion of a growth period outward, increasing brightness towards either side of a boundary, and periods of constant brightness, for a full or partial period. Most mineral inclusions appear as single crystals ( 10-25%) or as groups of 2-4 crystals ( 60-75%). Large clusters of 10 or more individuals are less common ( 5-15%), and clusters of >20 crystals are rare ( 1-3%). Most crystals (85-95%) occur on growth boundaries or within the core. Magnetite is common in the more central parts of the interior zone, appearing only occasionally in the core and towards the rim. Accessories, amphibole, and biotite are more evenly distributed within the megacryst. Biotite and titanite grains large enough to display habit appear to be within 20 degrees of parallel with zone boundaries. Most other inclusions are small or not elongated enough to display clear alignment. The total volume of inclusions (excluding quartz and plagioclase, which have X-ray attenuation very similar to that of alkali feldspar) does not exceed 1% of megacryst volume. Plagioclase seems to be at least equal in volume to all other inclusions combined, but as noted above, its exact volume is currently indiscernible. Magnetite makes up about 1/6 of inclusion volume, zircon 1/3, and all others the remaining half. We will complement our dataset by performing XCT, BSE, EDS, and LA-ICP-MS analysis on the crystals, and continue to improve methods to better discern the zoning patterns. Identifying zoning patterns that are discernable from one another is an important first step towards understanding individual megacryst histories.

Bread board float zone experiment system for high purity silicon

NASA Technical Reports Server (NTRS)

Kern, E. L.; Gill, G. L., Jr.

1982-01-01

A breadboard float zone experimental system has been established at Westech Systems for use by NASA in the float zone experimental area. A used zoner of suitable size and flexibility was acquired and installed with the necessary utilities. Repairs, alignments and modifications were made to provide for dislocation free zoning of silicon. The zoner is capable of studying process parameters used in growing silicon in gravity and is flexible to allow trying of new features that will test concepts of zoning in microgravity. Characterizing the state of the art molten zones of a growing silicon crystal will establish the data base against which improvements of zoning in gravity or growing in microgravity can be compared. 25 mm diameter was chosen as the reference size, since growth in microgravity will be at that diameter or smaller for about the next 6 years. Dislocation free crystals were growtn in the 100 and 111 orientations, using a wide set of growth conditions. The zone shape at one set of conditions was measured, by simultaneously aluminum doping and freezing the zone, lengthwise slabbing and delineating by etching. The whole set of crystals, grown under various conditions, were slabbed, polished and striation etched, revealing the growth interface shape and the periodic and aperiodic natures of the striations.

Ignition and growth modeling of detonation reaction zone experiments on single crystals of PETN and HMX

NASA Astrophysics Data System (ADS)

White, Bradley W.; Tarver, Craig M.

2017-01-01

It has long been known that detonating single crystals of solid explosives have much larger failure diameters than those of heterogeneous charges of the same explosive pressed or cast to 98 - 99% theoretical maximum density (TMD). In 1957, Holland et al. demonstrated that PETN single crystals have failure diameters of about 8 mm, whereas heterogeneous PETN charges have failure diameters of less than 0.5 mm. Recently, Fedorov et al. quantitatively determined nanosecond time resolved detonation reaction zone profiles of single crystals of PETN and HMX by measuring the interface particle velocity histories of the detonating crystals and LiF windows using a PDV system. The measured reaction zone time durations for PETN and HMX single crystal detonations were approximately 100 and 260 nanoseconds, respectively. These experiments provided the necessary data to develop Ignition and Growth (I&G) reactive flow model parameters for the single crystal detonation reaction zones. Using these parameters, the calculated unconfined failure diameter of a PETN single crystal was 7.5 +/- 0.5 mm, close to the 8 mm experimental value. The calculated failure diameter of an unconfined HMX single crystal was 15 +/- 1 mm. The unconfined failure diameter of an HMX single crystal has not yet been determined precisely, but Fedorov et al. detonated 14 mm diameter crystals confined by detonating a HMX-based plastic bonded explosive (PBX) without initially overdriving the HMX crystals.

Relationship of Optical Anomalies, Zoning, and Microtopography in Vesuvianite from Jeffrey Mine, Asbestos, Quebec

NASA Astrophysics Data System (ADS)

Smith, Varina Campbell

The role of growth steps in inducing disequilibrium is investigated in crystals of vesuvianite from the Jeffrey mine, Asbestos, Quebec, using optical microscopy, atomic force microscopy, electron microprobe analysis, and single-crystal X-ray diffraction. The selective uptake of elements Fe and Al by asymmetric growth-steps on three crystallographic forms, {100}, {110}, and {121}, is documented. The prisms {100} and {110} show hillocks that display kinetically controlled oscillatory zoning along growth steps parallel to <010> and <11¯1>, but not on vicinal faces defined by [001] steps. Sector-specific zoning of extinction angles and 2V angles indicate different degrees of optical dissymmetrization in crystals spanning a range of growth habits. Unit-cell parameters and the presence of violating reflections confirm sectoral deviations from P4/nnc symmetry in the prismatic sectors. The partial loss of three glide planes follows the pattern expected from order of the cations Al and Fe induced by tangential selectivity at the edge of non-equivalent steps during layer-by-layer growth.

Single crystal growth of spin-ladder compound La8Cu7O19 by the travelling-solvent floating zone method

NASA Astrophysics Data System (ADS)

Mohan, A.; Singh, S.; Partzsch, S.; Zwiebler, M.; Geck, J.; Wurmehl, S.; Büchner, B.; Hess, C.

2016-08-01

Large single crystals of La8Cu7O19 have been grown using the travelling-solvent floating zone method. A rather high oxygen pressure of 9 bar in the growth chamber and a slow growth speed of 0.5 mm/h were among the most important parameters in stabilizing the growth of this incongruently melting compound. Interestingly, a novel growth scenario has been witnessed. The crystal structure of the grown La8Cu7O19 crystal has been analyzed using single crystal diffractometry to extract important structural parameters of this compound. We find that La8Cu7O19 crystallizes in a monoclinic structure with space group C 2 / c and has the lattice parameters a ≈ 13.83 Å, b ≈ 3.75 Å, c ≈ 34.59 Å, and β ≈ 99.33 °, in good agreement with the data obtained on polycrystalline samples in the literature. The magnetization shows a highly anisotropic behavior, and an anomaly at T ≈103 K.

Mineral and organic matrix interaction in normally calcifying tendon visualized in three dimensions by high-voltage electron microscopic tomography and graphic image reconstruction

NASA Technical Reports Server (NTRS)

Landis, W. J.; Song, M. J.; Leith, A.; McEwen, L.; McEwen, B. F.

1993-01-01

To define the ultrastructural accommodation of mineral crystals by collagen fibrils and other organic matrix components during vertebrate calcification, electron microscopic 3-D reconstructions were generated from the normally mineralizing leg tendons from the domestic turkey, Meleagris gallopavo. Embedded specimens containing initial collagen mineralizing sites were cut into 0.5-micron-thick sections and viewed and photographed at 1.0 MV in the Albany AEI-EM7 high-voltage electron microscope. Tomographic 3-D reconstructions were computed from a 2 degree tilt series of micrographs taken over a minimum angular range of +/- 60 degrees. Reconstructions of longitudinal tendon profiles confirm the presence of irregularly shaped mineral platelets, whose crystallographic c-axes are oriented generally parallel to one another and directed along the collagen long axes. The reconstructions also corroborate observations of a variable crystal length (up to 170 nm measured along crystallographic c-axes), the presence of crystals initially in either the hole or overlap zones of collagen, and crystal growth in the c-axis direction beyond these zones into adjacent overlap and other hole regions. Tomography shows for the first time that crystal width varies (30-45 nm) but crystal thickness is uniform (approximately 4-6 nm at the resolution limit of tomography); more crystals are located in the collagen hole zones than in the overlap regions at the earliest stages of tendon mineralization; the crystallographic c-axes of the platelets lie within +/- 15-20 degrees of one another rather than being perfectly parallel; adjacent platelets are spatially separated by a minimum of 4.2 +/- 1.0 nm; crystals apparently fuse in coplanar alignment to form larger platelets; development of crystals in width occurs to dimensions beyond single collagen hole zones; and a thin envelope of organic origin may be present along or just beneath the surfaces of individual mineral platelets. Implicit in the results is that the formation of crystals occurs at different sites and times by independent nucleation events in local regions of collagen. These data provide the first direct visual evidence from 3-D imaging describing the size, shape, orientation, and growth of mineral crystals in association with collagen of a normally mineralizing vertebrate tissue. They support concepts that c-axial crystal growth is unhindered by collage hole zone dimensions, that crystals are organized in the tendon in a series of generally parallel platelets, and that crystal growth in width across collagen fibrils may follow channels or grooves formed by adjacent hole zones in register.

Influence of Containment on the Growth of Germanium-Silicon in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.; Sorgenfrei, T.

2017-01-01

This investigation involves the comparison of results achieved from three types of crystal growth of germanium and germanium-silicon alloys: Float zone growth, Bridgman growth, and Detached Bridgman growth. The fundamental goal of the proposed research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon (GeSi) crystals (silicon concentration in the solid up to 5%) for three different growth configurations in order to quantitatively assess the improvements of crystal quality possible by detached growth.

Can Solution Supersaturation Affect Protein Crystal Quality?

NASA Technical Reports Server (NTRS)

Gorti, Sridhar

2013-01-01

The formation of large protein crystals of "high quality" is considered a characteristic manifestation of microgravity. The physical processes that predict the formation of large, high quality protein crystals in the microgravity environment of space are considered rooted in the existence of a "depletion zone" in the vicinity of crystal. Namely, it is considered reasonable that crystal quality suffers in earth-grown crystals as a result of the incorporation of large aggregates, micro-crystals and/or large molecular weight "impurities", processes which are aided by density driven convective flow or mixing at the crystal-liquid interface. Sedimentation and density driven convection produce unfavorable solution conditions in the vicinity of the crystal surface, which promotes rapid crystal growth to the detriment of crystal size and quality. In this effort, we shall further present the hypothesis that the solution supersaturatoin at the crystal surface determines the growth mechanism, or mode, by which protein crystals grow. It is further hypothesized that protein crystal quality is affected by the mechanism or mode of crystal growth. Hence the formation of a depletion zone in microgravity environment is beneficial due to inhibition of impurity incorporatoin as well as preventing a kinetic roughening transition. It should be noted that for many proteins the magnitude of neither protein crystal growth rates nor solution supersaturation are predictors of a kinetic roughening transition. That is, the kinetic roughening transition supersaturation must be dtermined for each individual protein.

A Simple Inexpensive Bridgman-Stockbarger Crystal Growth System for Organic Materials

NASA Technical Reports Server (NTRS)

Choi, J.; Aggarwal, M. D.; Wang, W. S.; Metzl, R.; Bhat, K.; Penn, Benjamin G.; Frazier, Donald O.

1996-01-01

Direct observation of solid-liquid interface is important for the directional solidification to determine the desired interface shape by controlling the growth parameters. To grow good quality single crystals of novel organic nonlinear optical materials, a simple inexpensive Bridgman-Stockbarger (BS) crystal growth system has been designed and fabricated. Two immiscible liquids have been utilized to create two zones for this crystal growth system. Bulk single crystals of benzil derivative and n-salicylidene-aniline have been successfully grown in this system. The optimum lowering rate has been found to be 0.1 mm/h for the flat interface. Results on the crystal growth and other parameters of the grown crystals are presented.

Meeting the Continental Crust: the Hidden Olivine Trauma in Subduction Settings

NASA Astrophysics Data System (ADS)

Salas Reyes, P.; Ruprecht, P.; Rabbia, O. M.; Hernandez, L.

2017-12-01

In a conventional framework, olivine zonation represents concentric growth from an evolving liquid. Alternatively, it has been suggested (e.g. Welsch et al. 2014) that olivine develop dendritic textures and compositional discontinuities due to rapid growth and boundary layer effects, respectively, where any complex zoning is quickly erased through diffusive re-equilibration in the high temperature magmatic environment. In particular, olivine crystals from large volcanic centers in convergent margins rarely preserve such dendritic textures and complex zoning due prolonged magma residence. Small volume, mafic monogenetic vents may bypass such crustal re-equilibration and potentially record the otherwise elusive early olivine growth history. We selected tephra deposits from Los Hornitos, in the Andean arc of Central Chile (35.5˚S), that represents primitive magmas ( 15 wt.% MgO) and contain magnesian olivines (Fo>88) hosting quenched melt inclusions. We obtained detailed quantitative EPMA zoning profiles and measured volatile contents (H, C, S, Cl) in the co-existing melt inclusions. Furthermore, we analyzed mineral morphologies connecting compositional zoning with growth textures. We find that 40% of the olivine crystals retain dendritic shapes while the others are polyhedral with trapped melt inclusions and cavities. The polyhedral crystals are normally zoned (Fo92 to Fo88; Ni 4000 ppm to 1000 ppm), however an oscillatory zonation depicted by concentric -coupled Fo and Ni- enriched layers exist and therefore even those crystals still preserve also a more complete growth history. The related melt inclusions yield values of up to 6000 ppm of S. Such zonation may imply sudden growth during elevated degrees of undercooling (-ΔT > 60°C) as the magmas transit from the hot mantle to the cooler conditions in the crust. Moreover, the preservation of such Fo and Ni zonation requires limited time between crystal growth and eruption. The elevated S content in melt inclusions may suggest that the crystallization occurred in the lower crust or upper mantle, and thus a quick passage through the arc crust that retains the normally hidden dendritic trauma the olivine experiences during its transfer from the mantle to the crust. References: Welsch et al 2014. Geology v.42 p.867-870

Controllable fabrication of copper phthalocyanine nanostructure crystals.

PubMed

Liu, Fangmei; Sun, Jia; Xiao, Si; Huang, Wenglong; Tao, Shaohua; Zhang, Yi; Gao, Yongli; Yang, Junliang

2015-06-05

Copper phthalocyanine (CuPc) nanostructure crystals, including nanoflower, nanoribbon, and nanowire, were controllably fabricated by temperature gradient physical vapor deposition (TG-PVD) through controlling the growth parameters. In a controllable growth system with carrier gas N2, nanoflower, nanoribbon, and nanowire crystals were formed in a high-temperature zone, medium-temperature zone, and low-temperature zone, respectively. They were proved to be β-phase, coexist of α-phase and β-phase, and α-phase respectively based on x-ray diffraction results. Furthermore, ultralong CuPc nanowires up to several millimeters could be fabricated by TG-PVD without carrier gas, and they were well-aligned to form large-area CuPc nanowire crystal arrays by the Langmuir-Blodgett method. The nanostructure crystals showed unusual optical absorption spectra from the ultraviolet-visible to near-infrared range, which was explained by the diffraction and scattering caused by the wavelength-sized nanostructures. These CuPc nanostructure crystals show potential applications in organic electronic and optoelectronic devices.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

Szofran, Frank R.; Benz, K. W.; Croell, Arne; Dold, Peter; Cobb, Sharon D.; Volz, Martin P.; Motakef, Shariar; Walker, John S.

1999-01-01

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.

Three-dimensional modelling of thermal stress in floating zone silicon crystal growth

NASA Astrophysics Data System (ADS)

Plate, Matiss; Krauze, Armands; Virbulis, Jānis

2018-05-01

During the growth of large diameter silicon single crystals with the industrial floating zone method, undesirable level of thermal stress in the crystal is easily reached due to the inhomogeneous expansion as the crystal cools down. Shapes of the phase boundaries, temperature field and elastic material properties determine the thermal stress distribution in the solid mono crystalline silicon during cylindrical growth. Excessive stress can lead to fracture, generation of dislocations and altered distribution of intrinsic point defects. Although appearance of ridges on the crystal surface is the decisive factor of a dislocation-free growth, the influence of these ridges on the stress field is not completely clear. Here we present the results of thermal stress analysis for 4” and 5” diameter crystals using a quasi-stationary three dimensional mathematical model including the material anisotropy and the presence of experimentally observed ridges which cannot be addressed with axis-symmetric models. The ridge has a local but relatively strong influence on thermal stress therefore its relation to the origin of fracture is hypothesized. In addition, thermal stresses at the crystal rim are found to increase for a particular position of the crystal radiation reflector.

STS-30 MS Cleave uses camcorder to record FEA-2 crystal growth

NASA Image and Video Library

1989-05-08

STS030-10-002 (8 May 1989) --- STS-30 Mission Specialist Mary L. Cleave operates 8mm video camcorder at Fluids Experiment Apparatus 2 (FEA-2) (SK73-000102) unit located in aft middeck locker onboard Atlantis, Orbiter Vehicle (OV) 103. Two 8mm video camcorders are positioned above FEA-2 unit to record experiment titled "Floating Zone Crystal Growth and Purification". Rockwell International (RI) through its Space Transportation Systems Division, Downey, California, is engaged in a joint endeavor agreement (JEA) with NASA's Office of Commercial Programs in the field for floating zone crystal growth research. Utah State University Aggies decal appears on aft bulkhead above FEA-2 unit.

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Plechov, P.; Eichelberger, J. C.

2015-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, Augustine and Cleveland Volcanoes in Alaska, as well as from the drilling into an active magma body at Krafla, Iceland.

Phenytoin crystal growth rates in the presence of phosphate and chloride ions

NASA Astrophysics Data System (ADS)

Zipp, G. L.; Rodríguez-Hornedo, N.

1992-09-01

Phenytoin crystal growth kinetics have been measured as a function of supersaturation in pH 2.2 phosphoric acid and pH 2.2 hydrochloric acid solutions. Two different methods were used for the kinetic analysis. The first involved a zone-sensing device which provided an analysis of the distribution of crystals in a batch crystallizer. Crystal growth rates were calculated from the increase in the size of the distribution with time. In the second method, growth rates were evaluated from the change in size with time of individual crystals observed under an inverted microscope. The results from each method compare favorably. The use of both techniques provides an excellent opportunity to exploit the strengths of each: an average growth rate from a population of crystals from batch crystallization and insight into the effect of growth on the morphology of the crystals from the individual crystal measurements.

Determination of crystal residence timescales in magma reservoirs by diffusion modeling of dendritic phosphorus zoning patterns in olivine

NASA Astrophysics Data System (ADS)

Chakraborty, S.; Potrafke, A.

2016-12-01

Deciphering the early stages of crystallization and the chronological evolution of phenocrysts in magma reservoirs is one of the main goals in volcanology. Established approaches that model the concentration evolution of fast diffusing elements like Fe/Mg carry limited information on timescales once the concentration gradients are homogenized. Elements that diffuse more slowly, such as P and Al, become useful in these cases. We present a novel modeling tool that combines high-resolution EMP mapping of slow diffusing phosphorus in olivine with 2D kinetic modeling of the diffusive relaxation of initial chemical zoning pattern of P as well as Fe/Mg. The modeling approach offers a new possibility for determining crystal residence times in magma reservoirs. P diffusion coefficients from the experimental determination of [1] and Fe/Mg diffusion coefficients from [2] were used. The method yields a time-bracket between the minimum time required to homogenize the zoning of fast-diffusing Fe/Mg and the maximum time period for which details of chemical zoning of slow-diffusing P may be retained. To illustrate the approach we have studied the compositional zoning patterns of 7 olivine crystals from Piton de la Fournaise volcano, La Réunion. All crystals show a narrow range of forsterite contents (=Fo82-84) with fully homogenized Fe/Mg distribution, whereas P-mapping reveals oscillatory to dendritic zoning patterns [3]. P concentrations scatter in the range of 0.4 wt-% to below detection limit. Revealed phosphorus zoning patterns were considered to display the initial crystal architecture, whereas Fe and Mg zoning has been wiped out due to faster diffusion. For La Réunion magmas at 1453 K, timescales between few days to weeks were determined to be the time brackets for growth and residence of the olivine crystals in the magmas. These short residence times combined with knowledge of very fast developing dendritic crystals that have recently been revealed worldwide [e.g. 3] indicate that dendritic crystal growth in such rapidly evolving dynamic environments should be considered as a widespread feature of olivine growth and evolution of many basaltic volcanic systems. [1] Watson et al., 2015, Am Min, 100, pp. 2053-2065 [2] Dohmen et al., 2007, Phys Chem Miner, 34(6), pp. 389-407 [3] Welsch et al., 2014, Geology, 42, pp. 867-870

Magnetic field controlled single crystal growth and surface modification of titanium alloys exposed for biocompatibility

NASA Astrophysics Data System (ADS)

Hermann, Regina; Uhlemann, Margitta; Wendrock, Horst; Gerbeth, Gunter; Büchner, Bernd

2011-03-01

The aim of this work is growth and characterisation of Ti55Nb45 (wt%) single crystals by floating-zone single crystal growth of intermetallic compounds using two-phase radio-frequency (RF) electromagnetic heating. Thereby, the process and, in particular, the flow field in the molten zone is influenced by additional magnetic fields. The growth of massive intermetallic single crystals is very often unsuccessful due to an unfavourable solid-liquid interface geometry enclosing concave fringes. It is generally known that the crystallization process stability is enhanced if the crystallization interface is convex. For this, a tailored magnetic two-phase stirrer system has been developed, which enables a controlled influence on the melt ranging from intensive inwards to outwards flows. Since Ti is favourably light, strong and biocompatible, it is one of the few materials that naturally match the requirements for implantation in the human body. Therefore, the magnetic system was applied to crystal growth of Ti alloys. The grown crystals were oriented and cut to cubes with the desired crystallographic orientations [1 0 0] and [1 0 1] normally on a plane. The electron backscatter diffraction (EBSD) technique was applied to clearly determine crystal orientation and to localize grain boundaries. The formation of oxidic nanotubes on Ti surfaces in dependence of the grain orientation was investigated, performed electrochemically by anodic oxidation from fluoride containing electrolyte.

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

NASA Technical Reports Server (NTRS)

Szofran, F. R.; Volz, M. P.; Cobb, S. D.; Motakef, S.; Croell, A.; Dold, P.

2001-01-01

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

Zircon growth in shear zones

NASA Astrophysics Data System (ADS)

Kaulina, Tatiana

2013-04-01

The possibility of direct dating of the deformation process is critical for understanding of orogenic belts evolution. Establishing the age of deformation by isotopic methods is indispensable in the case of uneven deformation overlapping, when later deformation inherits the structural plan of the early strains, and to distinguish them on the basis of the structural data only is impossible. A good example of zircon from the shear zones is zircon formed under the eclogite facies conditions. On the one hand, the composition of zircon speaks about its formation simultaneously to eclogitic paragenesis (Rubatto, Herman, 1999; Rubatto et al., 2003). On the other hand, geological studies show that mineral reactions of eclogitization are often held only in areas of shear deformations, which provides access of fluid to the rocks (Austrheim, 1987; Jamtveit et al., 2000; Bingen et al., 2004). Zircons from mafic and ultramafic rocks of the Tanaelv and Kolvitsa belts (Kola Peninsula, the Baltic Shield) have showed that the metamorphic zircon growth is probably controlled by the metamorphic fluid regime, as evidenced by an increase of zircon quantity with the degree of shearing. The internal structure of zircon crystals can provide an evidence of zircon growth synchronous with shearing. The studied crystals have a sector zoning and often specific "patchy" zoning (Fig. 1), which speaks about rapid change of growth conditions. Such internal structure can be compared with the "snowball" garnet structure reflecting the rotation of crystals during their growth under a shift. Rapidly changing crystallization conditions can also be associated with a small amount of fluid, where supersaturation is changing even at a constant temperature. Thus, the growth of metamorphic zircon in shear zones is more likely to occur in the fluid flow synchronous with deformation. A distinctive feature of zircons in these conditions is isometric shape and sector "patchy" zoning. The work was supported by Russian Foundation of Basic Research (project: 13-05-00035.) and the DES-6 program.

Thermocapillary flow and melt/solid interfaces in floating-zone crystal growth under microgravity

NASA Technical Reports Server (NTRS)

Lan, C. W.; Kou, Sindo

1990-01-01

Computer simulation of steady-state axisymmetrical heat transfer and fluid flow was conducted to study thermocapillary flow and melt/solid interfaces in floating-zone crystal growth under microgravity. The effects of key variables on the extent of thermocapillary flow in the melt zone, the shapes of melt/solid interfaces and the length of the melt zone were discussed. These variables are: (1) the temperature coefficient of surface tension (or the Marangoni number), (2) the pulling speed (or the Peclet number), (3) the feed rod radius, (4) the ambient temperature distribution, (5) the heat transfer coefficient (or the Biot number), and (6) the thermal diffusivity of the material (or the Prandtl number).

Integrated melt inclusion and crystal zoning study to track the timescales and pre-eruption dynamics of violent Strombolian eruptions at Llaima volcano, Chile

NASA Astrophysics Data System (ADS)

Ruth, D. C.; Costa Rodriguez, F.; Bouvet de Maisonneuve, C.; Calder, E. S.

2013-12-01

Melt inclusion compositions in crystals from many volcanic systems are notoriously variable and some times difficult to interpret. Their compositions can be a combination of rapid crystal growth, entrapment of local melt, and diffusive re-equilibration, among other processes. Additionally, chemical zoning in olivine records changing environmental conditions, most importantly temperature and magma composition. Many geochemical studies focus on either melt inclusion data or chemical zoning data to ascertain volcanic processes. Here we combine melt inclusion data with that of chemical zoning of the olivine host crystals from the 2008 violent Strombolian eruption of Llaima volcano, Chile, to obtain a more refined understanding of the processes related to crystal growth, melt inclusion formation, and magma dynamics. We investigated zoning characteristics in a suite of olivine crystals, created X-ray element maps (Al, Ca, Mg, P, Fe), and collected quantitative elemental abundances across chemical zones for detailed diffusion modeling. Melt inclusion compositions were collected via electron microprobe analysis and LA-ICPMS. We observe three types of zoning in the host olivine crystals: normal, reverse, and multiple zones with fluctuating Fo content. Reverse zoning was more common than the other types. Regardless of zoning character, multiple melt inclusions are present within a given olivine, often found near the crystal rim. For some of these melt inclusions, the olivine surrounding the melt inclusion was also zoned, often to a similar composition as the olivine rim. This implies that these inclusions remained connected with interstitial matrix melt until melt inclusion closure. These ';open' melt inclusions exhibited slightly different major (higher SiO2, Na2O+K2O, TiO2) and trace elements (positive Eu and Sr anomalies) compared to melt inclusions in the same olivine that were not surrounded by compositional zoning. Quantitative elemental profiles produce modeled timescales on the order of 10s-100s days prior to eruption. Zoning textures, melt inclusion compositions, and timescale modeling indicates that crystal dissolution (open melt inclusions), mafic magma injection (reverse zoning), and partial melting of upper crustal plagioclase-rich cumulates (positive Eu and Sr anomalies) were occurring in the months prior to the 2008 eruption. The combination of both melt inclusion data and textural data of the host crystals provides deeper insight into the nature and timing of deep and shallow reservoir processes that generate violent Strombolian eruptions at Llaima.

Three-Dimensional Dendrite Growth Within the Shrouds of Single Crystal Blades of a Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Wang, Fu; Wu, Zining; Huang, Can; Ma, Dexin; Jakumeit, Jürgen; Bührig-Polaczek, Andreas

2017-12-01

The effect of withdrawal rates on the three-dimensional dendrite growth within the shrouds of single crystal blades during directional solidification was studied by both experiments and numerical simulations. The results showed that at given withdrawal rates, the dendrite pattern within the shrouds comprised three zones: primary dendrite zone, secondary dendrite spread zone, and a higher-order dendrite branched zone. With increasing withdrawal rate, the average primary dendrite arm spacing in the primary dendrite zone and the average secondary dendrite arm spacings in both the secondary dendrite spread zone and the higher-order dendrite branched zone were reduced. Independent of the variation in withdrawal rate, two analogous dendrite growth routes were observed within the shrouds of the employed blade geometry. These routes originated from the primary dendrites in the primary dendrite zone and filled in the shrouds by directly spreading secondary or successively branching higher-order dendrites. Except for a withdrawal rate of 6 mm min-1, these dendrites impinged at the shroud's highest extremity and could be explained by the simulated moving isotherms. As the withdrawal rate was increased to 2.5 mm min-1, undercooling and contraction stress-related equiaxed grains were observed in the interdendritic region at the lowest shroud extremity. With increasing withdrawal rate, the amount of the defects was increased. Since the defects destroy the integrity of single crystal blades, the solidification condition within the shroud should be controlled to avoid their occurrence. Along the dendrite growth route, an accumulated misorientation of the dendrites was observed. At the same positions, this accumulation increased with increasing withdrawal rate.

The 3-5 semiconductor solid solution single crystal growth. [low gravity float zone growth experiments using gallium indium antimonides and cadmium tellurides

NASA Technical Reports Server (NTRS)

Gertner, E. R.

1980-01-01

Techniques used for liquid and vapor phase epitaxy of gallium indium arsenide are described and the difficulties encountered are examined. Results show that the growth of bulk III-V solid solution single crystals in a low gravity environment will not have a major technological impact. The float zone technique in a low gravity environment is demonstrated using cadmium telluride. It is shown that this approach can result in the synthesis of a class of semiconductors that can not be grown in normal gravity because of growth problems rooted in the nature of their phase diagrams.

Gordon Research Conference on Crystal Growth (1990)

DTIC Science & Technology

1990-04-01

Labs, MH) 14. Cox Vapor Levitation Epitaxy of Quantum Wires and Wire-like Structures Using Laterally Propagating Surface Steps. (Bellcore, Red Bank) 15...introduced many new aspects of crystal growth, including strained layer superlattices, quantum cluster growth, and vertical zone melting of GaAs...Films 2. E. Bauser Semiconductor Liquid Phase Epitaxy: Growth and Properties of Layers and Heterostructures 3. M. L. Steigerwald Growth of Quantum

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Eichelberger, J. C.; Plechov, P.

2016-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Augustine and Cleveland Volcanoes in Alaska, Sakurajima Volcano in Japan, Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, as well as from the drilling into an active magma body at Krafla, Iceland.

Temperature and emissivity measurements at the sapphire single crystal fiber growth process

NASA Astrophysics Data System (ADS)

Bufetova, G. A.; Rusanov, S. Ya.; Seregin, V. F.; Pyrkov, Yu. N.; Tsvetkov, V. B.

2017-12-01

We present a new method for evaluation the absorption coefficient of the crystal melt around the phase transition zone for the spectral range of semitransparency. The emissivity distribution across the crystallization front of the sapphire crystal fiber was measured at the quasi-stationary laser heated pedestal growth (LHPG) process (Fejer et al., 1984; Feigelson, 1986) and the data for solid state, melt and phase transition zone (melt-solid interface) were obtained. The sapphire melt absorption coefficient was estimated to be 14 ± 2 cm-1 in the spectral range 1-1.4 μm around the melt point. It is consistent with data, obtained by different other methods. This method can be applied to determine the absorption coefficient for other materials.

The control of float zone interfaces by the use of selected boundary conditions

NASA Technical Reports Server (NTRS)

Foster, L. M.; Mcintosh, J.

1983-01-01

The main goal of the float zone crystal growth project of NASA's Materials Processing in Space Program is to thoroughly understand the molten zone/freezing crystal system and all the mechanisms that govern this system. The surface boundary conditions required to give flat float zone solid melt interfaces were studied and computed. The results provide float zone furnace designers with better methods for controlling solid melt interface shapes and for computing thermal profiles and gradients. Documentation and a user's guide were provided for the computer software.

Crystal growth of intermetallic clathrates: Floating zone process and ultra rapid crystallization

NASA Astrophysics Data System (ADS)

Prokofiev, A.; Yan, X.; Ikeda, M.; Löffler, S.; Paschen, S.

2014-09-01

We studied the crystal growth process of type-I transition metal clathrates in two different regimes: a regime of moderate cooling rate, realized with the floating zone technique, and a regime of ultra rapid cooling, realized by the melt spinning technique. In the former regime, bulk Ba8AuxSi46-x and Ba8Cu4.8GaxGe41.2-x single crystals were grown. We investigated segregation effects of the constituting elements by measurements of the composition profiles along the growth direction. The compositional non-uniformity results in a spatial variation of the electrical resistivity which is discussed as well. Structural features of clathrates and their extremely low thermal conductivities imply specifics in growth behavior which manifest themselves most pronouncedly in a rapid crystallization process. Our melt spinning experiments on Ba8Au5Si41 and Ba8Ni3.5Si42.5 (and earlier on some other clathrates) have revealed surprisingly large grains of at least 1 μm. Because of the anomalously high growth rate of the clathrate phase the formation of impurity phases is considerably kinetically suppressed. We present our scanning and transmission electron microscopy investigations of melt spun samples and discuss structural, thermodynamic and kinetic aspects of the unusual clathrate nucleation and crystallization.

Improving the growth of CZT crystals for radiation detectors: a modeling perspective

NASA Astrophysics Data System (ADS)

Derby, Jeffrey J.; Zhang, Nan; Yeckel, Andrew

2012-10-01

The availability of large, single crystals of cadmium zinc telluride (CZT) with uniform properties is key to improving the performance of gamma radiation detectors fabricated from them. Towards this goal, we discuss results obtained by computational models that provide a deeper understanding of crystal growth processes and how the growth of CZT can be improved. In particular, we discuss methods that may be implemented to lessen the deleterious interactions between the ampoule wall and the growing crystal via engineering a convex solidification interface. For vertical Bridgman growth, a novel, bell-curve furnace temperature profile is predicted to achieve macroscopically convex solid-liquid interface shapes during melt growth of CZT in a multiple-zone furnace. This approach represents a significant advance over traditional gradient-freeze profiles, which always yield concave interface shapes, and static heat transfer designs, such as pedestal design, that achieve convex interfaces over only a small portion of the growth run. Importantly, this strategy may be applied to any Bridgman configuration that utilizes multiple, controllable heating zones. Realizing a convex solidification interface via this adaptive bell-curve furnace profile is postulated to result in better crystallinity and higher yields than conventional CZT growth techniques.

Crystal zoning in a large-volume ignimbrite: constraints on the thermal history of a supervolcano magma system

NASA Astrophysics Data System (ADS)

Matthews, N. E.; Pyle, D. M.; Wilson, C. J.

2009-12-01

Chemical zoning of crystals provides an important archive of information that allows for the reconstruction of complex thermal histories and changes in melt composition of the magma reservoir during crystallization. Here we investigate cathodoluminescence (CL) and Ti zonation in quartz crystals extracted from pumices from the Whakamaru and Rangitaiki ignimbrite units (part of the large-volume Whakamaru Group Ignimbrites), New Zealand, to reconstruct the thermal history of the parent magma chamber(s). CL intensity images are taken as a proxy for Ti content and temperature variation during crystal growth, and direct estimates of temperature are made using the TitaniQ geothermometer (Wark & Watson 2006 Cont. Min. Pet.) based on Ti concentration in quartz. These results are reviewed in comparison with temperatures from Fe-Ti oxide geothermometry. Quartz zoning is also compared to zonation in feldspars (using BSE imaging) from the same pumice clasts in order to establish the degree to which different crystal species record similar or contrasting magmatic histories. Quartz crystals in Whakamaru pumice display a variety of CL zoning patterns and resorption boundaries. Overgrowths typically appear to truncate CL growth zoning within the crystal core, indicating periods of resorption and subsequent re-growth - consistent with magma recharge causing a marked change in conditions (temperature and/or volatile saturation) and multi-stage crystallisation. Crystals typically display a dark (lower Ti) resorbed core, with an abrupt change to a CL-bright rim, although irregular textures and complex variations between crystals are observed. Core-to-rim profiles of Ti concentration in analysed quartz crystals show Ti variations within the range 50-225 ppm, corresponding to crystallisation temperatures of 733-935°C (assuming TiO2 activity in the melt of 0.6), with the lowest values recorded in the crystal core, increasing in a step-wise pattern towards the rim. These values are consistent with Fe-Ti oxide temperature data for the same pumice clasts which provide a temperature range of 660-933°C. It is inferred that the major steps in Ti content (and thus CL brightness) represent short-term temperature fluctuations due to magma chamber recharge and rejuvenation of a crystal mush, while rim temperatures are likely to record the magma temperature at the time of eruption.

Growth and surface topography of WSe{sub 2} single crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dixit, Vijay, E-mail: vijdix1@gmail.com; Vyas, Chirag; Pataniya, Pratik

2016-05-06

Tungsten Di-Selenide belongs to the family of TMDCs showing their potential applications in the fields of Optoelectronics and PEC solar cells. Here in the present investigation single crystals of WSe{sub 2} were grown by Direct Vapour Transport Technique in a dual zone furnace having temperature difference of 50 K between the two zones. These single crystals were characterized by EDAX which confirms the stiochiometry of the grown crystals. Surface topography of the crystal was studied by optical micrograph showing the left handed spirals on the surface of WSe{sub 2} crystals. Single crystalline nature of the crystals was confirmed by SAED.

Temperature and melt solid interface control during crystal growth

NASA Technical Reports Server (NTRS)

Batur, Celal

1990-01-01

Findings on the adaptive control of a transparent Bridgman crystal growth furnace are summarized. The task of the process controller is to establish a user specified axial temperature profile by controlling the temperatures in eight heating zones. The furnace controller is built around a computer. Adaptive PID (Proportional Integral Derivative) and Pole Placement control algorithms are applied. The need for adaptive controller stems from the fact that the zone dynamics changes with respect to time. The controller was tested extensively on the Lead Bromide crystal growth. Several different temperature profiles and ampoule's translational rates are tried. The feasibility of solid liquid interface quantification by image processing was determined. The interface is observed by a color video camera and the image data file is processed to determine if the interface is flat, convex or concave.

Laminar mixing in a small floating zone

NASA Technical Reports Server (NTRS)

Harriott, George M.

1987-01-01

The relationship between the flow and solute fields during steady mass transfer of a dilute component is analyzed for multi-cellular rotating flows in the floating zone process of semiconductor growth. When the recirculating flows are weak in relation to the rate of crystal growth, a closed-form solution clearly shows the link between the convection pattern in the melt and the solute distribution across the surface of the growing solid. In the limit of strong convection, finite element calculations demonstrate the tendency of the composition to become uniform over the majority of the melt. The solute segregation in the product crystal is greatest when the recirculating motion is comparable to the rate of crystal growth, and points to the danger in attempting to grow compositionally uniform materials from a nearly convectionless melt.

The influence of impurities on phosphoric acid hemihydrate crystallization

NASA Astrophysics Data System (ADS)

Dang, Leping; Wei, Hongyuan; Zhu, Zheng; Wang, Jingkang

2007-09-01

The influence of four typical impurities on phosphoric acid hemihydrate (H 3PO 4·0.5H 2O) crystallization in terms of kinetics and morphology is studied quantitatively. A new method for estimating growth rate is developed by taking the slopes of linearlized lines of transient chord length distribution (CLD) of crystals during the process using an in-line device of Focused Beam Reflectance Monitoring (FBRM). The presence of cations can reduce the nucleation rate of phosphoric acid while anions have less effect. Impurities of Fe 3+, Al 3+, and F - (>50 ppm) can widen the metastable zone to some extent. Adding small amounts of H 2SO 4 (<150 ppm) can enlarge metastable zone, but such effect becomes less after adding more H 2SO 4. The presence of the SO 42- tends to encourage H 3PO 4·0.5H 2O crystal growth in a wide concentration range with the maximum growth rate at 5000 ppm. Addition of Fe 3+ and Al 3+ at low level can increase crystal growth rate until it reaches a maximum at 500, 50, and 100 ppm for F -, Al 3+, and Fe 3+, respectively. Impurities of cations appear to have significant effect on crystal morphology; anions, however, appear not to change crystal shapes much.

Autonomous magnetic float zone microgravity crystal growth application to TiC and GaAs

NASA Astrophysics Data System (ADS)

Chan, Tony Y.-T.; Choi, Sang-Keun

1992-10-01

The floating zone process is ideal for high temperature (greater than 3000 K) growth of titanium carbide because it is containerless. However, float zoning requires small melt volumes in order to maintain a stable melt configuration. The short melt columns make it difficult to achieve a controlled thermal profile, a necessity for producing crystals of high quality. Thus, an automated control strategy based upon continuous monitoring of the growth process with processing parameters adjusted to values based upon the physical transport processes of the growth process is very desirable for maintaining stability and reproducibility of the process. The present work developed a Float-zone Acquisition and Control Technology (FACT) system which uses relations derived by combining empirical relations with a knowledge data base deduced from detailed numerical analysis of fluid mechanics and thermal transport of the growth process. The FACT system was assembled, tested and employed to grow two TiC ingots. One of the ingots was characterized by x-ray diffraction at different axial locations. The x-ray rocking curves showed consistent characteristics of a manually grown ingot. It was also found that with the FACT system, the process conditions can be operated closer to the stability limits, due to fast response time and repetitive amounts of adjustment from the FACT system. The FACT system shows a major potential in growing quality TiC crystals in a cost-effective manner.

SIMS Investigations on Growth and Sector Zoning in Natural Hydrothermal Quartz: Isotopic and Trace Element Analyses

NASA Astrophysics Data System (ADS)

May, E.; Vennemann, T. W.; Baumgartner, L. P.; Meisser, N.

2014-12-01

Quartz is the most abundant mineral in the Earth's crust and is found in virtually every geological context. Despite its ubiquity and the detailed studies on the conditions of quartz crystallization, some questions concerning its growth and sector zoning with regard to trace element incorporation and oxygen isotope fractionations and the implications thereof for interpretations on the conditions of formation remain (e.g., Jourdan et al., 2009). This study presents new in-situ measurements of trace element and oxygen isotope ratios on natural hydrothermal quartz from an extensional gold-bearing quartz vein in the western Swiss Alps. The temperature of formation of the veins is estimated by quartz-hematite oxygen isotope thermometry to be about 360°C. A detailed SEM-CL study of this sample shows cyclic lamellar growth, alternating with phases of dissolution that are directly followed by macro-mosaic growth of the quartz, before returning to a cyclic lamellar growth again. Trace element concentrations (measured for Na, K, Li, Al, and Ti) notably showed Al/Si variations of three orders of magnitude and coupled Al and Li variations, likely substituting for Si in different growth zones with lower values in macro-mosaic zones precipitating after the period of dissolution. The oxygen isotope composition of the crystal, in contrast, is homogeneous through all growth zones (δ18O values between 15.6‰ and 16.2‰) indicating that the fluid must have been buffered by the host-rock and/or the source of the fluid remained the same despite the period of quartz dissolution. Furthermore, the temperature during crystallization of the quartz crystal has likely also remained similar. The fact that no variations are measured in oxygen isotope compositions but some variations in trace element contents may suggest that changes in pressure were important during the formation of this quartz crystal. Give the pressure effects on the solubility of quartz (Fournier and Potter, 1982), both the cyclic character of quartz growth and perhaps also the changes in Al/Si may be related to pressure variations caused by seismic activity during retrograde Alpine metamorphism. A-L. Jourdan et al. (2009) Mineralogical Magazine, 73, 615-632. R.O. Fournier and R.W. Potter (1982) Geochimica et Cosmochimica Acta, 46, 1969-1973.

Laser-Heated Floating Zone Production of Single-Crystal Fibers

NASA Technical Reports Server (NTRS)

Ritzert, Frank; Westfall, Leonard

1996-01-01

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.

Control of heat transfer in continuous-feeding Czochralski-silicon crystal growth with a water-cooled jacket

NASA Astrophysics Data System (ADS)

Zhao, Wenhan; Liu, Lijun

2017-01-01

The continuous-feeding Czochralski method is an effective method to reduce the cost of single crystal silicon. By promoting the crystal growth rate, the cost can be reduced further. However, more latent heat will be released at the melt-crystal interface under a high crystal growth rate. In this study, a water-cooled jacket was applied to enhance the heat transfer at the melt-crystal interface. Quasi-steady-state numerical calculation was employed to investigate the impact of the water-cooled jacket on the heat transfer at the melt-crystal interface. Latent heat released during the crystal growth process at the melt-crystal interface and absorbed during feedstock melting at the feeding zone was modeled in the simulations. The results show that, by using the water-cooled jacket, heat transfer in the growing crystal is enhanced significantly. Melt-crystal interface deflection and thermal stress increase simultaneously due to the increase of radial temperature at the melt-crystal interface. With a modified heat shield design, heat transfer at the melt-crystal interface is well controlled. The crystal growth rate can be increased by 20%.

Growth rates and interface shapes in germanium and lead tin telluride observed in-situ, real-time in vertical Bridgman furnaces

NASA Technical Reports Server (NTRS)

Barber, P. G.; Berry, R. F.; Debnam, W. J.; Fripp, A. L.; Woodell, G.; Simchick, R. T.

1995-01-01

Using the advanced technology developed to visualize the melt-solid interface in low Prandtl number materials, crystal growth rates and interface shapes have been measured in germanium and lead tin telluride semiconductors grown in vertical Bridgman furnaces. The experimental importance of using in-situ, real time observations to determine interface shapes, to measure crystal growth rates, and to improve furnace and ampoule designs is demonstrated. The interface shapes observed in-situ, in real-time were verified by quenching and mechanically induced interface demarcation, and they were also confirmed using machined models to ascertain the absence of geometric distortions. Interface shapes depended upon the interface position in the furnace insulation zone, varied with the nature of the crystal being grown, and were dependent on the extent of transition zones at the ends of the ampoule. Actual growth rates varied significantly from the constant translation rate in response to the thermophysical properties of the crystal and its melt and the thermal conditions existing in the furnace at the interface. In the elemental semiconductor germanium the observed rates of crystal growth exceeded the imposed translation rate, but in the compound semiconductor lead tin telluride the observed rates of growth were less than the translation rate. Finally, the extent of ampoule thermal loading influenced the interface positions, the shapes, and the growth rates.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Junjie; Zheng, Hong; Ren, Yang

We report the first single crystal growth of the correlated metal LaNiO 3 using a high-pressure optical-image floating zone furnace. The crystals were studied using single crystal/powder X-ray diffraction, resistivity, specific heat, and magnetic susceptibility. The availability of bulk LaNiO 3 crystals will (i) promote deep understanding in this correlated material, including the mechanism of enhanced paramagnetic susceptibility, and (ii) provide rich opportunities as a substrate for thin film growth such as important ferroelectric and/or multiferroic materials. As a result, this study demonstrates the power of high pO 2 single crystal growth of nickelate perovskites and correlated electron oxides moremore » generally.« less

Fluid mechanics and mass transfer in melt crystal growth: Analysis of the floating zone and vertical Bridgman processes

NASA Technical Reports Server (NTRS)

Brown, R. A.

1986-01-01

This research program focuses on analysis of the transport mechanisms in solidification processes, especially one of interest to the Microgravity Sciences and Applications Program of NASA. Research during the last year has focused on analysis of the dynamics of the floating zone process for growth of small-scale crystals, on studies of the effect of applied magnetic fields on convection and solute segregation in directional solidification, and on the dynamics of microscopic cell formation in two-dimensional solidification of binary alloys. Significant findings are given.

Center for the development of commercial crystal growth in space

NASA Technical Reports Server (NTRS)

Wilcox, William R.

1989-01-01

The second year of operation of the Center for Commercial Crystal Growth in Space is described. This center is a consortium of businesses, universities and national laboratories. The primary goal of the Center's research is the development of commercial crystal growth in space. A secondary goal is to develop scientific understanding and technology which will improve commercial crystal growth on earth. In order to achieve these goals the Center's research is organized into teams by growth technique; melt growth, solution growth, and vapor growth. The melt growth team is working on solidification and characterization of bulk crystals of gallium arsenide and cadmium telluride. They used high resolution X-ray topography performed at the National Synchrotron Light Source at Brookhaven National Laboratory. Streak-like features were found in the diffraction images of semi-insulating undoped LEC GaAs. These were shown to be (110) antiphase boundaries, which have not been reported before but appear to be pervasive and responsible for features seen via less-sensitive characterization methods. The results on CdTe were not as definitive, but indicate that antiphase boundaries may also be responsible for the double peaks often seen in X-ray rocking curves of this material. A liquid encapsulated melt zone system for GaAs has been assembled and techniques for casting feed rods developed. It was found that scratching the inside of the quartz ampoules with silicon carbide abrasive minimized sticking of the GaAs to the quartz. Twelve floating zone experiments were done.

Compositional Zoning in Kilauea Olivine: A Geochemical Tool for Investigating Magmatic Processes at Hawaiian Volcanoes

NASA Astrophysics Data System (ADS)

Lynn, Kendra J.

Olivine compositions and zoning patterns have been widely used to investigate the evolution of magmas from their source to the Earthfs surface. Modeling the formation of compositional zoning in olivine crystals has been used to retrieve timescales of magma residence, mixing, and transit. This dissertation is composed of three projects that apply diffusion chronometry principles to investigate how zoned olivine phenocrysts record magmatic processes at Hawaiian volcanoes. Olivine phenocrysts from K.lauea, the most active and thoroughly studied volcano in Hawaiei, are used to develop a better understanding of how Hawaiian olivine crystals record magmatic histories. This work begins by examining how crustal processes such as magma mixing and diffusive reequilibration can modify olivine compositions inherited from growth in parental magmas (Chapter 2). Diffusive re-equilibration of Fe-Mg, Mn, and Ni in olivine crystals overprints the chemical relationships inherited during growth, which strongly impacts interpretations about mantle processes and source components. These issues are further complicated by sectioning effects, where small (400 ƒEm along the c-axis) olivine crystals are more susceptible to overprinting compared to large (800 ƒEm) crystals. Olivine compositions and zoning patterns are then used to show that magmas during K.laueafs explosive Keanak.koei Tephra period (1500-1823 C.E.) were mixed and stored in crustal reservoirs for weeks to months prior to eruption (Chapter 3). Fe-Mg disequilibrium between olivine rims and their surrounding glasses show that a late-stage mixing event likely occurred hours to days prior to eruption, but the exact timescale is difficult to quantify using Fe-Mg and Ni diffusion. Lithium, a rapidly diffusing trace element in olivine, is modeled for the first time in a natural volcanic system to quantify this late-stage, short-duration mixing event (Chapter 4). Lithium zoning in olivine records both growth and diffusion processes that are affected by charge balancing requirements with growth zoning of P. Timescales from modeling diffuse Li zoning range from a few hours to three weeks, but most record short storage durations of four days or less. These timescales correspond to short storage periods after mixing. Thus, Li probably records the final perturbation of a magmatic system prior to eruption.

Modulation of calcium oxalate dihydrate growth by selective crystal-face binding of phosphorylated osteopontin and polyaspartate peptide showing occlusion by sectoral (compositional) zoning.

PubMed

Chien, Yung-Ching; Masica, David L; Gray, Jeffrey J; Nguyen, Sarah; Vali, Hojatollah; McKee, Marc D

2009-08-28

Calcium oxalate dihydrate (COD) mineral and the urinary protein osteopontin/uropontin (OPN) are commonly found in kidney stones. To investigate the effects of OPN on COD growth, COD crystals were grown with phosphorylated OPN or a polyaspartic acid-rich peptide of OPN (DDLDDDDD, poly-Asp(86-93)). Crystals grown with OPN showed increased dimensions of the {110} prismatic faces attributable to selective inhibition at this crystallographic face. At high concentrations of OPN, elongated crystals with dominant {110} faces were produced, often with intergrown, interpenetrating twin crystals. Poly-Asp(86-93) dose-dependently elongated crystal morphology along the {110} faces in a manner similar to OPN. In crystal growth studies using fluorescently tagged poly-Asp(86-93) followed by imaging of crystal interiors using confocal microscopy, sectoral (compositional) zoning in COD was observed resulting from selective binding and incorporation (occlusion) of peptide exclusively into {110} crystal sectors. Computational modeling of poly-Asp(86-93) adsorption to COD {110} and {101} surfaces also suggests increased stabilization of the COD {110} surface and negligible change to the natively stable {101} surface. Ultrastructural, colloidal-gold immunolocalization of OPN by transmission electron microscopy in human stones confirmed an intracrystalline distribution of OPN. In summary, OPN and its poly-Asp(86-93) sequence similarly affect COD mineral growth; the {110} crystallographic faces become enhanced and dominant attributable to {110} face inhibition by the protein/peptide, and peptides can incorporate into the mineral phase. We, thus, conclude that the poly-Asp(86-93) domain is central to the OPN ability to interact with the {110} faces of COD, where it binds to inhibit crystal growth with subsequent intracrystalline incorporation (occlusion).

Electromigration process for the purification of molten silicon during crystal growth

DOEpatents

Lovelace, Alan M. Administrator of the National Aeronautics and Space; Shlichta, Paul J.

1982-01-01

A process for the purification of molten materials during crystal growth by electromigration of impurities to localized dirty zones. The process has particular applications for silicon crystal growth according to Czochralski techniques and edge-defined film-fed growth (EFG) conditions. In the Czochralski crystal growing process, the impurities are electromigrated away from the crystallization interface by applying a direct electrical current to the molten silicon for electromigrating the charged impurities away from the crystal growth interface. In the EFG crystal growth process, a direct electrical current is applied between the two faces which are used in forming the molten silicon into a ribbon. The impurities are thereby migrated to one side only of the crystal ribbon. The impurities may be removed or left in place. If left in place, they will not adversely affect the ribbon when used in solar collectors. The migration of the impurity to one side only of the silicon ribbon is especially suitable for use with asymmetric dies which preferentially crystallize uncharged impurities along one side or face of the ribbon.

Crystallographic control of surface structure on the sectoral zoning of iron in a diopside from Orford nickel mine (Quebec), Canada

NASA Astrophysics Data System (ADS)

Paquette, J.; Zangooi, A.; Thornton, K.

2004-05-01

The influence of surface structure on partitioning between mineral and melt (or solution) has been noted by other workers in a handful of minerals, including calcite, dolomite, apatite, topaz and diamond. Each one of these minerals displays at least one crystallographic face where steps present during crystal growth are not equivalent by symmetry. When this is the case, sectors grown at the edge of these steps commonly show differential incorporation of minor or trace elements. In the diopside investigated here, electron probe microanalyses performed on the as-grown (100) surface of several crystals show concentric and sectoral zoning defined by variations in Fe content. Atomic force microscopy (AFM) was used to study the surfaces of the three crystallographic forms present on the diopside crystals, with the goal of relating the compositional zoning to the surface structure of the faces. The dominant {100} faces are covered with growth hillocks consisting of four vicinal faces defined by steps parallel to [010] and [001]. The steps are often bunched into macrosteps and the resulting hillocks are visible optically. The steps along the two crystallographic directions show significant differences in straightness and smoothness that indicate non-equivalent kinetics. The wavier steps correspond to Fe-enriched areas within the {100} sectors. The {010} faces, next in morphological importance, are dominated by a single step orientation and show no differential incorporation. They display topography related to polysynthetic twinning. The {110} faces are much smaller and very few show resolvable steps. Sector zoning (i.e. diffential partitioning among non-equivalent crystallographic faces) has been described in the past from pyroxenes. Explanations have invoked either differences in surface structure among non-equivalent faces or their unequal growth rates. This particular occurrence indicates that trace element incorporation is, in fact, highly site-specific and that significant compositioinal zoning can be induced on a single face without invoking the effect of growth rate. The natural diopside crystals from the Orford nickel mine (Brompton, Quebec) show a unusual bladed habit flattened on {100} faces. Exceptional fluid chemistry during crystallization may therefore be required for the persistence of steps responsible for differential incorporation. Nevertheless, whenever this zoning is present, the trace element involved cannot be expected to reflect thermodynamic equilibrium between the solid and the fluid from which it crystallized.

High water concentrations in a primitive Deccan lava: evidence from clinopyroxene crystals

NASA Astrophysics Data System (ADS)

Seaman, Sheila

2017-04-01

Measurements of water concentrations in clinopyroxene phenocrysts in the Powai ankaramite flow, located near Mumbai, west of the Western Ghats escarpment of the Deccan province, India, indicate that the parent magma of the flow hosted at least 4.3 wt.% water, an unusually high water concentration for a continental flood basalt magma. However, similar water concentrations (3.39 to 6.61 wt.%) were calculated by Xia et al. (2016), also on the basis of water concentrations in clinopyroxene crystals, for continental basalts of the Tarin basin in northwestern China, which hosts >200,000 km3 of flood basalts (Xia et al., 2016). In the Powai ankaramite flow, textural and compositional features of clinopyroxene phenocrysts further support crystallization in a water-rich melt. The flow hosts clinopyroxene and olivine phenocrysts. Chatterjee and Sheth (2015) showed that phenocrysts in the flow were part of a cumulate layer intruded by high-temperature basaltic melt at 6 kb and 1230oC, so the phenocrysts record characteristics of the cumulate parent melt. Clinopyroxene phenocrysts are large (to 0.5 cm diameter), euhedral, are oscillatorily zoned in water, Mg, Fe, and Ca concentrations, and have concentric bands 100-200 microns thick of fine (10-20 micron diameter) melt inclusions. Olivine phenocrysts are smaller (to 0.1 cm diameter, are unzoned, and host only larger isolated melt inclusions. Zones in the cpx phenocrysts where melt inclusion-rich concentric bands occur have higher concentrations of water than inclusion-free zones. Water concentrations of cpx were used to calculate water concentrations in the melt from which the crystals formed using partition coefficients of Hauri et al. (2004). Water concentrations in the parent magma were between 4.35 and 8.26 wt. % based on water concentrations in cpx. Both Mg and Fe are relatively depleted in the water- and melt inclusion-rich zones in cpx, and Ca is enriched in these zones. Oscillatory zoning in cpx may be a result of repeated growth of cpx in water-richer and water-poorer boundary layers in which water lowered melt viscosity and enhanced diffusion and crystal growth rates. Water-enhanced growth rates may have resulted in capture of melt inclusions preserved in water-rich cpx zones. Mg was preferentially incorporated into the cpx, causing Ca and water to build up in the boundary layer, and Mg and Fe to become relatively depleted in the boundary layer, as discussed for oscillatorially-zoned minerals by Wang and Merino (1993). These apparently water-dependent variations in crystal growth processes ugsuggest that at least this Deccan magma was relatively hydrous. Melt inclusions in olivine phenocrysts, however, preserve lower water concentrations ( 1.2 wt. %) than those indicated by water concentration in cpx phenocrysts. This disparity may be evidence of water loss from melt inclusions in olivine (Gaetani et al., 2009) or may indicate that cpx and ol crystals did not crystallize from the same parent at the same time.

Aspects of rf-heating and gas-phase doping of large scale silicon crystals grown by the Float Zone technique

NASA Astrophysics Data System (ADS)

Zobel, F.; Mosel, F.; Sørensen, J.; Dold, P.

2018-05-01

Float Zone growth of silicon crystals is known as the method for providing excellent material properties. Basic principle of this technique is the radiofrequency induction heating, main aspects of this method will be discussed in this article. In contrast to other methods, one of the advantages of the Float Zone technique is the possibility for in-situ doping via gas phase. Experimental results on this topic will be shown and discussed.

The formation age of ores from the Pebble Cu-Au-Mo giant deposit (Alaska, United States)

NASA Astrophysics Data System (ADS)

Kremenetskii, A. A.; Popov, V. S.; Gromalova, N. A.

2012-02-01

Zircons from the porphyry-like quartz-diorite boss of the Pebble Cu-Au-Mo deposit (southwest Alaska) have been examined. By their appearance and internal structure (cathode luminescence and electron probing), the zircons have been subdivided into four genetic groups: (1) xenogenic detrital (mainly rounded); (2) magmatogene (protolith crystal in the center and growth zone at the edge); (3) hydrothermally altered (with new-formed regeneration edges in growth zones); (4) metamict-altered (unconsolidated center of the crystal and sectoring in growth zones). Based on SHRIMP U-Pb dating for the principal heterogeneous elements in every group, the following stages of ore formation have been identified for the Pebble deposit: (a) crystallization of quartz diorite-porphyry bosses (95-92 Ma, the concordant age is 94.7 ± 1.5 Ma); (b) late magmatic metasomatic alterations with copper-molybdenum mineralization (92-85 Ma, the concordant age is 90.15 ± 0.78 Ma); (c) postmagmatic argillization with epithermal gold-sulfide mineralization (82-80 Ma, the concordant age is 82.9 ± 2.7 Ma).

An Electron Microscopy Study of Graphite Growth in Nodular Cast Irons

NASA Astrophysics Data System (ADS)

Laffont, L.; Jday, R.; Lacaze, J.

2018-04-01

Growth of graphite during solidification and high-temperature solid-state transformation has been investigated in samples cut out from a thin-wall casting which solidified partly in the stable (iron-graphite) and partly in the metastable (iron-cementite) systems. Transmission electron microscopy has been used to characterize graphite nodules in as-cast state and in samples having been fully graphitized at various temperatures in the austenite field. Nodules in the as-cast material show a twofold structure characterized by an inner zone where graphite is disoriented and an outer zone where it is well crystallized. In heat-treated samples, graphite nodules consist of well-crystallized sectors radiating from the nucleus. These observations suggest that the disoriented zone appears because of mechanical deformation when the liquid contracts during its solidification in the metastable system. During heat-treatment, the graphite in this zone recrystallizes. In turn, it can be concluded that nodular graphite growth mechanism is the same during solidification and solid-state transformation.

Morphology of growth of Bi2Sr2CaCu2O8 single crystals

NASA Astrophysics Data System (ADS)

Indenbom, M. V.; van der Beek, C. J.; Berseth, V.; Wolf, Th.; Berger, H.; Benoit, W.

1996-12-01

A good correlation of twins on the basal surface of flux-grown Bi2Sr2CaCu2Ox (BSCCO) single crystals with surface. growth steps is observed, the b-axis being perpendicular to the steps and, thus, parallel to the growth direction. It is found that mono-twin BSCCO single crystals produced by the travelling solvent floating zone method also grow preferentially along b, i.e. nearly perpendicularly to the boule axis, contrary to the common belief. This new understanding of the morphology of growth explains the nature of major defects in these crystals, which considerably change their measured superconducting properties, in a different way.

The Growth and Characterization of the Bismuth Strontium-Calcium 2212 Superconductor

NASA Astrophysics Data System (ADS)

Moulton, Linda Vidale

A miniaturized float zone technique, sometimes referred to as the Laser-heated Pedestal Growth (LHPG) method, was used to produce high quality crystals of the incongruently melting rm Bi_2Sr_2CaCu _2O_{8+delta} (2212) superconductor. The main focus of this research was to (1) produce superconducting samples having different compositions, (2) identify the melt compositions and growth temperatures which produced these samples, and (3) determine the variation of their superconducting transition temperature (T _{rm C}) with composition and processing conditions. The rm Bi_2(Sr,Ca) _3Cu_2O_{8+delta} crystallization experiments were supplemented by a series of similar experiments on the incongruently melting compound rm Ca_3Al_2O_6. The phase equilibria in the CaO-rm Al_2O _3 system has been thoroughly studied, and by analyzing the float-zone growth of this simpler and better-characterized material, it was verified that phase equilibria information and solidification behavior could be extracted from and explained by these solidification experiments. Two different types of nonplanar, crystal/melt interface morphologies were observed in the rm Ca_3Al_2O_6 experiments. Each reflected the influence of the phase equilibria in the CaO-rm Al_2O_3 system and component segregation in the melt. The molten zone compositions were found to approach those predicted by the CaO-rm Al_2O_3 phase diagram as the growth rate decreased, in accordance with the Burton-Prim Slichter relationship. Excellent agreement was obtained between actual phases found to coexist at the rm Ca_3Al_2O_6 /melt interface and the predictions of classical crystal growth theory. Based on the results of the rm Ca _3Al_2O_6 crystallization study, the crystal/melt equilibria in the far more complex rm Bi_2O_3-SrO-CaO-CuO system was evaluated by determining the phases formed during the superconductor growth experiments. The melt compositions were found to be rm Bi_2O_3 -rich and SrO-poor relative to the compositions of the 2212 crystals grown from them. The CaO and CuO segregation coefficients, on the other hand, were observed to be near unity. As one would expect for an incongruently -melting compound, segregation at the solidification front generally decreased with increasing crystallization temperature, but all the segregation coefficients were not observed to simultaneously approach unity. The superconducting transition temperatures (T _{rm C}'s) of six as-crystallized samples having homogeneous crystal compositions were also measured. Sample T_{rm C} was observed to increase with increasing growth temperature and, therefore, change with crystal composition. The results of this study suggested that it is desirable to grow crystals at the highest possible crystallization temperature since they will: (1) have the highest as-grown T_{rm C} 's, and (2) solidify with the least component segregation at the growth interface. In addition, the analysis presented here suggests that such growth is not recommended at higher growth rates, since crystals with mid-range solidus compositions (and consequently, moderate growth temperatures) should crystallize most reliably as single-phase samples at higher growth rates.

Effect of NH4-N/P and Ca/P molar ratios on the reactive crystallization of calcium phosphates for phosphorus recovery from wastewater

NASA Astrophysics Data System (ADS)

Vasenko, Liubov; Qu, Haiyan

2017-02-01

In this work, the effects of operational parameters, initial phosphorus concentration and molar ratios of Ca/P and NH4-N/P (further in the text N/P), on the nature and purity of precipitated phosphorus products have been investigated in an artificial system that mimics the supernatant in wastewater treatment plants. Metastable zone width was determined for two target phosphorus products: DCPD (dicalcium phosphate dihydrate) and HAp (hydroxyapatite) in the range of pH 4.5 - 7. HAp crystallizes at final pH higher than 6.3 while DCPD crystallizes at the final pH in between 4.7 and 5.7. At the final pH 5.7 - 6.3 and at pH lower than 4.7 the mixtures of DCPD and HAp were obtained. It was observed that N/P ratio affects not only the metastable zone width but also the kinetics of crystal growth for both DCPD and HAp: the higher the N/P ratio, the lower is the growth rate for both P-products. Investigation of the effect of Ca/P and N/P ratios on the nucleation and crystal growth of DCPD in batch crystallization experiment was performed. It showed that at high supersaturation level, crystals with larger median size can be obtained at higher N/P ratio despite the negative effects of N/P ratio on the growth rate of the crystals.

Analytics of crystal growth in space

NASA Technical Reports Server (NTRS)

Chang, C. E.; Lefever, R. A.; Wilcox, W. R.

1975-01-01

The variation of radial impurity distribution induced by surface tension driven flow increases as the zone length decreases in silicon crystals grown by floating zone melting. In combined buoyancy driven and surface tension driven convection at the gravity of earth, the buoyancy contribution becomes relatively smaller as the zone diameter decreases and eventually convection is dominated by the surface tension driven flow (in the case of silicon, for zones of less than about 0.8 cm in diameter). Preliminary calculations for sapphire suggest the presence of an oscillatory surface tension driven convection as a result of an unstable melt surface temperature that results when the zone is heated by a radiation heater.

Float zone growth and spectroscopic properties of Yb:CaYAlO4 single crystal for ultra-short pulse lasers

NASA Astrophysics Data System (ADS)

Narita, Moe; Higuchi, Mikio; Ogawa, Takayo; Wada, Satoshi; Miura, Akira; Tadanaga, Kiyoharu

2018-06-01

Yb:CaYAlO4 single crystals were grown by the floating zone method and their spectral properties were investigated. Void formation was effectively suppressed by using a feed rod of Y-rich composition with the aid of a double zone-pass technique. For the oxygen excess composition of Yb:Ca0.9925Y1.0075AlO4.00375, a void-free crystal was obtained by performing only the double zone-pass. On the other hand, for cation-deficient type of Yb:Ca0.9925Y1.005AlO4, void-free crystal could not be obtained by performing the double zone-pass. The void formation is attributable to the constitutional supercooling caused by segregation of main constituents of Y and Ca, and the congruent composition may exist in the Y-rich region with existence of interstitial excess oxide ions. The absorption cross section for σ-polarization was slightly larger than that for π-polarization, which is reasonable on the basis of the crystal structure of CaYAlO4.

Purification and Crystal Growth of Lead Iodide by Physical Vapor Transport Method

NASA Technical Reports Server (NTRS)

Wright, G. W.; Cole, M.; Chen, Y.-F.; Chen, K.-T.; Chen, H.; Chattopadhyay, K.; Burger, A.

1998-01-01

Lead iodide (PbI2) is a layered compound semiconductor being developed as room temperature x- and gamma-ray detector. Compared to the more studied material, mercuric iodide, PbI2 has a higher melting temperature and no phase transition until liquid phase which are indications of better mechanical properties. In this study, the source material was purified by the zone-refining process, and the purest section was extracted from center of the the zone-refined ingot to be grown by physical vapor transport (PVT) method. The zone-refined material and as-grown crystals were characterized by optical microscopy and differential scanning calorimetry (DSC) to reveal the surface morphology, purity and stoichiometry. The results shows that both materials are near-stoichiometric composition, with the purity of the as-grown crystals higher than zone-refined materials. The resistivity of the as-grown crystal (10" Omega-cm) was derived from current-voltage (I-V) measurement, and is 10 times higher than the zone-refined materials. Detail results will be presented and discussed.

Guidance system for low angle silicon ribbon growth

DOEpatents

Jewett, David N.; Bates, Herbert E.; Milstein, Joseph B.

1986-07-08

In a low angle silicon sheet growth process, a puller mechanism advances a seed crystal and solidified ribbon from a cooled growth zone in a melt at a low angle with respect to the horizontal. The ribbon is supported on a ramp adjacent the puller mechanism. Variations in the vertical position of the ribbon with respect to the ramp are isolated from the growth end of the ribbon by (1) growing the ribbon so that it is extremely thin, preferably less than 0.7 mm, (2) maintaining a large growth zone, preferably one whose length is at least 5.0 cm, and (3) spacing the ramp from the growth zone by at least 15 cm.

Advanced crystal growth techniques for thallium bromide semiconductor radiation detectors

NASA Astrophysics Data System (ADS)

Datta, Amlan; Becla, Piotr; Guguschev, Christo; Motakef, Shariar

2018-02-01

Thallium Bromide (TlBr) is a promising room-temperature radiation detector candidate with excellent charge transport properties. Currently, Travelling Molten Zone (TMZ) technique is widely used for growth of semiconductor-grade TlBr crystals. However, there are several challenges associated with this type of crystal growth process including lower yield, high thermal stress, and low crystal uniformity. To overcome these shortcomings of the current technique, several different crystal growth techniques have been implemented in this study. These include: Vertical Bridgman (VB), Physical Vapor Transport (PVT), Edge-defined Film-fed Growth (EFG), and Czochralski Growth (Cz). Techniques based on melt pulling (EFG and Cz) were demonstrated for the first time for semiconductor grade TlBr material. The viability of each process along with the associated challenges for TlBr growth has been discussed. The purity of the TlBr crystals along with its crystalline and electronic properties were analyzed and correlated with the growth techniques. Uncorrected 662 keV energy resolutions around 2% were obtained from 5 mm x 5 mm x 10 mm TlBr devices with virtual Frisch-grid configuration.

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

NASA Technical Reports Server (NTRS)

McEwen, B. F.; Song, M. J.; Landis, W. J.

1991-01-01

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.

Fluid mechanics in crystal growth - The 1982 Freeman scholar lecture

NASA Technical Reports Server (NTRS)

Ostrach, S.

1983-01-01

An attempt is made to unify the current state of knowledge in crystal growth techniques and fluid mechanics. After identifying important fluid dynamic problems for such representative crystal growth processes as closed tube vapor transport, open reactor vapor deposition, and the Czochralski and floating zone melt growth techniques, research results obtained to date are presented. It is noted that the major effort to date has been directed to the description of the nature and extent of bulk transport under realistic conditions, where bulk flow determines the heat and solute transport which strongly influence the temperature and concentration fields in the vicinity of the growth interface. Proper treatment of near field, or interface, problems cannot be given until the far field, or global flow, involved in a given crystal growth technique has been adequately described.

Thermal Modeling of Bridgman Crystal Growth

NASA Technical Reports Server (NTRS)

Cothran, E.

1983-01-01

Heat Flow modeled for moving or stationary rod shaped sample inside directional-solidification furnace. Program effectively models one-dimensional heat flow in translating or motionless rod-shaped sample inside of directionalsolidification furnace in which adiabatic zone separates hot zone and cold zone. Applicable to systems for which Biot numbers in hot and cold zones are less than unity.

Future float zone development in industry

NASA Technical Reports Server (NTRS)

Sandfort, R. M.

1980-01-01

The present industrial requirements for float zone silicon are summarized. Developments desired by the industry in the future are reported. The five most significant problems faced today by the float zone crystal growth method in industry are discussed. They are economic, large diameter, resistivity uniformity, control of carbon, and swirl defects.

Characterization of CdGeAs 2 grown by the float zone technique under microgravity

NASA Astrophysics Data System (ADS)

Labrie, D.; George, A. E.; Simpson, A. M.; Paton, B. E.; Ginovker, A.; Saghir, M. Z.

2000-01-01

One polycrystalline and one single-crystal CdGeAs 2 feed rods with 9 mm diameter were processed by the float-zone technique under microgravity on SPACEHAB-SH04 during the STS-77 Space Shuttle Endeavour mission. An eutectic salt of LiCl and KCl was used as an encapsulant to suppress Cd and As evaporation from the melt. Post-flight chemical, structural, electronic, and optical characterization of the two samples is presented. Single-crystal growth was achieved using a seed crystal.

Electron microprobe study of lunar and planetary zoned plagioclase feldspars: An analytical and experimental study of zoning in plagioclase

NASA Technical Reports Server (NTRS)

Smith, R. K.; Lofgren, G. E.

1982-01-01

Natural and experimentally grown zoned plagioclase feldspars were examined by electron microprobe. The analyses revealed discontinuous, sector, and oscillary chemical zoning superimposed on continuous normal or reverse zoning trends. Postulated mechanisms for the origin of zoning are based on either physical changes external to the magma (P, T, H2O saturation) or kinetic changes internal to the magma (diffusion, supersaturation, growth rate). Comparison of microprobe data on natural zoned plagioclase with zoned plagioclase grown in controlled experiments show that it may be possible to distinguish zonal development resulting from physio-chemical changes to the bulk magma from local kinetic control on the growth of individual crystals.

An inverse modeling strategy and a computer program to model garnet growth and resorption

NASA Astrophysics Data System (ADS)

Lanari, Pierre; Giuntoli, Francesco

2017-04-01

GrtMod is a computer program that allows numerical simulation of the pressure-temperature (P-T) evolution of garnet porphyroblasts based on the composition of successive growth zones preserved in natural samples. For each garnet growth stage, a new reactive bulk composition is optimized, allowing for resorption and/or fractionation of the previously crystalized garnet. The successive minimizations are performed using a heuristic search method and an objective function that quantify the amount by which the predicted garnet composition deviates from the measured values. The automated strategy of GrtMod includes a two stages optimization and one refinement stage. In this contribution, we will present several application examples. The new strategy provides quantitative estimates of the optimal P-T conditions whereas it was generally derived in a qualitatively way by using garnet isopleth intersections in equilibrium phase diagrams. GrtMod can also be used to model the evolution of the reactive bulk composition along any P-T trajectories. The results for typical MORB and metapelite compositions demonstrate that fractional crystallization models are required to derive accurate P-T information from garnet compositional zoning. GrtMod can also be used to retrieve complex garnet histories involving several stages of resorption. For instance, it has been used to model the P-T condition of garnet growth in grains from the Sesia Zone (Western Alps). The compositional variability of successive growth zones is characterized using standardized X-ray maps and the program XMapTools. Permian garnet cores crystalized under granulite facies conditions (T > 800°C and P = 6 kbar), whereas Alpine garnet rims grew at eclogite facies conditions (650°C and 16 kbar) involving several successive episodes of resorption. The model predicts that up to 50 vol% of garnet was dissolved before a new episode of garnet growth.

Understanding Growth Rate Limitations in Production of Single-Crystal Cadmium Zinc Telluride (CZT) by the Traveling Heater Method (THM)

NASA Astrophysics Data System (ADS)

Peterson, Jeffrey H.

Cadmium telluride (CdTe) and cadmium zinc telluride (CZT) are important optoelectronic materials with applications ranging from medical imaging to nuclear materials monitoring. However, CZT and CdTe have long been plagued by second-phase particles, inhomogeneity, and other defects. The traveling heater method (THM) is a promising approach for growing CZT and other compound semiconductors that has been shown to grow detector-grade crystals. In contrast to traditional directional solidification, the THM consists of a moving melt zone that simultaneously dissolves a polycrystalline feed while producing a single-crystal of material. Additionally, the melt is highly enriched in tellurium, which allows for growth at lower temperatures, limiting the presence of precipitated tellurium second-phase particles in the final crystal. Unfortunately, the THM growth of CZT is limited to millimeters per day when other growth techniques can grow an order of magnitude faster. To understand these growth limits, we employ a mathematical model of the THM system that is formulated to realistically represent the interactions of heat and species transport, fluid flow, and interfacial dissolution and growth under conditions of local thermodynamic equilibrium and steady-state growth. We examine the complicated interactions among zone geometry, continuum transport, phase change, and fluid flow driven by buoyancy. Of particular interest and importance is the formation of flow structures in the liquid zone of the THM that arise from the same physical mechanism as lee waves in atmospheric flows and demonstrate the same characteristic Brunt-Vaisala scaling. We show that flow stagnation and reversal associated with lee-wave formation are responsible for the accumulation of tellurium and supercooled liquid near the growth interface, even when the lee-wave vortex is not readily apparent in the overall flow structure. The supercooled fluid is posited to result in morphological instability at growth rates far below the limit predicted by the classical criterion by Tiller et al. for constitutional supercooling.

Material and detector properties of cadmium manganese telluride (Cd 1-xMn xTe) crystals grown by the modified floating-zone method

DOE PAGES

Hossain, A.; Gu, G. D.; Bolotnikov, A. E.; ...

2014-12-24

We demonstrated the material- and radiation-detection properties of cadmium manganese telluride (Cd 1-xMn xTe; x=0.06), a wide-band-gap semiconductor crystal grown by the modified floating-zone method. We investigated the presence of various bulk defects, such as Te inclusions, twins, and dislocations of several as-grown indium-doped Cd 1-xMn xTe crystals using different techniques, viz., IR transmission microscopy, and chemical etching. We then fabricated four planar detectors from selected CdMnTe crystals, characterized their electrical properties, and tested their performance as room-temperature X- and gamma-ray detectors. Thus, our experimental results show that CMT crystals grown by the modified floating zone method apparently are freemore » from Te inclusions. However, we still need to optimize our growth parameters to attain high-resistivity, large-volume single-crystal CdMnTe.« less

Crystal nucleation in metallic alloys using x-ray radiography and machine learning

PubMed Central

Arteta, Carlos; Lempitsky, Victor

2018-01-01

The crystallization of solidifying Al-Cu alloys over a wide range of conditions was studied in situ by synchrotron x-ray radiography, and the data were analyzed using a computer vision algorithm trained using machine learning. The effect of cooling rate and solute concentration on nucleation undercooling, crystal formation rate, and crystal growth rate was measured automatically for thousands of separate crystals, which was impossible to achieve manually. Nucleation undercooling distributions confirmed the efficiency of extrinsic grain refiners and gave support to the widely assumed free growth model of heterogeneous nucleation. We show that crystallization occurred in temporal and spatial bursts associated with a solute-suppressed nucleation zone. PMID:29662954

Experiment 13: The Study of Dopant Segregation Behavior During the Growth of GaAs in Microgravity on USML-2

NASA Technical Reports Server (NTRS)

Matthiesen, David H.; Kaforey, Monica L.; Bly, J. M.; Chait, Arnon; Kafalas, James; Carlson, Douglas

1998-01-01

An investigation into the segregation behavior of selenium doped gallium arsenide (Se/GaAs) during directional solidification in the microgravity environment was conducted using the Crystal Growth Furnace (CGF) aboard the second United States Microgravity Laboratory (USML-2). Two crystals were successfully processed on USML-2, which lasted from October 20 to November 7, 1995. The first sample was processed for 67 hours, 45 minutes (MET 5/04:53:45-8/00:23:50) and included 19 hours of growth at 0.5 microns/sec which yielded 3.42 cm of sample length, and 5 hours of growth at 1.5 microns/sec which yielded 2.7 cm of sample. During the second experiment, the furnace temperature was adjusted to move the melt-solid interface position towards the hot end of the furnace. The second sample was processed for 50 hours, 10 minutes (MET 8/18:48:49-10/21:58:54) and included 11 hours of growth at 0.5 microns/sec which yielded 1.98 cm of sample, and 1 hour, 25 minutes of growth at 5.0 microns/sec which yielded 2.6 cm of sample. This sample provides an order of magnitude change in growth rate and reproduces one of the growth rates used during USML-1. In contrast to the results from USML-1, no voids were present in either crystal grown on USML-2. The absence of voids in either sample indicates that growth rate changes alone were not responsible for the formation of voids found in the crystals grown on USML-1. Sections of the ground-based and flight crystals grown on USML-2 were cut and polished. All of the interface demarcation lines expected from the current pulse interface demarcation (CPID) system have been identified. These measurements have been analyzed for interface positions, interface shapes, and growth rates. Using a newly developed technique, based on experimental and numerical results, the seeding interface reproducibility from run to run was <= 2.5 mm. The seeding interface position could be controllably moved, with respect to the furnace zones, by adjusting the control set points of the heating zones. The interface shapes flattened slightly as the interface position moved closer to the hot zone but was always an unfavorable concave into the solid shape. The growth rate was found to equal the furnace translation rate, after a 2 -hour transient, for growth rates <= 1.0 microns/sec. Segregation measurements for the ground-based crystals are indicative of complete mixing behavior, as expected. Segregation measurements of the flight crystals are still in progress.

THF water hydrate crystallization: an experimental investigation

NASA Astrophysics Data System (ADS)

Devarakonda, Surya; Groysman, Alexander; Myerson, Allan S.

1999-08-01

Supersaturated solutions of THF-water hydrate system were experimentally studied before and during crystallization, to examine the system's behavior in the metastable zone and observe any anomalies suggesting cluster formation. Nucleation induction time measurements, with and without additives, were performed to screen potential growth inhibitors. Shifts in the onset points of crystallization for water and THF-water mixtures with additives were measured using differential scanning calorimetry (DSC). Aspartame was among one of the few successfully screened inhibitors. Preliminary on-line crystal size distribution (CSD) measurements were performed on this system to monitor the crystal size during crystallization. The CSD data was also used to compute the hydrate crystal growth rates, which were found to be in the order of 145 μm/h.

Space- and Ground-Based Crystal Growth Using a Baffle (CGB)

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Marin, C.; Peignier, T.; Duffar, T.; Volz, M.; Jeter, L.; Luz, P.

2001-01-01

The composition of semiconductor crystals produced in space by conventional melt-growth processes (directional solidification and zone melting) is affected by minute levels of residual micro-acceleration, which causes natural convection. The residual acceleration has random magnitude, direction and frequency. Therefore, the velocity field in the melt is apriori unpredictable. As a result, the composition of the crystals grown in space can not be predicted and reproduced. The method for directional solidification with a submerged heater or a baffle was developed under NASA sponsorship. The disk-shaped baffle acts as a partition, creating a small melt zone at the solid-liquid interface. As a result, in ground based experiment the level of buoyancy-driven convection at the interface is significantly reduced. In several experiments with Te-doped GaSb, nearly diffusion controlled segregation was achieved.

Crystallization kinetics of olivine-phyric shergottites

NASA Astrophysics Data System (ADS)

Ennis, Megan E.; McSween, Harry Y.

2014-08-01

Crystal size distribution (CSD) and spatial distribution pattern (SDP) analyses are applied to the early crystallizing phases, olivine and pyroxene, in olivine-phyric shergottites (Elephant moraine [EET] 79001A, Dar al Gani [DaG] 476, and dhofar [Dho] 019) from each sampling locality inferred from Mars ejection ages. Trace element zonation patterns (P and Cr) in olivine are also used to characterize the crystallization history of these Martian basalts. Previously reported 2-D CSDs for these meteorites are re-evaluated using a newer stereographically corrected methodology. Kinks in the olivine CSD plots suggest several populations that crystallized under different conditions. CSDs for pyroxene in DaG 476 and EET 79001A reveal single populations that grew under steady-state conditions; pyroxenes in Dho 019 were too intergrown for CSD analysis. Magma chamber residence times of several days for small grains to several months for olivine megacrysts are calculated using the CSD slopes and growth rates inferred from previous experimental data. Phosphorus imaging in olivines in DaG 476 and Dho 019 indicate rapid growth of skeletal, sector-zoned, or patchy cores, probably in response to delayed nucleation, followed by slow growth, and finally rapid dendritic growth with back-filling to form oscillatory zoning in rims. SPD analyses indicate that olivine and pyroxene crystals grew or accumulated in clusters rather than as randomly distributed grains. These data reveal complex solidification histories for Martian basalts, and are generally consistent with the formation at depth of olivine megacryst cores, which were entrained in ascending magmas that crystallized pyroxenes, small olivines, and oscillatory rims on megacrysts.

Face-by-face growth of sucrose crystals from aqueous solutions in the presence of raffinose—II: Growth morphology and segregation

NASA Astrophysics Data System (ADS)

Sgualdino, G.; Aquilano, D.; Pastero, L.; Vaccari, G.

2007-10-01

Raffinose segregation into sucrose crystals is experimentally determined along with the modifications of the quantitative sucrose growth morphology, which are in turn related to the different growth conditions. ( Craff, σ) morphodromes nicely represent the conflict between the supersaturation and the raffinose concentration in the solution on the growth morphology, while the overall segregation rate is nearly proportional to the linear overall crystal growth rate. Chernov and Burton-Prim-Slichter models, checked to fit our keff and ln(keff-1-1) coefficients as a function of the supersaturation and of the mean linear overall growth rate, do not allow to know whether the segregation occurs either by a process dominated by surface integration, or by additive transfer dominated by volume diffusion within the boundary layer. The distribution of segregated raffinose strictly depends on the { h k l} growth sectors and doped crystals contain deformed lattice zones, as it comes out from X-ray powder diagrams.

Optimizing alignment and growth of low-loss YAG single crystal fibers using laser heated pedestal growth technique.

PubMed

Bera, Subhabrata; Nie, Craig D; Soskind, Michael G; Harrington, James A

2017-12-10

The effect of misalignments of different optical components in the laser heated pedestal growth apparatus have been modeled using Zemax optical design software. By isolating the misalignments causing the non-uniformity in the melt zone, the alignment of the components was fine-tuned. Using this optimized alignment, low-loss YAG single crystal fibers of 120 μm diameter were grown, with total attenuation loss as low as 0.5 dB/m at 1064 nm.

3D numerical simulation of free surface shape during the crystal growth of floating zone (FZ) silicon

NASA Astrophysics Data System (ADS)

Han, Xue-Feng; Liu, Xin; Nakano, Satoshi; Harada, Hirofumi; Miyamura, Yoshiji; Kakimoto, Koichi

2018-02-01

In FZ growth processes, the stability of the free surface is important in the production of single crystal silicon with high quality. To investigate the shape of the free surface in the FZ silicon crystal growth, a 3D numerical model that included gas and liquid phases was developed. In this present study, 3D Young-Laplacian equations have been solved using the Volume of Fluid (VOF) Model. Using this new model, we predicted the 3D shape of the free surface in FZ silicon crystal growth. The effect of magnetic pressure on shape of free surface has been considered. In particular, the free surface of the eccentric growth model, which could not be previously solved using the 2D Young-Laplacian equations, was solved using the VOF model. The calculation results are validated by the experimental results.

TlBr purification and single crystal growth for the detector applications

NASA Astrophysics Data System (ADS)

Kozlov, Vasilij; Heikkilä, Mikko; Kostamo, Pasi; Lipsanen, Harri; Leskelä, Markku

2011-05-01

The combination of distillation, Bridgman-Stockbarger, hydrothermal recrystallisation and travelling molten zone (TMZ) methods were used for TlBr purification. Grown crystals were characterised by XRD rocking curve and FTIR spectroscopy methods, and by electrical measurements made from 200 to 300 K.

The nature of the mineral component of bone and the mechanism of calcification.

PubMed

Glimcher, M J

1987-01-01

From the physical chemical standpoint, the formation of a solid phase of Ca-P in bone represents a phase transformation, a process exemplified by the formation of ice from water. Considering the structural complexity and abundance of highly organized macromolecules in the cells and extracellular tissue spaces of mineralized tissues generally and in bone particularly, it is inconceivable that this phase transformation occurs by homogeneous nucleation, i.e., without the active participation of an organic component acting as a nucleator. This is almost surely true in biologic mineralization in general. Electron micrographs and low-angle neutron and X-ray diffraction studies clearly show that calcification of collagen fibrils occurs in an extremely intimate and highly organized fashion: initiation of crystal formation within the collagen fibrils in the hole zone region, with the long axes (c-axis) of the crystals aligned roughly parallel to the long axis of the fibril within which they are located. Crystals are initially formed in hole zone regions within individual fibrils separated by unmineralized regions. Calcification is initiated in spatially distinct nucleation sites. This indicates that such regions within a single, undirectional fibril represents independent sites for heterogeneous nucleation. Clearly, sites where mineralization is initiated in adjacent collagen fibrils are even further separated, emphasizing even more clearly that the process of progressive calcification of the collagen fibrils and therefore of the tissue is characterized principally by the presence of increasing numbers of independent nucleation sites within additional hole zone regions of the collagen fibrils. The increase in the mass of Ca-P apatite accrues principally by multiplication of more crystals, mostly by secondary nucleation from the crystals initially deposited in the hole zone region. Very little additional growth of the crystals occurs with time, the additional increase in mineral mass being principally the result of increase in the number of crystals (multiplication), not size of the crystals (crystal growth). The crystals within the collagen fibers grow in number and possibly in size to extend into the overlap zone of the collagen fibrils ("pores") so that all of the available space within the fibrils, which has possibly expanded in volume from its uncalcified level, is eventually occupied by the mineral crystals. It must be recognized that the calcification of separate tissue components and compartments (collagen, mitochondria, matrix vesicles) must be an independent physical chemical event.(ABSTRACT TRUNCATED AT 400 WORDS)

Float-zone crystal growth of CdGeAs 2 in microgravity: numerical simulation and experiment

NASA Astrophysics Data System (ADS)

Saghir, M. Z.; Labrie, D.; Ginovker, A.; Paton, B. E.; George, A. E.; Olson, K.; Simpson, A. M.

2000-01-01

Two CdGeAs 2 samples have been successfully grown under microgravity on SPACEHAB-SH04 during the STS-77 Space Shuttle Endeavour mission. One polycrystalline and one single crystal CdGeAs 2 feed rods with 9 mm diameter were processed by the float-zone method. An eutectic salt of LiCl and KCl was used as an encapsulant to suppress Cd and As evaporation from the melt. Numerical modeling of the float zone shows that salt encapsulation plays an important role in reducing Marangoni convection. The interface between the salt and CdGeAs 2 was shown not to deform in the float zone due to the weak capillary pressure.

Radiative heat transport during the vertical Bridgman growth of oxide single crystals: slabs versus cylinders

NASA Astrophysics Data System (ADS)

Virozub, Alexander; Brandon, Simon

1998-10-01

Internal radiative heat transport in oxide crystals during their growth via the vertical Bridgman technique is known to promote severely deflected melt/crystal interface shapes. These highly curved interfaces are likely to encourage unwanted phenomena such as inhomogeneous distribution of impurities in the solidified crystalline material. Past computational analyses of oxide growth systems have mostly been confined to cylindrical geometries. In this letter a two-dimensional finite-element model, describing the growth of slab-shaped oxide crystals via the vertical Bridgman technique, is presented; internal radiative heat transport through the transparent crystalline phase is accounted for in the formulation. Comparison with calculations of cylindrical-shaped crystal growth systems shows a strong dependence of thermal fields and of melt/crystal interface shapes on the crystal geometry. Specifically, the interface position is strongly shifted toward the hot zone and its curvature dramatically increases in slab-shaped systems compared to what is observed in cylindrical geometries. This significant qualitative difference in interface shapes is shown to be linked to large quantitative differences in values of the viewing angle between the hot melt/crystal interface and the cold part of the crucible.

III-V semiconductor solid solution single crystal growth

NASA Technical Reports Server (NTRS)

Gertner, E. R.

1982-01-01

The feasibility and desirability of space growth of bulk IR semiconductor crystals for use as substrates for epitaxial IR detector material were researched. A III-V ternary compound (GaInSb) and a II-VI binary compound were considered. Vapor epitaxy and quaternary epitaxy techniques were found to be sufficient to permit the use of ground based binary III-V crystals for all major device applications. Float zoning of CdTe was found to be a potentially successful approach to obtaining high quality substrate material, but further experiments were required.

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Pusey, M.; Snell, E.; Judge, R.; Chayen, N.; Boggon, T.

2000-01-01

The molecular structure of biological macromolecules is important in understanding how these molecules work and has direct application to rational drug design for new medicines and for the improvement and development of industrial enzymes. In order to obtain the molecular structure, large, well formed, single macromolecule crystals are required. The growth of macromolecule crystals is a difficult task and is often hampered on the ground by fluid flows that result from the interaction of gravity with the crystal growth process. One such effect is the bulk movement of the crystal through the fluid due to sedimentation. A second is buoyancy driven convection close to the crystal surface. On the ground the crystallization process itself induces both of these flows. Buoyancy driven convection results from density differences between the bulk solution and fluid close to the crystal surface which has been depleted of macromolecules due to crystal growth. Schlieren photograph of a growing lysozyme crystal illustrating a 'growth plume' resulting from buoyancy driven convection. Both sedimentation and buoyancy driven convection have a negative effect on crystal growth and microgravity is seen as a way to both greatly reduce sedimentation and provide greater stability for 'depletion zones' around growing crystals. Some current crystal growth hardware however such as those based on a vapor diffusion techniques, may also be introducing unwanted Marangoni convection which becomes more pronounced in microgravity. Negative effects of g-jitter on crystal growth have also been observed. To study the magnitude of fluid flows around growing crystals we have attached a number of different fluorescent probes to lysozyme molecules. At low concentrations, less than 40% of the total protein, the probes do not appear to effect the crystal growth process. By using these probes we expect to determine not only the effect of induced flows due to crystal growth hardware design but also hope to optimize crystallization hardware so that destructive flows are minimized both on the ground and in microgravity.

Growth of 2 Inch Eu-doped SrI2 single crystals for scintillator applications

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Shoji, Yasuhiro; Yokota, Yuui; Kurosawa, Shunsuke; Hayasaka, Shoki; Chani, Valery I.; Ito, Tomoki; Kamada, Kei; Ohashi, Yuji; Kochurikhin, Vladimir

2016-10-01

A vertical Bridgman (VB) crystal growth process was established using modified micro-pulling-down (μ-PD) crystal growth system with a removable chamber that was developed for the growth of deliquescent halide single crystals because conventional μ-PD method does not allow growth of large bulk single crystals. Eu:SrI2 crystals were grown from the melt of (Sr0.98Eu0.02)I2 composition using carbon crucibles. Undoped μ-PD SrI2 crystals were used as seeds that were affixed to the bottom of the crucible. All the preparations preceding the growths and the hot zone assembling were performed in a glove box with Ar gas. Then the removable chamber was taken out of the glove box, attached to the μ-PD system, connected with a Turbo Molecular pump, and evacuated down to 10-4 Pa at 300 °C. After the baking procedure, high purity Ar gas (6N) was injected into the chamber. The crucible was heated by a high frequency induction coil up to the melting point of Eu:SrI2. After melting the starting materials, the crucible was displaced in downward direction for the crystal growth and then cooled down to room temperature. Thus, 2 in. and crack-free Eu:SrI2 bulk crystals were produced. The crystals had high transparency and did not contain any visible inclusions. The crystals were cut and polished in the glove box and then sealed in an aluminum container with an optical window for characterization. The details of the crystal growth are discussed.

Deducing Water Concentrations in the Parent Magma of Cumulate Clinopyroxene and Olivine: Implications for a Hydrous Parent Melt of a Primitive Deccan Lava

NASA Astrophysics Data System (ADS)

Seaman, S. J.

2017-12-01

Water concentrations of clinopyroxene megacrysts in the Powai ankaramite flow, located near Mumbai, Deccan province, India, indicate that the parent magma of the flow hosted at least 4.3 wt.% water, an unusually high water concentration for a continental flood basalt magma. The Powai flow hosts clinopyroxene and olivine phenocrysts. Chatterjee and Sheth (2015) showed that phenocrysts in the flow were part of a cumulate layer intruded by basaltic melt at 6 kb and 1230oC, so the phenocrysts record characteristics of the cumulate parent melt. Clinopyroxene phenocrysts are oscillatorily zoned in water, Mg, Fe, and Ca concentrations, and have concentric bands 100-200 microns thick of 10-20 micron diameter melt inclusions. Olivine phenocrysts host only larger isolated melt inclusions. Zones in the cpx phenocrysts where melt inclusion-rich concentric bands occur have higher concentrations of water than inclusion-free zones. Water concentrations of cpx were used to calculate water concentrations in the melt from which the crystals formed using partition coefficients of Hauri et al. (2004). Water concentrations in the parent magma were between 4.3 and 8.2 wt. % based on water concentrations in cpx. Both Mg and Fe are relatively depleted in the water- and melt inclusion-rich zones in cpx, and Ca is enriched in these zones. Oscillatory zoning in cpx may be a result of repeated growth of cpx in water- richer and water-poorer boundary layers where water lowered melt viscosity and enhanced diffusion and crystal growth rates. Water-enhanced growth rates may have resulted in capture of melt inclusions preserved in water-rich cpx zones. Melt inclusions in olivine phenocrysts preserve lower water concentrations ( 1.2 wt. %) than those indicated by water concentration in cpx phenocrysts. This disparity may be evidence of water loss from melt inclusions in olivine (Gaetani et al., 2009) or may indicate that cpx and ol crystals did not crystallize from the same parent at the same time.

Changes in copper sulfate crystal habit during cooling crystallization

NASA Astrophysics Data System (ADS)

Giulietti, M.; Seckler, M. M.; Derenzo, S.; Valarelli, J. V.

1996-09-01

The morphology of technical grade copper(II) sulfate pentahydrate crystals produced from batch cooling experiments in the temperature range of 70 to 30°C is described and correlated with the process conditions. A slow linear cooling rate (batch time of 90 min) predominantly caused the appearance of well-formed crystals. Exponential cooling (120 min) resulted in the additional formation of agglomerates and twins. The presence of seeds for both cooling modes led to round crystals, agglomerates and twins. Fast linear cooling (15 min) gave rise to a mixture of the former types. Broken crystals and adhering fragments were often found. Growth zoning was pronounced in seeded and linear cooling experiments. Fluid inclusions were always found and were more pronounced for larger particles. The occurrence of twinning, zoning and fluid inclusions was qualitatively explained in terms of fundamental principles.

Crystal growth and characterization of Ce:Gd3(Ga,Al)5O12 single crystal using floating zone method in different O2 partial pressure

NASA Astrophysics Data System (ADS)

Yoshikawa, Akira; Fujimoto, Yutaka; Yamaji, Akihiro; Kurosawa, Shunsuke; Pejchal, Jan; Sugiyama, Makoto; Wakahara, Shingo; Futami, Yoshisuke; Yokota, Yuui; Kamada, Kei; Yubuta, Kunio; Shishido, Toetsu; Nikl, Martin

2013-09-01

Multicomponent garnet Ce:Gd3(Ga,Al)5O12 (Ce:GAGG) single crystals show very high light yield with reasonably fast scintillation response. Therefore, they can be promising scintillators for gamma-ray detection. However, in the decay curve a very slow component does exist. Therefore, it is necessary to optimize further the crystal growth technology of Ce:GAGG. In this study, Ce:GAGG single crystals were grown by the floating zone (FZ) method under atmospheres of various compositions such as Ar 100%, Ar 80% + O2 20%, Ar 60% + O2 40% and O2 100%. Radioluminescence spectra are dominated by the band at about 540 nm due to Ce3+ 5d1-4f transition. The Ce:GAGG single crystal grown under Ar atmosphere shows an intense slower decay component. It can be related to the processes of the delayed radiative recombination and thermally induced ionization of 5d1 level of Ce3+ center possibly further affected by oxygen vacancies. This slower decay process is significantly suppressed in the samples grown under the O2 containing atmosphere.

Ultra-fast scintillation properties of β-Ga2O3 single crystals grown by Floating Zone method

NASA Astrophysics Data System (ADS)

He, Nuotian; Tang, Huili; Liu, Bo; Zhu, Zhichao; Li, Qiu; Guo, Chao; Gu, Mu; Xu, Jun; Liu, Jinliang; Xu, Mengxuan; Chen, Liang; Ouyang, Xiaoping

2018-04-01

In this investigation, β-Ga2O3 single crystals were grown by the Floating Zone method. At room temperature, the X-ray excited emission spectrum includes ultraviolet and blue emission bands. The scintillation light output is comparable to the commercial BGO scintillator. The scintillation decay times are composed of the dominant ultra-fast component of 0.368 ns and a small amount of slightly slow components of 8.2 and 182 ns. Such fast component is superior to most commercial inorganic scintillators. In contrast to most semiconductor crystals prepared by solution method such as ZnO, β-Ga2O3 single crystals can be grown by traditional melt-growth method. Thus we can easily obtain large bulk crystals and mass production.

Titanium zoning and diffusion chronometry reveal dynamic and late-stage quartz growth in the Youngest Toba Tuff, Indonesia

NASA Astrophysics Data System (ADS)

Tierney, C. R.; Reid, M. R.; Burns, D. H.; Costa Rodriguez, F.; Chesner, C. A.

2017-12-01

The enormous 74 ka Youngest Toba Tuff (YTT) ejected 2800 km3 of compositionally zoned (68-77 wt.% SiO2) ignimbrite and co-ignimbrite ash. Titanium zoning within YTT quartz records a dynamic growth history, and sometimes concludes with a final growth stage under different conditions. We investigated the timescales of quartz growth using diffusion chronometry, and determined whether the last stage of crystallization was the result of a discrete and chamber-wide magmatic event. This work offers insight into the dynamics and timescales of storage and remobilization of voluminous silicic magmas - an important consideration for hazards assessment. High-resolution (1 µm steps) hyperspectral CL was mapped from 5-20 quartz crystals from each of five pumices spanning the YTT compositional spectrum. CL intensity was calibrated to Ti concentration via EPMA, and numerically modeled time-dependent diffusional relaxation curves where fit to concentration profiles across zone boundaries. CL-bright/high-Ti rims are found in quartz from all samples, but become less common and have lower Ti concentrations with increasing host pumice silica content (e.g., 70 ppm vs 50 ppm). Some large crystals contain distinct CL-bright interior zones with similar Ti concentration to the rims. Onset of growth of CL-bright rims commenced between 15 and 100 years before eruption, and interior bands between 30 and 1500 years. Neither rim nor interior ages correlate significantly with host pumice silica. Rim growth on quartz evidently occurred closer to eruption than a previous estimate of several decades to centuries for quartz from a single YTT pumice (Matthews et al., 2012). The similar timing for the onset of high-Ti quartz rim growth across all samples suggests a marked and temporally discrete magmatic event in the years to decades prior to eruption and may be recording the chamber-wide influence of magmatic recharge or remobilization. High-Ti interior zones likely record older recharge events that did not lead to eruption. The lower abundance and lower Ti concentrations of CL-bright rims in high-silica pumices indicates that the agent of recharge/remobilization may not have chemically impacted the more evolved parts of the system appreciably, potentially due to thermal buffering by the near-eutectoid composition of the magmatic system.

A modified Chang Brown model for the determination of the dopant distribution in a Bridgman Stockbarger semiconductor crystal growth system

NASA Astrophysics Data System (ADS)

Balint, A. M.; Mihailovici, M. M.; Bãltean, D. G.; Balint, St.

2001-08-01

In this paper, we start from the Chang-Brown model which allows computation of flow, temperature and dopant concentration in a vertical Bridgman-Stockbarger semiconductor growth system. The modifications made by us concern the melt/solid interface. Namely, we assume that the phase transition does not take place on a flat mathematical surface, but in a thin region (the so-called precrystallization-zone), masking the crystal, where both phases, liquid and solid, co-exist. We deduce for this zone new effective equations which govern flow, heat and dopant transport and make the coupling of these equations with those governing the same phenomena in the pure melt. We compute flow, temperature and dopant concentration for crystal and melt with thermophysical properties similar to gallium-doped germanium using the modified Chang-Brown model and compare the results to those obtained using the Chang-Brown model.

Numerical analysis of melt-solid interface shapes and growth rates of gallium antimonide in a single-zone vertical Bridgman furnace

NASA Astrophysics Data System (ADS)

Dutta, P. S.; Bhat, H. L.; Kumar, Vikram

1995-09-01

Numerical analysis has been carried out to determine the deviation of the growth rate from the ampoule lowering rate and the shape of the isotherms during the growth of gallium antimonide using the vertical Bridgman technique in a single-zone furnace. Electrical analogues have been used to model the thermal behaviour of the growth system. The standard circuit analysis technique has been used to calculate the temperature distribution in the growing crystal under various growth conditions. The effects of furnace temperature gradient near the melt-solid interface, the ampoule lowering rate, the ampoule geometry, the thermal conductivity of the melt, the mode of heat extraction from the tip of the ampoule and the extent of lateral heat loss from the side walls of the ampoule on the shape of isotherms in the crystal have been evaluated. The theoretical results presented here agree well with our previously obtained experimental results.

Genetic implications of the trace element distribution pattern in the upper knox carbonate rocks, copper ridge district, East Tennessee

NASA Astrophysics Data System (ADS)

Churnet, Habte G.; Misra, Kula C.

1981-11-01

The Lower Ordovician, Upper Knox Group rocks (the Kingsport and Mascot formations) in the Copper Ridge district consist predominantly of fine-grained dolostones, medium and coarser grained dolostones, and limestones. Dolomite crystals of medium and coarser grained dolostones show up to eight cathodoluminescent zones of variable width and intensity. Electron microprobe analyses indicate that the zoning is related to variation in Fe/Mn ratios, the brighter luminescent zones corresponding to lower ratios. Superposed on this growth zoning is a compositional zoning characterized by a general increase in Fe from core to rim of individual dolomite crystals. Field and petrographic studies (Churnet, 1979; Churnet et al., 1981) indicate that the fine-grained dolostones formed in supratidal to upper intratidal environments, whereas the precursor lime muds of the limestones as well as of the medium and coarser grained dolostones formed in shallow subtidal to lower intertidal environments. The large areal extent of the dolostones must have required a regionally abundant source of Mg such as marine water. Yet, both limestones and dolostones have low Na and Sr contents suggestive of their formation in solutions more dilute than normal marine water. It is proposed that the fine-grained dolostones formed by aggradation of initially very fine-grained dolostones in presence of fresh water, and that the limestones stabilized and the medium and coarser grained dolostones formed in environments of mixed marine and fresh waters. Considered in the light of ordering of partition coefficients, such a mixing model can account for the observed correlation pattern of trace elements (especially, SMn and SrFe) as well as the Fe distribution in the zoned dolomite crystals. Variation of the partition coefficient of Mn due to fluctuations in the relative proportions of fresh and marine waters in the diagenetic solution may explain the different Fe/Mn ratios observed in the growth zones (luminescence bands) of zoned dolomite crystals.

Disequilibrium growth of olivine in mafic magmas revealed by phosphorus zoning patterns of olivine from mafic-ultramafic intrusions

NASA Astrophysics Data System (ADS)

Xing, Chang-Ming; Wang, Christina Yan; Tan, Wei

2017-12-01

Olivine from mafic-ultramafic intrusions rarely displays growth zoning in major and some minor elements, such as Fe, Mg and Ni, due to fast diffusion of these elements at high temperatures. These elements in olivine are thus not useful in deciphering magma chamber processes, such as magma convection, multiple injection and mixing. High-resolution X-ray elemental intensity mapping reveals distinct P zoning patterns of olivine from two mafic-ultramafic intrusions in SW China. Polyhedral olivine grains from lherzolite and dunite of the Abulangdang intrusion show P-rich dendrites similar to those observed in volcanic rocks. Rounded olivine grains from net-textured Fe-Ti oxide ores of the Baima layered intrusion have irregular P-rich patches/bands crosscut and interlocked by P-poor olivine domains. P-rich patches/bands contain 250 to 612 ppm P, much higher than P-poor olivine domains with 123 to 230 ppm P. In electron backscattered diffraction (EBSD) maps, P-rich patches/bands within a single olivine grain have the same crystallographic orientation, indicating that they were remnants of the same crystal. Thus, both P-rich patches/bands and P-poor olivine domains in the same grain show a disequilibrium texture and clearly record two-stage growth. The P-rich patches/bands are likely the remnants of a polyhedral olivine crystal that formed in the first stage, whereas the P-poor olivine domains containing rounded Ti-rich magnetite and Fe-rich melt inclusions may have formed from an Fe-rich ambient melt in the second stage. The complex P zoning of olivine can be attributed to the dissolution of early polyhedral olivine and re-precipitation from the Fe-rich ambient melt. The early polyhedral olivine was in chemical disequilibrium with the ambient melt that may have been developed by silicate liquid immiscibility in a crystal mush. Our study implies that olivine crystals in igneous cumulates with an equilibrium appearance may have experienced disequilibrium growth processes during slow cooling. Therefore, the crystallization sequence of mafic magmas based on textural relationships should be treated with caution.

Orthopyroxene oikocrysts in the MG1 chromitite layer of the Bushveld Complex: implications for cumulate formation and recrystallisation

NASA Astrophysics Data System (ADS)

Kaufmann, Felix E. D.; Vukmanovic, Zoja; Holness, Marian B.; Hecht, Lutz

2018-02-01

Two typical mineral textures of the MG 1 chromitite of the Bushveld Complex, South Africa, were observed; one characterised by abundant orthopyroxene oikocrysts, and the other by coarse-grained granular chromitite with only minor amounts of interstitial material. Oikocrysts form elongate clusters of several crystals aligned parallel to the layering, and typically have subhedral, almost chromite-free, core zones containing remnants of olivine. The core zones are surrounded by poikilitic aureoles overgrowing euhedral to subhedral chromite chadacrysts. Chromite grains show no preferred crystal orientation, whereas orthopyroxene grains forming clusters commonly share the same crystallographic orientation. Oikocryst core zones have lower Mg# and higher concentrations of incompatible trace elements compared to their poikilitic aureoles. Core zones are relatively enriched in REE compared to a postulated parental magma (B1) and did not crystallise in equilibrium with the surrounding minerals, whereas the composition of the poikilitic orthopyroxene is consistent with growth from the B1 magma. These observations cannot be explained by the classic cumulus and post-cumulus models of oikocryst formation. Instead, we suggest that the oikocryst core zones in the MG1 chromitite layer formed by peritectic replacement of olivine primocrysts by reaction with an upwards-percolating melt enriched in incompatible trace elements. Poikilitic overgrowth on oikocryst core zones occurred in equilibrium with a basaltic melt of B1 composition near the magma-crystal mush interface. Finally, adcumulus crystallisation followed by grain growth resulted in the surrounding granular chromitite.

Growth Angle - a Microscopic View

NASA Technical Reports Server (NTRS)

Mazurak, K.; Volz, M. P.; Croll, A.

2017-01-01

The growth angle that is formed between the side of the growing crystal and the melt meniscus is an important parameter in the detached Bridgman crystal growth method, where it determines the extent of the crystal-crucible wall gap, and in the Czochralski and float zone methods, where it influences the size and stability of the crystals. The growth angle is a non-equilibrium parameter, defined for the crystal growth process only. For a melt-crystal interface translating towards the crystal (melting), there is no specific angle defined between the melt and the sidewall of the solid. In this case, the corner at the triple line becomes rounded, and the angle between the sidewall and the incipience of meniscus can take a number of values, depending on the position of the triple line. In this work, a microscopic model is developed in which the fluid interacts with the solid surface through long range van der Waals or Casimir dispersive forces. This growth angle model is applied to Si and Ge and compared with the macroscopic approach of Herring. In the limit of a rounded corner with a large radius of curvature, the wetting of the melt on the crystal is defined by the contact angle. The proposed microscopic approach addresses the interesting issue of the transition from a contact angle to a growth angle as the radius of curvature decreases.

Development of the vertical Bridgman technique for 6-inch diameter c-axis sapphire growth supported by numerical simulation

NASA Astrophysics Data System (ADS)

Miyagawa, Chihiro; Kobayashi, Takumi; Taishi, Toshinori; Hoshikawa, Keigo

2014-09-01

Based on the growth of 3-inch diameter c-axis sapphire using the vertical Bridgman (VB) technique, numerical simulations were made and used to guide the growth of a 6-inch diameter sapphire. A 2D model of the VB hot-zone was constructed, the seeding interface shape of the 3-inch diameter sapphire as revealed by green laser scattering was estimated numerically, and the temperature distributions of two VB hot-zone models designed for 6-inch diameter sapphire growth were numerically simulated to achieve the optimal growth of large crystals. The hot-zone model with one heater was selected and prepared, and 6-inch diameter c-axis sapphire boules were actually grown, as predicted by the numerical results.

A low temperature furnace for solution crystal growth on the International Space Station

NASA Astrophysics Data System (ADS)

Baç, Nurcan; Harpster, Joseph; Maston, Robert A.; Sacco, Albert

2000-01-01

The Zeolite Crystal Growth Furnace Unit (ZCG-FU) is the first module in an integrated payload designed for low temperature crystal growth in solutions on the International Space Station (ISS). This payload is scheduled to fly on the ISS flight 7A.1 in an EXPRESS rack. Its name originated from early shuttle flight experiments limited to the growth of zeolite crystals but has since grown to include other materials of significant commercial interest using the solution method of crystal growth. Zeolites, ferroelectrics, piezeoelectrics and silver halides are some of the materials considered. The ZCG-FU experiment consists of a furnace unit and its electronic control system, and mechanically complex, crystal growth autoclaves suitable for use with a particular furnace and solution. The ZCG facility is being designed to grow into four independent furnaces controlled by IZECS (Improved Zeolite Electronic Control System). IZECS provides monitoring of critical parameters, data logging, safety monitoring, air-to-ground control and operator interfacing. It is suitable for controlling the four furnaces either individually or all at one time. It also contains the power management solid-state drivers and switches for the ZCG-FU furnace. The furnace contains 19 tubes operating at three different temperature zones. .

Adaptive control of interface by temperature and interface profile feedback in transparent multi-zone crystal growth furnace

NASA Technical Reports Server (NTRS)

Batur, Celal

1991-01-01

The objective of this research is to control the dynamics of multizone programmable crystal growth furnaces. Due to the inevitable heat exchange among different heating zones and the transient nature of the process, the dynamics of multizone furnaces is time varying, distributed, and therefore complex in nature. Electrical power to heating zones and the translational speed of the ampoule are employed as inputs to control the dynamics. Structural properties of the crystal is the ultimate aim of this adaptive control system. These properties can be monitored in different ways. Following an order of complexity, these may include: (1) on line measurement of the material optical properties such as the refractive index of crystal; (2) on line x-ray imaging of the interface topology; (3) on line optical quantification of the interface profile such as the determination of concavity or convexity of the interface shape; and (4) on line temperature measurement at points closest to the material such as measurements of the ampoule's outside and inside surface temperatures. The research performed makes use of the temperature and optical measurements, specified in (3) and (4) as the outputs of furnace dynamics. However, if the instrumentation is available, the proposed control methodology can be extended to the measurements listed in (1) and (2).

Large area Czochralski silicon

NASA Technical Reports Server (NTRS)

Rea, S. N.; Gleim, P. S.

1977-01-01

The overall cost effectiveness of the Czochralski process for producing large-area silicon was determined. The feasibility of growing several 12 cm diameter crystals sequentially at 12 cm/h during a furnace run and the subsequent slicing of the ingot using a multiblade slurry saw were investigated. The goal of the wafering process was a slice thickness of 0.25 mm with minimal kerf. A slice + kerf of 0.56 mm was achieved on 12 cm crystal using both 400 grit B4C and SiC abrasive slurries. Crystal growth experiments were performed at 12 cm diameter in a commercially available puller with both 10 and 12 kg melts. Several modifications to the puller hoz zone were required to achieve stable crystal growth over the entire crystal length and to prevent crystallinity loss a few centimeters down the crystal. The maximum practical growth rate for 12 cm crystal in this puller design was 10 cm/h, with 12 to 14 cm/h being the absolute maximum range at which melt freeze occurred.

Bulk Group-III Nitride Crystal Growth in Supercritical Ammonia-Sodium Solutions

NASA Astrophysics Data System (ADS)

Griffiths, Steven Herbert

Gallium nitride (GaN) and its alloys with indium nitride (InGaN) and aluminum nitride (AlGaN), collectively referred to as Group-III Nitride semiconductors, have enabled white solid-state lighting (SSL) sources and power electronic devices. While these technologies have already made a lasting, positive impact on society, improvements in design and efficiency are anticipated by shifting from heteroepitaxial growth on foreign substrates (such as sapphire, Si, SiC, etc.) to homoepitaxial growth on native, bulk GaN substrates. Bulk GaN has not supplanted foreign substrate materials due to the extreme conditions required to achieve a stoichiometric GaN melt (temperatures and pressures in excess of 2200°C and 6 GPa, respectively). The only method used to produce bulk GaN on an industrial scale is hydride vapor phase epitaxy (HVPE), but the high cost of gaseous precursors and relatively poor crystal quality have limited the adoption of this technology. A solution growth technique known as the ammonothermal method has attracted interest from academia and industry alike for its ability to produce bulk GaN boules of exceedingly high crystal quality. The ammonothermal method employs supercritical ammonia (NH3) solutions to dissolve, transport, and crystallize GaN. However, ammonothermal growth pressures are still relatively high (˜200 MPa), which has thus far prevented the acquisition of fundamental crystal growth knowledge needed to efficiently (i.e. through data-driven approaches) advance the field. This dissertation focused on addressing the gaps in the literature through two studies employing in situ fluid temperature analysis. The first study focused on identifying the solubility of GaN in supercritical NH3-Na solutions. The design and utilization of in situ and ex situ monitoring equipment enabled the first reports of the two-phase nature of supercritical NH3-Na solutions, and of Ga-alloying of Ni-containing autoclave components. The effects of these error sources on the gravimetric determination of GaN solubility were explored in detail. The second study was aimed at correlating autoclave dissolution and growth zone fluid temperatures with bulk GaN crystal growth kinetics, crystal quality, and impurity incorporation. The insights resulting from this analysis include the identification of the barrier between mass transport and surface integration-limited GaN growth regimes, GaN crystal shape evolution with fluid temperature, the sensitivity of (0001)-orientation crystal quality with fluid temperature, and impurity-specific incorporation activated from the dissolution and growth zones of the autoclave. The results of the aforementioned studies motivated a paradigm-shift in ammonothermal growth. To address this need, a fundamentally different crystal growth approach involving isothermal solutions and tailor-made Group-III alloy source materials was developed/demonstrated. This growth method enabled impurity incorporation reduction compared to traditional ammonothermal GaN growth, and the realization of bulk, ternary Group-III Nitride crystals.

Interface shapes during vertical Bridgman growth of (Pb, Sn)Te crystals

NASA Technical Reports Server (NTRS)

Huang, YU; Debnam, William J.; Fripp, Archibald L.

1990-01-01

Melt-solid interfaces obtained during vertical Bridgman growth of (Pb, Sn)Te crystals were investigated with a quenching technique. The shapes of these interfaces, revealed by etching longitudinally cut sections, were correlated with the composition variations determined by EMPA. These experiments demonstrated that the interface shape can be changed from concave to convex by moving its location from the edge of the cold zone into the hot zone. The metallography and microsegregation near the melt-solid interface were analyzed in detail. A sharp change in composition above the interface indicated the existence of a diffusion boundary layer 40-90 microns thick. This small diffusion boundary layer is consistent with strong convective mixing in the (Pb, Sn)Te melt.

A numerical study of steady crystal growth in a vertical Bridgman device

NASA Astrophysics Data System (ADS)

Jalics, Miklos Kalman

Electronics based on semiconductors creates an enormous demand for high quality semiconductor single crystals. The vertical Bridgman device is commonly used for growing single crystals for a variety of materials such as GaAs, InP and HgCdTe. A mathematical model is presented for steady crystal growth under conditions where crystal growth is determined strictly by heat transfer. The ends of the ampoule are chosen far away from the insulation zone to allow for steady growth. A numerical solution is sought for this mathematical model. The equations are transformed into a rectangular geometry and appropriate finite difference techniques are applied on the transformed equations. Newton's method solves the nonlinear problem. To improve efficiency GMRES with preconditioning is used to compute the Newton iterates. The numerical results are used to compare with two current asymptotic theories that assume small Biot numbers. Results indicate that one of the asymptotic theories is accurate for even moderate Biot numbers.

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge Si crystal growth experiments are planned to be conducted in the Low 1-x x Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. 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 crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Recycling and recharge processes at the Hasandağ Stratovolcano, Central Anatolia: Insights on magma chamber systematics from plagioclase textures and zoning patterns

NASA Astrophysics Data System (ADS)

Gall, H. D.; Cipar, J. H.; Crispin, K. L.; Kürkçüoğlu, B.; Furman, T.

2017-12-01

We elucidate crystal recycling and magma recharge processes at Hasandağ by investigating compositional zoning patterns and textural variation in plagioclase crystals from Quaternary basaltic andesite through dacite lavas. Previous work on Hasandağ intermediate compositions identified thermochemical disequilibrium features and showed abundant evidence for magma mixing1,2. We expand on this work through detailed micro-texture and mineral diffusion analysis to explore the mechanisms and timescales of crystal transport and mixing processes. Thermobarometric calculations constrain the plumbing system to 1.2-2 kbar and 850-950°C, corresponding to a felsic magma chamber at 4.5 km. Electron microprobe results reveal plagioclase phenocrysts from all lava types have common core (An33-46) and rim (An36-64) compositions, with groundmass laths (An57-67) resembling the phenocryst rims. Low An cores are ubiquitous, regardless of bulk rock chemistry, and suggest a consistent composition within the magma reservoir prior to high An rim growth. High An rims are regularly enriched in Mg, Fe, Ti and Sr, which we attribute to mafic recharge and magma mixing. We assess mixing timescales by inverse diffusion modeling of Mg profiles across the core-rim boundaries. Initial results suggest mixing to eruption processes occur on the order of days to months. Heterogeneous calculated timescales within thin sections indicate crystal populations with different growth histories. Crystals often display prominent sieve-textured zones just inside the rim, as well as other disequilibrium features such as oscillatory zoning or resorbed and patchy-zoned cores. We interpret these textures to indicate mobilization of a homogeneous dacitic reservoir with abundant An35 plagioclase crystals by frequent injection of mafic magma. Variability in observed textures and calculated timescales manifests during defrosting of a highly crystalline felsic mush, through different degrees of magma mixing. This process results in distinct crystal populations, some of which record punctuated ascent and storage, while others are erupted rapidly after the influx of new magma. Aydar, E., & Gourgaud, A. (1998). J. Volcanol. Geotherm. Res., 85(1), 129-152. Ustunisik, G., & Kilinc, A. (2011). Lithos, 125(3), 984-993.

Nucleation kinetics, crystal growth and optical studies on lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

Chandran, Senthilkumar; Paulraj, Rajesh; Ramasamy, P.

2017-06-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution technique at 40 °C. The nucleation parameters such as critical radius, interfacial tension, and critical free energy change have been evaluated using the experimental data. The solubility and the nucleation curve of the crystal at different temperatures have been analyzed. The crystal has a positive temperature coefficient of solubility. The metastable zone width and induction period have been determined for the aqueous solution growth of lithium hydrogen oxalate monohydrate. The UV-vis-NIR spectrum showed this crystal has high transparency. The photoconductivity studies indicate lithium hydrogen oxalate monohydrate has positive photoconductivity behaviour. The low etch pit density observed on (0 0 1) crystal surface and the high resolution x-ray difraction analysis indicate the good quality of the grown crystals

Crystal growth and characterization of undoped and Dy-doped TlPb2Br5 for infrared lasers and nuclear radiation detection

NASA Astrophysics Data System (ADS)

Hömmerich, U.; Brown, E.; Kabir, A.; Hart, D.; Trivedi, S. B.; Jin, F.; Chen, H.

2017-12-01

We report results of the crystal growth and characterization of undoped and Dy-doped TlPb2Br5 for applications in infrared (IR) lasers and nuclear radiation detection. TlPb2Br5 (TPB) was synthesized from commercial starting materials of PbBr2 and TlBr and further purified through a combination of zone-refinement and directional solidification. For doping experiments, 2 wt% of DyBr3 was added to the purified TPB material. Crystal growth of TPB and Dy: TPB was carried out in a two-zone tube furnace by a vertical Bridgman method. Following optical excitation at ∼1.36 μm, the Dy: TPB crystal exhibited efficient mid-IR emission bands centered at 2.87 μm and 4.35 μm with room-temperature lifetimes of 9.5 ms and 5.2 ms, respectively. The peak emission cross-sections were determined to be ∼0.8 × 10-20 cm2 and ∼0.5 × 10-20 cm2, respectively, which makes Dy: TPB a promising candidate for mid-IR laser applications. Besides its potential as a solid-state laser host, an undoped TPB crystal was also tested for gamma-ray detection. Using Cs-137 and Am-241 sources resulted in energy resolutions for gamma-rays as good as 1-2% (FWHM) at room-temperature under non-optimized conditions.

The effect factors of potassium dihydrogen phosphate crystallization in aqueous solution

NASA Astrophysics Data System (ADS)

Zhou, Cun; Sun, Fei; Liu, Xuzhao

2017-01-01

The effects of cooling rate and pH on the potassium dihydrogen phosphate crystallization process were studied by means of batch crystallization process. The experiment shows that with the increase of cooling rate, the metastable zone width increase and the induction period decrease. When the pH is 3.0, the metastable zone width and induction period are both the minimum, while the crystallization rate is the highest. The crystallization products were characterized by scanning election microscope. Potassium Dihydrogen Phosphate (KDP) is a kind of excellent nonlinear optical materials, and belongs to tetragonal system, and ideal shape is aggregate of tetragonal prism and tetragonal dipyramid, the (100) cone is alternating accumulation by double positive ions and double negative ions [1-4]. The crystals of aqueous solution method to grow have large electro-optical nonlinear coefficient and high loser-damaged threshold, and it is the only nonlinear optical crystal could be used in inertial confinement fusion (ICF), KDP crystals are the ideal system to study the native defects of complex oxide insulating material [5-7]. With the development of photovoltaic technology, KDP crystals growth and performance have become a research focus worldwide [8, 9]. The merits of the crystallization process directly affect the quality of KDP products, so the study of the effect of crystallization conditions has an important significance on industrial production. This paper studied the change rule of metastable zone width, induction period, crystallization rate and particle size distribution in crystal process, and discussed the technical condition of KDP crystallization.

Surface-structural Control on Minor Element Zoning and Growth Mechanism in Synthetic Magmatic Clinopyroxene

NASA Astrophysics Data System (ADS)

Paquette, J.; Deakin, M.; Baker, D. R.

2006-12-01

Because in situ observations of actively growing surfaces are technically impractical, our understanding of crystal growth mechanisms at hydrothermal and magmatic conditions lags behind that of minerals that can be grown from aqueous solutions at or near room temperature. Growing silicate minerals from hydrous synthetic carbonate melts offers the opportunity to relate directly minor element incorporation to their surface microtopography. Natural hydrothermal diopside was used to seed experiments in which synthetic clinopyroxene crystals were grown at 800 degrees C and 10 kbars for 24 hours, from alkaline melts modelled after the lavas of the Tanzanian volcano Oldoinyo Lengai. The melts were prepared from Na2CO3, K2CO3, CaCO3, MgCO3 and Fe3O4 reagents. One run was anhydrous and the others contained either 2.5 or 5 wt. % H2O. Euhedral tabular crystals ranging in size from 100 to 300 ìm across were found in all three runs, hand-picked and freed from their carbonate matrix by overnight immersion in dilute acetic acid. The crystals consist of \\{110\\} prism, \\{100\\} and \\{001\\} pinacoids and a \\{111\\} dipyramid. AFM images resolved a distinct surface microtopography on each form: arrays of broad macrosteps on \\{100\\}, lens- shaped islands on \\{001\\} facets and striated fiber-like crystallites on \\{110\\}. EMP analyses of polished grain mounts show that compositional zoning of Na and Fe occurs not only among non-equivalent growth sectors but also within single \\{100\\} sectors. Electron microprobe maps of sequentially polished sections indicate that zoning within \\{100\\} sectors reflects differential uptake of Na and Fe on symmetrically non-equivalent steps. Near the crystal surface, the non- equivalent coeval vicinal faces of growth hillocks on \\{100\\} are either diopside-like, Na.007Ca1.00(Mg0.754Fe2+0.22Mn2+0.013Al_{0.003)Si2.00O6 , or acmitic, Ca0.63Na0.35(Mg0.64Fe3+ 0.36)Al0.01Si1.99O6 in composition. Step-specific incorporation of minor elements in a clinopyroxene face has only been documented once, in a hydrothermal diopside from Orford (Quebec), where Fe(II) and Mn(II) were differentially incorporated on steps oriented parallel to [010] on \\{100\\} faces. This natural example and our synthetic crystals reflect growth regimes where minor element incorporation was limited by surface-structural kinetics rather than diffusion- controlled kinetics. Such step-specific surface-structural control has never been reported in clinopyroxenes grown from silicate melts. Is it present, but more subtle, or do silicate melts promote a significantly different growth regime? Comparing zoning patterns in synthetic silicates grown from carbonate versus silicate melts could put new constraints on current models of element partitioning.

Synthesis, purification and bulk crystal growth of radiation detector materials using melt growth technique

NASA Astrophysics Data System (ADS)

Surabhi, Raja Rahul Reddy

In the past decade, there has been new and increased usage of radiation-detection technologies for applications in homeland security, non-proliferation, and national defense. Most of these applications require a portable device with high gamma-ray energy resolution and detection efficiency, compact size, room-temperature operation, and low cost. Consequently, there is a renewed understanding of the material limitations for these technologies and a great demand to develop next-generation radiation-detection materials that can operate at room temperature. Mercuric iodide (HgI2), Lead iodide (PbI2), and CdZnTe (CZT) are the current leading candidates for radiation detector applications. This is because of their high atomic number and large band gap that makes them particularly well suited for fabrication of high resolution and high efficiency compact devices. PbI2 is a promising material for room temperature nuclear radiation detectors, characterized by its wide band gap (EG=2.32eV) and high-density (rho=6.2g/cm3). It has been reported that PbI2 crystal detectors are able to detect gamma-ray in the range of 1KeV-1MeV, with good energy resolution. However, PbI 2 detectors have not been studied in detail because of non-availability of high quality single crystals. This study presents the synthesis, purification, growth and characterization of PbI2 single crystals grown. In this research, solid-state synthesis technique has been utilized for obtaining PbI2 as a starting material. For the first time, a unique low-temperature purification technique has been developed to obtain high-purity starting material. The crystals were grown using 2-zone Bridgman-Stockbarger (B.S) technique wherein growth rate and temperature gradient at the solid-liquid interface were optimized. Single crystals of PbI2 were successfully grown in quartz glass ampoule under different growth conditions. Material purity was determined by measuring the elemental concentration using the Inductively coupled plasma-optical emission spectroscopy (ICP-OES). ICP-OES is utilized for estimating impurities present in the low-temperature purified material, zone refined material and melt grown PbI2 crystals. The zone-refined material contains no traceable amounts of impurities, whereas the low-temperature purified material and melt grown PbI2 crystals show very low concentration of K (potassium) and Na (sodium) impurities. Crystal characterization has been performed for determining optical properties by UV-VIS spectroscopy. The energy band gap (EG) is an important parameter for materials used for room temperature gamma-ray detector applications. The absorption peak at 530nm is a characteristic of PbI2 and corresponds to the onset of the transitions from the valence band to the exciton level. From this absorption spectrum the calculated indirect band gap of PbI 2 was 2.33+/-0.025 eV at room temperature. For measuring the electrical properties (Dielectric and I-V characteristics) of the crystal, Ag (silver) contacts are applied to both sides of the sample. Dielectric analysis on melt grown PbI2 showed that space charge polarization was dominant at lower frequencies but stabilizes at higher frequencies over different operating temperatures. On the other hand, dielectric analysis for zone-refined material space charge polarization was constant over the operating range resulting in fewer lattice defects. Therefore the low temperature purified material followed by zone-refined purification provides detector grade material with fewer lattice defects. The measured electrical resistivity for melt grown PbI2 and zone-refined material are 3.185 x 10 10 O-cm and 0.754 x 109 O-cm at room temperature along (001) plane respectively.

Crystal Growth of New Functional Materials for Electro-Optical Applications

DTIC Science & Technology

2001-01-01

Ga2O3 single crystals have been grown by the floating zone technique as promising transparent conductive oxides. 1. INTRODUCTION The important role of...through the addition of dopants while preserving the transparency of the pure B- Ga2O3 makes of this material a substitutive candidate for transparent

Plagioclase populations and zoning in dacite of the 2004-2005 Mount St. Helens eruption: constraints for magma origin and dynamics: Chapter 34 in A volcano rekindled: the renewed eruption of Mount St. Helens, 2004-2006

USGS Publications Warehouse

Streck, Martin J.; Broderick, Cindy A.; Thronber, Carl R.; Clynne, Michael A.; Pallister, John S.; Sherrod, David R.; Scott, William E.; Stauffer, Peter H.

2008-01-01

We propose that crystals with no dissolution surfaces are those that were supplied last to the shallow reservoir, whereas plagioclase with increasingly more complex zoning patterns (that is, the number of zoned bands bounded by dissolution surfaces) result from prolonged residency and evolution in the reservoir. We propose that banding and An zoning across multiple bands are primarily a response to thermally induced fluctuations in crystallinity of the magma in combination with recharge; a lesser role is ascribed to cycling crystals through pressure gradients. Crystals without dissolution surfaces, in contrast, could have grown only in response to steady(?) decompression. Some heating-cooling cycles probably postdate the final eruption in 1986. They resulted from small recharge events that supplied new crystals that then experienced resorption-growth cycles. We suggest that magmatic events shortly prior to the current eruption, recorded in the outermost zones of plagioclase phenocrysts, began with the incorporation of acicular orthopyroxene, followed by last resorption, and concluded with crystallization of euhedral rims. Finally, we propose that 2004-5 dacite is composed mostly of dacite magma that remained after 1986 and underwent subsequent magmatic evolution but, more importantly, contains a component of new dacite from deeper in the magmatic system, which may have triggered the new eruption.

Evaluation of Temperature Gradient in Advanced Automated Directional Solidification Furnace (AADSF) by Numerical Simulation

NASA Technical Reports Server (NTRS)

Bune, Andris V.; Gillies, Donald C.; Lehoczky, Sandor L.

1996-01-01

A numerical model of heat transfer using combined conduction, radiation and convection in AADSF was used to evaluate temperature gradients in the vicinity of the crystal/melt interface for variety of hot and cold zone set point temperatures specifically for the growth of mercury cadmium telluride (MCT). Reverse usage of hot and cold zones was simulated to aid the choice of proper orientation of crystal/melt interface regarding residual acceleration vector without actual change of furnace location on board the orbiter. It appears that an additional booster heater will be extremely helpful to ensure desired temperature gradient when hot and cold zones are reversed. Further efforts are required to investigate advantages/disadvantages of symmetrical furnace design (i.e. with similar length of hot and cold zones).

Bridgman-Stockbarger growth of SrI2:Eu2+ single crystal

NASA Astrophysics Data System (ADS)

Raja, A.; Daniel, D. Joseph; Ramasamy, P.; Singh, S. G.; Sen, S.; Gadkari, S. C.

2018-05-01

Strontium Iodide (SrI2): Europium Iodide (EuI2) was purified by Zone-refinement process. Europium doped strontium iodide (SrI2:Eu2+) single crystal was grown by modified vertical Bridgman - Stockbarger technique. Photoluminescence (PL) excitation and emission (PLE) spectra were measured for Eu2+ doped SrI2 crystal. The sharp emission was recorded at 432 nm. Scintillation properties of the SrI2:Eu2+ crystal were checked by the gamma ray spectrometer using 137Cs gamma source.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hossain, M. Anwar; Center for Crystal Science and Technology, University of Yamanashi, Miyamae 7-32, Kofu, Yamanashi 400-8511; Tanaka, Isao

We studied thermoelectric properties of YB{sub 41}Si{sub 1.3} single crystals grown by the floating zone method. The composition of the grown crystal was confirmed by electron probe micro-analysis. We have determined the growth direction for the first time for these borosilicides, and discovered relatively large anisotropy in electrical properties. We measured the electrical resistivity and Seebeck coefficient along [510] (the growth direction) and [052] directions and we found that this crystal exhibits strong electrical anisotropy with a maximum of more than 8 times. An interesting layered structural feature is revealed along [510] with dense boron cluster layers and yttrium layers,more » with conductivity enhanced along this direction. We obtained 3.6 times higher power factor along [510] compared to that along [052]. Although the ZT of the present system is low, anisotropy in the thermoelectric properties of a boride was reported for the first time, and can be a clue in developing other boride systems also. - Graphical abstract: The growth direction ([510]) was determined for the first time in YB{sub 41}Si{sub 1.3} single crystals and revealed an interesting layered feature of boron clusters and metal atoms, along which the electrical conductivity and thermoelectric power factor was strongly enhanced. - Highlights: • We have grown YB{sub 41}Si{sub 1.3} single crystals by the floating zone method. • Growth direction of [510] determined for first time in REB{sub 41}Si{sub 1.2}. • Electrical resistivity was strongly anisotropic with possible enhancement along metal layers. • The obtained power factor along [510] is 3.6 times higher than that along [052].« less

Growth of binary organic NLO crystals: m.NA-p.NA and m.NA-CNA system

NASA Technical Reports Server (NTRS)

Singh, N. B.; Henningsen, T.; Hopkins, R. H.; Mazelsky, R.

1993-01-01

Experiments were carried out to grow 3.Nitroaniline (m.NA) crystals doped with 4.Nitroaniline (p.NA) and 2.chloro 4.Nitroaniline (CNA). The measured undercooling for m.NA, p.NA, and CNA were 0.21 tm K, 0.23 tm K, and 0.35 tm K respectively, where tm represents the melting temperature of the pure component. Because of the crystals' large heat of fusion and large undercooling, it was not possible to grow good quality crystals with low thermal gradients. In the conventional two-zone Bridgman furnace we had to raise the temperature of the hot zone above the decomposition temperature of CNA, p.NA, and m.NA to achieve the desired thermal gradient. To avoid decomposition, we used an unconventional Bridgman furnace. Two immiscible liquids, silicone oil and ethylene glycol, were used to build a special two-zone Bridgman furnace. A temperature gradient of 18 K/cm was achieved without exceeding the decomposition temperature of the crystal. The binary crystals, m.NA-p.NA and m.NA-CNA, were grown in centimeter size in this furnace. X-ray and optical characterization showed good optical quality.

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

NASA Technical Reports Server (NTRS)

Dold, P.; Corell, A.; Schweizer, M.; Kaiser, Th.; Szofran, F.; Nakamura, S.; Hibiya, T.; Benz, K. W.

1998-01-01

Fluctuations of the electrical resistivity due to inhomogeneous dopant distribution are still a serious problem for the industrial processing yield of doped silicon crystals. In the case of silicon floating-zone growth, the main sources of these inhomogeneities are time- dependent flows in the liquid phase during the growth process. Excluding radio frequency (RF) induced convection, buoyancy and thermocapillary (Marangoni) convection are the two natural reasons for fluid flow. Both originate from temperature/concentration gradients in the melt, buoyancy convection through thermal/concentrational volume expansion, and thermocapillary convection through the temperature/concentration dependence of the surface tension. To improve the properties of grown crystals, knowledge of the strength, the characteristic, and the relation of these two flow mechanisms is essential. By the use of microgravity, the effect and the strength of buoyancy (gravity dependent) and thermocapillary (gravity independent) convection can be separated and clarified. Applying magnetic fields, both convective modes can be influenced: fluid flow can either be damped (static magnetic fields) or overlaid by a regular flow regime (rotating magnetic fields). Two complementary approaches have been pursued: Silicon full zones (experiments on the German sounding rockets TEXUS 7, 12, 22, 29, and 36) with the maximum temperature at half of the zone height and silicon half zones (experiments on the Japanese sounding rockets TR-IA4 and 6) with the maximum temperature at the top of the melt. With the full zone arrangement, the intensity and the frequency of the dopant striations could be determined and the critical Marangoni number could be identified. The half zone configuration is suited to classify the flow pattern and to measure the amplitude and the frequency of temperature fluctuations in the melt by inserting thermocouples or temperature sensors into the melt. All experiments have been carried out in monoellipsoid mirror furnaces. Typical zone geometries are approx. 8 to 14 mm in diameter and height. The crystals grown under microgravity are compared to crystals grown in static axial magnetic fields (B<5 tesla) and in transversal rotating magnetic fields (B<7.5 mT / f=50 Hz). Experimental results are completed by 3D numerical simulations: the obtained temperature and concentration distribution in the melt confirm the damping effect of rotating magnetic fields and explain the change in the radial segregation under static magnetic fields.

Discerning crystal growth from diffusion profiles in zoned olivine by in situ Mg–Fe isotopic analyses

USGS Publications Warehouse

Sio, Corliss Kin I.; Dauphas, Nicolas; Teng, Fang-Zhen; Chaussidon, Marc; Helz, Rosalind T.; Roskosz, Mathieu

2013-01-01

Mineral zoning is used in diffusion-based geospeedometry to determine magmatic timescales. Progress in this field has been hampered by the challenge to discern mineral zoning produced by diffusion from concentration gradients inherited from crystal growth. A zoned olivine phenocryst from Kilauea Iki lava lake (Hawaii) was selected for this study to evaluate the potential of Mg and Fe isotopes for distinguishing these two processes. Microdrilling of the phenocryst (∼300 μm drill holes) followed by MC-ICPMS analysis of the powders revealed negatively coupled Mg and Fe isotopic fractionations (δ26Mg from +0.1‰ to −0.2‰ and δ56Fe from −1.2‰ to −0.2‰ from core to rim), which can only be explained by Mg–Fe exchange between melt and olivine. The data can be explained with ratios of diffusivities of Mg and Fe isotopes in olivine scaling as D2/D1 = (m1/m2)β with βMg ∼0.16 and βFe ∼0.27. LA-MC-ICPMS and MC-SIMS Fe isotopic measurements are developed and are demonstrated to yield accurate δ56Fe measurements within precisions of ∼0.2‰ (1 SD) at spatial resolutions of ∼50 μm. δ56Fe and δ26Mg stay constant with Fo# in the rim (late-stage overgrowth), whereas in the core (original phenocryst) δ56Fe steeply trends toward lighter compositions and δ26Mg trends toward heavier compositions with higher Fo#. A plot of δ56Fe vs. Fo# immediately distinguishes growth-controlled from diffusion-controlled zoning in these two regions. The results are consistent with the idea that large isotopic fractionation accompanies chemical diffusion in crystals, whereas fractional crystallization induces little or no isotopic fractionation. The cooling timescale inferred from the chemical-isotope zoning profiles is consistent with the documented cooling history of the lava lake. In the absence of geologic context, in situ stable isotopic measurements may now be used to interpret the nature of mineral zoning. Stable isotope measurements by LA-MC-ICPMS and MC-SIMS can be used as standard petrologic tools to identify samples for diffusion-based geospeedometry.

Numerical Optimization of the Thermal Field in Bridgman Detached Growth

NASA Technical Reports Server (NTRS)

Stelian, C.; Volz, M. P.; Derby, J. J.

2009-01-01

The global modeling of the thermal field in two vertical Bridgman-like crystal growth configurations, has been performed to get optimal thermal conditions for a successful detached growth of Ge and CdTe crystals. These computations are performed using the CrysMAS code and expand upon our previous analysis [1] that propose a new mechanism involving the thermal field and meniscus position to explain stable conditions for dewetted Bridgman growth. The analysis of the vertical Bridgman configuration with two heaters, used by Palosz et al. for the detached growth of Ge, shows, consistent with their results, that the large wetting angle of germanium on boron nitride surfaces was an important factor to promote a successful detached growth. Our computations predict that by initiating growth much higher into the hot zone of the furnace, the thermal conditions will be favorable for continued detachment even for systems that did not exhibit high contact angles. The computations performed for a vertical gradient freeze configuration with three heaters representative of that used for the detached growth of CdTe, show favorable thermal conditions for dewetting during the entirely growth run described. Improved thermal conditions are also predicted for coated silica crucibles when the solid-liquid interface advances higher into the hot zone during the solidification process. The second set of experiments on CdTe growth described elsewhere has shown the reattachment of the crystal to the crucible after few centimeters of dewetted growth. The thermal modeling of this configuration shows a second solidification front appearing at the top of the sample and approaching the middle line across the third heater. In these conditions, the crystal grows detached from the bottom, but will be attached to the crucible in the upper part because of the solidification without gap in this region. The solidification with two interfaces can be avoided when the top of the sample is positioned below the middle position of the third furnace.

Modeling the growth processes of polyelectrolyte multilayers using a quartz crystal resonator.

PubMed

Salomäki, Mikko; Kankare, Jouko

2007-07-26

The layer-by-layer buildup of chitosan/hyaluronan (CH/HA) and poly(l-lysine)/hyaluronan (PLL/HA) multilayers was followed on a quartz crystal resonator (QCR) in different ionic strengths and at different temperatures. These polyelectrolytes were chosen to demonstrate the method whereby useful information is retrieved from acoustically thick polymer layers during their buildup. Surface acoustic impedance recorded in these measurements gives a single or double spiral when plotted in the complex plane. The shape of this spiral depends on the viscoelasticity of the layer material and regularity of the growth process. The polymer layer is assumed to consist of one or two zones. A mathematical model was devised to represent the separation of the layer to two zones with different viscoelastic properties. Viscoelastic quantities of the layer material and the mode and parameters of the growth process were acquired by fitting a spiral to the experimental data. In all the cases the growth process was mainly exponential as a function of deposition cycles, the growth exponent being between 0.250 and 0.275.

Characterization of 4H <000-1> Silicon Carbide Films Grown by Solvent-Laser Heated Floating Zone

NASA Technical Reports Server (NTRS)

Woodworth, Andrew, A; Sayir, Ali; Neudeck, Philip, G; Raghothamachar, Balaji; Dudley, Michael

2012-01-01

Commercially available bulk silicon carbide (SiC) has a high number (>2000/sq cm) of screw dislocations (SD) that have been linked to degradation of high-field power device electrical performance properties. Researchers at the NASA Glenn Research Center have proposed a method to mass-produce significantly higher quality bulk SiC. In order for this bulk growth method to become reality, growth of long single crystal SiC fibers must first be achieved. Therefore, a new growth method, Solvent-Laser Heated Floating Zone (Solvent-LHFZ), has been implemented. While some of the initial Solvent-LHFZ results have recently been reported, this paper focuses on further characterization of grown crystals and their growth fronts. To this end, secondary ion mass spectroscopy (SIMS) depth profiles, cross section analysis by focused ion beam (FIB) milling and mechanical polishing, and orientation and structural characterization by x-ray transmission Laue diffraction patterns and x-ray topography were used. Results paint a picture of a chaotic growth front, with Fe incorporation dependant on C concentration.

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science ISS Investigation

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.

2014-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processinginduced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. 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 crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croell, A.

2012-01-01

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. 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 crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Crystal growth and characterization of the CMR compound La 1.2(Sr,Ca) 1.8Mn 2O 7

NASA Astrophysics Data System (ADS)

Velázquez, M.; Haut, C.; Hennion, B.; Revcolevschi, A.

2000-12-01

High-quality centimeter-sized single crystals of La 1.2Sr 1.8- yCa yMn 2O 7 (0.0⩽ y⩽0.2) were successfully grown using a floating zone method associated with an image furnace. We present the growth conditions together with a characterization of the single crystals by means of optical and electron microscopy, EDX and ICP⧸AES analysis, DTA-TGA measurements and redox titration, X-ray powder diffraction, Laue X-ray back-reflection and neutron diffraction. We also stress the main aspects of the complex thermodynamical and kinetic behaviors of these compounds.

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

NASA Astrophysics Data System (ADS)

Zhang, Fangkun; Liu, Tao; Wang, Xue Z.; Liu, Jingxiang; Jiang, Xiaobin

2017-02-01

In this paper calibration model building based on using an ATR-FTIR spectroscopy is investigated for in-situ measurement of the solution concentration during a cooling crystallization process. The cooling crystallization of L-glutamic Acid (LGA) as a case is studied here. It was found that using the metastable zone (MSZ) data for model calibration can guarantee the prediction accuracy for monitoring the operating window of cooling crystallization, compared to the usage of undersaturated zone (USZ) spectra for model building as traditionally practiced. Calibration experiments were made for LGA solution under different concentrations. Four candidate calibration models were established using different zone data for comparison, by using a multivariate partial least-squares (PLS) regression algorithm for the collected spectra together with the corresponding temperature values. Experiments under different process conditions including the changes of solution concentration and operating temperature were conducted. The results indicate that using the MSZ spectra for model calibration can give more accurate prediction of the solution concentration during the crystallization process, while maintaining accuracy in changing the operating temperature. The primary reason of prediction error was clarified as spectral nonlinearity for in-situ measurement between USZ and MSZ. In addition, an LGA cooling crystallization experiment was performed to verify the sensitivity of these calibration models for monitoring the crystal growth process.

Large single crystal growth, transport property, and spectroscopic characterizations of three-dimensional Dirac semimetal Cd3As2.

PubMed

Sankar, R; Neupane, M; Xu, S-Y; Butler, C J; Zeljkovic, I; Panneer Muthuselvam, I; Huang, F-T; Guo, S-T; Karna, Sunil K; Chu, M-W; Lee, W L; Lin, M-T; Jayavel, R; Madhavan, V; Hasan, M Z; Chou, F C

2015-08-14

The three dimensional (3D) Dirac semimetal is a new quantum state of matter that has attracted much attention recently in physics and material science. Here, we report on the growth of large plate-like single crystals of Cd3As2 in two major orientations by a self-selecting vapor growth (SSVG) method, and the optimum growth conditions have been experimentally determined. The crystalline imperfections and electrical properties of the crystals were examined with transmission electron microscopy (TEM), scanning tunneling microscopy (STM), and transport property measurements. This SSVG method makes it possible to control the as-grown crystal compositions with excess Cd or As leading to mobilities near 5-10(5) cm(2)V(-1)s(-1). Zn-doping can effectively reduce the carrier density to reach the maximum residual resistivity ratio (RRRρ300K/ρ5K) of 7.6. A vacuum-cleaved single crystal has been investigated using angle-resolved photoemission spectroscopy (ARPES) to reveal a single Dirac cone near the center of the surface Brillouin zone with a binding energy of approximately 200 meV.

Growth, and magnetic study of Sm0.4Er0.6FeO3 single crystal grown by optical floating zone technique

NASA Astrophysics Data System (ADS)

Wu, Anhua; Zhao, Xiangyang; Man, Peiwen; Su, Liangbi; Kalashnikova, A. M.; Pisarev, R. V.

2018-03-01

Sm0.4Er0.6FeO3 single crystals were successfully grown by optical floating zone method; high quality samples with various orientations were manufactured. Based on these samples, Magnetic property of Sm0.4Er0.6FeO3 single crystals were investigated systemically by means of the temperature dependence of magnetization. It indicated that compositional variations not only alter the spin reorientation temperature, but also the compensation temperature of the orthoferrites. Unlike single rare earth orthoferrites, the reversal transition temperature point of Sm0.4Er0.6FeO3 increases as magnetic field increases, which is positive for designing novel spin switching or magnetic sensor device.

Microgravity

NASA Image and Video Library

1991-09-01

The Advanced Automated Directional Solidification Furnace (AADSF) flew during the USMP-2 mission. During USMP-2, the AADSF was used to study the growth of mercury cadmium telluride crystals in microgravity by directional solidification, a process commonly used on earth to process metals and grow crystals. The furnace is tubular and has three independently controlled temperature zones. The sample travels from the hot zone of the furnace (1600 degrees F) where the material solidifies as it cools. The solidification region, known as the solid/liquid interface, moves from one end of the sample to the other at a controlled rate, thus the term directional solidification.

Feasibility investigation of growing gallium arsenide single crystals in ribbon form

NASA Technical Reports Server (NTRS)

Richardson, D. L.

1975-01-01

Polycrystalline GaAs ribbons have been grown in graphite boats by passage of a wide zone through B2O3 encapsulated feed stock, confined by a quartz cover plate. By controlling the heat flow in the graphite boat and controlling the zoning rate, large grained, single phase polycrystalline samples with directional solidification and good thickness control were achieved. Arsenic vaporization was effectively suppressed at the melting point of GaAs by the B2O3 moat and 3 atmospheres of pressure. A vertical constrained-zone-melting apparatus with a B2O3 moat seal, rf heating, and water cooling on the bottom will be used to control the heat flow and temperature patterns required for growth of single crystal ribbons.

Multiple hydrothermal and metamorphic events in the Kidd Creek volcanogenic massive sulphide deposit, Timmins, Ontario: evidence from tourmalines and chlorites

USGS Publications Warehouse

Slack, J.F.; Coad, P.R.

1989-01-01

The tourmalines and chlorites record a series of multiple hydrothermal and metamorphic events. Paragenetic studies suggest that tourmaline was deposited during several discrete stages of mineralization, as evidence by brecciation and cross-cutting relationships. Most of the tourmalines have two concentric growth zones defined by different colours (green, brown, blue, yellow). Some tourmalines also display pale discordant rims that cross-cut and embay the inner growth zones and polycrystalline, multiple-extinction domains. Late sulphide veinlets (chalcopyrite, pyrrhotite) transect the inner growth zones and pale discordant rims of many crystals. The concentric growth zones are interpreted as primary features developed by the main ore-forming hydrothermal system, whereas the discordant rims, polycrystalline domains, and cross-cutting sulphide veinlets reflect post-ore metamorphic processes. Variations in mineral proportions and mineral chemistry within the deposit mainly depend on fluctuations in temperature, pH, water/rock ratios, and amounts of entrained seawater. -from Authors

Crucible-free pulling of germanium crystals

NASA Astrophysics Data System (ADS)

Wünscher, Michael; Lüdge, Anke; Riemann, Helge

2011-03-01

Commonly, germanium crystals are grown after the Czochralski (CZ) method. The crucible-free pedestal and floating zone (FZ) methods, which are widely used for silicon growth, are hardly known to be investigated for germanium. The germanium melt is more than twice as dense as liquid silicon, which could destabilize a floating zone. Additionally, the lower melting point and the related lower radiative heat loss is shown to reduce the stability especially of the FZ process with the consequence of a screw-like crystal growth. We found that the lower heat radiation of Ge can be compensated by the increased convective cooling of a helium atmosphere instead of the argon ambient. Under these conditions, the screw-like growth could be avoided. Unfortunately, the helium cooling deteriorates the melting behavior of the feed rod. Spikes appear along the open melt front, which touch on the induction coil. In order to improve the melting behavior, we used a lamp as a second energy source as well as a mixture of Ar and He. With this, we found a final solution for growing stable crystals from germanium by using both gases in different parts of the furnace. The experimental work is accompanied by the simulation of the stationary temperature field. The commercially available software FEMAG-FZ is used for axisymmetric calculations. Another tool for process development is the lateral photo-voltage scanning (LPS), which can determine the shape of the solid-liquid phase boundary by analyzing the growth striations in a lateral cut of a grown crystal. In addition to improvements of the process, these measurements can be compared with the calculated results and, hence, conduce to validate the calculation.

Purification of organic nonlinear optical materials for bulk crystal growth from melt

NASA Astrophysics Data System (ADS)

Gebre, Tesfaye; Bhat, Kamala N.; Batra, Ashok K.; Lal, Ravindra B.; Aggarwal, Mohan D.; Penn, Benjamin G.; Frazier, Donald O.

2002-10-01

The techniques developed for purification of nonlinear optical organic materials, such as benzil, 2-methyl-4-nitroaniline (MNA), Dicyanovinyl anisole (DIVA) and its derivatives, nitrophenyl prolinol (NPP) and other Schiff's base compounds, include Kugelrohy method, physical vapor transport, zone refining and recrystallization from the solvent are described. Purity of the materials is tested using differential thermal analysis, gas chromatograph/Mass detector, Fourier Transform Infrared spectroscopy and melting point measurements. The purified materials were later used in the growth of single crystal by Bridgman-Stockbarger and Czochralski techniques.

Investigation of materials for inert electrodes in aluminum electrodeposition cells

NASA Astrophysics Data System (ADS)

Haggerty, J. S.; Sadoway, D. R.

1987-09-01

Work was divided into major efforts. The first was the growth and characterization of specimens; the second was Hall cell performance testing. Cathode and anode materials were the subject of investigation. Preparation of specimens included growth of single crystals and synthesis of ultra high purity powders. Special attention was paid to ferrites as they were considered to be the most promising anode materials. Ferrite anode corrosion rates were studied and the electrical conductivities of a set of copper-manganese ferrites were measured. Float Zone, Pendant Drop Cryolite Experiments were undertaken because unsatisfactory choices of candidate materials were being made on the basis of a flawed set of selection criteria applied to an incomplete and sometimes inaccurate data base. This experiment was then constructed to determine whether the apparatus used for float zone crystal growth could be adapted to make a variety of important based melts and their interactions with candidate inert anode materials. Compositions), driven by our perception that the basis for prior selection of candidate materials was inadequate. Results are presented.

High pressure floating zone growth and structural properties of ferrimagnetic quantum paraelectric BaFe 12O 19

DOE PAGES

Cao, Huibo B.; Zhao, Zhiying Y.; Lee, Minseong; ...

2015-06-24

High quality single crystals of BaFemore » $$_{12}$$O$$_{19}$$ were grown with the floating zone technique in flowing oxygen atmosphere of 100 atm. BaFe$$_{12}$$O$$_{19}$$ melts incongruently in atmospheric oxygen. High oxygen pressure above 50 atm modifies the melting behavior to be congruent, which allows for the crystal growth with the crucible-free floating zone technique. Single crystal neutron diffraction were measured to determine the nuclear and magnetic structures at 4 K and 295 K. At both temperatures, there exist local electric dipoles formed by the off-mirror-plane displacements of magnetic Fe$$^{3+}$$ ions at the bypyramidal sites. The displacement at 4 K is about half of that at room temperature. The temperature dependence of specific heat shows no anomaly associated with the long range polar ordering in the temperature range of 1.90-300~K. The inverse dielectric constant along the c-axis shows a $T^2$ temperature dependence below 20 K and then following by a plateau below 10 K, recognized as quantum paraelectric features. Further cooling below 1.4 K, the upturn region was clearly revealed and indicates BaFe$$_{12}$$O$$_{19}$$ is a critical quantum paraelectric system with Fe$$^{3+}$$ ions playing roles for both magnetic and electric dipoles.« less

An analytical approach to thermal modeling of Bridgman-type crystal growth. I - One-dimensional analysis

NASA Technical Reports Server (NTRS)

Naumann, R. J.

1982-01-01

A relatively simple one-dimensional thermal model of the Bridgman growth process has been developed which is applicable to the growth of small diameter samples with conductivities similar to those of metallic alloys. The heat flow in a translating rod is analyzed in a way that is applicable to Biot numbers less than unity. The model accommodates an adiabatic zone, different heat transfer coefficients in the hot and cold zones, and changes in sample material properties associated with phase change. The analysis is applied to several simplified cases. The effect of the rod's motion is studied in a three-zone furnace for a rod sufficiently long that end effects can be neglected; end effects are then investigated for a motionless rod. Finally, the addition of a fourth zone, an independently controlled booster heater between the main heater and the adiabatic zone, is evaluated for its ability to increase the gradient in the sample at the melt interface and to control the position of the interface.

Compositional zoning of the bishop tuff

USGS Publications Warehouse

Hildreth, W.; Wilson, C.J.N.

2007-01-01

Compositional data for >400 pumice clasts, organized according to eruptive sequence, crystal content, and texture, provide new perspectives on eruption and pre-eruptive evolution of the >4600 km3 of zoned rhyolitic magma ejected as the BishopTuff during formation of Long Valley caldera. Proportions and compositions of different pumice types are given for each ignimbrite package and for the intercalated plinian pumice-fall layers that erupted synchronously. Although withdrawal of the zoned magma was less systematic than previously realized, the overall sequence displays trends toward greater proportions of less evolved pumice, more crystals (0-5 24 wt %), and higher FeTi-oxide temperatures (714-818??C). No significant hiatus took place during the 6 day eruption of the BishopTuff, nearly all of which issued from an integrated, zoned, unitary reservoir. Shortly before eruption, however, the zoned melt-dominant portion of the chamber was invaded by batches of disparate lower-silica rhyolite magma, poorer in crystals than most of the resident magma but slightly hotter and richer in Ba, Sr, andTi. Interaction with resident magma at the deepest levels tapped promoted growth ofTi-rich rims on quartz, Ba-rich rims on sanidine, and entrapment of near-rim melt inclusions relatively enriched in Ba and CO2.Varied amounts of mingling, even in higher parts of the chamber, led to the dark gray and swirly crystal-poor pumices sparsely present in all ashflow packages. As shown by FeTi-oxide geothermometry, the zoned rhyolitic chamber was hottest where crystal-richest, rendering any model of solidification fronts at the walls or roof unlikely.The main compositional gradient (75-195 ppm Rb; 0.8-2.2 ppm Ta; 71-154 ppm Zr; 0.40-1.73% FeO*) existed in the melt, prior to crystallization of the phenocryst suite observed, which included zircon as much as 100 kyr older than the eruption.The compositions of crystals, though themselves largely unzoned, generally reflect magma temperature and the bulk compositional gradient, implying both that few crystals settled or were transported far and that the observed crystals contributed little to establishing that gradient. Upward increases in aqueous gas and dissolved water, combined with the adiabatic gradient (for the 5 km depth range tapped) and the roofward decline in liquidus temperature of the zoned melt, prevented significant crystallization against the roof, consistent with dominance of crystal-poor magma early in the eruption and lack of any roof-rind fragments among the Bishop ejecta, before or after onset of caldera collapse. A model of secular incremental zoning is advanced wherein numerous batches of crystal-poor melt were released from a mush zone (many kilometers thick) that floored the accumulating rhyolitic melt-rich body. Each batch rose to its own appropriate level in the melt-buoyancy gradient, which was selfsustaining against wholesale convective re-homogenization, while the thick mush zone below buffered it against disruption by the deeper (non-rhyolitic) recharge that augmented the mush zone and thermally sustained the whole magma chamber. Crystal-melt fractionation was the dominant zoning process, but it took place not principally in the shallow melt-rich body but mostly in the pluton-scale mush zone before and during batchwise melt extraction. ?? Published by Oxford University Press (2007).

Phosphorus as indicator of magmatic olivine residence time, morphology and growth rate

NASA Astrophysics Data System (ADS)

Sobolev, Alexander; Batanova, Valentina

2015-04-01

Phosphorus is among of slowest elements by diffusion rate in silicate melts and crystals (e.g. Spandler et al, 2007). In the same time it is moderately incompatible to compatible with olivine (Brunet & Chazot, 2001; Grant & Kohn, 2013). This makes phosphorus valuable tracer of olivine crystallization in natural conditions. Indeed, it is shown that natural magmatic olivine crystals commonly posses strong and complicated zoning in phosphorus (Milman-Barris et al, 2008; Welsch et al, 2014). In this paper we intend to review phosphorus behavior in olivine in published experimental and natural olivine studies and present large set of new EPMA data on phosphorus zoning in olivine phenocrysts from MORBs, OIBs, komatiites and kimberlites. We will show that sharp olivine zones enriched in phosphorus by a factor of 10-20 over prediction by equilibrium partition may be due to formation of P-rich boundary layer on the interface of fast growing olivine. This is proved by finding of small-size (normally 10 mkm or less) exceptionally P-rich melt inclusions in olivine, which are otherwise similar in composition to typical melt. These observations could provide potential olivine growth speedometer. We will also demonstrate, that sharp zoning in phosphorus may provide valuable information on the residence time of olivine crystals in different environments: magma chambers and conduits as well as mantle sources. This study has been founded by Russian Science Foundation grant 14-17-00491. References: Spandler, et al, 2007, Nature, v. 447, p. 303-306; Brunet & Chazot, 2001, Chemical Geology, v. 176, p. 51-72; Grant & Kohn, 2013, American Mineralogist, v. 98, p. 1860-1869; Milman-Barris et al, 2008, Contr. Min. Petrol. v. 155, p.739-765; Welsch et al, 2014, Geology, v. 42, p.867-870.

Preparative crystallization of a single chain antibody using an aqueous two-phase system.

PubMed

Huettmann, Hauke; Berkemeyer, Matthias; Buchinger, Wolfgang; Jungbauer, Alois

2014-11-01

A simultaneous crystallization and aqueous two-phase extraction of a single chain antibody was developed, demonstrating process integration. The process conditions were designed to form an aqueous two-phase system, and to favor crystallization, using sodium sulfate and PEG-2000. At sufficiently high concentrations of PEG, a second phase was generated in which the protein crystallization occurred simultaneously. The single chain antibody crystals were partitioned to the top, polyethylene glycol-rich phase. The crystal nucleation took place in the sodium sulfate-rich phase and at the phase boundary, whereas crystal growth was progressing mainly in the polyethylene glycol-rich phase. The crystals in the polyethylene glycol-rich phase grew to a size of >50 µm. Additionally, polyethylene glycol acted as an anti-solvent, thus, it influenced the crystallization yield. A phase diagram with an undersaturation zone, crystallization area, and amorphous precipitation zone was established. Only small differences in polyethylene glycol concentration caused significant shifts of the crystallization yield. An increase of the polyethylene glycol content from 2% (w/v) to 4% (w/v) increased the yield from approximately 63-87%, respectively. Our results show that crystallization in aqueous two-phase systems is an opportunity to foster process integration. © 2014 Wiley Periodicals, Inc.

High purith low defect FZ silicon

NASA Technical Reports Server (NTRS)

Kimura, H.; Robertson, G.

1985-01-01

The most common intrinsic defects in dislocation-free float zone (FZ) silicon crystals are the A- and B-type swirl defects. The mechanisms of their formation and annihilation have been extensively studied. Another type of defect in dislocation-free FZ crystals is referred to as a D-type defect. Concentrations of these defects can be minimized by optimizing the growth conditions, and the residual swirls can be reduced by the post-growth extrinsic gettering process. Czochralski (Cz) silicon wafers are known to exhibit higher resistance to slip and warpage due to thermal stress than do FZ wafers. The Cz crystals containing dislocations are more resistant to dislocation movement than dislocated FZ crystals because of the locking of dislocations by oxygen atoms present in the Cz crystals. Recently a transverse magnetic field was applied during the FZ growth of extrinsic silicon. Resultant flow patterns, as revealed by striation etching and spreading resistance in Ga-doped silicon crystals, indicate strong effects of the transverse magnetic field on the circulation within the melt. At fields of 5500 gauss, the fluid flow in the melt volume is so altered as to affect the morphology of the growing crystal.

Phase diagrams and crystal growth

NASA Astrophysics Data System (ADS)

Venkrbec, Jan

1980-04-01

Phase diagrams are briefly treated as generalized property-composition relationships, with respect to crystal technology optimization. The treatment is based on mutual interaction of three systems related to semiconductors: (a) the semiconducting material systems, (b0 the data bank, (c) the system of crystallization methods. A model is proposed enabling optimatization on the path from application requirements to the desired material. Further, several examples of the selection as to the composition of LED and laser diode material are given. Some of molten-solution-zone methods are being successfully introduced for this purpose. Common features of these methods, the application of phase diagrams, and their pecularities compared with other crystallization methods are illustrated by schematic diagrams and by examples. LPE methods, particularly the steady-state LPE methods such as Woodall's ISM and Nishizawa's TDM-CVP, and the CAM-S (Crystallization Method Providing Composition Autocontrol in Situ) have been chosen as examples. Another approach of exploiting phase diagrams for optimal material selection and for determination of growth condition before experimentation through a simple calculation is presented on InP-GaP solid solutions. Ternary phase diagrams are visualized in space through calculation and constructions based on the corresponding thermodynamic models and anaglyphs. These make it easy to observe and qualitatively analyze the crystallization of every composition. Phase diagrams can be also used as a powerful tool for the deduction of new crystallization methods. Eutectic crystallization is an example of such an approach where a modified molten-solution-zone method can give a sandwich structure with an abrupt concentration change. The concentration of a component can range from 0 to 100% in the different solid phases.

Single crystal growth of the Er2PdSi3 intermetallic compound

NASA Astrophysics Data System (ADS)

Mazilu, I.; Frontzek, M.; Löser, W.; Behr, G.; Teresiak, A.; Schultz, L.

2005-02-01

Single crystals of the Er2PdSi3 intermetallic compound melting congruently at 1648 ∘C, were grown by a floating zone method with radiation heating. The control of oxygen content was the key factor to avoid oxide precipitates, which can affect effective grain selection in the crystal growth process. Crystals grown at velocities of 5 mm/h with a preferred direction close to (1 0 0) with inclination angles of about 12 ∘ against the rod axis show very distinct facets at the rod surface. The crystals are Pd-depleted and Si-rich with respect to the nominal Er2PdSi3 stoichiometry, but exhibit inferior element segregation. Measurements on oriented single crystalline samples revealed antiferromagnetic ordering below 7 K, a magnetic easy axis parallel to the (0 0 1) axis of the AlB2-type hexagonal unit cell, and anisotropic electric properties.

High-purity silicon crystal growth investigations

NASA Technical Reports Server (NTRS)

Ciszek, T. F.; Hurd, J. L.; Schuyler, T.

1985-01-01

The study of silicon sheet material requirements for high efficiency solar cells is reported. Research continued on obtaining long lifetime single crystal float zone silicon and on understanding and reducing the mechanisms that limit the achievement of long lifetimes. The mechanisms studied are impurities, thermal history, point defects, and surface effect. The lifetime related crystallographic defects are characterized by X-ray topography and electron beam induced current.

Complex fragmentation and silicification structures in fault zones: quartz crystallization and repeated fragmentation in the Rusey fault zone (Cornwall/UK)

NASA Astrophysics Data System (ADS)

Yilmaz, Tim I.; Blenkinsop, Tom; Duschl, Florian; Kruhl, Jörn H.

2015-04-01

Silicified fault rocks typically show structures resulting from various stages of fragmentation and quartz crystallization. Both processes interact episodically and result in complex structures on various scales, which require a wide spectrum of analysis tools. Based on field and microstructural data, the spatial-temporal connection between deformation, quartz crystallization and fluid and material flow along the Rusey fault zone was investigated. The fault can be examined in detail in three dimensions on the north Cornwall coast, UK. It occurs within Carboniferous sandstones, siltstones, mudstones and slates of the Culm basin, and is likely to have had a long history. The fault rocks described here formed during the younger events, possibly due to Tertiary strike-slip reactivation. Frequent fragmentation, flow and crystallization events and their interaction led to various generations of complex-structured quartz units, among them quartz-mantled and partly silicified wall-rock fragments, microcrystalline quartz masses of different compositions and structures, and quartz vein patterns of various ages. Lobate boundaries of quartz masses indicate viscous flow. Fragments are separated by quartz infill, which contains cm-sized open pores, in which quartz crystals have pyramidal terminations. Based on frequent occurrence of feathery textures and the infill geometry, quartz crystallization from chalcedony appears likely, and an origin from silica gel is discussed. Fragmentation structures are generally fractal. This allows differentiation between various processes, such as corrosive wear, wear abrasion and hydraulic brecciation. Material transport along the brittle shear zone, and displacement of the wall-rocks, were at least partly governed by flow of mobile fluid-quartz-particle suspensions. The complex meso- to microstructures were generated by repeated processes of fragmentation, quartz precipitation and grain growth. In general, the brittle Rusey fault zone represents a zone of multiple fragmentation, fluid flow, crystallization and quartz dissolution and precipitation, and is regarded as key example of large-scale cyclic interaction of these processes. The geological evidence of interactions between processes implies that feedbacks and highly non-linear mechanical behaviour generated the complex meso- and microstructures. The fault zone rheology may also therefore have been complex.

Microgravity

NASA Image and Video Library

1992-03-12

The Advanced Automated Directional Solidification Furnace (AADSF) with the Experimental Apparatus Container (EAC) removed flew during the USMP-2 mission. During USMP-2, the AADSF was used to study the growth of mercury cadmium telluride crystals in microgravity by directional solidification, a process commonly used on earth to process metals and grow crystals. The furnace is tubular and has three independently controlled temperature zones . The sample travels from the hot zone of the furnace (1600 degrees F) where the material solidifies as it cools. The solidification region, known as the solid/liquid interface, moves from one end of the sample to the other at a controlled rate, thus the term directional solidification.

Effect of nitrogen on the growth of boron doped single crystal diamond

DOE PAGES

Karna, Sunil; Vohra, Yogesh

2013-11-18

Boron-doped single crystal diamond films were grown homoepitaxially on synthetic (100) Type Ib diamond substrates using microwave plasma assisted chemical vapor deposition. A modification in surface morphology of the film with increasing boron concentration in the plasma has been observed using atomic force microscopy. Use of nitrogen during boron doping has been found to improve the surface morphology and the growth rate of films but it lowers the electrical conductivity of the film. The Raman spectra indicated a zone center optical phonon mode along with a few additional bands at the lower wavenumber regions. The change in the peak profilemore » of the zone center optical phonon mode and its downshift were observed with the increasing boron content in the film. Furthermore, sharpening and upshift of Raman line was observed in the film that was grown in presence of nitrogen along with diborane in process gas.« less

Solar energy concentrator system for crystal growth and zone refining in space

NASA Technical Reports Server (NTRS)

Mcdermit, J. H.

1975-01-01

The technological feasibility of using solar concentrators for crystal growth and zone refining in space has been performed. Previous studies of space-deployed solar concentrators were reviewed for their applicability to materials processing and a new state-of-the-art concentrator-receiver radiation analysis was developed. The radiation analysis is in the form of a general purpose computer program. It was concluded from this effort that the technology for fabricating, orbiting and deploying large solar concentrators has been developed. It was also concluded that the technological feasibility of space processing materials in the focal region of a solar concentrator depends primarily on two factors: (1) the ability of a solar concentrator to provide sufficient thermal energy for the process and (2) the ability of a solar concentrator to provide a thermal environment that is conductive to the processes of interest. The analysis indicate that solar concentrators can satisfactorily provide both of these factors.

Phosphorus and other trace elements from secondary olivine in composite mantle xenoliths (CMX) from Cima Volcanic Field (CVF; California, USA): implications for crystal growth kinetics

NASA Astrophysics Data System (ADS)

Baziotis, Ioannis; Asimow, Paul; Ntaflos, Theodoros; Boyce, Jeremy; Koroneos, Antonios; Perugini, Diego; Liu, Yongsheng; Klemme, Stephan; Berndt, Jasper

2015-04-01

Phosphorus(P)-rich zones in olivine may reflect excess incorporation of P during rapid growth; zoning patterns may then record growth rate variations (Milman-Barris et al., 2008; Stolper et al., 2009). We report data on interior cuts of two CMX from alkali basalt flows (Mukasa & Wilshire, 1997) in the CVF with second-generation P-rich olivines. In Ci-1-196, a dark layer (~200 μm wide) between lherzolite and websterite is interpreted as a rapidly crystallized melt layer (ML), consisting of Ol+Gl+Pl+Spl+Cpx+Ap+Ilm. Glass (~15 vol%) is variable in composition (P2O5 ≤1.2 wt%, Li 8.22-20.0 ppm). Olivines in the layer have 0.03-0.62 wt% P2O5; P-rich Ol (P2O5 >0.1 wt%) are Fo85-89.3. The lowest P concentrations are consistent with equilibrium with liquid parental to Gl, but the higher concentrations are not. Li concentrations, zoned from 3.84 to 4.90 ppm (core-rim), indicate equilibrium incorporation during crystal growth from a small, evolving melt pool and preservation of this rapidly relaxing gradient. REEs are mostly consistent with equilibrium growth from liquids evolving towards the observed LREE-enriched glass. Most of the clinopyroxenes are diopsides with some augites. Apatite inclusions occur in the rim of P-rich Fo85 and in An54. In Ki-5-301, a dark-coloured area of irregular shape (~200 μm wide) is present along the contact between lherzolite and orthopyroxenite, consisting of Ol+Pl+Gl+Cpx+Spl+Ilm+Ap. It resembles a tabular dyke but is connected to melt-patches infiltrating the host rock. Widespread Glass in the layer has variable composition with two populations not related by fractional crystallization: 1) P2O5 1.02-1.09 wt% and 2) P2O51.62-2.35 wt% (a Gl inclusion in Ol has P2O5 3.57 wt% may have captured melt from the P-rich boundary layer at the interface with the rapidly growing olivine). REEs cluster in the same two groups. Li is as low as 3.66 ppm group 1 and 3-4× higher (9.64-13.3 ppm) in group 2. Olivine occurs as small idiomorphic crystals embedded in Gl and as large (~100 μm) idiomorphic to hypidiomorphic crystals with Gl and Spl inclusions; Mg# ranges from Fo74.5 (rim in contact with Gl) to Fo90.3; P2O5 reaches 3.5 wt% (in a ~Fo84 rim); Li varies from 2.80 (core) to 6.35 ppm (rim). Clinopyroxene (Wo41-43En50-54Fs5-8; P2O5 0.04-0.08 wt%; Li 3.33 ppm) is found both within the ML and as a reaction product between melt and matrix Opx. Trace element geochemistry shows possible equilibrium with ML glass for some elements, but clear disequilibrium for others. Apatite occurs as large (~100 μm) crystals in contact with Ol or Gl, as near-rim inclusions in P-rich Fo84 and as tiny prismatic crystals in Gl; REEs show slight negative Eu anomalies (Eu/Eu*=0.79-0.86) due to prior crystallization of plagioclase. High-resolution X-ray mapping of P in Ol from Ci-1-196 reveals 3-7 μm wide P-rich bands parallel to facets. P2O5 correlates negatively with Si and Mg+Fe+Ca, suggesting a substitution Mg2SiO4 + 1 /2 P2O5 →Mg1.5[]0.5PO4 + 1 /2MgO+SiO2. P-Al-rich areas may grow in minutes, whereas P-Al-poor over few weeks (Jambon et al., 1992). At such rates, dendritic growth (Welsch et al., 2014) implies that core to rim zoning may not be simple growth stratigraphy. A slight correlation between P and Al in our data implies either diffusive relaxation of Al gradients or, judging by dynamic experiments (Grant & Kohn, 2013), cooling rates >10° C/h that generate disequilibrium solute trapping of P but near-equilibrium incorporation of Al. The petrogenetic history following melt intrusion requires rapid cooling and reaction with matrix minerals and crystallization sequence Ol→Cpx→Pl→Ap→Fe-Ox→quench of Gl. P and Li concentrations set upper and lower limits on growth rates after intrusion of melt into CVF xenoliths. Early-crystallized olivine grew rapidly enough that sluggish P became over-enriched but not so fast as to over-enrich other elements. Cpx formed later either as neoblasts or reaction rims in which P was homogeneous (Baziotis et al. 2014) and growth was slower compared to Ol but fast enough to preserve the Li zoning. Li diffuses in Ol a factor of 3 faster than Mg-Fe (Qian et al., 2010) and hence sets a lower limit on time from Ol growth to eruption.

Visual observation of gas hydrates nucleation and growth at a water - organic liquid interface

NASA Astrophysics Data System (ADS)

Stoporev, Andrey S.; Semenov, Anton P.; Medvedev, Vladimir I.; Sizikov, Artem A.; Gushchin, Pavel A.; Vinokurov, Vladimir A.; Manakov, Andrey Yu.

2018-03-01

Visual observation of nucleation sites of methane and methane-ethane-propane hydrates and their further growth in water - organic liquid - gas systems with/without surfactants was carried out. Sapphire Rocking Cell RCS6 with transparent sapphire cells was used. The experiments were conducted at the supercooling ΔTsub = 20.2 °C. Decane, toluene and crude oils were used as organics. Gas hydrate nucleation occurred on water - metal - gas and water - sapphire - organic liquid three-phase contact lines. At the initial stage of growth hydrate crystals rapidly covered the water - gas or water - organics interfaces (depending on the nucleation site). Further hydrate phase accrete on cell walls (sapphire surface) and into the organics volume. At this stage, growth was accompanied by water «drawing out» from under initial hydrate film formed at water - organic interface. Apparently, it takes place due to water capillary inflow in the reaction zone. It was shown that the hydrate crystal morphology depends on the organic phase composition. In the case of water-in-decane emulsion relay hydrate crystallization was observed in the whole sample, originating most likely due to the hydrate crystal intergrowth through decane. Contacts of such crystals with adjacent water droplets result in rapid hydrate crystallization on this droplet.

Unraveling the history of complex zoned garnets from the North Motagua Mélange (Guatemala)

NASA Astrophysics Data System (ADS)

Barickman, M. H.; Martin, C.; Flores, K. E.; Harlow, G. E.; Bonnet, G.

2016-12-01

The Guatemala Suture Zone (GSZ) is situated in central Guatemala, between the North American and Caribbean plates. Two serpentinite mélanges straddle the Motagua Fault system: the North Motagua Mélange (NMM) and the South Motagua Mélange (SMM). In this study, chemically zoned garnet grains from four eclogite blocks from the NMM were analyzed by EMPA for major elements and LA-ICP-MS for trace elements to unravel the geological history of the eclogites. These eclogites typically consist of euhedral to subhedral garnets, partly retrogressed omphacite grains, and accessory minerals such as phengite and epidote as inclusions in garnet. EBSD was employed to examine apparent garnet inclusions in garnet. The garnet grains in NMM eclogites display complex chemical zonations: all grains roughly show a spessartine-rich core, an almandine-rich core and/or intermediate zone, and a pyrope and grossular-rich rim. Additionally, crystal resorption can be observed between the different zones, and the pyrope-grossular rim can display oscillatory zoning. Finally, grossular-rich zones (crystallographically syntactic) within garnet are present in all studied samples. REE and spider diagrams do not show any significant difference in the patterns of the different zones within the garnet, or indicating that the chemical environment from which each garnet zone grew was broadly the same. The lack of significant variation in LILE content indicates that a fluid influx during garnet growth is unlikely. Consequently, we interpret that garnet grains grew in a largely closed system; however, the presence of the grossular-rich zones, argues for occasional excursions into conditions when either two garnets crystallized or Ca-rich overgrowths that were largely resorbed prior to subsequent continued garnet growth.

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

NASA Astrophysics Data System (ADS)

Frazer, Laszlo; Chang, Kelvin B.; Poeppelmeier, Kenneth R.; Ketterson, John B.

2015-06-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity.

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

PubMed Central

Frazer, Laszlo; Chang, Kelvin B; Poeppelmeier, Kenneth R; Ketterson, John B

2015-01-01

Phase-pure cuprous oxide (Cu2O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity. PMID:27877798

Phosphorus zoning in olivine of Kilauea Iki lava lake, Hawaii

NASA Astrophysics Data System (ADS)

Fabbrizio, Alessandro; Beckett, John R.; Baker, Michael B.; Stolper, Edward M.

2010-05-01

Kilauea Iki lava lake was formed when the lavas of the 1959 summit eruption of Kilauea volcano ponded in Kilauea Iki pit crater, as described by [1]. The main chamber of this lake has been drilled repeatedly from 1960 to 1981 as the lake has cooled and crystallized and partial descriptions of core can be found in [2-7]. The bulk of the core consists of a gray, olivine-phyric basalt matrix [3]. Rapid diffusion of divalent cations through olivine at magmatic temperatures can delete information on early-formed zoning and thus information on early magmatic history, recorded in olivine during its growth, is often largely lost [8-11]. In the last years many studies [8-11] have shown that natural olivine, terrestrial and extraterrestrial, from several localities and rock types can preserve a complex zoning in P (sometimes associated with Cr and Al). Simple crystallization experiments conducted by [10] and [11] were able to replicate these features (i.e., sector and oscillatory zoning). Here, we describe P, Cr and Al zoning in olivine from the 1981 drilling of Kilauea Iki lava lake hole #1 (KI81-1) [6]. Kα X-ray intensity maps and major and minor element quantitative analyses were obtained using the Caltech JEOL JXA-8200 electron microprobe. We acquired P, Cr, Al, Fe and Ti X-ray maps simultaneously at 15 kV and 400 nA, a beam diameter of 1 μm, pixel spacing of 1-2 μm, and count times of 420-1500 msec/step were used depending on the dimension of the crystal. 15 kV and 40 nA with a beam diameter of 1 μm were used to collect quantitative analyses. P2O5 contents of the Iki olivines range from below detection limit to 0.30 wt%. Zoning in phosphorus, based on X-ray intensity maps, was observed in all olivines we examined. The P zoning patterns of the olivines display several styles. P shows oscillatory zoning comparable to that seen in terrestrial and extraterrestrial igneous olivines and in experimentally grown olivine [8-11]; high P regions, inside the crystals, outline low P chambers and P enriched zones were also observed; near the margins of the crystals is possible to find the presence of discontinuous sets of P-enriched bands that generally outline euhedral crystal forms; some crystals are characterized by P-enriched ghosts of relict crystals in their interior that are associated with probable undercooling and/or with an initial pulse of rapid crystal growth [8, 10]. Phenocrysts and microphenocrysts are frequently unzoned in major and minor divalent cations (Fe, Mg, Mn, Ca, Ni), but all are zoned in P. Variations in Cr and Al correlate spatially with P but are much fainter or absents, in some crystal the P-enriched bands are superimposed with small crystals of chromite (≤1 μm) aligned along the P zoning. Probably these chromites were formed by precipitation from the original Cr and Al bands. In no case was observed Ti zoning. [1] Richter D.H. et al. (1970) US Geol Surv Prof Pap 537-E, 73 p. [2] Richter D.H., Moore J.G. (1966) US Geol Surv Prof Pap 537-B, 26 p. [3] Helz R.T. (1980) Bull Volcanol 43-4, 675-701. [4] Helz R.T. et al. (1984) US Geol Surv Open File Rep 84-484, 72 p. [5] Hardee H.C. et al. (1981) Geophys Res Lett 8, 1211-1214. [6] Helz R.T., Wright T.L. (1983) US Geol Surv Open File Rep 83-326, 66 p. [7] Helz R.T. (1987) Geochem Soc Spec Pub 1, 241-258. [8] Beckett J.R. et al. (2008) LPSC abs. 1726. [9] Mccanta M.C. et al. (2008) LPSC abs. 1807. [10] Milmann-Barris M.S. et al. (2008) CMP 155, 739-765. [11] Mccanta M.C. et al. (2008) GCA 72-12, S1, A610.

First results from the PROTEIN experiment on board the International Space Station

NASA Astrophysics Data System (ADS)

Decanniere, Klaas; Potthast, Lothar; Pletser, Vladimir; Maes, Dominique; Otalora, Fermin; Gavira, Jose A.; Pati, Luis David; Lautenschlager, Peter; Bosch, Robert

On March 15 2009 Space Shuttle Discovery was launched, carrying the Process Unit of the Protein Crystallization Diagnostics Facility (PCDF) to the International Space Station. It contained the PROTEIN experiment, aiming at the in-situ observation of nucleation and crystal growth behaviour of proteins. After installation in the European Drawer Rack (EDR) and connection to the PCDF Electronics Unit, experiment runs were performed continuously for 4 months. It was the first time that protein crystallization experiments could be modified on-orbit in near real-time, based on data received on ground. The data included pseudo-dark field microscope images, interferograms, and Dynamic Light Scattering data. The Process Unit with space grown crystals was returned to ground on July 31 2009. Results for the model protein glucose isomerase (Glucy) from Streptomyces rubiginosus crystallized with ammonium sulfate will be reported concerning nucleation and the growth from Protein and Impurities Depletion Zones (PDZs). In addition, results of x-ray analyses for space-grown crystals will be given.

An examination of anticipated g-jitter on Space Station and its effects on materials processes

NASA Technical Reports Server (NTRS)

Nelson, Emily

1992-01-01

Information on anticipated g-jitter on Space Station Freedom and the effect of the jitter on materials processes is given in viewgraph form. It was concluded that g-jitter will dominate the acceleration environment; that it is a 3D multifrequency phenomenon; and that it varies dramatically in orientation. Information is given on calculated or measured sources of residual acceleration, aerodynamic drag, Shuttle acceleration measurements, the Space Station environment, tolerable g-levels as a function of frequency, directional solidification, vapor crystal growth, protein crystal growth, float zones, and liquid bridges.

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

NASA Technical Reports Server (NTRS)

Chen, Po-Shou; Wilcox, Roy C.

1990-01-01

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Crystal growth of compound semiconductors in a low-gravity environment (InGaAs crystals) (M-22)

NASA Technical Reports Server (NTRS)

Tatsumi, Masami

1993-01-01

Compound semiconductor crystals, such as gallium arsenide and indium phosphide crystals, have many interesting properties that silicon crystals lack, and they are expected to be used as materials for optic and/or electro-optic integrated devices. Generally speaking, alloy semiconductors, which consist of more than three elements, demonstrate new functions. For example, values of important parameters, such as lattice constant and emission wavelength, can be chosen independently. However, as it is easy for macroscopic and/or microscopic fluctuations of composition to occur in alloy semiconductor crystals, it is difficult to obtain crystals having homogeneous properties. Macroscopic change of composition in a crystal is caused by the segregation phenomenon. This phenomenon is due to a continuous change in the concentration of constituent elements at the solid-liquid interfacing during solidification. On Earth, attempts were made to obtain a crystal with homogeneous composition by maintaining a constant melt composition near the solid-liquid interface, through suppression of the convection flow of the melt by applying a magnetic field. However, the attempt was not completely successful. Convective flow does not occur in microgravity because the gravity in space is from four to six orders of magnitude less than that on Earth. In such a case, mass transfer in the melt is dominated by the diffusion phenomenon. So, if crystal growth is carried out at a rate that is higher than the rate of mass transfer due to this phenomenon, it is expected that crystals having a homogeneous composition will be obtained. In addition, it is also possible that microscopic composition fluctuations (striation) may disappear because microscopic fluctuations diminish in the absence of convection. We are going to grow a bulk-indium gallium arsenide (InGaAs) crystal using the gradient heating furnace (GHF) in the first material processing test (FMPT). The structure of the sample is shown where InGaAs polycrystals in a crucible are doubly sealed in two quartz tubes for safety. The GHF consists of two zones, namely, high temperature and low temperature zones, which results in a large temperature gradient at the interface. Crystal growth is performed by moving the furnace (i.e. the temperature profile) from the left to right at a definite rate. Thus, we will grow crystals both on Earth and in space under the same conditions. As previously described, it is possible to obtain good quality crystals which are homogeneous in composition both macroscopically and microscopically due to the lack of convection in space. We are planning to study the effects of convection on crystal growth from a melt by comparing and characterizing the properties of crystals grown on Earth with those grown in space.

SM50 Repeat-Polypeptides Self-Assemble into Discrete Matrix Subunits and Promote Appositional Calcium Carbonate Crystal Growth during Sea Urchin Tooth Biomineralization

PubMed Central

Mao, Yelin; Satchell, Paul G.; Luan, Xianghong; Diekwisch, Thomas G.H.

2015-01-01

The two major proteins involved in vertebrate enamel formation and echinoderm sea urchin tooth biomineralization, amelogenin and SM50, are both characterized by elongated polyproline repeat domains in the center of the macromolecule. To determine the role of polyproline repeat polypeptides in basal deuterostome biomineralization, we have mapped the localization of SM50 as it relates to crystal growth, conducted self-assembly studies of SM50 repeat polypeptides, and examined their effect on calcium carbonate and apatite crystal growth. Electron micrographs of the growth zone of Strongylocentrotus purpuratus sea urchin teeth documented a series of successive events from intravesicular mineral nucleation to mineral deposition at the interface between tooth surface and odontoblast syncytium. Using immunohistochemistry, SM50 was detected within the cytoplasm of cells associated with the developing tooth mineral, at the mineral secreting front, and adjacent to initial mineral deposits, but not in muscles and ligaments. Polypeptides derived from the SM50 polyproline alternating hexa- and hepta-peptide repeat region (SM50P6P7) formed highly discrete, donut-shaped self-assembly patterns. In calcium carbonate crystal growth studies, SM50P6P7 repeat peptides triggered the growth of expansive networks of fused calcium carbonate crystals while in apatite growth studies, SM50P6P7 peptides facilitated the growth of needle-shaped and parallel arranged crystals resembling those found in developing vertebrate enamel. In comparison, SM50P6P7 surpassed the PXX24 polypeptide repeat region derived from the vertebrate enamel protein amelogenin in its ability to promote crystal nucleation and appositional crystal growth. Together, these studies establish the SM50P6P7 polyproline repeat region as a potent regulator in the protein-guided appositional crystal growth that occurs during continuous tooth mineralization and eruption. In addition, our studies highlight the role of species-specific polyproline repeat motifs in the formation of discrete self-assembled matrices and the resulting control of mineral growth. PMID:26194158

SM50 repeat-polypeptides self-assemble into discrete matrix subunits and promote appositional calcium carbonate crystal growth during sea urchin tooth biomineralization.

PubMed

Mao, Yelin; Satchell, Paul G; Luan, Xianghong; Diekwisch, Thomas G H

2016-01-01

The two major proteins involved in vertebrate enamel formation and echinoderm sea urchin tooth biomineralization, amelogenin and SM50, are both characterized by elongated polyproline repeat domains in the center of the macromolecule. To determine the role of polyproline repeat polypeptides in basal deuterostome biomineralization, we have mapped the localization of SM50 as it relates to crystal growth, conducted self-assembly studies of SM50 repeat polypeptides, and examined their effect on calcium carbonate and apatite crystal growth. Electron micrographs of the growth zone of Strongylocentrotus purpuratus sea urchin teeth documented a series of successive events from intravesicular mineral nucleation to mineral deposition at the interface between tooth surface and odontoblast syncytium. Using immunohistochemistry, SM50 was detected within the cytoplasm of cells associated with the developing tooth mineral, at the mineral secreting front, and adjacent to initial mineral deposits, but not in muscles and ligaments. Polypeptides derived from the SM50 polyproline alternating hexa- and hepta-peptide repeat region (SM50P6P7) formed highly discrete, donut-shaped self-assembly patterns. In calcium carbonate crystal growth studies, SM50P6P7 repeat peptides triggered the growth of expansive networks of fused calcium carbonate crystals while in apatite growth studies, SM50P6P7 peptides facilitated the growth of needle-shaped and parallel arranged crystals resembling those found in developing vertebrate enamel. In comparison, SM50P6P7 surpassed the PXX24 polypeptide repeat region derived from the vertebrate enamel protein amelogenin in its ability to promote crystal nucleation and appositional crystal growth. Together, these studies establish the SM50P6P7 polyproline repeat region as a potent regulator in the protein-guided appositional crystal growth that occurs during continuous tooth mineralization and eruption. In addition, our studies highlight the role of species-specific polyproline repeat motifs in the formation of discrete self-assembled matrices and the resulting control of mineral growth. Copyright © 2015 Elsevier GmbH. All rights reserved.

Rapid assessment of crystal orientation in semi-crystalline polymer films using rotational zone annealing and impact of orientation on mechanical properties

DOE PAGES

Ye, Changhuai; Wang, Chao; Wang, Jing; ...

2017-08-17

Crystal orientation in semi-crystalline polymers tends to enhance their performance, such as increased yield strength and modulus, along the orientation direction. Zone annealing (ZA) orients the crystal lamellae through a sharp temperature gradient that effectively directs the crystal growth, but the sweep rate (V ZA) of this gradient significantly impacts the extent of crystal orientation. Here in this work, we demonstrate rotational zone annealing (RZA) as an efficient method to elucidate the influence of V ZA on the crystal morphology of thin films in a single experiment using isotactic poly(1-butene), PB-1, as a model semi-crystalline polymer. These RZA results aremore » confirmed using standard, serial linear ZA to tune the structure from an almost unidirectional oriented morphology to weakly oriented spherulites. The overall crystallinity is only modestly changed in comparison to isothermal crystallization (maximum of 55% from ZA vs. 48% for isothermal crystallization). However, the average grain size increases and the spherulites become anisotropic from ZA. Due to these structural changes, the Young's modulus of the oriented films, both parallel and perpendicular to the spherulite orientation direction, is significantly increased by ZA. The modulus does become anisotropic after ZA due to the directionality in the crystal structure, with more than a threefold increase in the modulus parallel to the orientation direction for the highest oriented film in comparison to the modulus from isothermal crystallization. Lastly, RZA enables rapid identification of conditions to maximize orientation of crystals in thin polymer films, which could find utility in determining conditions to improve crystallinity and performance in organic electronics.« less

Rapid assessment of crystal orientation in semi-crystalline polymer films using rotational zone annealing and impact of orientation on mechanical properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ye, Changhuai; Wang, Chao; Wang, Jing

Crystal orientation in semi-crystalline polymers tends to enhance their performance, such as increased yield strength and modulus, along the orientation direction. Zone annealing (ZA) orients the crystal lamellae through a sharp temperature gradient that effectively directs the crystal growth, but the sweep rate (V ZA) of this gradient significantly impacts the extent of crystal orientation. Here in this work, we demonstrate rotational zone annealing (RZA) as an efficient method to elucidate the influence of V ZA on the crystal morphology of thin films in a single experiment using isotactic poly(1-butene), PB-1, as a model semi-crystalline polymer. These RZA results aremore » confirmed using standard, serial linear ZA to tune the structure from an almost unidirectional oriented morphology to weakly oriented spherulites. The overall crystallinity is only modestly changed in comparison to isothermal crystallization (maximum of 55% from ZA vs. 48% for isothermal crystallization). However, the average grain size increases and the spherulites become anisotropic from ZA. Due to these structural changes, the Young's modulus of the oriented films, both parallel and perpendicular to the spherulite orientation direction, is significantly increased by ZA. The modulus does become anisotropic after ZA due to the directionality in the crystal structure, with more than a threefold increase in the modulus parallel to the orientation direction for the highest oriented film in comparison to the modulus from isothermal crystallization. Lastly, RZA enables rapid identification of conditions to maximize orientation of crystals in thin polymer films, which could find utility in determining conditions to improve crystallinity and performance in organic electronics.« less

Numerical analysis of impurity separation from waste salt by investigating the change of concentration at the interface during zone refining process

NASA Astrophysics Data System (ADS)

Choi, Ho-Gil; Shim, Moonsoo; Lee, Jong-Hyeon; Yi, Kyung-Woo

2017-09-01

The waste salt treatment process is required for the reuse of purified salts, and for the disposal of the fission products contained in waste salt during pyroprocessing. As an alternative to existing fission product separation methods, the horizontal zone refining process is used in this study for the purification of waste salt. In order to evaluate the purification ability of the process, three-dimensional simulation is conducted, considering heat transfer, melt flow, and mass transfer. Impurity distributions and decontamination factors are calculated as a function of the heater traverse rate, by applying a subroutine and the equilibrium segregation coefficient derived from the effective segregation coefficients. For multipass cases, 1d solutions and the effective segregation coefficient obtained from three-dimensional simulation are used. In the present study, the topic is not dealing with crystal growth, but the numerical technique used is nearly the same since the zone refining technique was just introduced in the treatment of waste salt from nuclear power industry because of its merit of simplicity and refining ability. So this study can show a new application of single crystal growth techniques to other fields, by taking advantage of the zone refining multipass possibility. The final goal is to achieve the same high degree of decontamination in the waste salt as in zone freezing (or reverse Bridgman) method.

Zeolite crystal growth in space

NASA Technical Reports Server (NTRS)

Sacco, Albert, Jr.; Thompson, Robert W.; Dixon, Anthony G.

1991-01-01

The growth of large, uniform zeolite crystals in high yield in space can have a major impact on the chemical process industry. Large zeolite crystals will be used to improve basic understanding of adsorption and catalytic mechanisms, and to make zeolite membranes. To grow large zeolites in microgravity, it is necessary to control the nucleation event and fluid motion, and to enhance nutrient transfer. Data is presented that suggests nucleation can be controlled using chemical compounds (e.g., Triethanolamine, for zeolite A), while not adversely effecting growth rate. A three-zone furnace has been designed to perform multiple syntheses concurrently. The operating range of the furnace is 295 K to 473 K. Teflon-lined autoclaves (10 ml liquid volume) have been designed to minimize contamination, reduce wall nucleation, and control mixing of pre-gel solutions on orbit. Zeolite synthesis experiments will be performed on USML-1 in 1992.

Crystal growth and near infrared optical properties of Pr 3+ doped lead halide materials for resonantly pumped eye safe laser applications

NASA Astrophysics Data System (ADS)

Jones, Ivy Krystal

In this dissertation the material development and optical spectroscopy of Pr3+ activated low phonon energy halide crystals is presented for possible applications in resonantly pumped eye-safe solid-state laser gain media. In the last twenty years, the developments in fiber and diode lasers have enabled highly efficient resonant pumping of Pr3+ doped crystals for possible lasing in the 1.6--1.7 microm region. In this work, the results of the purification, crystal growth, and near-infrared (NIR) spectroscopic characterization of Pr3+ doped lead (II) chloride, PbCl2 and lead (II) bromide, PbBr2 are presented. The investigated PbCl2 and PbBr2 crystals are non-hygroscopic with maximum phonon energies between ~180--200 cm-1, which enable efficient emission in the NIR spectral region (~ 1.6 microm) from the 3F3/3F4 → 3H4 transition of Pr3+ ions. The commercial available starting materials were purchased as ultra dry, high purity (~ 99.999 %) beads and purified through a combination of zone-refinement and halogenation. The crystal growth of Pr3+ doped PbCl 2 and PbBr2 was performed via vertical Bridgman technique using a two-zone furnace. The resulting Pr3+ doped PbCl 2 and PbBr2 crystals exhibited characteristic IR absorption bands in the 1.5--1.7 microm region (3H4 → 3F3/3F4), which allow for resonant pumping using commercial diode lasers. A broad IR emission band centered at ~1.6 microm was observed under ~1445 nm diode laser excitation from both Pr3+ doped halides. This dissertation presents comparative spectroscopic results for Pr 3+:PbCl2 and Pr3+:PbBr2 including NIR absorption and emission studies, lifetime measurements, modelling of radiative and non-radiative decay rates, determination of transition cross-section, and the net effective gain cross sections.

A case of Alzheimer's disease in magmatic crystals

NASA Astrophysics Data System (ADS)

Costa Rodriguez, F.; Bouvet de Maisonneuve, C.

2012-12-01

The reequilibration of chemical zoning in crystals from volcanic rocks is increasingly used to determine the duration of the processes involved in their origin, residence and transport. There now exist a good number of determinations of diffusion coefficients in olivine (Fe-Mg, Mn, Ca, Ni, Cr), plagioclase (CaAl-NaSi, Mg, Sr, Ba, REE), pyroxenes (Fe-Mg, Mn, Ca, REE) and quartz (Ti), but most studies have used a single element or component in a single mineral group. Although this is a good approach, it can only access a limited range of time scales, typically the short-term memory of the crystal. In other words, for process durations that are longer than the combination of the diffusivity and diffusion distance (and for a constant boundary), the long-term memory of the crystal might have been lost. This could explain why most time determinations of magmatic processes from volcanic rocks give times of about < 100 years, and why these are shorter than the thousands of years obtained from U-Th series disequilibrium isotopes. We have done a series of numerical calculations and natural observation to determine the time windows that can be accessed with different elements and minerals, and how they may affect the time scales and interpretations of processes that the crystals might be recording. We have looked at two end-members representative of mafic and silicic magmas by changing the temperature and mineral compositions. 3 dimensional calculations of diffusion reequilibration at the center of a 1 x 0.5 x 0.5 mm crystal and using a constant boundary as first case. We find that for mafic magma and olivine, 90 % of equilibration of Fe-Mg, Mn, and Ni occurs in a few decades, but gradients in Ca and Cr persist for a few thousand years. These results can for example explain the large ranges of Ca and Cr contents at a given Fe/Mg of olivine, and why apparently contradictory times can be obtained from elements with different diffusivities in the same crystal. At the same time these findings also highlight that there is a long-term memory of the crystal that is typically not accessed by current studies. However, unraveling this memory is more complex because it seems unrealistic to assume a constant composition at the boundary for hundreds or thousands of years, and because crystals can be growing and dissolving multiple times. Additional models considering growth and a variable boundary show that a significant part of the memory is lost by multiple changes in concentration being superimposed at the crystal rim. Here we also report a case where accessing the older history of the crystals might be possible by a combination of X-Ray element maps plus multiple element zoning traverses (Fe-Mg, Ca, Mn, Ni, Al, P, Cr) in olivine from Llaima volcano (Chile). Element distributions reveal that the crystals had an early history of fast growth. The delicate structures of P zoning have been used to recognize any crystal dissolution. Cr, Fe-Mg, Ni, Mn are zoned but the times obtained from Cr are 4 x longer than those of the other elements. Our interpretation is that the Cr zoning records the older memory of the crystal since eruption but that of Fe-Mg has lost part of the memory due to multiple changes at the rim or complete homogenization of the crystal. Thus using multiple elements and minerals allow accessing the long and short term memory of the crystals and associated magma.

Thermal analysis of the vertical bridgman semiconductor crystal growth technique. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Jasinski, T. J.

1982-01-01

The quality of semiconductor crystals grown by the vertical Bridgman technique is strongly influenced by the axial and radial variations of temperature within the charge. The relationship between the thermal parameters of the vertical Bridgman system and the thermal behavior of the charge are examined. Thermal models are developed which are capable of producing results expressable in analytical form and which can be used without recourse to extensive computer work for the preliminary thermal design of vertical Bridgman crystal growth systems. These models include the effects of thermal coupling between the furnace and the charge, charge translation rate, charge diameter, thickness and thermal conductivity of the confining crucible, thermal conductivity change and liberation of latent heat at the growth interface, and infinite charge length. The hot and cold zone regions, considered to be at spatially uniform temperatures, are separated by a gradient control region which provides added thermal design flexibility for controlling the temperature variations near the growth interface.

Stability and instability of thermocapillary convection in models of the float-zone crystal-growth process

NASA Technical Reports Server (NTRS)

Neitzel, G. P.

1993-01-01

This project was concerned with the determination of conditions of guaranteed stability and instability for thermocapillary convection in a model of the float-zone crystal-growth process. This model, referred to as the half-zone, was studied extensively, both experimentally and theoretically. Our own earlier research determined, using energy-stability theory, sufficient conditions for stability to axisymmetric disturbances. Nearly all results computed were for the case of a liquid with Prandtl Number Pr = 1. Attempts to compute cases for higher Prandtl numbers to allow comparison with the experimental results of other researchers were unsuccessful, but indicated that the condition guaranteeing stability against axisymmetric disturbances would be a value of the Marangoni number (Ma), significantly higher than that at which oscillatory convection was observed experimentally. Thus, additional results were needed to round out the stability picture for this model problem. The research performed under this grant consisted of the following: (1) computation of energy-stability limits for non-axisymmetric disturbances; (2) computation of linear-stability limits for axisymmetric and non-axisymmetric disturbances; (3) numerical simulation of the basic state for half- and full-zones with a deformable free surface; and (4) incorporation of radiation heat transfer into a model energy-stability problem. Each of these is summarized briefly below.

The Fe2(+)-Mg interdiffusion in orthopyroxene: Constraints from cation ordering and structural data and implications for cooling rates of meteorites

NASA Technical Reports Server (NTRS)

Ganguly, J.; Tazzoli, V.

1993-01-01

Orthopyroxene crystals in a number of meteorites exhibit compositional zoning of Fe and Mg, which provide important constraint on their cooling rates. However, attempts to model cooling rate of these crystals from Fe-Mg zoning profiles suffer from the lack of any measured or theoretically well constrained Fe-Mg interdiffusion data in OP(x) It has been assumed that Fe-Mg interdiffusion in OP(x) only slightly slower than that in olivine. The purpose of this paper is to (1) calculate the Fe-Mg fractionation, and (2) provide analytical formulation relating cooling rate to the length of the diffusion zone across the interface of the overgrowth of a mineral on itself with application to Mg diffusion profile across OP(x) growth on OP(x) in certain mesosiderites.

Travelling-solvent floating-zone growth of the dilutely Co-doped spin-ladder compound Sr14(Cu, Co)24O41

NASA Astrophysics Data System (ADS)

Bag, Rabindranath; Karmakar, Koushik; Singh, Surjeet

2017-01-01

We present here crystal growth of dilutely Co-doped spin-ladder compounds Sr14(Cu 1-x, Cox)24O41 (x = 0, 0.01, 0.03, 0.05, 0.1) using the Travelling Solvent Floating Zone (TSFZ) technique associated with an image furnace. We carried out detailed microstructure and compositional analysis. The microstructure of the frozen-in FZ revealed two bands: a lower band consisting of well-aligned single-crystalline stripes of the phase Sr14(Cu, Co)24O41 embedded in the eutectic mixture of composition SrO 18% and (Cu, Co)O 82%; and an upper band consisting of a criss-crossed pattern of these stripes. These analyses were also employed to determine the distribution coefficient of the dopants in Sr14Cu24O41. The distribution coefficient turned out to be close to 1, different from Sr2CuO3 reported previously where Co tend to accumulate in the molten zone. Direct access to the composition of the frozen-in zone eliminated any previous ambiguities associated with the composition of the peritectic point of Sr14Cu24O41; and also the eutectic point in the binary SrO-CuO phase diagram. The lattice parameters show an anisotropic variation upon Co-doping with parameters a and b increasing, c decreasing; and with an overall decrease of the unit cell volume. Magnetic susceptibility measurements were carried out on the pristine and the Co-doped crystals along the principal crystallographic axes. The spin susceptibility of the x = 0.01 crystal exhibits a strong anisotropy, which is in stark contrast with the isotropic behaviour of the pristine crystal. This anisotropy seems to arise from the intradimer exchange interaction as inferred from the anisotropy of the dimer contribution to the susceptibility of the Co-doped crystal. The Curie-tail in the magnetic susceptibility of Sr14(Cu 1-x, Cox)24O41 (x = 0, 0.01, 0.03, 0.05, 0.1) crystals (field applied parallel to the ladder) was found to scale with Co-doping - the scaling is employed to confirm a homogeneous distribution of Co in a x = 0.1 crystal boule.

Magnetic damping of thermocapillary convection in the floating-zone growth of semiconductor crystals

NASA Astrophysics Data System (ADS)

Morthland, Timothy Edward

The floating zone is one process used to grow high purity semiconductor single crystals. In the floating-zone process, a liquid bridge of molten semiconductor, or melt, is held by surface tension between the upper, melting polycrystalline feed rod and the lower, solidifying single crystal. A perfect crystal would require a quiescent melt with pure diffusion of dopants during the entire period needed to grow the crystal. However, temperature variations along the free surface of the melt lead to gradients of the temperature-dependent surface tension, driving a strong and unsteady flow in the melt, commonly labeled thermocapillary or Marangoni convection. For small temperature differences along the free surface, unsteady thermocapillary convection occurs, disrupting the diffusion controlled solidification and creating undesirable dopant concentration variations in the semiconductor single crystal. Since molten semiconductors are good electrical conductors, an externally applied, steady magnetic field can eliminate the unsteadiness in the melt and can reduce the magnitude of the residual steady motion. Crystal growers hope that a strong enough magnetic field will lead to diffusion controlled solidification, but the magnetic field strengths needed to damp the unsteady thermocapillary convection as a function of floating-zone process parameters is unknown. This research has been conducted in the area of the magnetic damping of thermocapillary convection in floating zones. Both steady and unsteady flows have been investigated. Due to the added complexities in solving Maxwells equations in these magnetohydrodynamic problems and due to the thin boundary layers in these flows, a direct numerical simulation of the fluid and heat transfer in the floating zone is virtually impossible, and it is certainly impossible to run enough simulations to search for neutral stability as a function of magnetic field strength over the entire parameter space. To circumvent these difficulties, we have used matched asymptotic expansions, linear stability theory and numerics to characterize these flows. Some fundamental aspects of the heat transfer and fluid mechanics in these magnetohydrodynamic flows are elucidated in addition to the calculation of the magnetic field strengths required to damp unsteady thermocapillary convection as a function of process parameters.

Solution synthesis of lead seeded germanium nanowires and branched nanowire networks and their application as Li-ion battery anodes

NASA Astrophysics Data System (ADS)

Flynn, Grace; Palaniappan, Kumaranand; Sheehan, Martin; Kennedy, Tadhg; Ryan, Kevin M.

2017-06-01

Herein, we report the high density growth of lead seeded germanium nanowires (NWs) and their development into branched nanowire networks suitable for application as lithium ion battery anodes. The synthesis of the NWs from lead seeds occurs simultaneously in both the liquid zone (solution-liquid-solid (SLS) growth) and solvent rich vapor zone (vapor-liquid-solid (VLS) growth) of a high boiling point solvent growth system. The reaction is sufficiently versatile to allow for the growth of NWs directly from either an evaporated catalyst layer or from pre-defined nanoparticle seeds and can be extended to allowing extensive branched nanowire formation in a secondary reaction where these seeds are coated onto existing wires. The NWs are characterized using TEM, SEM, XRD and DF-STEM. Electrochemical analysis was carried out on both the single crystal Pb-Ge NWs and the branched Pb-Ge NWs to assess their suitability for use as anodes in a Li-ion battery. Differential capacity plots show both the germanium wires and the lead seeds cycle lithium and contribute to the specific capacity that is approximately 900 mAh g-1 for the single crystal wires, rising to approximately 1100 mAh g-1 for the branched nanowire networks.

Using Garnet to Reconstruct Subduction Zone Dehydration Flux

NASA Astrophysics Data System (ADS)

Baxter, E. F.; Dragovic, B.; Samanta, L. M.; Selverstone, J.; Caddick, M. J.

2011-12-01

Coupled geodynamic-thermodynamic models make predictions about the progressive dehydration flux from subducted lithologies. However, it has been difficult to test or confirm these predictions through direct petrologic assessment of natural systems. We have developed a method that may be used to reconstruct the rate, timing, and flux of dehydration from diverse lithologies within subduction zones. Here, we summarize the fundamentals of the method and highlight data from two blueschist facies lithologies from the island of Sifnos, Greece. The data indicate that garnet growth and related dehydration from individual lithologies can be focused into relatively brief (100,000s of years) pulses. In general, most garnet forming reactions (in initially hydrous lithologies) also involve the consumption of hydrous minerals (including chlorite, biotite, chloritoid, amphibole, epidote, lawsonite) and the consequent liberation of water. Depending on the exact reaction and on the pressure and temperature vector over which the reaction occurs, the stoichiometric (i.e. molar) ratio between garnet produced and water produced can vary. If this stoichiometry can be constrained via thermodynamic and textural reaction analysis, then garnet may be used as a direct monitor of the progressive dehydration of the rock for the P-T-t span over which garnet grew. To a first order, rocks with greater modal proportion of garnet have released greater amounts of water. Modern techniques are available to directly date the span of garnet growth from single crystals larger than about 5mm diameter. Sm-Nd geochronology of chemically contoured microsampled prograde garnet growth zones from single crystals can produce constraints on garnet growth duration at better than 1 million year resolution. Integration of zoned garnet geochronology and thermodynamic reaction analysis permits reconstruction of the dehydration rate and duration from individual samples. Recent studies of contrasting lithologies on Sifnos demonstrate the utility of the method for unlocking information about natural dehydration timescales within subduction zones. A mafic blueschist sample contains large garnet crystals (up to 1.5cm) whose growth occurred very rapidly, in only hundreds of thousands of years. A quartzofeldspathic rock containing larger (up to 5cm) garnets reveals rapidly accelerating garnet growth, most of which also occurred within just a few hundred thousand years. Both samples provide evidence for rapid dehydration associated with garnet-forming reactions over brief timespans. Observed garnet modal abundances and thermodynamically modeled garnet:water production ratios indicate that approximately 0.5 to 1.0 wt% water - a significant amount - was liberated from these lithologies during the brief time spans recorded by garnet growth. Whether these dehydration pulses require a kinetic-triggering explanation or whether they can be explained either geodynamically by rapid P-T shifts or thermodynamically by passage through narrowly spaced garnet reaction isopleths remains a question for further study.

Crystal growth furnace with trap doors

DOEpatents

Sachs, Emanual M.; Mackintosh, Brian H.

1982-06-15

An improved furnace is provided for growing crystalline bodies from a melt. The improved furnace is characterized by a door assembly which is remotely controlled and is arranged so as to selectively shut off or permit communication between an access port in the furnace enclosure and a hot zone within that enclosure. The invention is especially adapted to facilitate use of crystal growing cartridges of the type disclosed in U.S. Pat. No. 4,118,197.

Crystal growth furnace with trap doors

NASA Technical Reports Server (NTRS)

Sachs, Emanual M. (Inventor); Mackintosh, Brian H. (Inventor)

1982-01-01

An improved furnace is provided for growing crystalline bodies from a melt. The improved furnace is characterized by a door assembly which is remotely controlled and is arranged so as to selectively shut off or permit communication between an access port in the furnace enclosure and a hot zone within that enclosure. The invention is especially adapted to facilitate use of crystal growing cartridges of the type disclosed in U.S. Pat. No. 4,118,197.

Large and high-quality single-crystal growth of cuprate superconductor Bi-2223 using the traveling-solvent floating-zone (TSFZ) method

NASA Astrophysics Data System (ADS)

Adachi, Shintaro; Usui, Tomohiro; Kosugi, Kenta; Sasaki, Nae; Sato, Kentaro; Fujita, Masaki; Yamada, Kazuyoshi; Fujii, Takenori; Watanabe, Takao

In high superconducting transition temperature (high-Tc) cuprates, it is empirically known that Tc increases on increasing the number of CuO2 planes in a unit cell n from 1 to 3. Bi-family cuprates are ideal for investigating the microscopic mechanism involved. However, it is difficult to grow tri-layered Bi-2223, probably owing to its narrow crystallization field. Here, we report improved crystal growth of this compound using the TSFZ method under conditions slightly different from those in an earlier report [J. Cryst. Growth 223, 175 (2001)]. A Bi-rich feed-rod composition of Bi2.2Sr1.9Ca2Cu3Oy and a slightly oxygen-reduced atmosphere (mixed gas flow of O2 (10%) and Ar (90%)) were adopted for the crystal growth. In addition, to increase the supersaturation of the melts, we applied a large temperature gradient along the solid-liquid interface by shielding a high-angle light beam using Al foil around the quartz tube. In this way, we succeeded in preparing large (2 × 2 × 0 . 05 mm3) and high-quality (almost 100% pure) Bi-2223 single crystals. Hirosaki University Grant for Exploratory Research by Young Scientists and Newly-appointed Scientists.

Influence of Containment on the Growth of Germanium-Silicon in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.; Croll, A.; Sorgenfrei, T.

2017-01-01

A series of Ge(sub 1-x)Si(sub x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and 'detached' Bridgman methods and the ground-based float zone technique. 'Detached' or 'dewetted' Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. A meniscus bridges this gap between the top of the crystal and the crucible wall. Theoretical models indicate that an important parameter governing detachment is the pressure differential across this meniscus. An experimental method has been developed to control this pressure differential in microgravity that does not require connection of the ampoule volume to external gases or changes in the temperature profile during growth. Experiments will be conducted with positive, negative or zero pressure differential across the meniscus. Characterization results of ground-based experiments, including etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction will also be described.

In Situ Determination of Thermal Profiles during Czochralski Silicon Crystal Growth by an Eddy Current Technique.

NASA Astrophysics Data System (ADS)

Choe, Kwang Su.

An eddy current testing method was developed to continuously monitor crystal growth process and determine thermal profiles in situ during Czochralski silicon crystal growth. The work was motivated by the need to improve the quality of the crystal by controlling thermal gradients and annealing history over the growth cycle. The experimental concept is to monitor intrinsic electrical conductivities of the growing crystal and deduce temperature values from them. The experiments were performed in a resistance-heated Czochralski puller with a 203 mm (8 inch) diameter crucible containing 6.5 kg melt. The silicon crystals being grown were about 80 mm in diameter and monitored by an encircling sensor operating at three different test frequencies (86, 53 and 19 kHz). A one-dimensional analytical solution was employed to translate the detected signals into electrical conductivities. In terms of experiments, the effects of changes in growth condition, which is defined by crystal and crucible rotation rates, crucible position, pull rate, and hot-zone configuration, were investigated. Under a given steady-state condition, the thermal profile was usually stable over the entire length of crystal growth. The profile shifted significantly, however, when the crucible rotation rate was kept too high. As a direct evidence to the effects of melt flow on heat transfer process, a thermal gradient minimum was observed about the crystal/crucible rotation combination of 20/-10 rpm cw. The thermal gradient reduction was still most pronounced when the pull rate or the radiant heat loss to the environment was decreased: a nearly flat axial thermal gradient was achieved when either the pull rate was halved or the height of the exposed crucible wall was effectively doubled. Under these conditions, the average axial thermal gradient along the surface of the crystal was about 4-5 ^{rm o}C/mm. Regardless of growth condition, the three-frequency data revealed radial thermal gradients much larger than what were predicted by existing theoretical models. This discrepancy seems to indicate that optical effects, which are neglected in theoretical modeling, play a major role in the internal heat transfer of the crystal.

Growth of copper-zinc and copper-magnesium particles by gas-evaporation technique

NASA Astrophysics Data System (ADS)

Ohno, T.

1984-12-01

Fine particles of Cu-Zn and Cu-Mg systems of diameter less than 500 nm were prepared by evaporating the constituent metals simultaneously from two evaporation sources in an atmosphere of argon of 10 to 30 Torr. The composition, crystal structure and habit of the alloy particles were investigated by electron microscopy. The composition of the alloy particles varied depending on the growth zone of metal smoke and almost all phases known in Cu-Zn or Cu-Mg system were found at the same time. The particles with single phase showed generally well-defined crystal habits characteristic of their crystal structures. For the particles with two phases, a fixed lattice relation between the two phases was generally recognized. The formation process of the alloy particles is discussed through these observations.

Crystal Growth and Scintillation Properties of Eu2+ doped Cs4CaI6 and Cs4SrI6

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Chakoumakos, B.; Johnson, J.; Loyd, M.; Wu, Y.; Koschan, M.; Melcher, C. L.

2018-03-01

In this work we present the crystal growth and scintillation properties of two new ternarymetal halide scintillators activated with divalent europium, Cs4CaI6 and Cs4SrI6. Single crystals of each compound were grown in evacuated quartz ampoules via the vertical Bridgman technique using a two-zone transparent furnace. Single crystal X-ray diffraction experiments showed that both crystals have a trigonal (R-3c) structure, with a density of 3.99 g/cm3 and 4.03 g/cm3. The radioluminescence and photoluminescence measurements showed typical luminescence properties due to the 5d-4f radiative transitions in Eu2+. At this early stage of development Cs4SrI6:Eu and Cs4CaI6:Eu have shown very promising scintillation properties, with light yields and energy resolutions of 62,300 ph/MeV and 3.3%, and 51,800 photons/MeV and 3.6% at 662 keV, respectively.

Convective Flow Induced by Localized Traveling Magnetic Fields

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Rose, M. Franklin (Technical Monitor)

2001-01-01

An axisymmetric traveling magnetic field induces a meridional base flow in a cylindrical zone of an electrically conducting liquid. This remotely induced flow can be conveniently controlled, in magnitude and direction, and can have benefits for crystal growth applications. In particular, it can be used to offset natural convection. For long vertical cylinders, non-uniform and localized in the propagating direction, magnetic fields are required for this purpose. Here we investigate a particular form of this field, namely that induced by a set of a few electric current coils. An order of magnitude reduction of buoyancy convection is theoretically demonstrated for a vertical Bridgman crystal growth configuration.

Two-dimensional liquid crystalline growth within a phase-field-crystal model.

PubMed

Tang, Sai; Praetorius, Simon; Backofen, Rainer; Voigt, Axel; Yu, Yan-Mei; Wang, Jincheng

2015-07-01

By using a two-dimensional phase-field-crystal (PFC) model, the liquid crystalline growth of the plastic triangular phase is simulated with emphasis on crystal shape and topological defect formation. The equilibrium shape of a plastic triangular crystal (PTC) grown from an isotropic phase is compared with that grown from a columnar or smectic-A (CSA) phase. While the shape of a PTC nucleus in the isotropic phase is almost identical to that of the classical PFC model, the shape of a PTC nucleus in CSA is affected by the orientation of stripes in the CSA phase, and irregular hexagonal, elliptical, octagonal, and rectangular shapes are obtained. Concerning the dynamics of the growth process, we analyze the topological structure of the nematic order, which starts from nucleation of +1/2 and -1/2 disclination pairs at the PTC growth front and evolves into hexagonal cells consisting of +1 vortices surrounded by six satellite -1/2 disclinations. It is found that the orientational and the positional order do not evolve simultaneously; the orientational order evolves behind the positional order, leading to a large transition zone, which can span over several lattice spacings.

METHOD FOR PREPARATION OF SPHERICAL UO$sub 4$

DOEpatents

Gregory, J.F. Jr.; Levey, R.P. Jr.

1962-06-01

A method is given for continuously precipitating ura nium peroxide in the form of spherical particles. Seed crystals are formed in a first reaction zone by introducing an acidified aqueous uranyl nitrate solution and an aqueous hydrogen peroxide solution at a ratio of 5 to 20 per cent of the stoichiometric amount required for complete precipitation. After a mean residence time of 2 to 5 minutes in the first reaction zone, the resulting mixture is introduced into a second reaction zone, together with a large excess of hydrogen peroxide solution. The resulting UO4 is rapidly separated from the mother liquor after an over-all residence time of 5 to 11 minutes. The first reaction is maintained at a temperature of 85 to 90 deg C and the second zone above 50 deg C. Additional reaction zones may be employed for further crystal growth. The UO/sub 4/ is converted to U/sub 3/O/sub 8/ or UO/sub 2/ by heating in air or hydrogen atmosphere. This method is particularly useful for the preparation of spherical UO/sub 2/ particles 10 to 25 microns in diameter. (AEC)

Growth of II-VI Solid Solutions in the Presence of a Rotating Magnetic Field

NASA Technical Reports Server (NTRS)

Gillies, D. C; Motakef, S.; Dudley, M.; Matyi, R.; Volz, H.

1999-01-01

The application of a rotating magnetic field (RMF)in the frequency range 60-400 Hz and field strength of the order of 2-8 mT to crystal growth has received increasing attention in recent years. To take full advantage of the control of fluid flow by the forces applied by the field, the liquid column must be electrically conducting. Also, the application of RMF to the directional solidification of a column of liquid can result in complete mixing in the resultant solid. Thus, the technique of RMF is suited to solvent zones and float zones where the composition of the liquid is more readily controlled. In the work we report on, numerical modeling has been applied to II-VI systems, particularly tellurium based traveling heater techniques (THM). Results for a spectrum of field strengths and acceleration levels will be presented. These show clearly the effects of competing buoyancy forces and electromagnetic stirring. Crystals of cadmium zinc telluride and mercury cadmium telluride have been grown terrestrially from a tellurium solvent zone. The effects of the RMF during these experiments will be demonstrated with micrographs showing etch pits, white beam x-ray synchrotron topographs and triple axis x-ray diffraction.

Utilizing Controlled Vibrations in a Microgravity Environment to Understand and Promote Microstructural Homogeneity During Floating-Zone Crystal Growth

NASA Technical Reports Server (NTRS)

Anilkumar, A. V.; Bhowmick, J.; Grugel, R. N.

2001-01-01

Our previous experiments with NaNO3 float-zones revealed that steady thermocapillary flow can be balanced/offset by the controlled surface streaming flow induced by end-wall vibration. In the current experiments we are examining the effects of streaming flow on steadying/stabilizing nonsteady thermocapillary flow in such zones. To this effect we have set up a controlled NaNO3 half-zone experiment, where the processing parameters, like zone dimensions and temperature gradients, can be easily varied to generate nonsteady thermocapillary flows. In the present paper we present preliminary results of our investigations into stabilizing such flows by employing endwall vibration.

Utilizing Controlled Vibrations in a Microgravity Environment to Understand and Promote Microstructural Homogeneity During Float-Zone Crystal Growth

NASA Technical Reports Server (NTRS)

Anilkumar, A. V.; Bhowmick, J.; Grugel, R. N.a

2000-01-01

Our previous experiments with NaNO3 float-zones revealed that steady thermocapillary flow can be balanced/offset by the controlled surface streaming flow induced by end-wall vibration. In the current experiments we are examining the effects of streaming flow on steadying/stabilizing nonsteady thermocapillary flow in such zones. To this effect we have set up a controlled NaNO3 half-zone experiment, where the processing parameters, like zone dimensions and temperature gradients, can be easily varied to generate nonsteady thermocapillary flows. In the present paper we present preliminary results of our investigations into stabilizing such flows by employing end-wall vibration.

3D visualization of additive occlusion and tunable full-spectrum fluorescence in calcite

PubMed Central

Green, David C.; Ihli, Johannes; Thornton, Paul D.; Holden, Mark A.; Marzec, Bartosz; Kim, Yi-Yeoun; Kulak, Alex N.; Levenstein, Mark A.; Tang, Chiu; Lynch, Christophe; Webb, Stephen E. D.; Tynan, Christopher J.; Meldrum, Fiona C.

2016-01-01

From biomineralization to synthesis, organic additives provide an effective means of controlling crystallization processes. There is growing evidence that these additives are often occluded within the crystal lattice. This promises an elegant means of creating nanocomposites and tuning physical properties. Here we use the incorporation of sulfonated fluorescent dyes to gain new understanding of additive occlusion in calcite (CaCO3), and to link morphological changes to occlusion mechanisms. We demonstrate that these additives are incorporated within specific zones, as defined by the growth conditions, and show how occlusion can govern changes in crystal shape. Fluorescence spectroscopy and lifetime imaging microscopy also show that the dyes experience unique local environments within different zones. Our strategy is then extended to simultaneously incorporate mixtures of dyes, whose fluorescence cascade creates calcite nanoparticles that fluoresce white. This offers a simple strategy for generating biocompatible and stable fluorescent nanoparticles whose output can be tuned as required. PMID:27857076

Studies of rotating liquid floating zones on Skylab IV

NASA Technical Reports Server (NTRS)

Carruthers, J. R.; Gibson, E. G.; Klett, M. G.; Facemire, B. R.

1975-01-01

Liquid zones of water, soap solution and soap foam were deployed between two aligned circular disks which were free to rotate about the zone axis in the microgravity environment of Skylab IV. Such a configuration is of interest in the containerless handling of melts for possible future space processing crystal growth experiments. Three basic types of zone surface deformation and instability were observed for these rotational conditions; axisymmetric shape changes under single disk rotation, nonaxisymmetric, whirling, C-modes for long zones with equal rotation of both disks, and capillary wave phenomena for short zones with equal rotation of both disks. The sources of these instabilities and the conditions promoting them are analyzed in detail from video tape recordings of the Skylab experiments.

Advances in crystal growth, device fabrication and characterization of thallium bromide detectors for room temperature applications

NASA Astrophysics Data System (ADS)

Datta, Amlan; Moed, Demi; Becla, Piotr; Overholt, Matthew; Motakef, Shariar

2016-10-01

Thallium bromide (TlBr) is a promising room-temperature radiation detector candidate with excellent charge transport properties. However, several critical issues need to be addressed before deployment of this material for long-term field applications can be realized. In this paper, progress made towards solving some of these challenges is discussed. The most significant factors for achieving long-term performance stability for TlBr devices include residual stress as generated during crystal growth and fabrication processes, surface conditions, and the choice of contact metal. Modifications to the commonly used traveling molten zone growth technique for TlBr crystals can significantly minimize the stresses generated by large temperature gradients near the melt-solid interface of the growing crystal. Plasma processing techniques were introduced for the first time to modify the Br-etched TlBr surfaces, which resulted in improvements to the surface conditions, and consequently the spectroscopic response of the detectors. Palladium electrodes resulted a 20-fold improvement in the room-temperature device lifetime when compared to its Br-etched Pt counterpart.

Reduction of Defects in Germanium-Silicon

NASA Technical Reports Server (NTRS)

2003-01-01

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 or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Pre-eruptive processes and timescales recorded in olivine crystals and melt inclusions from the 2007 caldera-forming eruption of Piton de la Fournaise (La Réunion Island)

NASA Astrophysics Data System (ADS)

Albert, H.; Costa Rodriguez, F.; Herrin, J. S.; Di Muro, A.; Metrich, N.

2017-12-01

Summit caldera collapse is a rare event at Piton de la Fournaise. One such event occurred in 2007 during one of the largest historic eruptions of more than 200 Mm3 of magma. Effusion of aphyric basalts initiated at the summit area in mid-February, followed by the migration of active vents in March and early April to progressively lower elevations. Collapse of a 1 km diameter summit caldera occurred on April 5th while effusion of crystal rich lava continued until May 1st. Here we investigate these events through timescales recorded in olivine crystals and their melt inclusions (MIs) using a diffusion modelling approach. Olivine crystals from the early tephra emitted just before caldera collapse and from the post caldera collapse lava display similar compositions and zoning patterns. Fo [%Fo=100*Mg/(Mg+Fe)] values range from ≈82 to ≈86 and the phenocrysts are complexly zoned including a reverse followed by normal zoning. Fo≈84 cores are surrounded by a Fo≈86 plateau. In contact with the surrounding matrix or MIs, crystals exhibit normal zoning toward values of Fo≈82-83. Phosphorus distribution revealed in 2D X-Ray maps shows complex patterns that can be interpreted as early skeletal growth likely responsible for entrapment of MIs. Diffusion modeling of Fo, Ca, and Ni reveals two distinct magma residence timescales recorded in olivine. The inner reversed-zoned profiles yield timescales of 1-2 years, while normally-zoned profiles at crystal rims and also adjacent to MIs yield timescales of only a few days. Modelling of the P zoning patterns is consistent with the 1-2 year timescales obtained from reversely-zoned profiles. H2O contents of olivine-hosted MIs range from 0.35-1.16 wt%. Selective loss of water in some MIs suggests diffusive re-equilibration between the MIs and host magma during ascent. We have applied H2O diffusion modeling to estimate timescales of water loss of a few days, consistent with the results of Fo/Ca/Ni modeling of olivine profiles. We infer that the timescales of one to two years obtained from reversely-zoned profiles and P in olivine could record residence in a long-lived intrusive body sitting below the volcano summit which was fluidized during the eruption leading to caldera collapse. Timescales of one to a few days obtained from normal zoning and water loss record magma ascent during the 2007 eruption.

LA-ICP-MS trace element mapping: insights into the crystallisation history of a metamorphic garnet population

NASA Astrophysics Data System (ADS)

George, Freya; Gaidies, Fred

2017-04-01

In comparison to our understanding of major element zoning, relatively little is known about the incorporation of trace elements into metamorphic garnet. Given their extremely slow diffusivities and sensitivity to changing mineral assemblages, the analysis of the distribution of trace elements in garnet has the potential to yield a wealth of information pertaining to interfacial attachment mechanisms during garnet crystallisation, the mobility of trace elements in both garnet and the matrix, and trace element geochronology. Due to advances in the spatial resolution and analytical precision of modern microbeam techniques, small-scale trace element variations can increasingly be documented and used to inform models of metamorphic crystallisation. Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) in particular, can be used to rapidly quantify a wide range of elemental masses as a series of laser rasters, producing large volumes of spatially constrained trace element data. In this study, we present LA-ICP-MS maps of trace element concentrations from numerous centrally-sectioned garnets representative of the crystal size-distribution of a single sample's population. The study sample originates from the garnet-grade Barrovian zone of the Lesser Himalayan Sequence in Sikkim, northeast India, and has been shown to have crystallised garnet within a single assemblage between 515 ˚C and 565˚C, with no evidence for accessory phase reaction over the duration of garnet growth. Previous models have indicated that the duration of garnet crystallisation was extremely rapid (<1 Myr), with negligible diffusional homogenisation of major divalent cations. Consequently, the trace element record likely documents the primary zonation generated during garnet growth. In spite of straightforward (i.e. concentrically-zoned) major element garnet zonation, trace elements maps are characterised by significant complexity and variability. Y and the heavy rare earth elements are strongly enriched in crystal cores, where there is overprinting of the observed internal fabric, and exhibit numerous concentric annuli towards crystal rims. Conversely, the medium rare earth elements (e.g. Gd, Eu and Sm) exhibit bowl-shaped zoning from core to rim, with no annuli, and core and rim compositions of the medium rare earth elements are the same throughout the population within crystals of differing size. Cr exhibits pronounced spiral zoning, and the average Cr content increases towards garnet rims. In all cases, spirals are centered on the geometric core of the crystals. These LA-ICP-MS maps highlight the complexity of garnet growth over a single prograde event, and indicate that there is still much to be learnt from the analysis of garnet using ever-improving analytical methods. We explore the potential causes of the variations in the distribution of trace elements in garnet, and assess how these zoning patterns may be used to refine our understanding of the intricacies of garnet crystallisation and the spatial and temporal degree of trace element equilibration during metamorphism.

Development of Advanced Multizone Facilities for Microgravity Processing

NASA Technical Reports Server (NTRS)

1998-01-01

NASA has been interested in experimental ground based study to investigate the fundamental processes involved in phase transformation processes during growth of metallic, nonmetallic and electronic materials. Solidification, vapor growth and solution growth techniques of growing crystals are of special interest because of the inherent importance of convection in the nutrient solution. Convection enhances the mass transport through the nutrient and results in faster growth rates. Availability of low gravity environment of space has provided scientists a new variable to control the extent of convection and thus isolate the diffusive phenomena for their better understanding. The thermal gradient at the liquid-solid interface is determined by the alloy characteristics, the hot zone temperature, cold zone temperature and the width of the insulating zone. The thermal profiles get established by the existing material and geometrical constraints of the experimental set up. The major effort under this research was devoted to designing a programmable furnace which can be used to obtain thermal profiles along the length of the sample as per the demands of the scientists. The furnace did not have active cooling of the zones. Only active heating and passive cooling were utilized.

Morphology and composition of spinel in Pu'u 'O'o lava (1996-1998), Kilauea volcano, Hawaii

USGS Publications Warehouse

Roeder, P.L.; Thornber, C.; Poustovetov, Alexei; Grant, A.

2003-01-01

The morphology and composition of spinel in rapidly quenched Pu'u 'O'o vent and lava tube samples are described. These samples contain glass, olivine phenocrysts (3-5 vol.%) and microphenocrysts of spinel (~0.05 vol.%). The spinel surrounded by glass occurs as idiomorphic octahedra 5-50 μm in diameter and as chains of octahedra that are oriented with respect to each other. Spinel enclosed by olivine phenocrysts is sometimes rounded and does not generally form chains. The temperature before quenching was calculated from the MgO content of the glass and ranges from 1150oC to 1180oC. The oxygen fugacity before quenching was calculated by two independent methods and the log f O2 ranged from -9.2 to -9.9 (delta QFM=-1). The spinel in the Pu'u'O'o samples has a narrow range in composition with Cr/(Cr+Al)=0.61 to 0.73 and Fe2+/(Fe2++Mg) =0.46 to 0.56. The lower the calculated temperature for the samples, the higher the average Fe2+/(Fe2++Mg), Fe3+ and Ti in the spinel. Most zoned spinel crystals decrease in Cr/(Cr+Al) from core to rim and, in the chains, the Cr/(Cr+Al) is greater in the core of larger crystals than in the core of smaller crystals. The occurrence of chains and hopper crystals and the presence of Cr/(Cr+Al) zoning from core to rim of the spinel suggest diffusion-controlled growth of the crystals. Some of the spinel crystals may have grown rapidly under the turbulent conditions of the summit reservoir and in the flowing lava, and the crystals may have remained in suspension for a considerable period. The rapid growth may have caused very local (μm) gradients of Cr in the melt ahead of the spinel crystal faces. The crystals seem to have retained the Cr/(Cr+Al) ratio that developed during the original growth of the crystal, but the Fe2+/(Fe2++Mg) ratio may have equilibrated fairly rapidly with the changing melt composition due to olivine crystallization. Six of the samples were collected on the same day at various locations along a 10-km lava tube and the calculated pre-collection temperatures of the samples show a 5oC drop with distance from the vent. The average Fe2+/(Fe2++Mg) of the spinel in these samples shows a weak positive correlation with decreasing MgO in the glass of these samples. The range in Cr2O3 (0.041-0.045 wt.%) of the glass for these six samples is too small to distinguish a consistent change along the lava tube. The spinel in the Pu'u 'O'o samples shows a zoning trend in a Cr-Al-Fe3+ diagram almost directly away from the Cr apex. This compares with a zoning trend in rapidly quenched MORB samples away from Cr coupled with decreasing Fe3+. The trend away from Cr displayed by spinel in rapidly quenched samples is in marked contrast to the trend of increasing Fe3+ shown by spinel in slowly cooled lava. 

Characterization and modeling of illite crystal particles and growth mechanisms in a zoned hydrothermal deposit, Lake City, Colorado

USGS Publications Warehouse

Bove, D.J.; Eberl, D.D.; McCarty, D.K.; Meeker, G.P.

2002-01-01

Mean thickness measurements and crystal-thickness distributions (CTDs) of illite particles vary systematically with changes in hydrothermal alteration type, fracture density, and attendant mineralization in a large acid-sulfate/Mo-porphyry hydrothermal system at Red Mountain, near Lake City, Colorado. The hydrothermal illites characterize an extensive zone of quartz-sericite-pyrite alteration beneath two deeply rooted bodies of magmatic-related, quartz-alunite altered rock. Nineteen illites from a 3000 ft vertical drill hole were analyzed by XRD using the PVP-10 intercalation method and the computer program MudMaster (Bertaut-Warren-Averbach technique). Mean crystallite thicknesses, as determined from 001 reflections, range from 5-7 nanometers (nm) at depths from 0-1700 ft, then sharply increase to 10-16 nm at depths between 1800-2100 ft, and decrease again to 4-5 nm below this level. The interval of largest particle thickness correlates strongly with the zone of most intense quartz-sericite-pyrite alteration (QSP) and attendant high-density stockwork fracturing, and with the highest concentrations of Mo within the drill core. CTD shapes for the illite particles fall into two main categories: asymptotic and lognormal. The shapes of the CTDs are dependent on conditions of illite formation. The asymptotic CTDs correspond to a nucleation and growth mechanism, whereas surface-controlled growth was the dominant mechanism for the lognormal CTDs. Lognormal CTDs coincide with major through-going fractures or stockwork zones, whereas asymptotic CTDs are present in wallrock distal to these intense fracture zones. The increase in illite particle size and the associated zone of intense QSP alteration and stockwork veining was related by proximity to the dacitic magma(s), which supplied both reactants and heat to the hydrothermal system. However, no changes in illite polytype, which in other studies reflect temperature transitions, were observed within this interval.

Glancing angle deposition of Fe triangular nanoprisms consisting of vertically-layered nanoplates

NASA Astrophysics Data System (ADS)

Li, Jianghao; Li, Liangliang; Ma, Lingwei; Zhang, Zhengjun

2016-10-01

Fe triangular nanoprisms consisting of vertically-layered nanoplates were synthesized on Si substrate by glancing angle deposition (GLAD) with an electron beam evaporation system. It was found that Fe nanoplates with a crystallographic plane index of BCC (110) were stacked vertically to form triangular nanoprisms and the axial direction of the nanoprisms, BCC <001>, was normal to the substrate. The effects of experimental parameters of GLAD on the growth and morphology of Fe nanoprisms were systematically studied. The deposition rate played an important role in the morphology of Fe nanoprisms at the same length, the deposition angle just affected the areal density of nanoprisms, and the rotation speed of substrate had little influence within the parameter range we investigated. In addition, the crystal growth mechanism of Fe nanoprisms was explained with kinetically-controlled growth mechanism and zone model theory. The driving force of crystal growth was critical to the morphology and microstructure of Fe nanoprisms deposited by GLAD. Our work introduced an oriented crystal structure into the nanomaterials deposited by GLAD, which provided a new approach to manipulate the properties and functions of nanomaterials.

The historical trend in float zone crystal diameters and power requirements for float zoned silicon crystals

NASA Technical Reports Server (NTRS)

Kramer, H. G.

1981-01-01

The power needed to zone silicon crystals by radio frequency heating was analyzed. The heat loss mechanisms are examined. Curves are presented for power as a function of crystal diameter for commercial silicon zoning.

Estimation of the growth kinetics for the cooling crystallisation of paracetamol and ethanol solutions

NASA Astrophysics Data System (ADS)

Mitchell, Niall A.; Ó'Ciardhá, Clifford T.; Frawley, Patrick J.

2011-08-01

This work details the estimation of the growth kinetics of paracetamol in ethanol solutions for cooling crystallisation processes, by means of isothermal seeded batch experiments. The growth kinetics of paracetamol crystals were evaluated in isolation, with the growth rate assumed to be size independent. Prior knowledge of the Metastable Zone Width (MSZW) was required, so that supersaturation ratios of 1.7-1.1 could be induced in solution without the occurrence of nucleation. The technique involved the utilisation of two in-situ Process Analytical Techniques (PATs), with a Focused Beam Reflectance Measurement (FBRM ®) utilised to ensure that negligible nucleation occurred and an Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) probe employed for online monitoring of solute concentration. Initial Particle Size Distributions (PSDs) were used in conjunction with desupersaturation profiles to determine the growth rate as a function of temperature and supersaturation. Furthermore, the effects of seed loading and size on the crystal growth rate were investigated. A numerical model, incorporating the population balance equation and the method of moments, was utilised to describe the crystal growth process. Experimental parameters were compared to the model simulation, with the accuracy of the model validated by means of the final product PSDs and solute concentration.

Use of Traveling Magnetic Fields to Control Melt Convection

NASA Technical Reports Server (NTRS)

Ramachandran, Narayanan; Mazuruk, Konstantin; Volz, Martin P.

2000-01-01

An axially traveling magnetic wave induces a meridional base flow in an electrically conducting molten cylindrical zone. This flow can be beneficial for crystal growth applications. In particular, it can be effectively used to stir the melt in long cylindrical columns. It can also be tailored to modify the thermal and species concentration fields in the melt and to control the interface shape of the growing crystal. The basic theory of such an application is developed and data from a preliminary mercury column experiment are presented.

Stability of Detached Solidification

NASA Technical Reports Server (NTRS)

Mazuruk, K.; Volz, M. P.; Croell, A.

2009-01-01

Bridgman crystal growth can be conducted in the so-called "detached" solidification regime, where the growing crystal is detached from the crucible wall. A small gap between the growing crystal and the crucible wall, of the order of 100 micrometers or less, can be maintained during the process. A meniscus is formed at the bottom of the melt between the crystal and crucible wall. Under proper conditions, growth can proceed without collapsing the meniscus. The meniscus shape plays a key role in stabilizing the process. Thermal and other process parameters can also affect the geometrical steady-state stability conditions of solidification. The dynamic stability theory of the shaped crystal growth process has been developed by Tatarchenko. It consists of finding a simplified autonomous set of differential equations for the radius, height, and possibly other process parameters. The problem then reduces to analyzing a system of first order linear differential equations for stability. Here we apply a modified version of this theory for a particular case of detached solidification. Approximate analytical formulas as well as accurate numerical values for the capillary stability coefficients are presented. They display an unexpected singularity as a function of pressure differential. A novel approach to study the thermal field effects on the crystal shape stability has been proposed. In essence, it rectifies the unphysical assumption of the model that utilizes a perturbation of the crystal radius along the axis as being instantaneous. It consists of introducing time delay effects into the mathematical description and leads, in general, to stability over a broader parameter range. We believe that this novel treatment can be advantageously implemented in stability analyses of other crystal growth techniques such as Czochralski and float zone methods.

Edge-defined contact heater apparatus and method for floating zone crystal growth

NASA Technical Reports Server (NTRS)

Kou, Sindo (Inventor)

1992-01-01

An apparatus for growing a monocrystalline body (30) from a polycrystalline feed rod (22) includes a heater (20) that is positioned to heat a short section of the polycrystalline rod (22) to create a molten zone (34). The heater (20) is formed to include a shaper (40) that contacts the polycrystalline rod (22) in the molten zone (34) and has a hole (46) to allow flow in the molten zone (34) between the polycrystalline rod (22) side and the monocrystalline body (30) side of the shaper. The shaper (40) has an edge (42) that defines the boundary of the cross-section of the monocrystalline body (30) that is formed as the molten material solidifies.

Mineralogical Evidence for the Palaeohydrogeological Stability of a Deep Groundwater System in Fractured Rock, in West Cumbria, Northwest England

NASA Astrophysics Data System (ADS)

Milodowski, A. E.; Gillespie, M. R.; Chenery, S. R. N.; Naden, J.; Shaw, R. P.

2014-12-01

An important requirement of the safety assessment for a geological disposal facility (GDF) for radioactive waste is to be able to demonstrate the long-term chemical stability of the groundwater system at repository depth over the long period of time during which the waste will be a hazard, typically up to one million years. Of particular concern in the UK is the potential for oxidising groundwater to penetrate to repository depth during periods of glaciation, thereby increasing the mobility of some transuranic radionuclides.Between 1990 and 1998, United Kingdom Nirex Limited carried out geological investigations into the suitability of a potential site in the Sellafield area of NW England, for a GDF for L/ILW. As part of these investigations, detailed petrological analysis of fracture mineralisation in 23 deep boreholes identified a complex sequence of mineralisation events referred to as ME1-ME9. The distribution of the ME9 calcite mineralisation correlates closely with present-day groundwater flows. The ME9 calcite has been studied in more detail to understand the evolution of the deep groundwater system. The morphology and growth zoning characteristics of the calcites reflects the groundwater chemistry. Freshwater calcites display c-axis flattened to equant crystals, and are non-ferroan and strongly zoned with Mn-rich and Mn-free bands. Deeper saline-zone calcites display c-axis elongated crystals, with high Mn:Fe and low Mn:Fe growth zones. Calcite in the transition zone between the saline and fresh groundwater display saline-type cores overgrown by freshwater-type calcite, indicating a small depression of the position of the transition zone during the growth of the calcites. Sr isotope ratios and fluid inclusion chemistry confirm a link between ME9 calcite and the present regional groundwater system. Modelling of the oxygen isotope data indicates that some growth zones in the ME9 calcite precipitated from groundwater potentially containing a significant proportion of glacially-recharged water, and that this may have reached depths of up to 1000 m. However, the chemical (REE,Fe and Mn) compositions of the ME9 calcite show that despite the potential contribution of glacially-recharged water to the deep groundwater system, conditions at repository depth (< 500 m) have continually remained reducing.

Measurement of Microscopic Growth Rates in Float-Zone Silicon Crystals

NASA Technical Reports Server (NTRS)

Dold, P.; Schweizer, M.; Benz, K. W.; Rose, M. Franklin (Technical Monitor)

2001-01-01

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.

Study of silicon crystal surface formation based on molecular dynamics simulation results

NASA Astrophysics Data System (ADS)

Barinovs, G.; Sabanskis, A.; Muiznieks, A.

2014-04-01

The equilibrium shape of <110>-oriented single crystal silicon nanowire, 8 nm in cross-section, was found from molecular dynamics simulations using LAMMPS molecular dynamics package. The calculated shape agrees well to the shape predicted from experimental observations of nanocavities in silicon crystals. By parametrization of the shape and scaling to a known value of {111} surface energy, Wulff form for solid-vapor interface was obtained. The Wulff form for solid-liquid interface was constructed using the same model of the shape as for the solid-vapor interface. The parameters describing solid-liquid interface shape were found using values of surface energies in low-index directions known from published molecular dynamics simulations. Using an experimental value of the liquid-vapor interface energy for silicon and graphical solution of Herring's equation, we constructed angular diagram showing relative equilibrium orientation of solid-liquid, liquid-vapor and solid-vapor interfaces at the triple phase line. The diagram gives quantitative predictions about growth angles for different growth directions and formation of facets on the solid-liquid and solid-vapor interfaces. The diagram can be used to describe growth ridges appearing on the crystal surface grown from a melt. Qualitative comparison to the ridges of a Float zone silicon crystal cone is given.

Composition and automated crystal orientation mapping of rapid solidification products in hypoeutectic Al-4 at.%Cu alloys

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zweiacker, K. W.; Liu, Can; Gordillo, M. A.

Rmore » apid solidification can produce metastable phases and unusual microstructure modifications in multi-component alloys during additive manufacturing or laser beam welding. Composition and phase mapping by transmission electron microscopy have been used in this paper to characterize the morphologically distinct zones developing in hypoeutectic Al-4 at.% Cu alloy after pulsed laser melting for different crystal growth rate regimes. Deviations of the compositions of the alloy phases from equilibrium predictions and unique orientation relationships between the solidification transformation products have been determined. Specifically, for the columnar growth zone at solidification rates of 0.8 m s - 1 < v < v a = 1.8 m s - 1 , two distinct orientation relationships were established between the concomitantly forming non-equilibrium phases, supersaturated α-Al solid solution and the discontinuously distributed α-Al 2Cu-based θ'-phase, which can be described as {110} θ ∥ {001} α, [001] θ ∥ [110] α and {001} θ ∥ {001} α, [100] θ ∥ [100] α. These orientation relationships permit formation of coherent interphase interfaces with low interfacial free energy. Finally, this endows a kinetic advantage to the thermodynamically less stable θ'-Al 2Cu phase relative to the more stable equilibrium θ-Al 2Cu phase during formation of the morphologically modified eutectic of the columnar growth zone grains, since repeated nucleation is required to establish the discontinuous distribution of θ'-Al 2Cu phase.« less

Composition and automated crystal orientation mapping of rapid solidification products in hypoeutectic Al-4 at.%Cu alloys

DOE PAGES

Zweiacker, K. W.; Liu, Can; Gordillo, M. A.; ...

2017-12-05

Rmore » apid solidification can produce metastable phases and unusual microstructure modifications in multi-component alloys during additive manufacturing or laser beam welding. Composition and phase mapping by transmission electron microscopy have been used in this paper to characterize the morphologically distinct zones developing in hypoeutectic Al-4 at.% Cu alloy after pulsed laser melting for different crystal growth rate regimes. Deviations of the compositions of the alloy phases from equilibrium predictions and unique orientation relationships between the solidification transformation products have been determined. Specifically, for the columnar growth zone at solidification rates of 0.8 m s - 1 < v < v a = 1.8 m s - 1 , two distinct orientation relationships were established between the concomitantly forming non-equilibrium phases, supersaturated α-Al solid solution and the discontinuously distributed α-Al 2Cu-based θ'-phase, which can be described as {110} θ ∥ {001} α, [001] θ ∥ [110] α and {001} θ ∥ {001} α, [100] θ ∥ [100] α. These orientation relationships permit formation of coherent interphase interfaces with low interfacial free energy. Finally, this endows a kinetic advantage to the thermodynamically less stable θ'-Al 2Cu phase relative to the more stable equilibrium θ-Al 2Cu phase during formation of the morphologically modified eutectic of the columnar growth zone grains, since repeated nucleation is required to establish the discontinuous distribution of θ'-Al 2Cu phase.« less

Anatomy of a metabentonite: nucleation and growth of illite crystals and their colescence into mixed-layer illite/smectite

USGS Publications Warehouse

Eberl, D.D.; Blum, A.E.; Serravezza, M.

2011-01-01

The illite layer content of mixed-layer illite/smectite (I/S) in a 2.5 m thick, zoned, metabentonite bed from Montana decreases regularly from the edges to the center of the bed. Traditional X-ray diffraction (XRD) pattern modeling using Markovian statistics indicated that this zonation results from a mixing in different proportions of smectite-rich R0 I/S and illite-rich R1 I/S, with each phase having a relatively constant illite layer content. However, a new method for modeling XRD patterns of I/S indicates that R0 and R1 I/S in these samples are not separate phases (in the mineralogical sense of the word), but that the samples are composed of illite crystals that have continuous distributions of crystal thicknesses, and of 1 nm thick smectite crystals. The shapes of these distributions indicate that the crystals were formed by simultaneous nucleation and growth. XRD patterns for R0 and R1 I/S arise by interparticle diffraction from a random stacking of the crystals, with swelling interlayers formed at interfaces between crystals from water or glycol that is sorbed on crystal surfaces. It is the thickness distributions of smectite and illite crystals (also termed fundamental particles, or Nadeau particles), rather than XRD patterns for mixed-layer I/S, that are the more reliable indicators of geologic history, because such distributions are composed of well-defined crystals that are not affected by differences in surface sorption and particle arrangements, and because their thickness distribution shapes conform to the predictions of crystal growth theory, which describes their genesis.

Linking Crystal Populations to Dynamic States: Crystal Dissolution and Growth During an Open-System Event

NASA Astrophysics Data System (ADS)

Bergantz, G. W.; Schleicher, J.; Burgisser, A.

2016-12-01

The identification of shared characteristics in zoned crystals has motivated the definition of crystal populations. These populations reflect the simultaneous transport of crystals, heat and composition during open-system events. An obstacle to interpreting the emergence of a population is the absence of a way to correlate specific dynamic conditions with the characteristic attributes of a population. By combining a boundary-layer diffusion controlled model for crystal growth/dissolution with discrete-element magma dynamics simulations of crystal-bearing magmas, the creation of populations can be simulated. We have implemented a method that decomposes the chemical potential into the thermal and compositional contributions to crystal dissolution/growth. This allows for the explicit treatment of thermal inertia and thermal-compositional decoupling as fluid circulation stirs the system during an open-system event. We have identified three distinct dynamic states producing crystal populations. They are based on the volume fraction of crystals. In a mushy system, thermal and compositional states are tightly linked as the volume involved in the mixing is constrained by the so-called mixing bowl (Bergantz et al., 2015). The mixing bowl volume is a function of the visco-plastic response of the mush and the intrusion width, not by the progressive entrainment of the new intrusion as commonly assumed. Crystal dissolution is the dominate response to input of more primitive magma. At the other endmember, under very dilute conditions, thermal and compositional conditions can become decoupled, and the in-coming magma forms a double-diffusive low-Re jet. This can allow for both dissolution and growth as crystals circulate widely into an increasingly stratified system. A middle range of crystal concentration produces a very complex feedback, as sedimenting crystals form fingers and chains that interact with the incoming magma, break-up the entrainment with chaotic stirring and add a second length scale to the mixing. It simultaneously forms a small mixing bowl in the pile of crystals sedimenting at the base. This can produce very complex populations even in a simple open-system event. Bergantz et al., 2015, Open-system dynamics and mixing in magma mushes, Nature Geosci., DOI: 10.1038/NGEO2534

HRTEM Analysis of Crystallographic Defects in CdZnTe Single Crystal

NASA Astrophysics Data System (ADS)

Yasar, Bengisu; Ergunt, Yasin; Kabukcuoglu, Merve Pinar; Parlak, Mehmet; Turan, Rasit; Kalay, Yunus Eren

2018-01-01

In recent years, CdZnTe has attracted much attention due to its superior electrical and structural properties for room-temperature operable gamma and x-ray detectors. However, CdZnTe (CZT) material has often suffered from crystallographic defects encountered during the growth and post-growth processes. The identification and structural characterization of these defects is crucial to synthesize defect-free CdZnTe single crystals. In this study, Cd0.95 Zn0.05 Te single crystals were grown using a three-zone vertical Bridgman system. The single crystallinity of the material was ensured by using x-ray diffraction measurements. High-resolution electron microscopy (HRTEM) was used to characterize the nano-scale defects on the CdZnTe matrix. The linear defects oriented along the ⟨211⟩ direction were examined by transmission electron microscopy (TEM) and the corresponding HRTEM image simulations were performed by using a quantitative scanning TEM simulation package.

Melt Flow before Crystal Seeding in Cz Si Growth with Transversal MF

NASA Astrophysics Data System (ADS)

Iizuka, Masaya; Mukaiyama, Yuji; Demina, S. E.; Kalaev, V. V.

2017-06-01

Industrial Cz growth of Si crystal of 300 mm and higher diameter usually requires DC magnetic fields (MFs) to suppress turbulence in the melt. We present 3D unsteady analysis of melt turbulent convection in an industrial Cz system coupled with the effect of the transversal MF for different argon gas flow rates for the stage before crystal seeding. We have performed detailed 2D axisymmetric modeling of global heat transfer in the whole Cz furnace. Radiative heat fluxes obtained in 2D modeling have been used in detailed 3D steady and unsteady modeling of crystallization zone. LES method is applied as a predictive approach for modeling of turbulent flow of silicon melt. We have obtained flow structure and temperature distribution in the melt, which were different from previously reported data. We have observed a well-fixed dark spike which includes low temperature melt area on the melt free surface in MF cases. These results indicates that MF and argon flow rate conditions are important to achieve stable positioning of the dark spike on the melt free surface for optimized crystal seeding without uncontrollable meltdown and single crystal structure loss.

Crystal growth and disequilibrium distribution of oxygen isotopes in an igneous Ca-Al-rich inclusion from the Allende carbonaceous chondrite

NASA Astrophysics Data System (ADS)

Kawasaki, Noriyuki; Simon, Steven B.; Grossman, Lawrence; Sakamoto, Naoya; Yurimoto, Hisayoshi

2018-01-01

TS34 is a Type B1 Ca-Al-rich inclusion (CAI) from the Allende CV3 chondrite, consisting of spinel, melilite, Ti-Al-rich clinopyroxene (fassaite) and minor anorthite in an igneous texture. Oxygen and magnesium isotopic compositions were measured by secondary ion mass spectrometry in spots of known chemical composition in all major minerals in TS34. Using the sequence of formation from dynamic crystallization experiments and from chemical compositions of melilite and fassaite, the oxygen isotopic evolution of the CAI melt was established. Oxygen isotopic compositions of the constituent minerals plot along the carbonaceous chondrite anhydrous mineral line. The spinel grains are uniformly 16O-rich (Δ17O = -22.7 ± 1.7‰, 2SD), while the melilite grains are uniformly 16O-poor (Δ17O = -2.8 ± 1.8‰) irrespective of their åkermanite content and thus their relative time of crystallization. The fassaite crystals exhibit growth zoning overprinting poorly-developed sector zoning; they generally grow from Ti-rich to Ti-poor compositions. The fassaite crystals also show continuous variations in Δ17O along the inferred directions of crystal growth, from 16O-poor (Δ17O ∼ -3‰) to 16O-rich (Δ17O ∼ -23‰), covering the full range of oxygen isotopic compositions observed in TS34. The early-crystallized 16O-poor fassaite and the melilite are in oxygen isotope equilibrium and formed simultaneously. The correlation of oxygen isotopic compositions with Ti content in the fassaite imply that the oxygen isotopic composition of the CAI melt evolved from 16O-poor to 16O-rich during fassaite crystallization, presumably due to oxygen isotope exchange with a surrounding 16O-rich nebular gas. Formation of spinel, the liquidus phase in melts of this composition, predates crystallization of all other phases, so its 16O-rich composition is a relic of an earlier stage. Anorthite exhibits oxygen isotopic compositions between Δ17O ∼ -2‰ and -9‰, within the range of those of fassaite, indicating co-crystallization of these two minerals during the earliest to intermediate stage of fassaite growth. The melilite and fassaite yield an 26Al-26Mg mineral isochron with an initial value of (26Al/27Al)0 = (5.003 ± 0.075) × 10-5, corresponding to a relative age of 0.05 ± 0.02 Myr from the canonical Al-Mg age of CAIs. These data demonstrate that both 16O-rich and 16O-poor reservoirs existed in the solar nebula at least ∼0.05 Myr after the birth of the Solar System.

Zone leveling and solution growth of complex compound semiconductors in space

NASA Technical Reports Server (NTRS)

Bachmann, K. J.

1986-01-01

A research program on complex semiconducting compounds and alloys was completed that addressed the growth of single crystals of CdSe(y)Te(1-y), Zn(x)Cd(1-x)Te, Mn(x)Cd(1-x)Te, InP(y)As(1-y) and CuInSe2 and the measurement of fundamental physico-chemical properties characterizing the above materials. The purpose of this ground based research program was to lay the foundations for further research concerning the growth of complex ternary compound semiconductors in a microgravity environment.

Identification of Gravity-Related Effects on Crystal Growth From Melts With an Immiscibility Gap

NASA Technical Reports Server (NTRS)

Kassemi, M.; Sayir, A.; Farmer, S.

1999-01-01

This work involves an experimental-numerical approach to study the effects of natural and Marangoni convections on solidification of single crystals from a silicate melt with a liquid-liquid immiscibility gap. Industrial use of crystals grown from silicate melts is becoming increasingly important in electronic, optical, and high temperature structural applications. Even the simplest silicate systems like Al203-SiO2 have had, and will continue to have, a significant role in the development of traditional and advanced ceramics. A unique feature of crystals grown from the silicate systems is their outstanding linear electro-optic properties. They also exhibit exceptionally high optical rotativity. As a result, these crystals are attractive materials for dielectric, optical, and microwave applications. Experimental work in our laboratory has indicated that directional solidification of a single crystal mullite appears to be preceded by liquid-liquid phase separation in the melt. Disruption of the immiscible state results in crystallization of a two phase structure. There is also evidence that mixing in the melt caused by density-driven convection can significantly affect the stability of the immiscible liquid layers and result in poly-crystalline growth. On earth, the immiscible state has only been observed for small diameter crystals grown in float zone systems where natural convection is almost negligible. Therefore, it is anticipated that growth of large single crystals from silicate melts would benefit from microgravity conditions because of the reduction of the natural convective mixing. The main objective of this research is to determine the effects of transport processes on the phase separation in the melt during growth of a single crystal while addressing the following issues: (1) When do the immiscible layers form and are they real?; (2) What are the main physical characteristics of the immiscible liquids?; and (3) How mixing by natural or Marangoni convection affects the stability of the phase separated melt.

The effect of growth rate on the production of Ti-enriched rims of quartz phenocrysts in the Bishop magma bodies.

NASA Astrophysics Data System (ADS)

Pamukcu, A. S.; Ghiorso, M. S.; Gualda, G. A. R.

2015-12-01

Quartz commonly displays cathodoluminescence (CL) zoning correlated with elevated Ti concentrations. This zoning has been attributed to changes in magmatic intensive variables, suggesting for example, that in the Bishop Tuff (BT) magma bodies, bright-CL rims on quartz phenocrysts grew during a late-stage eruption-triggering thermal event. Yet, these rims are not ubiquitous, discounting their origin by variation in equilibrium growth conditions. Huang & Audetat (2012) suggest that Ti contents in quartz depend strongly on growth rate. Diffusion chronometry indicates that BT bright-CL quartz rims crystallized rapidly (days-weeks) at growth rates of 10-7-10-8 m/s, while interiors grew over centennial-millennial timescales (10-11-10-13 m/s). This result is consistent with CSD analyses that suggest eruptive decompression began <1 year before eruption. We use a numerical model based on the crystal growth equation of Lasaga (1982) to test if BT bright-CL rims could have resulted from elevated syn-eruptive growth rates. Results indicate that Ti contents at the quartz-melt boundary are strongly dependent on growth rate if it exceeds ~10-9 m/s. At 10-8 m/s, enrichment of 1.5-2.5 times the initial concentration is achieved at the boundary in a time frame of days-a week. At 10-7 m/s, enrichment jumps to 4-8 times over the same period. BT quartz interiors contain ~50 ppm Ti, while bright-CL rims have ~75-100 ppm (Wark et al. 2007). Our modeling successfully reproduces these concentrations using the growth rates, and over the timescales, indicated by diffusion chronometry. It also suggests that the rims grew chiefly at a rate of ~10-8 m/s; slower rates do not produce enrichment, and faster rates result in over-enrichment, relative to that observed in natural crystals. We conclude that high-Ti, bright-CL rims on BT quartz resulted from increased growth rates due to eruptive decompression, rather than late-stage fluctuations in magmatic intensive variables, over timescales of days to weeks.

Linear-stability theory of thermocapillary convection in a model of float-zone crystal growth

NASA Technical Reports Server (NTRS)

Neitzel, G. P.; Chang, K.-T.; Jankowski, D. F.; Mittelmann, H. D.

1992-01-01

Linear-stability theory has been applied to a basic state of thermocapillary convection in a model half-zone to determine values of the Marangoni number above which instability is guaranteed. The basic state must be determined numerically since the half-zone is of finite, O(1) aspect ratio with two-dimensional flow and temperature fields. This, in turn, means that the governing equations for disturbance quantities will remain partial differential equations. The disturbance equations are treated by a staggered-grid discretization scheme. Results are presented for a variety of parameters of interest in the problem, including both terrestrial and microgravity cases.

Advantages of a Special Post-Growth THM Program for the Reduction of Inclusions in CdTe Crystals

NASA Astrophysics Data System (ADS)

Fochuk, P.; Zakharuk, Z.; Nykonyuk, Ye.; Rarenko, A.; Kolesnik, M.; Bolotnikov, A. E.; Yang, G.; James, R. B.

2016-06-01

CdTe crystals are used widely for manufacturing gamma-ray radiation sensors, and we can improve their properties if we eliminate as many as possible of their Te inclusions. In this paper, we describe our two modes of removing them; first, we used the traveling heater method for growing them, and then we applied post-growth cooling, for which we used a special slow-cooling program. Here, we placed the CdTe ingot, containing inclusions, into a quartz container, and moved a narrow heater zone along it. The molten inclusions moved together with the hot zone, and, at end of the process, they were concentrated heavily at the ingot's surface. Consequently, very few inclusions were observed in much of the CdTe ingot. Hall effect measurements showed that after such annealing the value of the carrier mobility was increased significantly, and the concentration of ionized centers was reduced. One major advantage of this treatment, compared to thermal annealing alone, is that both the inclusions and impurities are eliminated simultaneously.

Transport phenomena during vapor growth of optoelectronic material - A mercurous chloride system

NASA Technical Reports Server (NTRS)

Singh, N. B.

1990-01-01

Crystal growth velocity was measured in a mercurous chloride system in a two-zone transparent furnace as a function of the Rayleigh number by varying a/L, where a is the radius of the growth tube and L is the transport length. Growth velocity data showed different trends at low and high aspect ratio, a result that does not support the velocity-aspect ratio trend predicted by theories. The system cannot be scaled on the basis of measurements done at a low aspect ratio. Some change in fluid flow behavior occurs in the growth tube as the aspect ratio increases.

Complicated secondary textures in zircon record evolution of the host granitic rocks: Studies from Western Tauern Window and Ötztal-Stubai Crystalline Complex (Eastern Alps, Western Austria)

NASA Astrophysics Data System (ADS)

Kovaleva, Elizaveta; Harlov, Daniel; Klötzli, Urs

2017-07-01

Samples of metamorphosed and deformed granitic rocks were collected from two Alpine complexes with well-constrained metamorphic history: Western Tauern Window and Ötztal-Stubai Crystalline Complex. Zircon grains from these samples were investigated in situ by a combination of scanning electron microscope techniques, cathodoluminescence (CL) imaging and Raman spectroscopy. The aims were: to describe and interpret complicated secondary textures and microstructures in zircon; based on cross-cutting relationships between secondary microstructures, reconstruct the sequence of processes, affecting zircon crystals; link the evolution of zircon with the history of the host rocks. The results indicate that zircon in the sampled granitic rocks forms growth twins and multi-grain aggregates, which are unusual for this mineral. Moreover, various secondary textures have been found in the sampled zircon, often cross-cutting each other in a single crystal. These include: distorted oscillatory CL zoning with inner zones forming inward-penetrating, CL-bright embayments, which are the evidence of dry recrystallization via annealing/lattice recovery; CL mosaicism with no preservation of growth zoning, but abundant nano- and micro-scale pores and mineral inclusions, which are the evidence of recrystallization by coupled dissolution-reprecipitation and/or leaching; embayed zircon boundaries filled with apatite, monazite, epidote and mylonitic matrix, indicating mineral-fluid reactions resulting in zircon dissolution and fragmentation; overgrowth CL-dark rims, which contain nano-pores and point to transport and precipitation of dissolved zircon matter. We conclude that zircon in our meta-granites is sensitive to metamorphism/deformation events, and was reactive with metamorphic fluids. Additionally, we have found evidence of crystal-plastic deformation in the form of low angle boundaries and bent grain tips, which is a result of shearing and ductile deformation of the host rock. We suggest that the observed complicated secondary textures in zircon can be linked to the evolutionary stages of the host rocks such as magmatic crystallization, prograde metamorphism, peak of amphibolite-facies metamorphism, post-peak cooling and exhumation, formation of ductile shear zones and final cooling to 250 °C.

Giant magmatic water reservoirs at mid-crustal depth inferred from electrical conductivity and the growth of the continental crust

NASA Astrophysics Data System (ADS)

Laumonier, Mickael; Gaillard, Fabrice; Muir, Duncan; Blundy, Jon; Unsworth, Martyn

2017-01-01

The formation of the continental crust at subduction zones involves the differentiation of hydrous mantle-derived magmas through a combination of crystallization and crustal melting. However, understanding the mechanisms by which differentiation occurs at depth is hampered by the inaccessibility of the deep crust in active continental arcs. Here we report new high-pressure electrical conductivity and petrological experiments on hydrated andesitic melt from Uturuncu volcano on the Bolivian Altiplano. By applying our results to regional magnetotelluric data, we show that giant conductive anomalies at mid-crustal levels in several arcs are characterized by relatively low amounts of intergranular andesitic partial melts with unusually high dissolved water contents (≥8 wt.% H2O). Below Uturuncu, the Altiplano-Puna Magma Body (APMB) displays an electrical conductivity that requires high water content (up to 10 wt.%) dissolved in the melt based on crystal-liquid equilibria and melt H2O solubility experiments. Such a super-hydrous andesitic melt must constitute about 10% of the APMB, the remaining 90% being a combination of magmatic cumulates and older crustal rocks. The crustal ponding level of these andesites at around 6 kbar pressure implies that on ascent through the crust hydrous magmas reach their water saturation pressure in the mid-crust, resulting in decompression-induced crystallization that increases magma viscosity and in turn leads to preferential stalling and differentiation. Similar high conductivity features are observed beneath the Cascades volcanic arc and Taupo Volcanic Zone. This suggests that large amounts of water in super-hydrous andesitic magmas could be a common feature of active continental arcs and may illustrate a key step in the structure and growth of the continental crust. One Sentence Summary: Geophysical, laboratory conductivity and petrological experiments reveal that deep electrical conductivity anomalies beneath the Central Andes, Cascades and Taupo Volcanic Zone image the ponding of super-hydrous andesitic melts which contributes to the growth of continental crust.

Growth and characterization of LiInSe2 single crystals

NASA Astrophysics Data System (ADS)

Ma, Tianhui; Zhu, Chongqiang; Lei, Zuotao; Yang, Chunhui; Sun, Liang; Zhang, Hongchen

2015-04-01

Large and crack-free LiInSe2 single crystals were obtained by the vertical gradient freezing method with adding a temperature oscillation technology in a two-zone furnace. X-ray diffraction data showed that the pure LiInSe2 compound was synthesized. The grown crystals had different color depending on melt composition. The atomic ratios of elements of LiInSe2 crystals were obtained by an Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), and the structural formula were calculated according to the relative contents of elements. The average absorption coefficients were estimated by using average reflection indices. The absorption coefficients of the thermal annealing samples are 0.6 cm-1 at 2-3 μm. The transparent range of our LiInSe2 crystals is from 0.6 μm to 13.5 μm.

Oxidation-Assisted Crack Growth in Single-Crystal Superalloys during Fatigue with Compressive Holds

NASA Astrophysics Data System (ADS)

Lafata, M. A.; Rettberg, L. H.; He, M. Y.; Pollock, T. M.

2018-01-01

The mechanism of oxidation-assisted growth of surface cracks during fatigue with compressive holds has been studied experimentally and via a model that describes the role of oxide and substrate properties. The creep-based finite element model has been employed to examine the role of material parameters in the damage evolution in a Ni-base single-crystal superalloy René N5. Low-cycle fatigue experiments with compressive holds were conducted at 1255 K and 1366 K (982 °C and 1093 °C). Interrupted and failed specimens were characterized for crack depth and spacing, oxide thickness, and microstructural evolution. Comparison of experimental to modeled hysteresis loops indicates that transient creep drives the macroscopic stress-strain response. Crack penetration rates are strongly influenced by growth stresses in the oxide, structural evolution in the substrate, and the development of γ ^' } denuded zones. Implications for design of alloys resistant to this mode of degradation are discussed.

Growth of plutons by incremental emplacement of sheets in crystal-rich host: Evidence from Miocene intrusions of the Colorado River region, Nevada, USA

NASA Astrophysics Data System (ADS)

Miller, Calvin F.; Furbish, David J.; Walker, Barry A.; Claiborne, Lily L.; Koteas, G. Christopher; Bleick, Heather A.; Miller, Jonathan S.

2011-03-01

Growing evidence supports the notion that plutons are constructed incrementally, commonly over long periods of time, yet field evidence for the multiple injections that seem to be required is commonly sparse or absent. Timescales of up to several million years, among other arguments, indicate that the dominant volume does not remain largely molten, yet if growing plutons are constructed from rapidly solidifying increments it is unlikely that intrusive contacts would escape notice. A model wherein magma increments are emplaced into melt-bearing but crystal-rich host, rather than either solid or crystal-poor material, provides a plausible explanation for this apparent conundrum. A partially solidified intrusion undoubtedly comprises zones with contrasting melt fraction and therefore strength. Depending on whether these zones behave elastically or ductilely in response to dike emplacement, intruding magma may spread to form sheets by either of two mechanisms. If the melt-bearing host is elastic on the relevant timescale, magma spreads rather than continuing to propagate upward, where it encounters a zone of higher rigidity (higher crystal fraction). Similarly, if the dike at first ascends through rigid, melt-poor material and then encounters a zone that is weak enough (poor enough in crystals) to respond ductilely, the ascending material will also spread because the dike tip ceases to propagate as in rigid material. We propose that ascending magma is thus in essence trapped, by either mechanism, within relatively crystal-poor zones. Contacts will commonly be obscure from the start because the contrast between intruding material (crystal-poorer magma) and host (crystal-richer material) is subtle, and they may be obscured even further by subsequent destabilization of the crystal-melt framework. Field evidence and zircon zoning stratigraphy in plutons of the Colorado River region of southern Nevada support the hypothesis that emplacement of magma replenishments into a crystal-laden host is important in pluton construction. The dominant granite unit of the Spirit Mountain batholith displays only subtle internal contacts. However, ages and elemental zoning in zircons demonstrate a protracted history of almost 2 million years, major fluctuations in T and host melt chemistry, and mixing of strongly contrasting populations of magmatic zircon in single samples. We interpret this to reflect reactivation of rigid sponge and mush and entrainment of earlier-formed crystals, and we infer that this was in response to granitic replenishment. Much of the smaller Aztec Wash pluton comprises interlayered cumulate-textured quartz monzonite and mafic sheets. The latest phase of pluton emplacement is marked by numerous thick, fine-grained granite "sills" that intruded the subhorizontal quartz monzonite sheets. Contacts between granite and quartz monzonite are "soft," highly irregular on cm-dm scale with coarse xenocrysts from the quartz monzonite entrained in the fine-grained granite. We interpret the granite replenishments to have spread laterally within crystal-rich, melt-bearing quartz monzonite beneath rigid mafic sheets. In this case, clear evidence for the emplacement process is fortuitously preserved because the granite was emplaced in the waning stage of the thermal lifetime of the pluton, and because the mafic sheets enhance the strength contrast and make the geometry more visible. Similar "sills" of fine-grained granite were also preserved during the late stages of the history of the Spirit Mountain batholith.

Growth of plutons by incremental emplacement of sheets in crystal-rich host: Evidence from Miocene intrusions of the Colorado River region, Nevada, USA

USGS Publications Warehouse

Miller, C.F.; Furbish, D.J.; Walker, B.A.; Claiborne, L.L.; Koteas, G.C.; Bleick, H.A.; Miller, J.S.

2011-01-01

Growing evidence supports the notion that plutons are constructed incrementally, commonly over long periods of time, yet field evidence for the multiple injections that seem to be required is commonly sparse or absent. Timescales of up to several million years, among other arguments, indicate that the dominant volume does not remain largely molten, yet if growing plutons are constructed from rapidly solidifying increments it is unlikely that intrusive contacts would escape notice. A model wherein magma increments are emplaced into melt-bearing but crystal-rich host, rather than either solid or crystal-poor material, provides a plausible explanation for this apparent conundrum. A partially solidified intrusion undoubtedly comprises zones with contrasting melt fraction and therefore strength. Depending on whether these zones behave elastically or ductilely in response to dike emplacement, intruding magma may spread to form sheets by either of two mechanisms. If the melt-bearing host is elastic on the relevant timescale, magma spreads rather than continuing to propagate upward, where it encounters a zone of higher rigidity (higher crystal fraction). Similarly, if the dike at first ascends through rigid, melt-poor material and then encounters a zone that is weak enough (poor enough in crystals) to respond ductilely, the ascending material will also spread because the dike tip ceases to propagate as in rigid material. We propose that ascending magma is thus in essence trapped, by either mechanism, within relatively crystal-poor zones. Contacts will commonly be obscure from the start because the contrast between intruding material (crystal-poorer magma) and host (crystal-richer material) is subtle, and they may be obscured even further by subsequent destabilization of the crystal-melt framework. Field evidence and zircon zoning stratigraphy in plutons of the Colorado River region of southern Nevada support the hypothesis that emplacement of magma replenishments into a crystal-laden host is important in pluton construction. The dominant granite unit of the Spirit Mountain batholith displays only subtle internal contacts. However, ages and elemental zoning in zircons demonstrate a protracted history of almost 2 million years, major fluctuations in T and host melt chemistry, and mixing of strongly contrasting populations of magmatic zircon in single samples. We interpret this to reflect reactivation of rigid sponge and mush and entrainment of earlier-formed crystals, and we infer that this was in response to granitic replenishment. Much of the smaller Aztec Wash pluton comprises interlayered cumulate-textured quartz monzonite and mafic sheets. The latest phase of pluton emplacement is marked by numerous thick, fine-grained granite "sills" that intruded the subhorizontal quartz monzonite sheets. Contacts between granite and quartz monzonite are "soft," highly irregular on cm-dm scale with coarse xenocrysts from the quartz monzonite entrained in the fine-grained granite. We interpret the granite replenishments to have spread laterally within crystal-rich, melt-bearing quartz monzonite beneath rigid mafic sheets. In this case, clear evidence for the emplacement process is fortuitously preserved because the granite was emplaced in the waning stage of the thermal lifetime of the pluton, and because the mafic sheets enhance the strength contrast and make the geometry more visible. Similar "sills" of fine-grained granite were also preserved during the late stages of the history of the Spirit Mountain batholith. ?? 2009 Elsevier B.V.

Cross correlation of chemical profiles in minerals: Technical issues and numerical methods

NASA Astrophysics Data System (ADS)

Probst, Line; Caricchi, Luca; Gander, Martin; Wallace, Glen; Sheldrake, Tom

2017-04-01

Crystals grown in magma reservoirs and develop chemical zoning because of the lack of re-equilibration when thermodynamic conditions change. Therefore, the study of chemical zoning in minerals offers the opportunity to reconstruct the pre-eruptive conditions and the temporal evolution of magma reservoirs. We are building a quantitative method that allows the comparison between zonation patterns within minerals. The aim of this method is to identify if similar crystal have partially similar zonation patterns and thus shared a part of their growth history. Our method is based on the correlation method developed first by G. Wallace and G. Bergantz (2004). Here we present some technical issues linked to the use of a numerical method to compare crystals within their textural context in thin sections. The first issue is related to the acquisition of chemical profiles from images of thin sections (e.g. BSE or cathodoluminescence images). We present a new procedure that significantly improves both image and profile processing. A second issue is related to the random orientation of crystals in a thin section. The software we are building takes in account different orientation of crystals by applying different stretching factors to chemical profiles. Thus the automated selection of the best stretching factor is crucial for the rest of the procedure. The last point is the significance level, the threshold above which the correlation between two profiles is considered as real (and not random). This threshold must also be carefully defined and justified. All these points were studied with statistical analysis and we present results leading to a more reliable and robust method. [1] Wallace, G.S. and Bergantz, G.W., 2004. Constraints on mingling of crystal populations from off-center zoning profiles: A statistical approach. American Mineralogist, vol. 89 (1), pp. 64-73. [2] Wallace, G.S. and Bergantz, G.W., 2004. Reconciling heterogeneity in crystal zoning data: An application of shared characteristic diagrams at Chaos Crags, Lassen Volcanic Center, California. Contributions to Mineralogy and Petrology, vol. 149, pp. 98-112.

Magmatic conditions and processes in the storage zone of the 2004-2006 Mount St. Helens dacite: Chapter 31 in A volcano rekindled: the renewed eruption of Mount St. Helens, 2004-2006

USGS Publications Warehouse

Rutherford, Malcom J.; Devine, Joseph D.; Sherrod, David R.; Scott, William E.; Stauffer, Peter H.

2008-01-01

O2 values of NNO +1 log unit. Magnetite compositions suggest that the 2004-6 magma was formed by mingling of magmas less than 5-8 weeks before eruption and that the magma last equilibrated within this temperature range. The amphibole phenocryst zoning involves approximately equal amounts of a pressure-sensitive Al-Tschermak molecular substitution and a temperature-sensitive edenite substitution in one cycle of growth. Hydrothermal experiments done on the natural dacite show that crystallization of the Fe- and Al-rich amphibole end member requires pressures of 200-300 MPa at temperatures of 900°C, conditions approaching the upper temperature limit of amphibole stability. The dacitic magma crystallizes the An68 plagioclase when the pressure drops to 200 MPa at 900°C. The magma must cool at this depth to produce a complete An68-An40 plagioclase zone and a Mg-rich layer on the amphiboles before the magma is cycled back to a high pressure, when a new layer of Fe-rich amphibole is acquired. The amphibole crystallizing in the dacite experiments at less than 200 MPa is lower in aluminum than any compositions in the natural cyclically zoned phenocrysts. The outer rim on some 2004-6 amphibole phenocrysts appears to have formed in the 100-200 MPa range, as do some phenocrysts in the May 1980 dacite pumice. Plagioclase rims of An35 in the 2004-6 magmas indicate that phenocryst growth continued until the pressure decreased to 130 MPa and that ascent was slow until this depth. Magma then entered the conduit for a relatively rapid ascent to the surface as indicated by the very thin (less than 5 μm) decompression-induced rims on the amphibole phenocrysts.

Digital Control of the Czochralski Growth of Gallium Arsenide-Controller Software Reference Manual

DTIC Science & Technology

1987-07-15

possible with regard to the format of the commands. Several help menus and extensive command prompts guide the operator. The dialog between the...single-zone heater is in use.) - 4 - Kfc ^&S^^ p IS’ K: i 1. Digital Control of Czochralski GaAs Crystal Growth (2) Four tachometers which are...commands for the display of menus or auxiliary information. The scrolled portion shrinks to four lines if auxiliary data display is re- quested with the

Control of Melt Conversion Using Traveling Magnetic Fields

NASA Technical Reports Server (NTRS)

Mazurruk, Konstantin; Rose, M. Franklin (Technical Monitor)

2000-01-01

An axisymmetric traveling magnetic wave induces a meridional base flow in a cylindrical zone of an electrically conducting liquid. This remotely induced flow can be conveniently controlled, in magnitude and direction, and can have benefits for crystal growth applications. In particular, it can be used to significantly offset natural convection. Theoretical basics of this new technological method are presented.

Control of Melt Convection Using Traveling Magnetic Fields

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin

2000-01-01

An axisymmetric traveling magnetic wave induces a meridional base flow in a cylindrical zone of an electrically conducting liquid. This remotely induced flow can be conveniently controlled, in magnitude and direction, and can have benefits for crystal growth applications. In particular, it can be used to offset natural convection. Theoretical basics of this new technological method are presented.

Is Eruption Style Linked to Magma Residence Time at Kilauea Volcano? Results from Chemical Zoning in Olivine

NASA Astrophysics Data System (ADS)

Lynn, K. J.; Costa Rodriguez, F.; Shea, T.; Garcia, M. O.

2015-12-01

Kilauea is generally characterized by its modern effusive activity, but the past 2500 years were dominated by cycles of explosive and effusive eruptions lasting 100's of years (Swanson et al. 2012). These different eruption styles may reflect variable volatile contents in the source that control magma ascent rate and storage durations (e.g., Sides et al. 2014). A detailed petrological study of the dominantly explosive Keanakako'i tephras (1500-1820 CE) was undertaken to better understand the storage and transport conditions preceding high-energy eruptions. Here, we focus on preliminary results for olivine from the 1500 CE Basal Reticulite (>600 m fountain; May et al. 2015). Olivine major (Fe, Mg), minor (Mn, Ca, Ni) and trace (Li, Na, Al, P, Sc, Ti, V, Cr, Co, Zn) element traverses and 2D maps were collected for 10 crystals and reveal two major populations. The dominant population has homogeneous Fo89 and Fo87 cores with thin (3-12 μm) rims of intermediate composition (Fo87.5-88.5). Normal, reverse, and complex trace element zoning (Al, P, Ti, Cr) is prominent in these otherwise homogenous (Fo, Ni, Ca, Mn) crystals. 2D maps reveal early skeletal growth and the progressive decrease of Cr from core to rim suggests olivine and Cr-spinel crystallization, which should produce significant Fo zoning. Absence of Fo zoning could imply significant storage time in a reservoir allowing homogenization. The majority of rim compositions are out of equilibrium with adhering glass, and Fe-Mg modeling indicates that their residence within the carrier melt was of a few days. A second population consists of strongly zoned (normal and reverse) crystals with a wide range of core Fo (78 to 89) and Fo82-84 rims. Timescales from Fe-Mg zoning are up to 1 year, and may record storage histories before interaction with the carrier melt. The diversity in olivine zoning suggests at least two stages of magma mixing, and a more complex evolution for the magmas that fed the reticulite eruptions than a simple closed-system and fast transport of a volatile-rich magma from the source to the surface.

Rapid Crystallization of the Bishop Magma

NASA Astrophysics Data System (ADS)

Gualda, G. A.; Anderson, A. T.; Sutton, S. R.

2007-12-01

Substantial effort has been made to understand the longevity of rhyolitic magmas, and particular attention has been paid to the systems in the Long Valley area (California). Recent geochronological data suggest discrete magma bodies that existed for hundreds of thousands of years. Zircon crystallization ages for the Bishop Tuff span 100-200 ka, and were interpreted to reflect slow crystallization of a liquid-rich magma. Here we use the diffusional relaxation of Ti zoning in quartz to investigate the longevity of the Bishop magma. We have used such an approach to show the short timescales of crystallization of Ti-rich rims on quartz from early- erupted Bishop Tuff. We have now recognized Ti-rich cores in quartz that can be used to derive the timescales of their crystallization. We studied four samples of the early-erupted Bishop. Hand-picked crystals were mounted on glass slides and polished. Cathodoluminescence (CL) images were obtained using the electron microprobe at the University of Chicago. Ti zoning was documented using the GeoSoilEnviroCARS x-ray microprobe at the Advanced Photon Source (Argonne National Lab). Quartz crystals in all 4 samples include up to 3 Ti-bearing zones: a central core (50-100 μm in diameter, ca. 50 ppm Ti), a volumetrically predominant interior (~40 ppm Ti), and in some crystals a 50-100 μm thick rim (50 ppm Ti). Maximum estimates of core residence times were calculated using a 1D diffusion model, as the time needed to smooth an infinitely steep profile to fit the observed profile. Surprisingly, even for the largest crystals studied - ca. 2 mm in diameter - core residence times are less than 1 ka. Calculated growth rates imply that even cm-sized crystals crystallized in less than 10 ka. Crystal size distribution data show that crystals larger than 3 mm are exceedingly rare, such that the important inference is that the bulk of the crystallization of the early-erupted Bishop magma occurred in only a few thousand years. This timescale is 2 orders of magnitude smaller than the shortest durations derived from geochronology. In the current paradigm, this implies that the Bishop magma existed virtually free of crystals for 100-200 ka. Occasional recharge of the system could cause resorption of crystals. The challenge, however, is to explain how a large- volume, liquid- and volatile-rich system, was prevented from erupting for over 100 ka. The trouble is such that it puts into question the whole concept of a long-lived, liquid-rich magma body. Evidence has accumulated to show that the Bishop magma was stratified and did not convect during crystallization, the stratification was established prior to phenocryst crystallization, and crystal migration did not significantly perturb the stratification. All these are simpler to explain if liquid-rich magma only existed for a short period of time, and we estimate the time as being on the order of 1 ka. The geospeedometric timescale inferred can be reconciled with the geochronological evidence if we interpret zircon crystallization ages as reflecting episodic growth in response to waxing and waning of a mushy body, rather than continuous crystallization from liquid-rich magma in a long-lived, large-volume magma body. We speculate that only after 100-200 ka did favorable conditions emerge and allowed for the generation of a large volume of liquid-rich magma. Once such a body of magma was established, it progressed rather quickly towards eruption.

The growth of homogeneous semiconductor crystals in a centrifuge by the stabilizing influence of the Coriolis force

NASA Astrophysics Data System (ADS)

Müller, G.; Neumann, G.; Weber, W.

1992-04-01

Both experimental and numerical results on crystal growth and fluid flow studies carried out in a centrifuge are reported. It is shown that the formation of doping striations can be avoided in the vertical Bridgman and the horizontal zone melting growth of Te-doped InSb if the centrifugal acceleration is increased beyond a critical value depending on the thermal boundary conditions. Furthermore, the maximum rate for the growth of inclusion free GaSb crystals grown by the travelling heater method (THM) is increased by a factor of 10 if this method is carried out at an acceleration of 20 times earth gravity. Model experiments in the Bridgman configuration using a test cell with liquid Ga and a larger series of thermocouples are conducted by varying the thermal boundary conditions and the rotation rate of the centrifuge. A three-dimensional time dependent numerical simulation of the fluid flow under the experimental conditions was carried out using a finite difference numerical scheme. It follows clearly that the Coriolis force acting on the melt in the rotating centrifuge system significantly influences the buoyancy-driven convection with respect to the flow patterns as well as the stability. The Coriolis force causes two very different flow states (I and II), depending on whether the rotation sense of the flow is in the same or in the opposite direction to that of the centrifuge. Type I is very similar to that normally observed on earth. Type II is only observed on the centrifuge and has a very large stability range of steady convection which can be used to grow striation-free crystals. All results give excellent agreement between model experiments and numerical calculations, which finally leads to a fully satisfying explanation of the crystal growth results on our centrifuge.

Adsorption mechanisms of the nonequilibrium incorporation of admixtures in a growing crystal

NASA Astrophysics Data System (ADS)

Franke, V. D.; Punin, Yu. O.; Smetannikova, O. G.; Kenunen, D. S.

2007-12-01

The nonequilibrium partition of components between a crystal and solution is mainly controlled by impurity adsorption on the surface of the growing crystal. The specificity of adsorption on the faces of various simple forms leads to the sectorial zoning of crystals. This effect was studied experimentally for several crystallizing systems with different impurities, including isomorphous, 2d-isomorphous, and nonisomorphous, readily adsorbed impurities. In all systems, the sectorial selectivity of impurity incorporation into host crystals has been detected with partition coefficients many times higher than in the case of equilibrium partition. Specific capture of impurities by certain faces is accompanied by inhibition of their growth and modification of habit. The decrease in nonequilibrium partition coefficients with degree of oversaturation provides entrapment of impurities in the growing crystals. Thereby, the adsorption mechanism works in much the same mode for impurities of quite different nature. The behavior of partition coefficient differs drastically from impurity capturing by diffusion mechanism.

Diagenesis of Miocene siliceous shales, Temblor Range, California

USGS Publications Warehouse

Murata, K.J.; Larson, R.R.

1975-01-01

Siliceous Monterey Shale and related shales of the Temblor Range, Calif., are subdivided into three depth-controlled zones characterized by different forms of silica. These are, in descending stratigraphic order: (1) Biogenic opal zone, with remains of diatoms and other siliceous organisms, (2) diagenetic cristobalite zone, and (3) diagenetic quartz zone. Using the top of the youngest marine unit, the overlying Etchegoin Formation, as datum, the transition from biogenic opal to disordered cristobalite occurs within the Monterey Shale of Chico Martinez Creek at -730 m, and the ordered cristobalite-to-microquartz transition at about -2,030 m. Temperatures that prevailed at these transition depths while the sedimentary pile lay at the bottom of the sea are estimated at about 50° and 110°C, respectively. Diagenetic cristobalite manifests, downward through a 1,300-m interval of section, a progressive decrease in its d(101) spacing because of a gradual ordering of its internal structure through adjustments in the solid state. Diagenetic microquartz forms only from well-ordered cristobalite that provides the most appropriate concentration of dissolved silica for precipitation of microquartz. Scanning electron micrographs of the silica mineral in pores of rocks made up of disordered cristobalite show aggregates of well-formed bladed crystals, like those described from deep-sea cherts. The pore silica minerals in rocks made up of ordered cristobalite occur as dendritic growths of poorly formed stubby crystals, and the change in crystal habit could be an external expression of the internal ordering process.

Influence of calcium ions on the crystallization of sodium bicarbonate

NASA Astrophysics Data System (ADS)

Zhu, Yi; Demilie, Paul; Davoine, Perrine; Cartage, Thierry; Delplancke-Ogletree, Marie-Paule

2005-02-01

In industrial crystallization of sodium bicarbonate (sodium hydrogenocarbonate), the presence of calcium ions in solutions is unavoidable due to the production process. The understanding of the Ca 2+ role in NaHCO 3 crystallization would be helpful for improving the quality of the final products. The influence of calcium ions on NaHCO 3 crystallization was investigated in a 5-l mixed suspension mixed product removal crystallizer under controlled conditions. A density meter was used for continuous supersaturation monitoring. After a steady state had been reached, different CaCl 2 amounts were added at a constant flow rate. It was found that limited calcium ion levels in the system reduce drastically the nucleation frequency of NaHCO 3 and has a limited influence on crystal growth rate. The supersaturation measurements and other methods confirmed this phenomenon. The relationship between the Ca 2+ influence on NaHCO 3 crystallization, the calcium carbonate solubility and its metastable zone in concentrated NaHCO 3 solution was established. In fact, Ca 2+ has a maximum effect on NaHCO 3 crystallization kinetics when the saturation of calcium carbonate in NaHCO 3 solution has been reached, and the effect is constant in the metastable zone. The excess of Ca 2+ precipitates in NaHCO 3 solution as CaCO 3, as observed by energy dispersive X-ray and X-ray diffraction. This explained why an increasing Ca 2+ concentration in the solution has a limited influence on NaHCO 3 crystal size distribution and habit, but decreases the crystal purity. It is also confirmed that an impurity as Ca 2+ has no influence on the equilibrium NaHCO 3-Na 2CO 3.

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

DOE PAGES

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

2017-10-26

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

Clinopyroxene Diffusion Chronometry of the Scaup Lake Rhyolite, Yellowstone Caldera, WY

NASA Astrophysics Data System (ADS)

Brugman, K. K.; Till, C. B.; Bose, M.

2016-12-01

Eruption of the Scaup Lake flow (SCL) ended 220,000 years of dormancy and began the youngest sequence of eruptions at Yellowstone caldera [Christiansen et al., USGS, 2007]. Quantification of the time intervals between magmatic events and eruption recorded in SCL is critical to interpreting signs of unrest at modern-day Yellowstone. SCL rhyolite includes zoned phenocrysts and accessory phases that indicate multiple rejuvenation events occurred shortly before eruption; previous studies focused on feldspar and zircon crystal records [e.g. Bindeman et al., J.Pet, 2008; Till et al., Geology, 2015]. Here we exploit zoned clinopyroxene (cpx)—one of the earliest-crystalized minerals in SCL as indicated by petrographic relationships—as a diffusion dating tool and utilize elements with different diffusivities to more precisely resolve rejuvenation-eruption timescales. Using NanoSIMS concentration profiles with 300-900 nanometer spacing, we employ the slower-diffusing REE Ce as a proxy for the initial profile shape of faster-diffusing Fe to calculate diffusive timescales. The outermost resolvable zone boundary in SCL cpx yields a rejuvenation-eruption timescale of 166 ± 80 yrs (1 SD). In comparison, modeling relaxation of Fe from a step function initial condition at the same temperature (920°C) yields a less precise timescale of 488 +9000 -300 yrs. Examination of our results, in concert with observed petrographic relationships, indicates SCL cpx may record an older, separate rejuvenation event than those recorded in feldspar rims at < 10 months and 10-40 years prior to eruption [Till et al., Geology, 2015]. The difference in the youngest recorded event between feldspar and cpx may be due to different crystallization intervals for these phases and/or slower crystal growth rates for cpx relative to feldspar. Our diffusion modeling results reinforce that intracrystalline zoning timescales modeled using a step function initial condition should be considered maxima, especially in viscous rhyolitic magmas, and that different phases may not record the same series of pre-eruptive events due to differences in crystallization behavior.

A strategic approach to physico-chemical analysis of bis (thiourea) lead chloride - A reliable semi-organic nonlinear optical crystal

NASA Astrophysics Data System (ADS)

Rajagopalan, N. R.; Krishnamoorthy, P.; Jayamoorthy, K.

2017-03-01

Good quality crystals of bis thiourea lead chloride (BTLC) have been grown by slow evaporation method from aqueous solution. Orthorhombic structure and Pna21 space group of the crystals have been identified by single crystal X-ray diffraction. Studies on nucleation kinetics of grown BTLC has been carried out from which meta-stable zone width, induction period, free energy change, critical radius, critical number and growth rate have been calculated. The experimental values of interfacial surface energy for the crystal growth process have been compared with theoretical models. Ultra violet transmittance studies resulted in a high transmittance and wide band gap energy suggested the required optical transparency of the crystal. The second harmonic generation (SHG) and phase matching nature of the crystal have been justified by Kurtz-Perry method. The SHG nature of the crystal has been further attested by the higher values of theoretical hyper polarizability. The dielectric nature of the crystals at different temperatures with varying frequencies has been thoroughly studied. The activation energy values of the electrical process have been calculated from ac conductivity study. Solid state parameters including valence electron plasma energy, Penn gap, Fermi energy and polarisability have been unveiled by theoretical approach and correlated with the crystal's SHG efficiency. The values of hardness number, elastic stiffness constant, Meyer's Index, minimum level of indentation load, load dependent constant, fracture toughness, brittleness index and corrected hardness obtained from Vicker's hardness test clearly showed that the BTLC crystal has good mechanical stability required for NLO device fabrication.

Impurity effects in crystal growth from solutions: Steady states, transients and step bunch motion

NASA Astrophysics Data System (ADS)

Ranganathan, Madhav; Weeks, John D.

2014-05-01

We analyze a recently formulated model in which adsorbed impurities impede the motion of steps in crystals grown from solutions, while moving steps can remove or deactivate adjacent impurities. In this model, the chemical potential change of an atom on incorporation/desorption to/from a step is calculated for different step configurations and used in the dynamical simulation of step motion. The crucial difference between solution growth and vapor growth is related to the dependence of the driving force for growth of the main component on the size of the terrace in front of the step. This model has features resembling experiments in solution growth, which yields a dead zone with essentially no growth at low supersaturation and the motion of large coherent step bunches at larger supersaturation. The transient behavior shows a regime wherein steps bunch together and move coherently as the bunch size increases. The behavior at large line tension is reminiscent of the kink-poisoning mechanism of impurities observed in calcite growth. Our model unifies different impurity models and gives a picture of nonequilibrium dynamics that includes both steady states and time dependent behavior and shows similarities with models of disordered systems and the pinning/depinning transition.

On the protein crystal formation as an interface-controlled process with prototype ion-channeling effect.

PubMed

Siódmiak, Jacek; Uher, Jan J; Santamaría-Holek, Ivan; Kruszewska, Natalia; Gadomski, Adam

2007-08-01

A superdiffusive random-walk action in the depletion zone around a growing protein crystal is considered. It stands for a dynamic boundary condition of the growth process and competes steadily with a quasistatic, curvature-involving (thermodynamic) free boundary condition, both of them contributing to interpret the (mainly late-stage) growth process in terms of a prototype ion-channeling effect. An overall diffusion function contains quantitative signatures of both boundary conditions mentioned and indicates whether the new phase grows as an orderly phase or a converse scenario occurs. This situation can be treated in a quite versatile way both numerically and analytically, within a generalized Smoluchowski framework. This study can help in (1) elucidating some dynamic puzzles of a complex crystal formation vs biomolecular aggregation, also those concerning ion-channel formation, and (2) seeing how ion-channel-type dynamics of non-Markovian nature may set properly the pace of model (dis)ordered protein aggregation.

High-Precision Temperature Control of a Crystal Growth Furnace at 1,500 C

NASA Technical Reports Server (NTRS)

Stenzel, Ch.; Hess, A.; Croell, A.; Breuer, D.; Sauermann, H.

2012-01-01

For crystal growth of semiconductor materials a short-term temperature stability of 0.1 C at 1500 C is one of the essential parameters to be addressed for achieving high-quality crystals. Hence, for temperature monitoring and control with high precision in a floating zone furnace two sets of thermo-sensors, type B thermocouples and optical fibre thermometers, have been implemented and successfully operated in the furnace for more than 2000 h. The optical fibre thermometers consist of an optical system made of sapphire (two fibres plus a prism in between for deflection) and transmit the infra-red radiation of the heater to the outside of the hot core of the furnace for pyrometric temperature measurement. A dedicated control algorithm has been set up which controlled the power settings to the individual heaters. Both sensor types showed no degradation after this period and yielded a short-term stability at 1200 C of 0.05 C (optical fibre thermometers), respectively 0.08 C (thermocouples).

On The Importance of Connecting Laboratory Measurements of Ice Crystal Growth with Model Parameterizations: Predicting Ice Particle Properties

NASA Astrophysics Data System (ADS)

Harrington, J. Y.

2017-12-01

Parameterizing the growth of ice particles in numerical models is at an interesting cross-roads. Most parameterizations developed in the past, including some that I have developed, parse model ice into numerous categories based primarily on the growth mode of the particle. Models routinely possess smaller ice, snow crystals, aggregates, graupel, and hail. The snow and ice categories in some models are further split into subcategories to account for the various shapes of ice. There has been a relatively recent shift towards a new class of microphysical models that predict the properties of ice particles instead of using multiple categories and subcategories. Particle property models predict the physical characteristics of ice, such as aspect ratio, maximum dimension, effective density, rime density, effective area, and so forth. These models are attractive in the sense that particle characteristics evolve naturally in time and space without the need for numerous (and somewhat artificial) transitions among pre-defined classes. However, particle property models often require fundamental parameters that are typically derived from laboratory measurements. For instance, the evolution of particle shape during vapor depositional growth requires knowledge of the growth efficiencies for the various axis of the crystals, which in turn depends on surface parameters that can only be determined in the laboratory. The evolution of particle shapes and density during riming, aggregation, and melting require data on the redistribution of mass across a crystals axis as that crystal collects water drops, ice crystals, or melts. Predicting the evolution of particle properties based on laboratory-determined parameters has a substantial influence on the evolution of some cloud systems. Radiatively-driven cirrus clouds show a broader range of competition between heterogeneous nucleation and homogeneous freezing when ice crystal properties are predicted. Even strongly convective squall lines show a substantial influence to predicted particle properties: The more natural evolution of ice crystals during riming produces graupel-like particles with size and fall-speeds required for the formation of a classic transition zone and extended stratiform precipitation region.

Microstructure and Low-Temperature Mechanical Properties of 304 Stainless Steel Joints by PAW + GTAW Combined Welding

NASA Astrophysics Data System (ADS)

Liu, Kun; Li, Yajiang; Wang, Juan

2016-10-01

The combined double-pass process of plasma arc welding (PAW) + gas tungsten arc welding (GTAW) was performed on 304 austenitic stainless steel with the thickness of 12 mm. Results indicated that two different morphologies of ferrite (e.g., lathy δ-ferrite and skeletal δ-ferrite) were formed within the austenite matrix in PAW weld metal (PAW-WM). GTAW weld metal (GTAW-WM) was mainly composed of fine austenite and skeletal δ-ferrite. In transition zone between PAW-WM and GTAW-WM, epitaxial growth contributed to cellular dendritic crystals transforming into columnar crystals. The tensile strength of joint is about 700 MPa. The impact toughness of WM varied from 281 J (20 °C) to 122 (-196 °C), while the impact toughness of heat-affected zone (HAZ) varied from 205 J (20 °C) to 112 J (-196 °C).

The Year Leading to a Supereruption.

PubMed

Gualda, Guilherme A R; Sutton, Stephen R

2016-01-01

Supereruptions catastrophically eject 100s-1000s of km3 of magma to the surface in a matter of days to a few months. In this study, we use zoning in quartz crystals from the Bishop Tuff (California) to assess the timescales over which a giant magma body transitions from relatively quiescent, pre-eruptive crystallization to rapid decompression and eruption. Quartz crystals in the Bishop Tuff have distinctive rims (<200 μm thick), which are Ti-rich and bright in cathodoluminescence (CL) images, and which can be used to calculate Ti diffusional relaxation times. We use synchrotron-based x-ray microfluorescence to obtain quantitative Ti maps and profiles along rim-interior contacts in quartz at resolutions of 1-5 μm in each linear dimension. We perform CL imaging on a scanning electron microscope (SEM) using a low-energy (5 kV) incident beam to characterize these contacts in high resolution (<1 μm in linear dimensions). Quartz growth times were determined using a 1D model for Ti diffusion, assuming initial step functions. Minimum quartz growth rates were calculated using these calculated growth times and measured rim thicknesses. Maximum rim growth times span from ~1 min to 35 years, with a median of ~4 days. More than 70% of rim growth times are less than 1 year, showing that quartz rims have mostly grown in the days to months prior to eruption. Minimum growth rates show distinct modes between 10-8 and 10-10 m/s (depending on sample), revealing very fast crystal growth rates (100s of nm to 10s of μm per day). Our data show that quartz rims grew well within a year of eruption, with most of the growth happening in the weeks or days preceding eruption. Growth took place under conditions of high supersaturation, suggesting that rim growth marks the onset of decompression and the transition from pre-eruptive to syn-eruptive conditions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gualda, Guilherme A. R.; Sutton, Stephen R.

Supereruptions catastrophically eject 100s-1000s of km 3 of magma to the surface in a matter of days to a few months. In this study, we use zoning in quartz crystals from the Bishop Tuff (California) to assess the timescales over which a giant magma body transitions from relatively quiescent, pre-eruptive crystallization to rapid decompression and eruption. Quartz crystals in the Bishop Tuff have distinctive rims (<200 μm thick), which are Ti-rich and bright in cathodoluminescence (CL) images, and which can be used to calculate Ti diffusional relaxation times. We use synchrotron-based x-ray microfluorescence to obtain quantitative Ti maps and profilesmore » along rim-interior contacts in quartz at resolutions of 1–5 μm in each linear dimension. We perform CL imaging on a scanning electron microscope (SEM) using a low-energy (5 kV) incident beam to characterize these contacts in high resolution (<1 μm in linear dimensions). Quartz growth times were determined using a 1D model for Ti diffusion, assuming initial step functions. Minimum quartz growth rates were calculated using these calculated growth times and measured rim thicknesses. Maximum rim growth times span from ~1 min to 35 years, with a median of ~4 days. More than 70% of rim growth times are less than 1 year, showing that quartz rims have mostly grown in the days to months prior to eruption. Minimum growth rates show distinct modes between 10 -8 and 10 -10 m/s (depending on sample), revealing very fast crystal growth rates (100s of nm to 10s of μm per day). Our data show that quartz rims grew well within a year of eruption, with most of the growth happening in the weeks or days preceding eruption. Growth took place under conditions of high supersaturation, suggesting that rim growth marks the onset of decompression and the transition from pre-eruptive to syn-eruptive conditions.« less

The Year Leading to a Supereruption

DOE PAGES

Gualda, Guilherme A. R.; Sutton, Stephen R.

2016-07-20

Supereruptions catastrophically eject 100s-1000s of km 3 of magma to the surface in a matter of days to a few months. In this study, we use zoning in quartz crystals from the Bishop Tuff (California) to assess the timescales over which a giant magma body transitions from relatively quiescent, pre-eruptive crystallization to rapid decompression and eruption. Quartz crystals in the Bishop Tuff have distinctive rims (<200 μm thick), which are Ti-rich and bright in cathodoluminescence (CL) images, and which can be used to calculate Ti diffusional relaxation times. We use synchrotron-based x-ray microfluorescence to obtain quantitative Ti maps and profilesmore » along rim-interior contacts in quartz at resolutions of 1–5 μm in each linear dimension. We perform CL imaging on a scanning electron microscope (SEM) using a low-energy (5 kV) incident beam to characterize these contacts in high resolution (<1 μm in linear dimensions). Quartz growth times were determined using a 1D model for Ti diffusion, assuming initial step functions. Minimum quartz growth rates were calculated using these calculated growth times and measured rim thicknesses. Maximum rim growth times span from ~1 min to 35 years, with a median of ~4 days. More than 70% of rim growth times are less than 1 year, showing that quartz rims have mostly grown in the days to months prior to eruption. Minimum growth rates show distinct modes between 10 -8 and 10 -10 m/s (depending on sample), revealing very fast crystal growth rates (100s of nm to 10s of μm per day). Our data show that quartz rims grew well within a year of eruption, with most of the growth happening in the weeks or days preceding eruption. Growth took place under conditions of high supersaturation, suggesting that rim growth marks the onset of decompression and the transition from pre-eruptive to syn-eruptive conditions.« less

Purification of HgI.sub.2 for nuclear detector fabrication

DOEpatents

Schieber, Michael M.

1978-01-01

A process for purification of mercuric iodide (HgI.sub.2) to be used as a source material for the growth of detector quality crystals. The high purity HgI.sub.2 raw material is produced by a combination of three stages: synthesis of HgI.sub.2 from Hg and I.sub.2, repeated sublimation, and zone refining.

Iron snow in the Martian core?

NASA Astrophysics Data System (ADS)

Davies, Christopher J.; Pommier, Anne

2018-01-01

The decline of Mars' global magnetic field some 3.8-4.1 billion years ago is thought to reflect the demise of the dynamo that operated in its liquid core. The dynamo was probably powered by planetary cooling and so its termination is intimately tied to the thermochemical evolution and present-day physical state of the Martian core. Bottom-up growth of a solid inner core, the crystallization regime for Earth's core, has been found to produce a long-lived dynamo leading to the suggestion that the Martian core remains entirely liquid to this day. Motivated by the experimentally-determined increase in the Fe-S liquidus temperature with decreasing pressure at Martian core conditions, we investigate whether Mars' core could crystallize from the top down. We focus on the "iron snow" regime, where newly-formed solid consists of pure Fe and is therefore heavier than the liquid. We derive global energy and entropy equations that describe the long-timescale thermal and magnetic history of the core from a general theory for two-phase, two-component liquid mixtures, assuming that the snow zone is in phase equilibrium and that all solid falls out of the layer and remelts at each timestep. Formation of snow zones occurs for a wide range of interior and thermal properties and depends critically on the initial sulfur concentration, ξ0. Release of gravitational energy and latent heat during growth of the snow zone do not generate sufficient entropy to restart the dynamo unless the snow zone occupies at least 400 km of the core. Snow zones can be 1.5-2 Gyrs old, though thermal stratification of the uppermost core, not included in our model, likely delays onset. Models that match the available magnetic and geodetic constraints have ξ0 ≈ 10% and snow zones that occupy approximately the top 100 km of the present-day Martian core.

The Fish Canyon magma body, San Juan volcanic field, Colorado: Rejuvenation and eruption of an upper-crustal batholith

USGS Publications Warehouse

Bachmann, Olivier; Dungan, M.A.; Lipman, P.W.

2002-01-01

More than 5000 km3 of nearly compositionally homogeneous crystalrich dacite (~68 wt % SiO2: ~45% Pl + Kfs + Qtz + Hbl + Bt + Spn + Mag + Ilm + Ap + Zrn + Po) erupted from the Fish Canyon magma body during three phases: (1) the pre-caldera Pagosa Peak Dacite (an unusual poorly fragmented pyroclastic deposit, ~ 200 km3); (2) the syn-collapse Fish Canyon Tuff (one of the largest known ignimbrites, ~ 5000 km3); (3) the post-collapse Nutras Creek Dacite (a volumetrically minor lava). The late evolution of the Fish Canyon magma is characterized by rejuvenation of a near-solidus upper-crustal intrusive body (mainly crystal mush) of batholithic dimensions. The necessary thermal input was supplied by a shallow intrusion of more mafic magma represented at the surface by sparse andesitic enclaves in late-erupted Fish Canyon Tuff and by the post-caldera Huerto Andesite. The solidified margins of this intrusion are represented by holocrystalline xenoliths with Fish Canyon mineralogy and mineral chemistry and widely dispersed partially remelted polymineralic aggregates, but dehydration melting was not an important mechanism in the rejuvenation of the Fish Canyon magma. Underlying mafic magma may have evolved H2O-F-S-Cl-rich fluids that fluxed melting in the overlying crystal mush. Manifestations of the late up-temperature magma evolution are: (1) resorbed quartz, as well as feldspars displaying a wide spectrum of textures indicative of both resorption and growth, including Rapakivi textures and reverse growth zoning (An27-28 to An32-33) at the margins of many plagioclase phenocrysts; (2) high Sr, Ba, and Eu contents in the high-SiO2 rhyolite matrix glass, which are inconsistent with extreme fractional crystallization of feldspar; (3) oscillatory and reverse growth zoning toward the margins of many euhedral hornblende phenocrysts (rimward increases from ~5??5-6 to 7??7-8??5 wt % Al2O3). Homogeneity in magma composition at the chamber-wide scale, contrasting with extreme textural and chemical complexities at the centimeter-millimeter scale, is consistent with a dynamic environment, wherein crystals with a variety of growth and resorption histories were juxtaposed shortly before eruption by convective currents.

Growth and optical waveguide fabrication in spinel MgGa2O4 crystal

NASA Astrophysics Data System (ADS)

Wang, Liang-Ling; Cui, Xiao-Jun; Rensberg, Jura; Wu, Kui; Wesch, Werner; Wendler, Elke

2017-10-01

We report on optical waveguide fabrication in a spinel MgGa2O4 crystal by 6.0 MeV carbon ion implantation at a fluence of 2 × 1015 ions/cm2 for the first time to our knowledge. The MgGa2O4 crystal was grown by the floating zone method. The refractive index profile reconstructed by reflectivity calculation method showed that the MgGa2O4 waveguide is a typical barrier waveguide. The typical barrier-shaped refractive index profile is attributed mainly to the nuclear energy deposition of the incident carbon ions into the MgGa2O4 crystal. By performing end-coupling measurements and using the beam propagation method (BPM) for the analysis of the observed modes, it can be concluded that the modes can be confined inside the waveguide.

High-quality single crystal growth and magnetic property of Mn4Ta2O9

NASA Astrophysics Data System (ADS)

Cao, Yiming; Xu, Kun; Yang, Ya; Yang, Wangfan; Zhang, Yuanlei; Kang, Yanru; He, Xijia; Zheng, Anmin; Liu, Mian; Wei, Shengxian; Li, Zhe; Cao, Shixun

2018-06-01

A large-size single crystal of Mn4Ta2O9 with ∼3.5 mm in diameter and ∼65 mm in length was successfully grown for the first time by a newly designed one-step method based on the optical floating zone technique. Both the clear Laue spots and sharp XRD Bragg reflections suggest the high quality of the single crystal. In Mn4Ta2O9 single crystal, an antiferromagnetic phase transition was observed below Néel temperature 102 K along c axis, which is similar to the isostructural compound Mn4Nb2O9, but differs from the isostructural Co4Nb2O9. Relative dielectric constant at 30 kOe suggests that no magnetoelectric coupling exists in Mn4Ta2O9.

Production of fibers by a floating zone fiber drawing technique

NASA Technical Reports Server (NTRS)

Haggerty, J. S.

1972-01-01

A CO2 laser heated, floating zone fiber growth process was developed. The resulting Al2O3 fibers exhibited the high room temperature strengths for large diameter fibers as well as high specific creep rupture strengths observed at 1093 C and 1316 C (2000 F and 2400 F). Single crystal fibers of TiC and Y2O3 were also grown. An optical system was developed to focus four CO2 laser beams onto the surface of a feed rod permitting the formation of highly controllable molten zones. The optical system permitted energy densities and angle of incidence of the beams to be adjusted over wide ranges. This optical system was incorporated into a controlled atmosphere, fiber growth furnace. The two principal advantages of a CO2 laser heat source are that ambient atmospheres may be freely selected to optimize fiber properties and the laser has no inherent temperature limit, so extremely high melting point materials can be melted. Both advantages were demonstrated.

Igneous phenocrystic origin of K-feldspar megacrysts in granitic rocks from the Sierra Nevada batholith

USGS Publications Warehouse

Moore, J.G.; Sisson, T.W.

2008-01-01

Study of four K-feldspar megacrystic granitic plutons and related dikes in the Sierra Nevada composite batholith indicates that the megacrysts are phenocrysts that grew in contact with granitic melt. Growth to megacrystic sizes was due to repeated replenishment of the magma bodies by fresh granitic melt that maintained temperatures above the solidus for extended time periods and that provided components necessary for K-feldspar growth. These intrusions cooled 89-83 Ma, are the youngest in the range, and represent the culminating magmatic phase of the Sierra Nevada batholith. They are the granodiorite of Topaz Lake, the Cathedral Peak Granodiorite, the Mono Creek Granite, the Whitney Granodiorite, the Johnson Granite Porphyry, and the Golden Bear Dike. Megacrysts in these igneous bodies attain 4-10 cm in length. All have sawtooth oscillatory zoning marked by varying concentration of BaO ranging generally from 3.5 to 0.5 wt%. Some of the more pronounced zones begin with resorption and channeling of the underlying zone. Layers of mineral inclusions, principally plagioclase, but also biotite, quartz, hornblende, titanite, and accessory minerals, are parallel to the BaO-delineated zones, are sorted by size along the boundaries, and have their long axes preferentially aligned parallel to the boundaries. These features indicate that the K-feldspar megacrysts grew while surrounded by melt, allowing the inclusion minerals to periodically attach themselves to the faces of the growing crystals. The temperature of growth of titanite included within the K-feldspar megacrysts is estimated by use of a Zr-in-titanite geothermometer. Megacryst-hosted titanite grains all yield temperatures typical of felsic magmas, mainly 735-760 ??C. Titanite grains in the granodiorite hosts marginal to the megacrysts range to lower growth temperatures, in some instances into the subsolidus. The limited range and igneous values of growth temperatures for megacryst-hosted titanite grains support the interpretation that the megacrysts formed ag igneous sanidine phenocrysts, that intrusion temperatures varied by only small amounts while the megacrysts grew, and that megacryst growth ceased before the intrusions cooled below the solidus. Individual Ba-enriched zones were apparently formed by repeated surges of new, hotter granitic melt that replenished these large magma chambers. Each recharge of hot magron offset cooling, maintained the partially molten or mushy character of the chamber, stirred up crystals, and induced convective currents that lofted, settling megacrysts back up into the chamber. Because of repeated reheating of the magma chamber and prolonged maintenance of the melt, this process apparently continued long enough to provide the ideal environment for the growth of these extraordinarily large K-feldspar phenocrysts. ??2008 Geological Society of America.

Crystallochemistry and origin of pyroxenes in komatiites

NASA Astrophysics Data System (ADS)

Bouquain, Sebastien; Arndt, N. T.; Hellebrand, E.; Faure, F.

2009-11-01

We present a detailed mineralogical and major- and trace-element study of pyroxenes in two Archean komatiitic flows in Alexo, Canada. The pyroxenes in spinifex-textured lavas commonly are zoned with cores of magnesian pigeonite and rims of augite. Concentrations of incompatible trace elements are low in pigeonite and jump to higher values in the augite mantles, a variation that can be modelled using accepted partition coefficients and assuming crystallization from komatiitic liquids. Crystallization sequences are very different in different parts of both flows. In the flow top, the sequence is olivine followed by augite: deeper in the spinifex sequence, pigeonite crystallizes after olivine, followed by augite; in lower cumulates, orthopyroxene or augite accompany olivine. In spinifex lavas, pigeonite crystallizes sooner than would be predicted on the basis of equilibrium phase relations. We propose that contrasting crystallization sequences depend on the position in the flow and on the conditions of crystal growth. In the flowtop, rapid cooling causes quench crystallization. Deeper in the spinifex layer, constrained growth in a thermal gradient, perhaps augmented by Soret differentiation, accounts for the early crystallization of pigeonite. The cumulus minerals represent a near-equilibrium assemblage. Augites in Al-undepleted Archean komatiites in various localities in Canada and Zimbabwe have high moderate to high Wo contents but their Mg# (Mg/(Mg + Fe) are lower than in augites in komatiites from Barberton, South Africa. We attribute the combination of high Wo and high Mg# in Barberton rocks to the unusually high CaO/Al2O3 of these Al-depleted komatiites.

Modelling of the MEA float zone using accelerometer data

NASA Technical Reports Server (NTRS)

Alexander, J. Iwan D.

1993-01-01

During a floating zone experiment involving the growth of indium on a recent orbiter mission, (STS 32) oscillation of the zone shapes were observed to occur in response to the background acceleration. An understanding of the nature of the response of the zone shape to forced (g-jitter) oscillations and predictions of its impact on future experiments is of great interest not only to the PI's but to other commercial and academic investigators who plan to fly similar experiments in the orbiter and on space station. Motivated by this, a 15 month study was undertaken to analyze the nature of the g-sensitivity of the STS 32 floating zone crystal growth experiment. Numerical models were used to describe the time-dependent free surface motion of the zone as it responds to the spacecraft residual acceleration. Relevant experimental data concerning the acceleration environment was obtained from the Honeywell in Space Accelerometer (HISA) investigators through MSFC's ACAP program and processed and analyzed. For the indium floating zone experiment, a series of calculations were made using time-dependent axial accelerations g(t). The form of g(t) included simple sinusoidal disturbances as well as actual data (subject to appropriate filtering) measured on the STS 32 mission. Focus was on the calculation of the response of the free surface of the zone as well as the internal flows and internal heat transfer. The influence of solidification on the response of the zone shape was also examined but found to be negligible.

Rapid assembly and rejuvenation of a large silicic magmatic system: Insights from mineral diffusive profiles in the Kidnappers and Rocky Hill deposits, New Zealand

NASA Astrophysics Data System (ADS)

Cooper, George F.; Morgan, Daniel J.; Wilson, Colin J. N.

2017-09-01

The timescales over which magmas in large silicic systems are reactivated, assembled and stored remains a fundamental question in volcanology. To address this question, we study timescales from Fe-Mg interdiffusion in orthopyroxenes and Ti diffusion in quartz from the caldera-forming 1200 km3 Kidnappers and 200 km3 Rocky Hill eruptions from the Mangakino volcanic centre (Taupo Volcanic Zone, New Zealand). The two eruptions came from the same source area, have indistinguishable 40Ar/39Ar ages (∼1.0 Ma) and zircon U-Pb age spectra, but their respective deposits are separated by a short period of erosion. Compositions of pumice, glass and mineral species in the collective eruption deposits define multiple melt dominant bodies but indicate that these shared a common magmatic mush zone. Diffusion timescales from both eruptions are used to build on chemical and textural crystal signatures and interpret both the crystal growth histories and the timing of magma accumulation. Fe-Mg interdiffusion profiles in orthopyroxenes imply that the three melt-dominant bodies, established through extraction of melt and crystals from the common source, were generated within 600 years and with peak accumulation rates within 100 years of each eruption. In addition, a less-evolved melt interacted with the Kidnappers magma, beginning ∼30 years prior to and peaking within 3 years of the eruption. This interaction did not directly trigger the eruption, but may have primed the magmatic system. Orthopyroxene crystals with the same zoning patterns from the Kidnappers and Rocky Hill pumices yield consistently different diffusion timescales, suggesting a time break between the eruptions of ∼20 years (from core-rim zones) to ∼10 years (outer rim zones). Diffusion of Ti in quartz reveals similarly short timescales and magmatic residence times of <30 years, suggesting quartz is only recording the last period of crystallization within the final eruptible melt. Accumulation of the eruptible magma for these two, closely successive eruptions was accomplished over centuries to decades, in contrast to the gestation time of the magmatic system of ∼200 kyr, as indicated by zircon age patterns. The magmatic system was able to recover after the Kidnappers eruption in only ∼10-20 years to accumulate enough eruptible melt and crystals for a second ∼ 200 km3 eruption. Our data support concepts of large silicic systems being stored as long-lived crystal mushes, with eruptible melts generated over extraordinarily short timescales prior to eruption.

Growth, morphological properties and pulsed photo response of MoTe2 single crystal synthesized by DVT technique

NASA Astrophysics Data System (ADS)

Dixit, Vijay; Vyas, Chirag; Patel, Abhishek; Pathak, V. M.; Solanki, G. K.; Patel, K. D.

2018-05-01

Molybednum Di Telluride of group VI belongs to the family of layered transition metal di-chalcogenides (TMDCs). These TMDCs show good potential for applications in the field of optoelectronic devices as they are chemically inert trilayered structure of MX2 type. In the present investigation crystals of MoTe2 are grown by direct vapor transport technique in a dual zone horizontal furnace. The grown crystals were characterized by Energy Dispersive Analysis of X-rays (EDAX) to study its elemental and stoichiometric composition, Selected Area Electron Diffraction (SAED) confirms the hexagonal structure. Spot pattern of electron diffraction shows formation of single phase. Scanning Electron Microscope (SEM) shows the layer by layer growth of the crystals, Thermo Electric Power (TEP) reflects the p-type semiconducting nature of the grown crystals. As this material is photosensitive material having band gap of approximately 1.0 eV, a transient photo response against polychromatic radiation (40 mW/cm2) of photodetector is also measured which showed slow decay in generated photocurrent due to low trapping density within the active area of the prepared device. Thus, it shows that this material can be a good photovoltaic material for constructing a solar cell also.

Processes and time scales of magmatic evolution as revealed by Fe-Mg chemical and isotopic zoning in natural olivines

NASA Astrophysics Data System (ADS)

Oeser, Martin; Dohmen, Ralf; Horn, Ingo; Schuth, Stephan; Weyer, Stefan

2015-04-01

In this study, we applied high-precision in situ Fe and Mg isotope analyses by femtosecond laser ablation (fs-LA) MC-ICP-MS on chemically zoned olivine xeno- and phenocrysts from intra-plate volcanic regions in order to investigate the magnitude of Fe and Mg isotope fractionation and its suitability to gain information on magma evolution. Our results show that chemical zoning (i.e., Mg#) in magmatic olivines is commonly associated with significant zoning in δ56Fe and δ26Mg (up to 1.7‰ and 0.7‰, respectively). We explored different cases of kinetic fractionation of Fe and Mg isotopes by modeling diffusion in the melt or olivine and simultaneous growth or dissolution. Combining the information of chemical and isotopic zoning in olivine allows to distinguish between various processes that may occur during magma evolution, namely diffusive Fe-Mg exchange between olivine and melt, rapid crystal growth, and Fe-Mg inter-diffusion simultaneous to crystal dissolution or growth. Chemical diffusion in olivine appears to be the dominant process that drives isotope fractionation in magmatic olivine. Simplified modeling of Fe and Mg diffusion is suitable to reproduce both the chemical and the isotopic zoning in most of the investigated olivines and, additionally, provides time information about magmatic processes. For the Massif Central (France), modeling of diffusive re-equilibration of mantle olivines in basanites revealed a short time span (<2 years) between the entrainment of a mantle xenolith in an intra-plate basaltic magma and the eruption of the magma. Furthermore, we determined high cooling rates (on the order of a few tens to hundreds of °C per year) for basanite samples from a single large outcrop in the Massif Central, which probably reflects the cooling of a massive lava flow after eruption. Results from the modeling of Fe and Mg isotope fractionation in olivine point to a systematic difference between βFe and βMg (i.e., βFe/βMg ≈ 2), implying that the diffusivity ratio of 54Fe and 56Fe (i.e., D54Fe/D56Fe) is very similar to that of 24Mg and 26Mg, despite the smaller relative mass difference for the 54Fe-56Fe pair. This study demonstrates that a combined investigation of Fe-Mg chemical and isotopic zoning in olivine provides additional and more reliable information on magma evolution than chemical zoning alone.

Experimental and quantum chemical studies on Nsbnd Hsbnd sbnd sbnd O hydrogen bonded helical chain type Morpholinium 2-chloro-4-nitrobenzoate: A phasematchable organic nonlinear optical material

NASA Astrophysics Data System (ADS)

Karthick, S.; Thirupugalmani, K.; Shanmugam, G.; Kannan, V.; Brahadeeswaran, S.

2018-03-01

We report on the studies performed on Morpholinium 2-chloro-4-nitrobenzoate (M2C4N), a second order nonlinear optical (NLO) material, which has been proved to crystallize with chiral structure as compared to its other two variants. The synthesized powder was studied for its composition, crystalline phase and NLO efficiency and phasematchability. The solubility and the metastable zone width (MSZW) of the title compound were measured for the growth of bulk crystals of M2C4N. A smoky pattern observed in the middle region of the crystals that could prevent it from optical applications was greatly reduced, through suitable modifications in the growth process. The optical properties such as luminescence and laser damage threshold resistance were studied for the bulk crystals whereas the molecular vibrations of M2C4N were studied through Fourier transform infrared (FTIR) and FT-Raman spectral analysis using the polycrystalline powders derived from the single crystals. In addition, quantum chemical studies on M2C4N molecule were performed by using density functional theory (DFT) at the B3LYP/6-311++G (d, p) basis set. These studies showed that the M2C4N is a phasematchable NLO crystal and could be used for device fabrication.

Tiny crystals give away the where and when of magma ascent

NASA Astrophysics Data System (ADS)

Ruth, D. C. S.; Costa Rodriguez, F.; Bouvet de Maisonneuve, C.; Franco, L.; Cortes, J. A.; Calder, E.

2016-12-01

Open vent volcanoes exhibit passive degassing and can transition to explosive behavior, with limited or no warning. Melt inclusion chemistry and volatile contents have been used to infer the inner dynamics of magma storage, recharge, degassing, and eruption triggering mechanisms. However, the interpretation of melt inclusion chemistry is ambiguous because it cannot constrain the residence times of the host crystals, which could have various sources and growth histories. To resolve this issue we combine diffusion chronometry and melt inclusion entrapment pressures from olivine crystals sourced from the 2008 eruption of Llaima volcano (Chile). Olivine crystals (core Fo70-84, rim Fo77-84) are dominantly reverse zoned, although normal zoned and complex zoned crystals are observed. These data reflect mixing between the mafic injecting magma and the crystal-rich resident magma. Fe/Mg diffusion timescales range between 16 and 1375 days. The diffusion data show a non-uniform distribution with no discernible peaks, indicating that magma injection is likely progressive, rather than punctuated. Entrapment pressures range between 8 and 151 MPa, overlapping with an inferred crystal-rich region. Longer timescales correspond to higher pressures, strongly suggesting a link between magma residence time and ascent from depth. To our knowledge, this relationship has not been previously demonstrated. We infer that mafic magma intruded at depths of 5 km below the edifice and mingled with a pre-existing crystal-mush 3 yr before the eruption. Magma migration and mingling continued and stalled at 2.5 km depth about a year prior to the eruption. Precursory activity such as volcano-tectonic and long period seismicity, and a series of minor explosions overlap with the diffusion times 6 months before the eruption. Similar diffusion timescales have been reported for eruptions at other open vent volcanoes. Our study provides the first temporal and spatial constraints on magma storage and ascent before an eruption. Furthermore at Llaima, and potentially open vent systems, the progressive nature of magma injection suggests that additional processes (e.g. variable ascent rates, changing viscosity, etc.) are needed to trigger an eruption.

Crystal growth and magnetic characterization of a tetragonal polymorph of NiNb2O6

NASA Astrophysics Data System (ADS)

Munsie, T. J. S.; Millington, A.; Dube, P. A.; Dabkowska, H. A.; Britten, J.; Luke, G. M.; Greedan, J. E.

2016-04-01

A previously unidentified polymorph of nickel niobate, NiNb2O6, was grown and stabilized in single crystalline form using an optical floating zone furnace. Key parameters of the growth procedure involved use of a slight excess of NiO (1.2% by mol), an O2 atmosphere and a growth rate of 25 mm/h. The resulting boule consisted of a polycrystalline exterior shell of the columbite structure - columbite is the thermodynamically stable form of NiNb2O6 under ambient conditions - and a core region consisting of transparent yellow-green single crystals up to 5 mm×2 mm×1 mm in dimension of the previously unidentified phase. The crystal structure, solved from single crystal x-ray diffraction data, is described in the P42/n space group. Interestingly, this is not a subgroup of P42/mnm, the rutile space group. The Ni2+ ions form layers which are displaced such that interlayer magnetic frustration is anticipated. Magnetic susceptibility data shows a broad maximum at approximately 22 K and evidence for long range antiferromagnetic order at approximately 14 K, obtained by Fisher heat capacity analysis as well as heat capacity measurements. The susceptibility data for T > 25 K are well fit by a square lattice S = 1 model, consistent with the Ni sublattice topology.

U-series disequilibria in crystals: ages as tracers

NASA Astrophysics Data System (ADS)

Cooper, K. M.

2005-12-01

U-series disequilibria offer a unique perspective on the fates of crystals within magmatic systems. In addition to delimiting the timescales of magmatic processes, crystal ages can be used as a tracer of different crystal populations even in the case where only subtle differences exist between major- and trace-element chemistries of populations. For example, 226Ra-230Th ages of crystals in Mt St Helens lavas erupted since 2 ka are in some cases several kyr older than eruption ages which, when combined with significant Ra-Th disequilibria in the whole-rocks, suggests protracted crystal storage and entrainment in subsequent batches of magma passing through the reservoir. More broadly, in many cases 230Th-238U and 226Ra-230Th ages measured in the same crystals are discordant. This pattern likely indicates progressive and/or episodic crystal growth where the Th-U ages more closely represent average crystallization ages while Ra-Th ages are weighted toward recent growth, suggesting in turn that some significant fraction of the mass of crystals represent xenocrysts or "antecrysts" recycled from earlier generations of magmas within the same system. Conversely, in cases where ages of different parent-daughter pairs are concordant, mineral separates must be dominated by crystal growth within a relatively narrow time interval relative to the half-life of the shortest-lived daughter isotope. The duration of the crystal record within a given magma can be complicated by crystal recycling and obscured by average ages derived from measurement of bulk mineral separates. One way to extract more information about the proportion and ages of older and younger parts of the crystal population(s) is to analyze different size fractions within the same sample; for example, analyses of different sizes of plagioclase from the ongoing eruption at Mt St Helens are in progress. U-series ages and other crystal-scale geochemical information can also be a powerful combination. For example, preservation of major- or trace-element disequilibrium between zones within crystals limits the duration of crystal residence at high temperature; when combined with absolute age information from U-series disequilibria, these data can provide clues about the thermal conditions of crystal storage and thus whether such storage is likely to have occurred in a mostly-liquid or mostly-crystalline part of the magma system.

Control of Meridional Flow in Circular Cylinders by a Travelling Axial Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, K.; Ramachandran, N.; Volz, M. P.

1999-01-01

Convective flow in a Bridgman or float zone configuration significantly affects the interface shape and segregation phenomena. While the primary causative factor for this flow is buoyancy induced convection in an enclosed Bridgman melt, the presence of a free surface gives rise to surface tension driven flows in the floating zone processing of melts. It is of interest to curtail these flows in order to realize near quiescent growth conditions that have shown to result in crystals with good longitudinal and radial homogeneity and thereby of better overall quality. While buoyancy effects can be reduced by careful processing in a low gravity (space) environment, the reduction of Marangoni flows due to surface tension variations is not that straight forward. Attempts have been made with some limited success with the use of external fields to affect the melt thermo-fluid behavior. The use of a static magnetic field that reduces convective contamination through the effects of a non-intrusively induced, dissipative Lorentz force in an electrically conducting melt is one such approach. Experiments have shown that axial fields of the order of 5 Tesla can significantly eliminate convection and yield close to diffusion limited crystal growth conditions. The generation and use of such high magnetic fields require substantial hardware and incur significant costs for its operation. Lately, the use of rotating magnetic fields has been tested in semiconductor crystal growth. The method is fairly well known and commonly used in metal processing but its adaptation to crystal growth of semiconductors is fairly recent. The elegance of the technique rests in its low power requirement (typically 10-20 milli-Tesla at 50-400 Hz) and its efficacy in curtailing deleterious temperature fluctuations in the melt. A rotating magnetic field imposes a rotational force and thereby induces a circulation within the melt that tends to dominate other sporadic convective effects. Thus a known low level of convective flow is introduced into the system. A new novel variation of the Lorentz force mechanism is proposed and investigated in this study. Since one of the desired process conditions in melt crystal growth is the minimization of convective effects, this investigation examines the use of an external field of magnetic origin to counteract existing convective flow within the melt. This is accomplished by utilizing a running or traveling axial magnetic wave in the system. The concept is similar to the use of vibrational means in order to induce streaming flows that oppose buoyant or surface tension driven convection in the system. The rotation direction as well as the magnitude (strength) of this circulation can be easily controlled by external inputs thus affording a direct means of controlling the developing shape of the crystallizing front (interface). The theoretical model of this technique is fully developed and presented in this paper. Results from the solution of the developed governing equations and boundary conditions are also presented. An experimental demonstration of the concept is presented through the suppression of natural convective flow in a mercury column. Implications to crystal growth systems will be fully explored in the final manuscript.

Magnetic Control in Crystal Growth from a Melt

NASA Astrophysics Data System (ADS)

Huang, Yue

Control of bulk melt crystal growth techniques is desirable for producing semiconductors with the highest purity and ternary alloys with tunable electrical properties. Because these molten materials are electrically conducting, external magnetic fields are often employed to regulate the flow in the melt. However, complicated by the coupled flow, thermal, electromagnetic and chemical physics, such magnetic control is typically empirical or even an educated guess. Two magnetic flow control mechanisms: flow damping by steady magnetic fields, and flow stirring by alternating magnetic fields, are investigated numerically. Magnetic damping during optically-heated float-zone crystal growth is modeled using a spectral collocation method. The Marangoni convection at the free melt-gas interface is suppressed when exposed to a steady axial magnetic field, measured by the Hartmann number Ha. As a result, detrimental flow instabilities are suppressed, and an almost quiescent region forms in the interior, ideal for single crystal growth. Using normal mode linear stability analyses, dominant flow instabilities are determined in a range applicable to experiments (up to Ha = 300 for Pr = 0.02, and up to Ha = 500 for Pr = 0.001). The hydrodynamic nature of the instability for small Prandtl number Pr liquid bridges is confirmed by energy analyses. Magnetic stirring is modeled for melt crystal growth in an ampule exposed to a transverse rotating magnetic field. Decoupled from the flow field at small magnetic Reynolds number, the electromagnetic field is first solved via finite element analysis. The flow field is then solved using the spectral element method. At low to moderate AC frequencies (up to a few kHz), the electromagnetic body force is dominant in the azimuthal direction, which stirs a steady axisymmetric flow primarily in the azimuthal direction. A weaker secondary flow develops in the meridional plane. However, at high AC frequencies (on the order of 10 kHz and higher), only the flow within a skin depth is directly stirred due to the magnetic shielding effect. By regulating the flow in the melt, magnetic control can improve grown-crystal properties in new materials, and achieve economically viable growth rates for production of novel crystalline semiconductors.

Growth and characterization of benzaldehyde 4-nitro phenyl hydrazone (BPH) single crystal: A proficient second order nonlinear optical material

NASA Astrophysics Data System (ADS)

Saravanan, M.; Abraham Rajasekar, S.

2016-04-01

The crystals (benzaldehyde 4-nitro phenyl hydrazone (BPH)) appropriate for NLO appliance were grown by the slow cooling method. The solubility and metastable zone width measurement of BPH specimen was studied. The material crystallizes in the monoclinic crystal system with noncentrosymmetric space group of Cc. The optical precision in the whole visible region was found to be excellent for non-linear optical claim. Excellence of the grown crystal is ascertained by the HRXRD and etching studies. Laser Damage Threshold and Photoluminescence studies designate that the grown crystal contains less imperfection. The mechanical behaviour of BPH sample at different temperatures was investigated to determine the hardness stability of the grown specimen. The piezoelectric temperament and the relative Second Harmonic Generation (for diverse particle sizes) of the material were also studied. The dielectric studies were executed at varied temperatures and frequencies to investigate the electrical properties. Photoconductivity measurement enumerates consummate of inducing dipoles due to strong incident radiation and also divulge the nonlinear behaviour of the material. The third order nonlinear optical properties of BPH crystals were deliberate by Z-scan method.

Growth of high quality and large-sized Rb 0.3MoO 3 single crystals by molten salt electrolysis method

NASA Astrophysics Data System (ADS)

Wang, Junfeng; Xiong, Rui; Yi, Fan; Yin, Di; Ke, Manzhu; Li, Changzhen; Liu, Zhengyou; Shi, Jing

2005-05-01

High quality and large-sized Rb 0.3MoO 3 single crystals were synthesized by molten salt electrolysis method. X-ray diffraction (XRD) patterns and rocking curves, as well as the white beam Laue diffraction of X-ray images show the crystals grown by this method have high quality. The lattice constants evaluated from XRD patterns are a0=1.87 nm, b0=0.75 nm, c0=1.00 nm, β=118.83∘. The in situ selected area electron diffraction (SAED) patterns along the [101¯], [11¯1¯] and [103¯] zone axes at room temperature indicate that the Rb 0.3MoO 3 crystal possess perfect C-centered symmetry. Temperature dependence of the resistivity shows this compound undergoes a metal to semiconductor transition at 183 K.

Laser furnace and method for zone refining of semiconductor wafers

NASA Technical Reports Server (NTRS)

Griner, Donald B. (Inventor); zur Burg, Frederick W. (Inventor); Penn, Wayne M. (Inventor)

1988-01-01

A method of zone refining a crystal wafer (116 FIG. 1) comprising the steps of focusing a laser beam to a small spot (120) of selectable size on the surface of the crystal wafer (116) to melt a spot on the crystal wafer, scanning the small laser beam spot back and forth across the surface of the crystal wafer (116) at a constant velocity, and moving the scanning laser beam across a predetermined zone of the surface of the crystal wafer (116) in a direction normal to the laser beam scanning direction and at a selectible velocity to melt and refine the entire crystal wafer (116).

Experimental Studies on Mass Transport of Cadmium-Zinc Telluride by Physical Vapor Transport

NASA Technical Reports Server (NTRS)

Palosz, W.; Szofran, F. R.; Lehoczky, S. L.

1995-01-01

Experimental studies on mass transport of ternary compound, Cd(1-x)Zn(x)Te by physical vapor transport (PVT) for source compositions up to X = 0.21 are presented. The effect of thermochemical (temperatures, vapor composition) and other factors (preparation of the source, crystal growth rate, temperature gradient) on composition and composition profiles of the grown crystals were investigated. A steep decrease in the mass flux with an increase in X(crystal) for X less than 0.1, and a difference in composition between the source and the deposited material have been observed. The composition profiles of the crystals were found to depend on the density and pretreatment of the source, and on the temperature gradient in the source zone. The homogeneity of the crystals improves at low undercoolings and/or when an appropriate excess of metal constituents is present in the vapor phase. The experimental results are in good agreement with our thermochemical model of this system.

High-quality Silicon Films Prepared by Zone-melting Recrystallization

NASA Technical Reports Server (NTRS)

Chen, C. K.; Geis, M. W.; Tsaur, B. Y.; Fan, J. C. C.

1984-01-01

The graphite strip heater zone melting recrystallization (ZMR) technique is described. The material properties of the ZMR films, and SOI device results are reviewed. Although our ZMR work is primarily motivated by integrated circuit applications, this work evolved in part from earlier research on laser crystallization of thick amorphous GaAs and Si films, which was undertaken with the goal of producing low cost photovoltaic materials. The ZMR growth process and its effect on the properties of the recrystallized films may contribute some insight to a general understanding of the rapid recrystallization of Si for solar cells. Adaptation of ZMR for solar cell fabrication is considered.

Influence of crucible support and radial heating on the interface shape during vertical Bridgman GaAs growth

NASA Astrophysics Data System (ADS)

Koai, K.; Sonnenberg, K.; Wenzl, H.

1994-03-01

Crucible assembly in a vertical Bridgman furnace is investigated by a numerical finite element model with the aim to obtain convex interfaces during the growth of GaAs crystals. During the growth stage of the conic section, a new funnel shaped crucible support has been found more effective than the concentric cylinders design similar to that patented by AT & T in promoting interface convexity. For the growth stages of the constant diameter section, the furnace profile can be effectively modulated by localized radial heating at the gradient zone. With these two features being introduced into a new furnace design, it is shown numerically that enhancement of interface convexity can be achieved using the presently available crucible materials.

Crystal Growth, Characterization and Fabrication of Cadmium Zinc Telluride-based Nuclear Detectors

NASA Astrophysics Data System (ADS)

Krishna, Ramesh M.

In today's world, nuclear radiation is seeing more and more use by humanity as time goes on. Nuclear power plants are being built to supply humanity's energy needs, nuclear medical imaging is becoming more popular for diagnosing cancer and other diseases, and control of weapons-grade nuclear materials is becoming more and more important for national security. All of these needs require high-performance nuclear radiation detectors which can accurately measure the type and amount of radiation being used. However, most current radiation detection materials available commercially require extensive cooling, or simply do not function adequately for high-energy gamma-ray emitting nuclear materials such as uranium and plutonium. One of the most promising semiconductor materials being considered to create a convenient, field-deployable nuclear detector is cadmium zinc telluride (CdZnTe, or CZT). CZT is a ternary semiconductor compound which can detect high-energy gamma-rays at room temperature. It offers high resistivity (≥ 1010 O-cm), a high band gap (1.55 eV), and good electron transport properties, all of which are required for a nuclear radiation detector. However, one significant issue with CZT is that there is considerable difficulty in growing large, homogeneous, defect-free single crystals of CZT. This significantly increases the cost of producing CZT detectors, making CZT less than ideal for mass-production. Furthermore, CZT suffers from poor hole transport properties, which creates significant problems when using it as a high-energy gamma-ray detector. In this dissertation, a comprehensive investigation is undertaken using a successful growth method for CZT developed at the University of South Carolina. This method, called the solvent-growth technique, reduces the complexity required to grow detector-grade CZT single crystals. It utilizes a lower growth temperature than traditional growth methods by using Te as a solvent, while maintaining the advantages of crystal homogeneity of other modern CZT growth techniques. However, information about crystals grown with this method has not been undertaken in a comprehensive way thus far. In this work, Cd0.9Zn0.1Te is grown using the solvent-growth method using zone-refined precursor materials loaded into carbon-coated quartz ampoules. Ampoules were sealed and crystal growth was performed using crystal growth furnaces built in-house at USC. Ingots 1-2" in diameter produced using the solvent-growth method were wafered, processed, and polished for characterization. Semiconductor characterization is performed on the CZT crystals to determine band gap, elemental stoichiometry, and electrical resistivity. Surface modification studies were undertaken to determine if surface leakage current can be reduced using sulfur passivation. XPS studies were used to confirm the effects of passivation on the surface states, and electrical characterization was performed to measure the effects of passivation on the CZT crystals. Deep-level and surface defect studies were conducted on the CZT samples to determine the type and intensity of defects present in the crystals which may affect detector performance. Finally, nuclear detectors were fabricated and characterized using analog and digital radiation detection systems to measure their performance and energy resolution.

Control of Meridional Flow by a Non-Uniform Rotational Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin; Ramachandran, Narayanan

1999-01-01

The diffusive mass transfer of species during crystal growth in vertical ampoules is significantly affected by fluid flow in the liquid mother phase (melt). For electrically conductive melts, an elegant way of remotely inducing and controlling this flow is by utilizing a uniform rotational magnetic field (RMF) in the transverse direction. It induces an azimuthal flow which tends to homogenize the thermal and solutal fields. The rotating field also reduces the diffusion boundary layer, stabilizes temperature fluctuations, and promotes better overall crystal growth. For moderate strengths of the applied magnetic field (2-20 m Tesla) with frequencies of up to 400 Hz, the induced secondary meridional flow becomes significant. It typically consists of one roll at the bottom of the liquid column and a second roll (vortex) at the top. The flow along the centerline (ampoule axis) is directed from the growing solid (interface) towards the liquid (melt). In case of convex interfaces (e.g. in floating zone crystal growth) such flow behavior is beneficial since it suppresses diffusion at the center. However, for concave interfaces (e.g. vertical Bridgman crystal growth) such a flow tends to exacerbate the situation in making the interface shape more concave. It would be beneficial to have some control of this meridional flow- for example, a single recirculating cell with controllable direction and flow magnitude will make this technique even more attractive for crystal growth. Such flow control is a possibility if a non-uniform PNE field is utilized for this purpose. Although this idea has been proposed earlier, it has not been conclusively demonstrated so far. In this work, we derive the governing equations for the fluid dynamics for such a system and obtain solutions for a few important cases. Results from parallel experimental measurements of fluid flow in a mercury column subjected to non-uniform RMF will also be presented.

The interplay between crystallization, replenishment and hybridization in large felsic magma chambers

NASA Astrophysics Data System (ADS)

Bateman, R.

1995-09-01

While hybridized granitoid magmas are readily identifiable, the mechanisms of hybridization in large crustal magma chambers are so not clearly understood. Characteristic features of hybrid granitoids are (1) both the granitoid and included enclaves are commonly hybrids, as shown by mineralogy, geochemistry and isotopes; (2) mixing seen in zoned plutons and synplutonic dykes and enclaves occurred early; (3) zoned plagioclase phenocrysts commonly show very complex life histories of growth and dissolution; (4) mafic end-members in hybrids are commonly fractionated magmas and (5) stratification in subvolcanic granitoid magma chambers is not uncommon, and stratification has been identified in some deeper level plutons. Hybridization must overcome the tendency to form a stable stratification of dense mafic magma underlying less dense felsic magma. Experimental work with magma analogues and theoretical considerations reveal very severe thermal, rheological and dynamical limitations on mixing: only very similar (composition, temperature) magmas are likely to mix to homogeneity, and only moderately silicic hybrids are likely to be produced. However, "impossibly" silicic hybrids do exist. Synchronous, interactive fractional crystallization and hybridization may provide a mechanism for hybridization of magmas, in the following manner. A mafic magma intrudes into the base of a stratified felsic magma and is cooled against it. Crystallization of the upper boundary layer of the mafic magma yields an eventually buoyant residual melt that overturns and mixes with an adjacent stratum of the felsic magma chamber. Subsequently, melt released by crystallization pf this, now-hybrid zone mixes with adjacent, more felsic zones. Thus, a suite of hybrid magmas are progressively formed. Density inhibitions are overcome by the generation of relatively low density residual melts. As crystallization proceeds, later injections are preserved as dykes and enclaves composed of hybrid magma. In this process, only physically adjacent and dynamically-thermally similar magmas directly interact, and so may mix to homogeneity. Finally, not simply felsic and mafic endmembers mix, but a whole suite of "intermediate" endmembers participate, ranging from relatively mafic through to felsic pairs of magmas. Direct mixing between the primary magmas only occurs at the beginning.

Growth and characterization of dexterous nonlinear optical material: Dimethyl amino pyridinium 4-nitrophenolate 4-nitrophenol (DMAPNP)

NASA Astrophysics Data System (ADS)

Saravanan, M.

2016-08-01

The crystals (dimethyl amino pyridinium 4-nitrophenolate 4-nitrophenol [DMAPNP] suitable for NLO applications were grown by the slow cooling method. The solubility and metastable zone width measurement of DMAPNP specimen was studied. The material crystallizes in the orthorhombic crystal system with noncentrosymmetric space group of P212121. The ocular precision in the intact visible region was found to be good for non-linear optical claim. Quality of the grown crystal is ascertained by the HRXRD and etching studies. Laser Damage Threshold and Photoluminescence studies designate that the grown crystal contains less imperfection. The mechanical behaviour of DMAPNP sample at different temperatures was investigated to determine the hardness stability of the grown specimen. The piezoelectric temperament and the relative Second Harmonic Generation (for diverse particle sizes) of the material were also studied. The third order nonlinear optical properties of DMAPNP crystals were premeditated by Z-scan method. Birefringence and optical homogeneity of the crystal were evaluated using modified channel spectrum method. The half wave voltage of the grown crystal deliberate from the elector optic experimentation. Photoconductivity measurement specified consummate of inducing dipoles owing to brawny incident radiation and also disclose the nonlinear activities of the grown specimen.

Characterisation of a garnet population from the Sikkim Himalaya: implications for the mechanisms and rates of porphyroblast crystallisation

NASA Astrophysics Data System (ADS)

George, Freya; Gaidies, Fred

2016-04-01

Analysis of porphyroblast distribution in metamorphic rocks yields insight into the processes controlling metamorphic reaction rates. By coupling this textural record with microprobe analysis and phase-equilibria and diffusion modelling, a detailed view of the nucleation and growth history of metamorphic minerals can be obtained. In this study, we comprehensively characterise the 3D distribution and compositional variation of a garnet population in a garnet-grade pelitic schist of the Lesser Himalayan Sequence (Sikkim), in order to investigate both the rates and kinetic controls of porphyroblastic crystallisation. Quantification of the size, shape and spatial distribution of garnet using high-resolution μ-computed X-ray tomography and statistical analysis reveals a log-normal crystal size distribution, systematic variation of aspect ratio with crystal size, and a significantly clustered garnet texture in the study sample. The latter is indicative of interface-controlled nucleation and growth, with nucleation sites controlled principally by a heterogeneous precursor assemblage. At length-scales less than 0.7 mm, there is evidence for adjacent grains that are on average smaller than the mean size of the population; this minor ordering is attributed to secondary redistribution of porphyroblast centers and reduction of crystal sizes due to syn-kinematic growth and resorption, respectively. Geochemical traverses through centrally sectioned garnet crystals of variable size highlight several features: (1) core compositions of even the smallest crystals preserve primary prograde growth zonation, with little evidence for diffusional modification in any crystal size; (2) rim compositions are within error between grains, suggestive of sample-scale equilibration of the growth medium at the time of cessation of crystallisation; (3) different grains of equal radii display equivalent compositional zoning; and (4) gradients of compositional profiles display a steepening trend in progressively smaller grain sizes, converse to anticipated trends based on classic kinetic crystallisation theory. The observed systematic behaviour is interpreted to reflect interface-controlled rates of crystallisation, with a decrease in the rate of crystal growth of newly nucleated grains as the crystallisation interval proceeds. Numerical simulations of garnet growth successfully reproduce observed core and rim compositions, and simulations of intracrystalline diffusion yield rapid heating/cooling rates along the P-T path, in excess of 100 °C/Ma. Radial garnet crystallisation is correspondingly rapid, with minimum growth rates of 1.5 mm/Ma in the smallest crystals. Simulations suggest progressive nucleation of new generations of garnet occurred with an exponentially decreasing frequency along the prograde path; however, measured gradients indicate that core compositions developed more slowly than predicted by the model, potentially resulting in a more evenly distributed pattern of nucleation.

Polarized Raman spectra in β-Ga2O3 single crystals

NASA Astrophysics Data System (ADS)

Onuma, T.; Fujioka, S.; Yamaguchi, T.; Itoh, Y.; Higashiwaki, M.; Sasaki, K.; Masui, T.; Honda, T.

2014-09-01

Polarized Raman spectra were measured from (010) Mg-doped, (100) Si-doped, and (001) unintentionally-doped β-Ga2O3 substrates prepared by either the floating zone growth or edge-defined film-fed growth methods. The Ag and Bg Raman active modes were perfectly separated in the spectra according to the polarization selection rules. To the best of our knowledge, this is the first experimental observation of a complete set of polarized Raman spectra of β-Ga2O3. The results are ensured by the high uniformity of crystalline orientation and surface flatness of the present substrates.

Hydride vapor phase epitaxy of AlN using a high temperature hot-wall reactor

NASA Astrophysics Data System (ADS)

Baker, Troy; Mayo, Ashley; Veisi, Zeinab; Lu, Peng; Schmitt, Jason

2014-10-01

Aluminum nitride (AlN) was grown on c-plane sapphire substrates by hydride vapor phase epitaxy (HVPE). The experiments utilized a two zone inductively heated hot-wall reactor. The surface morphology, crystal quality, and growth rate were investigated as a function of growth temperature in the range of 1450-1575 °C. AlN templates grown to a thickness of 1 μm were optimized with double axis X-ray diffraction (XRD) rocking curve full width half maximums (FWHMs) of 135″ for the (002) and 513″ for the (102).

Tracking magmatic processes through Zr/Hf ratios in rocks and Hf and Ti zoning in zircons: An example from the Spirit Mountain batholith, Nevada

USGS Publications Warehouse

Lowery, Claiborne L.E.; Miller, C.F.; Walker, B.A.; Wooden, J.L.; Mazdab, F.K.; Bea, F.

2006-01-01

Zirconium and Hf are nearly identical geochemically, and therefore most of the crust maintains near-chondritic Zr/Hf ratios of ???35-40. By contrast, many high-silica rhyolites and granites have anomalously low Zr/Hf (15-30). As zircon is the primary reservoir for both Zr and Hf and preferentially incorporates Zr, crystallization of zircon controls Zr/ Hf, imprinting low Zr/Hf on coexisting melt. Thus, low Zr/Hf is a unique fingerprint of effective magmatic fractionation in the crust. Age and compositional zonation in zircons themselves provide a record of the thermal and compositional histories of magmatic systems. High Hf (low Zr/ Hf) in zircon zones demonstrates growth from fractionated melt, and Ti provides an estimate of temperature of crystallization (TTiZ) (Watson and Harrison, 2005). Whole-rock Zr/Hf and zircon zonation in the Spirit Mountain batholith, Nevada, document repeated fractionation and thermal fluctuations. Ratios of Zr/Hf are ???30-40 for cumulates and 18-30 for high-SiO2 granites. In zircons, Hf (and U) are inversely correlated with Ti, and concentrations indicate large fluctuations in melt composition and TTiZ (>100??C) for individual zircons. Such variations are consistent with field relations and ion-probe zircon geochronology that indicate a >1 million year history of repeated replenishment, fractionation, and extraction of melt from crystal mush to form the low Zr/Hf high-SiO2 zone. ?? 2006 The Mineralogical Society.

Static Magnetic Fields in Semiconductor Floating-Zone Growth

NASA Technical Reports Server (NTRS)

Croll, Arne; Benz, K. W.

1999-01-01

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.

Internal morphology, habit and U-Th-Pb microanalysis of amphibolite-to-granulite facies zircons: geochronology of the Ivrea Zone (Southern Alps)

NASA Astrophysics Data System (ADS)

Vavra, Gerhard; Schmid, Rolf; Gebauer, Dieter

Several types of growth morphologies and alteration mechanisms of zircon crystals in the high-grade metamorphic Ivrea Zone (IZ) are distinguished and attributed to magmatic, metamorphic and fluid-related events. Anatexis of pelitic metasediments in the IZ produced prograde zircon overgrowths on detrital cores in the restites and new crystallization of magmatic zircons in the associated leucosomes. The primary morphology and Th-U chemistry of the zircon overgrowth in the restites show a systematic variation apparently corresponding to the metamorphic grade: prismatic (prism-blocked) low-Th/U types in the upper amphibolite facies, stubby (fir-tree zoned) medium-Th/U types in the transitional facies and isometric (roundly zoned) high-Th/U types in the granulite facies. The primary crystallization ages of prograde zircons in the restites and magmatic zircons in the leucosomes cannot be resolved from each other, indicating that anatexis in large parts of the IZ was a single and short lived event at 299+/-5Ma (95% c. l.). Identical U/Pb ages of magmatic zircons from a metagabbro (293+/-6Ma) and a metaperidotite (300+/-6Ma) from the Mafic Formation confirm the genetic context of magmatic underplating and granulite facies anatexis in the IZ. The U-Pb age of 299+/-5Ma from prograde zircon overgrowths in the metasediments also shows that high-grade metamorphic (anatectic) conditions in the IZ did not start earlier than 20Ma after the Variscan amphibolite facies metamorphism in the adjacent Strona-Ceneri Zone (SCZ). This makes it clear that the SCZ cannot represent the middle to upper crustal continuation of the IZ. Most parts of zircon crystals that have grown during the granulite facies metamorphism became affected by alteration and Pb-loss. Two types of alteration and Pb-loss mechanisms can be distinguished by cathodoluminescence imaging: zoning-controlled alteration (ZCA) and surface-controlled alteration (SCA). The ZCA is attributed to thermal and/or decompression pulses during extensional unroofing in the Permian, at or earlier than 249+/-7Ma. The SCA is attributed to the ingression of fluids at 210+/-12Ma, related to hydrothermal activity during the breakup of the Pangaea supercontinent in the Upper Triassic/Lower Jurassic.

Fe-Ti-oxide textures and microstructures in shear zones from oceanic gabbros at Atlantis Bank, Southwest Indian Ridge

NASA Astrophysics Data System (ADS)

Till, Jessica; Morales, Luiz F. G.; Rybacki, Erik

2016-04-01

Ocean drilling expeditions at several oceanic core complexes formed at slow- and ultra-slow-spreading ridges have recovered cores containing numerous zones of oxide-rich gabbros containing ilmenite and magnetite. In these cores, high modal concentrations of Fe-Ti-oxides are systematically associated with high-temperature plastic deformation features in silicates. We present observations of Fe-Ti-oxide mineral structures and textural characteristics from a series of oxide-rich shear zones from Atlantis Bank (ODP Site 735B) on the Southwest Indian Ridge aimed at determining how oxide mineral abundances relate to strain localization. Fe-Ti-oxide minerals in undeformed oxide gabbros and in highly deformed samples from natural shear zones generally have morphologies characteristic of crystallized melt, including highly cuspate grains and low dihedral angles. Anisotropy of magnetic susceptibility in oxide-rich shear zones is very strong, with fabrics mainly characterized by strong magnetic foliations parallel to the macroscopic foliation. Crystallographic preferred orientations (CPO) in magnetite are generally weak, with occasionally well-defined textures. Ilmenite typically displays well-developed CPOs, however, the melt-like ilmenite grain shapes indicate that at least part of the crystallographic texture results from oriented ilmenite growth during post-deformation crystallization. The oxides are hypothesized to have initially been present as isolated pockets of trapped melt (intercumulus liquid) in a load-bearing silicate framework. Progressive plastic deformation of silicate phases at high-temperature mainly produced two features: (i) elongated melt pockets, which crystallized to form strings of opaque minerals and (ii), interconnected networks of melt regions. The latter lead to intense strain localization of the rock, which appears as oxide-rich mylonites in the samples. In some samples, abundant low-angle grain boundaries in both magnetite and ilmenite suggest that deformation may have continued after crystallization of the late melt, imposing a weak strain on the oxides. Recent experimental deformation results indicate that magnetite and ilmenite should be weaker than most mafic silicates under anhydrous conditions. However, melt-like oxide morphologies observed in Atlantis Bank shear zones indicate that the redistribution of Fe-Ti-oxide melts may have more influence on the strength and strain localization behavior of oceanic gabbros than their solid-state rheology.

The Release of Trapped Gases from Amorphous Solid Water Films: I. “Top-Down” Crystallization-Induced Crack Propagation Probed using the Molecular Volcano

DOE Office of Scientific and Technical Information (OSTI.GOV)

May, Robert A.; Smith, R. Scott; Kay, Bruce D.

In this (Paper I) and the companion paper (Paper II) we investigate the mechanisms for the release of trapped gases from underneath of amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization ASW, a phenomenon that we termed the "molecular volcano". The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length and distributionmore » are independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2 or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ/mol. This value is consistent with the crystallization growth rate reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization/crack front into the film is in good agreement with the temperature programmed desorption results.« less

Crystal growth and scintillation properties of potassium strontium bromide

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Wei, H.; Melcher, C. L.

2015-08-01

In this work, potassium strontium bromide activated with divalent europium, (KSr2Br5:Eu) has been studied. It has a monoclinic crystal structure and a density of 3.98 g/cm3. Two single crystals of KSr2Br5 doped with 5% Eu2+, with diameters of 13 mm and 22 mm, were grown in a two zone transparent furnace via the Bridgman technique. The X-ray excited emission spectrum consisted of a single peak at ∼427 nm due to the 5d-4f transition in Eu2+. The measured light yield and energy resolution at 662 keV was 75,000 ph/MeV and 3.5%. At low energies KSr2Br5:Eu 5% also displays good energy resolution, 6.7% at 122 keV and 7.9% at 59.5 keV.

Optically induced melting of colloidal crystals and their recrystallization.

PubMed

Harada, Masashi; Ishii, Masahiko; Nakamura, Hiroshi

2007-04-15

Colloidal crystals melt by applying focused light of optical tweezers and recrystallize after removing it. The disturbed zone by the light grows radially from the focus point and the ordering starts from the interface with the crystal. Although the larger disturbed zone is observed for the higher power optical tweezers, a master curve is extracted by normalization of the disturbed zone. The temporal changes of the normalized disturbed zone are well described with exponential functions, indicating that the melting and recrystallization process is governed by a simple relaxation mechanism.

Researches on tungsten carbide

NASA Astrophysics Data System (ADS)

1994-11-01

This paper summarizes results of the researches on tungsten carbide (WC), carried out in the 5-year period starting 1989 by the Science and Technology Agency's National Institute for Researches in Inorganic Materials. The high-frequency heating, floating zone technique, generally suited for growth of large-size, single crystals of high melting materials, is inapplicable to the hexagonal WC system, which is decomposed. This problem has been solved by adding boron to the system, to allow it to exist with the W-C-B melt at an equilibrium. The computer-aided control techniques have enabled automatic growth of the single crystals of carbides and borides. The de Haas-Van Alphen effect of the single WC crystals has been observed, to establish the Fermi surface model. The single crystals of transition metal carbides, such as WC, have been coated with the monolayer of graphite at high repeatability, to create the surface layer materials. An attempt has been done to produce the halite type structure by substituting Ti as the atom in the outermost layer of TiC by W. The new method, based on the low-speed deuterium ion scattering, has been developed to analyze the surface bonding conditions, clarifying the conditions of alkalis adsorbed on and bonded to metallic surfaces, and their surface reactivities.

Skylab 3 and 4 science demonstrations: Preliminary report

NASA Technical Reports Server (NTRS)

Bannister, T. C.

1974-01-01

Twelve science demonstrations were accomplished on the Skylab 3 and 4 missions. These were defined in response to crew requests for time-gap fillers and were designed to be accomplished using onboard equipment. The following 12 are described and the preliminary results are given: liquid floating zone; diffusion in liquids; ice melting; immiscible liquids; liquid films; gyroscope; Rochelle salt growth; deposition of silver crystals; fluid mechanics series; neutron environment; orbital mechanics; and charged particle mobility.

Two-Step Vapor/Liquid/Solid Purification

NASA Technical Reports Server (NTRS)

Holland, L. R.

1986-01-01

Vertical distillation system combines in single operation advantages of multiple zone refining with those of distillation. Developed specifically to load Bridgman-Stockbarger (vertical-solidification) growth ampoules with ultrapure tellurium and cadmium, system, with suitable modifications, serves as material refiner. In first phase of purification process, ampoule heated to drive off absorbed volatiles. Second phase, evaporator heated to drive off volatiles in charge. Third phase, slowly descending heater causes distillation from evaporator to growing crystal in ampoule.

Development Of A Magnetic Directional-Solidification Furnace

NASA Technical Reports Server (NTRS)

Aldrich, Bill R.; Lehoczky, Sandor L.

1996-01-01

Report describes development of directional-solidification furnace in which axial magnetic field is imposed by surrounding ring permanent magnets and/or electromagnets and pole pieces. Furnace provides controlled axial temperature gradients in multiple zones, through which ampoule containing sample of material to be solidified is translated at controlled speed by low-vibration, lead-screw, stepping-motor-driven mechanism. Intended for use in low-gravity (spaceflight) experiments on melt growth of high-purity semiconductor crystals.

The effects of growth and collapse on the magmatic system below Mt Taranaki, New Zealand.

NASA Astrophysics Data System (ADS)

Procter, Jonathan; Marcroft, Grace; Zellmer, Georg; Zernack, Anke

2017-04-01

Mt. Taranaki exhibits one of the best long-term records of volcanic growth and destruction of any volcano worldwide, making it ideal for understanding the long-term effects of changing lithostatic pressure, or loading and unloading, on the magma chamber and magma supply. The ring-plain around Mt. Taranaki houses volcaniclastic deposits that provide a near continuous record of the evolution of the volcano, yet these records have remained relatively unexploited when investigating the interrelated cyclical phases of volcano collapse and growth, the geochemical evolution of the centre, and the consequent time-varying hazard potential. In this study, we systematically sampled pumice-rich tephra and pumice-rich mass flow deposits that were stratigraphically immediately before and after the 24,801 ± 268 years BP Pungarehu Formation debris avalanche ( 7.5 km3). Crystals (clinopyroxene and plagioclase) were characterised in detail. Mg and Fe zoning across selected crystals from samples pre-and post-debris avalanche were found to have completely equilibrated, yet zoning patterns in Al remained intact and showed major differences in their formation, allowing for the calculation of diffusion rates. These have enabled the determination of maximum residence times (depths and pressure regimes) of the magma system. It is intended that this technique will be applied across the stratigraphic record, which contains 14 collapse events. This will provide insights into crustal magma transport and residence times, and the propagation of fissures and the buoyancy of the magma pre- and post-collapse, in order to characterise the evolution of the centre and quantify the long-term relationship between magmatic rise and volcano growth and destruction.

Solid-state diffusion-controlled growth of the phases in the Au-Sn system

NASA Astrophysics Data System (ADS)

Baheti, Varun A.; Kashyap, Sanjay; Kumar, Praveen; Chattopadhyay, Kamanio; Paul, Aloke

2018-01-01

The solid state diffusion-controlled growth of the phases is studied for the Au-Sn system in the range of room temperature to 200 °C using bulk and electroplated diffusion couples. The number of product phases in the interdiffusion zone decreases with the decrease in annealing temperature. These phases grow with significantly high rates even at the room temperature. The growth rate of the AuSn4 phase is observed to be higher in the case of electroplated diffusion couple because of the relatively small grains and hence high contribution of the grain boundary diffusion when compared to the bulk diffusion couple. The diffraction pattern analysis indicates the same equilibrium crystal structure of the phases in these two types of diffusion couples. The analysis in the AuSn4 phase relating the estimated tracer diffusion coefficients with grain size, crystal structure, the homologous temperature of experiments and the concept of the sublattice diffusion mechanism in the intermetallic compounds indicate that Au diffuses mainly via the grain boundaries, whereas Sn diffuses via both the grain boundaries and the lattice.

Characterization of Structural Defects in Wide Band-Gap Compound Materials for Semiconductor and Opto-Electronic Applications

NASA Astrophysics Data System (ADS)

Goue, Ouloide Yannick

Single crystals of binary and ternary compounds are touted to replace silicon for specialized applications in the semiconductor industry. However, the relative high density of structural defects in those crystals has hampered the performance of devices built on them. In order to enhance the performance of those devices, structurally perfect single crystals must be grown. The aim of this thesis is to investigate the interplay between crystal growth process and crystal quality as well as structural defect types and transport property. To this end, the thesis is divided into two parts. The first part provides a general review of the theory of crystal growth (chapter I), an introduction to the materials being investigated (chapter II and III) and the characterization techniques being used (chapter IV). • In chapter I, a brief description of the theory of crystal growth is provided with an eye towards the driving force behind crystal nucleation and growth along with the kinetic factors affecting crystal growth. The case of crystal growth of silicon carbide (SiC) by physical vapor transport (PVT) and chemical vapor deposition (CVD) is discussed. The Bridgman, travelling heater method (THM) and physical transport growth of cadmium zinc telluride (CZT) is also treated. In chapters II and III, we introduce the compound materials being investigated in this study. While a description of their crystal structure and properties is provided, the issues associated with their growth are discussed. In chapter IV, a description of the characterization techniques used in these studies is presented. These techniques are synchrotron X-ray topography (SXRT), transmission electron microscopy, transmission infrared microscopy (TIM), micro-Raman spectroscopy (muRS) and light microscopy. Extensive treatment of SXRT technique is also provided. In the second part, the experimental results obtained in the course of these studies are presented and discussed. These results are divided into three subsections. • The development of a new technique for the production of large and high quality silicon carbide single crystal boule is proposed. This technique herein referred to as Large Tapered Crystal (LTC) growth consists of two steps: growth of long SiC rod crystal by solvent-laser heated floating zone (Solvent-LHFZ) and lateral expansion of a seed by hot wall chemical vapor deposition (HWCVD). Solvent-LHFZ was successful as SiC rod crystals, replicating the polytype structure of the starting seed, were achieved at a growth rate varying from 4 to 100mum/hr. However, SXRT revealed the presence of an inhomogeneous strain in the grown crystal rod. This was further confirmed by SEM images, which showed the platelet-like morphology of the growth front with pockets in which iron (Fe)-rich material from the Fe solvent is trapped. It was furthermore observed that at high Fe to Si ratio (˜1.9), no growth was achieved. HWCVD enlargement was also successful as SiC boules, replicating the polytype structure of the starting seed, were achieved at growth rate of about 180mum/hr. The boules had a faceted hexagonal morphology with a strain-free surface marked by steps. Combination of SXRT, TEM and muRS revealed the presence of stacking disorder in the seed (3C, 4H and 15R-SiC) that replicated in the homoepitaxial layer. The formation of the observed stacking disorder is attributed to the low energy difference between stacking configurations on the growth surface as proposed by Takahashi and Ohtani. • The influence of structural defect type and distribution on minority carrier lifetime in 4H-SiC epilayers was investigated. Structural defect type and distribution map was obtained using SXRT, whereas minority carrier lifetime map was obtained using muPCD. Decrease in carrier lifetime observed from muPCD map was associated with specific structural defects such as low angle grain boundaries (LAGBs), stacking faults (SFs), interfacial dislocations (IDs), half loop arrays (HLAs) as well as basal plane dislocations (BPDs) pinned at TSDs. While the effect of morphological defects was mitigated, combination of defects such as microcracks, overlapping triangular defects and BPD half loops were observed to reduce carrier lifetime. Furthermore, regions of high dislocation density were associated with low carrier lifetime. • Finally, the effect of cadmium (Cd) overpressure on the quality of cadmium zinc telluride crystal ingots was investigated for two set of samples (set 1 and 2). Overall, high resistivity single crystals were achieved. Evaluation of the crystal quality by SXRT revealed that under certain Cd overpressures and growth conditions, the quality of the grown boule improved. Similarly, transmission infrared (IR) microscopy showed a correlation between the size/density and distribution of Te inclusions/precipitates and Cd overpressure. The size of Te inclusions was observed to decrease as a function of Cd overpressure as predicted from partial pressure data for stoichiometric melt. The best improvement in crystalline quality were observed for samples from set 1at a Cd reservoir of 785 °C and for set 2 samples for a Cd reservoir at 825 °C. This difference in Cd reservoir temperature for stoichiometric growth between set 1 and set 2 was attributed to other factors such as rate of cooling of Cd reservoir, rate of cooling of the crystal along with control of the melt interface. The summary of these results and the implication of this growth approach for producing high quality CZT single crystals are discussed.

Protein crystal growth; Proceedings of the First International Conference, Stanford University, CA, August 14-16, 1985

NASA Technical Reports Server (NTRS)

Feigelson, R. S. (Editor)

1986-01-01

Papers are presented on mechanisms of nucleation and growth of protein crystals, the role of purification in the crystallization of proteins and nucleic acids, and the effect of chemical impurities in polyethylene glycol on macromolecular crystallization. Also considered are growth kinetics of tetragonal lysozyme crystals, thermodynamic and kinetic considerations for crystal growth of complex molecules from solution, protein single-crystal growth under microgravity, and growth of organic crystals in a microgravity environment. Papers are also presented on preliminary investigations of protein crystal growth using the Space Shuttle, convective diffusion in protein crystal growth, and the growth and characterization of membrane protein crystals.

Garnet cannibalism provides clues to extensive hydration of lower crustal fragments in a subduction channel (Sesia Zone, Northwestern Alps)

NASA Astrophysics Data System (ADS)

Giuntoli, Francesco; Lanari, Pierre; Engi, Martin

2015-04-01

The extent to which granulites are transformed to eclogites is thought to impose critical limits on the subduction of continental lower crust. Although it is seldom possible to document such densification processes in detail, the transformation is believed to depend on fluid access and deformation. Remarkably complex garnet porphyroblasts are widespread in eclogite facies micaschists in central parts of the Sesia Zone (Western Italian Alps). They occur in polydeformed samples in assemblages involving phengite+quartz+rutile ±paragonite, Na-amphibole, Na-pyroxene, chloritoid. Detailed study of textural and compositional types reveals a rich inventory of growth and partial resorption zones in garnet. These reflect several stages of the polycyclic metamorphic evolution. A most critical observation is that the relict garnet cores indicate growth at 900 °C and 0.9 GPa. This part of the Eclogitic Micaschist Complex thus derived from granulite facies metapelites of Permian age. These dry rocks must have been extensively hydrated during Cretaceous subduction, and garnet records the conditions of these processes. Garnet from micaschist containing rutile, epidote, paragonite and phengite were investigated in detail. Two types of garnet crystals are found in many thin sections: mm-size porphyroclasts and smaller atoll garnets, some 100 µm in diameter. X-ray maps of the porphyroclasts show complex zoning in garnet: a late Paleozoic HT-LP porphyroclastic core is overgrown by several layers of HP-LT Alpine garnet, these show evidence of growth at the expense of earlier garnet generations. Textures indicate 1-2 stages of resorption, with garnet cores that were fractured and then sealed by garnet veins, rimmed by multiple Alpine overgrowth rims with lobate edges. Garnet rim 1 forms peninsula and embayment structures at the expense of the core. Rim 2 surrounds rim 1, both internally and externally, and seems to have grown mainly at the expense of the core. Rim 3 grew mainly at the expense of earlier Alpine rims. In the same samples that show porphyroclastic garnet, atoll garnet occurs, filled with quartz, and the same Alpine overgrowth zones are observed in both types of garnet. Similar features of garnet zoning are present in various lithotypes, allowing the evolution of this continental domain during subduction to be traced. Modeling the different garnet growth zones is challenging, each growth step demanding an estimate the effective bulk composition. According to the XRF analyses of the bulk sample, the core is found to have formed at 900°C, 0.9 GPa. Based on effective bulk compositions, the successive Alpine rims are found to reflect an increase from 600°C, 1.55-1.60 GPa for rim 1 to 630-640°C, 1.9-2.0 GPa for rim 2. Allanite crystals contain inclusions of Alpine garnet; in situ geochronology (U-Th-Pb by LA-ICP-MS) on allanite yields a (minimum) age of ~69 Ma for the main growth of garnet. In summary, the textures and mineral compositions clearly reflect reactive interaction of major amounts of hydrous fluids with dry protoliths. The source of these fluids responsible for converting granulites back to micaschists at eclogite facies conditions within the Sesia subduction channel is being investigated.

Understanding Ice Supersaturation, Particle Growth, and Number Concentration in Cirrus Clouds

NASA Technical Reports Server (NTRS)

Comstock, Jennifer M.; Lin, Ruei-Fong; Starr, David O'C.; Yang, Ping

2008-01-01

Many factors control the ice supersaturation and microphysical properties in cirrus clouds. We explore the effects of dynamic forcing, ice nucleation mechanisms, and ice crystal growth rate on the evolution and distribution of water vapor and cloud properties in nighttime cirrus clouds using a one-dimensional cloud model with bin microphysics and remote sensing measurements obtained at the Department of Energy's Atmospheric Radiation Measurement (ARM) Climate Research Facility located near Lamont, OK. We forced the model using both large-scale vertical ascent and, for the first time, mean mesoscale velocity derived from radar Doppler velocity measurements. Both heterogeneous and homogeneous nucleation processes are explored, where a classical theory heterogeneous scheme is compared with empirical representations. We evaluated model simulations by examining both bulk cloud properties and distributions of measured radar reflectivity, lidar extinction, and water vapor profiles, as well as retrieved cloud microphysical properties. Our results suggest that mesoscale variability is the primary mechanism needed to reproduce observed quantities. Model sensitivity to the ice growth rate is also investigated. The most realistic simulations as compared with observations are forced using mesoscale waves, include fast ice crystal growth, and initiate ice by either homogeneous or heterogeneous nucleation. Simulated ice crystal number concentrations (tens to hundreds particles per liter) are typically two orders of magnitude smaller than previously published results based on aircraft measurements in cirrus clouds, although higher concentrations are possible in isolated pockets within the nucleation zone.

Laser-zone growth in a Ribbon-To-Ribbon, RTR, process silicon sheet growth development for the large area silicon sheet task of the low cost silicon solar array project

NASA Technical Reports Server (NTRS)

Gurtler, R. W.; Baghdadi, A.

1977-01-01

A ribbon-to-ribbon process was used for routine growth of samples for analysis and fabrication into solar cells. One lot of solar cells was completely evaluated: ribbon solar cell efficiencies averaged 9.23% with a highest efficiency of 11.7%. Spherical reflectors have demonstrated significant improvements in laser silicon coupling efficiencies. Material analyses were performed including silicon photovoltage and open circuit photovoltage diffusion length measurements, crystal morphology studies, modulus of rupture measurements, and annealing/gettering studies. An initial economic analysis was performed indicating that ribbon-to-ribbon add-on costs of $.10/watt might be expected in the early 1980's.

Timing of anatexis and melt crystallization in the Socorro-Guaxupé Nappe, SE Brazil: Insights from trace element composition of zircon, monazite and garnet coupled to Usbnd Pb geochronology

NASA Astrophysics Data System (ADS)

Rocha, B. C.; Moraes, R.; Möller, A.; Cioffi, C. R.; Jercinovic, M. J.

2017-04-01

The timing of partial melting and melt crystallization in granulite facies rocks of the Socorro-Guaxupé Nappe (SGN), Brazil is constrained using a combination of imaging techniques, LA-ICP-MS and EPMA dating, trace element geochemistry and thermobarometry. (Orthopyroxene)-garnet-bearing migmatite that records extensive biotite dehydration melting shows evidence for a clockwise P-T-t path. UHT peak conditions were attained at 1030 ± 110 °C, 11.7 ± 1.4 kbar, with post-peak cooling to 865 ± 38 °C, 8.9 ± 0.8 kbar. Cryogenian igneous inheritance of ca. 720-640 Ma is identified in oscillatory zoned zircon cores (n = 167) with steep HREE patterns. Resorbed, Y-rich monazite cores preserve a prograde growth stage at 631 ± 4 Ma prior to the partial melting event, providing an upper age limit for the granulite facies metamorphism in the SGN. REE-rich, Th-depleted monazite related to apatite records the initial stages of decompression at 628 ± 4 Ma. Multiple monazite growth episodes record melt crystallization events at 624 ± 3 Ma, 612 ± 5 Ma and 608 ± 6 Ma. Stubby, equant "soccer ball" zircon provide evidence for melt crystallization at 613 ± 2 Ma and 607 ± 4 Ma. The excess scatter in zircon and monazite age populations between 629 ± 4 and 601 ± 3 Ma is interpreted as discontinuous and episodic growth within this age range, characterizing a prolonged metamorphic event in the SGN lasting ca. 30 m.y. The development of Y + HREE-rich monazite rims at ca. 600 Ma documents retrograde garnet breakdown, extensive biotite growth and the final stages of melt crystallization. Th-rich, Y + HREE-poor monazite rims at ca. 590 Ma record monazite recrystallization.

Hydrothermal quartz formation during fluctuations of brittle shear-zone activity and fluid flow: grain growth and deformation structures of the Pfahl shear zone (Germany)

NASA Astrophysics Data System (ADS)

Yilmaz, T.; Prosser, G.; Liotta, D.; Kruhl, J. H.

2012-12-01

The Bavarian Pfahl shear zone is a WNW-ESE trending dextral strike-slip shear zone at the SW margin of the Bohemian Massif (Central Europe). It was discontinuously active during decreasing PT-conditions, i.e. from ductile to brittle, from the late-Carboniferous to the late-Cretaceous - Paleocene times. Triassic hydrothermal activity produced a 150 km long and 30-100 m wide quartz dyke along the main fault, surrounded by sheared basement rocks. Within a zone of >10 m metasomatism transformed the wall rocks to mostly kaolinite, chlorite and phyllosilicates. The quartz dyke exhibits a layered to lenticular and partly symmetric structure with different types of quartz masses, transected by a complex quartz vein network. This already indicates pulses of fluid flux and fragmentation during the lifetime of the shear zone. Analyses by optical microscopy, cathodoluminescence (CL) and SEM-EDX reveal at least four subsequent stages of quartz crystallization and fragmentation. (i) The oldest generation of quartz is represented by a homogeneous dark grey to reddish quartz mass made up by ~10-20 μm-sized crystals. It contains mm- to cm-sized angular wall-rock fragments, completely altered to kaolinite, indicating intense wall-rock alteration prior to the earliest event of silica precipitation. This rules out the possibility that the quartz mass developed from silicification of the wall rocks. This first type of quartz occurs as cm- to dm-large angular fragments in (ii) a light grey to pink quartz mass formed by ~10-50 μm-sized crystals. The different colours result from variable types and amounts of inclusions. Quartz of both generations shows random crystallographic orientations and complex inclusion structures. It probably developed during two fragmentation events and possibly from a silica gel precursor that crystallized after precipitation. (iii) The third quartz generation formed as a set of mm- to dm-wide veins roughly parallel to the trend of the Pfahl zone, crosscutting the first generations of fine-grained quartz mass and the wall rocks, in connection to intense fracturing and brecciation. The complex geometry of the vein sets points to multiple fluid injections and brecciation, as additionally indicated by coarse quartz with different inclusion and CL intensity. Temporal changes of strain rate are indicated by crystal plastic deformation structures in quartz, which overprint brittle structures. (iv) The fourth quartz generation occurs in mm- to dm-thick quartz veins, partly open as geodes, filling N-S oriented cm- to dm-spaced fractures that crosscut the earlier quartz masses and veins and extend at least several meters into the wall rock. They indicate the last activity of the shear-zone in a constant kinematic framework. Summarizing, the Pfahl shear zone shows brittle-ductile deformation during the long-term activity of a large-scale hydrothermal system. Consequently, it represents an excellent example where different generations of quartz precipitation can be connected to fluctuations of fluid flow and strain rate.

Interdiffusion behavior between NiAlHf coating and Ni-based single crystal superalloy with different crystal orientations

NASA Astrophysics Data System (ADS)

Wang, Ruili; Gong, Xueyuan; Peng, Hui; Ma, Yue; Guo, Hongbo

2015-01-01

NiAlHf coatings were deposited onto Ni-based single crystal (SC) superalloy with different crystal orientations by electron beam physical vapor deposition (EB-PVD). The effects of the crystal orientations of the superalloy substrate on inter-diffusion behavior between the substrate and the NiAlHf coating were investigated. Substrate diffusion zone (SDZ) containing needle-like μ phases and interdiffusion zone (IDZ) mainly consisting of the ellipsoidal and rod-like μ phases were formed in the SC alloy after heat-treatment 10 h at 1100 °C. The thickness of secondary reaction zone (SRZ) formed in the SC alloy with (0 1 1) crystal orientation is about 14 μm after 50 h heat-treatment at 1100 °C, which is relatively thicker than that in the SC alloy with (0 0 1) crystal orientation, whereas the IDZ revealed similar thickness.

Viewing zone duplication of multi-projection 3D display system using uniaxial crystal.

PubMed

Lee, Chang-Kun; Park, Soon-Gi; Moon, Seokil; Lee, Byoungho

2016-04-18

We propose a novel multiplexing technique for increasing the viewing zone of a multi-view based multi-projection 3D display system by employing double refraction in uniaxial crystal. When linearly polarized images from projector pass through the uniaxial crystal, two possible optical paths exist according to the polarization states of image. Therefore, the optical paths of the image could be changed, and the viewing zone is shifted in a lateral direction. The polarization modulation of the image from a single projection unit enables us to generate two viewing zones at different positions. For realizing full-color images at each viewing zone, a polarization-based temporal multiplexing technique is adopted with a conventional polarization switching device of liquid crystal (LC) display. Through experiments, a prototype of a ten-view multi-projection 3D display system presenting full-colored view images is implemented by combining five laser scanning projectors, an optically clear calcite (CaCO₃) crystal, and an LC polarization rotator. For each time sequence of temporal multiplexing, the luminance distribution of the proposed system is measured and analyzed.

Pre-eruption recharge of the Bishop magma system

USGS Publications Warehouse

Wark, D.A.; Hildreth, W.; Spear, F.S.; Cherniak, D.J.; Watson, E.B.

2007-01-01

The 650 km3 rhyolitic Bishop Tuff (eastern California, USA), which is stratigraphically zoned with respect to temperatures of mineral equilibration, reflects a corresponding thermal gradient in the source magma chamber. Consistent with previous work, application of the new TitaniQ (Ti-in-quartz) thermometer to quartz phenocryst rims documents an ???100 ??C temperature increase with chamber depth at the time of eruption. Application of TitaniQ to quartz phenocryst cores, however, reveals lower temperatures and an earlier gradient that was less steep, with temperature increasing with depth by only ???30 ??C. In many late-erupted crystals, sharp boundaries that separate low-temperature cores from high-temperature rims cut internal cathodoluminescent growth zoning, indicating partial phenocryst dissolution prior to crystallization of the high-temperature rims. Rimward jumps in Ti concentration across these boundaries are too abrupt (e.g., 40 ppm across a distance of <10 ??m) to have survived magmatic temperatures for more than ???100 yr. We interpret these observations to indicate heating-induced partial dissolution of quartz, followed by growth of high-temperature rims (made possible by lowering of water activity due to addition of CO2) within 100 yr of the climactic 760 ka eruption. Hot mafic melts injected into deeper parts of the magma system were the likely source of heat and CO2, raising the possibility that eruption and caldera collapse owe their origin to a recharge event. ?? 2007 Geological Society of America.

Experimentally determined isotope effect during Mg-Fe interdiffusion in olivine

NASA Astrophysics Data System (ADS)

Sio, C. K. I.; Roskosz, M.; Dauphas, N.; Bennett, N.; Mock, T. D.; Shahar, A.

2017-12-01

Isotopic fractionation provides the most direct means to investigate the nature of chemical zoning in minerals, which can be produced by either diffusive transport or crystal growth. Misinterpreting the nature of chemical zoning can result in erroneous conclusions regarding magmatic cooling rates and diffusion timescales. Isotopes are useful in this regard because the light isotopes diffuse faster than their heavier counterparts. As a result, isotopic fractionations should be associated with chemical zoning profiles if they are diffusion-driven. In contrast, little isotopic fractionation is associated with crystal growth during slow cooling at magmatic temperatures. The isotope effect for diffusion is described by β and is related to the mass (m) and diffusivity (D) of isotopes i and j of an element via: Di/Dj = (mj/mi)β. To model isotopic profiles, knowledge of β is required. Several estimates of β for Mg and Fe diffusion in olivine have been reported using natural samples but these estimates are uncertain because they depend on the choice of modeling parameters (Sio et al., 2013; Oeser et al., 2015; Collinet et al., 2017). We have experimentally determined β for Fe (βFe) in olivine as a function of crystallographic orientation, composition, and temperature. Thirty experiments have been conducted by juxtaposing crystallographically oriented olivine crystals to make Fo83.4-Fo88.8 and Fo88.8-Fo100 diffusion couples. These diffusion couples were annealed in a 1 atm gas mixing furnace at 1200 °C, 1300 °C or 1400 °C at QFM - 1.5 for up to 15 days. Chemical profiles were characterized using an electron microprobe and isotopic analyses were done using laser ablation MC-ICPMS. We found a crystallographic dependence of βFe for the Fo88.8-Fo100 couple where βFe [100] ≈ βFe [010] > βFe [001]. For the Fo83.4-Fo88.8 couple, βFe is 0.16 ± 0.09 (2σ) for all 3 major crystallographic axes. A temperature dependence of βFe could not be resolved. These experimentally determined β-values can be used in conjunction with the Mg-Fe diffusivities given in Dohmen and Chakraborty (2007) to simultaneously model the chemical-isotopic profiles of olivine to retrieve cooling and crystallization histories of magmatic rocks.

Lithium Zoning in Kīlauea Olivine: Growth vs. Diffusion?

NASA Astrophysics Data System (ADS)

Shea, T.; Lynn, K. J.; Garcia, M. O.; Costa Rodriguez, F.

2016-12-01

Lithium is a fast-diffusing element with the potential to characterize magmatic processes that occur on timescales of hours to days [1]. However, Li diffusion in olivine is complex. Experimental studies show that it can diffuse via two paths: a `fast' interstitial mechanism and a `slow' vacancy mechanism [1]. Charge balancing relationships with other incompatible trace elements may also play a role in Li diffusion [2]. A detailed study of lithium zoning in natural olivine was undertaken to better understand how Li is correlated with other trace elements and determine if Li diffusion profiles can be used to extract meaningful timescales of magmatic processes. Olivine crystals from the Keanakāko`i explosive period at Kīlauea Volcano (HI) were used in this study because (a) the lavas and tephra generally contain phenocrysts of only olivine in a rapidly quenched glass, which avoid complications of multi-phase systems and post-eruptive diffusion; (b) we previously constrained the magmatic histories of these crystals using major and minor elements; and (c) at concentrations (e.g. 1-10 ppm) and temperatures (e.g. 1150-1250 °C) typical of Kīlauea basalts, Li diffusion is probably dominated by the vacancy mechanism [1]. Euhedral crystals were carefully oriented and mounted on either the a- or b- crystallographic axes (c-axis is always within the plane of section) and polished to the crystal core. High precision LA-ICP-MS analyses of Li (2σ = 0.08 ppm), Na, Al, P, and Cr complement EPMA profiles of Si, Mg, Fe, Ni, and Ca (200 nA current). Core-to-rim transects were collected along two axes (c and a or b) to identify potential diffusion anisotropy effects for Li and other elements. Li zoning is correlated with Na, indicative of a growth signature (also observed for Al, P, and Cr), or is decoupled from incompatible trace elements and have profiles that indicate diffusive re-equilibration. Modeling of Li diffusion profiles yields timescales of hours to days, which probably represent the final stages of magma transport from crustal magma reservoirs and allow ascent rates to be estimated. [1] Dohmen et al. (2010), Geochimica et Cosmochimica Acta, 74, 274-292. [2] Spandler and O'Neill (2010), Contributions to Mineralogy and Petrology, 159, 791-818.

Amphibole-bearing multiphase solid inclusions in olivine, the Murotomisaki Gabbro, Southwest Japan: An evidence of hydrous flux melting

NASA Astrophysics Data System (ADS)

Hoshide, T.; Obata, M.

2009-12-01

The Murotomisaki Gabbro is a sill-like layered intrusion of up to 220m thickness exposed near Cape Muroto, Southwest Japan. Despite the small size of the intrusion, it contains well-developed centimeter- to meter-scale layered structures of modal variation of olivine, plagioclase and augite. Hoshide et al (2006a, b) identified the ’crystal accumulation zone’ (40m from the bottom) that was formed by gravitational settling of olivine crystals and the ’crystal growth zone’ (40-100m from the bottom), in which olivine crystals grew significantly. The fine-scale compositional layering is best developed in the ’crystal growth zone’. Amphibole-bearing multiphase solid inclusions (called ‘the amphibole-clot inclusions’) are common in olivine crystals from both the crystal accumulation- and the crystal growth zones. The amphibole clot inclusions show spherical or convex-polygonal shapes and are composed of pargasitic amphibole, biotite and orthopyroxene, with minor amounts of augite, apatite and opaque minerals. Plagioclase rarely occurs in the amphibole clot inclusions. Bulk chemical compositions of the inclusions, obtained from mineral microprobe analyses and modal composition, are characteristically high in MgO content (16-23 wt %) and they roughly lie between presumable fractionated melt compositions and olivine compositions. From observations above, it is likely that amphibole clot inclusions are of melt origin, which had formed from some hydrous melts probably entrapped in growing olivine crystals. However, it may be difficult to explain both the very magnesian nature of the inclusion and absence of plagioclase in the inclusion by the crystallization of the normal hydrous basaltic melt. The difficulty may be resolved if we suppose, for a trapped melt composition, a more magnesian (i.e., picritic) composition. The highly magnesian nature of the amphibole clot inclusions may suggest that significant amount of olivine component had been added to fractionated melts that was once equilibrated with olivine. Such addition of olivine component may be realized by dissolution of olivine, which may be induced by introduction of water from the lower horizons of the crystallization boundary layer (e.g., McBirney, 1987). Amphibole clot inclusion in olivine is, therefore, considered to be a new evidence for dissolution of olivine by hydrous fluxing.

Hiding the Evidence: Growth of plutons by incremental emplacement of sheets in crystal mush

NASA Astrophysics Data System (ADS)

Miller, C. F.; Furbish, D. J.; Claiborne, L. L.; Walker, B. A.; Bleick, H. A.; Steinwinder, T. R.; Koteas, G. C.

2006-12-01

Growing evidence supports the notion that plutons are constructed incrementally, commonly over long periods of time, yet field evidence for the multiple injections that seem to be required is commonly sparse or absent (e.g. Glazner et al. 2004). Timescales of up to several million years, among other arguments, indicate that the dominant volume does not remain largely molten, yet if growing plutons are constructed from rapidly solidifying increments it is unlikely that intrusive contacts would escape notice. A model wherein magma increments are emplaced into crystal mush rather than either solid or crystal-poor material provides a plausible explanation for this apparent conundrum. A partially solidified intrusion undoubtedly comprises zones with contrasting melt fraction and therefore strength. The emplacement of dikes that intrude such a strength-zoned intrusion will be guided by the contrasts in the same way that dikes intruding solid media: magma spreads rather than continuing to propagate upward where it encounters a zone of higher rigidity (e.g. experiments by Kavanagh et al. 2006). We propose that ascending magma is in essence trapped by low-strength zones in plutonic mushes that are relatively melt-rich. In many cases, such zones may be subhorizontal and thus sill-like in geometry, but shapes and orientations could be highly variable, depending on the prior history of the composite intrusion. Contacts will commonly be obscure from the start because the contrast between intruding material (crystal-poorer magma) and host (crystal-richer mush) is subtle, and it may be obscured even further by subsequent destabilization of the mush. Field evidence and zircon zoning stratigraphy in plutons of the Colorado River region of southern Nevada support the hypothesis that emplacement of magma replenishments into a mush host is important in pluton construction. Except for highly fractionated dikes and sills, the dominant granite unit of the Spirit Mountain batholith displays only subtle internal contacts. However, ages and elemental zoning in zircons demonstrate a protracted history of almost 2 million years, major fluctuations in T and host melt chemistry, and mixing of strongly contrasting zircon populations in single samples (Walker et al. in press; Claiborne et al. in press). We interpret this to reflect reactivation of mushes and entrainment of earlier-formed crystals, and we infer that this was in response to granitic replenishment. Much of the smaller Aztec Wash pluton comprises interlayered cumulate-textured quartz monzonite and mafic sheets. The latest phase of pluton emplacement is marked by numerous thick granite "sills" that intruded the subhorizontal quartz monzonite sheets. Contacts between granite and quartz monzonite are "soft," highly irregular on cm-dm scale with coarse xenocrysts from the quartz monzonite entrained in the fine-grained granite. We interpret the granite replenishments to have spread laterally within mushy, melt-bearing quartz monzonite, beneath rigid mafic sheets. In this case, clear evidence for the emplacement process is fortuitously preserved because the granite was emplaced in the waning stage of thermal lifetime of the pluton, and because the mafic sheets enhance the strength contrast and make the geometry more visible.

Detailed analysis of Honeywell In-Space Accelerometer data - STS-32. [crystal microstructure response to different types of residual acceleration

NASA Technical Reports Server (NTRS)

Rogers, Melissa J. B.; Alexander, J. I. D.; Schoess, Jeff

1993-01-01

The Honeywell In-Space Accelerometer (HISA) system collected data in the mid-deck area of the Shuttle Columbia during the flight of STS-32, January 1990. The resulting data were to be used to investigate the response of crystal microstructure to different types of residual acceleration. The HISA is designed to detect and record transient and oscillatory accelerations. The sampling and electronics package stored averaged accelerations over two sampling periods; two sampling rates were available: 1 Hz and 50 Hz. Analysis of the HISA data followed the CMMR Acceleration Data Processing Guide, considering in-house computer modelling of a float-zone indium crystal growth experiment. Characteristic examples of HISA data showing the response to the primary reaction control system, Orbiter Maneuvering System operations, and crew treadmill activity are presented. Various orbiter structural modes are excited by these and other activities.

Scanning electron microscope observations of sublimates from Merapi Volcano, Indonesia

USGS Publications Warehouse

Symonds, R.

1993-01-01

Sublimates were sampled from high-temperature (up to 800??C) fumaroles at Merapi volcano in January 1984. Sampling is accomplished by inserting silica tubes into high-temperature vents. Volcanic glass flows through the tubes and sublimates precipitate on the inner walls in response to the temperature gradient. With decreasing temperature (800-500??C) in the tubes, there are five sublimate zones. Texturally, the sublimate phases grade from large, well-formed crystals at their highest-temperature occurrence to more numerous, smaller crystals that are less perfect at lower temperatures. These changes imply that the crystal nucleation and growth rates increase and decrease, respectively, as temperature decreases. Overall, the textural data suggest that the gas is saturated or slightly super-saturated with the phases at their hottest occurrence, but that the gas becomes increasingly super-saturated with the phases at lower temperatures. -from Author

Crystal Growth and Scintillation Properties of $${\\rm Cs}_{2}{\\rm NaGdBr}_{6}{:}{\\rm Ce}^{3+}$$

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Pin; Zhou, Xiaowang; Deng, Haoran

2013-04-02

Single crystals of Cs 2NaGdBr 6 with different Ce +3 activator concentrations were grown by a two-zone Bridgman method. This new compound belongs to a large elpasolite halide (A 2BLnX 6) family. Many of these elpasolite compounds have shown high luminosity, good energy resolution and excellent proportionality in comparison to traditional scintillators such as CsI and NaI; therefore, they are particularly attractive for gamma-ray spectroscopy applications. This study investigated the scintillator properties of Cs 2NaGdBr 6:Ce +3 crystals as a new material for radiation detection. Special focus has been placed on the effects of activator concentration (0 to 50 mol.%)more » on the photoluminescence responses. Results of structural refinement, photoluminescence, radioluminescence, lifetime and proportionality measurements for this new compound are reported.« less

Quality of Heusler single crystals examined by depth-dependent positron annihilation techniques

NASA Astrophysics Data System (ADS)

Hugenschmidt, C.; Bauer, A.; Böni, P.; Ceeh, H.; Eijt, S. W. H.; Gigl, T.; Pfleiderer, C.; Piochacz, C.; Neubauer, A.; Reiner, M.; Schut, H.; Weber, J.

2015-06-01

Heusler compounds exhibit a wide range of different electronic ground states and are hence expected to be applicable as functional materials in novel electronic and spintronic devices. Since the growth of large and defect-free Heusler crystals is still challenging, single crystals of Fe2TiSn and Cu2MnAl were grown by the optical floating zone technique. Two positron annihilation techniques—angular correlation of annihilation radiation and Doppler broadening spectroscopy (DBS)—were applied in order to study both the electronic structure and lattice defects. Recently, we succeeded to observe clearly the anisotropy of the Fermi surface of Cu2MnAl, whereas the spectra of Fe2TiSn were disturbed by foreign phases. In order to estimate the defect concentration in different samples of Heusler compounds, the positron diffusion length was determined by DBS using a monoenergetic positron beam.

The release of trapped gases from amorphous solid water films. I. "Top-down" crystallization-induced crack propagation probed using the molecular volcano.

PubMed

May, R Alan; Smith, R Scott; Kay, Bruce D

2013-03-14

In this (Paper I) and the companion paper (Paper II; R. May, R. Smith, and B. Kay, J. Chem. Phys. 138, 104502 (2013)), we investigate the mechanisms for the release of trapped gases from underneath amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization of ASW, a phenomenon that we termed the "molecular volcano." The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper, we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length distribution is independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2, or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ∕mol. This value is consistent with the crystallization growth rates reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization∕crack front into the film is in good agreement with the temperature programmed desorption results.

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Static Magnetic Fields

NASA Technical Reports Server (NTRS)

Jauss, T.; SorgenFrei, T.; Croell, A.; Azizi, M.; Reimann, C.; Friedrich, J.; Volz, M. P.

2014-01-01

In the photovoltaics industry, the largest market share is represented by solar cells made from multicrystalline silicon, which is grown by directional solidification. During the growth process, the silicon melt is in contact with the silicon nitride coated crucible walls and the furnace atmosphere which contains carbon monoxide. The dissolution of the crucible coating, the carbon bearing gas, and the carbon already present in the feedstock, lead to the precipitation of silicon carbide, and silicon nitride, at later stages of the growth process. The precipitation of Si3N4 and SiC particles of up to several hundred micrometers in diameter leads to severe problems during the wire sawing process for wafering the ingots. Furthermore the growth of the silicon grains can be negatively influenced by the presence of particles, which act as nucleation sources and lead to a grit structure of small grains and are sources for dislocations. If doped with Nitrogen from the dissolved crucible coating, SiC is a semi conductive material, and can act as a shunt, short circuiting parts of the solar cell. For these reasons, the incorporation of such particles needs to be avoided. In this contribution we performed model experiments in which the transport of intentionally added SiC particles and their interaction with the solid-liquid interface during float zone growth of silicon in strong steady magnetic fields was investigated. SiC particles of 7µm and 60µm size are placed in single crystal silicon [100] and [111] rods of 8mm diameter. This is achieved by drilling a hole of 2mm diameter, filling in the particles and closing the hole by melting the surface of the rod until a film of silicon covers the hole. The samples are processed under a vacuum of 1x10(exp -5) mbar or better, to prevent gas inclusions. An oxide layer to suppress Marangoni convection is applied by wet oxidation. Experiments without and with static magnetic field are carried out to investigate the influence of melt convection on the distribution of particles and their incorporation into the crystal. The field strengths applied by a superconducting magnet are 1T, 3T, 4.5T, and 5T. The increase in field strength dampens the melt flow, and so this study provides comparative data to the crystal growth experiment to be carried out onboard the sounding rocket mission TEXUS 51, where purely diffusive growth condition will be achieved under microgravity conditions.

Can isotopic variations in structural water of gypsum reveal paleoclimatic changes?

NASA Astrophysics Data System (ADS)

Gatti, E.; Bustos, D.; Coleman, M. L.

2015-12-01

Water of crystallization in gypsum can be used as paleo-environmental proxy to study large scale climatic variability in arid areas. This is because changes in the isotopic composition of water of crystallization are due to isotopic variations in the mother brine from which the mineral precipitated, and the brine isotopic composition is linked to evaporation processes and humidity. This is particularly important when the salts are the only traces left of the original water, i.e. in modern arid areas. This study aims to prove that the 2-D/18-O compositions of the water of crystallization extracted from successive precipitates or even different growth zones of natural gypsum (CaSO4·H2O) can reconstruct the evaporation history and paleo-humidity of the source water basin. The method was tested in a laboratory experiment that evaporated CaSO4 brines under controlled temperature and humidity conditions. The brine was left to evaporate for five days at two different humidities (45 and 75 RH%); subsequently, brines and precipitated gypsum were sampled at 24 hour intervals. In this way we simulated zoned growth of gypsum. The samples were then analyzed for oxygen and hydrogen isotopic composition using a Thermo Scientific TC/EA with modified column, coupled to a MAT 253 Thermo Finnigan mass spectrometer at JPL. If preliminary results validate the novel hypothesis that changes in mineral composition can reveal details of paleo-environmental conditions the theory will be tested on natural gypsum collected from selected areas in White Sands National Monument, New Mexico. The study is currently ongoing but the full dataset will be presented at the conference.

Dermal miconazole nitrate nanocrystals - formulation development, increased antifungal efficacy & skin penetration.

PubMed

Pyo, Sung Min; Hespeler, David; Keck, Cornelia M; Müller, Rainer H

2017-10-05

Miconazole nitrate nanosuspension was developed to increase its antifungal activity and dermal penetration. In addition, the nanosuspension was combined with the synergistic additive chlorhexidine digluconate. The production was performed by wet bead milling and both production and formulation parameters were optimized. A stabilizer screening revealed poloxamer 407 and Tween 80 both at 0.15% as the most effective stabilizers for miconazole nanosuspensions at 1.0%. The nanocrystals were incorporated into a hydroxypropyl cellulose gel base. Short-term stability (3months) of the nanocrystal bulk population could be shown at room temperature and fridge. Besides the stable bulk nanocrystals, some longitudinal crystal growth to needle like crystals occurred. The addition of ionic compounds as the chlorhexidine digluconate often destabilizes suspensions. Surprisingly here, the addition minimized the crystal growth. An underlying mechanism is proposed. An inhibition zone assay was performed using Candida albicans (ATCC ® 10231™). When comparing the nanocrystals in suspension and in gel to μm-sized miconazole nitrate formulations and two market products, the increase in inhibition zone diameter for the nanosuspension formulations was most pronounced in the chlorhexidine digluconate free formulations. These nanocrystal formulations were closely or similarly effective as the microsuspensions and the market products containing the synergistic chlorhexidine digluconate, showing the potential of the nanosuspension formulation. Nanosuspension performance was even further increased when chlorhexidine digluconate was added. Ex-vivo skin penetration studies on porcine ears revealed distinctly less remaining miconazole nitrate on the skin surface for nanocrystals (e.g., 76-86%) compared to market products (e.g. 94%). Also, penetration was increased e.g. in skin depth of 5-10μm from <1.0/1.7% to e.g. 3.3-6.2% for nanocrystals. Copyright © 2017 Elsevier B.V. All rights reserved.

Thermodynamics of post-growth annealing of cadmium zinc telluride nuclear radiation detectors

NASA Astrophysics Data System (ADS)

Adams, Aaron Lee

Nuclear Radiation Detectors are used for detecting, tracking, and identifying radioactive materials which emit high-energy gamma and X-rays. The use of Cadmium Zinc Telluride (CdZnTe) detectors is particularly attractive because of the detector's ability to operate at room temperature and measure the energy spectra of gamma-ray sources with a high resolution, typically less than 1% at 662 keV. While CdZnTe detectors are acceptable imperfections in the crystals limit their full market potential. One of the major imperfections are Tellurium inclusions generated during the crystal growth process by the retrograde solubility of Tellurium and Tellurium-rich melt trapped at the growth interface. Tellurium inclusions trap charge carriers generated by gamma and X-ray photons and thus reduce the portion of generated charge carriers that reach the electrodes for collection and conversion into a readable signal which is representative of the ionizing radiation's energy and intensity. One approach in resolving this problem is post-growth annealing which has the potential of removing the Tellurium inclusions and associated impurities. The goal of this project is to use experimental techniques to study the thermodynamics of Tellurium inclusion migration in post-growth annealing of CdZnTe nuclear detectors with the temperature gradient zone migration (TGZM) technique. Systematic experiments will be carried out to provide adequate thermodynamic data that will inform the engineering community of the optimum annealing parameters. Additionally, multivariable correlations that involve the Tellurium diffusion coefficient, annealing parameters, and CdZnTe properties will be analyzed. The experimental approach will involve systematic annealing experiments (in Cd vapor overpressure) on different sizes of CdZnTe crystals at varying temperature gradients ranging from 0 to 60°C/mm (used to migrate the Tellurium inclusion to one side of the crystal), and at annealing temperatures ranging from 500 to 800°C. The characterization techniques that will be used to quantify the effects of the post-growth annealing experiments include: 1) 3D infrared transmission microscopy to measure the size, distribution, and concentration of Tellurium inclusions; 2) current-voltage measurements to determine the effect of post-growth annealing on the resistivity of CdZnTe crystals; and 3) X-ray diffraction topography, available at the National Synchrotron Light Source (NSLS) facilities at Brookhaven National Laboratory (BNL), to measure the correlation between device performance and annealing conditions

Crystal growth of ZnSe and related ternary compound semiconductors by physical vapor transport

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

1993-01-01

The materials to be investigated are ZnSe and related ternary semiconducting alloys (e.g., ZnS(x)Se(1-x), ZnTe(x)Se(1-x), and Zn(1-x)Cd(x)Se). These materials are useful for opto-electronic applications such as high efficient light emitting diodes and low power threshold and high temperature lasers in the blue-green region of the visible spectrum. The recent demonstration of its optical bistable properties also makes ZnSe a possible candidate material for digital optical computers. The investigation consists of an extensive ground-based study followed by flight experimentation, and involves both experimental and theoretical work. The objectives of the ground-based work are to establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low gravity environment and to obtain the experimental data and perform the analyses required to define the optimum parameters for the flight experiments. During the six months of the Preliminary Definition Phase, the research efforts were concentrated on the binary compound ZnSe - the purification of starting materials of Se by zone refining, the synthesis of ZnSe starting materials, the heat treatments of the starting materials, the vapor transport rate measurements, the vapor partial pressure measurements of ZnSe, the crystal growth of ZnSe by physical vapor transport, and various characterization on the grown ZnSe crystals.

The origin of plagioclase phenocrysts in basalts from continental monogenetic volcanoes of the Kaikohe-Bay of Islands field, New Zealand: implications for magmatic assembly and ascent

NASA Astrophysics Data System (ADS)

Coote, Alisha; Shane, Phil; Stirling, Claudine; Reid, Malcolm

2018-02-01

Late Quaternary, porphyritic basalts erupted in the Kaikohe-Bay of Islands area, New Zealand, provide an opportunity to explore the crystallization and ascent history of small volume magmas in an intra-continental monogenetic volcano field. The plagioclase phenocrysts represent a diverse crystal cargo. Most of the crystals have a rim growth that is compositionally similar to groundmass plagioclase ( An65) and is in equilibrium with the host basalt rock. The rims surround a resorbed core that is either less calcic ( An20-45) or more calcic (> An70), having crystallized in more differentiated or more primitive melts, respectively. The relic cores, particularly those that are less calcic (< An45), have 87Sr/86Sr ratios that are either mantle-like ( 0.7030) or crustal-like ( 0.7040 to 0.7060), indicating some are antecrysts formed in melts fractionated from plutonic basaltic forerunners, while others are true xenocrysts from greywacke basement and/or Miocene arc volcanics. It is envisaged that intrusive basaltic forerunners produced a zone where various degrees of crustal assimilation and fractional crystallization occurred. The erupted basalts represent mafic recharge of this system, as indicated by the final crystal rim growths around the entrained antecrystic and xenocrystic cargo. The recharge also entrained cognate gabbros that occur as inclusions, and produced mingled groundmasses. Multi-stage magmatic ascent and interaction is indicated, and is consistent with the presence of a partial melt body in the lower crust detected by geophysical methods. This crystallization history contrasts with traditional concepts of low-flux basaltic systems where rapid ascent from the mantle is inferred. From a hazards perspective, the magmatic system inferred here increases the likelihood of detecting eruption precursor phenomena such as seismicity, degassing and surface deformation.

Crystal growth formation in melt extrudates.

PubMed

Bruce, Caroline; Fegely, Kurt A; Rajabi-Siahboomi, Ali R; McGinity, James W

2007-08-16

The purpose of the study was to investigate the physical state of hot-melt extruded guaifenesin tablets containing either Acryl-EZE or Eudragit L100-55 and to study the physicochemical factors influencing crystal growth of guaifenesin on the surface of the extrudates. The powder mixtures containing Acryl-EZE were extruded on a single-screw Randcastle Microtruder at 20rpm and at temperatures of 90, 95, 110 degrees C (zones 1, 2, 3, respectively) and 115 degrees C (die), before being manually cut into tablets (250+/-5mg). Extrudates containing Eudragit L100-55, TEC and guaifenesin were extruded at temperatures ranging from 60 to 115 degrees C. Modulated differential calorimetry (DSC) was used to demonstrate the plasticizing effect of guaifenesin on Eudragit L100-55. Powder X-ray diffraction (PXRD) showed that while the drug powder is crystalline, extrudates containing up to 25% drug exhibited an amorphous diffraction profile. Extrudates containing higher drug concentrations showed an amorphous profile with some crystalline peaks corresponding to guaifenesin, indicating that the limit of solubility of drug in the matrix had been exceeded. Scanning electron microscopy was used to demonstrate that drug crystallization was a surface phenomenon and dependent on the drug concentration. In vitro dissolution testing showed no effect of surface crystallization of guaifenesin on drug release rates of extruded matrix tablets. The influence of hydrophilic polymeric additives including PVP K25, polycarbophil, PEG 3,350, poloxamer 188 or poly(ethylene oxide) as crystal growth inhibitors was investigated at a level of 10% based on the drug content. The extent of crystal growth was reduced for all additives. Complete drug release in pH 6.8 phosphate buffer was prolonged from 4h in extrudates containing Acryl-EZE and guaifenesin to 8h in extrudates containing Eudragit L100-55, TEC and guaifenesin. Drug release in extrudates containing Eudragit L100-55 and guaifenesin was not affected by the presence of hydrophilic additives present at 10% based on the drug content. In vitro drug release studies showed no significant change during storage for up to 6 months at 25 degrees C/60% relative humidity and 40 degrees C/75% relative humidity.

GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

DTIC Science & Technology

SINGLE CRYSTALS, CRYSTAL GROWTH), (*CRYSTAL GROWTH, SINGLE CRYSTALS), (*RARE EARTH COMPOUNDS, SINGLE CRYSTALS), EPITAXIAL GROWTH, SODIUM COMPOUNDS, CHLORIDES, VAPOR PLATING, ELECTROSTATIC FIELDS, ENERGY, ATOMIC PROPERTIES , BONDING

Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions

NASA Technical Reports Server (NTRS)

Gandin, Charles-Andre; Ratke, Lorenz

2008-01-01

The Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MSL-CETSOL and MICAST) are two investigations which supports research into metallurgical solidification, semiconductor crystal growth (Bridgman and zone melting), and measurement of thermo-physical properties of materials. This is a cooperative investigation with the European Space Agency (ESA) and National Aeronautics and Space Administration (NASA) for accommodation and operation aboard the International Space Station (ISS). Research Summary: Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing (CETSOL) and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST) are two complementary investigations which will examine different growth patterns and evolution of microstructures during crystallization of metallic alloys in microgravity. The aim of these experiments is to deepen the quantitative understanding of the physical principles that govern solidification processes in cast alloys by directional solidification.

Numerical simulation of CdTe vertical Bridgman growth

NASA Astrophysics Data System (ADS)

Ouyang, Hong; Shyy, Wei

1997-04-01

Numerical simulation has been conducted for steady-state Bridgman growth of the CdTe crystal with two ampoule configurations, namely, flat base and semi-spherical base. The present model accounts for conduction, convection and radiation, as well as phase change dynamics. The enthalpy formulation for phase change has been incorporated into a pressure-based algorithm with multi-zone curvilinear grid systems. The entire system which consists of the furnace enclosure wall, the encapsulated gas and the ampoule, contains irregularly configured domains. To meet the competing needs of producing accurate solutions with reasonable computing resources, a two-level approach is employed. The present study reveals that although the two ampoule configurations are quite different, their influence on the melt-solid interface shape is modest, and the undesirable concave interface appears in both cases. Since the interface shape strongly depends on thermal conductivities between the melt and the crystal, as well as ampoule wall temperature, accurate prescriptions of materials transport properties and operating environment are crucial for successful numerical predictions.

Methods for improved growth of group III nitride buffer layers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Melnik, Yurity; Chen, Lu; Kojiri, Hidehiro

Methods are disclosed for growing high crystal quality group III-nitride epitaxial layers with advanced multiple buffer layer techniques. In an embodiment, a method includes forming group III-nitride buffer layers that contain aluminum on suitable substrate in a processing chamber of a hydride vapor phase epitaxy processing system. A hydrogen halide or halogen gas is flowing into the growth zone during deposition of buffer layers to suppress homogeneous particle formation. Some combinations of low temperature buffers that contain aluminum (e.g., AlN, AlGaN) and high temperature buffers that contain aluminum (e.g., AlN, AlGaN) may be used to improve crystal quality and morphologymore » of subsequently grown group III-nitride epitaxial layers. The buffer may be deposited on the substrate, or on the surface of another buffer. The additional buffer layers may be added as interlayers in group III-nitride layers (e.g., GaN, AlGaN, AlN).« less

Oxide perovskite crystals for HTSC film substrates microwave applications

NASA Technical Reports Server (NTRS)

Bhalla, A. S.; Guo, Ruyan

1995-01-01

The research focused upon generating new substrate materials for the deposition of superconducting yttrium barium cuprate (YBCO) has yielded several new hosts in complex perovskites, modified perovskites, and other structure families. New substrate candidates such as Sr(Al(1/2)Ta(1/2))O3 and Sr(Al(1/2)Nb(1/2))O3, Ba(Mg(1/3)Ta(2/3))O3 in complex oxide perovskite structure family and their solid solutions with ternary perovskite LaAlO3 and NdGaO3 are reported. Conventional ceramic processing techniques were used to fabricate dense ceramic samples. A laser heated molten zone growth system was utilized for the test-growth of these candidate materials in single crystal fiber form to determine crystallographic structure, melting point, thermal, and dielectric properties as well as to make positive identification of twin free systems. Some of those candidate materials present an excellent combination of properties suitable for microwave HTSC substrate applications.

The structure of small, vapor-deposited particles. II - Experimental study of particles with hexagonal profile

NASA Technical Reports Server (NTRS)

Yacaman, M. J.; Heinemann, K.; Yang, C. Y.; Poppa, H.

1979-01-01

'Multiply-twinned' gold particles with hexagonal bright field TEM profile were determined to be icosahedra composed of 20 identical and twin-related tetrahedral building units that do not have an fcc structure. The crystal structure of these slightly deformed tetrahedra is rhombohedral. Experimental evidence supporting this particle model was obtained by selected-zone dark field and weak beam dark field electron microscopy. In conjunction with the results of part I, it has been concluded that multiply-twinned gold particles of pentagonal or hexagonal profile that are found during the early stages of the vapor deposition growth process on alkali halide surfaces do not have an fcc crystal structure, which is in obvious contrast to the structure of bulk gold.

Microstructural evidence for dissolution precipitation creep in high pressure metamorphic serpentinites from subduction zones

NASA Astrophysics Data System (ADS)

Wassmann, S.; Trepmann, C.; Krohe, A.; Stoeckhert, B.

2009-12-01

Serpentinite is generally believed to constitute weak material in subduction zones and to play an essential role for the development of a subduction channel. Information on deformation mechanisms and appropriate rheological models to describe these large scale flow processes is obtained from natural serpentinites exhumed from ancient subduction zones. In this study, we investigate the microstructural record of serpentinites exposed in the Zermatt-Saas-Zone, Western Alps. The metamorphic mineral assemblage comprises antigorite, forsterite, diopside, tremolite, chlorite, oxide phases, and in places titanclinohumite. Original mantle minerals are only locally preserved as relics. The conditions of Alpine metamorphism can be estimated from associated eclogites; the pressures are mostly between 1.5 and 2.5 GPa at temperatures of c. 500-600°C. The serpentinites show a complex structure with several generations of folds and foliations. An early foliation is defined by the combined shape and crystallographic preferred orientation (SPO and CPO) of antigorite and metamorphic diopside. These patterns are undistinguishable from the SPO and CPO of the same minerals in strain shadows, where the CPO must be developed by oriented growth from an aqueous solution. Therefore we suspect that the SPO and CPO in the polyphase matrix layers also result from oriented growth. Also, there is no microstructural evidence for any crystal plastic deformation of diopside. In places, antigorite flakes with SPO and CPO are overgrown by single crystals or aggregates of metamorphic forsterite, locally titanoclinohumite, and tremolite. The aggregates of forsterite exhibit a foam structure without CPO. All microfabrics indicate that dissolution precipitation creep was predominant in the investigated serpentinites, and most finite strain was accumulated by this mechanism. We see no evidence for a significant contribution of dislocation creep, both based on microstructure and on the CPO patterns. This does not preclude dislocation creep and a power law rheology to hold for higher stress levels, as expected for short episodes of postseismic creep. For the long term flow of serpentinites in subduction zones, however, Newtonian behaviour and a low viscosity are indicated.

Direct Visualization of an Impurity Depletion Zone

NASA Technical Reports Server (NTRS)

Chernov, Alex A.; Garcia-Ruiz, Juan Ma; Thomas, Bill R.

2000-01-01

When a crystal incorporates more impurity per unit of its volume than the impurity concentration in solution, the solution in vicinity of the growing crystal is depleted with respect to the impurity I,2. With a stagnant solution, e. g. in microgravity or gels, an impurity depletion zone expands as the crystal grows and results in greater purity in most of the outer portion of the crystal than in the core. Crystallization in gel provides an opportunity to mimic microgravity conditions and visualize the impurity depletion zone. Colorless, transparent apoferritin (M congruent to 450 KDa) crystals were grown in the presence of red holoferritin dimer as a microheterogeneous impurity (M congruent to 900 KDa) within agarose gel by counterdiffusion with Cd(2+) precipitant. Preferential trapping of dimers, (distribution coefficient K = 4 (exp 1,2)) results in weaker red color around the crystals grown in the left tube in the figure as compared to the control middle tube without crystals. The left and the middle tubes contain colored ferritin dimers, the right tube contains colored trimers. The meniscus in the left tube separate gel (below) and liquid solution containing Cd(2+) (above). Similar solutions, though without precipitants, were present on top of the middle and right tube allowing diffusion of dimers and trimers. The area of weaker color intensity around crystals directly demonstrates overlapped impurity depletion zones.

On the origin of size-dependent and size-independent crystal growth: Influence of advection and diffusion

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

2003-01-01

Crystal growth experiments were conducted using potassium alum and calcite crystals in aqueous solution under both non-stirred and stirred conditions to elucidate the mechanism for size-dependent (proportionate) and size-independent (constant) crystal growth. Growth by these two laws can be distinguished from each other because the relative size difference among crystals is maintained during proportionate growth, leading to a constant crystal size variance (??2) for a crystal size distribution (CSD) as the mean size increases. The absolute size difference among crystals is maintained during constant growth, resulting in a decrease in size variance. Results of these experiments show that for centimeter-sized alum crystals, proportionate growth occurs in stirred systems, whereas constant growth occurs in non-stirred systems. Accordingly, the mechanism for proportionate growth is hypothesized to be related to the supply of reactants to the crystal surface by advection, whereas constant growth is related to supply by diffusion. Paradoxically, micrometer-sized calcite crystals showed proportionate growth both in stirred and in non-stirred systems. Such growth presumably results from the effects of convection and Brownian motion, which promote an advective environment and hence proportionate growth for minute crystals in non-stirred systems, thereby indicating the importance of solution velocity relative to crystal size. Calcite crystals grown in gels, where fluid motion was minimized, showed evidence for constant, diffusion-controlled growth. Additional investigations of CSDs of naturally occurring crystals indicate that proportionate growth is by far the most common growth law, thereby suggesting that advection, rather than diffusion, is the dominant process for supplying reactants to crystal surfaces.

Solutions multiples thermocapillaires en zone flottante à gravité nulle

NASA Astrophysics Data System (ADS)

Chénier, E.; Delcarte, C.; Labrosse, G.

1998-04-01

An original model is adopted to analyse the melted phase hydrodynamics, in the floating zone technique configuration for crystal growth. In particular, a small capillary scale located near the fusion fronts is taken into account. Its size turns out to influence significantly the flow structure. For the first time, multiple solutions are exhibited in zero gravity. Un modèle original a été adopté pour analyser l'hydrodynamique de la phase fondue pour la technique de la zone flottante, en croissance cristalline. En particulier, une petite échelle capillaire, située près des fronts de fusion, est prise en considération. Son extension se révèle influencer significativement la structure des écoulements. L'existence de solutions multiples est, pour la première fois, mise en évidence en gravité zéro.

MgAl2O4 spinel refractory as containment liner for high-temperature alkali salt containing environments

DOEpatents

Peascoe-Meisner, Roberta A [Knoxville, TN; Keiser, James R [Oak Ridge, TN; Hemric, James G [Knoxville, TN; Hubbard, Camden R [Oak Ridge, TN; Gorog, J Peter [Kent, WA; Gupta, Amul [Jamestown, NY

2008-10-21

A method includes containing a high-temperature alkali salt containing environment using a refractory containment liner containing MgAl.sub.2O.sub.4 spinel. A method, includes forming a refractory brick containing MgAl.sub.2O.sub.4 spinel having an exterior chill zone defined by substantially columnar crystallization and an interior zone defined by substantially equiaxed crystallization; and removing at least a portion of the exterior chill zone from the refractory brick containing MgAl.sub.2O.sub.4 spinel by scalping the refractory brick containing MgAl.sub.2O.sub.4 spinel to define at least one outer surface having an area of substantially equiaxed crystallization. A product of manufacture includes a refractory brick containing MgAl.sub.2O.sub.4 spinel including an interior zone defined by substantially equiaxed crystallization; and at least one outer surface having an area of substantially equiaxed crystallization.

Integrative interactive visualization of crystal structure, band structure, and Brillouin zone

NASA Astrophysics Data System (ADS)

Hanson, Robert; Hinke, Ben; van Koevering, Matthew; Oses, Corey; Toher, Cormac; Hicks, David; Gossett, Eric; Plata Ramos, Jose; Curtarolo, Stefano; Aflow Collaboration

The AFLOW library is an open-access database for high throughput ab-initio calculations that serves as a resource for the dissemination of computational results in the area of materials science. Our project aims to create an interactive web-based visualization of any structure in the AFLOW database that has associate band structure data in a way that allows novel simultaneous exploration of the crystal structure, band structure, and Brillouin zone. Interactivity is obtained using two synchronized JSmol implementations, one for the crystal structure and one for the Brillouin zone, along with a D3-based band-structure diagram produced on the fly from data obtained from the AFLOW database. The current website portal (http://aflowlib.mems.duke.edu/users/jmolers/matt/website) allows interactive access and visualization of crystal structure, Brillouin zone and band structure for more than 55,000 inorganic crystal structures. This work was supported by the US Navy Office of Naval Research through a Broad Area Announcement administered by Duke University.

Photoconductivity in the chalcohalide semiconductor, SbSeI: a new candidate for hard radiation detection.

PubMed

Wibowo, Arief C; Malliakas, Christos D; Liu, Zhifu; Peters, John A; Sebastian, Maria; Chung, Duck Young; Wessels, Bruce W; Kanatzidis, Mercouri G

2013-06-17

We investigated an antimony chalcohalide compound, SbSeI, as a potential semiconductor material for X-ray and γ-ray detection. SbSeI has a wide band gap of 1.70 eV with a density of 5.80 g/cm(3), and it crystallizes in the orthorhombic Pnma space group with a one-dimensional chain structure comprised of infinite zigzag chains of dimers [Sb2Se4I8]n running along the crystallographic b axis. In this study, we investigate conditions for vertical Bridgman crystal growth using combinations of the peak temperature and temperature gradients as well as translation rate set in a three-zone furnace. SbSeI samples grown at 495 °C peak temperature and 19 °C/cm temperature gradient with 2.5 mm/h translation rate produced a single phase of columnar needlelike crystals aligned along the translational direction of the growth. The ingot sample exhibited an n-type semiconductor with resistivity of ∼10(8) Ω·cm. Photoconductivity measurements on these specimens allowed us to determine mobility-lifetime (μτ) products for electron and hole carriers that were found to be of similar order of magnitude (∼10(-4) cm(2)/V). Further, the SbSeI ingot with well-aligned, one-dimensional columnar needlelike crystals shows an appreciable response of Ag Kα X-ray.

Low-temperature growth and photoluminescence property of ZnS nanoribbons.

PubMed

Zhang, Zengxing; Wang, Jianxiong; Yuan, Huajun; Gao, Yan; Liu, Dongfang; Song, Li; Xiang, Yanjuan; Zhao, Xiaowei; Liu, Lifeng; Luo, Shudong; Dou, Xinyuan; Mou, Shicheng; Zhou, Weiya; Xie, Sishen

2005-10-06

At a low temperature of 450 degrees C, ZnS nanoribbons have been synthesized on Si and KCl substrates by a simple chemical vapor deposition (CVD) method with a two-temperature-zone furnace. Zinc and sulfur powders are used as sources in the different temperature zones. X-ray diffraction (XRD), selected area electron diffraction (SEAD), and transmission electron microscopy (TEM) analysis show that the ZnS nanoribbons are the wurtzite structure, and there are two types-single-crystal and bicrystal nanoribbons. Photoluminescence (PL) spectrum shows that the spectrum mainly includes two parts: a purple emission band centering at about 390 nm and a blue emission band centering at about 445 nm with a weak green shoulder around 510 nm.

The Faceted Discrete Growth and Phase Differentiation During the Directional Solidification of 20SiMnMo5 Steel

NASA Astrophysics Data System (ADS)

Ma, Xiaoping; Li, Dianzhong

2018-07-01

The microstructures, segregation and cooling curve were investigated in the directional solidification of 20SiMnMo5 steel. The typical characteristic of faceted growth is identified. The microstructures within the single cellular and within the single dendritic arm, together with the contradictive segregation distribution against the cooling curve, verify the discrete crystal growth in multi-scales. Not only the single cellular/dendritic arm but also the single martensite zone within the single cellular/dendritic arm is produced by the discrete growth. In the viewpoint of segregation, the basic domain following continuous growth has not been revealed. Along with the multi-scale faceted discrete growth, the phase differentiation happens for both the solid and liquid. The differentiated liquid phases appear and evolve with different sizes, positions, compositions and durations. The physical mechanism for the faceted discrete growth is qualitatively established based on the nucleation of new faceted steps induced by the composition gradient and temperature gradient.

The Faceted Discrete Growth and Phase Differentiation During the Directional Solidification of 20SiMnMo5 Steel

NASA Astrophysics Data System (ADS)

Ma, Xiaoping; Li, Dianzhong

2018-03-01

The microstructures, segregation and cooling curve were investigated in the directional solidification of 20SiMnMo5 steel. The typical characteristic of faceted growth is identified. The microstructures within the single cellular and within the single dendritic arm, together with the contradictive segregation distribution against the cooling curve, verify the discrete crystal growth in multi-scales. Not only the single cellular/dendritic arm but also the single martensite zone within the single cellular/dendritic arm is produced by the discrete growth. In the viewpoint of segregation, the basic domain following continuous growth has not been revealed. Along with the multi-scale faceted discrete growth, the phase differentiation happens for both the solid and liquid. The differentiated liquid phases appear and evolve with different sizes, positions, compositions and durations. The physical mechanism for the faceted discrete growth is qualitatively established based on the nucleation of new faceted steps induced by the composition gradient and temperature gradient.

Melt infiltration of silicon carbide compacts. II - Evaluation of solidification microstructures

NASA Technical Reports Server (NTRS)

Asthana, Rajiv; Rohatgi, Pradeep K.

1993-01-01

Microstructural aspects of alloy solidification within the interstices of porous compacts of platelet-shaped single crystals of alpha-SiC, when the latter are infiltrated with a hot metal under pressure, have been described. Microstructural evidence is presented of selective reorientation of platelets and nonhomogeneous solute distribution under shear of pressurized melt, of constrained growth of primary solid within finite width zones, and of the modulation of coring due to microsegregation as a result of variations in the pore size of compacts.

Paramagnetic resonance of LaGaO3: Mn single crystals grown by floating zone melting

NASA Astrophysics Data System (ADS)

Vazhenin, V. A.; Potapov, A. P.; Artyomov, M. Yu.; Salosin, M. A.; Fokin, A. V.; Gil'mutdinov, I. F.; Mukhamedshin, I. R.

2016-02-01

The EPR spectrum of Mn-doped lanthanum gallate single crystals grown by floating zone melting with optical heating has been studied. In contrast to the crystals grown according to the Czochralski method, no manganese is found in these crystals even after high-temperature annealing in air. The spectral characteristics of Fe3+ and Gd3+ centers in crystals prepared by various methods have been compared in the rhombohedral phase, and the fourth-rank nondiagonal parameters of the Fe3+ trigonal centers have been determined, as well.

A cathodoluminescence study on zircons with a complex thermal history traces back Permian crustal events in the Ivrea Zone (South Alpine, Northern Italy)

NASA Astrophysics Data System (ADS)

Peressini, G.; Poller, U.

2003-04-01

In the context of a U-Pb SHRIMP data-set, a cathodoluminescence (CL) study has been performed on zircons from the Ivrea-Verbano Zone; this is a tectonically bounded section of intermediate to deep crust, tilted and obducted in Alpine time, in which a large deep-crustal intrusion of mantle origin, the Mafic Complex (MC), was emplaced in the Early Permian. Zircons from 16 samples from the different units of the MC have been studied using CL. Three samples collected from the Paragneiss Bearing Belt (PBB) yield some partially reset spot-ages, reflecting the field observation that country rock slabs are frequent in that area. On the other side, unlike in zircons from granites, the cores are invisible under CL-imaging, and this makes the U-Pb spot-age results unpredictable, with a continuous range of ages in the same sample, spanning for an interval of over 35 Ma, followed by some much older peaks, up to 600 Ma. A fourth sample, collected 2 km far, but still within the PBB, defines instead a unique, well-defined age at 287±3 Ma, with no older peaks, its zircons showing a CL pattern typical for metamorphic grains. A different case is displayed by a sample collected from the deeper Amphibole Gabbro unit: each single grain records a complex story of magmatic growth with variable diffusivity conditions. All of them show a second major overprint, that lead to both (re)crystallization and resorption, always corresponding to much lower U and Th contents, with no sensible modification of the Th-U ratio. The age of the second event, though, is not distinguishable from that of first crystallization of the grains, and has not been at such a temperature as to obliterate the fine zoning pattern of the primary grain. The CL patterns of each single grain, composed of different domains, allow considerations on the environmental conditions of growth and (re)crystallization. CL is a very powerful tool itself, revealing crystal-chemical processes. The integration of the CL-study with the SHRIMP spot-age determination relates them to the sequence of geologic events. The study, performed on samples coming from all over the Complex, has allowed a better understanding of processes in the Carboniferous-Permian lower crust of the Ivrea Zone: the knowledge of the Complex, its structure and the field relationships has become a key for interpreting the results. Where the CL displays a composite pattern, mechanisms are needed to explain geochemical fingerprints: therefore, trace and REE analyses by ion probe are in progress to integrate the SHRIMP data.

Nucleation and growth constraints and outcome in the natural gas hydrate system

NASA Astrophysics Data System (ADS)

Osegovic, J. P.; Max, M. D.

2016-12-01

Hydrate formation processes are functions of energy distribution constrained by physical and kinetic parameters. The generation of energy and energy derivative plots of a constrained growth crucible are used to demonstrate nucleation probability zones (phase origin(s)). Nucleation sets the stage for growth by further constraining the pathways through changes in heat capacity, heat flow coefficient, and enthalpy which in turn modify the mass and energy flow into the hydrate formation region. Nucleation events result from the accumulation of materials and energy relative to pressure, temperature, and composition. Nucleation induction is predictive (a frequency parameter) rather than directly dependent on time. Growth, as mass tranfer into a new phase, adds time as a direct parameter. Growth has direct feedback on phase transfer, energy dynamics, and mass export/import rates. Many studies have shown that hydrate growth is largely an equilibrium process controlled by either mass or energy flows. Subtle changes in the overall energy distribution shift the equilibrium in a predictable fashion. We will demonstrate the localization of hydrate nucleation in a reservoir followed by likely evolution of growth in a capped, sand filled environment. The gas hydrate stability zone (GHSZ) can be characterized as a semi-batch crystallizer in which nucleation and growth of natural gas hydrate (NGH) is a continuous process that may result in very large concentrations of NGH. Gas flux, or the relative concentration of hydrate-forming gas is the critical factor in a GHSZ. In an open groundwater system in which flow rate exceeds diffusion transport rate, dissolved natural gas is transported into and through the GHSZ. In a closed system, such as a geological trap, diffusion of hydrate-forming gas from a free gas zone below the GHSZ is the primary mechanism for movement of gas reactants. Because of the lower molecular weight of methane, where diffusion is the principal transport mechanism, the natural system can be a purification process for formation of increasingly pure NGH from a mixed gas solution over time.

Petrology of gabbroic xenoliths in 1960 Kilauea basalt: crystalline remnants of prior (1955) magmatism

USGS Publications Warehouse

Fodor, R.V.; Moore, R.B.

1994-01-01

The 1960 Kapoho lavas of Kilauea's east rift zone contain 1-10 cm xenoliths of olivine gabbro, olivine gabbro-norite, and gabbro norite. Textures are poikilitic (ol+sp+cpx in pl) and intergranular (cpx+pl??ol??opx). Poikilitic xenoliths, which we interpret as cumulates, have the most primitive mineral compositions, Fo82.5, cpx Mg# 86.5, and An80.5. Many granular xenoliths (ol and noritic gabbro) contain abundant vesicular glass that gives them intersertal, hyaloophitic, and overall 'open' textures to suggest that they represent 'mush' and 'crust' of a magma crystallization environment. Their phase compositions are more evolved (Fo80-70, cpx Mg# 82-75, and An73-63) than those of the poikilitic xenoliths. Associated glass is basaltic, but evolved (MgO 5 wt%; TiO2 3.7-5.8 wt%). The gabbroic xenolith mineral compositions fit existing fractional crystallization models that relate the origins of various Kilauea lavas to one another. FeO/MgO crystal-liquid partitioning is consistent with the poikilitic ol-gabbro assemblage forming as a crystallization product from Kilauea summit magma with ???8 wt% MgO that was parental to evolved lavas on the east rift zone. For example, least squares calculations link summit magmas to early 1955 rift-zone lavas (???5 wt% MgO) through ???28-34% crystallization of the ol+sp+cpx+pl that comprise the poikilitic ol-gabbros. The other ol-gabbro assemblages and the olivine gabbro-norite assemblages crystallized from evolved liquids, such as represented by the early 1955 and late 1955 lavas (???6.5 wt% MgO) of the east rift zone. The eruption of 1960 Kapoho magmas, then, scoured the rift-zone reservoir system to entrain portions of cumulate and solidification zones that had coated reservoir margins during crystallization of prior east rift-zone magmas. ?? 1994 Springer-Verlag.

Control of interface shape during high melting sesquioxide crystal growth by HEM technique

NASA Astrophysics Data System (ADS)

Hu, Kaiwei; Zheng, Lili; Zhang, Hui

2018-02-01

During crystal growth in heat exchanger method (HEM) system, the shape of the growth interface changes with the proceeding of the growth process, which limits the crystal size and reduces the quality of the crystal. In this paper, a modified HEM system is proposed to control the interface shape for growth of sesquioxide crystals. Numerical simulation is performed to predict heat transfer, melt flow and interface shape during growth of high melting sesquioxide crystals by the heat exchanger method. The results show that a flat or slightly convex interface shape is beneficial to reduce the solute pileup in front of the melt/crystal interface and decrease the radial temperature gradient inside the crystal during growth of sesquioxide crystals. The interface shape can be controlled by adjusting the gap size d and lower resistance heater power during growth. The growth rate and the melt/crystal interface position can be obtained by two measured temperatures.

Near-surface clay authigenesis in exhumed fault rock of the Alpine Fault Zone (New Zealand); O-H-Ar isotopic, XRD and chemical analysis of illite and chlorite

NASA Astrophysics Data System (ADS)

Boles, Austin; Mulch, Andreas; van der Pluijm, Ben

2018-06-01

Exhumed fault rock of the central Alpine Fault Zone (South Island, New Zealand) shows extensive clay mineralization, and it has been the focus of recent research that aims to describe the evolution and frictional behavior of the fault. Using Quantitative X-ray powder diffraction, 40Ar/39Ar geochronology, hydrogen isotope (δD) geochemistry, and electron microbeam analysis, we constrain the thermal and fluid conditions of deformation that produced two predominant clay phases ubiquitous to the exposed fault damage zone, illite and chlorite. Illite polytype analysis indicates that most end-member illite and chlorite material formed in equilibrium with meteoric fluid (δD = -55 to -75‰), but two locations preserve a metamorphic origin of chlorite (δD = -36 to -45‰). Chlorite chemical geothermometry constrains crystal growth to T = 210-296 °C. Isotopic analysis also constrains illite growth to T < 100 °C, consistent with the mineralogy, with Ar ages <0.5 Ma. High geothermal gradients in the study area promoted widespread, near-surface mineralization, and limited the window of clay authigenesis in the Alpine Fault Zone to <5 km for chlorite and <2 km for illite. This implies a significant contrast between fault rock exposed at the surface and that at depth, and informs discussions about fault strength, clays and frictional behavior.

The timing of compositionally-zoned magma reservoirs and mafic 'priming' weeks before the 1912 Novarupta-Katmai rhyolite eruption

USGS Publications Warehouse

Singer, Brad S.; Costa, Fidel; Herrin, Jason S.; Hildreth, Wes; Fierstein, Judith

2016-01-01

The June 6, 1912 eruption of more than 13 km3 of dense rock equivalent (DRE) magma at Novarupta vent, Alaska was the largest of the 20th century. It ejected >7 km3 of rhyolite, ~1.3 km3 of andesite and ~4.6 km3 of dacite. Early ideas about the origin of pyroclastic flows and magmatic differentiation (e.g., compositional zonation of reservoirs) were shaped by this eruption. Despite being well studied, the timing of events that led to the chemically and mineralogically zoned magma reservoir remain poorly known. Here we provide new insights using the textures and chemical compositions of plagioclase and orthopyroxene crystals and by reevaluating previous U-Th isotope data. Compositional zoning of the magma reservoir likely developed a few thousand years before the eruption by several additions of mafic magma below an extant silicic reservoir. Melt compositions calculated from Sr contents in plagioclase fill the compositional gap between 68 and 76% SiO2 in whole pumice clasts, consistent with uninterrupted crystal growth from a continuum of liquids. Thus, our findings support a general model in which large volumes of crystal-poor rhyolite are related to intermediate magmas through gradual separation of melt from crystal-rich mush. The rhyolite is incubated by, but not mixed with, episodic recharge pulses of mafic magma that interact thermochemically with the mush and intermediate magmas. Hot, Mg-, Ca-, and Al-rich mafic magma intruded into, and mixed with, deeper parts of the reservoir (andesite and dacite) multiple times. Modeling the relaxation of the Fe-Mg concentrations in orthopyroxene and Mg in plagioclase rims indicates that the final recharge event occurred just weeks prior to the eruption. Rapid addition of mass, volatiles, and heat from the recharge magma, perhaps aided by partial melting of cumulate mush below the andesite and dacite, pressurized the reservoir and likely propelled a ~10 km lateral dike that allowed the overlying rhyolite to reach the surface.

The magma plumbing system in the Mariana Trough back-arc basin at 18° N

NASA Astrophysics Data System (ADS)

Lai, Zhiqing; Zhao, Guangtao; Han, Zongzhu; Huang, Bo; Li, Min; Tian, Liyan; Liu, Bo; Bu, Xuejiao

2018-04-01

Mafic magmas are common in back-arc basin, once stalled in the crust, these magmas may undergo different evolution. In this paper, compositional and textural variations of plagioclase as well as mineral-melt geothermobarometry are presented for basalts erupted from the central Mariana Trough (CMT). These data reveal crystallization conditions and we attempt a reconstruction of the magma plumbing system of the CMT. Plagioclase megacrysts, phenocrysts, microphenocrysts, microlites, olivine, spinel, and clinopyroxene have been recognized in basalt samples, using BSE images and compositional features. The last three minerals are homogeneous as microphenocrysts. Mineral-melt barometry indicates that plagioclase crystals crystallized and eventually grew into phenocrysts and megacrysts in mush zone with depth of 5-9 km, in which the normal zoning plagioclases crystallized in the interval of various batches of basic magma recharging. Plagioclase megacrysts and phenocrysts were dissolved and/or resorbed, when new basic magmas injected into the mush zone near Moho depth. It is inferred that magma extracted from the mush zone, and adiabatically ascended via different pathways. Some basaltic magmas underwent plagioclase and clinopyroxene microphenocrysts crystallization in low-pressure before eruption. Plagioclase microlites and outermost rims probably crystallized after eruption.

Solidification of II-VI Compounds in a Rotating Magnetic Field

NASA Technical Reports Server (NTRS)

Gillies, D. C.; Volz, M. P.; Mazuruk, K.; Motakef, S.; Dudley, M.; Matyi, R.

1999-01-01

This project is aimed at using a rotating magnetic field (RMF) to control fluid flow and transport during directional solidification of elemental and compound melts. Microgravity experiments have demonstrated that small amounts of residual acceleration of less than a micro-g can initiate and prolong fluid flow, particularly when there is a static component of the field perpendicular to the liquid solid interface. Thus a true diffusion boundary layer is not formed, and it becomes difficult to verify theories of solidification or to achieve diffusion controlled solidification. The RMF superimposes a stirring effect on an electrically conducting liquid, and with appropriate field strengths and frequencies, controlled transport of material through a liquid column can be obtained. As diffusion conditions are precluded and complete mixing conditions prevail, the technique is appropriate for traveling solvent zone or float zone growth methods in which the overall composition of the liquid can be maintained throughout the growth experiment. Crystals grown by RMF techniques in microgravity in previous, unrelated missions have shown exceptional properties. The objective of the project is two-fold, namely (1) using numerical modeling to simulate the behavior of a solvent zone with applied thermal boundary conditions and demonstrate the effects of decreasing gravity levels, or an increasing applied RMF, or both, and (2) to grow elements and II-VI compounds from traveling solvent zones both with and without applied RMFs, and to determine objectively how well the modeling predicts solidification parameters. Numerical modeling has demonstrated that, in the growth of CdTe from a tellurium solution, a rotating magnetic field can advantageously modify the shape of the liquid solid interface such that the interface is convex as seen from the liquid. Under such circumstances, the defect structure is reduced as any defects which are formed tend to grow out and not propagate. The flow of liquid, however, is complex due to the competing flow induced by the rotating magnetic field and the buoyancy driven convection. When the acceleration forces are reduced to one thousandth of gravity, the flow pattern is much simplified and well controlled material transport through the solvent zone can be readily achieved. Triple axis diffractometry and x-ray synchrotron topography have demonstrated that there is no significant improvement in crystal quality for HgCdTe grown on earth from a tellurium solution when a rotating magnetic field is applied. However, modeling shows that the flow in microgravity with a rotating magnetic field would produce a superior product.

Thermochronological evolution of an intra-plate magmatic event inferred from an integrated modeling approach: A case study in the Westerwald, Germany

NASA Astrophysics Data System (ADS)

Tirone, M.; Rokitta, K.; Schreiber, U.

2016-09-01

A lava sample from the Tertiary Westerwald volcanic field was selected for a detailed study using various analytical techniques in combination with petrological, thermodynamic and diffusion modeling to extract information related to the thermochronological evolution of a magmatic event before eruption. The lava sample contains large olivine phenocrysts which are compositionally zoned and two coexisting but chemically distinct melts, a host melt with basaltic composition and small spherical pockets of a less abundant trachytic melt (globules). The sample was analyzed by electron microprobe, x-ray fluorescence (XRF) X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). The primary melt of the host lava was determined using the program PRIMELT2.XLS. Partial fractional crystallization of olivine was modeled using the program alphaMELTS. Timescale and cooling rate were retrieved by fitting the measured Fe-Mg zoning along two directions in four olivine grains from the host lava using a 3-D numerical diffusion model. The measured variation of Ca is also consistent with a chemical diffusion process, while a numerical growth model applied to the same olivines does not appear to explain the Fe-Mg zoning. Chemical zoning of major elements in the melt globules were reproduced with a multicomponent diffusion model. The results of this study show that the host magma fractionated about 9% of olivine in a first stage, then the crystallization proceeded without further separation of mineral phases. Modeling of diffusion in the olivine crystals suggests that this second stage lasted at least 5 yrs and the temperature of the melt decreased from 1120-1150 °C to 1090 °C during this time. According to the results of the multicomponent diffusion model applied to the melt globules, the coexistence of the two melts was extremely short (less than few hours), possibly recording the assimilation of the globules during eruption or cooling of the whole system on the surface.

Surrogate Seeds For Growth Of Crystals

NASA Technical Reports Server (NTRS)

Shlichta, Paul J.

1989-01-01

Larger crystals of higher quality grown. Alternative method for starting growth of crystal involves use of seed crystal of different material instead of same material as solution. Intended for growing single-crystal proteins for experiments but applicable in general to growth of crystals from solutions and to growth of semiconductor or other crystals from melts.

Timescales and conditions of crystallization in the Pokai and Chimpanzee Ignimbrites, Taupo Volcanic Zone, New Zealand

NASA Astrophysics Data System (ADS)

Connor, M.; Gualda, G. A.; Gravley, D. M.

2013-12-01

Silicic magmas give rise to explosive eruptions that are both of scientific and societal interest. The central Taupo Volcanic Zone in New Zealand has been volcanically active for 2 Ma and represents the most active volcanic area in the world today. Particularly intense volcanic activity took place as part of a flare-up event that occurred from ~340 to ~240 ka, when 7 large ignimbrite eruptions took place, as well as many smaller eruptions, which erupted a total of at least 3000 km3 of magma. This project seeks to identify the conditions and timescales over which magma bodies that gave rise to these ignimbrite eruptions evolved. We aim to understand how much of the tens of thousands of years between successive eruptions were characterized by the presence of large bodies of silicic magma within the crust, as well the magma distribution within the crust during those times. We focus on the Chimpanzee and Pokai ignimbrites, which together erupted ~150 km3 of magma. The Pokai ignimbrite erupted at ~275 ka, while the Chimpanzee ignimbrite (undated) erupted between ~320 and 275 ka. Pumice clasts from the Chimpanzee and Pokai ignimbrite were collected in the field. Pumice bulk densities were measured using a submersion technique. Quartz and plagioclase crystals were extracted through a crushing, sieving, and winnowing procedure. Whole crystals were hand-picked under a conventional microscope, mounted on epoxy, and polished to expose grain interiors. Grain mounts were analyzed under an SEM using back-scattered electron, cathodoluminescence (CL), and energy-dispersive x-ray (EDX) imaging. Bulk-densities vary from 0.42 to 0.81 g/cm3 for Pokai and between 0.52 and 0.64 g/cm3 for Chimpanzee pumice clasts. Plagioclase is the dominant crystal phase in both units. Several plagioclase crystals have inclusions of orthopyroxene, ilmenite, magnetite, and zircon, which in some cases form clusters. Quartz is rare but is present in pumice from both deposits. Both plagioclase and quartz have glass inclusions. Quantitative EDX analyses under the SEM reveal high-silica rhyolite compositions (~78 wt. % SiO2), consistent with crystallization at shallow crustal levels (~100 MPa). Rhyolite-MELTS barometry confirms this suggestion, with estimated crystallization pressures of 70-110 MPa. Such crystallization depths are characteristic of magma bodies that give rise to ignimbrites in the Taupo Volcanic Zone. CL images of a small number of quartz crystals reveal zoning that is variable in character, from unzoned to distinctly zoned. Zoned crystals have several discrete zones, each one with its own characteristic homogeneous brightness; bright CL rims are observed in these crystals. Contacts between zones can be used to calculate crystallization times using diffusional relaxation assuming that CL intensity variations are due to Ti zonation. We estimate that quartz crystallization took place over decades to a few centuries, with rims crystallizing over months to years at most. These short timescales suggest that magma bodies with eruptible magma are very short-lived, much shorter-lived than the 10s of ka repose periods between eruptions that make up the flare-up event.

Mt. Etna plumbing system revealed by combined textural, compositional, and thermobarometric studies in clinopyroxenes

NASA Astrophysics Data System (ADS)

Giacomoni, P. P.; Coltorti, M.; Bryce, J. G.; Fahnestock, M. F.; Guitreau, M.

2016-04-01

Coupled textural and in situ geochemical studies of clinopyroxene (cpx) phenocrysts, from both historical and recent eruptions of Mt. Etna volcano, provide a means to investigate the processes occurring in the deepest portion of the feeding system (>10 km depth). Five distinct textures were recognized: (1) normal oscillatory zoning, (2) normal zoning with Fe-rich rim, (3) sieve-textured core, (4) reverse oscillatory zoning, and (5) dusty rim. Electron microprobe analyses indicate an almost constant diopside-augite composition, with a slight enrichment in the enstatite for more recent erupted cpx. Core-to-rim compositional profiles, performed along the cpx, reveal distinct compositional characteristics. Normal oscillatory zoning is often characterized by a sharp increase in FeO (Δ ~ 2 wt%) accompanied by a drop in Al2O3 on the outermost 30 μm. Reverse oscillatory zoning, by contrast, exhibits a drop in FeO, Al2O3 (Δ ~ 2 wt%), and a remarkable crystal rim increase in MgO (up to 5 wt%). Similar compositional changes are evident in dusty-textured rims, which are characterized by dissolution edges and overgrowth containing glass pockets and channels. No significant compositional variations have been observed across crystals with sieve-textured cores. Trace element concentrations show enrichments in Sr, La, Zr, and REE, together with a decreasing La/Yb ratio (from ~7 to ~4) in rims of normally zoned crystals. Cpx with reverse zoning and dusty rims has low Sr, La, Zr, and REE contents toward crystal rims. Thermometers and barometers, based on equilibrium cpx-melt pairs, suggest that cpx cores start nucleating at 720 MPa, with the majority of them forming between 600 and 400 MPa but continuing to crystallize until very shallow depths (<100 MPa). Normal oscillatory-zoned phenocrysts surrounded by rims form at pressures shallower than 400 MPa, while reverse zoning and dusty rims occur between 400 and 500 MPa. Coupled petrologic and thermobarometric studies on both clinopyroxenes and plagioclases, associated with detailed textural and in situ geochemical analyses, are promising tools to reconstruct the entire magma ascent path beneath open-system volcanoes. At Mt. Etna, two distinct processes could account for the observed textures: Fe-rich rims in normal oscillatory-zoned crystals can be related to decompression-induced crystallization, while reverse zoning and dusty rims can be produced by mixing with a more basic magma at 400-500 MPa (i.e., ~10 km). Textural features are not restricted to a particular evolutionary phase of the volcano, which suggest that the deep feeding system has not changed significantly since the first alkaline volcanic phase.

Reflection spectra and their angular dependences of one-dimensional photonic crystals based on aluminium oxide

NASA Astrophysics Data System (ADS)

Gorelik, V. S.; Yashin, M. M.; Pudovkin, A. V.; Vodchits, A. I.

2017-11-01

The article considers optical properties (transmission and reflection) of one-dimensional photonic crystals based on mesoporous anodic aluminum oxide, with periods of crystal lattices 188 and 194 nm. A comparison of the experimentally measured reflection spectrum in the spectral region of the first stop-zone with the theoretical dependence obtained from the dispersion relation for one-dimensional photonic crystal is carried out. The angular dependence of the first stop-zone spectral positions of one-dimensional photonic crystal is established. The authors analyze the possibility of applications of mesoporous one-dimensional photonic crystals based on aluminum oxide as the selective narrowband filters and mirrors.

Direct measurement of asperity contact growth in quartz at hydrothermal conditions

NASA Astrophysics Data System (ADS)

Beeler, N. M.; Hickman, S. H.

2008-12-01

Room-temperature friction and indentation experiments suggest fault strengthening during the interseismic period results from increases in asperity contact area due to solid-state deformation. However, field observations on exhumed fault zones indicate that solution-transport processes, pressure solution, crack healing and contact overgrowth, influence fault zone rheology near the base of the seismogenic zone. Contact overgrowths result from gradients in surface curvature, where material is dissolved from the pore walls, diffuses through the fluid and precipitates at the contact between two asperities, cementing the asperities together without convergence normal to the contact. To determine the mechanisms and kinetics of asperity cementation, we conducted laboratory experiments in which convex and flat lenses prepared from quartz single crystals were pressed together in an externally heated pressure vessel equipped with an optical observation port. Convergence between the two lenses and contact morphology were continuously monitored during these experiments using reflected-light interferometry through a long-working-distance microscope. Contact normal force is constant with an initial effective normal stress of 1.7 MPa. Four single-phase experiments were conducted at temperatures between 350 and 530C at 150 MPa water pressure, along with two controls: one single phase, dry at 425C and one bimaterial (qtz/sapphire) at 425C and 150 MPa water pressure. No contact growth or convergence was observed in either of the controls. For wet single-phase contacts, however, growth was initially rapid and then decreased with time following an inverse squared dependence of contact radius on aperture. No convergence was observed over the duration of these experiments, suggesting that neither significant pressure solution nor crystal plasticity occurred at these stresses and temperatures. The formation of fluid inclusions between the lenses indicate that the contact is not uniformly wetted. The contact is bounded by small regions of high aperture, reflecting local free-face dissolution as the source for the overgrowth, a definitive indication of diffusion-limited growth. Diffusion-limited growth is also consistent with the inverse squared aperture dependence. However, the apparent activation energy is ~125 kJ/mol, much higher than expected for silica diffusion in bulk water; at present we do not have a complete explanation for the high activation energy. When our lab-measured overgrowth rates are extrapolated to the 5 to 30 micron radius contacts inferred from near-field recordings of M-2 sized earthquakes in deep drill holes and mines (i.e., SAFOD and NELSAM), we predict rates of contact area increase that are orders of magnitude faster than seen in dry, room-temperature friction experiments. This suggests that natural strength recovery should be dominated by fluid-assisted processes at hypocentral conditions near the base of the seismogenic zone.

Detonation waves in pentaerythritol tetranitrate

NASA Astrophysics Data System (ADS)

Tarver, Craig M.; Breithaupt, R. Don; Kury, John W.

1997-06-01

Fabry-Perot laser interferometry was used to obtain nanosecond time resolved particle velocity histories of the free surfaces of tantalum discs accelerated by detonating pentaerythritol tetranitrate (PETN) charges and of the interfaces between PETN detonation products and lithium fluoride crystals. The experimental records were compared to particle velocity histories calculated using very finely zoned meshes of the exact dimensions with the DYNA2D hydrodynamic code. The duration of the PETN detonation reaction zone was demonstrated to be less than the 5 ns initial resolution of the Fabry-Perot technique, because the experimental records were accurately calculated using an instantaneous chemical reaction, the Chapman-Jouguet (C-J) model of detonation, and the reaction product Jones-Wilkins-Lee (JWL) equation of state for PETN detonation products previously determined by supracompression (overdriven detonation) studies. Some of the PETN charges were pressed to densities approaching the crystal density and exhibited the phenomenon of superdetonation. An ignition and growth Zeldovich-von Neumann-Doring (ZND) reactive flow model was developed to explain these experimental records and the results of previous PETN shock initiation experiments on single crystals of PETN. Good agreement was obtained for the induction time delays preceding chemical reaction, the run distances at which the initial shock waves were overtaken by the detonation waves in the compressed PETN, and the measured particle velocity histories produced by the overdriven detonation waves before they could relax to steady state C-J velocity and pressure.

Incident flux angle induced crystal texture transformation in nanostructured molybdenum films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, L.; Lu, T.-M.; Wang, G.-C.

2012-07-15

Molybdenum films were observed to undergo a dramatic change in crystal texture orientation when the incident flux angle was varied in an oblique angle sputter deposition on amorphous substrates. Reflection high-energy electron diffraction pole figure and scanning electron microscopy were used to analyze in detail the texture orientation of the films. The normal incident deposition resulted in a fiber texture film with the minimum energy (110) crystal plane parallel to the substrate surface. A (110)[110] biaxial texture was observed for the samples grown with low incident angles of less than 45 Degree-Sign , with respect to the surface normal. Onmore » the other hand, for an oblique angle deposition of larger than 60 Degree-Sign , a (111)[112] biaxial texture was observed and appeared to be consistent with a zone T structure where the geometrically fastest growth [001] direction of a crystal plays a dominant role in defining the texture. We argue that a structural transition had occurred when the incident flux was varied from near normal incidence to a large angle.« less

Single crystal growth, magnetic and thermal properties of perovskite YFe0.6Mn0.4O3 single crystal

NASA Astrophysics Data System (ADS)

Xie, Tao; Shen, Hui; Zhao, Xiangyang; Man, Peiwen; Wu, Anhua; Su, Liangbi; Xu, Jiayue

2016-11-01

High quality YFe0.6Mn0.4O3 single crystal was grown by floating zone technique using a four-mirror-image-furnace under flowing air. Powder X-ray diffraction gives well evidence that the specimen has an orthorhombic structure, with space group Pbnm. Temperature dependence of the magnetizations of YFe0.6Mn0.4O3 single crystal were studied under ZFC and FC modes in the temperature range from 5 K to 400 K. A clear spin reorientation transition behavior (Γ4→Γ1) is observed in the temperature range of 322-316 K, due to the substitution of Mn at the Fe site of YFeO3. Its Néel temperature is around 385 K. Moreover, the spin reorientation is verified by the change of magnetic hysteresis loops of the sample along [001] axis in the temperature range of 50-385 K. The thermal properties of the sample were measured by the differential scanning calorimeter (DSC) from 300 K to 500 K, which also clearly appear anomaly in the spin reorientation region.

Comparing pre- and post-chemical abrasion ages for Miocene Peach Springs Tuff zircon from ID-TIMS and SIMS analyses

NASA Astrophysics Data System (ADS)

Lidzbarski, M. I.; Mundil, R.; Miller, J. S.; Vazquez, J. A.

2012-12-01

The Miocene Peach Spring Tuff (PST) is a voluminous (>600 km3), zoned ignimbrite (trachyte to high-SiO2 rhyolite) that is exposed widely in eastern California, western Arizona, and southernmost Nevada, which was erupted from the Silver Creek caldera in the southwestern Black Mountains, AZ. PST serves as a regionally widespread marker unit and its eruption age has been determined to 18.8 to 18.9 Ma by 40Ar/39Ar methods, when corrected for systematic bias and normalized to the U-Pb system (Renne et al., 2010,). We performed ion-microprobe (SIMS) U-Pb dating of zircon from individual pumice clasts from PST to evaluate the growth history of zircon in the PST magma system. Sectioned, polished zircon from conventional epoxy mounts allows dating of internal growth domains (e.g. cores, interiors, and near-rim), whereas mounting unpolished zircon in indium and analyzing unpolished crystal faces provides a means to selectively sample the final increments of crystal growth (Reid and Coath, 2000). Combining U-Pb ages of unpolished zircon rims with near-rim interior analyses on sectioned grains yields a mean age of ca. 18.3 Ma, whereas ages of cores of sectioned crystals yield a mean of ca. 18.9 Ma. Several zircons have rim and/or core ages that are several hundred thousand years older or younger than these means (up to 1 m.y. total spread), although the uncertainties for individual SIMS ages are 2 to 5% (2 sigma uncertainty). Therefore, the distribution of ages is challenging to resolve. A modest number of the older grains are plausibly recycled antecrysts, but we suspect that the youngest zircons may have experienced Pb-loss. Failure to account for the possibility of inheritance and Pb-loss may lead to erroneous interpretations about crystallization in the PST system. In order to evaluate and mitigate the effects of Pb-loss, we employed the chemical abrasion (CA) technique of Mattinson (2005), which effectively eliminates domains in zircon that have suffered Pb-loss, and removes micro-inclusions that typically contain common Pb. Thermal annealing followed by CA techniques were used for ID-TIMS dating of a sub-set of zircon crystals previously analyzed by SIMS. Prior to TIMS analyses, zircon crystals were imaged by scanning electron microscopy (SEM) to evaluate the effects of CA on crystal domains sampled by SIMS. SEM images reveal that whole portions of crystals were removed by the CA technique, and a heterogeneous pattern of etching that was not confined to specific compositional zones visible in cathodoluminescence. Most of the SIMS sputter pits that yield spurious ages, are associated with etching and/or preferential annealing by the combined annealing and CA technique, suggesting that the young ages relative to the 40Ar/39Ar age may be due to Pb loss. ID-TIMS yields a coherent U-Pb age population of 18.8 Ma, with several older and younger crystals that might reflect xenocrysts, Pb-loss, and/or younger crystallization. In order to maintain spatial resolution and further evaluate the effects of Pb-loss in PST zircon, the annealing and CA-technique will be applied to zircon prior to SIMS dating. References: Reid and Coath, 2000, Geology 28: 443 Renne et al., 2010, GCA 78: 5349

Simulation, modeling, and crystal growth of Cd0.9Zn0.1Te for nuclear spectrometers

NASA Astrophysics Data System (ADS)

Mandal, Krishna C.; Kang, Sung Hoon; Choi, Michael; Bello, Job; Zheng, Lili; Zhang, Hui; Groza, Michael; Roy, Utpal N.; Burger, Arnold; Jellison, Gerald E.; Holcomb, David E.; Wright, Gomez W.; Williams, Joseph A.

2006-06-01

High-quality, large (10 cm long and 2.5 cm diameter), nuclear spectrometer grade Cd0.9Zn0.1Te (CZT) single crystals have been grown by a controlled vertical Bridgman technique using in-house zone refined precursor materials (Cd, Zn, and Te). A state-of-the-art computer model, multizone adaptive scheme for transport and phase-change processes (MASTRAP), is used to model heat and mass transfer in the Bridgman growth system and to predict the stress distribution in the as-grown CZT crystal and optimize the thermal profile. The model accounts for heat transfer in the multiphase system, convection in the melt, and interface dynamics. The grown semi-insulating (SI) CZT crystals have demonstrated promising results for high-resolution room-temperature radiation detectors due to their high dark resistivity (ρ≈2.8 × 1011 Θ cm), good charge-transport properties [electron and hole mobility-life-time product, μτe≈(2 5)×10-3 and μτh≈(3 5)×10-5 respectively, and low cost of production. Spectroscopic ellipsometry and optical transmission measurements were carried out on the grown CZT crystals using two-modulator generalized ellipsometry (2-MGE). The refractive index n and extinction coefficient k were determined by mathematically eliminating the ˜3-nm surface roughness layer. Nuclear detection measurements on the single-element CZT detectors with 241Am and 137Cs clearly detected 59.6 and 662 keV energies with energy resolution (FWHM) of 2.4 keV (4.0%) and 9.2 keV (1.4%), respectively.

Numerical simulations of porous medium with different permeabilities and positions in a laterally-heated cylindrical enclosure for crystal growth

NASA Astrophysics Data System (ADS)

Enayati, Hooman; Braun, Minel J.; Chandy, Abhilash J.

2018-02-01

This paper presents an investigation of flow and heat transfer in a large diameter (6.25 in) cylindrical enclosure heated laterally and containing a porous block that simulates the basket of nutrients used in a crystal growth reactor. The numerical model entails the use of a commercially available computational engine provided by ANSYS FLUENT, and based on a two-dimensional (2D) axisymmetric Reynolds-averaged Navier Stokes (RANS) equations. The porous medium is simulated using the Brinkman-extended model accounting for the Darcy and Forchheimer induced pressure drops. The porous 'plug' effects are analyzed as both its permeability/inertial resistance and locations in the reactor are changed on a parametric basis, while the Rayleigh number (Ra = gβΔTL3/να) is kept constant at 1.98 × 109. Additionally, the effect of different ratios of the hot to the cold zone lengths are investigated as a part of the current effort. For all cases, the velocity and temperature distributions in the reactor are analyzed together with the flow patterns in, and around the porous block. A comprehensive discussion is provided with regard to the effects of the position of the porous block and its permeability on both the immediately adjacent, and far flows. The consequences on the temperature distribution in the enclosure, when the ratio of the length of the hot-to-cold zones is changed, are also analyzed.

Crystallization Temperatures of Lower Crustal Gabbros from the Oman Ophiolite and the Persistence of the 'Mush Zone' at Intermediate/Fast Spreading Ridges

NASA Astrophysics Data System (ADS)

VanTongeren, J. A.

2017-12-01

Oceanic crust is formed when mantle-derived magmas are emplaced at the ridge axis, a zone of intense rifting and extension. Magmas begin to cool and crystallize on-axis, forming what is termed the "Mush Zone", a region of partially molten rocks. Several attempts have been made to understand the nature of the Mush Zone at fast spreading mid-ocean ridges, specifically how much partial melt exists and how far off-axis the Mush Zone extends. Geophysical estimates of P-wave velocity perturbations at the East Pacific Rise show a region of low velocity approximately 1.5-2.5 km off-axis, which can be interpreted to be the result of higher temperature [e.g. Dunn et al., 2000, JGR] or the existence of partial melt. New petrological and geochemical data and methods allow for the calculation of the lateral extent of the Mush Zone in the lower oceanic crust on exposed sections collected from the Oman ophiolite, a paleo-fast/intermediate spreading center. I will present new data quantifying the crystallization temperatures of gabbros from the Wadi Khafifah section of lower oceanic gabbros from the Oman ophiolite. Crystallization temperatures are calculated with the newly developed plagioclase-pyroxene REE thermometer of Sun and Liang [2017, Contrib. Min. Pet.]. There does not appear to be any systematic change in the crystallization temperature of lower crustal gabbros with depth in the crust. In order to quantify the duration of crystallization and the lateral extent of the Mush Zone of the lower crust, crystallization temperatures are paired with estimates of the solidus temperature and cooling rate determined from the same sample, previously constrained by the Ca diffusion in olivine geothermometer/ geospeedometer [e.g. VanTongeren et al., 2008 EPSL]. There is no systematic variation in the closure temperature of Ca in olivine, or the cooling rate to the 800°C isotherm. These results show that gabbros throughout the lower crust of the Oman ophiolite remain in a partially molten state for an average of 10,000 years. Assuming a paleo-spreading rate similar to that of the East Pacific Rise, this translates to a "Mush Zone" of partially molten rock up to 1 km off-axis, slightly less than the low velocity zone observed geophysically on the East Pacific Rise.

Convection Induced by Traveling Magnetic Fields in Semiconductor Melts

NASA Technical Reports Server (NTRS)

Konstantin, Mazuruk

2000-01-01

Axisymmetric traveling magnetic fields (TMF) can be beneficial for crystal growth applications. such as the vertical Bridgman, float zone or traveling heater methods. TMF induces a basic flow in the form of a single roll. This type of flow can enhance mass and heat transfer to the growing crystal. More importantly, the TMF Lorentz body force induced in the system can counterbalance the buoyancy forces, so the resulting convection can be much smaller and even the direction of it can be changed. In this presentation, we display basic features of this novel technique. In particular, numerical calculations of the Lorentz force for arbitrary frequencies will be presented along with induced steady-state fluid flow profiles. Also, numerical modeling of the TMF counter-balancing natural convection in vertical Bridgman systems will be demonstrated.

Thermal conductivity studies of CdZnTe with varying Te excess

DOE PAGES

Jackson, Maxx; Bennett, Brittany; Giltnane, Dustin; ...

2016-08-28

Cadmium Zine Telluride (CZT) has been extensively studied as a room temperature semiconductor gamma radiation detector. CZT continues to show promise as a bulk and pixelated gamma spectrometer with less than one percent energy resolution; however the fabrication costs are high. Improved yields of high quality, large CZT spectroscopy grade crystals must be achieved. CZT is grown by the Traveling Heater Method (THM) with a Te overpressure to account for vaporization losses. This procedure creates Te rich zones. During growth, boules will often cleave limiting the number of harvestable crystals. As a result, crystal growth parameter optimization was evaluated bymore » modeling the heat flow within the system. Interestingly, Cadmium Telluride (CdTe) is used as a thermal conductivity surrogate in the absence of a thorough study of the CZT thermal properties. The current study has measured the thermal conductivity of CZT pressed powders with varying Te concentrations from 50-100% over 25-800°C to understand the variation in this parameter from CdTe. Cd0.9Zn0.1Te1.0 is the base CZT (designated 50%). CZT exhibits a thermal conductivity of nearly 1 W/mK, an order of magnitude greater than CdTe. Lastly, the thermal conductivity decreased with increasing Te concentration.« less

Thermal conductivity studies of CdZnTe with varying Te excess

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jackson, Maxx; Bennett, Brittany; Giltnane, Dustin

Cadmium Zine Telluride (CZT) has been extensively studied as a room temperature semiconductor gamma radiation detector. CZT continues to show promise as a bulk and pixelated gamma spectrometer with less than one percent energy resolution; however the fabrication costs are high. Improved yields of high quality, large CZT spectroscopy grade crystals must be achieved. CZT is grown by the Traveling Heater Method (THM) with a Te overpressure to account for vaporization losses. This procedure creates Te rich zones. During growth, boules will often cleave limiting the number of harvestable crystals. As a result, crystal growth parameter optimization was evaluated bymore » modeling the heat flow within the system. Interestingly, Cadmium Telluride (CdTe) is used as a thermal conductivity surrogate in the absence of a thorough study of the CZT thermal properties. The current study has measured the thermal conductivity of CZT pressed powders with varying Te concentrations from 50-100% over 25-800°C to understand the variation in this parameter from CdTe. Cd0.9Zn0.1Te1.0 is the base CZT (designated 50%). CZT exhibits a thermal conductivity of nearly 1 W/mK, an order of magnitude greater than CdTe. Lastly, the thermal conductivity decreased with increasing Te concentration.« less

A Little Island With A Big Secret: Isla Rábida, Galápagos

NASA Astrophysics Data System (ADS)

Bercovici, H.; Geist, D.; Harpp, K. S.; Almeida, M.; Mahr, J.; Pimentel, R.; Cleary, Z.

2016-12-01

The Galápagos Archipelago is a hotspot island chain 1000 km west of Ecuador, where the vast majority of the lavas are basaltic. Four volcanoes in the archipelago, Rábida, Santiago, Pinzón, and Alcedo, erupt rhyolites and trachytes. Isla Rábida, a small island 50 km east of the mantle plume center, is the focus of this project. It is 5 km2 in area, and lavas range from 0.9 to 1.1 Ma. About 25% of the rocks in our suite are intermediate to felsic, extending from Mg#=2 to 57. Major and trace element data indicate the evolved rocks formed by advanced crystallization of basaltic magma. One of the unique aspects of Rábida is the cumulate xenolith suite ranging from olivine gabbro to ferroan granite. The basalts have 6 to 58 modal% plagioclase phenocrysts, which we interpret as mixtures of melt and accumulated plagioclase mush at the margins of the shallow reservoir. Thus, Rábida erupts material that has undergone different extents of crystallization and crystal sorting from pure melts, to melt-mush hybrids, to solidified cumulates. This hypothesis is evaluated by comparing plagioclase compositions from the xenoliths and the lavas. Plagioclases in two of the lavas, one with Mg#=57 and the other with Mg#=36, have similar compositions and zonation patterns to each other. There is on average less than 4% change in anorthite content from the core of the plagioclases in the basalts to the rim, with the compositions overall varying between An22 and An37. Both melts likely picked up the crystals from the same plagioclase mush before eruption. In comparison to plagioclases in an olivine-gabbro xenolith from Rábida, those in the lavas are less zoned, suggesting that the lavas' plagioclases experienced a different growth environment. Plagioclases in the xenolith are normally zoned, with cores averaging An37 and rims averaging An32. The xenolith's plagioclases also have more diverse compositions than those in the lavas. The normal zoning in the xenolith's plagioclase is likely from late-stage crystallization of evolved intercumulus melt. Our results suggest that the extraordinary petrologic diversity of Rábida is attributable to crystal-liquid segregation and reincorporation of plagioclase in various melts. These processes result in the eruption of pure melt, melt mixed with mush, and cumulates.

Study of the specific features of single-crystal boron microstructure

NASA Astrophysics Data System (ADS)

Blagov, A. E.; Vasil'ev, A. L.; Dmitriev, V. P.; Ivanova, A. G.; Kulikov, A. G.; Marchenkov, N. V.; Popov, P. A.; Presnyakov, M. Yu.; Prosekov, P. A.; Pisarevskii, Yu. V.; Targonskii, A. V.; Chernaya, T. S.; Chernyshov, D. Yu.

2017-09-01

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δ a/ a ≈ 0.4 and δ c/ c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [2\\bar 2013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3-0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50-300 K are indicative of its high structural quality.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shearer, C.K.; Papike, J.J.; Simon, S.B.

1989-05-01

To study the effects of crystallization sequence and rate on trace element zoning characteristics of pyroxenes, the authors used combined electron microprobe-ion microprobe techniques on four nearly isochemical Apollo 12 and 15 pigeonite basalts with different cooling rates and crystallization histories. Major and minor element zoning characteristics are nearly identical to those reported in the literature. All the pyroxenes have similar chondrite-normalized REE patterns: negative Eu anomalies, positive slopes as defined by Yb/Ce, and slopes of REE patterns from Ce to Sm much steeper than from Gd to Yb. These trace element zoning characteristics in pyroxene and the partitioning ofmore » trace elements between pyroxene and the melt are intimately related to the interplay among 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 within both the pyroxene and the associated crystallizing phases (i.e. plagioclase).« less

Exploring the zone of anisotropy and broken symmetries in DNA-mediated nanoparticle crystallization.

PubMed

O'Brien, Matthew N; Girard, Martin; Lin, Hai-Xin; Millan, Jaime A; Olvera de la Cruz, Monica; Lee, Byeongdu; Mirkin, Chad A

2016-09-20

In this work, we present a joint experimental and molecular dynamics simulations effort to understand and map the crystallization behavior of polyhedral nanoparticles assembled via the interaction of DNA surface ligands. In these systems, we systematically investigated the interplay between the effects of particle core (via the particle symmetry and particle size) and ligands (via the ligand length) on crystallization behavior. This investigation revealed rich phase diagrams, previously unobserved phase transitions in polyhedral crystallization behavior, and an unexpected symmetry breaking in the ligand distribution on a particle surface. To understand these results, we introduce the concept of a zone of anisotropy, or the portion of the phase space where the anisotropy of the particle is preserved in the crystallization behavior. Through comparison of the zone of anisotropy for each particle we develop a foundational roadmap to guide future investigations.

Timing of magma storage at the Vulcano Island during the last 1000 years

NASA Astrophysics Data System (ADS)

De Rosa, Rosanna; Donato, Paola; Gioncada, Anna; Giuffrida, Marisa; Nicotra, Eugenio; Viccaro, Marco

2016-04-01

Understanding the nature and timescales of magmatic processes is one of the primary goals of modern volcanology, and chemical zoning is an efficient tool to achieve this aim. In basic volcanic rocks, plagioclase is a common phase used for documenting magmatic processes and their timescales. This is chiefly due to its stability over a wide range of physical-chemical conditions and its sensitivity to changes in thermodynamic parameters during its growth in magma storage and transport zones. We present here textural analysis and major (SEM-EDS/WDS) and trace (LA-ICP-MS) element zoning data on plagioclase crystals from selected volcanic products of Vulcano (Aeolian Islands), emitted during the last 1000 years. The collected samples belong to the La Fossa cone (Palizzi latitic lava flow, latitic enclaves within Commenda and Pietre Cotte rhyolitic lava flows, 1888-90 spatter bombs) and Vulcanello peninsula (shoshonitic and shoshonitic-latitic lava flows at the end of Vulcanello I and Vulcanello 3 phases, respectively). Textural observations through polarizing optical microscope, high-contrast BSE images and SEM-EDS/WDS core-to-rim profiles, allowed to discriminate four different plagioclase textures, namely: 1) oscillatory-zoned crystals; 2) sieve-textured rims; 3) dissolved/resorbed cores; 4) cores with coarse sieve-textures. Plagioclase with sieve-textured rims and coarsely-sieved cores (Types 2 and 4) are the most abundant in the analyzed products. The estimates of maximum magma residence time have been obtained on crystals with exclusive oscillatory-zoned patterns (Type 1) or portions of crystals not severely affected by μm-sized glass inclusions caused by disequilibrium. We used one-step modeling of Sr diffusion considering the highest An content of each crystal and magma temperature ranging between 1075 and 1175° C. Textural observations and core-to-rim profiles on plagioclases show that dynamics of magma ascent and storage are markedly different at La Fossa and Vulcanello systems. Transfer mechanisms are however almost unchanged in each system during the considered timespan. Diffusion modelling gives residence times between 2 and 22 years. The most striking feature is that residence times are relatively low for the most evolved products (latites or latitic enclaves), especially at La Fossa eruptive system (2-19 years), with respect to the less evolved products of Vulcanello (19-21 years). It is worth to note that these timescales cannot account for the total amount of residence time of La Fossa magmas within the crust, but they can reflect the storage time of the most evolved products into the shallowest feeding system. Residence times for Vulcanello magmas could be related to longer magma storage at intermediate levels of the plumbing system followed by rapid transfer at the surface prior to the eruption.

Exploring Cumulates in Small, Shallow Parts of a Large Mafic Magma System to Provide Baseline Models for Crystallization in Larger Intrusions

NASA Astrophysics Data System (ADS)

Srogi, L.; Willis, K. V.; Lutz, T. M.; Plank, T. A.; Pollock, M.; Connolly, B.; Wood, A. M.

2016-12-01

Small, shallow portions of large magmatic systems cool more rapidly and potentially have less subsolidus overprinting than large mafic intrusions, but it is unclear whether they are small-scale analogs for the same crystallization processes. The Morgantown-Jacksonwald magmatic system (MJS), western Newark Basin, Pennsylvania, is part of the 201-Ma Central Atlantic Magmatic Province (CAMP) formed during Pangean rifting. The MJS consists of several interconnected intrusions exposed in cross-section from the Jacksonwald basalt at the paleosurface to 6 km depth (<0.2 GPa). Mg-rich orthopyroxene (opx) phenocrysts form crystal accumulations in some dikes and in basal and roof zones of sills in the MJS, in many CAMP intrusions, and in younger Ferrar dolerites, Antarctica. Some samples with opx phenocrysts have dm-scale modal layering. Despite ubiquitous occurrence, the opx is little-studied and our work tests most previous authors' assumption that opx was brought in from deeper intrusions. Opx cores with Mg/(Mg+Fe) of 80-77% yield mid-crustal pressures of 0.4-0.6 GPa (using method of Putirka, 2008). LA-ICPMS was used to obtain trace element concentrations in mm-size phenocrysts in a chill margin within 0.5m of the basal contact and cm-size phenocrysts from cumulate about 10m above. REE concentrations are similar in both samples: LREE-depleted cores (normalized La/Sm = 0.05-0.1); variably LREE-enriched rims; some negative Eu anomalies. REE patterns calculated for liquids in equilibrium with opx using published Kd values are roughly parallel to but significantly higher than REE in host chill margin diabase. CSDs of opx and matrix plagioclase from several samples within 10m of the basal contact will be used to evaluate models of crystal growth vs. mechanical sorting. Modes and mineral compositions are not consistent with MELTS fractionation models: opx crystallizes in place of pigeonite; pyroxenes are zoned in Ca not Fe-Mg; late-crystallizing quartz and K-feldspar are lacking. These features suggest crystallization buffered by earlier phases in the crystal mush with some melt migration, similar to processes that produce more extreme layering in large mafic intrusions.

High-Performance Doped Strontium Iodide Crystal Growth Using a Modified Bridgman Method

NASA Astrophysics Data System (ADS)

Rowe, Emmanuel

The importance of gamma-ray spectroscopy---the science of determining the distribution of energy in a gamma field---can rarely be overstated. High performance scintillators for gamma-ray spectroscopy in Nuclear Nonproliferation applications and homeland security require excellent energy resolution to distinguish neighboring element and isotope lines while minimizing the time and exposure to do so. Semiconductor detectors operate by converting incident photons directly into electrical pulses, but often have problems of high costs due to constituent segregation and surface states as is the case for Cadmium Zinc Telluride. The ideal scintillator material for gamma spectrometer will therefore requires high light yield, excellent proportionality between light yield and gamma photon energy, and material uniformity. A scintillator should possess the following properties; it should convert the kinetic energy of the generated charged particles (typically K-shell electrons) into detectable visible light. This conversion should be linear-the light yield should be proportional to deposited energy over as wide a range as possible. For good light collection, the medium should be transparent to the wavelength of its own emission. The decay time of the induced luminescence should be short so that fast signal pulses can be generated. The medium should be of good optical quality and subject to manufacture in sizes large enough to be of interest as a practical detector. Its index of refraction should be near that of glass (~1.5) to permit efficient coupling of scintillation light to a photomultiplier tube or other photo-sensor. In the past decade, inorganic scintillator research has focused less on improving the characteristics of known scintillators, but rather on the search for new hosts capable of fast response and high energy resolution. Extensive searches have been made for hosts doped with lanthanide activators utilizing the allowed 5d-4f transition. These 5d-4f transitions are dipole-allowed and thus are about 106 times stronger than the more frequently observed 4f-4f transition in the trivalent rare earth ions. Ce3+, Nd3+ and Pr3+ have been investigated for fast response applications while Ce3+, Eu 2+, and Yb2+ stand out as the most promising activators offering high light yield, and high energy resolution. Using a modified Bridgman growth technique we have grown crystals with a low energy resolution of 2.6% at 662 keV, which is lower than the previous 2.8% reported for SrI2:Eu 2+. The modified technique (called so for its vertical crystal growth orientation) is necessary due to the anisotropic thermal expansion coefficient of Strontium Iodide. The problem plaguing the growth of the crystal is spontaneous cracking, which usually appear during cooling in the bulk. With the use of a zone separating shield, one can achieve more control of the temperature gradient between the two zones without compromising the actual temperature of the two zones. Additionally the use of codopants, in particular divalent magnesium improved the crystalline quality by acting as a gathering for iodine ions, which led to reduction of defect density.

Peculiar Feldspar And Quartz Inclusions Within Zircons From Anorthosites, North Eastern Desert, Egypt

NASA Astrophysics Data System (ADS)

Eliwa, H. A.; Dawoud, M. I.; Khalaf, I. M.; Negendank, J. F.; Itaya, T.

2004-12-01

Zircons from three anorthosite outcrops along Wadi Dib area, north Eastern Desert of Egypt contain abundant and conspicuous inclusions of quartz, feldspar, amphibole and apatite. These anorthosites, as (50-100m thick) layers, represent the top of mafic-ultramafic intrusions exhibiting rhythmic layering visible by reputation of melanocratic and leucocratic layers. Field and microscopic studies exhibit that these anorthosites were affected by the action of residual magmatic solutions associated with the late stage crystallization of the younger granites, which modified their mineralogical composition. They are composed totally of plagioclase with subordinate amount of clinoenstatite, augite, amphibole, biotite, K-feldspar, and quartz. Accessories are magnetite, ilmenite, apatite and zircon. The abundance and the mode of occurrence of K-feldspar, quartz, and biotite with apatite and zircon among the megacrysts suggest their formation is ascribed to the interaction with the residual solutions. The microprobe data exhibit difference between feldspar and amphiboles contained herein zircons and those as anorthosite mineral constituents. The genetic relationship between zircons and their inclusions suggests later growth of zircons than inclusions and most probably at the final stage of rock modification. Zircons are magmatic and found in the interstitial feldspar and quartz among plagioclase megacrysts in aggregates or as individual grains. The microscopic and SEM images investigation exhibit that most zircons are subhedral to euhedral equant and prismatic crystals. Most zircons have same range of crystal morphologies and internal growth structures with predominance of prism /{100/} and pyramid /{101/} and occasionally prism /{110/} and pyramid /{111/}. No evidences for poly-faceted grains, inherited cores or later overgrowths were detected. CL images distinguished zircons with visible core-rim structures and others with regular and continuous growth zones contained herein various inclusions. The dark CL cores in the core-rim structured zircons are higher in U, Y and sometimes Hf relative to the CL bright rims. Microprobe data and x-ray chemical mapping of various zoned zircons suggest that U and Y with sometimes Hf have a negative correlation to the CL brightness, while Th doesn't exhibit any significant correlation.

Tourmaline's record of Alpine metamorphism and segregation formation in the Pfitsch Formation, Western Tauern Window

NASA Astrophysics Data System (ADS)

Berryman, E. J.; Kutzschbach, M.; Trumbull, R. B.; Meixner, A.; van Hinsberg, V.; Kasemann, S.; Franz, G.

2017-12-01

Tourmaline, a common accessory mineral in the metasedimentary units of the Pfitsch Formation in the Western Tauern Window, Eastern Alps, records the variation in fluid composition and B mobilization during Alpine metamorphism. These post-Variscan metasediments are part of the Subpenninic nappes, the former European distal margin, and experienced peak metamorphic conditions of 550°C, 1.0 GPa. In all investigated units, tourmaline is predominantly dravitic, with high Fe contents. Charge balance calculations combined with Fe-Mg and Fe-Al variation suggest a significant proportion of ferric iron. Tourmaline's composition reflects its host rock assemblage, with the relative predominance of Fe-Mg or Fe-Al exchange in tourmaline from different units corresponding to the presence of biotite/chlorite or muscovite, respectively. Boron content and correspondingly tourmaline abundance is highest in a 25 m thick unit of feldspathic gneiss ( 20-200 ppm B). The abundance and size of the tourmaline crystals increases near coarse-grained quartzofeldspathic segregations ( 1200 ppm B), reflecting the mobilization and concentration of B by the metamorphic fluid. Tourmaline crystals near segregations have up to three growth zones, recording pro- ( 350-500°C, 0.7-1.0 GPa) and retrograde (400°C, 0.2 GPa) growth. They show the largest amount of compositional variation, covering the range of compositional space represented by tourmaline occurring away from segregations. Tourmaline near segregations has the highest inferred ferric iron content, which decreases across growth zones, potentially reflecting the gradual reduction of the fluid during metamorphism. Whole rock δ11B values (-15 to -34‰) vary with the heaviest values found near B-rich segregations, and the lightest values in B-depleted samples. This correlation reflects the preferential mobilization of 11B towards the segregations. Isotopic zonation of individual tourmaline crystals with -11‰ in their cores and -20‰ in their rims suggests continuous volatilization and fractionation of B by a 10B-rich precursor mineral (e.g. mica) during prograde mobilization and redistribution of B within the Pfitsch Formation.

Shape Evolution of Detached Bridgman Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2015-01-01

Detached (or dewetted) Bridgman crystal growth defines that process in which a gap exists between a growing crystal and the crucible wall. In microgravity, the parameters that influence the existence of a stable gap are the growth angle of the solidifying crystal, the contact angle between the melt and the crucible wall, and the pressure difference across the meniscus. During actual crystal growth, the initial crystal radius will not have the precise value required for stable detached growth. Beginning with a crystal diameter that differs from stable conditions, numerical calculations are used to analyze the transient crystal growth process. Depending on the initial conditions and growth parameters, the crystal shape will either evolve towards attachment at the crucible wall, towards a stable gap width, or inwards towards eventual collapse of the meniscus. Dynamic growth stability is observed only when the sum of the growth and contact angles exceeds 180 degrees.

The Freyenstein Shear Zone - Implications for exhumation of the South Bohemian Batholith (Moldanubian Superunit, Strudengau, Austria)

NASA Astrophysics Data System (ADS)

Griesmeier, Gerit; Iglseder, Christoph; Konstantin, Petrakakis

2016-04-01

The Moldanubian superunit is part of the internal zone of the Variscan Orogen in Europe and borders on the Saxothuringian and Sudetes zones in the north. In the south, it is blanketed by the Alpine foreland molasse. Tectonically it is subdivided into the Moldanubian Nappes (MN), the South Bohemian Batholith (SBB) and the Bavarian Nappes. This work describes the ~ 500 m thick Freyenstein shear zone, which is located at the southern border of the Bohemian Massif north and south of the Danube near Freyenstein (Strudengau, Lower Austria). The area is built up by granites of Weinsberg-type, which are interlayered by numerous dikes and paragneisses of the Ostrong nappe system. These dikes include medium grained granites and finegrained granites (Mauthausen-type granites), which form huge intrusions. In addition, smaller intrusions of dark, finegrained diorites und aplitic dikes are observed. These rocks are affected by the Freyenstein shear zone und ductily deformed. Highly deformed pegmatoides containing white mica crystals up to one cm cut through the deformed rocks and form the last dike generation. The Freyenstein shear zone is a NE-SW striking shear zone at the eastern edge of the SBB. The mylonitic foliation is dipping to the SE with angles around 60°. Shear-sense criteria like clast geometries, SĆ structures as well as microstructures show normal faulting top to S/SW with steep (ca. 50°) angles. The Freyenstein shear zone records a polyphase history of deformation and crystallization: In a first phase, mylonitized mineral assemblages in deformed granitoides can be observed, which consist of pre- to syntectonic muscovite-porphyroclasts and biotite as well as dynamically recrystallized potassium feldspar, plagioclase and quartz. The muscovite porphyroclasts often form mica fishes and show top to S/SW directed shear-sense. The lack of syntectonic chlorite crystals points to metamorphic conditions of lower amphibolite-facies > than 450° C. In a later stage fluid infiltration under lower greenschist-facies conditions locally lead to sericitization of feldspar and development of pseudomorphs after it. In addition, syn-mylonitic biotite has been chloritized mimetically. Chlorite growth across the mylonitic foliation occurs rarely. Brittle faulting, overprinting the shear zone features, is documented by the occurrence of numerous harnish planes. They show normal faulting to the N with angles around 30° and locally sinistral shear-sense. The Freyenstein shear zone belongs to a system of NE-SW striking shear zones and faults in the Moldanubian superunit and is located at the border between the SBB and MN ductily deforming both. Therefore, it plays an important role in exhumation processes of last stage SBB (synkinematic) intrusions during Late Variscan orogenic extension. According to cooling ages in other shear zones and (synkinematic) intrusions an age of ca. 320-290 Ma for the ductile deformation can be assumed.

Spectral, electron microscopic and chemical investigations of gamma-induced purple color zonings in amethyst crystals from the Dursunbey-Balıkesir region of Turkey

NASA Astrophysics Data System (ADS)

Hatipoğlu, Murat; Kibar, Rana; Çetin, Ahmet; Can, Nurdoğan; Helvacı, Cahit; Derin, H.

2011-07-01

Amethyst crystals on matrix specimens from the Dursunbey-Balıkesir region in Turkey have five representative purple color zonings: dark purple, light purple, lilac, orchid, and violet. The purple color zonings have been analyzed with optical absorption spectra in the visible wavelength region, chemical full trace element analyses (inductively coupled plasma-atomic emission spectroscopy and inductively coupled plasma-mass spectroscopy), and scanning electron microscopic images with high magnification. It can be proposed that the production of the purple color in amethyst crystals is due to three dominant absorption bands centered at 375, 530, and 675 nm, respectively. In addition, the purple color zonings are also due to four minor absorption bands centered at 435, 480, 620, and 760 nm. X-ray diffraction graphics of the investigated amethyst crystals indicate that these crystals are composed of a nearly pure alpha-quartz phase and do not include any moganite silica phase and/or other mineral implications. Trace element analyses of the amethyst crystals show five representative purple color zonings, suggesting that the absorption bands can be mainly attributed to extrinsic defects (chemical impurities). However, another important factor that influences all structural defects in amethyst is likely to be the gamma irradiation that exists during amethyst crystallization and its inclusion in host materials. This gamma irradiation originates from the large underlying intrusive granitoid body in the region of amethyst formation. Irradiation modifies the valence values of the impurity elements in the amethyst crystals. It is observed that the violet-colored amethyst crystals have the most stable and the least reversible coloration when exposed to strong light sources. This situation can be related to the higher impurity content of Fe (2.50 ppm), Co (3.1 ppm), Ni (38 ppm), Cu (17.9 ppm), Zn (10 ppm), Zr (3.9 ppm), and Mo (21.8 ppm).

Crystals and Crystals: On the Mythology of Magmatic Processes

NASA Astrophysics Data System (ADS)

Marsh, B.

2008-12-01

The intimate records of the deep functioning of magmatic systems reside in the temporal and spatial records of magma flux, composition and crystal load. The records for a single system are piecemeal: Plutons show good spatial records, but poor temporal records. Volcanoes give through lava sequences good temporal records, but no spatial context. Because of this dichotomy, two, almost mutually exclusive, branches of magmatology have developed, whereas in Nature there is only a single process. The processes envisioned in these schools necessary to deliver the end rock record are distinct. It is our tools and historic perspectives that have steered the science, not the subject itself. Due to this approach an almost mythical conception of how magmas function has become commonplace. The circumvention of this dilemma rests in carefully evaluating the records on hand in the light of a broad understanding of the fundamental mechanics of how magma lives and dies. It is these basic principles that promise to unify plutonic and volcanic evidence to reveal the full nature of magmatism on all scales. The two most basic features of all magmatic processes are the universal presence of solidification fronts and the presence or absence of a crystal cargo. Almost without exception (e.g., shallow pressure quenching) all first generation crystals grow in marginal solidification fronts (SFs) bordering all magmas. The package of isotherms bounded by the liquidus and solidus define SFs, which propagate in response to the rate of cooling. All physical and chemical processes occurring within SFs compete with the advancement or retreat of solidification. SFs are governed by crystallinity regimes: Suspension Zone (<25 % xtals), Capture Front (~25 %), Mush Zone (25-55%), Rigidity Front (~55%; Critical Crystallinity), and Rigid Crust Zone (>55% xtals). Magmas are laced with nuclei that multiply and grow when overtaken. Crystal growth rates are bounded; tiny crystals reside at the front of SFs and big crystals at the rear. It is unlikely that crystals can ever escape SFs once beyond the Capture Front, and crystals that do fall (singly or in plumes) from the leading edge of SFs may suffer resorbtion upon transit through deeper, hotter magma. Above all, differentiation is severely limited as there is no crystallization in the central, hottest part of the body, and the crystals that are available for separation are tiny and have little effect on melt composition. Recall, ~50% loss of olivine enhances silica by 5%, but this places this magma at Critical Crystallinity. Phenocrysts come from disrupted SFs and are essential to read as such; they may come from a wide range of P's and T's. Ragged old crystals rolling about for untold numbers of flushing times record specious process times; telling more about transport and crystal-chemical noise in the system than the life of typical, first generation crystallization processes. Yet, noise is a system characteristic as is exemplified by the disharmonious isotope heritage of neighbor phenocrysts. Differentiation mainly comes from the sudden loss of a dynamically entrained load of crystals of diverse heritage equilibrating with the 'carrier' magma. Big crystals carrying fluid inclusions, for example, come from deep within SFs where residual melt is low and enriched and not from the central, early, primitive magma. All systems show these characteristics. They are exceedingly important to recognize and to put in the context of the power, longevity, and geometry of the system. Not recognizing them for what they are and what they are not recording only builds mythological magmatic systems.

Purification of Germanium Crystals by Zone Refining

NASA Astrophysics Data System (ADS)

Kooi, Kyler; Yang, Gang; Mei, Dongming

2016-09-01

Germanium zone refining is one of the most important techniques used to produce high purity germanium (HPGe) single crystals for the fabrication of nuclear radiation detectors. During zone refining the impurities are isolated to different parts of the ingot. In practice, the effective isolation of an impurity is dependent on many parameters, including molten zone travel speed, the ratio of ingot length to molten zone width, and number of passes. By studying the theory of these influential factors, perfecting our cleaning and preparation procedures, and analyzing the origin and distribution of our impurities (aluminum, boron, gallium, and phosphorous) identified using photothermal ionization spectroscopy (PTIS), we have optimized these parameters to produce HPGe. We have achieved a net impurity level of 1010 /cm3 for our zone-refined ingots, measured with van der Pauw and Hall-effect methods. Zone-refined ingots of this purity can be processed into a detector grade HPGe single crystal, which can be used to fabricate detectors for dark matter and neutrinoless double beta decay detection. This project was financially supported by DOE Grant (DE-FG02-10ER46709) and the State Governor's Research Center.

Finite-difference fluid dynamics computer mathematical models for the design and interpretation of experiments for space flight. [atmospheric general circulation experiment, convection in a float zone, and the Bridgman-Stockbarger crystal growing system

NASA Technical Reports Server (NTRS)

Roberts, G. O.; Fowlis, W. W.; Miller, T. L.

1984-01-01

Numerical methods are used to design a spherical baroclinic flow model experiment of the large scale atmosphere flow for Spacelab. The dielectric simulation of radial gravity is only dominant in a low gravity environment. Computer codes are developed to study the processes at work in crystal growing systems which are also candidates for space flight. Crystalline materials rarely achieve their potential properties because of imperfections and component concentration variations. Thermosolutal convection in the liquid melt can be the cause of these imperfections. Such convection is suppressed in a low gravity environment. Two and three dimensional finite difference codes are being used for this work. Nonuniform meshes and implicit iterative methods are used. The iterative method for steady solutions is based on time stepping but has the options of different time steps for velocity and temperature and of a time step varying smoothly with position according to specified powers of the mesh spacings. This allows for more rapid convergence. The code being developed for the crystal growth studies allows for growth of the crystal as the solid-liquid interface. The moving interface is followed using finite differences; shape variations are permitted. For convenience in applying finite differences in the solid and liquid, a time dependent coordinate transformation is used to make this interface a coordinate surface.

Can Supersaturation Affect Protein Crystal Quality?

NASA Technical Reports Server (NTRS)

Gorti, Sridhar

2013-01-01

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.

Electrical, Thermal, and Magnetic Properties of Single Crystal CaMn2O4 Marokite

NASA Astrophysics Data System (ADS)

White, B. D.; Neumeier, J. J.; Souza, J. A.; Chiorescu, C.; Cohn, J. L.

2008-03-01

CaMn2O4 was first described [1] in 1963 as a natural mineral called Marokite. Since its discovery, it has been studied as a minor structural impurity phase in CMR- related CaMnO3 and for its structural similarities to high-pressure phases of spinel-oxide compounds. However, little attention has previously been paid to physical properties beyond its temperature-dependent magnetization. We will present a detailed physical properties study of CaMn2O4 single crystals grown by the optical floating zone method. [2] These measurements, several of which display anisotropy as a result of an orthorhombic crystal structure, include electrical transport, thermal transport, thermal expansion, heat capacity, and magnetization. [1] C. Gaudefroy, G. Jouravsky, F. Permingeat, Bull. Soc. Franc. Min'er. Crist. 86 (1963) 359. [2] B. D. White, C. A. M. dos Santos, J. A. Souza, K. J. McClellan, J. J. Neumeier submitted to J. Cryst. Growth.

Timing and duration of garnet granulite metamorphism in magmatic arc crust, Fiordland, New Zealand

USGS Publications Warehouse

Stowell, H.; Tulloch, A.; Zuluaga, C.; Koenig, A.

2010-01-01

Pembroke Granulite from Fiordland, New Zealand provides a window into the mid- to lower crust of magmatic arcs. Garnet Sm-Nd and zircon U-Pb ages constrain the timing and duration of high-P partial melting that produced trondhjemitic high Sr/Y magma. Trace element zoning in large, euhedral garnet is compatible with little post growth modification and supports the interpretation that garnet Sm-Nd ages of 126.1??2.0 and 122.6??2.0. Ma date crystal growth. Integration of the garnet ages with U-Pb zircon ages elucidates a history of intrusion(?) and a protracted period of high-temperature metamorphism and partial melting. The oldest zircon ages of 163 to 150. Ma reflect inheritance or intrusion and a cluster of zircon ages ca. 134. Ma date orthopyroxene-bearing mineral assemblages that may be magmatic or metamorphic in origin. Zircon and garnet ages from unmelted gneiss and garnet reaction zones record garnet granulite facies metamorphism at 128 to 126. Ma. Peritectic garnet and additional zircon ages from trondhjemite veins and garnet reaction zones indicate that garnet growth and partial melting lasted until ca. 123. Ma. Two single fraction garnet ages and young zircon ages suggest continued high-temperature re-equilibration until ca. 95. Ma. Phase diagram sections constrain orthopyroxene assemblages to <0.6 GPa @ 650??C, peak garnet granulite facies metamorphic conditions to 680-815??C @ 1.1-1.4. GPa, and a P-T path with a P increase of???0.5. GPa. These sections are compatible with water contents???0.28wt.%, local dehydration during garnet granulite metamorphism, and <0.3. GPa P increases during garnet growth. Results demonstrate the utility of integrated U-Pb zircon and Sm-Nd garnet ages, and phase diagram sections for understanding the nature, duration, and conditions of deep crustal metamorphism and melting. Geochronologic and thermobarometric data for garnet granulite indicate that thickening of arc crust, which caused high-pressure metamorphism in northern Fiordland, must have occurred prior to 126. Ma, that loading occurred at a rate of ca. 0.06. GPa/m.y., and that garnet granulite metamorphism lasted 3-7m.y. Locally-derived partial melts formed and crystallized in considerably less than 10 and perhaps as little as 3m.y. ?? 2010 Elsevier B.V.

Unsteady-state transfer of impurities during crystal growth of sucrose in sugarcane solutions

NASA Astrophysics Data System (ADS)

Martins, P. M.; Ferreira, A.; Polanco, S.; Rocha, F.; Damas, A. M.; Rein, P.

2009-07-01

In this work, we present growth rate data of sucrose crystals in the presence of impurities that can be used by both sugar technologists and crystal growth scientists. Growth rate curves measured in a pilot-scale evaporative crystallizer suggest a period of slow growth that follows the seeding of crystals into supersaturated technical solutions. The observed trend was enhanced by adding typical sugarcane impurities such as starch, fructose or dextran to the industrial syrups. Maximum growth rates of sucrose resulted at intermediate rather than high supersaturation levels in the presence of the additives. The effects of the additives on the sucrose solubility and sucrose mass transfer in solution were taken into account to explain the observed crystal growth kinetics. A novel mechanism was identified of unsteady-state adsorption of impurities at the crystal surface and their gradual replacement by the crystallizing solute towards the equilibrium occupation of the active sites for growth. Specifically designed crystallization experiments at controlled supersaturation confirmed this mechanism by showing increasing crystal growth rates with time until reaching a steady-state value for a given supersaturation level and impurity content.

Formation of natural gas hydrates in marine sediments 1. Conceptual model of gas hydrate growth conditioned by host sediment properties

USGS Publications Warehouse

Clennell, M.B.; Hovland, M.; Booth, J.S.; Henry, P.; Winters, W.J.

1999-01-01

The stability of submarine gas hydrates is largely dictated by pressure and temperature, gas composition, and pore water salinity. However, the physical properties and surface chemistry of deep marine sediments may also affect the thermodynamic state, growth kinetics, spatial distributions, and growth forms of clathrates. Our conceptual model presumes that gas hydrate behaves in a way analogous to ice in a freezing soil. Hydrate growth is inhibited within fine-grained sediments by a combination of reduced pore water activity in the vicinity of hydrophilic mineral surfaces, and the excess internal energy of small crystals confined in pores. The excess energy can be thought of as a "capillary pressure" in the hydrate crystal, related to the pore size distribution and the state of stress in the sediment framework. The base of gas hydrate stability in a sequence of fine sediments is predicted by our model to occur at a lower temperature (nearer to the seabed) than would be calculated from bulk thermodynamic equilibrium. Capillary effects or a build up of salt in the system can expand the phase boundary between hydrate and free gas into a divariant field extending over a finite depth range dictated by total methane content and pore-size distribution. Hysteresis between the temperatures of crystallization and dissociation of the clathrate is also predicted. Growth forms commonly observed in hydrate samples recovered from marine sediments (nodules, and lenses in muds; cements in sands) can largely be explained by capillary effects, but kinetics of nucleation and growth are also important. The formation of concentrated gas hydrates in a partially closed system with respect to material transport, or where gas can flush through the system, may lead to water depletion in the host sediment. This "freeze-drying" may be detectable through physical changes to the sediment (low water content and overconsolidation) and/or chemical anomalies in the pore waters and metastable presence of free gas within the normal zone of hydrate stability. 

Mineral growth in rocks: kinetic-rheological models of replacement, vein formation, and syntectonic crystallization

NASA Astrophysics Data System (ADS)

Fletcher, Raymond C.; Merino, Enrique

2001-11-01

We model three cases of coupling between mineral growth kinetics and mechanical response of the rock: (i) dispersed spherical crystals growing by replacement in a hydrostatically stressed elastic rock; (ii) growth of veins or vein networks accommodated by viscous relaxation of surrounding rock; and (iii) syntectonic crystallization in a rock undergoing bulk pure shear. Such models for the microscopic environment of mineral growth, together with additional assumptions or knowledge about rheological behavior and aggregate geometry, provide refined estimates of the behavior of a macroscopic volume element, which could be combined with geochemical reaction-transport models. Crucial in the models are the various consequences-pressure solution, creep, fracturing-of the local stress that is necessarily generated by mineral growth in rocks (other than in pores). In the first model, the dispersed spherical crystals of mineral A are assumed to grow within a spherical volume of rock consisting of mineral B, the ;mineralized zone; (MZ), itself embedded in elastic rock. The macroscopic stress in the MZ and the far-field stress in the surrounding rock are uniform and hydrostatic. Mineral growth of the A crystals is driven by supersaturation with respect to mineral A, is accommodated by replacement of B grains, and leads to an expansion of the MZ described by an infinitesimal strain. The radial growth rate of a spherical crystal of mineral A, with replacement of mineral B, is da/dt=kARTln(ΩA)[kBV0B/(kBV0B+kAV0A)], where kA and kB are kinetic constants, R is the gas constant, T the temperature in kelvin, and V0A and V0B are specific volumes. Reference saturation states of mineral A, ΩA > 1, and host mineral B, ΩB = 1, are specified at the far-field hydrostatic stress, σ0. The microscopic environment of each crystal of A is modeled by a representative volume element (RVE) consisting of a sphere of mineral A embedded in a spherical shell of mineral B. In each RVE, stress is neither uniform nor hydrostatic. The model links the local microscopic stress with the macroscopic stress in the MZ and surrounding rock. The second model refers to veins that make room for themselves by growing, not to veins that form by cementation of previously opened, or opening, cracks. If the growth of mineral A as propagating veins or as an interconnected vein network takes place by deformation and expansion of the MZ-with the deformation itself driven by the stress arising from the supersaturation-driven growth-the surrounding rock undergoes deformation and is treated as viscous. The rate of growth in vein width, w, is dw/dt=2kA[RTln(ΩA)-SV0A]/(1+M), where M = 16ηkAV0Ac2/(3b3), η is the medium viscosity, c is the vein radius, and each vein is treated as centered in a spherical RVE of radius b. S is an effective tensile stress required for vein propagation. For a vein network, in which veins surround equant polyhedra of rock of radius b, we set c = b and drop the term in S for simplicity. Veins may also widen by replacement. The ratio of vein widening by expansion to that by replacement is (dw/dt)expansion/(dw/dt)replacement={(3b/16η)/[(3b/16η)+kAV0A]}/[kBV0B/(KBV0B+kAV0A)]. Both mechanisms of accommodation contribute equally when η = 3b/(16kBV0B); at higher viscosity, replacement is dominant. The incipient growth of a cylindrical crystal with circular cross section in a medium deforming in pure shear simulates syntectonic crystallization. Both dissolution and deformation of the host accommodate growth. In the model, the crystal tends to grow faster in the direction of maximum rate of extension. In this direction, the host mineral may either dissolve to accommodate growth, or precipitate to form a pressure shadow. Accommodation by host dissolution is greatest in the direction of maximum rate of shortening.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

2016-10-01

Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

An Apparatus for Growth of Small Crystals From Solutions.

ERIC Educational Resources Information Center

Mitrovic, Mico M.

1995-01-01

Describes an apparatus for crystal growth that was designed to study growth kinetics of small crystals from solutions and to obtain crystals of various substances. Describes the use of the apparatus in laboratory practical experiments in the field of crystal growth physics within the course "Solid State Physics". (JRH)

Solution Growth and Characterization of Single Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Currie, J. R.; Penn, B. G.; Batra, A. K.; Lal, R. B.

2007-01-01

Crystal growth has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high-technology devices, and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this Technical Memorandum (TM) an attempt is made to give the fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, the authors proposed a new cooled-sting technique to grow crystals in space. The authors experience from conducting two Space Shuttle solution crystal growth experiments are also detailed in this TM and the complexity of solution growth experiments to grow crystals in space are also discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that shares basic principles of the solution growth technique is given, along with some flight hardware information for growth in microgravity.

Growth and Characteristics of Bulk Single Crystals Grown from Solution on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Batra, A. K.; Lal, R. B.; Penn, Benjamin G.; Frazier, Donald O.

2011-01-01

The growth of crystals has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high technology devices and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this chapter an attempt is made to give some fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, authors had proposed a new cooled sting technique to grow crystals in space. Authors? experiences of conducting two space shuttle experiments relating to solution crystal growth are also detailed in this work. The complexity of these solution growth experiments to grow crystals in space are discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that also shares basic principles of solution growth technique is given along with some flight hardware information for its growth in microgravity.

Control of Thermal Convection in Layered Fluids Using Magnetic fields

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F. W.

2003-01-01

Immiscible fluid layers are found in a host of applications ranging from materials processing, for example the use of encapsulants in float zone crystal growth technique and a buffer layer in industrial Czochralski growth of crystals to prevent Marangoni convection, to heat transfer phenomena in day-to-day processes like the presence of air pockets in heat exchangers. In the microgravity and space processing realm, the exploration of other planets requires the development of enabling technologies in several fronts. The reduction in the gravity level poses unique challenges for fluid handling and heat transfer applications. The present work investigates the efficacy of controlling thermal convective flow using magnetic fluids and magnetic fields. The setup is a two-layer immiscible liquids system with one of the fluids being a diluted ferrofluid (super paramagnetic nano particles dispersed in carrier fluid). Using an external magnetic field one can essentially dial in a volumetric force - gravity level, on the magnetic fluid and thereby affect the system thermo-fluid behavior. The paper will describe the experimental and numerical modeling approach to the problem and discuss results obtained to date.

Progress and challenges for cost effective kerfless Silicon crystal growth for PV application

NASA Astrophysics Data System (ADS)

Serra, J. M.; Alves, J. Maia; Vallera, A. M.

2017-06-01

The major barrier for PV penetration is cost. And the single most important cost factor in silicon technology is the wafer (≈35% of the module cost). Although tremendous progress on cell processing has been reported in recent years, a much smaller evolution is seen on what should be the key point to address - the wafer. The ingot-slicing process is reaching its limits as the wafer thickness is reduced in an effort to lower material costs. Kerf losses of ≈50% and an increase in breakage of a high value added material are putting a lower bound to this approach. New ideas are therefore needed for producing wafers in a way to overcome these limitations. In this paper we present three new concepts being developed in our laboratory that have one thing in common: they all are zero kerf loss processes, aiming at significant reductions in material loss. One explores the concept of exfoliation, the other two aim at the growth of silicon directly into ribbons. These were conceived as continuous processes, based on a floating molten zone concept, to avoid impurity contamination during crystallization.

Modeling Czochralski growth of oxide crystals for piezoelectric and optical applications

NASA Astrophysics Data System (ADS)

Stelian, C.; Duffar, T.

2018-05-01

Numerical modeling is applied to investigate the impact of crystal and crucible rotation on the flow pattern and crystal-melt interface shape in Czochralski growth of oxide semi-transparent crystals used for piezoelectric and optical applications. Two cases are simulated in the present work: the growth of piezoelectric langatate (LGT) crystals of 3 cm in diameter in an inductive furnace, and the growth of sapphire crystals of 10 cm in diameter in a resistive configuration. The numerical results indicate that the interface shape depends essentially on the internal radiative heat exchanges in the semi-transparent crystals. Computations performed by applying crystal/crucible rotation show that the interface can be flattened during LGT growth, while flat-interface growth of large diameter sapphire crystals may not be possible.

Protein crystal growth in microgravity

NASA Technical Reports Server (NTRS)

Rosenblum, William M.; Delucas, Lawrence J.; Wilson, William W.

1989-01-01

Major advances have been made in several of the experimental aspects of protein crystallography, leaving protein crystallization as one of the few remaining bottlenecks. As a result, it has become important that the science of protein crystal growth is better understood and that improved methods for protein crystallization are developed. Preliminary experiments with both small molecules and proteins indicate that microgravity may beneficially affect crystal growth. For this reason, a series of protein crystal growth experiments using the Space Shuttle was initiated. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth. Various optical techniques are being utilized to monitor the crystal growth process from the incipient or nucleation stage and throughout the growth phase. The eventual goal of these studies is to develop a system which utilizes optical monitoring for dynamic control of the crystallization process.

Photonic crystal surface-emitting lasers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chua, Song Liang; Lu, Ling; Soljacic, Marin

2015-06-23

A photonic-crystal surface-emitting laser (PCSEL) includes a gain medium electromagnetically coupled to a photonic crystal whose energy band structure exhibits a Dirac cone of linear dispersion at the center of the photonic crystal's Brillouin zone. This Dirac cone's vertex is called a Dirac point; because it is at the Brillouin zone center, it is called an accidental Dirac point. Tuning the photonic crystal's band structure (e.g., by changing the photonic crystal's dimensions or refractive index) to exhibit an accidental Dirac point increases the photonic crystal's mode spacing by orders of magnitudes and reduces or eliminates the photonic crystal's distributed in-planemore » feedback. Thus, the photonic crystal can act as a resonator that supports single-mode output from the PCSEL over a larger area than is possible with conventional PCSELs, which have quadratic band edge dispersion. Because output power generally scales with output area, this increase in output area results in higher possible output powers.« less

Geochronology of Zircon in Eclogite Reveals Imbrication of the Ultrahigh-Pressure Western Gneiss Region of Norway.

NASA Astrophysics Data System (ADS)

Young, D. J.; Kylander-Clark, A. R.; Root, D. B.

2014-12-01

Eclogite provides the only record of kinematic events at the deepest levels of orogens. Integrating the U-Pb geochronology and trace element chemistry of zircon in eclogite reveals the most complete view of the PTt history, yet low concentrations of uranium and zirconium and drier compositions that hinder zircon growth at peak conditions render it a challenging rocktype for this approach. The iconic Western Gneiss Region (WGR) in Norway is one of the largest terranes of deeply subducted continental rocks in the world, and contains many indicators of ultrahigh-pressure metamorphic conditions (P>2.8 GPa) that developed during the Siluro-Devonian Caledonian Orogeny. A metamorphic transition from amphibolite-facies to ultrahigh-pressure eclogite facies broadly coincides with a km-scale shear zone that underlies the majority of the WGR. A critical unknown is the timing of movement on this feature, which emplaced allochthonous units above the Baltica basement, but might also have accommodated late-orogenic exhumation of the WGR from mantle depths. We carried out laser ablation split-stream ICPMS (LASS) and selected multigrain TIMS analyses of zircons from eleven eclogites across the southern WGR, of which eight are located within or above the shear zone. LASS spots on polished grains mostly yield weakly discordant Proterozoic intrusive ages, and often minimal indication of a Caledonian (U)HP metamorphic overprint. Direct ablation into unpolished zircon reveals thin rims of Caledonian age in some cases. Overall, the dataset shows that all samples began zircon growth at approximately the same time (ca. 430-420 Ma). Eclogite from lower levels of the shear zone does not contain any dates younger than ca. 410 Ma, however, while eclogite from higher levels continued growth until ca. 400 Ma. We interpret this to result from thrusting of the WGR above cooler basement after 410 Ma, terminating new zircon crystallization within the shear zone but allowing limited further growth in rocks above.

Protein crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1988-01-01

Protein crystal growth is a major experimental problem and is the bottleneck in widespread applications of protein crystallography. Research efforts now being pursued and sponsored by NASA are making fundamental contributions to the understanding of the science of protein crystal growth. Microgravity environments offer the possibility of performing new types of experiments that may produce a better understanding of protein crystal growth processes and may permit growth environments that are more favorable for obtaining high quality protein crystals. A series of protein crystal growth experiments using the space shuttle was initiated. The first phase of these experiments was focused on the development of micro-methods for protein crystal growth by vapor diffusion techniques, using a space version of the hanging drop method. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth.

Real time thermal imaging for analysis and control of crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Wargo, M. J.; Witt, A. F.

1992-01-01

A real time thermal imaging system with temperature resolution better than +/- 0.5 C and spatial resolution of better than 0.5 mm has been developed. It has been applied to the analysis of melt surface thermal field distributions in both Czochralski and liquid encapsulated Czochralski growth configurations. The sensor can provide single/multiple point thermal information; a multi-pixel averaging algorithm has been developed which permits localized, low noise sensing and display of optical intensity variations at any location in the hot zone as a function of time. Temperature distributions are measured by extraction of data along a user selectable linear pixel array and are simultaneously displayed, as a graphic overlay, on the thermal image.

Kinetic Roughening Transition and Energetics of Tetragonal Lysozyme Crystal Growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2004-01-01

Interpretation of lysozyme crystal growth rates using well-established physical theories enabled the discovery of a phenomenon possibly indicative of kinetic roughening. For example, lysozyme crystals grown above a critical supersaturation sigma, (where supersaturation sigma = ln c/c(sub eq), c = the protein concentration and c(sub eq) = the solubility concentration) exhibit microscopically rough surfaces due to the continuous addition of growth units anywhere on the surface of a crystal. The rate of crystal growth, V(sub c), for the continuous growth process is determined by the continuous flux of macromolecules onto a unit area of the crystal surface, a, from a distance, xi, per unit time due to diffusion, and a probability of attachment onto the crystal surface, expressed. Based upon models applied, the energetics of lysozyme crystal growth was determined. The magnitudes of the energy barriers of crystal growth for both the (110) and (101) faces of tetragonal lysozyme crystals are compared. Finally, evidence supportive of the kinetic roughening hypothesis is presented.

Growth and characterization of binary and pseudo-binary 3-5 compounds exhibiting non-linear optical behavior. Undergraduate research opportunities in microgravity science and technology

NASA Technical Reports Server (NTRS)

Witt, August F.

1992-01-01

In line with the specified objectives, a Bridgman-type growth configuration in which unavoidable end effects - conventionally leading to growth interface relocation - are compensated by commensurate input-power changes is developed; the growth rate on a microscale is predictable and unaffected by changes in heat transfer conditions. To permit quantitative characterization of the growth furnace cavity (hot-zone), a 3-D thermal field mapping technique, based on the thermal image, is being tested for temperatures up to 1100 C. Computational NIR absorption analysis was modified to now permit characterization of semi-insulating single crystals. Work on growth and characterization of bismuth-silicate was initiated. Growth of BSO (B12SiO20) for seed material by the Czochralski technique is currently in progress. Undergraduate research currently in progress includes: ground based measurements of the wetting behavior (contact angles) of semiconductor melts on substrates consisting of potential confinement materials for solidification experiments in a reduced gravity environment. Hardware modifications required for execution of the wetting experiments in a KC-135 facility are developed.

Crystal growth in fused solvent systems

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Noone, M. J.; Spear, K. E.; White, W. B.; Henry, E. C.

1973-01-01

Research is reported on the growth of electronic ceramic single crystals from solution for the future growth of crystals in a microgravity environment. Work included growth from fused or glass solvents and aqueous solutions. Topics discussed include: crystal identification and selection; aqueous solution growth of triglycine sulphate (TGS); and characterization of TGS.

Inclusion free cadmium zinc tellurium and cadmium tellurium crystals and associated growth method

DOEpatents

Bolotnikov, Aleskey E [South Setauket, NY; James, Ralph B [Ridge, NY

2010-07-20

The present disclosure provides systems and methods for crystal growth of cadmium zinc tellurium (CZT) and cadmium tellurium (CdTe) crystals with an inverted growth reactor chamber. The inverted growth reactor chamber enables growth of single, large, high purity CZT and CdTe crystals that can be used, for example, in X-ray and gamma detection, substrates for infrared detectors, or the like. The inverted growth reactor chamber enables reductions in the presence of Te inclusions, which are recognized as an important limiting factor in using CZT or CdTe as radiation detectors. The inverted growth reactor chamber can be utilized with existing crystal growth techniques such as the Bridgman crystal growth mechanism and the like. In an exemplary embodiment, the inverted growth reactor chamber is a U-shaped ampoule.

Isothermal Analysis of the Crystallization Kinetics in Lithium Disilicate Glass using Trans Temp Furnace

NASA Technical Reports Server (NTRS)

Fuss, T.; Ray, C. S.; Day, D. E.

2006-01-01

Crystallization kinetics for lithium disilicate, Li2O2SiO2, (LS2) glass has been studied extensively by nonisothermal methods, but only a few studies on the isothermal crystallization kinetics of LS2 are available. In the present research, isothermal crystallization experiments or the LS2 glass were conducted in a Trans Temp furnace between 600 and 635 C, and selected properties such as the activation energy for crystallization (E), crystal growth index or Avrami parameter (n), the concentration of quenched-in nuclei in the starting glass (Ni) and the crystal nucleation rate (I) were measured. The crystal nucleation rate (I) was measured at only one selected temperature of 452 C, at this time. This commercial furnace has a 13 cm long isothermal heating zone (+/- 1 C) that allows precise heat treatment of relatively large samples. By placing a thermocouple within approx. 2 mm of the sample, it was possible to detect the heat of crystallization in the form of an isothermal crystallization exotherm during isothermal heat treatment of the sample. The values of E (318 plus or minus 10 kJ/mol), n (3.6 plus or minus 0.l), and N(sub i) (1.6 x 10(exp l2) m(sup -3)) calculated by analyzing these isotherms using the standard Johnson-Mehl-Avrami (JMA) equation were reproducible and in agreement with the literature values. The value of I, 1.9 x 10(exp 10) m(sup -3) s(sup -1) at 452 C, is an order of magnitude higher than the reported value for LS2.

A contribution with review to the description of mineralization of bone and other calcified tissues in vivo

NASA Technical Reports Server (NTRS)

Christoffersen, J.; Landis, W. J.

1991-01-01

This manuscript considers certain aspects of mineral deposition in bone and other vertebrate calcifying tissues in order to examine physical, chemical, and biological factors important in the mineralization process. The paper in a discussion format principally presents a new data and the formulation of concepts based on such data as well as a summary of background material as necessary review. Mineralization is found to occur at spatially independent sites throughout the organic extracellular tissue matrices. Matrix vesicles and collagen fibrils each may serve as independent nucleation centers for mineral with vesicle mineralization being local and collagen mineralization dominating the tissues as a whole. Collagen fibril organization is suggested to be such that hole zones are aligned in three dimensions, creating extensive channels for mineral accommodation. Nucleation occurs initially in hole zones and crystal growth leads to the development of plate-like mineral particles whose orientation, disposition, and sizes within fibrils are detailed. Effects of diffusion, crystallinity, and critical nucleation and growth events are described with respect to their influence on mineral deposition in bulk and local regions of tissue matrices.

Crystal residence times from trace element zoning in plagioclase reveal changes in magma transfer dynamics at Mt. Etna during the last 400 years

NASA Astrophysics Data System (ADS)

Viccaro, Marco; Barca, Donatella; Bohrson, Wendy A.; D'Oriano, Claudia; Giuffrida, Marisa; Nicotra, Eugenio; Pitcher, Bradley W.

2016-04-01

Trace element zoning in plagioclase of selected alkaline lavas from the historic (1607-1892 AD) and recent (1983-2013 AD) activity of Mt. Etna volcano has been used to explore the possible role that volcano-tectonics exert on magma transfer dynamics. The observed textural characteristics of crystals include near-equilibrium textures (i.e., oscillatory zoning) and textures with variable extent of disequilibrium (patchy zoning, coarse sieve textures and dissolved cores). Historic crystals exhibit lower K concentrations at lower anorthite contents, a feature in agreement with the general more potassic character of the recent lavas if compared to the historic products. Historic plagioclases have statistically higher Ba and lower Sr concentrations than the recent crystals, which result in different Sr/Ba ratios for the two suites of plagioclase. Variations in the anorthite content along core-to-rim profiles obtained on crystals with different types of textures for both the historic and recent eruptive periods were evaluated particularly versus Sr/Ba. At comparable average An contents, crystals characterized by oscillatory zoning, which are representative of near-equilibrium crystallization from the magma, display distinct Sr/Ba ratios. We suggest that these features are primarily related to recharge of a new, geochemically-distinct magma into the storage and transport system of the volcano. In addition to distinct trace element and textural characteristics of plagioclase, Sr diffusion modeling for plagioclase suggests that residence times are generally shorter for crystals found in recently erupted lavas (25-77 years, average 43 years) compared to those of the historic products (43-163 years, average 99 years). Shorter residences times correlate with gradual increases in eruption volume and eruption frequency rates through time. We attribute these features to an increasing influence, since the 17th century, of extensional tectonic structures within the upper 10 km of the Etnean crust, which have promoted shorter residence times and higher eruption frequency.

Measurable characteristics of lysozyme crystal growth

NASA Technical Reports Server (NTRS)

Gorti, Sridhar; Forsythe, Elizabeth L.; Pusey, Marc L.

2005-01-01

The behavior of protein crystal growth is estimated from measurements performed at both the microscopic and molecular levels. In the absence of solutal flow, it was determined that a model that balances the macromolecular flux toward the crystal surface with the flux of the crystal surface well characterizes crystal growth observed using microscopic methods. Namely, it was determined that the model provides accurate estimates for the crystal-growth velocities upon evaluation of crystal-growth measurements obtained in time. Growth velocities thus determined as a function of solution supersaturation were further interpreted using established deterministic models. From analyses of crystal-growth velocities, it was found that the mode of crystal growth varies with respect to increasing solution supersaturation, possibly owing to kinetic roughening. To verify further the hypothesis of kinetic roughening, crystal growth at the molecular level was examined using atomic force microscopy (AFM). From the AFM measurements, it was found that the magnitude of surface-height fluctuations, h(x), increases with increasing solution supersaturation. In contrast, the estimated characteristic length, xi, decreases rapidly upon increasing solution supersaturation. It was conjectured that the magnitude of both h(x) and xi could possibly determine the mode of crystal growth. Although the data precede any exact theory, the non-critical divergence of h(x) and xi with respect to increasing solution supersaturation was nevertheless preliminarily established. Moreover, approximate models to account for behavior of both h(x) and xi are also presented.

Crystal Growth Rate Dispersion: A Predictor of Crystal Quality in Microgravity?

NASA Technical Reports Server (NTRS)

Kephart, Richard D.; Judge, Russell A.; Snell, Edward H.; vanderWoerd, Mark J.

2003-01-01

In theory macromolecular crystals grow through a process involving at least two transport phenomena of solute to the crystal surface: diffusion and convection. In absence of standard gravitational forces, the ratio of these two phenomena can change and explain why crystal growth in microgravity is different from that on Earth. Experimental evidence clearly shows, however, that crystal growth of various systems is not equally sensitive to reduction in gravitational forces, leading to quality improvement in microgravity for some crystals but not for others. We hypothesize that the differences in final crystal quality are related to crystal growth rate dispersion. If growth rate dispersion exists on Earth, decreases in microgravity, and coincides with crystal quality improvements then this dispersion is a predictor for crystal quality improvement. In order to test this hypothesis, we will measure growth rate dispersion both in microgravity and on Earth and will correlate the data with previously established data on crystal quality differences for the two environments. We present here the first crystal growth rate measurement data for three proteins (lysozyme, xylose isomerase and human recombinant insulin), collected on Earth, using hardware identical to the hardware to be used in microgravity and show how these data correlate with crystal quality improvements established in microgravity.

On geological interpretations of crystal size distributions: Constant vs. proportionate growth

USGS Publications Warehouse

Eberl, D.D.; Kile, D.E.; Drits, V.A.

2002-01-01

Geological interpretations of crystal size distributions (CSDs) depend on understanding the crystal growth laws that generated the distributions. Most descriptions of crystal growth, including a population-balance modeling equation that is widely used in petrology, assume that crystal growth rates at any particular time are identical for all crystals, and, therefore, independent of crystal size. This type of growth under constant conditions can be modeled by adding a constant length to the diameter of each crystal for each time step. This growth equation is unlikely to be correct for most mineral systems because it neither generates nor maintains the shapes of lognormal CSDs, which are among the most common types of CSDs observed in rocks. In an alternative approach, size-dependent (proportionate) growth is modeled approximately by multiplying the size of each crystal by a factor, an operation that maintains CSD shape and variance, and which is in accord with calcite growth experiments. The latter growth law can be obtained during supply controlled growth using a modified version of the Law of Proportionate Effect (LPE), an equation that simulates the reaction path followed by a CSD shape as mean size increases.

Connection between the growth rate distribution and the size dependent crystal growth

NASA Astrophysics Data System (ADS)

Mitrović, M. M.; Žekić, A. A.; IIić, Z. Z.

2002-07-01

The results of investigations of the connection between the growth rate dispersions and the size dependent crystal growth of potassium dihydrogen phosphate (KDP), Rochelle salt (RS) and sodium chlorate (SC) are presented. A possible way out of the existing confusion in the size dependent crystal growth investigations is suggested. It is shown that the size independent growth exists if the crystals belonging to one growth rate distribution maximum are considered separately. The investigations suggest possible reason for the observed distribution maxima widths, and the high data scattering on the growth rate versus the crystal size dependence.

A STUDY OF DISLOCATION STRUCTURE OF SUBBOUNDARIES IN MOLYBDENUM SINGLE CRYSTALS,

DTIC Science & Technology

MOLYBDENUM, *DISLOCATIONS), GRAIN STRUCTURES(METALLURGY), SINGLE CRYSTALS, ZONE MELTING, ELECTRON BEAM MELTING, GRAIN BOUNDARIES, MATHEMATICAL ANALYSIS, ETCHED CRYSTALS, ETCHING, ELECTROEROSIVE MACHINING, CHINA

Effect of Low-Concentration Polymers on Crystal Growth in Molecular Glasses: A Controlling Role for Polymer Segmental Mobility Relative to Host Dynamics.

PubMed

Huang, Chengbin; Powell, C Travis; Sun, Ye; Cai, Ting; Yu, Lian

2017-03-02

Low-concentration polymers can strongly influence crystal growth in small-molecule glasses, a phenomenon important for improving physical stability against crystallization. We measured the velocity of crystal growth in two molecular glasses, nifedipine (NIF) and o-terphenyl (OTP), each doped with four or five different polymers. For each polymer, the concentration was fixed at 1 wt % and a wide range of molecular weights was tested. We find that a polymer additive can strongly alter the rate of crystal growth, from a 10-fold reduction to a 10-fold increase. For a given polymer, increasing molecular weight slows down crystal growth and the effect saturates around DP = 100, where DP is the degree of polymerization. For all the systems studied, the polymer effect on crystal growth rate forms a master curve in the variable (T g,polymer - T g,host )/T cryst , where T g is the glass transition temperature and T cryst is the crystallization temperature. These results support the view that a polymer's effect on crystal growth is controlled by its segmental mobility relative to the host-molecule dynamics. In the proposed model, crystal growth rejects impurities and creates local polymer-rich regions, which must be traversed by host molecules to sustain crystal growth at rates determined by polymer segmental mobility. Our results do not support the view that host-polymer hydrogen bonding plays a controlling role in crystal growth inhibition.

Convection effects on radial segregation and crystal melt interface in vertical Bridgman growth

NASA Technical Reports Server (NTRS)

Tanveer, S.

1993-01-01

We analytically study the influence of convection caused by horizontal heat transfer through the sides of a vertical Bridgman apparatus. We consider the case when the heat transfer across the side walls is small so that the resulting interfacial deformation and fluid velocities are also small. This allows us to linearize the Navier-Stokes equations and express the interfacial conditions about a planar interface through a Taylor expansion. Using a no tangential stress conditions on the side walls, asymptotic expressions for both the interfacial slope, and radial segregation at the crystal-melt interface are obtained in closed form in the limit of large thermal Rayleigh number. It is suggested that these can be reduced by appropriately controlling a specific heat transfer property at the edge of the insulation zone in the solid side.

Record of Fluctuating Magmatic Environments, Melt Fractionation, and Mixing of Crystals: Elemental Compositions of Zircon Zones, Spirit Mountain Batholith, Nevada

NASA Astrophysics Data System (ADS)

Miller, C. F.; Claiborne, L. L.; Wooden, J. L.; Mazdab, F. K.; Walker, B. A.

2006-12-01

Spirit Mountain batholith is a large, tilted, subvolcanic intrusion in southernmost Nevada (Walker et al., in press; Lowery Claiborne et al., in press). Field relations and elemental chemistry of rocks ranging from felsic cumulates to leucogranites demonstrate both fractionation and frequent recharging. SHRIMP U-Pb analysis of zircon reveals a 2 m.y. history (17.4-15.3 Ma) for the batholith; almost all of the samples record multiple age populations. Elemental concentrations and zoning patterns document the utility of zircon in tracking magmatic environments and crystal transfer processes and provide important insights into the complex and protracted history of the batholith. The data lend strong support to the Watson et al. (2006) Ti-in-zircon thermometer. At reasonable a(TiO2) between 0.5 and 0.9, all calculated T's are consistent with petrological constraints and granite phase equilibria; using a(TiO2) = 0.7, T ranges from 675-900 C. Over this apparent T interval, which reflects a range in Ti from 3.2-34 ppm, concentrations of Hf (6000-18000 ppm), U (20-5000 ppm), and Th (50-13,000 ppm), and REE patterns all vary dramatically and systematically. Hf, U, Th, and Ce/Ce* are negatively correlated with T; LREE/MREE, MREE/HREE, and Eu/Eu* are positively correlated with T. These variations indicate that zircon preferentially incorporated Zr over Hf (hence falling Zr/Hf); U and Th behaved as strongly incompatible elements in the crystallizing assemblage as a whole; compatibility of REE increased with decreasing atomic number (effect of LREE accessories?); Eu+2 was more compatible (feldspars) and Ce+4 less compatible than equivalent +3 REE. All of these trends are consistent with the observed crystallizing assemblage and with general trends in whole rocks. More striking, however, is intrasample and intragrain variability. Although leucogranite samples have a larger proportion of zircon with compositions indicating low T and growth from fractionated melt, all samples have a very wide, and overlapping, range of zircon compositions. Many grains are very strongly zoned, and some individual grains show almost the full range of calculated T and elemental composition. Rims of zircons from the leucogranites are typically "cold" and evolved, but many have high-T interiors that contrast with host rock. Core-to-rim zoning is commonly not monotonic but rather strongly fluctuating, indicating that during growth zircon experienced episodes of increased T and immersion in less evolved melts. These patterns of compositional variability reveal that zircons survived heating events; were entrained in ascending fractionated melt; and were exchanged among contrasting magma batches. Such a history is consistent with protracted residence in a large, multiply replenished and rejuvenated mushy magma system in which melt fraction fluctuated in space and time.

Protein crystal growth in low gravity

NASA Technical Reports Server (NTRS)

Feigelson, Robert S.

1990-01-01

The effect of low gravity on the growth of protein crystals and those parameters which will affect growth and crystal quality was studied. The proper design of the flight hardware and experimental protocols are highly dependent on understanding the factors which influence the nucleation and growth of crystals of biological macromolecules. Thus, those factors are investigated and the body of knowledge which has been built up for small molecule crystallization. These data also provide a basis of comparison for the results obtained from low-g experiments. The flows around growing crystals are detailed. The preliminary study of the growth of isocitrate lyase, the crystal morphologies found and the preliminary x ray results are discussed. The design of two apparatus for protein crystal growth by temperature control are presented along with preliminary results.

Systematic Improvement of Protein Crystals by Determining the Supersolubility Curves of Phase Diagrams

PubMed Central

Saridakis, Emmanuel; Chayen, Naomi E.

2003-01-01

A systematic approach for improving protein crystals by growing them in the metastable zone using the vapor diffusion technique is described. This is a simple technique for optimization of crystallization conditions. Screening around known conditions is performed to establish a working phase diagram for the crystallization of the protein. Dilutions of the crystallization drops across the supersolubility curve into the metastable zone are then carried out as follows: the coverslips holding the hanging drops are transferred, after being incubated for some time at conditions normally giving many small crystals, over reservoirs at concentrations which normally yield clear drops. Fewer, much larger crystals are obtained when the incubation times are optimized, compared with conventional crystallization at similar conditions. This systematic approach has led to the structure determination of the light-harvesting protein C-phycocyanin to the highest-ever resolution of 1.45 Å. PMID:12547801

Northwest Africa 5790: Revisiting nakhlite petrogenesis

NASA Astrophysics Data System (ADS)

Jambon, A.; Sautter, V.; Barrat, J.-A.; Gattacceca, J.; Rochette, P.; Boudouma, O.; Badia, D.; Devouard, B.

2016-10-01

Northwest Africa 5790, the latest nakhlite find, is composed of 58 vol.% augite, 6% olivine and 36% vitrophyric intercumulus material. Its petrology is comparable to previously discovered nakhlites but with key differences: (1) Augite cores display an unusual zoning between Mg# 54 and 60; (2) Olivine macrocrysts have a primary Fe-rich core composition (Mg# = 35); (3) The modal proportion of mesostasis is the highest ever described in a nakhlite; (4) It is the most magnetite-rich nakhlite, together with MIL 03346, and exhibits the least anisotropic fabric. Complex primary zoning in cumulus augite indicates resorption due to complex processes such as remobilization of former cumulates in a new magma batch. Textural relationships indicate unambiguously that olivine was growing around resorbed augite, and that olivine growth was continuous while pyroxene growth resumed at a final stage. Olivine core compositions (Mg# = 35) are out of equilibrium with the augite core compositions (Mg# 60-63) and with the previously inferred nakhlite parental magma (Mg# = 29). The presence of oscillatory zoning in olivine and augite precludes subsolidus diffusion that could have modified olivine compositions. NWA 5790 evidences at least two magma batches before eruption, with the implication that melt in equilibrium with augite cores was never in contact with olivine. Iddingsite is absent. Accordingly, the previous scenarios for nakhlite petrogenesis must be revised. The first primary parent magmas of nakhlites generated varied augite cumulates at depth (Mg# 66-60) as they differentiated to different extents. A subsequent more evolved magma batch entrained accumulated augite crystals to the surface where they were partly resorbed while olivine crystallized. Trace element variations indicate unambiguously that they represent consanguineous but different magma batches. The compositional differences among the various nakhlites suggest a number of successive lava flows. To account for all observations we propose a petrogenetic model for nakhlites based on several (at least three) thick flows. Although NWA 5790 belongs to the very top of one flow, it should come from the lowest flow sampled, based on the lack of iddingsite.

Visualizing the Impurity Depletion Zone Around Holoferritin Crystals Growing in Gel with Ferritin Dimers

NASA Technical Reports Server (NTRS)

Chernov, A. A.; Garcia-Ruiz, J. M.; Thomas, B. R.

2000-01-01

Colorless transparent apoferritin (Mr = 450KDa) crystals have been grown from gel with Cd(2+) as precipitant in the presence of reddish brown-colored ferritin dimers (Mr = 900KDa). In agreement with our previous measurements, showing preferential trapping of dimers (distribution coefficient K = 4), the apoferritin crystals become strongly colored while the gel solution around them became nearly colorless. The depth of the depletion with respect to the colored dimer impurity allowed us to visualize the impurity depletion zone. Depletion with respect to impurity as compared to the crystallizing protein is discussed.

Origin of Aphyric Phonolitic Magmas: Natural Evidences and Experimental Constraints

NASA Astrophysics Data System (ADS)

Masotta, M.; Freda, C.; Gaeta, M.

2010-12-01

Large explosive phonolitic eruptions are commonly characterised by aphyric juvenile eruptive products. Taking into account the low density contrast among phonolitic composition and settling phases (i.e., feldspar and leucite), the almost complete lack of crystals in these differentiated compositions rises the question of which process could produce such an efficient crystal-melt separation. Seeking for an answer, we have investigated crystallization in presence of a thermal gradient as a possible mechanism for crystal-melt separation, considering both chemical and physical effects acting on a variably crystallized system. Using a natural tephri-phonolitic composition as starting material (M.te Aguzzo scoria cone, Sabatini Volcanic District, Central Italy), we have reproduced thermal gradient-driven crystallization in order to simulate the crystallization process in a thermally zoned magma chamber. Crystallization degree (paragenesis made of clinopyroxene±feldspars±leucite) as well as melt composition varies along the thermal gradient. In particular, melt composition ranges from the tephri-phonolitic starting composition at the bottom of the charge (hottest and aphyric zone) to phonolitic at the top (cooler and heterogeneously-crystallised zone). Backscattered images of experimental products clearly evidence: i) the aphyric tephri-phonolitic melt region at the bottom of the charge; ii) a drop-shaped crystal clustering in the middle zone; and iii) large aphyric belt and pockets (up to 100 µm wide) of phonolitic melt, with large deformed-shaped sanidine occurring at their margin, at the charge top region. The latter two features, resulting from solid-melt displacements, suggest that the segregation of phonolitic melt can be related to crystal sinking and compaction. On the other hand, the compositional variability of the melt along the thermal gradient is directly related to the crystallization degree, indicating that chemical diffusion and thermal migration have negligible effect at the experimental scale. Experimental results suggest that, in presence of a thermal gradient, a filter-press differentiation mechanism (i.e. sinking+compaction) is able to produce heterogeneous magma differentiation characterised by a wide range of melt compositions (in our case from tephri-phonolitic to phonolitic). Although the limitation due to the vertical shape of the charge and consequent shear effects occurring at the lateral walls (thus limiting the mobility of the crystal clusters), experimental duration of 24 h is enough to allow crystal-melt separation by means of settling and compaction, indicating that timescale for such a process is extremely rapid and effective at experimental conditions. Actually, experimental textures and phase relations are in good agreement with those observed in natural lithic enclaves (from Sabatini Volcanic District) representative of the crystallizing boundary layer of a phonolitic magma chamber. Thus, we speculate that gravitative collapses of a mushy zone from the magma chamber roof of a thermally zoned magma chamber may produce top accumulation of highly differentiated and aphyric melts.

Face-selective crystal growth behavior of L-aspartic acid in the presence of L-asparagine

NASA Astrophysics Data System (ADS)

Sato, Hiroyasu; Doki, Norihito; Yoshida, Saki; Yokota, Masaaki; Shimizu, Kenji

2016-02-01

The kinetic mechanism of L-asparagine (L-Asn) action on L-aspartic acid (L-Asp) crystal growth, namely the face-selective effect of L-Asn on the L-Asp crystal growth rate in each direction, was examined. In the a-axis direction, the effect of L-Asn on the L-Asp crystal growth rate was small. Enhancement and inhibition of L-Asp crystal growth, and interestingly the dissolution of the L-Asp crystal face, were observed in the b-axis direction, depending on the amount of L-Asn added. In the c-axis direction, the L-Asp crystal growth rate decreased with the increase in the amount of L-Asn added, and the experimental results were well fitted with a Langmuir adsorption isotherm. The study showed that there were crystal growth conditions where enhancement and inhibition, as well as inhibition and dissolution, coexisted in the presence of an additive with a structure similar to the growing crystal.

Delta L: An Apparatus for Measuring Macromolecular Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

In order to determine how macromolecule crystal quality improvement in microgravity is related to crystal growth characteristics, is was necessary to develop new hardware that could measure the crystal growth rates of a population of crystals growing under the same solution conditions. As crystal growth rate is defined as the change or delta in a defined dimension or length (L) of a crystal over time, the hardware was named Delta L. Delta L consists of fluids, optics, and data acquisition, sub-assemblies. Temperature control is provided for the crystal growth chamber. Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS). Delta L prototype hardware has been assembled. This paper will describe an overview of the design of Delta L and present preliminary crystal growth rate data.

Detonation waves in pentaerythritol tetranitrate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tarver, C.M.; Breithaupt, R.D.; Kury, J.W.

1997-06-01

Fabry{endash}Perot laser interferometry was used to obtain nanosecond time resolved particle velocity histories of the free surfaces of tantalum discs accelerated by detonating pentaerythritol tetranitrate (PETN) charges and of the interfaces between PETN detonation products and lithium fluoride crystals. The experimental records were compared to particle velocity histories calculated using very finely zoned meshes of the exact dimensions with the DYNA2D hydrodynamic code. The duration of the PETN detonation reaction zone was demonstrated to be less than the 5 ns initial resolution of the Fabry{endash}Perot technique, because the experimental records were accurately calculated using an instantaneous chemical reaction, the Chapman{endash}Jouguetmore » (C-J) model of detonation, and the reaction product Jones{endash}Wilkins{endash}Lee (JWL) equation of state for PETN detonation products previously determined by supracompression (overdriven detonation) studies. Some of the PETN charges were pressed to densities approaching the crystal density and exhibited the phenomenon of superdetonation. An ignition and growth Zeldovich{endash}von Neumann{endash}Doring (ZND) reactive flow model was developed to explain these experimental records and the results of previous PETN shock initiation experiments on single crystals of PETN. Good agreement was obtained for the induction time delays preceding chemical reaction, the run distances at which the initial shock waves were overtaken by the detonation waves in the compressed PETN, and the measured particle velocity histories produced by the overdriven detonation waves before they could relax to steady state C-J velocity and pressure. {copyright} {ital 1997 American Institute of Physics.}« less

Fitful and protracted magma assembly leading to a giant eruption, Youngest Toba Tuff, Indonesia

USGS Publications Warehouse

Reid, Mary R; Vazquez, Jorge A.

2017-01-01

The paroxysmal eruption of the 74 ka Youngest Toba Tuff (YTT) of northern Sumatra produced an extraordinary 2800 km3 of non-welded to densely welded ignimbrite and co-ignimbrite ash-fall. We report insights into the duration of YTT magma assembly obtained from ion microprobe U-Th and U-Pb dates, including continuous age spectra over >50% of final zircon growth, for pumices and a welded tuff spanning the compositional range of the YTT. A relatively large subpopulation of zircon crystals nucleated before the penultimate caldera-related eruption at 501 ka, but most zircons yielded interior dates 100-300 ka thereafter. Zircon nucleation and growth was likely episodic and from diverse conditions over protracted time intervals of >100 to >500 ka. Final zircon growth is evident as thin rim plateaus that are in Th/U chemical equilibrium with hosts, and that give crystallization ages within tens of ka of eruption. The longevity and chemical characteristics of the YTT zircons, as well as evidence for intermittent zircon isolation and remobilization associated with magma recharge, is especially favored at the cool and wet eutectoid conditions that characterize at least half of the YTT, wherein heat fluxes could dissolve major phases but have only a minor effect on larger zircon crystals. Repeated magma recharge may have contributed to the development of compositional zoning in the YTT but, considered together with limited allanite, quartz, and other mineral dating and geospeedometry, regular perturbations to the magma reservoir over >400 ka did not lead to eruption until 74 ka ago.

System and method for crystalline sheet growth using a cold block and gas jet

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kellerman, Peter L.; Mackintosh, Brian; Carlson, Frederick M.

A crystallizer for growing a crystalline sheet from a melt may include a cold block having a cold block surface that faces an exposed surface of the melt, the cold block configured to generate a cold block temperature at the cold block surface that is lower than a melt temperature of the melt at the exposed surface. The system may also include a nozzle disposed within the cold block and configured to deliver a gas jet to the exposed surface, wherein the gas jet and the cold block are interoperative to generate a process zone that removes heat from themore » exposed surface at a first heat removal rate that is greater than a second heat removal rate from the exposed surface in outer regions outside of the process zone.« less

1. Innovative Relaxor-Based PiezoCrystals: Phase Diagrams, Crystal Growth, Domain Structures and Electric Properties. 2. Piezo- and Ferroelectric Materials Based on Morphotropic Phase Boundary Synthesis, Characterization and Structure - Property Relations

DTIC Science & Technology

2006-03-31

crystals by the flux method and modified Bridgman technique, the growth results were hardly reproducible, and the quality of the crystals was still a serious... growth . 2.2.1.2.2) Solution Bridgman Growth A modified Bridgman method using excess of PbO as solvent was developed for the growth of PZNT91/9 crystals ...of growth , the grown crystal can be rotated via the A120 3 rod which was driven by a motor at a speed of 0 to 30 rmp. Figure 15(b) gives the

Crystal Growth Furnace - An overview of the system configuration and planned experiments on the First United States Microgravity Laboratory mission

NASA Technical Reports Server (NTRS)

Srinivas, R.; Schaefer, D. A.

1992-01-01

The Crystal Growth Furnace (CGF) system configuration for the First United States Microgravity Laboratory (USML-1) mission is reviewed, and the planned on-orbit experiments are briefly described. The CGF is configured to accommodate four scientific experiments involving crystal growth which are based on the classical Bridgman method and CVT method, including vapor transport crystal growth of mercury cadmium telluride; crystal growth of mercury zinc telluride by directional solidification; seeded Bridgman growth of zinc-doped cadmium telluride; and Bridgman growth of selenium-doped gallium arsenide.

Optical Diagnostics of Solution Crystal Growth

NASA Technical Reports Server (NTRS)

Kim, Yongkee; Reddy, B. R.; George, T. G.; Lal, R. B.

1996-01-01

Non-contact optical techniques such as, optical heterodyne, ellipsometry and interferometry, for real time in-situ monitoring of solution crystal growth are demonstrated. Optical heterodyne technique has the capability of measuring the growth rate as small as 1A/sec. In a typical Michelson interferometer set up, the crystal is illuminated by a Zeeman laser with frequency omega(sub 1) and the reference beam with frequency omega(sub 2). As the crystal grows, the phase of the rf signal changes with respect to the reference beam and this phase change is related to the crystal growth rate. This technique is demonstrated with two examples: (1) by measuring the copper tip expansion/shrinkage rate and (2) by measuring the crystal growth rate of L-Arginine Phosphate (LAP). The first test shows that the expansion/shrinkage rate of copper tip was fast in the beginning, and gets slower as the expansion begins to stabilize with time. In crystal growth, the phase change due the crystal growth is measured using a phase meter and a strip chart recorder. Our experimental results indicate a varied growth rate from 69.4 to 92.6A per sec. The ellipsometer is used to study the crystal growth interface. From these measurements and a theoretical modeling of the interface, the various optical parameters can be deduced. Interferometry can also be used to measure the growth rate and concentration gradient in the vicinity of the crystal.

Hopper Growth of Salt Crystals.

PubMed

Desarnaud, Julie; Derluyn, Hannelore; Carmeliet, Jan; Bonn, Daniel; Shahidzadeh, Noushine

2018-06-07

The growth of hopper crystals is observed for many substances, but the mechanism of their formation remains ill understood. Here we investigate their growth by performing evaporation experiments on small volumes of salt solutions. We show that sodium chloride crystals that grow very fast from a highly supersaturated solution form a peculiar form of hopper crystal consisting of a series of connected miniature versions of the original cubic crystal. The transition between cubic and such hopper growth happens at a well-defined supersaturation where the growth rate of the cubic crystal reaches a maximum (∼6.5 ± 1.8 μm/s). Above this threshold, the growth rate varies as the third power of supersaturation, showing that a new mechanism, controlled by the maximum speed of surface integration of new molecules, induces the hopper growth of cubic crystals in cascade.

A study of crystal growth by solution technique. [triglycine sulfate single crystals

NASA Technical Reports Server (NTRS)

Lal, R. B.

1979-01-01

The advantages and mechanisms of crystal growth from solution are discussed as well as the effects of impurity adsorption on the kinetics of crystal growth. Uncertainities regarding crystal growth in a low gravity environment are examined. Single crystals of triglycine sulfate were grown using a low temperature solution technique. Small components were assembled and fabricated for future space flights. A space processing experiment proposal accepted by NASA for the Spacelab-3 mission is included.

Effect of precipitation inhibitors on indomethacin supersaturation maintenance: mechanisms and modeling.

PubMed

Patel, Dhaval D; Anderson, Bradley D

2014-05-05

This study quantitatively explores the mechanisms underpinning the effects of model pharmaceutical polymeric precipitation inhibitors (PPIs) on the crystal growth and, in turn, maintenance of supersaturation of indomethacin, a model poorly water-soluble drug. A recently developed second-derivative UV spectroscopy method and a first-order empirical crystal growth model were used to determine indomethacin crystal growth rates in the presence of model PPIs. All three model PPIs including HP-β-CD, PVP, and HPMC inhibited indomethacin crystal growth at both high and low degrees of supersaturation (S). The bulk viscosity changes in the presence of model PPIs could not explain their crystal growth inhibitory effects. At 0.05% w/w, PVP (133-fold) and HPMC (28-fold) were better crystal growth inhibitors than HP-β-CD at high S. The inhibitory effect of HP-β-CD on the bulk diffusion-controlled indomethacin crystal growth at high S was successfully modeled using reactive diffusion layer theory, which assumes reversible complexation in the diffusion layer. Although HP-β-CD only modestly inhibited indomethacin crystal growth at either high S (∼15%) or low S (∼2-fold), the crystal growth inhibitory effects of PVP and HPMC were more dramatic, particularly at high S (0.05% w/w). The superior crystal growth inhibitory effects of PVP and HPMC as compared with HP-β-CD at high S were attributed to a change in the indomethacin crystal growth rate-limiting step from bulk diffusion to surface integration. Indomethacin crystal growth inhibitory effects of all three model PPIs at low S were attributed to retardation of the rate of surface integration of indomethacin, a phenomenon that may reflect the adsorption of PPIs onto the growing crystal surface. The quantitative approaches outlined in this study should be useful in future studies to develop tools to predict supersaturation maintenance effects of PPIs.

Segregation control in vertical Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Tao, Y.; Kou, S.

1996-11-01

To help the crystal grow at a constant dopant concentration in vertical Bridgman crystal growth, the dopant concentration of the growth melt, i.e. the melt from which the crystal grows, was kept constant. To achieve this, three different methods were used to replenish the growth melt at a controlled rate and suppress dopant diffusion between the growth melt and the replenishing melt. In method one, a replenishing crucible having a long melt passageway was immersed in the growth melt. In method two, a replenishing crucible having an independent feed-rate control mechanism was held above the growth melt. In method three, a submerged diffusion baffle was used to form a long melt passageway between the growth melt and the replenishing melt. NaNO 3 was used as a model material for crystal growth. Single crystals were grown by these three methods with effective segregation control. Method two was applied to InSb and single crystals were also grown with effective segregation control.

A numerical study of zone-melting process for the thermoelectric material of Bi2Te3

NASA Astrophysics Data System (ADS)

Chen, W. C.; Wu, Y. C.; Hwang, W. S.; Hsieh, H. L.; Huang, J. Y.; Huang, T. K.

2015-06-01

In this study, a numerical model has been established by employing a commercial software; ProCAST, to simulate the variation/distribution of temperature and the subsequent microstructure of Bi2Te3 fabricated by zone-melting technique. Then an experiment is conducted to measure the temperature variation/distribution during the zone-melting process to validate the numerical system. Also, the effects of processing parameters on crystallization microstructure such as moving speed and temperature of heater are numerically evaluated. In the experiment, the Bi2Te3 powder are filled into a 30mm diameter quartz cylinder and the heater is set to 800°C with a moving speed 12.5 mm/hr. A thermocouple is inserted in the Bi2Te3 powder to measure the temperature variation/distribution of the zone-melting process. The temperature variation/distribution measured by experiment is compared to the results of numerical simulation. The results show that our model and the experiment are well matched. Then the model is used to evaluate the crystal formation for Bi2Te3 with a 30mm diameter process. It's found that when the moving speed is slower than 17.5 mm/hr, columnar crystal is obtained. In the end, we use this model to predict the crystal formation of zone-melting process for Bi2Te3 with a 45 mm diameter. The results show that it is difficult to grow columnar crystal when the diameter comes to 45mm.

Bridgman growth of large-aperture yttrium calcium oxyborate crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Anhua, E-mail: wuanhua@mail.sic.ac.cn; Jiang, Linwen; Qian, Guoxing

2012-09-15

Highlights: ► YCOB is a novel non-linear optical crystal possessing good thermal, mechanical and nonlinear optical properties. ► Large size crystal growth is key technology question for YCOB crystal. ► YCOB crystals 3 in. in diameter were grown with modified vertical Bridgman method. ► It is a more effective growth method to obtain large size and high quality YCOB crystal. -- Abstract: Large-aperture yttrium calcium oxyborate YCa{sub 4}O(BO{sub 3}){sub 3} (YCOB) crystals with 3 in. in diameter were grown with modified vertical Bridgman method, and the large crystal plate (63 mm × 68 mm × 20 mm) was harvested formore » high-average power frequency conversion system. The crack, facet growth and spiral growth can be effectively controlled in the as-grown crystal, and Bridgman method displays more effective in obtain large size and high quality YCOB crystal plate than Czochralski technique.« less

The crustal magma storage system of Volcán Quizapu, Chile, and the effects of magma mixing on magma diversity

USGS Publications Warehouse

Bergantz, George W.; Cooper, Kari M.; Hildreth, Edward; Ruprecht, Phillipp

2012-01-01

Crystal zoning as well as temperature and pressure estimates from phenocryst phase equilibria are used to constrain the architecture of the intermediate-sized magmatic system (some tens of km3) of Volcán Quizapu, Chile, and to document the textural and compositional effects of magma mixing. In contrast to most arc magma systems, where multiple episodes of open-system behavior obscure the evidence of major magma chamber events (e.g. melt extraction, magma mixing), the Quizapu magma system shows limited petrographic complexity in two large historical eruptions (1846–1847 and 1932) that have contrasting eruptive styles. Quizapu magmas and peripheral mafic magmas exhibit a simple binary mixing relationship. At the mafic end, basaltic andesite to andesite recharge magmas complement the record from peripheral cones and show the same limited range of compositions. The silicic end-member composition is almost identical in both eruptions of Quizapu. The effusive 1846–1847 eruption records significant mixing between the mafic and silicic end-members, resulting in hybridized andesites and mingled dacites. These two compositionally simple eruptions at Volcán Quizapu present a rare opportunity to isolate particular aspects of magma evolution—formation of homogeneous dacite magma and late-stage magma mixing—from other magma chamber processes. Crystal zoning, trace element compositions, and crystal-size distributions provide evidence for spatial separation of the mafic and silicic magmas. Dacite-derived plagioclase phenocrysts (i.e. An25–40) show a narrow range in composition and limited zonation, suggesting growth from a compositionally restricted melt. Dacite-derived amphibole phenocrysts show similar restricted compositions and furthermore constrain, together with more mafic amphibole phenocrysts, the architecture of the magmatic system at Volcán Quizapu to be compositionally and thermally zoned, in which an andesitic mush is overlain by a homogeneous dacitic magma that is the source for most of the 1846–1847 and 1932 erupted magmas. Dacite formation is best explained by mineral–melt separation (crystal fractionation) from an andesitic mush, which is inferred to have thermally and compositionally buffered the dacite magma thereby keeping it at relatively low crystallinity (<30 vol. %). The dominant cause of compositional diversity is melt separation. Back-mixing of mush (i.e. crystals with signatures of growth both in the andesitic mush and in the dacite magma) into the overlying dacite magma is rarely observed. Recharge events that increase crystal and magma diversity in the dacite magma are limited to an episode of mafic recharge and mixing just prior to the 1846–1847 eruption, where evidence for magma mixing is present on all scales. Chamber-wide mixing was incomplete (mixing efficiency of ∼0·53–0·85) as flow lobes vary significantly in composition along the proposed mixing array. Estimates of viscosity variations during the course of magma mixing suggest that mixing dynamics and the degree of magma interaction on all scales were established at the beginning of the recharge event.

Crystal growth and annealing for minimized residual stress

DOEpatents

Gianoulakis, Steven E.

2002-01-01

A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF.sub.2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing.

Large-scale magmatic layering in the Main Zone of the Bushveld Complex and episodic downward magma infiltration

NASA Astrophysics Data System (ADS)

Hayes, Ben; Ashwal, Lewis D.; Webb, Susan J.; Bybee, Grant M.

2017-03-01

The Bellevue drillcore intersects 3 km of Main and Upper Zone cumulates in the Northern Limb of the Bushveld Complex. Main Zone cumulates are predominately gabbronorites, with localized layers of pyroxenite and anorthosite. Some previous workers, using bulk rock major, trace and isotopic compositions, have suggested that the Main Zone crystallized predominantly from a single pulse of magma. However, density measurements throughout the Bellevue drillcore reveal intervals that show up-section increases in bulk rock density, which are difficult to explain by crystallization from a single batch of magma. Wavelet analysis of the density data suggests that these intervals occur on length-scales of 40 to 170 m, thus defining a scale of layering not previously described in the Bushveld Complex. Upward increases in density in the Main Zone correspond to upward increases in modal pyroxene, producing intervals that grade from a basal anorthosite (with 5% pyroxene) to gabbronorite (with 30-40% pyroxene). We examined the textures and mineral compositions of a 40 m thick interval showing upwardly increasing density to establish how this type of layering formed. Plagioclase generally forms euhedral laths, while orthopyroxene is interstitial in texture and commonly envelops finer-grained and embayed plagioclase grains. Minor interstitial clinopyroxene was the final phase to crystallize from the magma. Plagioclase compositions show negligible change up-section (average An62), with local reverse zoning at the rims of cumulus laths (average increase of 2 mol%). In contrast, interstitial orthopyroxene compositions become more primitive up-section, from Mg# 57 to Mg# 63. Clinopyroxene similarly shows an up-section increase in Mg#. Pyroxene compositions record the primary magmatic signature of the melt at the time of crystallization and are not an artefact of the trapped liquid shift effect. Combined, the textures and decoupled mineral compositions indicate that the upward density increase is produced by the downward infiltration of noritic magma into a previously emplaced plagioclase-rich crystal mush. Fresh noritic magma soaked down into the crystallizing anorthositic mush, partially dissolving plagioclase laths and assimilating Fe-enriched pore melt. The presence of multiple cycles showing upward increases in density in the Bellevue drillcore suggests that downward magma infiltration occurred episodically during crystallization of the Main Zone.

Photonic crystal surface-emitting lasers enabled by an accidental Dirac point

DOEpatents

Chua, Song Liang; Lu, Ling; Soljacic, Marin

2014-12-02

A photonic-crystal surface-emitting laser (PCSEL) includes a gain medium electromagnetically coupled to a photonic crystal whose energy band structure exhibits a Dirac cone of linear dispersion at the center of the photonic crystal's Brillouin zone. This Dirac cone's vertex is called a Dirac point; because it is at the Brillouin zone center, it is called an accidental Dirac point. Tuning the photonic crystal's band structure (e.g., by changing the photonic crystal's dimensions or refractive index) to exhibit an accidental Dirac point increases the photonic crystal's mode spacing by orders of magnitudes and reduces or eliminates the photonic crystal's distributed in-plane feedback. Thus, the photonic crystal can act as a resonator that supports single-mode output from the PCSEL over a larger area than is possible with conventional PCSELs, which have quadratic band edge dispersion. Because output power generally scales with output area, this increase in output area results in higher possible output powers.

An assessment of calcite crystal growth mechanisms based on crystal size distributions

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.; Hoch, A.R.; Reddy, M.M.

2000-01-01

Calcite crystal growth experiments were undertaken to test a recently proposed model that relates crystal growth mechanisms to the shapes of crystal size distributions (CSDs). According to this approach, CSDs for minerals have three basic shapes: (1) asymptotic, which is related to a crystal growth mechanism having constant-rate nucleation accompanied by surface-controlled growth; (2) lognormal, which results from decaying-rate nucleation accompanied by surface-controlled growth; and (3) a theoretical, universal, steady-state curve attributed to Ostwald ripening. In addition, there is a fourth crystal growth mechanism that does not have a specific CSD shape, but which preserves the relative shapes of previously formed CSDs. This mechanism is attributed to supply-controlled growth. All three shapes were produced experimentally in the calcite growth experiments by modifying nucleation conditions and solution concentrations. The asymptotic CSD formed when additional reactants were added stepwise to the surface of solutions that were supersaturated with respect to calcite (initial Ω = 20, where Ω = 1 represents saturation), thereby leading to the continuous nucleation and growth of calcite crystals. Lognormal CSDs resulted when reactants were added continuously below the solution surface, via a submerged tube, to similarly supersaturated solutions (initial Ω = 22 to 41), thereby leading to a single nucleation event followed by surface-controlled growth. The Ostwald CSD resulted when concentrated reactants were rapidly mixed, leading initially to high levels of supersaturation (Ω >100), and to the formation and subsequent dissolution of very small nuclei, thereby yielding CSDs having small crystal size variances. The three CSD shapes likely were produced early in the crystallization process, in the nanometer crystal size range, and preserved during subsequent growth. Preservation of the relative shapes of the CSDs indicates that a supply-controlled growth mechanism was established and maintained during the constant-composition experiments. CSDs having shapes intermediate between lognormal and Ostwald also were generated by varying the initial levels of supersaturation (initial Ω = 28.2 to 69.2) in rapidly mixed solutions. Lognormal CSDs were observed for natural calcite crystals that are found in septarian concretions occurring in southeastern Colorado. Based on the model described above, these CSDs indicate initial growth by surface control, followed by supply-controlled growth. Thus, CSDs may be used to deduce crystal growth mechanisms from which geologic conditions early in the growth history of a mineral can be inferred. Conversely, CSD shape can be predicted during industrial crystallization by applying the appropriate conditions for a particular growth mechanism.

Topotactical growth of thick perovskite oxynitride layers by nitridation of single crystalline oxides

NASA Astrophysics Data System (ADS)

Ebbinghaus, Stefan G.; Aguiar, Rosiana; Weidenkaff, Anke; Gsell, Stefan; Reller, Armin

2008-06-01

Thick films of the perovskite-related oxynitrides LaTiO 2N, NdTiO 2N, SrNbO 2N and SrTaO 2N were synthesised by nitridation of single crystals of the corresponding oxides with general composition ABO 3.5. The oxide crystals were obtained by optical floating zone growth. They correspond to n = 4 member of the A nB nO 3 n+2 family of layered perovskites and were reacted at temperatures between 900 °C and 1050 °C to form the oxynitrides. Electron probe microanalysis proved the presence of nitrogen in a surface layer of a few micrometer thickness. Cross-section SEM revealed additional thin stripes of oxynitride within the bulk of the crystals, indicating that nitrogen is incorporated preferably parallel to the perovskite-type layers, which in turn are connected in a zipper-type mechanism. The formation of the desired perovskite-type oxynitrides was confirmed by X-ray diffraction. Pole figure measurements proved an epitaxial orientation ABO 2N (110)[001] ‖ ABO 3.5 (001)[100]. The mosaicity of the oxynitrides both in polar and azimuthal direction was very small (<2°) indicating a nearly single crystalline quality of the surface layer. The nitridation of the crystals results in a dramatic change in colour. Optical spectroscopy revealed shifts of the absorption edge by more than 200 nm to longer wavelengths with respect to the parent oxides, corresponding to a reduction of the band gap energies by 1.4-1.8 eV.

In situ study of the growth and degradation processes in tetragonal lysozyme crystals on a silicon substrate by high-resolution X-ray diffractometry

NASA Astrophysics Data System (ADS)

Kovalchuk, M. V.; Prosekov, P. A.; Marchenkova, M. A.; Blagov, A. E.; D'yakova, Yu. A.; Tereshchenko, E. Yu.; Pisarevskii, Yu. V.; Kondratev, O. A.

2014-09-01

The results of an in situ study of the growth of tetragonal lysozyme crystals by high-resolution X-ray diffractometry are considered. The crystals are grown by the sitting-drop method on crystalline silicon substrates of different types: both on smooth substrates and substrates with artificial surface-relief structures using graphoepitaxy. The crystals are grown in a special hermetically closed crystallization cell, which enables one to obtain images with an optical microscope and perform in situ X-ray diffraction studies in the course of crystal growth. Measurements for lysozyme crystals were carried out in different stages of the crystallization process, including crystal nucleation and growth, developed crystals, the degradation of the crystal structure, and complete destruction.

The control of ice crystal growth and effect on porous structure of konjac glucomannan-based aerogels.

PubMed

Ni, Xuewen; Ke, Fan; Xiao, Man; Wu, Kao; Kuang, Ying; Corke, Harold; Jiang, Fatang

2016-11-01

Konjac glucomannan (KGM)-based aerogels were prepared using a combination of sol-gel and freeze-drying methods. Preparation conditions were chosen to control ice crystal growth and aerogel structure formation. The ice crystals formed during pre-freezing were observed by low temperature polarizing microscopy, and images of aerogel pores were obtained by scanning electron microscopy. The size of ice crystals were calculated and size distribution maps were drawn, and similarly for aerogel pores. Results showed that ice crystal growth and aerogel pore sizes may be controlled by varying pre-freezing temperatures, KGM concentration and glyceryl monostearate concentration. The impact of pre-freezing temperatures on ice crystal growth was explained as combining ice crystal growth rate with nucleation rate, while the impacts of KGM and glyceryl monostearate concentration on ice crystal growth were interpreted based on their influences on sol network structure. Copyright © 2016 Elsevier B.V. All rights reserved.

Growth of benzil crystals by vertical dynamic gradient freeze technique in a transparent furnace

NASA Astrophysics Data System (ADS)

Lan, C. W.; Song, C. R.

1997-09-01

The vertical dynamic gradient freeze technique using a transparent furnace was applied to the growth of benzil single crystals. A flat-bottom ampoule with a <0001> seed was used for growth. During crystal growth, dynamic heating profiles were controlled through a computer, and the growth interface was recorded by a CCD camera. Computer simulation was also conducted, and the calculated convex interface and dynamic growth rate were consistent with the observed ones for various growth conditions. Conditions for growing single crystals were also determined, and they were mainly limited by constitutional supercooling. As the grown crystals were clear in appearance, their optical absorption spectra were insensitive to growth conditions and post-annealing.

Protein crystal growth tray assembly

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor); Miller, Teresa Y. (Inventor)

1992-01-01

A protein crystal growth tray assembly includes a tray that has a plurality of individual crystal growth chambers. Each chamber has a movable pedestal which carries a protein crystal growth compartment at an upper end. The several pedestals for each tray assembly are ganged together for concurrent movement so that the solutions in the various pedestal growth compartments can be separated from the solutions in the tray's growth chambers until the experiment is to be activated.

Rate limits in silicon sheet growth - The connections between vertical and horizontal methods

NASA Technical Reports Server (NTRS)

Thomas, Paul D.; Brown, Robert A.

1987-01-01

Meniscus-defined techniques for the growth of thin silicon sheets fall into two categories: vertical and horizontal growth. The interactions of the temperature field and the crystal shape are analyzed for both methods using two-dimensional finite-element models which include heat transfer and capillarity. Heat transfer in vertical growth systems is dominated by conduction in the melt and the crystal, with almost flat melt/crystal interfaces that are perpendicular to the direction of growth. The high axial temperature gradients characteristic of vertical growth lead to high thermal stresses. The maximum growth rate is also limited by capillarity which can restrict the conduction of heat from the melt into the crystal. In horizontal growth the melt/crystal interface stretches across the surface of the melt pool many times the crystal thickness, and low growth rates are achievable with careful temperature control. With a moderate axial temperature gradient in the sheet a substantial portion of the latent heat conducts along the sheet and the surface of the melt pool becomes supercooled, leading to dendritic growth. The thermal supercooling is surpressed by lowering the axial gradient in the crystal; this configuration is the most desirable for the growth of high quality crystals. An expression derived from scaling analysis relating the growth rate and the crucible temperature is shown to be reliable for horizontal growth.

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

DOE PAGES

Godinho, Jose R. A.; Stack, Andrew G.

2015-03-30

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

Growth Kinetics and Morphology of Barite Crystals Derived from Face-Specific Growth Rates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Godinho, Jose R. A.; Stack, Andrew G.

Here we investigate the growth kinetics and morphology of barite (BaSO 4) crystals by measuring the growth rates of the (001), (210), (010), and (100) surfaces using vertical scanning interferometry. Solutions with saturation indices 1.1, 2.1, and 3.0 without additional electrolyte, in 0.7 M NaCl, or in 1.3 mM SrCl2 are investigated. Face-specific growth rates are inhibited in the SrCl 2 solution relative to a solution without electrolyte, except for (100). Contrarily, growth of all faces is promoted in the NaCl solution. The variation of face-specific rates is solution-specific, which leads to a. change of the crystal morphology and overallmore » growth rate of crystals. The measured face-specific growth rates are used to model the growth of single crystals. Modeled crystals have a morphology and size similar to those grown from solution. Based on the model the time dependence of surface area and growth rates is analyzed. Growth rates change with time due to surface area normalization for small crystals and large growth intervals. By extrapolating rates to crystals with large surfaces areas, time-independent growth rates are 0.783, 2.96, and 0.513 mmol∙m -2∙h -1, for saturation index 2.1 solutions without additional electrolyte, NaCl, and SrCl 2, respectively.« less

Unidirectional growth of benzil crystal from solution by Sankaranarayanan-Ramasamy method and its characterization

NASA Astrophysics Data System (ADS)

Rajalakshmi, M.; Shyju, T. S.; Indirajith, R.; Gopalakrishnan, R.

2012-02-01

Good quality <1 0 0> benzil single crystal with a diameter 18 mm and length 75 mm was successfully grown from solution by the unidirectional growth method of Sankaranarayanan-Ramasamy (SR) for the first time in the literature. The seed crystals have been harvested from conventional solution growth technique and subsequently used for unidirectional growth. The grown crystal was subjected to various characterization studies. The results of UV-vis spectral analysis, photoluminescence, etching and microhardness studies were compared with conventional solution grown crystal to that of SR method grown crystal. The quality of SR method grown benzil crystal is better than conventional solution grown crystal.

Fast growth of n-type 4H-SiC bulk crystal by gas-source method

NASA Astrophysics Data System (ADS)

Hoshino, Norihiro; Kamata, Isaho; Tokuda, Yuichiro; Makino, Emi; Kanda, Takahiro; Sugiyama, Naohiro; Kuno, Hironari; Kojima, Jun; Tsuchida, Hidekazu

2017-11-01

Fast growth of n-type 4H-SiC crystals was attempted using a high-temperature gas-source method. High growth rates exceeding 9 mm/h were archived at a seed temperature of 2550 °C, although the formation of macro-step bunching caused doping fluctuation and voids in the grown crystal. We investigated a trade-off between growth-rate enhancement and macro-step formation and how to improve the trade-off. By controlling the growth conditions, the growth of highly nitrogen-doped 4H-SiC crystals without the doping fluctuation and void formation were accomplished under a high growth rate exceeding 3 mm/h, maintaining the density of threading screw dislocations in the same level with the seed crystal. The influence of growth parameters on nitrogen incorporations into grown crystals was also surveyed.

Maintenance of supersaturation I: indomethacin crystal growth kinetic modeling using an online second-derivative ultraviolet spectroscopic method.

PubMed

Patel, Dhaval D; Joguparthi, Vijay; Wang, Zeren; Anderson, Bradley D

2011-07-01

Formulations that produce supersaturated solutions after their oral administration have received increased attention as a means to improve bioavailability of poorly water-soluble drugs. Although it is widely recognized that excipients can prolong supersaturation, the mechanisms by which these beneficial effects are realized are generally unknown. Difficulties in separately measuring the kinetics of nucleation and crystal growth have limited progress in understanding the mechanisms by which excipients contribute to the supersaturation maintenance. This paper describes the crystal growth kinetic modeling of indomethacin, a poorly water-soluble drug, from supersaturated aqueous suspensions using a newly developed, online second-derivative ultraviolet spectroscopic method. The apparent indomethacin equilibrium solubility after crystal growth at a high degree of supersaturation (S=6) was approximately 55% higher than the indomethacin equilibrium solubility determined prior to growth, which was attributed to the deposition of a higher energy indomethacin form on the seed crystals. The indomethacin crystal growth kinetics (S=6) was of first order. By comparing the mass transfer coefficients from indomethacin dissolution and crystal growth, it was shown that the indomethacin crystal growth kinetics at S=6 was bulk diffusion controlled. The change in indomethacin seed crystal size distribution before and after crystal growth was determined and modeled using a mass-balance relationship. Copyright © 2011 Wiley-Liss, Inc. and the American Pharmacists Association

Crystal growth mechanisms in miarolitic cavities in the Lake George ring complex and vicinity, Colorado

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

1999-01-01

The Crystal Peak area of the Pikes Peak batholith, near Lake George in central Colorado, is world-renowned for its crystals of amazonite (the blue-green variety of microcline) and smoky quartz. Such crystals, collected from individual miarolitic pegmatites, have a remakably small variation in crystal size within each pegmatite, and the shapes of plots of their crystal size distributions (CSDs) are invariably lognormal or close to lognormal in all cases. These observations are explained by a crystal growth mechanism that was governed initially by surface-controlled kinetics, during which crystals tended to grow larger in proportion to their size, thereby establishing lognormal CSDs. Surface-controlled growth was followed by longer periods of supply controlled growth, during which growth rate was predominantly size-independent, consequently preserving the lognormal shapes of the CSDs and the small size variation. The change from surface- to supply controlled growth kinetics may have resulted from an increasing demand for nutrients that exceeded diffusion limitations of the system. The proposed model for crystal growth in this locality appears to be common in the geologic record, and can be used with other information, such as isotopic data, to deduce physico-chemical conditions during crystal formation.

Calculation Of Clinopyroxene And Olivine Growth Rates Using Plagioclase Residence Time

NASA Astrophysics Data System (ADS)

Kilinc, A. I.; Borell, A.; Leu, A.

2012-12-01

According to the Crystal Size Distribution theory (CSD) in a plot of logarithm of number of crystals of a given size range per unit volume [ln(n)], against crystal size [L] shows a straight line. Slope of that line is given by where is the crystal residence time and G is the crystal growth rate. Therefore if is known then G can be calculated. We used thin sections of the Kilauea basalt from Hawaii where olivine, clinopyroxene and plagioclase crystallized within a small temperature range, and the crystal growth rate of plagioclase is known. Assuming that crystal residence times of these three minerals are the same, we plotted ln(n) against L and using the slope and the known crystal growth rate of plagioclase we calculated the crystal growth rates of clinopyroxene and olivine. For the clinopyroxene growth rate we report 10-10.9cm/sec, which is in good agreement with Congdon's data of 10-10 cm/sec. We also calculated the growth rate of olivine is a basaltic melt as 10-8.5 cm/sec which is comparable to < 10-10 to 10-7 cm/sec given by Donaldson and Jambon.

Protein Crystal Growth With the Aid of Microfluidics

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark

2003-01-01

Protein crystallography is one of three well-known methods to obtain the structure of proteins. A major rate limiting step in protein crystallography is protein crystal nucleation and growth, which is still largely a process conducted by trial-and-error methods. Many attempts have been made to improve protein crystal growth by performing growth in microgravity. Although the use of microgravity appears to improve crystal quality in some attempts, this method has been inefficient because several reasons: we lack a fundamental understanding of macromolecular crystal growth in general and of the influence of microgravity in particular, we have to start with crystal growth conditions in microgravity based on conditions on the ground and finally the hardware does not allow for experimental iteration without reloading samples on the ground. To partially accommodate the disadvantages of the current hardware, we have used microfluidic technology (Lab-on-a-Chip devices) to design the concept of a more efficient crystallization device, suitable for use on the International Space Station and in high-throughput applications on the ground. The concept and properties of microfluidics, the application design process, and the advances in protein crystal growth hardware will be discussed in this presentation. Some examples of proteins crystallized in the new hardware will be discussed, including the differences between conventional crystallization versus crystallization in microfluidics.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1989-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into an adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Liquid encapsulated crystal growth

NASA Technical Reports Server (NTRS)

Morrison, Andrew D. (Inventor)

1987-01-01

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into and adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB6 Single Crystals

PubMed Central

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; Tutmaher, J. A.; Leiner, J. C.; Lumsden, M. D.; Lavelle, C. M.; Wang, X. P.; Hoffmann, C.; Siegler, M. A.; Haldolaarachchige, N.; Young, D. P.; McQueen, T. M.

2016-01-01

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-ray computed tomography experiments we observe that natural isotope containing (SmB6) and doubly isotope enriched (154Sm11B6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB6. These results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported. PMID:26892648

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB 6 Single Crystals

DOE PAGES

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; ...

2016-02-19

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB 6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB 6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB 6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-raymore » computed tomography experiments we observe that natural isotope containing (SmB 6) and doubly isotope enriched ( 154Sm 11B 6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB 6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB 6. Finally, these results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB 6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported.« less

Life prediction and constitutive models for engine hot section anisotropic materials program

NASA Technical Reports Server (NTRS)

Nissley, D. M.; Meyer, T. G.; Walker, K. P.

1992-01-01

This report presents a summary of results from a 7 year program designed to develop generic constitutive and life prediction approaches and models for nickel-based single crystal gas turbine airfoils. The program was composed of a base program and an optional program. The base program addressed the high temperature coated single crystal regime above the airfoil root platform. The optional program investigated the low temperature uncoated single crystal regime below the airfoil root platform including the notched conditions of the airfoil attachment. Both base and option programs involved experimental and analytical efforts. Results from uniaxial constitutive and fatigue life experiments of coated and uncoated PWA 1480 single crystal material formed the basis for the analytical modeling effort. Four single crystal primary orientations were used in the experiments: group of zone axes (001), group of zone axes (011), group of zone axes (111), and group of zone axes (213). Specific secondary orientations were also selected for the notched experiments in the optional program. Constitutive models for an overlay coating and PWA 1480 single crystal materials were developed based on isothermal hysteresis loop data and verified using thermomechanical (TMF) hysteresis loop data. A fatigue life approach and life models were developed for TMF crack initiation of coated PWA 1480. A life model was developed for smooth and notched fatigue in the option program. Finally, computer software incorporating the overlay coating and PWA 1480 constitutive and life models was developed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Astrophysics Data System (ADS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-09-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-01-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

Crystal Growth of ZnSe and Related Ternary Compound Semiconductors by Vapor Transport

NASA Technical Reports Server (NTRS)

Su, Ching-Hua; Brebrick, Robert F.; Volz, Martin P.; Burger, Arnold; Dudley, Michael; Matyi, Richard J.; Ramachandran, Narayanan; Sha, Yi-Gao; Volz, Martin P.; Shih, Hung-Dah

2001-01-01

Crystal growth by vapor transport has several distinct advantages over melt growth techniques. Among various potential benefits from material processing in reduced gravity the followings two are considered to be related to crystal growth by vapor transport: (1) elimination of the crystal weight and its influence on the defect formation and (2) reduction of natural buoyancy-driven convective flows arising from thermally and/ or solutally induced density gradient in fluids. The previous results on vapor crystal growth of semiconductors showed the improvements in surface morphology, crystalline quality, electrical properties and dopant distribution of the crystals grown in reduced gravity as compared to the crystals grown on Earth. But the mechanisms, which are responsible for the improvements and cause the gravitational effects on the complicated and coupled processes of vapor mass transport and growth kinetics, are not well understood.

Elastic response of zone axis (001)-oriented PWA 1480 single crystal: The influence of secondary orientation

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

1991-01-01

The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

Single crystalline growth of a soluble organic semiconductor in a parallel aligned liquid crystal solvent using rubbing-treated polyimide films

NASA Astrophysics Data System (ADS)

Matsuzaki, Tomoya; Shibata, Yosei; Takeda, Risa; Ishinabe, Takahiro; Fujikake, Hideo

2017-01-01

For directional control of organic single crystals, we propose a crystal growth method using liquid crystal as the solvent. In this study, we examined the formation of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) single crystals using a parallel aligned liquid crystal (LC) cell and rubbing-treated polyimide films in order to clarify the effects of LC alignment on anisotropic C8-BTBT crystal growth. Based on the results, we found that the crystal growth direction of C8-BTBT single crystals was related to the direction of the aligned LC molecules because of rubbing treatment. Moreover, by optical evaluation, we found that the C8-BTBT single crystals have a aligned molecular structure.

Protein crystals and their growth

NASA Technical Reports Server (NTRS)

Chernov, Alexander A.

2003-01-01

Recent results on the associations between protein molecules in crystal lattices, crystal-solution surface energy, elastic properties, strength, and spontaneous crystal cracking are reviewed and discussed. In addition, some basic approaches to understanding the solubility of proteins are followed by an overview of crystal nucleation and growth. It is argued that variability of mixing in batch crystallization may be a source of the variation in the number of crystals ultimately appearing in the sample. The frequency at which new molecules join a crystal lattice is measured by the kinetic coefficient and is related to the observed crystal growth rate. Numerical criteria used to discriminate diffusion- and kinetic-limited growth are discussed on this basis. Finally, the creation of defects is discussed with an emphasis on the role of impurities and convection on macromolecular crystal perfection.

STS-30 onboard closeup of the fluids experiment apparatus (FEA) equipment

NASA Image and Video Library

1989-05-08

STS030-01-015 (4-8 May 1989) --- A 35mm close-up view of the Fluids Experiment Apparatus (FEA) aboard Atlantis for NASA’s STS-30 mission. Rockwell International is engaged in a joint endeavor agreement with NASA’s Office of Commercial Programs in the field of floating zone crystal growth and purification research. The March 1987 agreement provides for microgravity experiments to be performed in the company’s Microgravity Laboratory, the FEA. Crewmembers, especially Mary L. Cleave, devoted a great deal of onboard time to the monitoring of various materials science experiments using the apparatus.

Method for the growth of large low-defect single crystals

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor); Neudeck, Philip G. (Inventor); Trunek, Andrew J. (Inventor); Spry, David J. (Inventor)

2008-01-01

A method and the benefits resulting from the product thereof are disclosed for the growth of large, low-defect single-crystals of tetrahedrally-bonded crystal materials. The process utilizes a uniquely designed crystal shape whereby the direction of rapid growth is parallel to a preferred crystal direction. By establishing several regions of growth, a large single crystal that is largely defect-free can be grown at high growth rates. This process is particularly suitable for producing products for wide-bandgap semiconductors, such as SiC, GaN, AlN, and diamond. Large low-defect single crystals of these semiconductors enable greatly enhanced performance and reliability for applications involving high power, high voltage, and/or high temperature operating conditions.

The Effects of Impurities on Protein Crystal Growth and Nucleation: A Preliminary Study

NASA Technical Reports Server (NTRS)

Schall, Constance A.

1998-01-01

Kubota and Mullin (1995) devised a simple model to account for the effects of impurities on crystal growth of small inorganic and organic molecules in aqueous solutions. Experimentally, the relative step velocity and crystal growth of these molecules asymptotically approach zero or non-zero values with increasing concentrations of impurities. Alternatively, the step velocity and crystal growth can linearly approach zero as the impurity concentration increases. The Kubota-Mullin model assumes that the impurity exhibits Langmuirian adsorption onto the crystal surface. Decreases in step velocities and subsequent growth rates are related to the fractional coverage (theta) of the crystal surface by adsorbed impurities; theta = Kx / (I +Kx), x = mole fraction of impurity in solution. In the presence of impurities, the relative step velocity, V/Vo, and the relative growth rate of a crystal face, G/Go, are proposed to conform to the following equations: V/Vo approx. = G/Go = 1 - (alpha)(theta). The adsorption of impurity is assumed to be rapid and in quasi-equilibrium with the crystal surface sites available. When the value of alpha, an effectiveness factor, is one the growth will asymptotically approach zero with increasing concentrations of impurity. At values less than one, growth approaches a non-zero value asymptotically. When alpha is much greater than one, there will be a linear relationship between impurity concentration and growth rates. Kubota and Mullin expect alpha to decrease with increasing supersaturation and shrinking size of a two dimensional nucleus. It is expected that impurity effects on protein crystal growth will exhibit behavior similar to that of impurities in small molecule growth. A number of proteins were added to purified chicken egg white lysozyme, the effect on crystal nucleation and growth assessed.

Crystal growth and annealing method and apparatus

DOEpatents

Gianoulakis, Steven E.; Sparrow, Robert

2001-01-01

A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF.sub.2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing. An embodiment of the present invention comprises a secondary heater incorporated into a conventional crystal growth and annealing apparatus. The secondary heater supplies heat to minimize the temperature gradients in the crystal during the annealing process. The secondary heater can mount near the bottom of the crucible to effectively maintain appropriate temperature gradients.

Protein crystal growth in space

NASA Technical Reports Server (NTRS)

Bugg, C. E.; Clifford, D. W.

1987-01-01

The advantages of protein crystallization in space, and the applications of protein crystallography to drug design, protein engineering, and the design of synthetic vaccines are examined. The steps involved in using protein crystallography to determine the three-dimensional structure of a protein are discussed. The growth chamber design and the hand-held apparatus developed for protein crystal growth by vapor diffusion techniques (hanging-drop method) are described; the experimental data from the four Shuttle missions are utilized to develop hardware for protein crystal growth in space and to evaluate the effects of gravity on protein crystal growth.