Crystallization processes in Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass

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

Svoboda, Roman, E-mail: roman.svoboda@upce.cz; Bezdička, Petr; Gutwirth, Jan

2015-01-15

Highlights: • Crystallization kinetics of Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass was studied in dependence on particle size by DSC. • All studied fractions were described in terms of the SB autocatalytic model. • Relatively high amount of Te enhances manifestation of bulk crystallization mechanisms. • XRD analysis of samples crystallized under different conditions showed correlation with DSC data. • XRD analysis revealed a new crystallization mechanism indistinguishable by DSC. - Abstract: Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) analysis were used to study crystallization in Ge{sub 2}Sb{sub 2}Se{sub 4}Te glass under non-isothermal conditions as a function of the particlemore » size. The crystallization kinetics was described in terms of the autocatalytic Šesták–Berggren model. An extensive discussion of all aspects of a full-scale kinetic study of a crystallization process was undertaken. Dominance of the crystallization process originating from mechanically induced strains and heterogeneities was confirmed. Substitution of Se by Te was found to enhance the manifestation of the bulk crystallization mechanisms (at the expense of surface crystallization). The XRD analysis showed significant dependence of the crystalline structural parameters on the crystallization conditions (initial particle size of the glassy grains and applied heating rate). Based on this information, a new microstructural crystallization mechanism, indistinguishable by DSC, was proposed.« less

Investigation of the Evolution of Crystal Size and Shape during Temperature Cycling and in the Presence of a Polymeric Additive Using Combined Process Analytical Technologies

PubMed Central

2017-01-01

Crystal size and shape can be manipulated to enhance the qualities of the final product. In this work the steady-state shape and size of succinic acid crystals, with and without a polymeric additive (Pluronic P123) at 350 mL, scale is reported. The effect of the amplitude of cycles as well as the heating/cooling rates is described, and convergent cycling (direct nucleation control) is compared to static cycling. The results show that the shape of succinic acid crystals changes from plate- to diamond-like after multiple cycling steps, and that the time required for this morphology change to occur is strongly related to the type of cycling. Addition of the polymer is shown to affect both the final shape of the crystals and the time needed to reach size and shape steady-state conditions. It is shown how this phenomenon can be used to improve the design of the crystallization step in order to achieve more efficient downstream operations and, in general, to help optimize the whole manufacturing process. PMID:28867966

Reverse engineering the kidney: modelling calcium oxalate monohydrate crystallization in the nephron.

PubMed

Borissova, A; Goltz, G E; Kavanagh, J P; Wilkins, T A

2010-07-01

Crystallization of calcium oxalate monohydrate in a section of a single kidney nephron (distal convoluted tubule) is simulated using a model adapted from industrial crystallization. The nephron fluid dynamics is represented as a crystallizer/separator series with changing volume to allow for water removal along the tubule. The model integrates crystallization kinetics and crystal size distribution and allows the prediction of the calcium oxalate concentration profile and the nucleation and growth rates. The critical supersaturation ratio for the nucleation of calcium oxalate crystals has been estimated as 2 and the mean crystal size as 1 mum. The crystal growth order, determined as 2.2, indicates a surface integration mechanism of crystal growth and crystal growth dispersion. The model allows the exploration of the effect of varying the input calcium oxalate concentration and the rate of water extraction, simulating real life stressors for stone formation such as dietary loading and dehydration.

Theoretical and experimental analyses to determine the effects of crystal orientation and grain size on the thermoelectric properties of oblique deposited bismuth telluride thin films

NASA Astrophysics Data System (ADS)

Morikawa, Satoshi; Satake, Yuji; Takashiri, Masayuki

2018-06-01

The effects of crystal orientation and grain size on the thermoelectric properties of Bi2Te3 thin films were investigated by conducting experimental and theoretical analyses. To vary the crystal orientation and grain size, we performed oblique deposition, followed by thermal annealing treatment. The crystal orientation decreased as the oblique angle was increased, while the grain size was not changed significantly. The thermoelectric properties were measured at room temperature. A theoretical analysis was performed using a first principles method based on density functional theory. Then the semi-classical Boltzmann transport equation was used in the relaxation time approximation, with the effect of grain size included. Furthermore, the effect of crystal orientation was included in the calculation based on a simple semi-experimental model. A maximum power factor of 11.6 µW/(cm·K2) was obtained at an oblique angle of 40°. The calculated thermoelectric properties were in very good agreement with the experimentally measured values.

The influence of orientation on the stress rupture properties of nickel-base superalloy single crystals

NASA Technical Reports Server (NTRS)

Mackay, R. A.; Maier, R. D.

1982-01-01

Constant load creep rupture tests were performed on MAR-M247 single crystals at 724 MPa and 774 C where the effect of anisotropy is prominent. The initial orientations of the specimens as well as the final orientations of selected crystals after stress rupture testing were determined by the Laue back-reflection X-ray technique. The stress rupture lives of the MAR-M247 single crystals were found to be largely determined by the lattice rotations required to produce intersecting slip, because second-stage creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited the shortest stress rupture lives, whereas crystals requiring little or no rotations exhibited the lowest minimum creep rates, and consequently, the longest stress rupture lives.

In-situ nano-crystal-to-crystal transformation synthesis of energetic materials based on three 5,5′-azotetrazolate Cr(III) salts

PubMed Central

Miao, Yu; Qiu, Yanxuan; Cai, Jiawei; Wang, Zizhou; Yu, Xinwei; Dong, Wen

2016-01-01

The in-situ nano-crystal-to-crystal transformation (SCCT) synthesis provides a powerful approach for tailoring controllable feature shapes and sizes of nano crystals. In this work, three nitrogen-rich energetic nano-crystals based on 5,5′-azotetrazolate(AZT2−) Cr(III) salts were synthesized by means of SCCT methodology. SEM and TEM analyses show that the energetic nano-crystals feature a composition- and structure-dependent together with size-dependent thermal stability. Moreover, nano-scale decomposition products can be obtained above 500 °C, providing a new method for preparing metallic oxide nano materials. PMID:27869221

Human serum albumin crystals and method of preparation

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor)

1989-01-01

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

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging.

PubMed

Coughlan, H D; Darmanin, C; Phillips, N W; Hofmann, F; Clark, J N; Harder, R J; Vine, D J; Abbey, B

2015-07-01

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

PubMed Central

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.; Hofmann, F.; Clark, J. N.; Harder, R. J.; Vine, D. J.; Abbey, B.

2015-01-01

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources. PMID:26798804

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

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

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Radiation damage in a micron-sized protein crystal studied via reciprocal space mapping and Bragg coherent diffractive imaging

DOE PAGES

Coughlan, H. D.; Darmanin, C.; Phillips, N. W.; ...

2015-04-29

For laboratory and synchrotron based X-ray sources, radiation damage has posed a significant barrier to obtaining high-resolution structural data from biological macromolecules. The problem is particularly acute for micron-sized crystals where the weaker signal often necessitates the use of higher intensity beams to obtain the relevant data. Here, we employ a combination of techniques, including Bragg coherent diffractive imaging to characterise the radiation induced damage in a micron-sized protein crystal over time. The approach we adopt here could help screen for potential protein crystal candidates for measurement at X-ray free election laser sources.

Impact of interaction range and curvature on crystal growth of particles confined to spherical surfaces.

PubMed

Paquay, Stefan; Both, Gert-Jan; van der Schoot, Paul

2017-07-01

When colloidal particles form a crystal phase on a spherical template, their packing is governed by the effective interaction between them and the elastic strain of bending the growing crystal. For example, if growth commences under appropriate conditions, and the isotropic crystal that forms reaches a critical size, growth continues via the incorporation of defects to alleviate elastic strain. Recently, it was experimentally found that, if defect formation is somehow not possible, the crystal instead continues growing in ribbons that protrude from the original crystal. Here we report on computer simulations in which we observe both the formation of ribbons at short interaction ranges and packings that incorporate defects if the interaction is longer-ranged. The ribbons only form above some critical crystal size, below which the nucleus is disk-shaped. We find that the scaling of the critical crystal size differs slightly from the one proposed in the literature, and we argue that this is because the actual morphology transition is caused by the competition between line tension and elastic stress, rather than the competition between chemical potential and elastic stress.

Impact of interaction range and curvature on crystal growth of particles confined to spherical surfaces

NASA Astrophysics Data System (ADS)

Paquay, Stefan; Both, Gert-Jan; van der Schoot, Paul

2017-07-01

When colloidal particles form a crystal phase on a spherical template, their packing is governed by the effective interaction between them and the elastic strain of bending the growing crystal. For example, if growth commences under appropriate conditions, and the isotropic crystal that forms reaches a critical size, growth continues via the incorporation of defects to alleviate elastic strain. Recently, it was experimentally found that, if defect formation is somehow not possible, the crystal instead continues growing in ribbons that protrude from the original crystal. Here we report on computer simulations in which we observe both the formation of ribbons at short interaction ranges and packings that incorporate defects if the interaction is longer-ranged. The ribbons only form above some critical crystal size, below which the nucleus is disk-shaped. We find that the scaling of the critical crystal size differs slightly from the one proposed in the literature, and we argue that this is because the actual morphology transition is caused by the competition between line tension and elastic stress, rather than the competition between chemical potential and elastic stress.

Influence of computational domain size on the pattern formation of the phase field crystals

NASA Astrophysics Data System (ADS)

Starodumov, Ilya; Galenko, Peter; Alexandrov, Dmitri; Kropotin, Nikolai

2017-04-01

Modeling of crystallization process by the phase field crystal method (PFC) represents one of the important directions of modern computational materials science. This method makes it possible to research the formation of stable or metastable crystal structures. In this paper, we study the effect of computational domain size on the crystal pattern formation obtained as a result of computer simulation by the PFC method. In the current report, we show that if the size of a computational domain is changed, the result of modeling may be a structure in metastable phase instead of pure stable state. The authors present a possible theoretical justification for the observed effect and provide explanations on the possible modification of the PFC method to account for this phenomenon.

Ultrasonically controlled particle size distribution of explosives: a safe method.

PubMed

Patil, Mohan Narayan; Gore, G M; Pandit, Aniruddha B

2008-03-01

Size reduction of the high energy materials (HEM's) by conventional methods (mechanical means) is not safe as they are very sensitive to friction and impact. Modified crystallization techniques can be used for the same purpose. The solute is dissolved in the solvent and crystallized via cooling or is precipitated out using an antisolvent. The various crystallization parameters such as temperature, antisolvent addition rate and agitation are adjusted to get the required final crystal size and morphology. The solvent-antisolvent ratio, time of crystallization and yield of the product are the key factors for controlling antisolvent based precipitation process. The advantages of cavitationally induced nucleation can be coupled with the conventional crystallization process. This study includes the effect of the ultrasonically generated acoustic cavitation phenomenon on the solvent antisolvent based precipitation process. CL20, a high-energy explosive compound, is a polyazapolycyclic caged polynitramine. CL-20 has greater energy output than existing (in-use) energetic ingredients while having an acceptable level of insensitivity to shock and other external stimuli. The size control and size distribution manipulation of the high energy material (CL20) has been successfully carried out safely and quickly along with an increase in the final mass yield, compared to the conventional antisolvent based precipitation process.

Effects of crystal refining on wear behaviors and mechanical properties of lithium disilicate glass-ceramics.

PubMed

Zhang, Zhenzhen; Guo, Jiawen; Sun, Yali; Tian, Beimin; Zheng, Xiaojuan; Zhou, Ming; He, Lin; Zhang, Shaofeng

2018-05-01

The purpose of this study is to improve wear resistance and mechanical properties of lithium disilicate glass-ceramics by refining their crystal sizes. After lithium disilicate glass-ceramics (LD) were melted to form precursory glass blocks, bar (N = 40, n = 10) and plate (N = 32, n = 8) specimens were prepared. According to the differential scanning calorimetry (DSC) of precursory glass, specimens G1-G4 were designed to form lithium disilicate glass-ceramics with different crystal sizes using a two-step thermal treatment. In the meantime, heat-pressed lithium disilicate glass-ceramics (GC-P) and original ingots (GC-O) were used as control groups. Glass-ceramics were characterized using X-ray diffraction (XRD) and were tested using flexural strength test, nanoindentation test and toughness measurements. The plate specimens were dynamically loaded in a chewing simulator with 350 N up to 2.4 × 10 6 loading cycles. The wear analysis of glass-ceramics was performed using a 3D profilometer after every 300,000 wear cycles. Wear morphologies and microstructures were analyzed by scanning electron microscopy (SEM). One-way analysis of variance (ANOVA) was used to analyze the data. Multiple pairwise comparisons of means were performed by Tukey's post-hoc test. Materials with different crystal sizes (p < 0.05) exhibited different properties. Specifically, G3 with medium-sized crystals presented the highest flexural strength, hardness, elastic modulus and fracture toughness. G1 and G2 with small-sized crystals showed lower flexural strength, whereas G4, GC-P, and GC-O with large-sized crystals exhibited lower hardness and elastic modulus. The wear behaviors of all six groups showed running-in wear stage and steady wear stage. G3 showed the best wear resistance while GC-P and GC-O exhibited the highest wear volume loss. After crystal refining, lithium disilicate glass-ceramic with medium-sized crystals showed the highest wear resistance and mechanical properties. Copyright © 2018 Elsevier Ltd. All rights reserved.

New water soluble heterometallic complex showing unpredicted coordination modes of EDTA

NASA Astrophysics Data System (ADS)

Mudsainiyan, R. K.; Jassal, A. K.; Chawla, S. K.

2015-10-01

A mesoporous 3D polymeric complex (I) having formula {[Zr(IV)O-μ3-(EDTA)Fe(III)OH]·H2O}n has been crystallized and characterized by various techniques. Single-crystal X-ray diffraction analysis revealed that complex (I) crystallized in chiral monoclinic space group Cc (space group no. 9) with unexpected coordination modes of EDTA and mixture of two transition metal ions. In this complex, the coordination number of Zr(IV) ion is seven where four carboxylate oxygen atoms, two nitrogen atoms, one oxide atom are coordinating with Zr(IV). Fe(III) is four coordinated and its coordination environment is composed of three different carboxylic oxygen atoms from three different EDTA and one oxygen atom of -OH group. The structure consists of 4-c and 16-c (2-nodal) net with new topology and point symbol for net is (336·454·530)·(36). TGA study and XRPD pattern showed that the coordination polymer is quite stable even after losing water molecule and -OH ion. Quenching behavior in fluorescence of ligand is observed by complexation with transition metal ions is due to n-π* transition. The SEM micrograph shows the morphology of complex (I) exhibits spherical shape with size ranging from 50 to 280 nm. The minimum N2 (SBET=8.7693 m2/g) and a maximum amount of H2 (high surface area=1044.86 m2/g (STP)) could be adsorbed at 77 K. From DLS study, zeta potential is calculated i.e. -7.94 shows the negative charges on the surface of complex. Hirshfeld surface analysis and fingerprint plots revealed influence of weak or non bonding interactions in crystal packing of complex.

Applications of thin-film sandwich crystallization platforms.

PubMed

Axford, Danny; Aller, Pierre; Sanchez-Weatherby, Juan; Sandy, James

2016-04-01

Examples are shown of protein crystallization in, and data collection from, solutions sandwiched between thin polymer films using vapour-diffusion and batch methods. The crystallization platform is optimal for both visualization and in situ data collection, with the need for traditional harvesting being eliminated. In wells constructed from the thinnest plastic and with a minimum of aqueous liquid, flash-cooling to 100 K is possible without significant ice formation and without any degradation in crystal quality. The approach is simple; it utilizes low-cost consumables but yields high-quality data with minimal sample intervention and, with the very low levels of background X-ray scatter that are observed, is optimal for microcrystals.

End-pumped continuous-wave intracavity yellow Raman laser at 590 nm with SrWO4 Raman crystal

NASA Astrophysics Data System (ADS)

Yang, F. G.; You, Z. Y.; Zhu, Z. J.; Wang, Y.; Li, J. F.; Tu, C. Y.

2010-01-01

We present an end-pumped continuous-wave intra-cavity yellow Raman laser at 590 nm with a 60 mm long pure crystal SrWO4 and an intra-cavity LiB3O5 frequency doubling crystal. The highest output power of yellow laser at 590 nm was 230 mW and the output power and threshold were found to be correlative with the polarized directions of pure single crystal SrWO4 deeply. Along different directions, the minimum and maximum thresholds of yellow Raman laser at 590 nm were measured to be 2.8 W and 14.3 W with respect to 808 nm LD pump power, respectively.

Glass Forming Ability in Systems with Competing Orderings

NASA Astrophysics Data System (ADS)

Russo, John; Romano, Flavio; Tanaka, Hajime

2018-04-01

Some liquids, if cooled rapidly enough to avoid crystallization, can be frozen into a nonergodic glassy state. The tendency for a material to form a glass when quenched is called "glass-forming ability," and it is of key significance both fundamentally and for materials science applications. Here, we consider liquids with competing orderings, where an increase in the glass-forming ability is signaled by a depression of the melting temperature towards its minimum at triple or eutectic points. With simulations of two model systems where glass-forming ability can be tuned by an external parameter, we are able to interpolate between crystal-forming and glass-forming behavior. We find that the enhancement of the glass-forming ability is caused by an increase in the structural difference between liquid and crystal: stronger competition in orderings towards the melting point minimum makes a liquid structure more disordered (more complex). This increase in the liquid-crystal structure difference can be described by a single adimensional parameter, i.e., the interface energy cost scaled by the thermal energy, which we call the "thermodynamic interface penalty." Our finding may provide a general physical principle for not only controlling the glass-forming ability but also the emergence of glassy behavior of various systems with competing orderings, including orderings of structural, magnetic, electronic, charge, and dipolar origin.

Phosphates (V) recovery from phosphorus mineral fertilizers industry wastewater by continuous struvite reaction crystallization process.

PubMed

Hutnik, Nina; Kozik, Anna; Mazienczuk, Agata; Piotrowski, Krzysztof; Wierzbowska, Boguslawa; Matynia, Andrzej

2013-07-01

Continuous DT MSMPR (Draft Tube Mixed Suspension Mixed Product Removal) crystallizer was provided with typical wastewater from phosphorus mineral fertilizers industry (pH < 4, 0.445 mass % of PO4(3-), inorganic impurities presence), dissolved substrates (magnesium and ammonium chlorides) and solution alkalising the environment of struvite MgNH4PO4·6H2O reaction crystallization process. Research ran in constant temperature 298 K assuming stoichiometric proportions of substrates or 20% excess of magnesium ions. Influence of pH (8.5-10) and mean residence time (900-3600 s) on product size distribution, its chemical composition, crystals shape, size-homogeneity and process kinetics was identified. Crystals of mean size ca. 25-37 μm and homogeneity CV 70-83% were produced. The largest crystals, of acceptable homogeneity, were produced using 20% excess of magnesium ions, pH 9 and mean residence time 3600 s. Under these conditions nucleation rate did not exceed 9 × 10(7) 1/(s m(3)) according to SIG (Size Independent Growth) MSMPR kinetic model. Linear crystal growth rate was 4.27 × 10(-9) m/s. Excess of magnesium ions influenced struvite reaction crystallization process yield advantageously. Concentration of phosphate(V) ions decreased from 0.445 to 9.2 × 10(-4) mass %. This can be regarded as a very good process result. In product crystals, besides main component - struvite, all impurities from wastewater were detected analytically. Copyright © 2013 Elsevier Ltd. All rights reserved.

Crystallization of calcium oxalate in minimally diluted urine

NASA Astrophysics Data System (ADS)

Bretherton, T.; Rodgers, A.

1998-09-01

Crystallization of calcium oxalate was studied in minimally diluted (92%) urine using a mixed suspension mixed product crystallizer in series with a Malvern particle sizer. The crystallization was initiated by constant flow of aqueous sodium oxalate and urine into the reaction vessel via two independent feed lines. Because the Malvern cell was in series with the reaction vessel, noninvasive measurement of particle sizes could be effected. In addition, aliquots of the mixed suspension were withdrawn and transferred to a Coulter counter for crystal counting and sizing. Steady-state particle size distributions were used to determine nucleation and growth kinetics while scanning electron microscopy was used to examine deposited crystals. Two sets of experiments were performed. In the first, the effect of the concentration of the exogenous sodium oxalate was investigated while in the second, the effect of temperature was studied. Calcium oxalate nucleation and growth rates were found to be dependent on supersaturation levels inside the crystallizer. However, while growth rate increased with increasing temperature, nucleation rates decreased. The favored phases were the trihydrate at 18°C, the dihydrate at 38° and the monohydrate at 58°C. The results of both experiments are in agreement with those obtained in other studies that have been conducted in synthetic and in maximally diluted urine and which have employed invasive crystal counting and sizing techniques. As such, the present study lends confidence to the models of urinary calcium oxalate crystallization processes which currently prevail in the literature.

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.

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.

User's Guide to Galoper: A Program for Simulating the Shapes of Crystal Size Distributions from Growth Mechanisms - and Associated Programs

USGS Publications Warehouse

Eberl, Dennis D.; Drits, V.A.; Srodon, J.

2000-01-01

GALOPER is a computer program that simulates the shapes of crystal size distributions (CSDs) from crystal growth mechanisms. This manual describes how to use the program. The theory for the program's operation has been described previously (Eberl, Drits, and Srodon, 1998). CSDs that can be simulated using GALOPER include those that result from growth mechanisms operating in the open system, such as constant-rate nucleation and growth, nucleation with a decaying nucleation rate and growth, surface-controlled growth, supply-controlled growth, and constant-rate and random growth; and those that result from mechanisms operating in the closed system such as Ostwald ripening, random ripening, and crystal coalescence. In addition, CSDs for two types weathering reactions can be simulated. The operation of associated programs also is described, including two statistical programs used for comparing calculated with measured CSDs, a program used for calculating lognormal CSDs, and a program for arranging measured crystal sizes into size groupings (bins).

MUDMASTER: A Program for Calculating Crystalline Size Distributions and Strain from the Shapes of X-Ray Diffraction Peaks

USGS Publications Warehouse

Eberl, D.D.; Drits, V.A.; Środoń, Jan; Nüesch, R.

1996-01-01

Particle size may strongly influence the physical and chemical properties of a substance (e.g. its rheology, surface area, cation exchange capacity, solubility, etc.), and its measurement in rocks may yield geological information about ancient environments (sediment provenance, degree of metamorphism, degree of weathering, current directions, distance to shore, etc.). Therefore mineralogists, geologists, chemists, soil scientists, and others who deal with clay-size material would like to have a convenient method for measuring particle size distributions. Nano-size crystals generally are too fine to be measured by light microscopy. Laser scattering methods give only average particle sizes; therefore particle size can not be measured in a particular crystallographic direction. Also, the particles measured by laser techniques may be composed of several different minerals, and may be agglomerations of individual crystals. Measurement by electron and atomic force microscopy is tedious, expensive, and time consuming. It is difficult to measure more than a few hundred particles per sample by these methods. This many measurements, often taking several days of intensive effort, may yield an accurate mean size for a sample, but may be too few to determine an accurate distribution of sizes. Measurement of size distributions by X-ray diffraction (XRD) solves these shortcomings. An X-ray scan of a sample occurs automatically, taking a few minutes to a few hours. The resulting XRD peaks average diffraction effects from billions of individual nano-size crystals. The size that is measured by XRD may be related to the size of the individual crystals of the mineral in the sample, rather than to the size of particles formed from the agglomeration of these crystals. Therefore one can determine the size of a particular mineral in a mixture of minerals, and the sizes in a particular crystallographic direction of that mineral.

Effect of the Inhomogeneity of Ice Crystals on Retrieving Ice Cloud Optical Thickness and Effective Particle Size

NASA Technical Reports Server (NTRS)

Xie, Yu; Minnis, Patrick; Hu, Yong X.; Kattawar, George W.; Yang, Ping

2008-01-01

Spherical or spheroidal air bubbles are generally trapped in the formation of rapidly growing ice crystals. In this study the single-scattering properties of inhomogeneous ice crystals containing air bubbles are investigated. Specifically, a computational model based on an improved geometric-optics method (IGOM) has been developed to simulate the scattering of light by randomly oriented hexagonal ice crystals containing spherical or spheroidal air bubbles. A combination of the ray-tracing technique and the Monte Carlo method is used. The effect of the air bubbles within ice crystals is to smooth the phase functions, diminish the 22deg and 46deg halo peaks, and substantially reduce the backscatter relative to bubble-free particles. These features vary with the number, sizes, locations and shapes of the air bubbles within ice crystals. Moreover, the asymmetry factors of inhomogeneous ice crystals decrease as the volume of air bubbles increases. Cloud reflectance lookup tables were generated at wavelengths 0.65 m and 2.13 m with different air-bubble conditions to examine the impact of the bubbles on retrieving ice cloud optical thickness and effective particle size. The reflectances simulated for inhomogeneous ice crystals are slightly larger than those computed for homogenous ice crystals at a wavelength of 0.65 microns. Thus, the retrieved cloud optical thicknesses are reduced by employing inhomogeneous ice cloud models. At a wavelength of 2.13 microns, including air bubbles in ice cloud models may also increase the reflectance. This effect implies that the retrieved effective particle sizes for inhomogeneous ice crystals are larger than those retrieved for homogeneous ice crystals, particularly, in the case of large air bubbles.

Effect of particle size on hydroxyapatite crystal-induced tumor necrosis factor alpha secretion by macrophages.

PubMed

Nadra, Imad; Boccaccini, Aldo R; Philippidis, Pandelis; Whelan, Linda C; McCarthy, Geraldine M; Haskard, Dorian O; Landis, R Clive

2008-01-01

Macrophages may promote a vicious cycle of inflammation and calcification in the vessel wall by ingesting neointimal calcific deposits (predominantly hydroxyapatite) and secreting tumor necrosis factor (TNF)alpha, itself a vascular calcifying agent. Here we have investigated whether particle size affects the proinflammatory potential of hydroxyapatite crystals in vitro and whether the nuclear factor (NF)-kappaB pathway plays a role in the macrophage TNFalpha response. The particle size and nano-topography of nine different crystal preparations was analyzed by X-ray diffraction, Raman spectroscopy, scanning electron microscopy and gas sorbtion analysis. Macrophage TNFalpha secretion was inversely related to hydroxyapatite particle size (P=0.011, Spearman rank correlation test) and surface pore size (P=0.014). A necessary role for the NF-kappaB pathway was demonstrated by time-dependent I kappaB alpha degradation and sensitivity to inhibitors of I kappaB alpha degradation. To test whether smaller particles were intrinsically more bioactive, their mitogenic activity on fibroblast proliferation was examined. This showed close correlation between TNFalpha secretion and crystal-induced fibroblast proliferation (P=0.007). In conclusion, the ability of hydroxyapatite crystals to stimulate macrophage TNFalpha secretion depends on NF-kappaB activation and is inversely related to particle and pore size, with crystals of 1-2 microm diameter and pore size of 10-50 A the most bioactive. Microscopic calcific deposits in early stages of atherosclerosis may therefore pose a greater inflammatory risk to the plaque than macroscopically or radiologically visible deposits in more advanced lesions.

Free Energy Calculations of Crystalline Hard Sphere Complexes Using Density Functional Theory

DOE PAGES

Gunawardana, K. G.S.H.; Song, Xueyu

2014-12-22

Recently developed fundamental measure density functional theory (FMT) is used to study binary hard sphere (HS) complexes in crystalline phases. By comparing the excess free energy, pressure and phase diagram, we show that the fundamental measure functional yields good agreements to the available simulation results of AB, AB 2 and AB 13 crystals. Additionally, we use this functional to study the HS models of five binary crystals, Cu 5Zr(C15 b), Cu 51Zr 14(β), Cu 10Zr 7(φ), CuZr(B2) and CuZr 2 (C11 b), which are observed in the Cu-Zr system. The FMT functional gives well behaved minimum for most of themore » hard sphere crystal complexes in the two dimensional Gaussian space, namely a crystalline phase. However, the current version of FMT functional (white Bear) fails to give a stable minimum for the structure Cu 10Zr 7(φ). We argue that the observed solid phases for the HS models of the Cu-Zr system are true thermodynamic stable phases and can be used as a reference system in perturbation calculations.« less

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.

Lattice Boltzmann Simulation of Kinetic Isotope Effect During Snow Crystal Formation

NASA Astrophysics Data System (ADS)

Lu, G.; Depaolo, D. J.; Kang, Q.; Zhang, D.

2007-12-01

The isotopic composition of precipitation, especially that of snow, plays a special role in the global hydrological cycle and in reconstruction of past climates using polar ice cores. The fractionation of the major water isotope species (HHO, HDO, HHO-18) during ice crystal formation is critical to understanding the global distribution of isotopes in precipitation. Ice crystal growth in clouds is traditionally treated with a spherically-symmetric steady state diffusion model, with semi-empirical modifications added to account for ventilation and for complex crystal morphology. Although it is known that crystal growth rate, which depends largely on the degree of vapor over- saturation, determines crystal morphology, there are no quantitative models that relate morphology to the vapor saturation factor. Since kinetic (vapor phase diffusion-controlled) isotopic fractionation also depends on growth rate, there should be direct relationships between vapor saturation, crystal morphology, and crystal isotopic composition. We use a 2D lattice Boltzmann model to simulate diffusion-controlled ice crystal growth from vapor- oversaturated air. In the model, crystals grow solely according to the diffusive fluxes just above the crystal surfaces, and hence crystal morphology arises from the initial and boundary conditions in the model and does not need to be specified a priori. Crystal growth patterns can be varied between random growth and deterministic growth (along the maximum concentration gradient for example). The input parameters needed are the isotope- dependent vapor deposition rate constant (k) and the water vapor diffusivity in air (D). The values of both k and D can be computed from kinetic theory, and there are also experimentally determined values of D. The deduced values of k are uncertain to the extent that the condensation coefficient for ice is uncertain. The ratio D/k is a length (order 1 micron) that determines the minimum scale of dendritic growth features and allows us to scale the numerical calculations to atmospheric conditions. Our calculations confirm that the crystal/vapor isotopic fractionation approaches the equilibrium value, and the crystals are compact (circular in 2D) as the saturation factor approaches unity (S= 1.0). However, few natural crystals form under such conditions. At higher oversaturation (e.g. S = 1.2), dendritic crystals of millimeter size develop on timescales appropriate to cloud processes, and kinetic effects control isotopic fractionation. Fractionation factors for dendritic crystals are similar to those predicted by the spherical diffusion model, but the model also gives estimates of crystal heterogeneity. Dendritic crystals are constrained to be relatively large, with dimension much greater than about 20D/k. The most difficult aspect of the modeling is to account for the large density difference between air and ice, which requires us to use a fictitious higher density for the vapor-oversaturated air and scale the crystal growth time accordingly. An approach using a larger scale simulation and the domain decomposition method can provide a vapor flux for a nested smaller scale calculation. The results clarify the controls on crystal growth, and the relationships between saturation state, growth rate, crystal morphology and isotopic fractionation.

Analysis of Crystallization Kinetics

NASA Technical Reports Server (NTRS)

Kelton, Kenneth F.

1997-01-01

A realistic computer model for polymorphic crystallization (i.e., initial and final phases with identical compositions), which includes time-dependent nucleation and cluster-size-dependent growth rates, is developed and tested by fits to experimental data. Model calculations are used to assess the validity of two of the more common approaches for the analysis of crystallization data. The effects of particle size on transformation kinetics, important for the crystallization of many systems of limited dimension including thin films, fine powders, and nanoparticles, are examined.

Electron Scattering at Surfaces of Epitaxial Metal Layers

NASA Astrophysics Data System (ADS)

Chawla, Jasmeet Singh

In the field of electron transport in metal films and wires, the 'size effect' refers to the increase in the resistivity of the films and wires as their critical dimensions (thickness of film, width and height of wires) approach or become less than the electron mean free path lambda, which is, for example, 39 nm for bulk copper at room temperature. This size-effect is currently of great concern to the semiconductor industry because the continued downscaling of feature sizes has already lead to Cu interconnect wires in this size effect regime, with a reported 2.5 times higher resistivity for 40 nm wide Cu wires than for bulk Cu. Silver is a possible alternate material for interconnect wires and titanium nitride is proposed as a gate metal in novel field-effect-transistors. Therefore, it is important to develop an understanding of how the growth, the surface morphology, and the microstructure of ultrathin (few nanometers) Cu, Ag and TiN layers affect their electrical properties. This dissertation aims to advance the scientific knowledge of electron scattering at surfaces (external surfaces and grain boundaries), that are, the primary reasons for the size-effect in metal conductors. The effect of surface and grain boundary scattering on the resistivity of Cu thin films and nanowires is separately quantified using (i) in situ transport measurements on single-crystal, atomically smooth Cu(001) layers, (ii) textured polycrystalline Cu(111) layers and patterned wires with independently varying grain size, thickness and line width, and (iii) in situ grown interfaces including Cu-Ta, Cu-MgO, Cu-vacuum and Cu-oxygen. In addition, the electron surface scattering is also measured in situ for single-crystal Ag(001), (111) twinned epitaxial Ag(001), and single-crystal TiN(001) layers. Cu(001), Ag(001), and TiN(001) layers with a minimum continuous thickness of 4, 3.5 and 1.8 nm, respectively, are grown by ultra-high vacuum magnetron sputter deposition on MgO(001) substrates with and without thin epitaxial TiN(001) wetting layers and are studied for structure, crystalline quality, surface morphology, density and composition by a combination of x-ray diffraction theta-2theta scans, o-rocking curves, pole figures, reciprocal space mapping, Rutherford backscattering, x-ray reflectometry and transmission electron microscopy. The TiN(001) surface suppresses Cu and Ag dewetting, yielding lower defect density, no twinning, and smaller surface roughness than if grown on MgO(001). Textured polycrystalline Cu(111) layers 25-50-nm-thick are deposited on a stack of 7.5-nm-Ta on SiO2/Si(001), and subsequent in situ annealing at 350°C followed by sputter etching in Ar plasma yields Cu layers with independently variable thickness and grain size. Cu nanowires, 75 to 350 nm wide, are fabricated from Cu layers with different average grain size using a subtractive patterning process. In situ electron transport measurements at room temperature in vacuum and at 77 K in liquid nitrogen for single-crystal Cu and Ag layers is consistent with the Fuchs-Sondheimer (FS) model and indicates specular scattering at the metal-vacuum boundary with an average specularity parameter p = 0.8 and 0.6, respectively. In contrast, layers measured ex situ show diffuse surface scattering due to sub-monolayer oxidation. Also, addition of Ta atoms on Cu(001) surface perturbs the smooth interface potential and results in completely diffuse scattering at the Cu-Ta interface, and in turn, a higher resistivity of single-crystal Cu layers. In situ exposure of Cu(001) layers to O2 between 10 -3 and 105 Pa-s results in a sequential increase, decrease and increase of the electrical resistance which is attributed to specular surface scattering for clean Cu(001) and for surfaces with a complete adsorbed monolayer, but diffuse scattering at partial coverage and after chemical oxidation. Electron transport measurements for polycrystalline Cu layers and wires show a 10-15% and 7-9% decrease in resistivity, respectively, when increasing the average lateral grain size by a factor of 1.8. The maximum resistivity decrease that can be achieved by increasing the grain size of polycrystalline Cu layers with an average grain size approximately ˜2.5x the layer thickness is 20-26%.

Ultra-Broad-Band Optical Parametric Amplifier or Oscillator

NASA Technical Reports Server (NTRS)

Strekalov, Dmitry; Matsko, Andrey; Savchenkov, Anatolly; Maleki, Lute

2009-01-01

A concept for an ultra-broad-band optical parametric amplifier or oscillator has emerged as a by-product of a theoretical study in fundamental quantum optics. The study was originally intended to address the question of whether the two-photon temporal correlation function of light [in particular, light produced by spontaneous parametric down conversion (SPDC)] can be considerably narrower than the inverse of the spectral width (bandwidth) of the light. The answer to the question was found to be negative. More specifically, on the basis of the universal integral relations between the quantum two-photon temporal correlation and the classical spectrum of light, it was found that the lower limit of two-photon correlation time is set approximately by the inverse of the bandwidth. The mathematical solution for the minimum two-photon correlation time also provides the minimum relative frequency dispersion of the down-converted light components; in turn, the minimum relative frequency dispersion translates to the maximum bandwidth, which is important for the design of an ultra-broad-band optical parametric oscillator or amplifier. In the study, results of an analysis of the general integral relations were applied in the case of an optically nonlinear, frequency-dispersive crystal in which SPDC produces collinear photons. Equations were found for the crystal orientation and pump wavelength, specific for each parametric-down-converting crystal, that eliminate the relative frequency dispersion of collinear degenerate (equal-frequency) signal and idler components up to the fourth order in the frequency-detuning parameter

Characterization of CuCl quantum dots grown in NaCl single crystals via optical measurements, X-ray diffraction, and transmission electron microscopy

NASA Astrophysics Data System (ADS)

Miyajima, Kensuke; Akatsu, Tatsuro; Itoh, Ken

2018-05-01

We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs) embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and transmission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work will play an important role in progressing the study of optical phenomena originating from assembled semiconductor QDs.

Self-cavity lasing in optically pumped single crystals of p-sexiphenyl

NASA Astrophysics Data System (ADS)

Yanagi, Hisao; Tamura, Kenji; Sasaki, Fumio

2016-08-01

Organic single-crystal self-cavities are prepared by solution growth of p-sexiphenyl (p-6P). Based on Fabry-Pérot feedback inside a quasi-lozenge-shaped platelet crystal, edge-emitting laser is obtained under optical pumping. The multimode lasing band appears at the 0-1 or 0-2 vibronic progressions depending on the excitation conditions which affect the self-absorption effect. Cavity-size dependence of amplified spontaneous emission (ASE) is investigated with laser-etched single crystals of p-6P. As the cavity length of square-shaped crystal is reduced from 100 to 10 μm, ASE threshold fluence is decreased probably due to size-dependent light confinement in the crystal cavity.

Highly crystallized nanometer-sized zeolite a with large Cs adsorption capability for the decontamination of water.

PubMed

Torad, Nagy L; Naito, Masanobu; Tatami, Junichi; Endo, Akira; Leo, Sin-Yen; Ishihara, Shinsuke; Wu, Kevin C-W; Wakihara, Toru; Yamauchi, Yusuke

2014-03-01

Nanometer-sized zeolite A with a large cesium (Cs) uptake capability is prepared through a simple post-milling recrystallization method. This method is suitable for producing nanometer-sized zeolite in large scale, as additional organic compounds are not needed to control zeolite nucleation and crystal growth. Herein, we perform a quartz crystal microbalance (QCM) study to evaluate the uptake ability of Cs ions by zeolite, to the best of our knowledge, for the first time. In comparison to micrometer-sized zeolite A, nanometer-sized zeolite A can rapidly accommodate a larger amount of Cs ions into the zeolite crystal structure, owing to its high external surface area. Nanometer-sized zeolite is a promising candidate for the removal of radioactive Cs ions from polluted water. Our QCM study on Cs adsorption uptake behavior provides the information of adsorption kinetics (e.g., adsorption amounts and rates). This technique is applicable to other zeolites, which will be highly valuable for further consideration of radioactive Cs removal in the future. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Size effects on negative thermal expansion in cubic ScF{sub 3}

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

Yang, C.; Guo, X. G.; Zhang, K.

2016-07-11

Scandium trifluoride (ScF{sub 3}), adopting a cubic ReO{sub 3}-type structure at ambient pressure, undergoes a pronounced negative thermal expansion (NTE) over a wide range of temperatures (10 K–1100 K). Here, we report the size effects on the NTE properties of ScF{sub 3}. The magnitude of NTE is reduced with diminishing the crystal size. As revealed by the specific heat measurement, the low-energy phonon vibrations which account for the NTE behavior are stiffened as the crystal size decreases. With decreasing the crystal size, the peaks in high-energy X-ray pair distribution function (PDF) become broad, which cannot be illuminated by local symmetry breaking. Instead,more » the broadened PDF peaks are strongly indicative of enhanced atomic displacements which are suggested to be responsible for the stiffening of NTE-related lattice vibrations. The present study suggests that the NTE properties of ReO{sub 3}-type and other open-framework materials can be effectively adjusted by controlling the crystal size.« less

The minimum or natural rate of flow and droplet size ejected by Taylor cone-jets: physical symmetries and scaling laws

NASA Astrophysics Data System (ADS)

Gañán-Calvo, A. M.; Rebollo-Muñoz, N.; Montanero, J. M.

2013-03-01

We aim to establish the scaling laws for both the minimum rate of flow attainable in the steady cone-jet mode of electrospray, and the size of the resulting droplets in that limit. Use is made of a small body of literature on Taylor cone-jets reporting precise measurements of the transported electric current and droplet size as a function of the liquid properties and flow rate. The projection of the data onto an appropriate non-dimensional parameter space maps a region bounded by the minimum rate of flow attainable in the steady state. To explain these experimental results, we propose a theoretical model based on the generalized concept of physical symmetry, stemming from the system time invariance (steadiness). A group of symmetries rising at the cone-to-jet geometrical transition determines the scaling for the minimum flow rate and related variables. If the flow rate is decreased below that minimum value, those symmetries break down, which leads to dripping. We find that the system exhibits two instability mechanisms depending on the nature of the forces arising against the flow: one dominated by viscosity and the other by the liquid polarity. In the former case, full charge relaxation is guaranteed down to the minimum flow rate, while in the latter the instability condition becomes equivalent to the symmetry breakdown by charge relaxation or separation. When cone-jets are formed without artificially imposing a flow rate, a microjet is issued quasi-steadily. The flow rate naturally ejected this way coincides with the minimum flow rate studied here. This natural flow rate determines the minimum droplet size that can be steadily produced by any electrohydrodynamic means for a given set of liquid properties.

Application Of Empirical Phase Diagrams For Multidimensional Data Visualization Of High Throughput Microbatch Crystallization Experiments.

PubMed

Klijn, Marieke E; Hubbuch, Jürgen

2018-04-27

Protein phase diagrams are a tool to investigate cause and consequence of solution conditions on protein phase behavior. The effects are scored according to aggregation morphologies such as crystals or amorphous precipitates. Solution conditions affect morphological features, such as crystal size, as well as kinetic features, such as crystal growth time. Common used data visualization techniques include individual line graphs or symbols-based phase diagrams. These techniques have limitations in terms of handling large datasets, comprehensiveness or completeness. To eliminate these limitations, morphological and kinetic features obtained from crystallization images generated with high throughput microbatch experiments have been visualized with radar charts in combination with the empirical phase diagram (EPD) method. Morphological features (crystal size, shape, and number, as well as precipitate size) and kinetic features (crystal and precipitate onset and growth time) are extracted for 768 solutions with varying chicken egg white lysozyme concentration, salt type, ionic strength and pH. Image-based aggregation morphology and kinetic features were compiled into a single and easily interpretable figure, thereby showing that the EPD method can support high throughput crystallization experiments in its data amount as well as its data complexity. Copyright © 2018. Published by Elsevier Inc.

Large-volume protein crystal growth for neutron macromolecular crystallography.

PubMed

Ng, Joseph D; Baird, James K; Coates, Leighton; Garcia-Ruiz, Juan M; Hodge, Teresa A; Huang, Sijay

2015-04-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.

Particle size studies to reveal crystallization mechanisms of the metal organic framework HKUST-1 during sonochemical synthesis.

PubMed

Armstrong, Mitchell R; Senthilnathan, Sethuraman; Balzer, Christopher J; Shan, Bohan; Chen, Liang; Mu, Bin

2017-01-01

Systematic studies of key operating parameters for the sonochemical synthesis of the metal organic framework (MOF) HKUST-1(also called CuBTC) were performed including reaction time, reactor volume, sonication amplitude, sonication tip size, solvent composition, and reactant concentrations analyzed through SEM particle size analysis. Trends in the particle size and size distributions show reproducible control of average particle sizes between 1 and 4μm. These results along with complementary studies in sonofragmentation and temperature control were conducted to compare these results to kinetic crystal growth models found in literature to develop a plausible hypothetical mechanism for ultrasound-assisted growth of metal-organic-frameworks composed of a competitive mechanism including constructive solid-on-solid (SOS) crystal growth and a deconstructive sonofragmentation. Copyright © 2016 Elsevier B.V. All rights reserved.

Application of linker technique to trap transiently interacting protein complexes for structural studies

PubMed Central

Reddy Chichili, Vishnu Priyanka; Kumar, Veerendra; Sivaraman, J.

2016-01-01

Protein-protein interactions are key events controlling several biological processes. We have developed and employed a method to trap transiently interacting protein complexes for structural studies using glycine-rich linkers to fuse interacting partners, one of which is unstructured. Initial steps involve isothermal titration calorimetry to identify the minimum binding region of the unstructured protein in its interaction with its stable binding partner. This is followed by computational analysis to identify the approximate site of the interaction and to design an appropriate linker length. Subsequently, fused constructs are generated and characterized using size exclusion chromatography and dynamic light scattering experiments. The structure of the chimeric protein is then solved by crystallization, and validated both in vitro and in vivo by substituting key interacting residues of the full length, unlinked proteins with alanine. This protocol offers the opportunity to study crucial and currently unattainable transient protein interactions involved in various biological processes. PMID:26985443

Emerging technologies in medical applications of minimum volume vitrification

PubMed Central

Zhang, Xiaohui; Catalano, Paolo N; Gurkan, Umut Atakan; Khimji, Imran; Demirci, Utkan

2011-01-01

Cell/tissue biopreservation has broad public health and socio-economic impact affecting millions of lives. Cryopreservation technologies provide an efficient way to preserve cells and tissues targeting the clinic for applications including reproductive medicine and organ transplantation. Among these technologies, vitrification has displayed significant improvement in post-thaw cell viability and function by eliminating harmful effects of ice crystal formation compared to the traditional slow freezing methods. However, high cryoprotectant agent concentrations are required, which induces toxicity and osmotic stress to cells and tissues. It has been shown that vitrification using small sample volumes (i.e., <1 μl) significantly increases cooling rates and hence reduces the required cryoprotectant agent levels. Recently, emerging nano- and micro-scale technologies have shown potential to manipulate picoliter to nanoliter sample sizes. Therefore, the synergistic integration of nanoscale technologies with cryogenics has the potential to improve biopreservation methods. PMID:21955080

Micro-apparatus for rapid determinations of protein solubilities

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Munson, Sibyl

1991-01-01

We have developed a column-based micro-technique for rapid determinations of protein solubilities. While retaining a large crystal surface area, the column dead volume has been reduced to equal to or less than 5 micro liters. The technique was tested with tetragonal lysozyme (pH 4.5, 0.1 M acetate, 3.0 percent NaCl, 5-25 C) and column volumes of about 60, 300, and 900 micro liters. Identical solubility data were obtained, indicating that equilibration was obtained even in the smallest columns. In addition, solubility data for Br- and I- salts of lysozyme (pH 4.5, 0.1 M acetate buffer, 0.5 M salt concentrations) were obtained. It appears that the technique can be further miniaturized. The limit in further reducing the crystalline column volume is determined by the minimum solution sample size needed to determine the protein concentration.

Strain relaxation in epitaxial GaAs/Si (0 0 1) nanostructures

NASA Astrophysics Data System (ADS)

Kozak, Roksolana; Prieto, Ivan; Arroyo Rojas Dasilva, Yadira; Erni, Rolf; Skibitzki, Oliver; Capellini, Giovanni; Schroeder, Thomas; von Känel, Hans; Rossell, Marta D.

2017-11-01

Crystal defects, present in 100 nm GaAs nanocrystals grown by metal organic vapour phase epitaxy on top of (0 0 1)-oriented Si nanotips (with a tip opening 50-90 nm), have been studied by means of high-resolution aberration-corrected high-angle annular dark-field scanning transmission electron microscopy. The role of 60° perfect, 30° and 90° Shockley partial misfit dislocations (MDs) in the plastic strain relaxation of GaAs on Si is discussed. Formation conditions of stair-rod dislocations and coherent twin boundaries in the GaAs nanocrystals are explained. Also, although stacking faults are commonly observed, we show here that synthesis of GaAs nanocrystals with a minimum number of these defects is possible. On the other hand, from the number of MDs, we have to conclude that the GaAs nanoparticles are fully relaxed plastically, such that for the present tip sizes no substrate compliance can be observed.

The Effect of Solution Conditions on the Nucleation Kinetics of Tetragonal Lysozyme Crystals

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Baird, James K.; Pusey, Marc L.

1998-01-01

An understanding of protein crystal nucleation rates and the effect of solution conditions upon them, is fundamental to the preparation of protein crystals of the desired size and shape for X-ray diffraction analysis. The ability to predict the effect of supersaturation, temperature, pH and precipitant concentration on the number and size of crystals formed is of great benefit in the pursuit of protein structure analysis. In this study we experimentally examine the effect of supersaturation, temperature, pH and sodium chloride concentration on the nucleation rate of tetragonal chicken egg white lysozyme crystals. In order to do this batch crystallization plates were prepared at given solution concentrations and incubated at three different temperatures over the period of one week. The number of crystals per well with their size and dimensions were recorded and correlated against solution conditions. Duplicate experiments indicate the reproducibility of the technique. Although it is well known that crystal numbers increase with increasing supersaturation, large changes in crystal number were also correlated against solution conditions of temperature, pH and salt concentration over the same supersaturation ranges. Analysis of these results enhance our understanding of the effect of solution conditions such as the dramatic effect that small changes in charge and ionic strength can have on the number of tetragonal lysozyme crystals that form and grow in solution.

Point Counts of Birds in Bottomland Hardwood Forests of the Mississippi Alluvial Valley: Duration, Minimum Sample Size, and Points Versus Visits

Treesearch

Winston Paul Smith; Daniel J. Twedt; David A. Wiedenfeld; Paul B. Hamel; Robert P. Ford; Robert J. Cooper

1993-01-01

To compare efficacy of point count sampling in bottomland hardwood forests, duration of point count, number of point counts, number of visits to each point during a breeding season, and minimum sample size are examined.

50 CFR 622.50 - Caribbean spiny lobster import prohibitions.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 50 Wildlife and Fisheries 8 2010-10-01 2010-10-01 false Caribbean spiny lobster import... ATLANTIC Management Measures § 622.50 Caribbean spiny lobster import prohibitions. (a) Minimum size limits for imported spiny lobster. There are two minimum size limits that apply to importation of spiny...

50 CFR 622.50 - Caribbean spiny lobster import prohibitions.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 50 Wildlife and Fisheries 10 2011-10-01 2011-10-01 false Caribbean spiny lobster import... ATLANTIC Management Measures § 622.50 Caribbean spiny lobster import prohibitions. (a) Minimum size limits for imported spiny lobster. There are two minimum size limits that apply to importation of spiny...

50 CFR 648.72 - Minimum surf clam size.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Atlantic Surf Clam and Ocean Quahog Fisheries § 648.72 Minimum surf clam size. Link to an amendment... quahog specifications. (a) Establishing catch quotas. The amount of surfclams or ocean quahogs that may... paragraph (b) of this section. The amount of surfclams available for harvest annually must be specified...

Out-of-equilibrium processes in suspensions of oppositely charged colloids: liquid-to-crystal nucleation and gel formation

NASA Astrophysics Data System (ADS)

Sanz, Eduardo

2009-03-01

We study the kinetics of the liquid-to-crystal transformation and of gel formation in colloidal suspensions of oppositely charged particles. We analyse, by means of both computer simulations and experiments, the evolution of a fluid quenched to a state point of the phase diagram where the most stable state is either a homogeneous crystalline solid or a solid phase in contact with a dilute gas. On the one hand, at high temperatures and high packing fractions, close to an ordered-solid/disordered-solid coexistence line, we find that the fluid-to-crystal pathway does not follow the minimum free energy route. On the other hand, a quench to a state point far from the ordered-crystal/disordered-crystal coexistence border is followed by a fluid-to-solid transition through the minimum free energy pathway. At low temperatures and packing fractions we observe that the system undergoes a gas-liquid spinodal decomposition that, at some point, arrests giving rise to a gel-like structure. Both our simulations and experiments suggest that increasing the interaction range favors crystallization over vitrification in gel-like structures. [4pt] In collaboration with Chantal Valeriani, Soft Condensed Matter, Debye Institute for Nanomaterials Science, Utrecht University, Princetonplein 5, 3584 CC Utrecht, The Netherlands and SUPA, School of Physics, University of Edinburgh, JCMB King's Buildings, Mayfield Road, Edinburgh EH9 3JZ, UK; Teun Vissers, Andrea Fortini, Mirjam E. Leunissen, and Alfons van Blaaderen, Soft Condensed Matter, Debye Institute for Nanomaterials Science, Utrecht University; Daan Frenke, FOM Institute for Atomic and Molecular Physics, Kruislaan 407, 1098 SJ Amsterdam, The Netherlands and Department of Chemistry, University of Cambridge, Lensfield Road, CB2 1EW, Cambridge, UK; and Marjolein Dijkstra, Soft Condensed Matter, Debye Institute for Nanomaterials Science, Utrecht University.

The effect of crystal size on tunneling phenomena in luminescent nanodosimetric materials

NASA Astrophysics Data System (ADS)

Pagonis, Vasilis; Bernier, Shannon; Vieira, Francisco Marques dos Santos; Steele, Shane

2017-12-01

The study of luminescence signals from nanodosimetric materials is an active research area, due to the many possible practical applications of such materials. In several of these materials it has been shown that quantum tunneling is a dominant mechanism for recombination processes associated with luminescence phenomena. This paper examines the effect of crystal size on quantum tunneling phenomena in nanocrystals, based on the assumption of a random distribution of electrons and positive ions. The behavior of such random distributions is determined by three characteristic lengths: the radius of the crystal R, the tunneling length a, and the initial average distance 〈d〉 between electrons and positive ions (which is directly related to the density of charges in the material). Two different cases are examined, depending on the relative concentrations of electrons and ions. In the first case the concentration of electrons is assumed to be much smaller than the concentration of positive ions. Examination of a previously derived analytical equation demonstrates two different types of crystal size effects. When the tunneling length a is much smaller than both R and 〈d〉, the analytical equations show that smaller crystals exhibit a faster tunneling recombination rate. However, when the tunneling length a is of the same order of magnitude as both R and 〈d〉, the opposite effect is observed, with smaller crystals exhibiting a slower tunneling recombination rate. As the crystal size increases, the rate of tunneling in both cases reaches the limit expected for bulk materials. In the second case we examine the situation where the concentrations of electrons and positive ions are equal at all times. In this situation there is no analytical equation available to describe the process, and the crystal size effects are simulated by using Monte Carlo (MC) techniques. The two opposite behaviors as a function of the crystal size are also observed in these MC simulations. The effect of sample temperature is also studied by extending the MC simulations to include thermal characteristics of the defects. The relevance of the simulated results for luminescence dosimetry is discussed.

Global statistics of microphysical properties of cloud-top ice crystals

NASA Astrophysics Data System (ADS)

van Diedenhoven, B.; Fridlind, A. M.; Cairns, B.; Ackerman, A. S.; Riedi, J.

2017-12-01

Ice crystals in clouds are highly complex. Their sizes, macroscale shape (i.e., habit), mesoscale shape (i.e., aspect ratio of components) and microscale shape (i.e., surface roughness) determine optical properties and affect physical properties such as fall speeds, growth rates and aggregation efficiency. Our current understanding on the formation and evolution of ice crystals under various conditions can be considered poor. Commonly, ice crystal size and shape are related to ambient temperature and humidity, but global observational statistics on the variation of ice crystal size and particularly shape have not been available. Here we show results of a project aiming to infer ice crystal size, shape and scattering properties from a combination of MODIS measurements and POLDER-PARASOL multi-angle polarimetry. The shape retrieval procedure infers the mean aspect ratios of components of ice crystals and the mean microscale surface roughness levels, which are quantifiable parameters that mostly affect the scattering properties, in contrast to "habit". We present global statistics on the variation of ice effective radius, component aspect ratio, microscale surface roughness and scattering asymmetry parameter as a function of cloud top temperature, latitude, location, cloud type, season, etc. Generally, with increasing height, sizes decrease, roughness increases, asymmetry parameters decrease and aspect ratios increase towards unity. Some systematic differences are observed for clouds warmer and colder than the homogeneous freezing level. Uncertainties in the retrievals will be discussed. These statistics can be used as observational targets for modeling efforts and to better constrain other satellite remote sensing applications and their uncertainties.

Global Statistics of Microphysical Properties of Cloud-Top Ice Crystals

NASA Technical Reports Server (NTRS)

Van Diedenhoven, Bastiaan; Fridlind, Ann; Cairns, Brian; Ackerman, Andrew; Riedl, Jerome

2017-01-01

Ice crystals in clouds are highly complex. Their sizes, macroscale shape (i.e., habit), mesoscale shape (i.e., aspect ratio of components) and microscale shape (i.e., surface roughness) determine optical properties and affect physical properties such as fall speeds, growth rates and aggregation efficiency. Our current understanding on the formation and evolution of ice crystals under various conditions can be considered poor. Commonly, ice crystal size and shape are related to ambient temperature and humidity, but global observational statistics on the variation of ice crystal size and particularly shape have not been available. Here we show results of a project aiming to infer ice crystal size, shape and scattering properties from a combination of MODIS measurements and POLDER-PARASOL multi-angle polarimetry. The shape retrieval procedure infers the mean aspect ratios of components of ice crystals and the mean microscale surface roughness levels, which are quantifiable parameters that mostly affect the scattering properties, in contrast to a habit. We present global statistics on the variation of ice effective radius, component aspect ratio, microscale surface roughness and scattering asymmetry parameter as a function of cloud top temperature, latitude, location, cloud type, season, etc. Generally, with increasing height, sizes decrease, roughness increases, asymmetry parameters decrease and aspect ratios increase towards unity. Some systematic differences are observed for clouds warmer and colder than the homogeneous freezing level. Uncertainties in the retrievals will be discussed. These statistics can be used as observational targets for modeling efforts and to better constrain other satellite remote sensing applications and their uncertainties.

The Effect of Temperature and Solution pH on the Nucleation of Tetragonal Lysozyme Crystals

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Jacobs, Randolph S.; Frazier, Tyralynn; Snell, Edward H.; Pusey, Marc L.

1999-01-01

Part of the challenge of macromolecular crystal growth for structure determination is obtaining crystals with a volume suitable for x-ray analysis. In this respect an understanding of the effect of solution conditions on macromolecule nucleation rates is advantageous. This study investigated the effects of supersaturation, temperature, and pH on the nucleation rate of tetragonal lysozyme crystals. Batch crystallization plates were prepared at given solution concentrations and incubated at set temperatures over 1 week. The number of crystals per well with their size and axial ratios were recorded and correlated with solution conditions. Crystal numbers were found to increase with increasing supersaturation and temperature. The most significant variable, however, was pH; crystal numbers changed by two orders of magnitude over the pH range 4.0-5.2. Crystal size also varied with solution conditions, with the largest crystals obtained at pH 5.2. Having optimized the crystallization conditions, we prepared a batch of crystals under the same initial conditions, and 50 of these crystals were analyzed by x-ray diffraction techniques. The results indicate that even under the same crystallization conditions, a marked variation in crystal properties exists.

Relation between inflammables and ignition sources in aircraft environments

NASA Technical Reports Server (NTRS)

Scull, Wilfred E

1951-01-01

A literature survey was conducted to determine the relation between aircraft ignition sources and inflammables. Available literature applicable to the problem of aircraft fire hazards is analyzed and discussed. Data pertaining to the effect of many variables on ignition temperatures, minimum ignition pressures, minimum spark-ignition energies of inflammables, quenching distances of electrode configurations, and size of openings through which flame will not propagate are presented and discussed. Ignition temperatures and limits of inflammability of gasoline in air in different test environments, and the minimum ignition pressures and minimum size of opening for flame propagation in gasoline-air mixtures are included; inerting of gasoline-air mixtures is discussed.

Utilisation of adsorption and desorption for simultaneously improving protein crystallisation success rate and crystal quality

NASA Astrophysics Data System (ADS)

Guo, Yun-Zhu; Sun, Li-Hua; Oberthuer, Dominik; Zhang, Chen-Yan; Shi, Jian-Yu; di, Jiang-Lei; Zhang, Bao-Liang; Cao, Hui-Ling; Liu, Yong-Ming; Li, Jian; Wang, Qian; Huang, Huan-Huan; Liu, Jun; Schulz, Jan-Mirco; Zhang, Qiu-Yu; Zhao, Jian-Lin; Betzel, Christian; He, Jian-Hua; Yin, Da-Chuan

2014-12-01

High-quality protein crystals of suitable size are an important prerequisite for applying X-ray crystallography to determine the 3-dimensional structure of proteins. However, it is often difficult to obtain protein crystals of appropriate size and quality because nucleation and growth processes can be unsuccessful. Here, we show that by adsorbing proteins onto porous polystyrene-divinylbenzene microspheres (SDB) floating on the surface of the crystallisation solution, a localised high supersaturation region at the surface of the microspheres and a low supersaturation region below the microspheres can coexist in a single solution. The crystals will easily nucleate in the region of high supersaturation, but when they grow to a certain size, they will sediment to the region of low supersaturation and continue to grow. In this way, the probability of crystallisation and crystal quality can be simultaneously increased in a single solution without changing other crystallisation parameters.

Influence of mixing and ultrasound frequency on antisolvent crystallisation of sodium chloride.

PubMed

Lee, Judy; Ashokkumar, Muthupandian; Kentish, Sandra E

2014-01-01

Ultrasound is known to promote nucleation of crystals and produce a narrower size distribution in a controlled and reproducible manner for the crystallisation process. Although there are various theories that suggest cavitation bubbles are responsible for sonocrystallisation, most studies use power ultrasonic horns that generate both intense shear and cavitation and this can mask the role that cavitation bubbles play. High frequency ultrasound from a plate transducer can be used to examine the effect of cavitation bubbles without the intense shear effect. This study reports the crystal size and morphology with various mixing speeds and ultrasound frequencies. The results show high frequency ultrasound produced sodium chloride crystals of similar size distribution as an ultrasonic horn. In addition, ultrasound generated sodium chloride crystals having a more symmetrical cubic structure compared to crystals produced by a high shear mixer. Copyright © 2013 Elsevier B.V. All rights reserved.

Nanoscale effects of silica particle supports on the formation and properties of TiO2 nanocatalysts

NASA Astrophysics Data System (ADS)

Li, Aize; Jin, Yuhui; Muggli, Darrin; Pierce, David T.; Aranwela, Hemantha; Marasinghe, Gaya K.; Knutson, Theodore; Brockman, Greg; Zhao, Julia Xiaojun

2013-06-01

Small TiO2 crystals in the anatase phase are in high demand as photocatalysts. Stable TiO2 crystals in the anatase phase were obtained using a silica nanoparticle as a support. The focus of this study was to investigate the nanoscale effect of the silica support on the formation and properties of small anatase crystals. The experiments were carried out using powder X-ray diffraction, differential thermal analysis, transmission electron microscopy, and energy dispersion spectroscopy. The results showed that the size of the silica support played a crucial role in crystallization of TiO2 and regulation of TiO2 properties, including phase transition, crystal size, thermodynamic property and catalytic activity. A nanoscale curvature model of the spherical silica support was proposed to explain these size effects. Finally, the developed TiO2 catalysts were applied to the oxidation of methanol using a high-throughput photochemical reactor. The size effect of the silica supports on the TiO2 catalytic efficiency was demonstrated using this system.

Microgravity

NASA Image and Video Library

1992-06-25

Zeolites are crystalline aluminosilicates that have complex framework structures. However, there are several features of zeolite crystals that make unequivocal structure determinations difficult. The acquisition of reliable structural information on zeolites is greatly facilitated by the availability of high-quality specimens. For structure determinations by conventional diffraction techniques, large single-crystal specimens are essential. Alternatively, structural determinations by powder profile refinement methods relax the constraints on crystal size, but still require materials with a high degree of crystalline perfection. Studies conducted at CAMMP (Center for Advanced Microgravity Materials Processing) have demonstrated that microgravity processing can produce larger crystal sizes and fewer structural defects relative to terrestrial crystal growth. Principal Investigator: Dr. Albert Sacco

Zeolites

NASA Technical Reports Server (NTRS)

1992-01-01

Zeolites are crystalline aluminosilicates that have complex framework structures. However, there are several features of zeolite crystals that make unequivocal structure determinations difficult. The acquisition of reliable structural information on zeolites is greatly facilitated by the availability of high-quality specimens. For structure determinations by conventional diffraction techniques, large single-crystal specimens are essential. Alternatively, structural determinations by powder profile refinement methods relax the constraints on crystal size, but still require materials with a high degree of crystalline perfection. Studies conducted at CAMMP (Center for Advanced Microgravity Materials Processing) have demonstrated that microgravity processing can produce larger crystal sizes and fewer structural defects relative to terrestrial crystal growth. Principal Investigator: Dr. Albert Sacco

Scanning electron microscope view of iron crystal growing on pyroxene crystal

NASA Technical Reports Server (NTRS)

1972-01-01

A scanning electron microscope photograph of a four-micron size iron crystal growing on a pyroxene crystal (calcium-magnesium-iron silicate) from the Apollo 15 Hadley-Apennino lunar landing site. The well developed crystal faces indicate that the crystal was formed from a hot vapor as the rock was cooling.

Modulating crystal grain size and optoelectronic properties of perovskite films for solar cells by reaction temperature

NASA Astrophysics Data System (ADS)

Ren, Xiaodong; Yang, Zhou; Yang, Dong; Zhang, Xu; Cui, Dong; Liu, Yucheng; Wei, Qingbo; Fan, Haibo; Liu, Shengzhong (Frank)

2016-02-01

Regulating the temperature during the direction contact and intercalation process (DCIP) for the transition from PbI2 to CH3NH3PbI3 modulated the crystallinity, crystal grain size and crystal grain orientation of the perovskite films. Higher temperatures produced perovskite films with better crystallinity, larger grain size, and better photovoltaic performance. The best cell, which had a PCE of 12.9%, was obtained on a film prepared at 200 °C. Further open circuit voltage decay and film resistance characterization revealed that the larger grain size contributed to longer carrier lifetime and smaller carrier transport resistance, both of which are beneficial for solar cell devices.Regulating the temperature during the direction contact and intercalation process (DCIP) for the transition from PbI2 to CH3NH3PbI3 modulated the crystallinity, crystal grain size and crystal grain orientation of the perovskite films. Higher temperatures produced perovskite films with better crystallinity, larger grain size, and better photovoltaic performance. The best cell, which had a PCE of 12.9%, was obtained on a film prepared at 200 °C. Further open circuit voltage decay and film resistance characterization revealed that the larger grain size contributed to longer carrier lifetime and smaller carrier transport resistance, both of which are beneficial for solar cell devices. Electronic supplementary information (ESI) available: XRD patterns and statistic results of solar cell performance. See DOI: 10.1039/c5nr08935b

Size-Dependent Grain-Boundary Structure with Improved Conductive and Mechanical Stabilities in Sub-10-nm Gold Crystals

NASA Astrophysics Data System (ADS)

Wang, Chunyang; Du, Kui; Song, Kepeng; Ye, Xinglong; Qi, Lu; He, Suyun; Tang, Daiming; Lu, Ning; Jin, Haijun; Li, Feng; Ye, Hengqiang

2018-05-01

Low-angle grain boundaries generally exist in the form of dislocation arrays, while high-angle grain boundaries (misorientation angle >15 ° ) exist in the form of structural units in bulk metals. Here, through in situ atomic resolution aberration corrected electron microscopy observations, we report size-dependent grain-boundary structures improving both stabilities of electrical conductivity and mechanical properties in sub-10-nm-sized gold crystals. With the diameter of a nanocrystal decreasing below 10 nm, the high-angle grain boundary in the crystal exists as an array of dislocations. This size effect may be of importance to a new generation of interconnects applications.

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization.

PubMed

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2017-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces.

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization

PubMed Central

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2018-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces. PMID:29657884

Effects of storage time and temperature on pH, specific gravity, and crystal formation in urine samples from dogs and cats.

PubMed

Albasan, Hasan; Lulich, Jody P; Osborne, Carl A; Lekcharoensuk, Chalermpol; Ulrich, Lisa K; Carpenter, Kathleen A

2003-01-15

To determine effects of storage temperature and time on pH and specific gravity of and number and size of crystals in urine samples from dogs and cats. Randomized complete block design. 31 dogs and 8 cats. Aliquots of each urine sample were analyzed within 60 minutes of collection or after storage at room or refrigeration temperatures (20 vs 6 degrees C [68 vs 43 degrees F]) for 6 or 24 hours. Crystals formed in samples from 11 of 39 (28%) animals. Calcium oxalate (CaOx) crystals formed in vitro in samples from 1 cat and 8 dogs. Magnesium ammonium phosphate (MAP) crystals formed in vitro in samples from 2 dogs. Compared with aliquots stored at room temperature, refrigeration increased the number and size of crystals that formed in vitro; however, the increase in number and size of MAP crystals in stored urine samples was not significant. Increased storage time and decreased storage temperature were associated with a significant increase in number of CaOx crystals formed. Greater numbers of crystals formed in urine aliquots stored for 24 hours than in aliquots stored for 6 hours. Storage time and temperature did not have a significant effect on pH or specific gravity. Urine samples should be analyzed within 60 minutes of collection to minimize temperature- and time-dependent effects on in vitro crystal formation. Presence of crystals observed in stored samples should be validated by reevaluation of fresh urine.

The structure of deposited metal clusters generated by laser evaporation

NASA Astrophysics Data System (ADS)

Faust, P.; Brandstättner, M.; Ding, A.

1991-09-01

Metal clusters have been produced using a laser evaporation source. A Nd-YAG laser beam focused onto a solid silver rod was used to evaporate the material, which was then cooled to form clusters with the help of a pulsed high pressure He beam. TOF mass spectra of these clusters reveal a strong occurrence of small and medium sized clusters ( n<100). Clusters were also deposited onto grid supported thin layers of carbon-films which were investigated by transmission electron microscopy. Very high resolution pictures of these grids were used to analyze the size distribution and the structure of the deposited clusters. The diffraction pattern caused by crystalline structure of the clusters reveals 3-and 5-fold symmetries as well as fcc bulk structure. This can be explained in terms of icosahedron and cuboctahedron type clusters deposited on the surface of the carbon layer. There is strong evidence that part of these cluster geometries had already been formed before the depostion process. The non-linear dependence of the cluster size and the cluster density on the generating conditions is discussed. Therefore the samples were observed in HREM in the stable DEEKO 100 microscope of the Fritz-Haber-Institut operating at 100 KV with the spherical aberration c S =0.5 mm. The quality of the pictures was improved by using the conditions of minimum phase contrast hollow cone illumination. This procedure led to a minimum of phase contrast artefacts. Among the well-crystallized particles were a great amount of five- and three-fold symmetries, icosahedra and cuboctahedra respectively. The largest clusters with five- and three-fold symmetries have been found with diameters of 7 nm; the smallest particles displaying the same undistorted symmetries were of about 2 mm. Even smaller ones with strong distortions could be observed although their classification is difficult. The quality of the images was improved by applying Fourier filtering techniques.

Polycrystalline silicon thin-film transistors with location-controlled crystal grains fabricated by excimer laser crystallization

NASA Astrophysics Data System (ADS)

Tsai, Chun-Chien; Lee, Yao-Jen; Chiang, Ko-Yu; Wang, Jyh-Liang; Lee, I.-Che; Chen, Hsu-Hsin; Wei, Kai-Fang; Chang, Ting-Kuo; Chen, Bo-Ting; Cheng, Huang-Chung

2007-11-01

In this paper, location-controlled silicon crystal grains are fabricated by the excimer laser crystallization method which employs amorphous silicon spacer structure and prepatterned thin films. The amorphous silicon spacer in nanometer-sized width formed using spacer technology is served as seed crystal to artificially control superlateral growth phenomenon during excimer laser irradiation. An array of 1.8-μm-sized disklike silicon grains is formed, and the n-channel thin-film transistors whose channels located inside the artificially-controlled crystal grains exhibit higher performance of field-effect-mobility reaching 308cm2/Vs as compared with the conventional ones. This position-manipulated silicon grains are essential to high-performance and good uniformity devices.

Oriented attachment by enantioselective facet recognition in millimeter-sized gypsum crystals.

PubMed

Viedma, Cristóbal; Cuccia, Louis A; McTaggart, Alicia; Kahr, Bart; Martin, Alexander T; McBride, J Michael; Cintas, Pedro

2016-09-22

Crystal growth by oriented attachment involves the spontaneous self-assembly of adjoining crystals with common crystallographic orientations. Herein, we report the oriented attachment of gypsum crystals on agitation to form stereoselective mesoscale aggregates.

Finite size effects in phase transformation kinetics in thin films and surface layers

NASA Astrophysics Data System (ADS)

Trofimov, Vladimir I.; Trofimov, Ilya V.; Kim, Jong-Il

2004-02-01

In studies of phase transformation kinetics in thin films, e.g. crystallization of amorphous films, until recent time is widely used familiar Kolmogorov-Johnson-Mehl-Avrami (KJMA) statistical model of crystallization despite it is applicable only to an infinite medium. In this paper a model of transformation kinetics in thin films based on a concept of the survival probability for randomly chosen point during transformation process is presented. Two model versions: volume induced transformation (VIT) when the second-phase grains nucleate over a whole film volume and surface induced transformation (SIT) when they form on an interface with two nucleation mode: instantaneous nucleation at transformation onset and continuous one during all the process are studied. At VIT-process due to the finite film thickness effects the transformation profile has a maximum in a film middle, whereas that of the grains population reaches a minimum inhere, the grains density is always higher than in a volume material, and the thinner film the slower it transforms. The transformation kinetics in a thin film obeys a generalized KJMA equation with parameters depending on a film thickness and in limiting cases of extremely thin and thick film it reduces to classical KJMA equation for 2D- and 3D-system, respectively.

Facile synthesis of pristine graphene-palladium nanocomposites with extraordinary catalytic activities using swollen liquid crystals

NASA Astrophysics Data System (ADS)

Vats, T.; Dutt, S.; Kumar, R.; Siril, P. F.

2016-09-01

Amazing conductivity, perfect honeycomb sp2 arrangement and the high theoretical surface area make pristine graphene as one of the best materials suited for application as catalyst supports. Unfortunately, the low reactivity of the material makes the formation of nanocomposite with inorganic materials difficult. Here we report an easy approach to synthesize nanocomposites of pristine graphene with palladium (Pd-G) using swollen liquid crystals (SLCs) as a soft template. The SLC template gives the control to deposit very small Pd particles of uniform size on G as well as RGO. The synthesized nanocomposite (Pd-G) exhibited exceptionally better catalytic activity compared with Pd-RGO nanocomposite in the hydrogenation of nitrophenols and microwave assisted C-C coupling reactions. The catalytic activity of Pd-G nanocomposite during nitrophenol reduction reaction was sixteen times higher than Pd nanoparticles and more than double than Pd-RGO nanocomposite. The exceptionally high activity of pristine graphene supported catalysts in the organic reactions is explained on the basis of its better pi interacting property compared to partially reduced RGO. The Pd-G nanocomposite showed exceptional stability under the reaction conditions as it could be recycled upto a minimum of 15 cycles for the C-C coupling reactions without any loss in activity.

48 CFR 52.247-61 - F.o.b. Origin-Minimum Size of Shipments.

Code of Federal Regulations, 2011 CFR

2011-10-01

... be the highest applicable minimum weight which will result in the lowest freight rate (or per car... minimum weight, the Contractor agrees to ship such scheduled quantity in one shipment. The Contractor...

48 CFR 52.247-61 - F.o.b. Origin-Minimum Size of Shipments.

Code of Federal Regulations, 2013 CFR

2013-10-01

... be the highest applicable minimum weight which will result in the lowest freight rate (or per car... minimum weight, the Contractor agrees to ship such scheduled quantity in one shipment. The Contractor...

48 CFR 52.247-61 - F.o.b. Origin-Minimum Size of Shipments.

Code of Federal Regulations, 2014 CFR

2014-10-01

... be the highest applicable minimum weight which will result in the lowest freight rate (or per car... minimum weight, the Contractor agrees to ship such scheduled quantity in one shipment. The Contractor...

48 CFR 52.247-61 - F.o.b. Origin-Minimum Size of Shipments.

Code of Federal Regulations, 2012 CFR

2012-10-01

... be the highest applicable minimum weight which will result in the lowest freight rate (or per car... minimum weight, the Contractor agrees to ship such scheduled quantity in one shipment. The Contractor...

A Crystallization-Temperature Profile Through Paleo-Oceanic Crust (Wadi Gideah Transect, Oman Ophiolite): Application of the REE-in-Plagioclase-Clinopyroxene Partitioning Thermometer

NASA Astrophysics Data System (ADS)

Mueller, S.; Hasenclever, J.; Garbe-Schönberg, D.; Koepke, J.; Hoernle, K.

2017-12-01

The accretion mechanisms forming oceanic crust at fast spreading ridges are still under controversial discussion. Thermal, petrological, and geochemical observations predict different end-member models, i.e., the gabbro glacier and the sheeted sill model. They all bear implications for heat transport, temperature distribution, mode of crystallization and hydrothermal heat removal over crustal depth. In a typical MOR setting, temperature is the key factor driving partitioning of incompatible elements during crystallization. LA-ICP-MS data for co-genetic plagioclase and clinopyroxene in gabbros along a transect through the plutonic section of paleo-oceanic crust (Wadi Gideah Transect, Oman ophiolite) reveal that REE partitioning coefficients are relatively constant in the layered gabbro section but increase for the overlying foliated gabbros, with an enhanced offset towards HREEs. Along with a systematic enrichment of REE's with crustal height, these trends are consistent with a system dominated by in-situ crystallization for the lower gabbros and a change in crystallization mode for the upper gabbros. Sun and Liang (2017) used experimental REE partitioning data for calibrating a new REE-in-plagioclase-clinopyroxene thermometer that we used here for establishing the first crystallization-temperature depth profile through oceanic crust that facilitates a direct comparison with thermal models of crustal accretion. Our results indicate crystallization temperatures of about 1220±8°C for the layered gabbros and lower temperatures of 1175±8°C for the foliated gabbros and a thermal minimum above the layered-to-foliated gabbro transition. Our findings are consistent with a hybrid accretion model for the oceanic crust. The thermal minimum is assumed to represent a zone where the descending crystal mushes originating from the axial melt lens meet with mushes that have crystallized in situ. These results can be used to verify and test thermal models (e.g., Maclennan et al., 2004, Theissen-Krah et al., 2016) and their predictions for heat flow and temperature distribution in the crust. Maclennan, J., Hulme, T., & Singh, S. C. (2004), G3, 5(2). / Sun, C., & Liang, Y., (2017), CMP, 172(4). / Theissen-Krah, S., Rüpke, L. H., & Hasenclever, J. (2016), GRL, 43(3).

Large-volume protein crystal growth for neutron macromolecular crystallography

DOE PAGES

Ng, Joseph D.; Baird, James K.; Coates, Leighton; ...

2015-03-30

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Large-volume protein crystal growth for neutron macromolecular crystallography

PubMed Central

Ng, Joseph D.; Baird, James K.; Coates, Leighton; Garcia-Ruiz, Juan M.; Hodge, Teresa A.; Huang, Sijay

2015-01-01

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for the growth of crystals to significant dimensions that are now relevant to NMC are revisited. These include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations. PMID:25849493

Large-volume protein crystal growth for neutron macromolecular crystallography

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

Ng, Joseph D.; Baird, James K.; Coates, Leighton

Neutron macromolecular crystallography (NMC) is the prevailing method for the accurate determination of the positions of H atoms in macromolecules. As neutron sources are becoming more available to general users, finding means to optimize the growth of protein crystals to sizes suitable for NMC is extremely important. Historically, much has been learned about growing crystals for X-ray diffraction. However, owing to new-generation synchrotron X-ray facilities and sensitive detectors, protein crystal sizes as small as in the nano-range have become adequate for structure determination, lessening the necessity to grow large crystals. Here, some of the approaches, techniques and considerations for themore » growth of crystals to significant dimensions that are now relevant to NMC are revisited. We report that these include experimental strategies utilizing solubility diagrams, ripening effects, classical crystallization techniques, microgravity and theoretical considerations.« less

Lattice Boltzmann Simulation of Water Isotope Fractionation During Growth of Ice Crystals in Clouds

NASA Astrophysics Data System (ADS)

Lu, G.; Depaolo, D.; Kang, Q.; Zhang, D.

2006-12-01

The isotopic composition of precipitation, especially that of snow, plays a special role in the global hydrological cycle and in reconstruction of past climates using polar ice cores. The fractionation of the major water isotope species (HHO, HDO, HHO-18) during ice crystal formation is critical to understanding the global distribution of isotopes in precipitation. Ice crystal growth in clouds is traditionally treated with a spherically- symmetric steady state diffusion model, with semi-empirical modifications added to account for ventilation and for complex crystal morphology. Although it is known that crystal growth rate, which depends largely on the degree of vapor over-saturation, determines crystal morphology, there are no existing quantitative models that directly relate morphology to the vapor saturation factor. Since kinetic (vapor phase diffusion-controlled) isotopic fractionation also depends on growth rate, there should be a direct relationship between vapor saturation, crystal morphology, and crystal isotopic composition. We use a 2D Lattice-Boltzmann model to simulate diffusion-controlled ice crystal growth from vapor- oversaturated air. In the model, crystals grow solely according to the diffusive fluxes just above the crystal surfaces, and hence crystal morphology arises from the initial and boundary conditions in the model and does not need to be specified a priori. The input parameters needed are the isotope-dependent vapor deposition rate constant (k) and the water vapor diffusivity in air (D). The values of both k and D can be computed from kinetic theory, and there are also experimentally determined values of D. The deduced values of k are uncertain to the extent that the sticking coefficient (or accommodation coefficient) for ice is uncertain. The ratio D/k is a length that determines the minimum scale of dendritic growth features and allows us to scale the numerical calculations to atmospheric conditions using a dimensionless Damkohler number: Da = kh/D, where h is the width of the 2D calculation domain. Varying the nondimensional Da in the model is equivalent to varying the scale (h) in the model. Our calculations confirm that the crystal/vapor isotopic fractionation approaches the equilibrium value, and the crystals are compact (circular in 2D) as the saturation factor approaches unity (S= 1.0). At higher oversaturation (e.g. S = 1.2), dendritic crystals of millimeter size develop on timescales appropriate to cloud processes, the isotopic fractionations are dominated by kinetic effects, and similar to those predicted by the spherical diffusion model. Dendritic crystals are constrained to be relatively large, with dimension much greater than D/k. The most difficult aspect of the modeling is to account for the large density difference between air and ice, which requires us to use a fictitious higher density for the vapor-oversaturated air and scale the crystal growth time accordingly. A different approach, using a larger scale simulation to derive boundary conditions for a nested smaller scale calculation is in progress. The results to date clarify the controls on dendritic crystal growth, the relationships between saturation state, growth rate, crystal morphology and isotopic fractionation, and provide limits on the value of the accommodation coefficient.

Generalized variational approach to Kim-Gordon electron gas theory for ionic crystals

NASA Astrophysics Data System (ADS)

Ivanov, O. V.; Maksimov, E. G.

1996-01-01

The generalized approach to the Kim-Gordon electron gas model is proposed. The total density of a crystal is considered as a superposition of densities of individual overlapping ions. The possible distortions of individual ion densities are calculated in the presence of some auxiliary external potentials. The real values of these distortions are calculated by a variational method from the minimum total energy of a crystal. The proper prescription of the ion self-energy with a distorted density is given using the method elaborated in the nonequilibrium thermodynamics. Some examples of the calculation for phonon frequencies are presented and demonstrate a good agreement with experimental data.

Laser-induced ferroelectric domain engineering in LiNbO3 crystals using an amorphous silicon overlayer

NASA Astrophysics Data System (ADS)

Zisis, G.; Martinez-Jimenez, G.; Franz, Y.; Healy, N.; Masaud, T. M.; Chong, H. M. H.; Soergel, E.; Peacock, A. C.; Mailis, S.

2017-08-01

We report laser-induced poling inhibition and direct poling in lithium niobate crystals (LiNbO3), covered with an amorphous silicon (a-Si) light-absorbing layer, using a visible (488 nm) continuous wave laser source. Our results show that the use of the a-Si overlayer produces deeper poling inhibited domains with minimum surface damage, as compared to previously reported UV laser writing experiments on uncoated crystals, thus increasing the applicability of this method in the production of ferroelectric domain engineered structures for nonlinear optical applications. The characteristics of the poling inhibited domains were investigated using differential etching and piezoresponse force microscopy.

Exploratory Factor Analysis with Small Sample Sizes

ERIC Educational Resources Information Center

de Winter, J. C. F.; Dodou, D.; Wieringa, P. A.

2009-01-01

Exploratory factor analysis (EFA) is generally regarded as a technique for large sample sizes ("N"), with N = 50 as a reasonable absolute minimum. This study offers a comprehensive overview of the conditions in which EFA can yield good quality results for "N" below 50. Simulations were carried out to estimate the minimum required "N" for different…

46 CFR 111.60-4 - Minimum cable conductor size.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 46 Shipping 4 2012-10-01 2012-10-01 false Minimum cable conductor size. 111.60-4 Section 111.60-4 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) ELECTRICAL ENGINEERING ELECTRIC SYSTEMS... conductor must be #18 AWG (0.82 mm2) or larger except— (a) Each power and lighting cable conductor must be...

46 CFR 111.60-4 - Minimum cable conductor size.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 46 Shipping 4 2013-10-01 2013-10-01 false Minimum cable conductor size. 111.60-4 Section 111.60-4 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) ELECTRICAL ENGINEERING ELECTRIC SYSTEMS... conductor must be #18 AWG (0.82 mm2) or larger except— (a) Each power and lighting cable conductor must be...

46 CFR 111.60-4 - Minimum cable conductor size.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 46 Shipping 4 2014-10-01 2014-10-01 false Minimum cable conductor size. 111.60-4 Section 111.60-4 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) ELECTRICAL ENGINEERING ELECTRIC SYSTEMS... conductor must be #18 AWG (0.82 mm2) or larger except— (a) Each power and lighting cable conductor must be...

7 CFR 51.1995 - U.S. No. 1.

Code of Federal Regulations, 2012 CFR

2012-01-01

...) Well formed; and, (2) Clean and bright. (3) Free from: (i) Blanks; and, (ii) Broken or split shells. (4... minimum diameter, minimum and maximum diameters, or in accordance with one of the size classifications in Table I. Table I Size classifications Maximum size—Will pass through a round opening of the following...

78 FR 52079 - Oranges, Grapefruit, Tangerines, and Tangelos Grown in Florida; Relaxing Size and Grade...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-08-22

... Requirements on Valencia and Other Late Type Oranges AGENCY: Agricultural Marketing Service, USDA. ACTION...). The interim rule reduced the minimum size for Valencia and other late type oranges shipped to... interim rule also lowered the minimum grade for Valencia and other late type oranges shipped to interstate...

78 FR 28115 - Oranges, Grapefruit, Tangerines, and Tangelos Grown in Florida; Relaxing Size and Grade...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-05-14

... Requirements on Valencia and Other Late Type Oranges AGENCY: Agricultural Marketing Service, USDA. ACTION...). This rule reduces the minimum size requirement for Valencia and other late type oranges shipped to... also reduces the minimum grade requirement for Valencia and other late type oranges shipped to...

76 FR 37867 - Self-Regulatory Organizations; Chicago Board Options Exchange, Incorporated; Order Approving...

Federal Register 2010, 2011, 2012, 2013, 2014

2011-06-28

..., as Modified by Amendment No. 1, to Reduce the Minimum Size of the Nominating and Governance Committee... proposed rule change to reduce the minimum size of the Nominating and Governance Committee (``NGC'') from... the original proposed rule change, it had not yet obtained formal approval from its Board of Directors...

7 CFR 51.2113 - Size requirements.

Code of Federal Regulations, 2010 CFR

2010-01-01

... of range in count of whole almond kernels per ounce or in terms of minimum, or minimum and maximum diameter. When a range in count is specified, the whole kernels shall be fairly uniform in size, and the average count per ounce shall be within the range specified. Doubles and broken kernels shall not be used...

The Nucleation and Growth of Protein Crystals

NASA Technical Reports Server (NTRS)

Pusey, Marc

2004-01-01

Obtaining crystals of suitable size and high quality continues to be a major bottleneck in macromolecular crystallography. Currently, structural genomics efforts are achieving on average about a 10% success rate in going from purified protein to a deposited crystal structure. Growth of crystals in microgravity was proposed as a means of overcoming size and quality problems, which subsequently led to a major NASA effort in microgravity crystal growth, with the agency also funding research into understanding the process. Studies of the macromolecule crystal nucleation and growth process were carried out in a number of labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. Based upon experimental evidence, as well as simple starting assumptions, we have proposed that crystal nucleation occurs by a series of discrete self assembly steps, which 'set' the underlying crystal symmetry. This talk will review the model developed, and its origins, in our laboratory for how crystals nucleate and grow, and will then present, along with preliminary data, how we propose to use this model to improve the success rate for obtaining crystals from a given protein.

Effect of polyglycerol esters additive on palm oil crystallization using focused beam reflectance measurement and differential scanning calorimetry.

PubMed

Saw, M H; Hishamuddin, E; Chong, C L; Yeoh, C B; Lim, W H

2017-01-01

The effect of 0.1-0.7% (w/w) of polyglycerol esters (PGEmix-8) on palm oil crystallization was studied using focused beam reflectance measurement (FBRM) to analyze the in-line changes of crystal size distribution during the crystallization. FBRM results show that 0.1-0.5% (w/w) of PGEmix-8 did not significantly affect nucleation but slightly retarded crystal growth. The use of 0.7% (w/w) additive showed greater heterogeneous nucleation compared to those with lower dosages of additive. Crystal growth was also greatly reduced when using 0.7% (w/w) dosage. The morphological study indicated that the palm oil crystals were smaller and more even in size than when more additive was added. Isothermal crystallization studies using differential scanning calorimetry (DSC) showed increased inhibitory effects on palm oil crystal growth with increasing concentration of PGEmix-8. These results imply that PGEmix-8 is a nucleation enhancing and crystal growth retarding additive in palm oil crystallization at 0.7% (w/w) dosage. Copyright © 2016 The Author(s). Published by Elsevier Ltd.. All rights reserved.

Improved reproducibility of unit-cell parameters in macromolecular cryocrystallography by limiting dehydration during crystal mounting.

PubMed

Farley, Christopher; Burks, Geoffry; Siegert, Thomas; Juers, Douglas H

2014-08-01

In macromolecular cryocrystallography unit-cell parameters can have low reproducibility, limiting the effectiveness of combining data sets from multiple crystals and inhibiting the development of defined repeatable cooling protocols. Here, potential sources of unit-cell variation are investigated and crystal dehydration during loop-mounting is found to be an important factor. The amount of water lost by the unit cell depends on the crystal size, the loop size, the ambient relative humidity and the transfer distance to the cooling medium. To limit water loss during crystal mounting, a threefold strategy has been implemented. Firstly, crystal manipulations are performed in a humid environment similar to the humidity of the crystal-growth or soaking solution. Secondly, the looped crystal is transferred to a vial containing a small amount of the crystal soaking solution. Upon loop transfer, the vial is sealed, which allows transport of the crystal at its equilibrated humidity. Thirdly, the crystal loop is directly mounted from the vial into the cold gas stream. This strategy minimizes the exposure of the crystal to relatively low humidity ambient air, improves the reproducibility of low-temperature unit-cell parameters and offers some new approaches to crystal handling and cryoprotection.

Improved reproducibility of unit-cell parameters in macromolecular cryocrystallography by limiting dehydration during crystal mounting

PubMed Central

Farley, Christopher; Burks, Geoffry; Siegert, Thomas; Juers, Douglas H.

2014-01-01

In macromolecular cryocrystallography unit-cell parameters can have low reproducibility, limiting the effectiveness of combining data sets from multiple crystals and inhibiting the development of defined repeatable cooling protocols. Here, potential sources of unit-cell variation are investigated and crystal dehydration during loop-mounting is found to be an important factor. The amount of water lost by the unit cell depends on the crystal size, the loop size, the ambient relative humidity and the transfer distance to the cooling medium. To limit water loss during crystal mounting, a threefold strategy has been implemented. Firstly, crystal manipulations are performed in a humid environment similar to the humidity of the crystal-growth or soaking solution. Secondly, the looped crystal is transferred to a vial containing a small amount of the crystal soaking solution. Upon loop transfer, the vial is sealed, which allows transport of the crystal at its equilibrated humidity. Thirdly, the crystal loop is directly mounted from the vial into the cold gas stream. This strategy minimizes the exposure of the crystal to relatively low humidity ambient air, improves the reproducibility of low-temperature unit-cell parameters and offers some new approaches to crystal handling and cryoprotection. PMID:25084331

Exchange-Hole Dipole Dispersion Model for Accurate Energy Ranking in Molecular Crystal Structure Prediction II: Nonplanar Molecules.

PubMed

Whittleton, Sarah R; Otero-de-la-Roza, A; Johnson, Erin R

2017-11-14

The crystal structure prediction (CSP) of a given compound from its molecular diagram is a fundamental challenge in computational chemistry with implications in relevant technological fields. A key component of CSP is the method to calculate the lattice energy of a crystal, which allows the ranking of candidate structures. This work is the second part of our investigation to assess the potential of the exchange-hole dipole moment (XDM) dispersion model for crystal structure prediction. In this article, we study the relatively large, nonplanar, mostly flexible molecules in the first five blind tests held by the Cambridge Crystallographic Data Centre. Four of the seven experimental structures are predicted as the energy minimum, and thermal effects are demonstrated to have a large impact on the ranking of at least another compound. As in the first part of this series, delocalization error affects the results for a single crystal (compound X), in this case by detrimentally overstabilizing the π-conjugated conformation of the monomer. Overall, B86bPBE-XDM correctly predicts 16 of the 21 compounds in the five blind tests, a result similar to the one obtained using the best CSP method available to date (dispersion-corrected PW91 by Neumann et al.). Perhaps more importantly, the systems for which B86bPBE-XDM fails to predict the experimental structure as the energy minimum are mostly the same as with Neumann's method, which suggests that similar difficulties (absence of vibrational free energy corrections, delocalization error,...) are not limited to B86bPBE-XDM but affect GGA-based DFT-methods in general. Our work confirms B86bPBE-XDM as an excellent option for crystal energy ranking in CSP and offers a guide to identify crystals (organic salts, conjugated flexible systems) where difficulties may appear.

Trophy Hunting and Sustainability: Temporal Dynamics in Trophy Quality and Harvesting Patterns of Wild Herbivores in a Tropical Semi-Arid Savanna Ecosystem.

PubMed

Muposhi, Victor K; Gandiwa, Edson; Bartels, Paul; Makuza, Stanley M; Madiri, Tinaapi H

2016-01-01

The selective nature of trophy hunting may cause changes in desirable phenotypic traits in harvested species. A decline in trophy size of preferred species may reduce hunting destination competitiveness thus compromising the sustainability of trophy hunting as a conservation tool. We explored the trophy quality and trends in harvesting patterns (i.e., 2004-2015) of Cape buffalo (Syncerus caffer), African elephant (Loxodonta africana), greater kudu (Tragelaphus strepsiceros) and sable (Hippotragus niger) in Matetsi Safari Area, northwest Zimbabwe. We used long-term data on horn and tusk size, age, quota size allocation and offtake levels of selected species. To analyse the effect of year, area and age on the trophy size, quota size and offtake levels, we used linear mixed models. One sample t-test was used to compare observed trophy size with Safari Club International (SCI) minimum score. Trophy sizes for Cape buffalo and African elephant were below the SCI minimum score. Greater kudu trophy sizes were within the minimum score threshold whereas sable trophy sizes were above the SCI minimum score between 2004 and 2015. Age at harvest for Cape buffalo, kudu and sable increased whilst that of elephant remained constant between 2004 and 2015. Quota size allocated for buffalo and the corresponding offtake levels declined over time. Offtake levels of African elephant and Greater kudu declined whilst the quota size did not change between 2004 and 2015. The quota size for sable increased whilst the offtake levels fluctuated without changing for the period 2004-2015. The trophy size and harvesting patterns in these species pose a conservation and management dilemma on the sustainability of trophy hunting in this area. We recommend: (1) temporal and spatial rotational resting of hunting areas to create refuge to improve trophy quality and maintenance of genetic diversity, and (2) introduction of variable trophy fee pricing system based on trophy size.

Structural transformation of crystallized debranched cassava starch during dual hydrothermal treatment in relation to enzyme digestibility.

PubMed

Boonna, Sureeporn; Tongta, Sunanta

2018-07-01

Structural transformation of crystallized debranched cassava starch prepared by temperature cycling (TC) treatment and then subjected to annealing (ANN), heat-moisture treatment (HMT) and dual hydrothermal treatments of ANN and HMT was investigated. The relative crystallinity, lateral crystal size, melting temperature and resistant starch (RS) content increased for all hydrothermally treated samples, but the slowly digestible starch (SDS) content decreased. The RS content followed the order: HMT → ANN > HMT > ANN → HMT > ANN > TC, respectively. The HMT → ANN sample showed a larger lateral crystal size with more homogeneity, whereas the ANN → HMT sample had a smaller lateral crystal size with a higher melting temperature. After cooking at 50% moisture, the increased RS content of samples was observed, particularly for the ANN → HMT sample. These results suggest that structural changes of crystallized debranched starch during hydrothermal treatments depend on initial crystalline characteristics and treatment sequences, influencing thermal stability, enzyme digestibility, and cooking stability. Copyright © 2018 Elsevier Ltd. All rights reserved.

Analysis of stochastic crystallization in micron-sized droplets of undercooled liquid l-arabitol.

PubMed

Guinet, Yannick; Carpentier, Laurent; Paccou, Laurent; Derollez, Patrick; Hédoux, Alain

2016-11-29

Kinetics of isothermal crystallization of l-arabitol were analyzed from the undercooled liquid state within micron-sized droplets from micro-Raman spectroscopy. This study reveals that crystallization slightly above T g is controlled by stochastic heterogeneous nucleation inherent to the droplet size. Microscopic Raman investigations performed in droplets give the unique opportunity to analyze the pure metastable Form II of l-arabitol. It was found that Form II is characterized by a molecular packing more compact than that of the stable Form I, inherent to strong intermolecular hydrogen bonding. Kinetics laws obtained by analyzing several droplets at different temperatures, reveal the transient character of Form II, quasi systematically detected during the crystallization process of form I. Form II appears as the first step of crystallization prior to successive short-living metastable states which is necessary to achieve a complete crystallization in Form I. It was found that the kinetics of conversion between the metastable states (Form II) into Form I is dependent on the amount of strong hydrogen bonding distinctive of Form II. Copyright © 2016 Elsevier Ltd. All rights reserved.

Relation Between Inflammables and Ignition Sources in Aircraft Environments

NASA Technical Reports Server (NTRS)

Scull, Wilfred E

1950-01-01

A literature survey was conducted to determine the relation between aircraft ignition sources and inflammables. Available literature applicable to the problem of aircraft fire hazards is analyzed and, discussed herein. Data pertaining to the effect of many variables on ignition temperatures, minimum ignition pressures, and minimum spark-ignition energies of inflammables, quenching distances of electrode configurations, and size of openings incapable of flame propagation are presented and discussed. The ignition temperatures and the limits of inflammability of gasoline in air in different test environments, and the minimum ignition pressure and the minimum size of openings for flame propagation of gasoline - air mixtures are included. Inerting of gasoline - air mixtures is discussed.

Biodiversity and body size are linked across metazoans

PubMed Central

McClain, Craig R.; Boyer, Alison G.

2009-01-01

Body size variation across the Metazoa is immense, encompassing 17 orders of magnitude in biovolume. Factors driving this extreme diversification in size and the consequences of size variation for biological processes remain poorly resolved. Species diversity is invoked as both a predictor and a result of size variation, and theory predicts a strong correlation between the two. However, evidence has been presented both supporting and contradicting such a relationship. Here, we use a new comprehensive dataset for maximum and minimum body sizes across all metazoan phyla to show that species diversity is strongly correlated with minimum size, maximum size and consequently intra-phylum variation. Similar patterns are also observed within birds and mammals. The observations point to several fundamental linkages between species diversification and body size variation through the evolution of animal life. PMID:19324730

Crystallization in a model glass: Influence of the boundary conditions

NASA Astrophysics Data System (ADS)

Jund, P.; Jullien, R.

1998-06-01

Using molecular dynamics calculations and the Voronoï tessellation, we study the evolution of the local structure of a soft-sphere glass vs. temperature starting from the liquid phase at different quenching rates. This study is done for different sizes and for two different boundary conditions, namely the usual cubic periodic boundary conditions and the isotropic hyperspherical boundary conditions for which the particles evolve on the surface of a hypersphere in four dimensions. Our results show that for small system sizes, crystallization can indeed be induced by the cubic boundary conditions. On the other hand, we show that finite-size effects are more pronounced on the hypersphere and that crystallization is artificially inhibited even for large system sizes.

Coupled crystal orientation-size effects on the strength of nano crystals

PubMed Central

Yuan, Rui; Beyerlein, Irene J.; Zhou, Caizhi

2016-01-01

We study the combined effects of grain size and texture on the strength of nanocrystalline copper (Cu) and nickel (Ni) using a crystal-plasticity based mechanics model. Within the model, slip occurs in discrete slip events exclusively by individual dislocations emitted statistically from the grain boundaries. We show that a Hall-Petch relationship emerges in both initially texture and non-textured materials and our values are in agreement with experimental measurements from numerous studies. We find that the Hall-Petch slope increases with texture strength, indicating that preferred orientations intensify the enhancements in strength that accompany grain size reductions. These findings reveal that texture is too influential to be neglected when analyzing and engineering grain size effects for increasing nanomaterial strength. PMID:27185364

Scaling laws and size effects for amorphous crystallization kinetics: Constraints imposed by nucleation and growth specificities.

PubMed

Descamps, Marc; Willart, Jean-François

2018-05-05

In the present paper we review different aspects of the crystallization of amorphous compounds in relation to specificities of the nucleation and growth rates. Its main purpose is: i) to underline the interest of a scaling analysis of recrystallization kinetics to identify similarities or disparities of experimental kinetic regimes. ii) to highlight the intrinsic link between the nucleation rate and growth rate with a temperature dependent characteristic transformation time τ(T), and a characteristic size ξ(T). The consequences on the influence of the sample size on kinetics of crystallization is considered. The significance of size effect and confinement for amorphous stabilization in the pharmaceutical sciences is discussed. Copyright © 2018. Published by Elsevier B.V.

LDPC Codes with Minimum Distance Proportional to Block Size

NASA Technical Reports Server (NTRS)

Divsalar, Dariush; Jones, Christopher; Dolinar, Samuel; Thorpe, Jeremy

2009-01-01

Low-density parity-check (LDPC) codes characterized by minimum Hamming distances proportional to block sizes have been demonstrated. Like the codes mentioned in the immediately preceding article, the present codes are error-correcting codes suitable for use in a variety of wireless data-communication systems that include noisy channels. The previously mentioned codes have low decoding thresholds and reasonably low error floors. However, the minimum Hamming distances of those codes do not grow linearly with code-block sizes. Codes that have this minimum-distance property exhibit very low error floors. Examples of such codes include regular LDPC codes with variable degrees of at least 3. Unfortunately, the decoding thresholds of regular LDPC codes are high. Hence, there is a need for LDPC codes characterized by both low decoding thresholds and, in order to obtain acceptably low error floors, minimum Hamming distances that are proportional to code-block sizes. The present codes were developed to satisfy this need. The minimum Hamming distances of the present codes have been shown, through consideration of ensemble-average weight enumerators, to be proportional to code block sizes. As in the cases of irregular ensembles, the properties of these codes are sensitive to the proportion of degree-2 variable nodes. A code having too few such nodes tends to have an iterative decoding threshold that is far from the capacity threshold. A code having too many such nodes tends not to exhibit a minimum distance that is proportional to block size. Results of computational simulations have shown that the decoding thresholds of codes of the present type are lower than those of regular LDPC codes. Included in the simulations were a few examples from a family of codes characterized by rates ranging from low to high and by thresholds that adhere closely to their respective channel capacity thresholds; the simulation results from these examples showed that the codes in question have low error floors as well as low decoding thresholds. As an example, the illustration shows the protograph (which represents the blueprint for overall construction) of one proposed code family for code rates greater than or equal to 1.2. Any size LDPC code can be obtained by copying the protograph structure N times, then permuting the edges. The illustration also provides Field Programmable Gate Array (FPGA) hardware performance simulations for this code family. In addition, the illustration provides minimum signal-to-noise ratios (Eb/No) in decibels (decoding thresholds) to achieve zero error rates as the code block size goes to infinity for various code rates. In comparison with the codes mentioned in the preceding article, these codes have slightly higher decoding thresholds.

The Effect of Temperature and Solution pH on Tetragonal Lysozyme Nucleation Kinetics

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Jacobs, Randolph S.; Frazier, Tyralynn; Snell, Edward H.; Pusey, Marc L.

1998-01-01

Part of the challenge of macromolecular crystal growth for structure determination is obtaining an appropriate number of crystals with a crystal volume suitable for x-ray analysis. In this respect an understanding of the effect of solution conditions on macromolecule nucleation rates is advantageous. This study investigated the effects of supersaturation, temperature and pH on the nucleation rate of tetragonal lysozyme crystals. Batch crystallization plates were prepared at given solution concentrations and incubated at set temperatures over one week. The number of crystals per well with their size and axial ratios were recorded and correlated with solution conditions, Duplicate experiments indicate the reproducibility of the technique, Crystal numbers were found to increase with increasing supersaturation and temperature. The most significant variable however, was pH, where crystal numbers changed by two orders of magnitude over the pH range 4.0 to 5.2. Crystal size varied also with solution conditions, with the largest crystals being obtained at pH 5.2. Having optimized the crystallization conditions, a batch of crystals were prepared under exactly the same conditions and fifty of these crystals were analyzed by x-ray techniques. The results indicate that even under the same crystallization conditions, a marked variation in crystal properties exists.

Magneto-optical properties of biogenic photonic crystals in algae

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

Iwasaka, M., E-mail: iwasaka-m@umin.ac.jp; Japan Science and Technology Agency, PRESTO, 4-1-8 Honcho, Kawaguchi 332-0012 Saitama; Mizukawa, Y.

In the present study, the effects of strong static magnetic fields on the structural colors of the cell covering crystals on a microalgae, coccolithophore, were investigated. The coccolithophore, Emiliania huxleyi, generates a precise assembly of calcite crystals called coccoliths by biomineralization. The coccoliths attached to the cells exhibited structural colors under side light illumination, and the colors underwent dynamic transitions when the magnetic fields were changed between 0 T and 5 T, probably due to diamagnetically induced changes of their inclination under the magnetic fields. The specific light-scattering property of individual coccoliths separated from the cells was also observed. Light scattering frommore » a condensed suspension of coccoliths drastically decreased when magnetic fields of more than 4 T were applied parallel to the direction of observation. The magnetically aligned cell-covering crystals of the coccolithophores exhibited the properties of both a photonic crystal and a minimum micromirror.« less

Actinide/beryllium neutron sources with reduced dispersion characteristics

DOEpatents

Schulte, Louis D.

2012-08-14

Neutron source comprising a composite, said composite comprising crystals comprising BeO and AmBe.sub.13, and an excess of beryllium, wherein the crystals have an average size of less than 2 microns; the size distribution of the crystals is less than 2 microns; and the beryllium is present in a 7-fold to a 75-fold excess by weight of the amount of AmBe.sub.13; and methods of making thereof.

Controlling ZIF-67 crystals formation through various cobalt sources in aqueous solution

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

Guo, Xiangli; Jiangsu Key Laboratory of Advanced Metallic Materials, Nanjing 211189; Xing, Tiantian

2016-03-15

Zeolitic imidazolate frameworks ZIF-67 were prepared under hydrothermal (120 °C) and non-hydrothermal (room temperature) from various cobalt sources and 2-methylimidazolate (Hmim) in aqueous solution within 30 min. The particle size and morphology were found to be related to the reactivity of the cobalt salt, Hmim/Co{sup 2+} molar ratios and experimental condition. Using Co(NO{sub 3}){sub 2} as cobalt source, small-sized ZIF-67 crystals with agglomeration were formed. For CoCl{sub 2}, small-sized rhombic dodecahedron were obtained. While large-sized crystals of rhombic dodecahedron structure were obtained from CoSO{sub 4} and Co(OAc){sub 2}. Under hydrothermal condition, the size of ZIF-67 crystals tended to be moremore » uniform and the morphology were more regular comparing to non-hydrothermal condition. This study provides a simple way to control the size and morphology of ZIF-67 crystals prepared in aqueous solution. - Graphical abstract: Zeolitic imidazolate frameworks ZIF-67 were prepared under hydrothermal (120 °C) and non-hydrothermal (room temperature) from four different cobalt sources (Co(NO{sub 3}){sub 2}, CoCl{sub 2}, CoSO{sub 4} and Co(OAc){sub 2}) in aqueous solution within 30 min. The particle size and morphology were found to be related to the reactivity of the cobalt salt, Hmim/Co{sup 2+} molar ratios and experimental condition. - Highlights: • The particle size and morphology were determined by the reactivity of cobalt salt. • ZIF-67 could be prepared from CoSO{sub 4} and Co(OAc){sub 2} at Hmim/Co{sup 2+} molar ratio of 10. • Uniform and regular particles were obtained under hydrothermal condition.« less

The Minimum Binding Energy and Size of Doubly Muonic D3 Molecule

NASA Astrophysics Data System (ADS)

Eskandari, M. R.; Faghihi, F.; Mahdavi, M.

The minimum energy and size of doubly muonic D3 molecule, which two of the electrons are replaced by the much heavier muons, are calculated by the well-known variational method. The calculations show that the system possesses two minimum positions, one at typically muonic distance and the second at the atomic distance. It is shown that at the muonic distance, the effective charge, zeff is 2.9. We assumed a symmetric planar vibrational model between two minima and an oscillation potential energy is approximated in this region.

Voltage controlled oscillator is easily aligned, has low phase noise

NASA Technical Reports Server (NTRS)

Sydnor, R. L.

1965-01-01

Voltage Controlled Oscillator /VCO/, represented by an equivalent RF circuit, is easily adjusted for optimum performance by varying the circuit parameter. It contains a crystal drive level which is also easily adjusted to obtain minimum phase noise.

Artistic Crystal Creations

ERIC Educational Resources Information Center

Lange, Catherine

2008-01-01

In this inquiry-based, integrative art and science activity, Grade 5-8 students use multicolored Epsom salt (magnesium sulfate) crystallizing solutions to reveal beautiful, cylindrical, 3-dimensional, needle-shaped structures. Through observations of the crystal art, students analyze factors that contribute to crystal size and formation, compare…

Effect of Cooling Rates on Shape and Crystal Size Distributions of Mefenamic Acid Polymorph in Ethyl Acetate

NASA Astrophysics Data System (ADS)

Mudalip, S. K. Abdul; Adam, F.; Parveen, J.; Abu Bakar, M. R.; Amran, N.; Sulaiman, S. Z.; Che Man, R.; Arshad, Z. I. Mohd; Shaarani, S. Md.

2017-06-01

This study investigate the effect of cooling rates on mefenamic acid crystallisation in ethyl acetate. The cooling rate was varied from 0.2 to 5 °C/min. The in-line conductivity system and turbidity system were employed to detect the onset of the crystallization process. The crystals produced were analysed using optical microscopy and Fourier transform infrared spectroscopy (FTIR). It was found that the crystals produced at different cooling rates were needle-like and exhibit polymorphic form type I. However, the aspect ratio and crystal size distributions were varied with the increased of cooling rate. A high crystals aspect ratio and narrower CSD (100-900 μm) was obtained at cooling rate of 0.5 °C/min. Thus, can be suggested as the most suitable cooling rate for crystallization of mefenamic acid in ethyl acetate.

Solid-liquid surface tensions of critical nuclei and nucleation barriers from a phase-field-crystal study of a model binary alloy using finite system sizes.

PubMed

Choudhary, Muhammad Ajmal; Kundin, Julia; Emmerich, Heike; Oettel, Martin

2014-08-01

Phase-field-crystal (PFC) modeling has emerged as a computationally efficient tool to address crystal growth phenomena on atomistic length and diffusive time scales. We use a two-dimensional phase-field-crystal model for a binary system based on Elder et al. [Phys. Rev. B 75, 064107 (2007)] to study critical nuclei and their liquid-solid phase boundaries, in particular the nucleus size dependence of the liquid-solid interface tension as well as of the nucleation barrier. Critical nuclei are stabilized in finite systems of various sizes, however, the extracted interface tension as function of the nucleus radius r is independent of system size. We suggest a phenomenological expression to describe the dependence of the extracted interface tension on the nucleus radius r for the liquid-solid system. Moreover, the numerical PFC results show that this dependency can not be fully described by the nonclassical Tolman formula.

The effect of impurity on temperature variations in the refractive indices and thickness of TGS crystals

NASA Astrophysics Data System (ADS)

Stadnyk, V. Yo.; Andriyevsky, B. V.; Gaba, V. M.; Kogut, Z. A.

2016-06-01

Temperature dependences of optical path difference δΔi and the relative changes in thickness δ l i/ l of TGS crystals doped with L-valine are studied. Temperature dependences of the relative changes in refractive indices δ n i/( n-1) are calculated. The anisotropy coefficients of refractive indices An-1(T) and linear expansion Aα(T) are calculated, and a characteristic minimum of these dependences is found near the phase transition temperature.

Low loss fusion splicing polarization-maintaining photonic crystal fiber and conventional polarization-maintaining fiber

NASA Astrophysics Data System (ADS)

Zuoming, Sun; Ningfang, Song; Jing, Jin; Jingming, Song; Pan, Ma

2012-12-01

An efficient and simple method of fusion splicing of a Polarization-Maintaining Photonic Crystal Fiber (PM-PCF) and a conventional Polarization-Maintaining Fiber (PMF) with a low loss of 0.65 dB in experiment is reported. The minimum bending diameter of the joint can reach 2 cm. Theoretical calculation of the splicing loss based on mode field diameters (MFDs) mismatch of the two kinds of fibers is given. All parameters affected the splicing loss were studied.

77 FR 23770 - Self-Regulatory Organizations; Financial Industry Regulatory Authority, Inc.; Notice of Filing of...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-04-20

... to Proposed Rule Change To Amend FINRA Rule 6433 (Minimum Quotation Size Requirements for OTC Equity... proposed rule change to amend FINRA Rule 6433 (Minimum Quotation Size Requirements for OTC Equity... investors, three from an inter-dealer quotation system and two from a member firm.\\4\\ FINRA responded to...

50 CFR 648.104 - Summer flounder minimum fish sizes.

Code of Federal Regulations, 2012 CFR

2012-10-01

....99 cm) TL for all vessels that do not qualify for a moratorium permit under § 648.4(a)(3), and... (commercial) permitted vessels. The minimum size for summer flounder is 14 inches (35.6 cm) TL for all vessels issued a moratorium permit under § 648.4(a)(3), except on board party and charter boats carrying...

50 CFR 648.104 - Summer flounder minimum fish sizes.

Code of Federal Regulations, 2013 CFR

2013-10-01

... cm) TL for all vessels that do not qualify for a moratorium permit under § 648.4(a)(3), and charter... (commercial) permitted vessels. The minimum size for summer flounder is 14 inches (35.6 cm) TL for all vessels issued a moratorium permit under § 648.4(a)(3), except on board party and charter boats carrying...

50 CFR 648.104 - Summer flounder minimum fish sizes.

Code of Federal Regulations, 2014 CFR

2014-10-01

... cm) TL for all vessels that do not qualify for a moratorium permit under § 648.4(a)(3), and charter... (commercial) permitted vessels. The minimum size for summer flounder is 14 inches (35.6 cm) TL for all vessels issued a moratorium permit under § 648.4(a)(3), except on board party and charter boats carrying...

Deducing growth mechanisms for minerals from the shapes of crystal size distributions

USGS Publications Warehouse

Eberl, D.D.; Drits, V.A.; Srodon, J.

1998-01-01

Crystal size distributions (CSDs) of natural and synthetic samples are observed to have several distinct and different shapes. We have simulated these CSDs using three simple equations: the Law of Proportionate Effect (LPE), a mass balance equation, and equations for Ostwald ripening. The following crystal growth mechanisms are simulated using these equations and their modifications: (1) continuous nucleation and growth in an open system, during which crystals nucleate at either a constant, decaying, or accelerating nucleation rate, and then grow according to the LPE; (2) surface-controlled growth in an open system, during which crystals grow with an essentially unlimited supply of nutrients according to the LPE; (3) supply-controlled growth in an open system, during which crystals grow with a specified, limited supply of nutrients according to the LPE; (4) supply- or surface-controlled Ostwald ripening in a closed system, during which the relative rate of crystal dissolution and growth is controlled by differences in specific surface area and by diffusion rate; and (5) supply-controlled random ripening in a closed system, during which the rate of crystal dissolution and growth is random with respect to specific surface area. Each of these mechanisms affects the shapes of CSDs. For example, mechanism (1) above with a constant nucleation rate yields asymptotically-shaped CSDs for which the variance of the natural logarithms of the crystal sizes (??2) increases exponentially with the mean of the natural logarithms of the sizes (??). Mechanism (2) yields lognormally-shaped CSDs, for which ??2 increases linearly with ??, whereas mechanisms (3) and (5) do not change the shapes of CSDs, with ??2 remaining constant with increasing ??. During supply-controlled Ostwald ripening (4), initial lognormally-shaped CSDs become more symmetric, with ??2 decreasing with increasing ??. Thus, crystal growth mechanisms often can be deduced by noting trends in ?? versus ??2 of CSDs for a series of related samples.

Biomolecular crystals for material applications and a mechanistic study of an iron oxide nanoparticle synthesis

NASA Astrophysics Data System (ADS)

Falkner, Joshua Charles

The three projects within this work address the difficulties of controlling biomolecular crystal formats (i.e. size and shape), producing 3-D ordered composite materials from biomolecular crystal templates, and understanding the mechanism of a practical iron oxide synthesis. The unifying thread consistent throughout these three topics is the development of methods to manipulate nanomaterials using a bottom-up approach. Biomolecular crystals are nanometer to millimeter sized crystals that have well ordered mesoporous solvent channels. The overall physical dimensions of these crystals are highly dependent on crystallization conditions. The controlled growth of micro- and nanoprotein crystals was studied to provide new pathways for creating smaller crystalline protein materials. This method produced tetragonal hen egg-white lysozyme crystals (250--100,000 nm) with near monodisperse size distributions (<15%). With this degree of control, existing protein crystal applications such as drug delivery and analytical sensors can reach their full potential. Applications for larger crystals with inherently ubiquitous pore structures could extend to materials used for membranes or templates. In this work, the porous structure of larger cowpea mosaic virus crystals was used to template metal nanoparticle growth within the body centered cubic crystalline network. The final composite material was found to have long range ordering of palladium and platinum nonocrystal aggregates (10nm) with symmetry consistent to the virus template. Nanoparticle synthesis itself is an immense field of study with an array of diverse applications. The final piece of this work investigates the mechanism behind a previously developed iron oxide synthesis to gain more understanding and direction to future synthesis strategies. The particle growth mechanism was found to proceed by the formation of a solvated iron(III)oleate complex followed by a reduction of iron (III) to iron (II). This unstable iron(II) nucleates to form a wustite (FeO) core which serves as an epitaxial surface for the magnetite (Fe3O4) shell growth. This method produces spherical particles (6-60nm) with relative size distributions of less than 15%.

Synthesis of nanometer-sized sodalite without adding organic additives.

PubMed

Fan, Wei; Morozumi, Kazumasa; Kimura, Riichiro; Yokoi, Toshiyuki; Okubo, Tatsuya

2008-06-01

Aggregates (80 nm) of sodalite nanocrystals with crystallite sizes ranging from 20 to 40 nm have been synthesized from a sodium aluminosilicate solution at low temperature, without adding any organic additives, while paying attention to the key factors for the synthesis of nanosized zeolite crystals. The physical properties of nanosized sodalite crystals were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, 29Si solid-state magic-angle spinning (MAS) NMR, and N2 adsorption. As expected, the external surface area of nanosized sodalite crystals is significantly increased compared with that of microsized sodalite crystals. The size of synthesized sodalite crystals can be controlled from 20 nm to 10 microm. It is found that the preparation of a homogeneous aluminosilicate solution followed by the formation of an aluminosilicate hard gel by adjusting the initial composition, for example, SiO2/Al2O3 and Na2O/H2O ratios, is critical for synthesis.

Preparation of fine single crystals of magnetic superconductor RuSr2GdCu2O8-δ by partial melting

NASA Astrophysics Data System (ADS)

Yamaki, Kazuhiro; Bamba, Yoshihiro; Irie, Akinobu

2018-03-01

In this study, fine uniform RuSr2GdCu2O8-δ (RuGd-1212) single crystals have been successfully prepared by partial melting. Synthesis temperature could be lowered to a value not exceeding the decomposition temperature of RuGd-1212 using the Sr-Gd-Cu-O flux. The crystals grown by alumina boats are cubic, which coincides with the result of a previous study of RuGd-1212 single crystals using platinum crucibles. The single crystals were up to 15 × 15 × 15 µm3 in size and their lattice constants were consistent with those of polycrystalline samples reported previously. Although the present size of single crystals is not sufficient for measurements, the partial melting technique will be beneficial for future progress of research using RuGd-1212 single crystals. Appropriate nominal composition, sintering atmosphere, and temperature are essential factors for growing RuGd-1212 single crystals.

Microfluidic sorting of protein nanocrystals by size for X-ray free-electron laser diffraction

PubMed Central

Abdallah, Bahige G.; Zatsepin, Nadia A.; Roy-Chowdhury, Shatabdi; Coe, Jesse; Conrad, Chelsie E.; Dörner, Katerina; Sierra, Raymond G.; Stevenson, Hilary P.; Camacho-Alanis, Fernanda; Grant, Thomas D.; Nelson, Garrett; James, Daniel; Calero, Guillermo; Wachter, Rebekka M.; Spence, John C. H.; Weierstall, Uwe; Fromme, Petra; Ros, Alexandra

2015-01-01

The advent and application of the X-ray free-electron laser (XFEL) has uncovered the structures of proteins that could not previously be solved using traditional crystallography. While this new technology is powerful, optimization of the process is still needed to improve data quality and analysis efficiency. One area is sample heterogeneity, where variations in crystal size (among other factors) lead to the requirement of large data sets (and thus 10–100 mg of protein) for determining accurate structure factors. To decrease sample dispersity, we developed a high-throughput microfluidic sorter operating on the principle of dielectrophoresis, whereby polydisperse particles can be transported into various fluid streams for size fractionation. Using this microsorter, we isolated several milliliters of photosystem I nanocrystal fractions ranging from 200 to 600 nm in size as characterized by dynamic light scattering, nanoparticle tracking, and electron microscopy. Sorted nanocrystals were delivered in a liquid jet via the gas dynamic virtual nozzle into the path of the XFEL at the Linac Coherent Light Source. We obtained diffraction to ∼4 Å resolution, indicating that the small crystals were not damaged by the sorting process. We also observed the shape transforms of photosystem I nanocrystals, demonstrating that our device can optimize data collection for the shape transform-based phasing method. Using simulations, we show that narrow crystal size distributions can significantly improve merged data quality in serial crystallography. From this proof-of-concept work, we expect that the automated size-sorting of protein crystals will become an important step for sample production by reducing the amount of protein needed for a high quality final structure and the development of novel phasing methods that exploit inter-Bragg reflection intensities or use variations in beam intensity for radiation damage-induced phasing. This method will also permit an analysis of the dependence of crystal quality on crystal size. PMID:26798818

Microfluidic sorting of protein nanocrystals by size for X-ray free-electron laser diffraction

DOE PAGES

Abdallah, Bahige G.; Zatsepin, Nadia A.; Roy-Chowdhury, Shatabdi; ...

2015-08-19

We report that the advent and application of the X-ray free-electron laser (XFEL) has uncovered the structures of proteins that could not previously be solved using traditional crystallography. While this new technology is powerful, optimization of the process is still needed to improve data quality and analysis efficiency. One area is sample heterogeneity, where variations in crystal size (among other factors) lead to the requirement of large data sets (and thus 10–100 mg of protein) for determining accurate structure factors. To decrease sample dispersity, we developed a high-throughput microfluidic sorter operating on the principle of dielectrophoresis, whereby polydisperse particles canmore » be transported into various fluid streams for size fractionation. Using this microsorter, we isolated several milliliters of photosystem I nanocrystal fractions ranging from 200 to 600 nm in size as characterized by dynamic light scattering, nanoparticle tracking, and electron microscopy. Sorted nanocrystals were delivered in a liquid jet via the gas dynamic virtual nozzle into the path of the XFEL at the Linac Coherent Light Source. We obtained diffraction to ~4 Å resolution, indicating that the small crystals were not damaged by the sorting process. We also observed the shape transforms of photosystem I nanocrystals, demonstrating that our device can optimize data collection for the shape transform-based phasing method. Using simulations, we show that narrow crystal size distributions can significantly improve merged data quality in serial crystallography. From this proof-of-concept work, we expect that the automated size-sorting of protein crystals will become an important step for sample production by reducing the amount of protein needed for a high quality final structure and the development of novel phasing methods that exploit inter-Bragg reflection intensities or use variations in beam intensity for radiation damage-induced phasing. Ultimately, this method will also permit an analysis of the dependence of crystal quality on crystal size.« less

Er3+-doped transparent glass ceramics containing micron-sized SrF2 crystals for 2.7 μm emissions

PubMed Central

Jiang, Yiguang; Fan, Jintai; Jiang, Benxue; Mao, Xiaojian; Tang, Junzhou; Xu, Yinsheng; Dai, Shixun; Zhang, Long

2016-01-01

Er3+-doped transparent glass ceramics containing micron-sized SrF2 crystals were obtained by direct liquid-phase sintering of a mixture of SrF2 powders and precursor glass powders at 820 °C for 15 min. The appearance and microstructural evolution of the SrF2 crystals in the resulting glass ceramics were investigated using X-ray diffraction, field-emission scanning electron microscopy and transmission microscopy. The SrF2 crystals are ~15 μm in size and are uniformly distributed throughout the fluorophosphate glass matrix. The glass ceramics achieve an average transmittance of 75% in the visible region and more than 85% in the near-IR region. The high transmittance of the glass ceramics results from matching the refractive index of the SrF2 with that of the precursor glass. Energy dispersive spectroscopy, photoluminescence spectra, and photoluminescence lifetimes verified the incorporation of Er3+ into the micron-sized SrF2 crystals. Intense 2.7 μm emissions due to the 4I11/2 → 4I13/2 transition were observed upon excitation at 980 nm using a laser diode. The maximum value of the emission cross section of Er3+ around 2.7 μm is more than 1.2 × 10−20 cm2, which indicates the potential of using transparent glass ceramics containing micron-sized SrF2 crystals for efficient 2.7 μm lasers and amplifiers. PMID:27430595

Er(3+)-doped transparent glass ceramics containing micron-sized SrF2 crystals for 2.7 μm emissions.

PubMed

Jiang, Yiguang; Fan, Jintai; Jiang, Benxue; Mao, Xiaojian; Tang, Junzhou; Xu, Yinsheng; Dai, Shixun; Zhang, Long

2016-07-19

Er(3+)-doped transparent glass ceramics containing micron-sized SrF2 crystals were obtained by direct liquid-phase sintering of a mixture of SrF2 powders and precursor glass powders at 820 °C for 15 min. The appearance and microstructural evolution of the SrF2 crystals in the resulting glass ceramics were investigated using X-ray diffraction, field-emission scanning electron microscopy and transmission microscopy. The SrF2 crystals are ~15 μm in size and are uniformly distributed throughout the fluorophosphate glass matrix. The glass ceramics achieve an average transmittance of 75% in the visible region and more than 85% in the near-IR region. The high transmittance of the glass ceramics results from matching the refractive index of the SrF2 with that of the precursor glass. Energy dispersive spectroscopy, photoluminescence spectra, and photoluminescence lifetimes verified the incorporation of Er(3+) into the micron-sized SrF2 crystals. Intense 2.7 μm emissions due to the (4)I11/2 → (4)I13/2 transition were observed upon excitation at 980 nm using a laser diode. The maximum value of the emission cross section of Er(3+) around 2.7 μm is more than 1.2 × 10(-20) cm(2), which indicates the potential of using transparent glass ceramics containing micron-sized SrF2 crystals for efficient 2.7 μm lasers and amplifiers.

An evaluation of adhesive sample holders for advanced crystallographic experiments

PubMed Central

Mazzorana, Marco; Sanchez-Weatherby, Juan; Sandy, James; Lobley, Carina M. C.; Sorensen, Thomas

2014-01-01

The hydration state of macromolecular crystals often affects their overall order and, ultimately, the quality of the X-ray diffraction pattern that they produce. Post-crystallization techniques that alter the solvent content of a crystal may induce rearrangement within the three-dimensional array making up the crystal, possibly resulting in more ordered packing. The hydration state of a crystal can be manipulated by exposing it to a stream of air at controlled relative humidity in which the crystal can equilibrate. This approach provides a way of exploring crystal hydration space to assess the diffraction capabilities of existing crystals. A key requirement of these experiments is to expose the crystal directly to the dehydrating environment by having the minimum amount of residual mother liquor around it. This is usually achieved by placing the crystal on a flat porous support (Kapton mesh) and removing excess liquid by wicking. Here, an alternative approach is considered whereby crystals are harvested using adhesives that capture naked crystals directly from their crystallization drop, reducing the process to a one-step procedure. The impact of using adhesives to ease the harvesting of different types of crystals is presented together with their contribution to background scattering and their usefulness in dehydration experiments. It is concluded that adhesive supports represent a valuable tool for mounting macromolecular crystals to be used in humidity-controlled experiments and to improve signal-to-noise ratios in diffraction experiments, and how they can protect crystals from modifications in the sample environment is discussed. PMID:25195752

Models for mean bonding length, melting point and lattice thermal expansion of nanoparticle materials

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

Omar, M.S., E-mail: dr_m_s_omar@yahoo.com

2012-11-15

Graphical abstract: Three models are derived to explain the nanoparticles size dependence of mean bonding length, melting temperature and lattice thermal expansion applied on Sn, Si and Au. The following figures are shown as an example for Sn nanoparticles indicates hilly applicable models for nanoparticles radius larger than 3 nm. Highlights: ► A model for a size dependent mean bonding length is derived. ► The size dependent melting point of nanoparticles is modified. ► The bulk model for lattice thermal expansion is successfully used on nanoparticles. -- Abstract: A model, based on the ratio number of surface atoms to thatmore » of its internal, is derived to calculate the size dependence of lattice volume of nanoscaled materials. The model is applied to Si, Sn and Au nanoparticles. For Si, that the lattice volume is increases from 20 Å{sup 3} for bulk to 57 Å{sup 3} for a 2 nm size nanocrystals. A model, for calculating melting point of nanoscaled materials, is modified by considering the effect of lattice volume. A good approach of calculating size-dependent melting point begins from the bulk state down to about 2 nm diameter nanoparticle. Both values of lattice volume and melting point obtained for nanosized materials are used to calculate lattice thermal expansion by using a formula applicable for tetrahedral semiconductors. Results for Si, change from 3.7 × 10{sup −6} K{sup −1} for a bulk crystal down to a minimum value of 0.1 × 10{sup −6} K{sup −1} for a 6 nm diameter nanoparticle.« less

Longitudinal uniformity, time performances and irradiation test of pure CsI crystals

NASA Astrophysics Data System (ADS)

Angelucci, M.; Atanova, O.; Baccaro, S.; Cemmi, A.; Cordelli, M.; Donghia, R.; Giovannella, S.; Happacher, F.; Miscetti, S.; Sarra, I.; Soleti, S. R.

2016-07-01

To study an alternative to BaF2, as the crystal choice for the Mu2e calorimeter, 13 pure CsI crystals from Opto Materials and ISMA producers have been characterized by determining their light yield (LY) and longitudinal response uniformity (LRU), when read with a UV extended PMT. The crystals show a LY of 100 p.e./MeV ( 150 p.e./MeV) when wrapped with Tyvek and coupled to the PMT without (with) optical grease. The LRU is well represented by a linear slope that is on average δ -0.6%/cm. The timing performances of the Opto Materials crystal, read with a UV extended MPPC, have been evaluated with minimum ionizing particles. A timing resolution of 330 ps ( 440 ps) is achieved when connecting the photosensor to the MPPC with (without) optical grease. The crystal radiation hardness to a ionization dose has also been studied for one pure CsI crystal from SICCAS. After exposing it to a dose of 900 Gy, a decrease of 33% in the LY is observed while the LRU remains unchanged.

The Effects of pH on the Growth and Aspect Ratio of Chicken Egg White Lysozyme Crystals Prepared in Different Buffers

NASA Technical Reports Server (NTRS)

Gibson, U. J.; Horrell, E. E.; Kou, Y.; Pusey, Marc

2000-01-01

We have measured the nucleation and aspect ratio of CEWL crystals grown by vapor diffusion in acetate, butyrate, carbonate, succinate, and phosphate buffers in a range of pH spanning the pK(sub a) of these buffers. The nucleation numbers drop off significantly in the vicinity of pK(sub a) for each of the buffers except the phosphate system, in which we used only the pH range around the second titration point(pK2). There is a concomitant increase in the sizes of the crystals. Some typical nucleation number results are shown. These data support and extend other observations. In addition, we have examined changes in aspect ratio which accompany the suppression of nucleation within each buffer system. The length of the face in the [001] direction was measured, and compared to the width of the (110) face in the [110] type directions. We find that while the aspect ratio of the crystals is affected by pH, it is dominated by a correlation with the size of the crystals. Small crystals are longer in the [0011 direction than crystals that are larger (higher pH within a buffer system). This relationship is found to hold independent of the choice of buffer. These results are consistent with those of Judge et al, who used a batch process which resulted in uniform sizing of crystals at each pH. In these experiments, we specifically avoid agitating the protein/salt buffer mixture when combining the two. This permits the formation of a range of sizes at a given pH. The results for a .05 M acetate 5% NaCl buffer are also shown. We will discuss these results in light of a growth model.

New polymorphs of 9-nitro-camptothecin prepared using a supercritical anti-solvent process.

PubMed

Huang, Yinxia; Wang, Hongdi; Liu, Guijin; Jiang, Yanbin

2015-12-30

Recrystallization and micronization of 9-nitro-camptothecin (9-NC) has been investigated using the supercritical anti-solvent (SAS) technology in this study. Five operating factors, i.e., the type of organic solvent, the concentration of 9-NC in the solution, the flow rate of 9-NC solution, the precipitation pressure and the temperature, were optimized using a selected OA16 (4(5)) orthogonal array design and a series of characterizations were performed for all samples. The results showed that the processed 9-NC particles exhibited smaller particle size and narrower particle size distribution as compared with 9-NC raw material (Form I), and the optimum micronization conditions for preparing 9-NC with minimum particle size were determined by variance analysis, where the solvent plays the most important role in the formation and transformation of polymorphs. Three new polymorphic forms (Form II, III and IV) of 9-NC, which present different physicochemical properties, were generated after the SAS process. The predicted structures of the 9-NC crystals, which were consistent with the experiments, were performed from their experimental XRD data by the direct space approach using the Reflex module of Materials Studio. Meanwhile, the optimal sample (Form III) was proved to have higher cytotoxicity against the cancer cells, which suggested the therapeutic efficacy of 9-NC is polymorph-dependent. Copyright © 2015 Elsevier B.V. All rights reserved.

Encapsulation of Multiple Microalgal Cells via a Combination of Biomimetic Mineralization and LbL Coating.

PubMed

Kim, Minjeong; Choi, Myoung Gil; Ra, Ho Won; Park, Seung Bin; Kim, Yong-Joo; Lee, Kyubock

2018-02-13

The encapsulation of living cells is appealing for its various applications to cell-based sensors, bioreactors, biocatalysts, and bioenergy. In this work, we introduce the encapsulation of multiple microalgal cells in hollow polymer shells of rhombohedral shape by the following sequential processes: embedding of microalgae in CaCO₃ crystals; layer-by-layer (LbL) coating of polyelectrolytes; and removal of sacrificial crystals. The microcapsule size was controlled by the alteration of CaCO₃ crystal size, which is dependent on CaCl₂/Na₂CO₃ concentration. The microalgal cells could be embedded in CaCO₃ crystals by a two-step process: heterogeneous nucleation of crystal on the cell surface followed by cell embedment by the subsequent growth of crystal. The surfaces of the microalgal cells were highly favorable for the crystal growth of calcite; thus, micrometer-sized microalgae could be perfectly occluded in the calcite crystal without changing its rhombohedral shape. The surfaces of the microcapsules, moreover, could be decorated with gold nanoparticles, Fe₃O₄ magnetic nanoparticles, and carbon nanotubes (CNTs), by which we would expect the functionalities of a light-triggered release, magnetic separation, and enhanced mechanical and electrical strength, respectively. This approach, entailing the encapsulation of microalgae in semi-permeable and hollow polymer microcapsules, has the potential for application to microbial-cell immobilization for high-biomass-concentration cultivation as well as various other bioapplications.

Anomalous transparency in photonic crystals and its application to point-by-point grating inscription in photonic crystal fibers.

PubMed

Baghdasaryan, Tigran; Geernaert, Thomas; Chah, Karima; Caucheteur, Christophe; Schuster, Kay; Kobelke, Jens; Thienpont, Hugo; Berghmans, Francis

2018-04-03

It is common belief that photonic crystals behave similarly to isotropic and transparent media only when their feature sizes are much smaller than the wavelength of light. Here, we counter that belief and we report on photonic crystals that are transparent for anomalously high normalized frequencies up to 0.9, where the crystal's feature sizes are comparable with the free space wavelength. Using traditional photonic band theory, we demonstrate that the isofrequency curves can be circular in the region above the first stop band for triangular lattice photonic crystals. In addition, by simulating how efficiently a tightly focused Gaussian beam propagates through the photonic crystal slab, we judge on the photonic crystal's transparency rather than on isotropy only. Using this approach, we identified a wide range of photonic crystal parameters that provide anomalous transparency. Our findings indicate the possibility to scale up the features of photonic crystals and to extend their operational wavelength range for applications including optical cloaking and graded index guiding. We applied our result in the domain of femtosecond laser micromachining, by demonstrating what we believe to be the first point-by-point grating inscribed in a multi-ring photonic crystal fiber.

Effects of organic matter on crystallization of struvite in biologically treated swine wastewater.

PubMed

Capdevielle, Aurélie; Sýkorová, Eva; Béline, Fabrice; Daumer, Marie-Line

2016-01-01

A sustainable way to recover phosphorus (P) in swine wastewater involves a preliminary step of P dissolution followed by the separation of particulate organic matter (OM). The next two steps are firstly the precipitation of struvite crystals done by adding a crystallization reagent (magnesia) and secondly the filtration of the crystals. To develop the process successfully at an industrial scale, the control of the mechanisms of precipitation is the key point in order to obtain high value-added products, that is, big struvite crystals easy to harvest and handle. Experiments with process parameters optimized previously in a synthetic swine wastewater were performed on real swine wastewater to assess the role of the OM on struvite crystallization. After 24 h, with a pH increase to 6.8 only, 90% of the initial P was precipitated and 60% was precipitated as struvite. 80% of the solid recovered was in the fraction > 100 µm. The other forms recovered were brushite, amorphous calcium phosphate, NaCl, KCl and OM. The influence of OM on struvite precipitation in acidified swine wastewater was negative on the reaction kinetics but positive on the size of the struvite crystals. The presence of colloidal particles increased the size of the struvite crystals but slowed down the kinetics due to the viscosity induced by the repulsive force of the colloids. The maximum size of single struvite crystals (200 µm) was observed with the presence of particulate OM.

Decrystallization of Crystals Using Gold “Nano-Bullets” and the Metal-Assisted and Microwave-Accelerated Decrystallization Technique

PubMed Central

Thompson, Nishone; Boone-Kukoyi, Zainab; Shortt, Raquel; Lansiquot, Carisse; Kioko, Bridgit; Bonyi, Enock; Toker, Salih; Ozturk, Birol; Aslan, Kadir

2017-01-01

Gout is caused by the overproduction of uric acid and the inefficient metabolism of dietary purines in humans. Current treatments of gout, which include anti-inflammatory drugs, cyclooxygenase-2 inhibitors, and systemic glucocorticoids, have harmful side-effects. Our research laboratory has recently introduced an innovative approach for the decrystallization of biological and chemical crystals using the Metal-Assisted and Microwave-Accelerated Evaporative Decrystallization (MAMAD) technique. In the MAMAD technique, microwave energy is used to heat and activate gold nanoparticles that behave as “nano-bullets” to rapidly disrupt the crystal structure of biological crystals placed on planar surfaces. In this study, crystals of various sizes and compositions were studied as models for tophaceous gout at different stages (i.e., uric acid as small crystals (~10–100 μm) and L-alanine as medium (~300 μm) and large crystals (~4400 μm). Our results showed that the use of the MAMAD technique resulted in the reduction of the size and number of uric acid and L-alanine crystals up to >40% when exposed to intermittent microwave heating (up to 20 W power at 8 GHz) in the presence of 20 nm gold nanoparticles up to 120 s. This study demonstrates that the MAMAD technique can be potentially used as an alternative therapeutic method for the treatment of gout by effective decrystallization of large crystals, similar in size to those that often occur in gout. PMID:27763557

Modeling solute clustering in the diffusion layer around a growing crystal.

PubMed

Shiau, Lie-Ding; Lu, Yung-Fang

2009-03-07

The mechanism of crystal growth from solution is often thought to consist of a mass transfer diffusion step followed by a surface reaction step. Solute molecules might form clusters in the diffusion step before incorporating into the crystal lattice. A model is proposed in this work to simulate the evolution of the cluster size distribution due to the simultaneous aggregation and breakage of solute molecules in the diffusion layer around a growing crystal in the stirred solution. The crystallization of KAl(SO(4))(2)12H(2)O from aqueous solution is studied to illustrate the effect of supersaturation and diffusion layer thickness on the number-average degree of clustering and the size distribution of solute clusters in the diffusion layer.

Analysis and sizing of Mars aerobrake structure

NASA Technical Reports Server (NTRS)

Raju, I. S.; Craft, W. J.

1993-01-01

A cone-sphere aeroshell structure for aerobraking into Martian atmosphere is studied. Using this structural configuration, a space frame load-bearing structure is proposed. To generate this structure efficiently and to perform a variety of studies of several configurations, a mesh generator that utilizes only a few configurational parameters is developed. A finite element analysis program that analyzes space frame structures was developed. A sizing algorithm that arrives at a minimum mass configuration was developed and integrated into the finite element analysis program. A typical 135-ft-diam aerobrake configuration was analyzed and sized. The minimum mass obtained in this study using high modulus graphite/epoxy composite material members is compared with the masses obtained from two other aerobrake structures using lightweight erectable tetrahedral truss and part-spherical truss configurations. Excellent agreement for the minimum mass was obtained with the three different aerobrake structures. Also, the minimum mass using the present structure was obtained when the supports were not at the base but at about 75 percent of the base diameter.

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.

Antisolvent crystallization of a cardiotonic drug in ionic liquids: Effect of mixing on the crystal properties

NASA Astrophysics Data System (ADS)

de Azevedo Jacqueline, Resende; Fabienne, Espitalier; Jean-Jacques, Letourneau; Inês, Ré Maria

2017-08-01

LASSBio-294 (3,4-methylenedioxybenzoyl-2-thienylhydrazon) is a poorly soluble drug which has been proposed to have major advantages over other cardiotonic drugs. Poorly water soluble drugs present limited bioavailability due to their low solubility and dissolution rate. An antisolvent crystallization processing can improve the dissolution rate by decreasing the crystals particle size. However, LASSBio-294 is also poorly soluble in organic solvents and this operation is limited. In order to open new perspectives to improve dissolution rate, this work has investigated LASSBio-294 in terms of its antisolvent crystallization in 1-ethyl-3-methylimidazolium methyl phosphonate [emim][CH3O(H)PO2] as solvent and water as antisolvent. Two modes of mixing are tested in stirred vessel with different pre-mixers (Roughton or T-mixers) in order to investigate the mixing effect on the crystal properties (crystalline structure, particle size distribution, residual solvent and in vitro dissolution rate). Smaller drug particles with unchanged crystalline structure were obtained. Despite the decrease of the elementary particles size, the recrystallized particles did not achieve a better dissolution profile. However, this study was able to highlight a certain number of findings such as the impact of the hydrodynamic conditions on the crystals formation and the presence of a gel phase limiting the dissolution rate.

Influence of nano-size inclusions on spall fracture of copper single crystals

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

Razorenov, S. V.; Ivanchihina, G. E.; Kanel, G. I.

2007-12-12

Spall experiments have been carried out for copper in different structural states. The samples were copper single crystals, crystals of Cu+0.1% Si, copper crystals with silica particles of 180 nm average size, and polycrystalline copper. In experiments, the free surface velocity histories were recorded with the VISAR. The recovered samples were studied using optical microscopy and SEM. Solid solution Cu+0.1% Si demonstrates slower spall process than pure copper crystals. At longer pulse durations its spall strength is slightly less than that of pure crystals but approaches the latter with decreasing pulse duration. Fracture of copper with silica inclusions is completedmore » much faster. The spall strength of this material is close to that of Cu+0.1% Si crystals at longer pulse duration and approaches the strength of polycrystalline copper with decreasing the load duration. Fractography of the spall surfaces correlates with the free surface velocity histories. The main fracture surface of the Cu+0.1% Si grains consists of net of dimples {approx}4 {mu}m to 40 {mu}m mean diameter. The fracture surfaces of copper with silica inclusions is covered by a net of dimples of 1 {mu}m to 5 {mu}m size.« less

Quantifying solubility enhancement due to particle size reduction and crystal habit modification: case study of acetyl salicylic acid.

PubMed

Hammond, Robert B; Pencheva, Klimentina; Roberts, Kevin J; Auffret, Tony

2007-08-01

The poor solubility of potential drug molecules is a significant problem in the design of pharmaceutical formulations. It is well known, however, that the solubility of crystalline materials is enhanced when the particle size is reduced to submicron levels and this factor can be expected to enhance drug product bioavailability. Direct estimation of solubility enhancement, as calculated via the Gibbs-Thompson relationship, demands reasonably accurate values for the particle/solution interfacial tension and, in particular, its anisotropy with respect to the crystal product's habit and morphology. In this article, an improved, more molecule-centered, approach is presented towards the calculation of solubility enhancement factors in which molecular modeling techniques are applied, and the effects associated with both crystal habit modification and solvent choice are examined. A case study for facetted, acetyl salicylic acid (aspirin) crystals in equilibrium with saturated aqueous ethanol solution reveals that their solubility will be enhanced in the range (7-58%) for a crystal size of 0.02 microm, with significantly higher enhancement for crystal morphologies in which the hydrophobic crystal faces are more predominant than the hydrophilic faces and for solvents in which the solubility is smaller. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Modeling of Macroscopic/Microscopic Transport and Growth Phenomena in Zeolite Crystal Solutions Under Microgravity Conditions

NASA Technical Reports Server (NTRS)

Gatsonis, Nikos A.; Alexandrou, Andreas; Shi, Hui; Ongewe, Bernard; Sacco, Albert, Jr.

1999-01-01

Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process. At the same time, however, there is increased urgency to develop such an understanding in order to more accurately quantify the process. In order to better understand the results obtained from our prior space experiments, and design future experiments, a detailed fluid dynamic model simulating the crystal growth mechanism is required. This will not only add to the fundamental knowledge on the crystallization of zeolites, but also be useful in predicting the limits of size and growth of these important industrial materials. Our objective is to develop macro/microscopic theoretical and computational models to study the effect of transport phenomena in the growth of crystals grown in solutions. Our effort has concentrated so far in the development of separate macroscopic and microscopic models. The major highlights of our accomplishments are described.

Dependence of crystal size on the catalytic performance of a porous coordination polymer.

PubMed

Kiyonaga, Tomokazu; Higuchi, Masakazu; Kajiwara, Takashi; Takashima, Yohei; Duan, Jingui; Nagashima, Kazuro; Kitagawa, Susumu

2015-02-14

Submicrosized MOF-76(Yb) exhibits a higher catalytic performance for esterification than microsized MOF-76(Yb). Control of the crystal size of porous heterogeneous catalysts, such as PCP/MOFs, offers a promising approach to fabricating high-performance catalysts based on accessibility to the internal catalytic sites.

76 FR 56120 - Atlantic Highly Migratory Species; North and South Atlantic Swordfish Quotas

Federal Register 2010, 2011, 2012, 2013, 2014

2011-09-12

... Contracting Parties. Contracting Parties may restrict fishermen to a minimum size of 25 kg live weight OR 125... restrict fishermen to a minimum size of 15 kg live weight OR 119 cm LJFL with no tolerance. In 2009, NMFS... quota, among other things. Per the ATCA, the United States is obligated to implement ICCAT-approved...

Determining ice water content from 2D crystal images in convective cloud systems

NASA Astrophysics Data System (ADS)

Leroy, Delphine; Coutris, Pierre; Fontaine, Emmanuel; Schwarzenboeck, Alfons; Strapp, J. Walter

2016-04-01

Cloud microphysical in-situ instrumentation measures bulk parameters like total water content (TWC) and/or derives particle size distributions (PSD) (utilizing optical spectrometers and optical array probes (OAP)). The goal of this work is to introduce a comprehensive methodology to compute TWC from OAP measurements, based on the dataset collected during recent HAIC (High Altitude Ice Crystals)/HIWC (High Ice Water Content) field campaigns. Indeed, the HAIC/HIWC field campaigns in Darwin (2014) and Cayenne (2015) provide a unique opportunity to explore the complex relationship between cloud particle mass and size in ice crystal environments. Numerous mesoscale convective systems (MCSs) were sampled with the French Falcon 20 research aircraft at different temperature levels from -10°C up to 50°C. The aircraft instrumentation included an IKP-2 (isokinetic probe) to get reliable measurements of TWC and the optical array probes 2D-S and PIP recording images over the entire ice crystal size range. Based on the known principle relating crystal mass and size with a power law (m=α•Dβ), Fontaine et al. (2014) performed extended 3D crystal simulations and thereby demonstrated that it is possible to estimate the value of the exponent β from OAP data, by analyzing the surface-size relationship for the 2D images as a function of time. Leroy et al. (2015) proposed an extended version of this method that produces estimates of β from the analysis of both the surface-size and perimeter-size relationships. Knowing the value of β, α then is deduced from the simultaneous IKP-2 TWC measurements for the entire HAIC/HIWC dataset. The statistical analysis of α and β values for the HAIC/HIWC dataset firstly shows that α is closely linked to β and that this link changes with temperature. From these trends, a generalized parameterization for α is proposed. Finally, the comparison with the initial IKP-2 measurements demonstrates that the method is able to predict TWC values larger than 0.3g/m3 with an error close to 20%. Fontaine, E., A. Schwarzenboeck, J. Delanoë, W. Wobrock, D. Leroy, R. Dupuy, C. Gourbeyre, and A. Protat, 2014: Constraining mass-diameter relations from hydrometeor images and cloud radar reflectivities in tropical continental and oceanic convective anvils. Atmos Chem Phys, 14, 11367-11392, doi:10.5194/acp-14-11367-2014. Leroy, D., E. Fontaine, A. Schwarzenboeck and J.W. Strapp : Ice Crystal Sizes in High Ice Water Content Clouds. Part 1: Mass-size Relationships Derived from Particle Images and TWC for Various Crystal Diameter Definitions and Impact on Median Mass Diameter. Submitted to Journal of Atmospheric and Oceanic Technology, 2015.

HREM study of irradiation damage in human dental enamel crystals.

PubMed

Brès, E F; Hutchison, J L; Senger, B; Voegel, J C; Frank, R M

1991-06-01

Several phenomena have been observed during the examination of human dental enamel crystals (mainly constituted by hydroxyapatite (OHAP] by high-resolution electron microscopy (HREM) at 300 and 400 keV: orientation-dependent damage in the form of mass loss from voids or uniform destruction of crystal structure, beam-induced diffusion creating outgrowths at the crystal surfaces, recrystallization of the bulk crystal and crystallization of the inorganic components of the matrix surrounding the crystals. These beam-induced crystals have the CaO structure. The phenomena observed are most likely due to various electron-crystal interaction mechanisms (ballistic knock-on damage, electronic excitations, temperature rise, etc.). In this paper, the contribution of the ballistic process to the phenomena observed is discussed. The quantitative description of the knock-on collisions rests on the McKinley-Feshbach cross-section formula. The minimum ion displacement energies which appear in this expression have been estimated on the basis of the electrostatic ion binding energies, and the covalent bond energies if required. It is shown that hydroxyl, calcium and oxygen ions can effectively be displaced by the incident 300 and 400 keV electrons. Thus, the formation of CaO crystals by the combination of calcium and oxygen ions diffusing from their initial sites inside the OHAP lattice can tentatively be explained.

Retrieval of ice crystals' mass from ice water content and particle distribution measurements: a numerical optimization approach

NASA Astrophysics Data System (ADS)

Coutris, Pierre; Leroy, Delphine; Fontaine, Emmanuel; Schwarzenboeck, Alfons; Strapp, J. Walter

2016-04-01

A new method to retrieve cloud water content from in-situ measured 2D particle images from optical array probes (OAP) is presented. With the overall objective to build a statistical model of crystals' mass as a function of their size, environmental temperature and crystal microphysical history, this study presents the methodology to retrieve the mass of crystals sorted by size from 2D images using a numerical optimization approach. The methodology is validated using two datasets of in-situ measurements gathered during two airborne field campaigns held in Darwin, Australia (2014), and Cayenne, France (2015), in the frame of the High Altitude Ice Crystals (HAIC) / High Ice Water Content (HIWC) projects. During these campaigns, a Falcon F-20 research aircraft equipped with state-of-the art microphysical instrumentation sampled numerous mesoscale convective systems (MCS) in order to study dynamical and microphysical properties and processes of high ice water content areas. Experimentally, an isokinetic evaporator probe, referred to as IKP-2, provides a reference measurement of the total water content (TWC) which equals ice water content, (IWC) when (supercooled) liquid water is absent. Two optical array probes, namely 2D-S and PIP, produce 2D images of individual crystals ranging from 50 μm to 12840 μm from which particle size distributions (PSD) are derived. Mathematically, the problem is formulated as an inverse problem in which the crystals' mass is assumed constant over a size class and is computed for each size class from IWC and PSD data: PSD.m = IW C This problem is solved using numerical optimization technique in which an objective function is minimized. The objective function is defined as follows: 2 J(m)=∥P SD.m - IW C ∥ + λ.R (m) where the regularization parameter λ and the regularization function R(m) are tuned based on data characteristics. The method is implemented in two steps. First, the method is developed on synthetic crystal populations in order to evaluate the behavior of the iterative algorithm, the influence of data noise on the quality of the results, and to set up a regularization strategy. Therefore, 3D synthetic crystals have been generated and numerically processed to recreate the noise caused by 2D projections of randomly oriented 3D crystals and by the discretization of the PSD into size classes of predefined width. Subsequently, the method is applied to the experimental datasets and the comparison between the retrieved TWC (this methodology) and the measured ones (IKP-2 data) will enable the evaluation of the consistency and accuracy of the mass solution retrieved by the numerical optimization approach as well as preliminary assessment of the influence of temperature and dynamical parameters on crystals' masses.

Compaction of Chromite Cumulates applying a Centrifuging Piston-Cylinder

NASA Astrophysics Data System (ADS)

Manoochehri, S.; Schmidt, M. W.

2012-12-01

Stratiform accumulations of chromite cumulates, such as the UG2 chromitite layer in the Bushveld Complex, is a common feature in most of the large layered mafic intrusions. The time scales and mechanics of gravitationally driven crystal settling and compaction and the feasibility of these processes for the formation of such cumulate layers is investigated through a series of high temperature (1280-1300 °C) centrifuge-assisted experiments at 100-2000 g, 0.4-0.6 GPa. A mixture of natural chromite, with defined grain sizes (means of 5 μm, 13 μm, and 52 μm), and a melt with a composition thought to represent the parental magma of the Bushveld Complex, was first chemically and texturally equilibrated at static conditions and then centrifuged. Centrifugation leads to a single cumulate layer formed at the gravitational bottom of the capsule. This layer was analysed for porosity, mean grain size, size distribution and also travelling distance of chromite crystals. The experimentally observed mechanical settling velocity of chromite grains in a suspension with ~ 24 vol% crystals is calculated to be about half (~ 0.53) of the Stokes settling velocity, consistent with a sedimentation exponent n of 2.35±0.3. The settling leads to a porosity of about 52 % in the chromite layer. Formation times of chromite orthocumulates with initial crystal content in the melt of 1 % and grain sizes of 2 mm are thus around 0.6 m/day. To achieve more compacted chromite piles, centrifugation times and acceleration were increased. Within each experiment the crystal content of the cumulate layer increases downward almost linearly at least in the lower 2/3 of the cumulate pile. Although porosity in the lowermost segment of the chromite layer decreases with increasing effective stress integrated over time, the absolute decrease is smaller than for experiments with olivine (from a previous study). Formation times of a ½ meter single chromite layer with 70 vol% chromite, is calculated to be around 20 years whereas this value is around 0.4 years for olivine cumulates. When considering a natural outcrop of a layered intrusion with multiple layers of about 50 meters height, adcumulate formation time decreases to a few months. With increasing the effective stress integrated over time, applied during centrifugation, crystal size distribution histograms move slightly toward larger grain sizes, but looking at mean grain sizes, a narrow range of changes can be observed. Classic crystal size distribution profiles corrected for real 3D sizes (CSDCorrectin program) of the chromite grains in different experiments illustrate a collection of parallel log-linear trends at larger grain sizes with a very slight overturn at small grain sizes. This is in close agreement with the idealized CSD plots of adcumulus growth.

Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

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

Witman, Matthew; Ling, Sanliang; Boyd, Peter

Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. Here, we hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area canmore » yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.« less

Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites.

PubMed

Witman, Matthew; Ling, Sanliang; Boyd, Peter; Barthel, Senja; Haranczyk, Maciej; Slater, Ben; Smit, Berend

2018-02-28

Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. We hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area can yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.

Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

PubMed Central

2018-01-01

Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. We hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area can yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal–organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc. PMID:29532024

Cutting Materials in Half: A Graph Theory Approach for Generating Crystal Surfaces and Its Prediction of 2D Zeolites

DOE PAGES

Witman, Matthew; Ling, Sanliang; Boyd, Peter; ...

2018-02-06

Scientific interest in two-dimensional (2D) materials, ranging from graphene and other single layer materials to atomically thin crystals, is quickly increasing for a large variety of technological applications. While in silico design approaches have made a large impact in the study of 3D crystals, algorithms designed to discover atomically thin 2D materials from their parent 3D materials are by comparison more sparse. Here, we hypothesize that determining how to cut a 3D material in half (i.e., which Miller surface is formed) by severing a minimal number of bonds or a minimal amount of total bond energy per unit area canmore » yield insight into preferred crystal faces. We answer this question by implementing a graph theory technique to mathematically formalize the enumeration of minimum cut surfaces of crystals. While the algorithm is generally applicable to different classes of materials, we focus on zeolitic materials due to their diverse structural topology and because 2D zeolites have promising catalytic and separation performance compared to their 3D counterparts. We report here a simple descriptor based only on structural information that predicts whether a zeolite is likely to be synthesizable in the 2D form and correctly identifies the expressed surface in known layered 2D zeolites. The discovery of this descriptor allows us to highlight other zeolites that may also be synthesized in the 2D form that have not been experimentally realized yet. Finally, our method is general since the mathematical formalism can be applied to find the minimum cut surfaces of other crystallographic materials such as metal-organic frameworks, covalent-organic frameworks, zeolitic-imidazolate frameworks, metal oxides, etc.« less

Synthesis, crystal growth and characterization of bioactive material: 2- Amino-1H-benzimidazolium pyridine-3-carboxylate single crystal- a proton transfer molecular complex

NASA Astrophysics Data System (ADS)

Fathima, K. Saiadali; Kavitha, P.; Anitha, K.

2017-09-01

The 1:1 molecular adducts 2- Amino-1H-benzimidazolium pyridine-3-carboxylate (2ABPC) was synthesized and grown as single crystal where 2-aminobenzimidazole (ABI) acts as a donor and nicotinic acid (NA) acts as an acceptor. The presence of proton and carbon were predicted using 1H and 13C NMR spectral analysis. The molecular structure of the crystal was elucidated by subjecting the grown crystals to the single crystal x-ray diffraction analysis and was refined by full matrix least-squares method to R = 0.038 for 2469 reflections. The vibrational modes of functional group have been studied using FTIR and Raman spectroscopic analysis. The UV-Vis spectrum exhibited a visible band at 246 nm for 2ABPC due to the nicotinate anion of the molecule. Further, the antimicrobial activity of 2ABPC complex against B. subtilis, klebsiella pneumonia, Pseudomonas eruginos and E. coli pathogens was investigated. Minimum Inhibitory Concentration (MIC) for this crystal was obtained using UV spectrometer against MRSA pathogen. It was found that the benzimidazole with aminogroup at position 2 increases the general antimicrobial activities of 2ABPC crystal.

Mapping crystal defects with a digital scanning ultramicroscope

NASA Astrophysics Data System (ADS)

Springer, John M., Jr.; Silberman, Enrique; Kroes, Roger L.; Reiss, Don

1991-12-01

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or 3-D perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometers , which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects, and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Mapping crystal defects with a digital scanning ultramicroscope

NASA Astrophysics Data System (ADS)

Springer, J. M.; Silberman, E.; Kroes, Roger; Reiss, D.

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Solar axion search technique with correlated signals from multiple detectors

DOE PAGES

Xu, Wenqin; Elliott, Steven R.

2017-01-25

The coherent Bragg scattering of photons converted from solar axions inside crystals would boost the signal for axion-photon coupling enhancing experimental sensitivity for these hypothetical particles. Knowledge of the scattering angle of solar axions with respect to the crystal lattice is required to make theoretical predications of signal strength. Hence, both the lattice axis angle within a crystal and the absolute angle between the crystal and the Sun must be known. In this paper, we examine how the experimental sensitivity changes with respect to various experimental parameters. We also demonstrate that, in a multiple-crystal setup, knowledge of the relative axismore » orientation between multiple crystals can improve the experimental sensitivity, or equivalently, relax the precision on the absolute solar angle measurement. However, if absolute angles of all crystal axes are measured, we find that a precision of 2°–4° will suffice for an energy resolution of σ E = 0.04E and a flat background. Lastly, we also show that, given a minimum number of detectors, a signal model averaged over angles can substitute for precise crystal angular measurements, with some loss of sensitivity.« less

Mapping crystal defects with a digital scanning ultramicroscope

NASA Technical Reports Server (NTRS)

Springer, J. M.; Silberman, E.; Kroes, Roger; Reiss, D.

1991-01-01

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Design and optimization of production parameters for boric acid crystals with the crystallization process in an MSMPR crystallizer using FBRM® and PVM® technologies

NASA Astrophysics Data System (ADS)

Kutluay, Sinan; Şahin, Ömer; Ceyhan, A. Abdullah; İzgi, M. Sait

2017-06-01

In crystallization studies, newly developed technologies, such as Focused Beam Reflectance Measurement (FBRM) and Particle Vision and Measurement (PVM) are applied for determining on-line monitoring of a representation of the Chord Length Distribution (CLD) and observe the photographs of crystals respectively; moreover recently they are widely used. Properly installed, the FBRM ensures on-line determination of the CLD, which is statistically associated to the Crystal Size Distribution (CSD). In industrial crystallization, CSD and mean crystal size as well as external habit and internal structure are important characteristics for further use of the crystals. In this paper, the effect of residence time, stirring speed, feeding rate, supersaturation level and the polyelectrolytes such as anionic polyacrylamide (APAM) and non-ionic polyacrylamide (NPAM) on the CLD as well as the shape of boric acid crystals were investigated by using the FBRM G600 and the PVM V819 probes respectively in an MSMPR (Mixed Suspension Mixed Product Removal) crystallizer. The CSD and kinetic data were determined experimentally using continuous MSMPR crystallizer running at steady state. The population density of nuclei, the nucleation rate and the growth rate were determined from the experimental population balance distribution when the steady state was reached.

50 CFR 622.275 - Size limits.

Code of Federal Regulations, 2013 CFR

2013-10-01

..., DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Dolphin and Wahoo Fishery Off the Atlantic States § 622.275 Size limits. All size limits in this section are minimum size...

50 CFR 622.275 - Size limits.

Code of Federal Regulations, 2014 CFR

2014-10-01

..., DEPARTMENT OF COMMERCE FISHERIES OF THE CARIBBEAN, GULF OF MEXICO, AND SOUTH ATLANTIC Dolphin and Wahoo Fishery Off the Atlantic States § 622.275 Size limits. All size limits in this section are minimum size...

7 CFR 51.344 - Size.

Code of Federal Regulations, 2010 CFR

2010-01-01

... Standards for Grades of Apples for Processing Size § 51.344 Size. (a) The minimum and maximum sizes or range... the apples determined by the smallest opening through which it will pass. Application of Standards ...

7 CFR 51.344 - Size.

Code of Federal Regulations, 2011 CFR

2011-01-01

... Standards for Grades of Apples for Processing Size § 51.344 Size. (a) The minimum and maximum sizes or range... the apples determined by the smallest opening through which it will pass. Application of Standards ...

7 CFR 51.344 - Size.

Code of Federal Regulations, 2012 CFR

2012-01-01

... Standards for Grades of Apples for Processing Size § 51.344 Size. (a) The minimum and maximum sizes or range... the apples determined by the smallest opening through which it will pass. Application of Standards ...

Microwave Heating of Crystals with Gold Nanoparticles and Synovial Fluid under Synthetic Skin Patches

PubMed Central

2017-01-01

Gout is a disease with elusive treatment options. Reduction of the size of l-alanine crystals as a model crystal for gouty tophi with the use of a monomode solid-state microwave was examined as a possible therapeutic aid. The effect of microwave heating on l-alanine crystals in the presence of gold nanoparticles (Au NPs) in solution and synovial fluid (SF) in a plastic pouch through a synthetic skin patch was investigated. In this regard, three experimental paradigms were employed: Paradigm 1 includes the effect of variable microwave power (5–10 W) and variable heating time (5–60 s) and Au NPs in water (20 nm size, volume of 10 μL) in a plastic pouch (1 × 2 cm2 in size). Paradigm 2 includes the effect of a variable volume of 20 nm Au NPs in a variable volume of SF up to 100 μL in a plastic pouch at a constant microwave power (10 W) for 30 s. Paradigm 3 includes the effect of constant microwave power (10 W) and microwave heating time (30 s), constant volume of Au NPs (100 μL), and variable size of Au NPs (20–200 nm) placed in a plastic pouch through a synthetic skin patch. In these experiments, an average of 60–100% reduction in the size of an l-alanine crystal (initial size = 450 μm) without damage to the synthetic skin or increasing the temperature of the samples beyond the physiological range was reported. PMID:28983527

Shock metamorphism of Elephant Moraine A79001: Implications for olivine-ringwoodite transformation and the complex thermal history of heavily shocked Martian meteorites

NASA Astrophysics Data System (ADS)

Walton, Erin L.

2013-04-01

Lithology A of Martian meteorite Elephant Moraine (EET) A79001 contains fragments entrained within a 100 μm-thick shear-induced shock vein. These fragments, the shock vein matrix and walls of olivine along the vein, as well as shock deformation and transformation in rock-forming minerals in the bulk rock, were investigated using scanning electron microscopy, the electron microprobe and Raman spectroscopy. The presence of ringwoodite, the spinel-structured high-pressure (Mg,Fe)2SiO4 polymorph, has been confirmed in EETA79001 for the first time. Ringwoodite occurs within and around the shock vein, exhibiting granular and lamellar textures. In both textures ringwoodite consists of ˜500 nm size distinct grains. Ringwoodite lamellae are 115 nm to 1.3 μm wide. Planar fractures in olivine provided sites for heterogeneous nucleation of ringwoodite. Analyses performed on the largest grains (⩾1 μm) show that ringwoodite is consistently higher in iron (Fa27.4-32.4) relative to surrounding olivine (Fa25.1-267.7), implying that there was Fe-Mg exchange during their transformation, and therefore their growth was diffusion-controlled. In the shock environment, diffusion takes place dynamically, i.e., with concurrent deformation and grain size reduction. This results in enhanced diffusion rates (⩾10-8 m2/s) over nm - μm distances. Shock deformation in host rock minerals including strong mosaicism, pervasive fracturing, polysynthetic twinning (pyroxene only), extensive shock melting, local transformation of olivine to ringwoodite, and complete transformation of plagioclase to maskelynite in the bulk rock, indicate that EETA79001 was strongly shocked. The short shock duration (0.01 s) combined with a complex thermal history, resulted in crystallization of the 100 μm thick shock vein in EETA79001 during the pressure release, and partial back-transformation of ringwoodite to olivine. Based on the pressure stabilities of clinopyroxene + ringwoodite, crystallization at the shock vein margin began at ˜18 GPa. Olivine and clinopyroxene crystallized at <14 GPa closer to the shock vein center. These represent a minimum limit to the shock pressure loading experienced by EETA79001.

Citrate, not phosphate, can dissolve calcium oxalate monohydrate crystals and detach these crystals from renal tubular cells.

PubMed

Chutipongtanate, Somchai; Chaiyarit, Sakdithep; Thongboonkerd, Visith

2012-08-15

Dissolution therapy of calcium oxalate monohydrate (COM) kidney stone disease has not yet been implemented due to a lack of well characterized COM dissolution agents. The present study therefore aimed to identify potential COM crystal dissolution compounds. COM crystals were treated with deionized water (negative control), 5 mM EDTA (positive control), 5 mM sodium citrate, or 5mM sodium phosphate. COM crystal dissolution activities of these compounds were evaluated by phase-contrast and video-assisted microscopic examinations, semi-quantitative analysis of crystal size, number and total mass, and spectrophotometric oxalate-dissolution assay. In addition, effects of these compounds on detachment of COM crystals, which adhered tightly onto renal tubular cell surface, were also investigated. The results showed that citrate, not phosphate, had a significant dissolution effect on COM crystals as demonstrated by significant reduction of crystal size (approximately 37% decrease), crystal number (approximately 53% decrease) and total crystal mass (approximately 72% decrease) compared to blank and negative controls. Spectrophotometric oxalate-dissolution assay successfully confirmed the COM crystal dissolution property of citrate. Moreover, citrate could detach up to 85% of the adherent COM crystals from renal tubular cell surface. These data indicate that citrate is better than phosphate for dissolution and detachment of COM crystals. Copyright © 2012 Elsevier B.V. All rights reserved.

Three Essays In and Tests of Theoretical Urban Economics

NASA Astrophysics Data System (ADS)

Zhao, Weihua

This dissertation consists of three essays on urban economics. The three essays are related to urban spatial structure change, energy consumption, greenhouse gas emissions, and housing redevelopment. Chapter 1 answers the question: Does the classic Standard Urban Model still describe the growth of cities? Chapter 2 derives the implications of telework on urban spatial structure, energy consumption, and greenhouse gas emissions. Chapter 3 investigates the long run effects of minimum lot size zoning on neighborhood redevelopment. Chapter 1 identifies a new implication of the classic Standard Urban Model, the "unitary elasticity property (UEP)", which is the sum of the elasticity of central density and the elasticity of land area with respect to population change is approximately equal to unity. When this implication of the SUM is tested, it fits US cities fairly well. Further analysis demonstrates that topographic barriers and age of housing stock are the key factors explaining deviation from the UEP. Chapter 2 develops a numerical urban simulation model with households that are able to telework to investigate the urban form, congestion, energy consumption and greenhouse gas emission implications of telework. Simulation results suggest that by reducing transportation costs, telework causes sprawl, with associated longer commutes and consumption of larger homes, both of which increase energy consumption. Overall effects depend on who captures the gains from telework (workers versus firms), urban land use regulation such as height limits or greenbelts, and the fraction of workers participating in telework. The net effects of telework on energy use and GHG emissions are generally negligible. Chapter 3 applies dynamic programming to investigate the long run effects of minimum lot size zoning on neighborhood redevelopment. With numerical simulation, comparative dynamic results show that minimum lot size zoning can delay initial land conversion and slow down demolition and housing redevelopment. Initially, minimum lot size zoning is not binding. However, as city grows, it becomes binding and can effectively distort housing supply. It can lower both floor area ratio and residential density, and reduce aggregate housing supply. Overall, minimum lot size zoning can stabilize the path of structure/land ratios, housing service levels, structure density, and housing prices. In addition, minimum lot size zoning provides more incentive for developer to maintain the building, slow structure deterioration, and raise the minimum level of housing services provided over the life cycle of development.

[Heart-attack in pregnancy].

PubMed

Výtisková, T; Suchá, D; Fučíková, Z

To describe hear-attack on crystal meth addicted pregnant woman. Case report. Acute heart-attack during pregnancy means unexpected obstetric complication. The consequences could be fatal for the mother and the fetus. Although good delivery management and treatment could reduce morbidity and mortality to a minimum.

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

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

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

Sparsity-based image monitoring of crystal size distribution during crystallization

NASA Astrophysics Data System (ADS)

Liu, Tao; Huo, Yan; Ma, Cai Y.; Wang, Xue Z.

2017-07-01

To facilitate monitoring crystal size distribution (CSD) during a crystallization process by using an in-situ imaging system, a sparsity-based image analysis method is proposed for real-time implementation. To cope with image degradation arising from in-situ measurement subject to particle motion, solution turbulence, and uneven illumination background in the crystallizer, sparse representation of a real-time captured crystal image is developed based on using an in-situ image dictionary established in advance, such that the noise components in the captured image can be efficiently removed. Subsequently, the edges of a crystal shape in a captured image are determined in terms of the salience information defined from the denoised crystal images. These edges are used to derive a blur kernel for reconstruction of a denoised image. A non-blind deconvolution algorithm is given for the real-time reconstruction. Consequently, image segmentation can be easily performed for evaluation of CSD. The crystal image dictionary and blur kernels are timely updated in terms of the imaging conditions to improve the restoration efficiency. An experimental study on the cooling crystallization of α-type L-glutamic acid (LGA) is shown to demonstrate the effectiveness and merit of the proposed method.

Recent Advances in the Understanding of the Influence of Electric and Magnetic Fields on Protein Crystal Growth

DOE PAGES

Pareja-Rivera, Carina; Cuéllar-Cruz, Mayra; Esturau-Escofet, Nuria; ...

2016-12-05

Here, in this contribution we use nonconventional methods that help to increase the success rate of a protein crystal growth, and consequently of structural projects using X-ray diffraction techniques. In order to achieve this purpose, this contribution presents new approaches involving more sophisticated techniques of protein crystallization, not just for growing protein crystals of different sizes by using electric fields, but also for controlling crystal size and orientation. Also, this latter was possible through the use of magnetic fields that allow to obtain protein crystals suitable for both high-resolution X-ray and neutron diffraction crystallography where big crystals are required. Thismore » contribution discusses some pros, cons and realities of the role of electromagnetic fields in protein crystallization research, and their effect on protein crystal contacts. Additionally, we discuss the importance of room and low temperatures during data collection. Finally, we also discuss the effect of applying a rather strong magnetic field of 16.5 T, for shorts and long periods of time, on protein crystal growth, and on the 3D structure of two model proteins.« less

Approaching the Minimum Thermal Conductivity in Rhenium-Substituted Higher Manganese Silicides

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

Chen, Xi; Girard, S. N.; Meng, F.

Higher manganese silicides (HMS) made of earth-abundant and non-toxic elements are regarded as promising p-type thermoelectric materials because their complex crystal structure results in low lattice thermal conductivity. It is shown here that the already low thermal conductivity of HMS can be reduced further to approach the minimum thermal conductivity via partial substitu- tion of Mn with heavier rhenium (Re) to increase point defect scattering. The solubility limit of Re in the obtained RexMn1 xSi1.8 is determined to be about x = 0.18. Elemental inhomogeneity and the formation of ReSi1.75 inclusions with 50 200 nm size are found within themore » HMS matrix. It is found that the power factor does not change markedly at low Re content of x 0.04 before it drops considerably at higher Re contents. Compared to pure HMS, the reduced lattice thermal conductivity in RexMn1 xSi1.8 results in a 25% increase of the peak figure of merit ZT to reach 0.57 0.08 at 800 K for x = 0.04. The suppressed thermal conductivity in the pure RexMn1 xSi1.8 can enable further investigations of the ZT limit of this system by exploring different impurity doping strategies to optimize the carrier concentration and power factor.« less

Q-space analysis of light scattering by ice crystals

NASA Astrophysics Data System (ADS)

Heinson, Yuli W.; Maughan, Justin B.; Ding, Jiachen; Chakrabarti, Amitabha; Yang, Ping; Sorensen, Christopher M.

2016-12-01

Q-space analysis is applied to extensive simulations of the single-scattering properties of ice crystals with various habits/shapes over a range of sizes. The analysis uncovers features common to all the shapes: a forward scattering regime with intensity quantitatively related to the Rayleigh scattering by the particle and the internal coupling parameter, followed by a Guinier regime dependent upon the particle size, a complex power law regime with incipient two dimensional diffraction effects, and, in some cases, an enhanced backscattering regime. The effects of significant absorption on the scattering profile are also studied. The overall features found for the ice crystals are similar to features in scattering from same sized spheres.

An expanded model and application of the combined effect of crystal-size distribution and crystal shape on the relative viscosity of magmas

NASA Astrophysics Data System (ADS)

Klein, Johannes; Mueller, Sebastian P.; Helo, Christoph; Schweitzer, Silja; Gurioli, Lucia; Castro, Jonathan M.

2018-05-01

This study examines the combined effect of crystal-size distributions (CSD) and crystal shape on the rheology of vesicle free magmatic suspensions and provides the first practical application of an empirical model to estimate the relative effect of crystal content and CSD's on the viscosity of magma directly from textural image analysis of natural rock samples in the form of a user-friendly texture-rheology spreadsheet calculator. We extend and apply established relationships between the maximum packing fraction ϕm of a crystal bearing suspension and both its rheological properties and the polydispersity γ of a CSD. By using analogue rotational rheometric experiments with glass fibres and glass flakes in silicone oil acting as magma equivalent, this study also provides new insights in the relationship between ϕm and the aspect ratio rp of suspended particles.

A compact high resolution flat panel PET detector based on the new 4-side buttable MPPC for biomedical applications.

PubMed

Wang, Qiang; Wen, Jie; Ravindranath, Bosky; O'Sullivan, Andrew W; Catherall, David; Li, Ke; Wei, Shouyi; Komarov, Sergey; Tai, Yuan-Chuan

2015-09-11

Compact high-resolution panel detectors using virtual pinhole (VP) PET geometry can be inserted into existing clinical or pre-clinical PET systems to improve regional spatial resolution and sensitivity. Here we describe a compact panel PET detector built using the new Though Silicon Via (TSV) multi-pixel photon counters (MPPC) detector. This insert provides high spatial resolution and good timing performance for multiple bio-medical applications. Because the TSV MPPC design eliminates wire bonding and has a package dimension which is very close to the MPPC's active area, it is 4-side buttable. The custom designed MPPC array (based on Hamamatsu S12641-PA-50(x)) used in the prototype is composed of 4 × 4 TSV-MPPC cells with a 4.46 mm pitch in both directions. The detector module has 16 × 16 lutetium yttrium oxyorthosilicate (LYSO) crystal array, with each crystal measuring 0.92 × 0.92 × 3 mm 3 with 1.0 mm pitch. The outer diameter of the detector block is 16.8 × 16.8 mm 2 . Thirty-two such blocks will be arranged in a 4 × 8 array with 1 mm gaps to form a panel detector with detection area around 7 cm × 14 cm in the full-size detector. The flood histogram acquired with Ge-68 source showed excellent crystal separation capability with all 256 crystals clearly resolved. The detector module's mean, standard deviation, minimum (best) and maximum (worst) energy resolution were 10.19%, +/-0.68%, 8.36% and 13.45% FWHM, respectively. The measured coincidence time resolution between the block detector and a fast reference detector (around 200 ps single photon timing resolution) was 0.95 ns. When tested with Siemens Cardinal electronics the performance of the detector blocks remain consistent. These results demonstrate that the TSV-MPPC is a promising photon sensor for use in a flat panel PET insert composed of many high resolution compact detector modules.

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.

Direct observation of hierarchical nucleation of martensite and size-dependent superelasticity in shape memory alloys.

PubMed

Liu, Lifeng; Ding, Xiangdong; Li, Ju; Lookman, Turab; Sun, Jun

2014-02-21

Martensitic transformation usually creates hierarchical internal structures beyond mere change of the atomic crystal structure. Multi-stage nucleation is thus required, where nucleation (level-1) of the underlying atomic crystal lattice does not have to be immediately followed by the nucleation of higher-order superstructures (level-2 and above), such as polysynthetic laths. Using in situ transmission electron microscopy (TEM), we directly observe the nucleation of the level-2 superstructure in a Cu-Al-Ni single crystal under compression, with critical super-nuclei size L2c around 500 nm. When the sample size D decreases below L2c, the superelasticity behavior changes from a flat stress plateau to a continuously rising stress-strain curve. Such size dependence definitely would impact the application of shape memory alloys in miniaturized MEMS/NEMS devices.

Influence of a mineral insecticide particle size on bait efficacy against Reticulitermes flavipes (Isoptera: Rhinotermitidae)

Treesearch

Thomas g. Shelton; Laurent Cartier; Terence L. Wagner; Christian Becker

2007-01-01

We examined the efficacy of termiticidal baits comprised of powdered acellulose and a mineral insecticide, cryolite crystals, in laboratory bioassays against pseudergates of Eastern subterranean termites [Reticulitermes flavipes (Kollar)]. The influence of cryolite crystal size [0 (control), 0.2, and 20 pm diameter particles] on the overall mortality...

Controlling morphology and crystallite size of Cu(In{sub 0.7}Ga{sub 0.3})Se{sub 2} nano-crystals synthesized using a heating-up method

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

Hsu, Wei-Hsiang; Hsiang, Hsing-I, E-mail: hsingi@mail.ncku.edu.tw; Chia, Chih-Ta

2013-12-15

CuIn{sub 0.7}Ga{sub 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process. The non-coordinating solvent (1-octadecene) and selenium/cations ratio effects on the crystalline phase and crystallite size of CIGS nano-crystallites were investigated. It was observed that the CIGS nano-crystallite morphology changed from sheet into spherical shape as the amount of 1-octadecene addition was increased. CIGS nano-crystals were obtained in 9–20 nm sizes as the selenium/cations ratio increased. These results suggest that the monomer reactivity in the solution can be adjusted by changing the solvent type and selenium/cations ratio, hence affecting the crystallite size and distribution. - Graphical abstract: CuIn{sub 0.7}Ga{submore » 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process in this study. The super-saturation in the solution can be adjusted by changing the OLA/ODE ratio and selenium/cation ratio.« less

Barium recovery by crystallization in a fluidized-bed reactor: effects of pH, Ba/P molar ratio and seed.

PubMed

Su, Chia-Chi; Reano, Resmond L; Dalida, Maria Lourdes P; Lu, Ming-Chun

2014-06-01

The effects of process conditions, including upward velocity inside the column, the amount of added seed and seed size, the pH value of the precipitant or the phosphate stream and the Ba/P molar ratio in a fluidized-bed reactor (FBR) were studied with a view to producing BaHPO₄ crystals of significant size and maximize the removal of barium. XRD were used to identify the products that were collected from the FBR. Experimental results show that an upward velocity of 48 cmmin(-1) produced the largest BaHPO₄ crystals with a size of around 0.84-1.0mm. The addition of seed crystals has no effect on barium removal. The use of a seed of a size in the ranges unseeded<0.149-0.29 mm<0.149 mm<0.29-0.42 mm produced increasing amounts of increasingly large crystals. The largest BaHPO₄ crystals were obtained at pH 8.4-8.8 with a Ba/P molar ratio of 1.0. In the homogeneous and heterogeneous processes, around 98% of barium was removed at pH 8.4-8.6 and [Ba]/[P]=1.0. The XRD results show that a significant amount of barium phosphate (Ba₃(PO₄)₂) was obtained at pH 11. The compounds BaHPO₄ and BaO were present at a pH of below 10. Copyright © 2014 Elsevier Ltd. All rights reserved.

Concentrated aqueous sodium chloride solution in clays at thermodynamic conditions of hydraulic fracturing: Insight from molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Svoboda, Martin; Lísal, Martin

2018-06-01

To address a high salinity of flow-back water during hydraulic fracturing, we use molecular dynamics (MD) simulations and study the thermodynamics, structure, and diffusion of concentrated aqueous salt solution in clay nanopores. The concentrated solution results from the dissolution of a cubic NaCl nanocrystal, immersed in an aqueous NaCl solution of varying salt concentration and confined in clay pores of a width comparable to the crystal size. The size of the nanocrystal equals to about 18 Å which is above a critical nucleus size. We consider a typical shale gas reservoir condition of 365 K and 275 bar, and we represent the clay pores as pyrophyllite and Na-montmorillonite (Na-MMT) slits. We employ the Extended Simple Point Charge (SPC/E) model for water, Joung-Cheatham model for ions, and CLAYFF for the slit walls. We impose the pressure in the normal direction and the resulting slit width varies from about 20 to 25 Å when the salt concentration in the surrounding solution increased from zero to an oversaturated value. By varying the salt concentration, we observe two scenarios. First, the crystal dissolves and its dissolution time increases with increasing salt concentration. We describe the dissolution process in terms of the number of ions in the crystal, and the crystal size and shape. Second, when the salt concentration reaches a system solubility limit, the crystal grows and attains a new equilibrium size; the crystal comes into equilibrium with the surrounding saturated solution. After crystal dissolution, we carry out canonical MD simulations for the concentrated solution. We evaluate the hydration energy, density profiles, orientation distributions, hydrogen-bond network, radial distribution functions, and in-plane diffusion of water and ions to provide insight into the microscopic behaviour of the concentrated aqueous sodium chloride solution in interlayer galleries of the slightly hydrophobic pyrophyllite and hydrophilic Na-MMT pores.

Concentrated aqueous sodium chloride solution in clays at thermodynamic conditions of hydraulic fracturing: Insight from molecular dynamics simulations.

PubMed

Svoboda, Martin; Lísal, Martin

2018-06-14

To address a high salinity of flow-back water during hydraulic fracturing, we use molecular dynamics (MD) simulations and study the thermodynamics, structure, and diffusion of concentrated aqueous salt solution in clay nanopores. The concentrated solution results from the dissolution of a cubic NaCl nanocrystal, immersed in an aqueous NaCl solution of varying salt concentration and confined in clay pores of a width comparable to the crystal size. The size of the nanocrystal equals to about 18 Å which is above a critical nucleus size. We consider a typical shale gas reservoir condition of 365 K and 275 bar, and we represent the clay pores as pyrophyllite and Na-montmorillonite (Na-MMT) slits. We employ the Extended Simple Point Charge (SPC/E) model for water, Joung-Cheatham model for ions, and CLAYFF for the slit walls. We impose the pressure in the normal direction and the resulting slit width varies from about 20 to 25 Å when the salt concentration in the surrounding solution increased from zero to an oversaturated value. By varying the salt concentration, we observe two scenarios. First, the crystal dissolves and its dissolution time increases with increasing salt concentration. We describe the dissolution process in terms of the number of ions in the crystal, and the crystal size and shape. Second, when the salt concentration reaches a system solubility limit, the crystal grows and attains a new equilibrium size; the crystal comes into equilibrium with the surrounding saturated solution. After crystal dissolution, we carry out canonical MD simulations for the concentrated solution. We evaluate the hydration energy, density profiles, orientation distributions, hydrogen-bond network, radial distribution functions, and in-plane diffusion of water and ions to provide insight into the microscopic behaviour of the concentrated aqueous sodium chloride solution in interlayer galleries of the slightly hydrophobic pyrophyllite and hydrophilic Na-MMT pores.

Understanding Crystal Populations; Looking Towards 3D Quantitative Analysis

NASA Astrophysics Data System (ADS)

Jerram, D. A.; Morgan, D. J.

2010-12-01

In order to understand volcanic systems, the potential record held within crystal populations needs to be revealed. It is becoming increasingly clear, however, that the crystal populations that arrive at the surface in volcanic eruptions are commonly mixtures of crystals, which may be representative of simple crystallization, recycling of crystals and incorporation of alien crystals. If we can quantify the true 3D population within a sample then we will be able to separate crystals with different histories and begin to interrogate the true and complex plumbing within the volcanic system. Modeling crystal populations is one area where we can investigate the best methodologies to use when dealing with sections through 3D populations. By producing known 3D shapes and sizes with virtual textures and looking at the statistics of shape and size when such populations are sectioned, we are able to gain confidence about what our 2D information is telling us about the population. We can also use this approach to test the size of population we need to analyze. 3D imaging through serial sectioning or x-ray CT, provides a complete 3D quantification of a rocks texture. Individual phases can be identified and in principle the true 3D statistics of the population can be interrogated. In practice we need to develop strategies (as with 2D-3D transformations), that enable a true characterization of the 3D data, and an understanding of the errors and pitfalls that exist. Ultimately, the reproduction of true 3D textures and the wealth of information they hold, is now within our reach.

Monitoring and modeling of ultrasonic wave propagation in crystallizing mixtures

NASA Astrophysics Data System (ADS)

Marshall, T.; Challis, R. E.; Tebbutt, J. S.

2002-05-01

The utility of ultrasonic compression wave techniques for monitoring crystallization processes is investigated in a study of the seeded crystallization of copper II sulfate pentahydrate from aqueous solution. Simple models are applied to predict crystal yield, crystal size distribution and the changing nature of the continuous phase. A scattering model is used to predict the ultrasonic attenuation as crystallization proceeds. Experiments confirm that modeled attenuation is in agreement with measured results.

Rice-like hollow nano-CaCO3 synthesis

NASA Astrophysics Data System (ADS)

Ulkeryildiz, Eda; Kilic, Sevgi; Ozdemir, Ekrem

2016-09-01

We have shown that Ca(OH)2 solution is a natural stabilizer for CaCO3 particles. We designed a CO2 bubbling crystallization reactor to produce nano-CaCO3 particles in homogenous size distribution without aggregation. In the experimental set-up, the crystallization region was separated from the stabilization region. The produced nanoparticles were removed from the crystallization region into the stabilization region before aggregation or crystal growth. It was shown that rice-like hollow nano-CaCO3 particles in about 250 nm in size were produced with almost monodispersed size distribution. The particles started to dissolve through their edges as CO2 bubbles were injected, which opened-up the pores inside the particles. At the late stages of crystallization, the open pores were closed as a result of dissolution-recrystallization of the newly synthesized CaCO3 particles. These particles were stable in Ca(OH)2 solution and no aggregation was detected. The present methodology can be used in drug encapsulation into inorganic CaCO3 particles for cancer treatment with some modifications.

Modified DHTT Equipment for Crystallization Studies of Mold Slags

NASA Astrophysics Data System (ADS)

Kölbl, Nathalie; Harmuth, Harald; Marschall, Irmtraud

2018-04-01

The double hot thermocouple technique (DHTT) enables simulations of the temperature gradient at near-service conditions during continuous casting of steel. With the equipment applied so far, a rectangular slag film of even thickness often cannot be achieved. Further, the minimum temperature frequently lies within the slag film. Modified equipment can avoid these disadvantages via the following design features. The entire furnace chamber is heated to the selected temperature of the cold wire, and the minimum temperature is not located within the slag film. Furthermore, the shape of the heating wire is improved, which enables mounting of a thin, rectangular slag film between four platinum wires. This modification allows for investigations on transparent and translucent slags. So far, the results from DHTT investigations were represented via snapshots of the samples at certain experimental times. Therefore, appropriate methods for the graphical representation of the results were suggested: the maximum crystallinity, the time related to certain crystallinities with a dependence on the position within the slag film, and the crystal growth rate. The CaO-MgO-Al2O3-SiO2 slag investigated with this equipment was mineralogically examined additionally, and based on thermodynamic calculations, the allocation of temperatures to certain positions within the crystallized slag film was possible.

Highly anisotropic solar-blind UV photodetector based on large-size two-dimensional α-MoO3 atomic crystals

NASA Astrophysics Data System (ADS)

Zhong, Mianzeng; Zhou, Ke; Wei, Zhongming; Li, Yan; Li, Tao; Dong, Huanli; Jiang, Lang; Li, Jingbo; Hu, Wenping

2018-07-01

Orthorhombic MoO3 (α-MoO3) is a typical layered n-type semiconductor with optical band gap over 2.7 eV, which have been widely studied in catalysis, gas sensing, lithium-ion batteries, field-emission, photoelectrical, photochromic and electrochromic devices, supercapacitors and organic solar cells. However, the bottleneck of generation large size atomic thin two-dimensional (2D) α-MoO3 crystals remain challenging this field (normally several micrometers size). Herein, we developed a facile vapor–solid (VS) process for controllable growth of large-size 2D α-MoO3 single crystals with a few nanometers thick and over 300 μm in lateral size. High-performance solar-blind photodetectors were fabricated based on individual 2D α-MoO3 single crystal. The detectors demonstrate outstanding optoelectronic properties under solar-blind UV light (254 nm), with a photoresponsivity of 67.9 A W‑1, external quantum efficiency of 3.3  ×  104%. More important, the devices showed strong in-plane anisotropy in optoelectronic response and transport properties, e.g. the photocurrent along b-axis was found to be 5 times higher than the values along c-axis under 254 nm UV light, and current ON/OFF ratio and mobility anisotropy is about 2 times high. Our work suggests an optimized synthesis routine for 2D crystals, and the great potential of 2D oxides in functional optoelectronics.

Encapsulation of Multiple Microalgal Cells via a Combination of Biomimetic Mineralization and LbL Coating

PubMed Central

Kim, Minjeong; Choi, Myoung Gil; Ra, Ho Won; Park, Seung Bin; Kim, Yong-Joo; Lee, Kyubock

2018-01-01

The encapsulation of living cells is appealing for its various applications to cell-based sensors, bioreactors, biocatalysts, and bioenergy. In this work, we introduce the encapsulation of multiple microalgal cells in hollow polymer shells of rhombohedral shape by the following sequential processes: embedding of microalgae in CaCO3 crystals; layer-by-layer (LbL) coating of polyelectrolytes; and removal of sacrificial crystals. The microcapsule size was controlled by the alteration of CaCO3 crystal size, which is dependent on CaCl2/Na2CO3 concentration. The microalgal cells could be embedded in CaCO3 crystals by a two-step process: heterogeneous nucleation of crystal on the cell surface followed by cell embedment by the subsequent growth of crystal. The surfaces of the microalgal cells were highly favorable for the crystal growth of calcite; thus, micrometer-sized microalgae could be perfectly occluded in the calcite crystal without changing its rhombohedral shape. The surfaces of the microcapsules, moreover, could be decorated with gold nanoparticles, Fe3O4 magnetic nanoparticles, and carbon nanotubes (CNTs), by which we would expect the functionalities of a light-triggered release, magnetic separation, and enhanced mechanical and electrical strength, respectively. This approach, entailing the encapsulation of microalgae in semi-permeable and hollow polymer microcapsules, has the potential for application to microbial-cell immobilization for high-biomass-concentration cultivation as well as various other bioapplications. PMID:29438340

Chemical composition, crystal size and lattice structural changes after incorporation of strontium into biomimetic apatite.

PubMed

Li, Z Y; Lam, W M; Yang, C; Xu, B; Ni, G X; Abbah, S A; Cheung, K M C; Luk, K D K; Lu, W W

2007-03-01

Recently, strontium (Sr) as ranelate compound has become increasingly popular in the treatment of osteoporosis. However, the lattice structure of bone crystal after Sr incorporation is yet to be extensively reported. In this study, we synthesized strontium-substituted hydroxyapatite (Sr-HA) with different Sr content (0.3%, 1.5% and 15% Sr-HA in mole ratio) to simulate bone crystals incorporated with Sr. The changes in chemical composition and lattice structure of apetite after synthetic incorporation of Sr were evaluated to gain insight into bone crystal changes after incorporation of Sr. X-ray diffraction (XRD) patterns revealed that 0.3% and 1.5% Sr-HA exhibited single phase spectrum, which was similar to that of HA. However, 15% Sr-HA induced the incorporation of HPO4(2-) and more CO3(2-), the crystallinity reduced dramatically. Transmission electron microscopy (TEM) images showed that the crystal length and width of 0.3% and 1.5% Sr-HA increased slightly. Meanwhile, the length and width distribution were broadened and the aspect ratio decreased from 10.68+/-4.00 to 7.28+/-2.80. The crystal size and crystallinity of 15% Sr-HA dropped rapidly, which may suggest that the fundamental crystal structure is changed. The findings from this work indicate that current clinical dosage which usually results in Sr incorporation of below 1.5% may not change chemical composition and lattice structure of bone, while it will broaden the bone crystal size distribution and strengthen the bone.

Historical and New Perspective of Moissanite in the Canyon Diablo Meteorite

NASA Astrophysics Data System (ADS)

Leung, I. S.; Winston, R.

2004-12-01

Silicon carbide (SiC) was reportedly found in the residue of a 50-kg sample of the Canyon Diablo meteorite dissolved in acid by Henri Moissan, and, in his honor, George F. Kunz coined the mineral name moissanite in 1904. Scholars of the same meteorite, unable to find SiC, believed that Moissan's sample might have been contaminated by synthetic SiC used in tools and abrasives. Thus, an intriguing mineralogical controversy ensued to this day. Recently, occurrence of SiC in carbonaceous chondrites has been confirmed. We present in this paper our finding of three varieties of SiC crystals in the Canyon Diablo meteorite. We found 5 crystals of SiC (size 70-150 microns) in a black nodule (1 cm in size), composed mostly of disordered graphite and diamond/lonsdaleite. The crystals are pale blue, but some have dark overgrowths of uneven thickness, and black spotty or feathery inclusions. Their forms are rounded and resorbed. Our second specimen is oxidized and friable, bearing a 2-cm nodule showing sandy and black magnetic layers. We found 3 apple-green crystals, up to 200 microns in size. Scattered over two of the sandy layers are many minute emerald-green SiC crystals. Carbon in these crystals might have a terrestrial origin. As Moissan's crystals are no longer available for re-examination, a study of large carbon nodules housed in museums might at least lend credence that meteoritic SiC crystals could be as large as ones reported by Moissan.

7 CFR 51.2836 - Size classifications.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 2 2012-01-01 2012-01-01 false Size classifications. 51.2836 Section 51.2836...) Size Classifications § 51.2836 Size classifications. The size of onions may be specified in accordance with one of the following classifications. Size designation Minimum diameter Inches Millimeters Maximum...

7 CFR 51.2836 - Size classifications.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 2 2013-01-01 2013-01-01 false Size classifications. 51.2836 Section 51.2836...-Granex-Grano and Creole Types) Size Classifications § 51.2836 Size classifications. The size of onions may be specified in accordance with one of the following classifications. Size designation Minimum...

7 CFR 51.2836 - Size classifications.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 2 2014-01-01 2014-01-01 false Size classifications. 51.2836 Section 51.2836...-Granex-Grano and Creole Types) Size Classifications § 51.2836 Size classifications. The size of onions may be specified in accordance with one of the following classifications. Size designation Minimum...

7 CFR 51.2836 - Size classifications.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Size classifications. 51.2836 Section 51.2836...) Size Classifications § 51.2836 Size classifications. The size of onions may be specified in accordance with one of the following classifications. Size designation Minimum diameter Inches Millimeters Maximum...

7 CFR 51.2836 - Size classifications.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Size classifications. 51.2836 Section 51.2836...) Size Classifications § 51.2836 Size classifications. The size of onions may be specified in accordance with one of the following classifications. Size designation Minimum diameter Inches Millimeters Maximum...

Population demographics and genetic diversity in remnant and translocated populations of sea otters

USGS Publications Warehouse

Bodkin, James L.; Ballachey, Brenda E.; Cronin, M.A.; Scribner, K.T.

1999-01-01

The effects of small population size on genetic diversity and subsequent population recovery are theoretically predicted, but few empirical data are available to describe those relations. We use data from four remnant and three translocated sea otter (Enhydra lutris) populations to examine relations among magnitude and duration of minimum population size, population growth rates, and genetic variation. Metochondrial (mt)DNA haplotype diversity was correlated with the number of years at minimum population size (r = -0.741, p = 0.038) and minimum population size (r = 0.709, p = 0.054). We found no relation between population growth and haplotype diversity, altough growth was significantly greater in translocated than in remnant populations. Haplotype diversity in populations established from two sources was higher than in a population established from a single source and was higher than in the respective source populations. Haplotype frequencies in translocated populations of founding sizes of 4 and 28 differed from expected, indicating genetic drift and differential reproduction between source populations, whereas haplotype frequencies in a translocated population with a founding size of 150 did not. Relations between population demographics and genetic characteristics suggest that genetic sampling of source and translocated populations can provide valuable inferences about translocations.

Characterizing the effect of growth conditions and crystal habit on the distribution of imperfections amongst populations of crystals

NASA Astrophysics Data System (ADS)

Price, C. J.

1993-03-01

The distribution of gross imperfections amongst populations of copper sulphate pentahydrate crystals grown under different conditions of purity and temperature are examined. The frequency of imperfection increases with decreasing crystal size. The nature of the imperfections vary with growth temperature and impurities present.

Modeling of the effect of freezer conditions on the hardness of ice cream using response surface methodology.

PubMed

Inoue, K; Ochi, H; Habara, K; Taketsuka, M; Saito, H; Ichihashi, N; Iwatsuki, K

2009-12-01

The effect of conventional continuous freezer parameters [mix flow (L/h), overrun (%), drawing temperature ( degrees C), cylinder pressure (kPa), and dasher speed (rpm)] on the hardness of ice cream under varying measured temperatures (-5, -10, and -15 degrees C) was investigated systematically using response surface methodology (central composite face-centered design), and the relationships were expressed as statistical models. The range (maximum and minimum values) of each freezer parameter was set according to the actual capability of the conventional freezer and applicability to the manufacturing process. Hardness was measured using a penetrometer. These models showed that overrun and drawing temperature had significant effects on hardness. The models can be used to optimize freezer conditions to make ice cream of the least possible hardness under the highest overrun (120%) and a drawing temperature of approximately -5.5 degrees C (slightly warmer than the lowest drawing temperature of -6.5 degrees C) within the range of this study. With reference to the structural elements of the ice cream, we suggest that the volume of overrun and ice crystal content, ice crystal size, and fat globule destabilization affect the hardness of ice cream. In addition, the combination of a simple instrumental parameter and response surface methodology allows us to show the relation between freezer conditions and one of the most important properties-hardness-visually and quantitatively on the practical level.

A Real Options Approach to Quantity and Cost Optimization for Lifetime and Bridge Buys of Parts

DTIC Science & Technology

2015-04-30

fixed EOS of 40 years and a fixed WACC of 3%, decreases to a minimum and then increases. The minimum of this curve gives the optimum buy size for...considered in both analyses. For a 3% WACC , as illustrated in Figure 9(a), the DES method gives an optimum buy size range of 2,923–3,191 with an average...Hence, both methods are consistent in determining the optimum lifetime/bridge buy size. To further verify this consistency, other WACC values

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

NASA Technical Reports Server (NTRS)

Landis, W. J.; Hodgens, K. J.; Arena, J.; Song, M. J.; McEwen, B. F.

1996-01-01

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

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.

Microstructural indicators of convection: insights from the Little Minch Sill Complex, Scotland

NASA Astrophysics Data System (ADS)

Nicoli, Gautier; Holness, Marian; Neufeld, Jerome; Farr, Robert

2017-04-01

The fluid dynamic behaviour of crystal-bearing magmas is a key parameter to understand the formation of magmatic bodies. There are two opposite views on the subject: Some argue that solidification in intrusive bodies is affected by convection whereas others claim solidification happens in a static environment. A consensus on the question may be reached by carefully studying the grain size distribution in the settled accumulations of cargo crystals. In the absence of significant crystal growth or particle coarsening by agglomeration, settling of a polydisperse crystal load will always result in a fining-upwards sequence in static magmas as well as in convecting environments. If we assume the particle concentration is always sufficiently low to prevent hindered settling, gravitational settling in a static magma leads to the settling of individual crystals at a constant rate determined by their Stokes' velocity. Each size class is deposited at a constant rate, until all the grains of that size class have fallen out of suspension, leading to a well-stratified sequence and the complete disappearance of progressively smaller size classes upwards in the accumulation. In contrast, in a vigorously convecting magma crystals settle when they enter the stagnant basal boundary layer. In a system containing a polydisperse crystal population most of the bigger particles are removed rapidly from the bulk magma, leading to the creation of a fining-upwards sequence on the floor. However, in detail the structure of this fining-upwards sequence is critically different from that created by settling from a stagnant magma, with the gradual phasing out of each size class instead of the abrupt termination of size classes seen in static systems. This provides us with the opportunity to distinguish between settling from static or convecting magma using the spatial variation of grain size in settled accumulations. We focus on the Little Minch Sill Complex in Scotland, which formed from olivine-phyric magma and is characterised by both composite and single-injection bodies with significant accumulation of olivine on their lower margins. Comparison of the fining-upwards sequences in the picrodolerite/crinanite unit of the composite Shiant Isles Main Sill,and related single-injection sills on the Trotternish Peninsula, Skye, illustrate the ability of this method to distinguish between convecting and non-convecting magma bodies.

CrystalMoM: a tool for modeling the evolution of Crystals Size Distributions in magmas with the Method of Moments

NASA Astrophysics Data System (ADS)

Colucci, Simone; de'Michieli Vitturi, Mattia; Landi, Patrizia

2016-04-01

It is well known that nucleation and growth of crystals play a fundamental role in controlling magma ascent dynamics and eruptive behavior. Size- and shape-distribution of crystal populations can affect mixture viscosity, causing, potentially, transitions between effusive and explosive eruptions. Furthermore, volcanic samples are usually characterized in terms of Crystal Size Distribution (CSD), which provide a valuable insight into the physical processes that led to the observed distributions. For example, a large average size can be representative of a slow magma ascent, and a bimodal CSD may indicate two events of nucleation, determined by two degassing events within the conduit. The Method of Moments (MoM), well established in the field of chemical engineering, represents a mesoscopic modeling approach that rigorously tracks the polydispersity by considering the evolution in time and space of integral parameters characterizing the distribution, the moments, by solving their transport differential-integral equations. One important advantage of this approach is that the moments of the distribution correspond to quantities that have meaningful physical interpretations and are directly measurable in natural eruptive products, as well as in experimental samples. For example, when the CSD is defined by the number of particles of size D per unit volume of the magmatic mixture, the zeroth moment gives the total number of crystals, the third moment gives the crystal volume fraction in the magmatic mixture and ratios between successive moments provide different ways to evaluate average crystal length. Tracking these quantities, instead of volume fraction only, will allow using, for example, more accurate viscosity models in numerical code for magma ascent. Here we adopted, for the first time, a quadrature based method of moments to track the temporal evolution of CSD in a magmatic mixture and we verified and calibrated the model again experimental data. We also show how the equations and the tool developed can be integrated in a magma ascent numerical model, with application to eruptive events occurred at Stromboli volcano (Italy).

Photocurrent enhancement of n-type Cu2O electrodes achieved by controlling dendritic branching growth.

PubMed

McShane, Colleen M; Choi, Kyoung-Shin

2009-02-25

Cu(2)O electrodes composed of dendritic crystals were produced electrochemically using a slightly acidic medium (pH 4.9) containing acetate buffer. The buffer played a key role for stabilizing dendritic branching growth as a pH drop during the synthesis prevents formation of morphologically unstable branches and promotes faceted growth. Dendritic branching growth enabled facile coverage of the substrate with Cu(2)O while avoiding growth of a thicker Cu(2)O layer and increasing surface areas. The resulting electrodes showed n-type behavior by generating anodic photocurrent without applying an external bias (zero-bias photocurrent under short-circuit condition) in an Ar-purged 0.02 M K(2)SO(4) solution. The zero-bias photocurrent of crystalline dendritic electrodes was significantly higher than that of the electrodes containing micrometer-size faceted crystals deposited without buffer. In order to enhance photocurrent further a strategy of improving charge-transport properties by increasing dendritic crystal domain size was investigated. Systematic changes in nucleation density and size of the dendritic Cu(2)O crystals were achieved by altering the deposition potential, Cu(2+) concentration, and acetate concentration. Increasing dendritic crystal size consistently resulted in the improvement of photocurrent regardless of the method used to regulate crystal size. The electrode composed of dendritic crystals with the lateral dimension of ca. 12000 microm(2) showed more than 20 times higher zero-bias photocurrent than that composed of dendritic crystals with the lateral dimension of ca. 100 microm(2). The n-type nature of the Cu(2)O electrodes prepared by this study were confirmed by linear sweep voltammetry with chopped light and capacitance measurements (i.e., Mott-Schottky plots). The flatband potential in a 0.2 M K(2)SO(4) solution (pH 6) was estimated to be -0.78 vs Ag/AgCl reference electrode. The IPCE measured without applying an external bias was approximately 1% for the visible region. With appropriate doping studies and surface treatment to improve charge transport and interfacial kinetics more efficient n-type Cu(2)O electrodes will be prepared for use in various photoelectrochemical and photovoltaic devices.

Pin-Hole Free Perovskite Film for Solar Cells Application Prepared by Controlled Two-Step Spin-Coating Method

NASA Astrophysics Data System (ADS)

Bahtiar, A.; Rahmanita, S.; Inayatie, Y. D.

2017-05-01

Morphology of perovskite film is a key important for achieving high performance perovskite solar cells. Perovskite films are commonly prepared by two-step spin-coating method. However, pin-holes are frequently formed in perovskite films due to incomplete conversion of lead-iodide (PbI2) into perovskite CH3NH3PbI3. Pin-holes in perovskite film cause large hysteresis in current-voltage curve of solar cells due to large series resistance between perovskite layer-hole transport material. Moreover, crystal structure and grain size of perovskite crystal are also other important parameters for achieving high performance solar cells, which are significantly affected by preparation of perovskite film. We studied the effect of preparation of perovskite film using controlled spin-coating parameters on crystal structure and morphological properties of perovskite film. We used two-step spin-coating method for preparation of perovskite film with varied spinning speed, spinning time and temperature of spin-coating process to control growth of perovskite crystal aimed to produce high quality perovskite crystal with pin-hole free and large grain size. All experiment was performed in air with high humidity (larger than 80%). The best crystal structure, pin-hole free with large grain crystal size of perovskite film was obtained from film prepared at room temperature with spinning speed 1000 rpm for 20 seconds and annealed at 100°C for 300 seconds.

Supersaturation of aqueous species and hydrothermal crystal growth of ZnO

NASA Astrophysics Data System (ADS)

Gelabert, M. C.

2015-05-01

Synthesis of ZnO crystals prepared with zinc acetate or chloride, disodium dihydrogen ethylenediaminetetraacetate (EDTA), potassium hydroxide and sodium triflate at 200 °C and variable pH 8-12 is reported. Crystals were imaged and size-analyzed with optical microscopy. Using aqueous speciation modeling software, supersaturation dependence on pH was calculated for five zinc species-Zn2+, Zn(OH)+, Zn(OH)2, Zn(OH)3- and Zn(OH)42- -to investigate connections between predominate crystal habits at different pH and dominant aqueous species. For zinc acetate and chloride systems, the zinc species with highest supersaturation was Zn(OH)42- throughout the pH 8-12 range, and the second highest was Zn2+ or Zn(OH)3-, with a crossover pH of 10.2-10.4 depending on counterion. The prominence of the tetrahydroxyl zinc species in ZnO crystal growth is supported by these calculations, and total supersaturation is inversely proportional to average crystal sizes, as expected. Optical microscopy and size analysis on products revealed crystals with a needle or prismatic habit throughout the studied pH range, and the change in aspect ratio correlates with supersaturation changes for the Zn2+ in this pH range, thus suggesting that growth rates along the [001] crystallographic direction are affected by small concentration changes of this ion.

Size Controllable, Transparent, and Flexible 2D Silver Meshes Using Recrystallized Ice Crystals as Templates.

PubMed

Wu, Shuwang; Li, Linhai; Xue, Han; Liu, Kai; Fan, Qingrui; Bai, Guoying; Wang, Jianjun

2017-10-24

Ice templates have been widely utilized for the preparation of porous materials due to the obvious advantages, such as environmentally benign and applicable to a wide range of materials. However, it remains a challenge to have controlled pore size as well as dimension of the prepared porous materials with the conventional ice template, since it often employs the kinetically not-stable growing ice crystals as the template. For example, there is no report so far for the preparation of 2D metal meshes with tunable pore size based on the ice template, although facile and eco-friendly prepared metal meshes are highly desirable for wearable electronics. Here, we report the preparation of 2D silver meshes with tunable mesh size employing recrystallized ice crystals as templates. Ice recrystallization is a kinetically stable process; therefore, the grain size of recrystallized ice crystals can be easily tuned, e.g., by adding different salts and changing the annealing temperature. Consequently, the size and line width of silver meshes obtained after freeze-drying can be easily adjusted, which in turn varied the conductivity of the obtained 2D silver film. Moreover, the silver meshes are transparent and display stable conductivity after the repeated stretching and bending. It can be envisioned that this approach for the preparation of 2D conducting films is of practical importance for wearable electronics. Moreover, this study provides a generic approach for the fabrication of 2D meshes with a controllable pore size.

The deformation mechanisms and size effects of single-crystal magnesium

NASA Astrophysics Data System (ADS)

Byer, Cynthia M.

In this work, we seek to understand the deformation mechanisms and size effects of single-crystal magnesium at the micrometer scale through both microcompression experiments and finite element simulations. Microcompression experiments are conducted to investigate the impact of initial dislocation density and orientation on size effects. Micropillars are fabricated using a focused ion beam and tested in a Nanoindenter using a diamond fiat tip as a compression platen. Two different initial dislocation densities are examined for [0001] oriented micropillars. Our results demonstrate that decreasing the initial dislocation density results in an increased size effect in terms of increased strength and stochasticity. Microcompression along the [23¯14] axis results in much lower strengths than for [0001] oriented samples. Post-mortem analysis reveals basal slip in both [0001] and [23¯14] micropillars. The application of a stochastic probability model shows good agreement between theoretical predictions and experimental results for size effects with our values of initial dislocation density and micropillar dimensions. Size effects are then incorporated into a single-crystal plasticity model (modified from Zhang and Joshi [1]) implemented in ABAQUS/STANDARD as a user-material subroutine. The model successfully captures the phenomena typically associated with size effects of increasing stochasticity and strength with decreasing specimen size and also accounts for the changing trends resulting from variations in initial dislocation density that we observe in the experiments. Finally, finite element simulations are performed with the original (traditional, without size effects) crystal plasticity model [1] to investigate the relative activities of the deformation modes of single-crystal magnesium for varying degrees of misalignment in microcompression. The simulations reveal basal activity in all micropillars, even for perfectly aligned compression along the [0001] axis. Pyramidal < c + a > activity dominates until the misalignment increases to 2°, when basal slip takes over as the dominant mode. The stress-strain curves for the case of 0° misalignment agrees well with experimental curves, indicating that good alignment was achieved during the experiments. Through this investigation, we gain a better understanding of how to control the size effects, as well as the deformation mechanisms operating at the small scale in magnesium.

On the influence of crystal size and wavelength on native SAD phasing.

PubMed

Liebschner, Dorothee; Yamada, Yusuke; Matsugaki, Naohiro; Senda, Miki; Senda, Toshiya

2016-06-01

Native SAD is an emerging phasing technique that uses the anomalous signal of native heavy atoms to obtain crystallographic phases. The method does not require specific sample preparation to add anomalous scatterers, as the light atoms contained in the native sample are used as marker atoms. The most abundant anomalous scatterer used for native SAD, which is present in almost all proteins, is sulfur. However, the absorption edge of sulfur is at low energy (2.472 keV = 5.016 Å), which makes it challenging to carry out native SAD phasing experiments as most synchrotron beamlines are optimized for shorter wavelength ranges where the anomalous signal of sulfur is weak; for longer wavelengths, which produce larger anomalous differences, the absorption of X-rays by the sample, solvent, loop and surrounding medium (e.g. air) increases tremendously. Therefore, a compromise has to be found between measuring strong anomalous signal and minimizing absorption. It was thus hypothesized that shorter wavelengths should be used for large crystals and longer wavelengths for small crystals, but no thorough experimental analyses have been reported to date. To study the influence of crystal size and wavelength, native SAD experiments were carried out at different wavelengths (1.9 and 2.7 Å with a helium cone; 3.0 and 3.3 Å with a helium chamber) using lysozyme and ferredoxin reductase crystals of various sizes. For the tested crystals, the results suggest that larger sample sizes do not have a detrimental effect on native SAD data and that long wavelengths give a clear advantage with small samples compared with short wavelengths. The resolution dependency of substructure determination was analyzed and showed that high-symmetry crystals with small unit cells require higher resolution for the successful placement of heavy atoms.

Homogeneous crystal nucleation in Ni droplets

NASA Astrophysics Data System (ADS)

Kožíšek, Zdeněk; Demo, Pavel

2017-10-01

Crystal nucleation kinetics is often represented by induction times or metastable zone widths (Kulkarni et al., 2013; Bokeloh et al., 2011). Repeating measurements of supercooling or time delay, at which phase transition is detected, are statistically processed to determine the so-called survivorship function, from which nucleation rate is computed. The size distribution of nuclei is difficult to measure near the critical size directly, and it is not clear which amount of nuclei is formed at the moment when the phase transition is detected. In the present paper, kinetic nucleation equations are solved for the crystal nucleation in Ni liquid droplet to determine the number of nuclei formed within a considered system. Analysis of supercooling experimental data, based on the classical nucleation theory CNT), computes appropriate values of the nucleation rate. However, CNT underestimates the number of nuclei F (F ≪ 1 for supercritical sizes). Taking into account the dependence of the surface energy on nucleus size to data analysis overcomes this discrepancy and leads to reasonable values of the size distribution of nuclei.

Geometrically distributed one-dimensional photonic crystals for light-reflection in all angles.

PubMed

Alagappan, G; Wu, P

2009-07-06

We demonstrate that a series of one-dimensional photonic crystals made of any dielectric materials, with the periods are distributed in a geometrical progression of a common ratio, r < rc (theta,P), where rc is a structural parameter that depends on the angle of incidence, theta, and polarization, P, is capable of blocking light of any spectral range. If an omni-directional reflection is desired for all polarizations and for all incident angles smaller than thetao, then r < rc (theta(o),p), where p is the polarization with the electric field parallel to the plane of incidence. We present simple and formula like expressions for rc, width of the bandgap, and minimum number of photonic crystals to achieve a perfect light reflection.

Minimum length from quantum mechanics and classical general relativity.

PubMed

Calmet, Xavier; Graesser, Michael; Hsu, Stephen D H

2004-11-19

We derive fundamental limits on measurements of position, arising from quantum mechanics and classical general relativity. First, we show that any primitive probe or target used in an experiment must be larger than the Planck length lP. This suggests a Planck-size minimum ball of uncertainty in any measurement. Next, we study interferometers (such as LIGO) whose precision is much finer than the size of any individual components and hence are not obviously limited by the minimum ball. Nevertheless, we deduce a fundamental limit on their accuracy of order lP. Our results imply a device independent limit on possible position measurements.

Equilibrium shape of 4He crystal under zero gravity below 200 mK

PubMed Central

Takahashi, Takuya; Ohuchi, Haruka; Nomura, Ryuji; Okuda, Yuichi

2015-01-01

Equilibrium crystal shape is the lowest energy crystal shape that is hardly realized in ordinary crystals because of their slow relaxation. 4He quantum crystals in a superfluid have been expected as unique exceptions that grow extremely fast at very low temperatures. However, on the ground, gravity considerably deforms the crystals and conceals the equilibrium crystal shape, and thus, gravity-free environment is needed to observe the equilibrium shape of 4He. We report the relaxation processes of macroscopic 4He crystals in a superfluid below 200 mK under zero gravity using a parabolic flight of a jet plane. When gravity was removed from a gravity-flattened 4He crystal, the crystal rapidly transformed into a shape with flat surfaces. Although the relaxation processes were highly dependent on the initial condition, the crystals relaxed to a nearly homothetic shape in the end, indicating that they were truly in an equilibrium shape minimizing the interfacial free energy. Thanks to the equilibrium shape, we were able to determine the Wulff’s origin and the size of the c-facet together with the vicinal surface profile next to the c-facet. The c-facet size was extremely small in the quantum crystals, and the facet-like flat surfaces were found to be the vicinal surfaces. At the same time, the interfacial free energy of the a-facet and s-facet was also obtained. PMID:26601315

Equilibrium shape of (4)He crystal under zero gravity below 200 mK.

PubMed

Takahashi, Takuya; Ohuchi, Haruka; Nomura, Ryuji; Okuda, Yuichi

2015-10-01

Equilibrium crystal shape is the lowest energy crystal shape that is hardly realized in ordinary crystals because of their slow relaxation. (4)He quantum crystals in a superfluid have been expected as unique exceptions that grow extremely fast at very low temperatures. However, on the ground, gravity considerably deforms the crystals and conceals the equilibrium crystal shape, and thus, gravity-free environment is needed to observe the equilibrium shape of (4)He. We report the relaxation processes of macroscopic (4)He crystals in a superfluid below 200 mK under zero gravity using a parabolic flight of a jet plane. When gravity was removed from a gravity-flattened (4)He crystal, the crystal rapidly transformed into a shape with flat surfaces. Although the relaxation processes were highly dependent on the initial condition, the crystals relaxed to a nearly homothetic shape in the end, indicating that they were truly in an equilibrium shape minimizing the interfacial free energy. Thanks to the equilibrium shape, we were able to determine the Wulff's origin and the size of the c-facet together with the vicinal surface profile next to the c-facet. The c-facet size was extremely small in the quantum crystals, and the facet-like flat surfaces were found to be the vicinal surfaces. At the same time, the interfacial free energy of the a-facet and s-facet was also obtained.

Far from the equilibrium crystallization of oxide quantum dots in dried inorganic gels

NASA Astrophysics Data System (ADS)

Costille, B.; Dumoulin, M.; Ntsame Abagha, A. M.; Thune, E.; Guinebretière, R.

2018-06-01

We synthesized, through the sol-gel process, far from the equilibrium amorphous materials in which heterogeneous crystallization allowed the formation of oxide quantum dots. The isothermal evolutions of the mean size of the nanocrystals and the crystallinity of the materials were determined through x-ray diffraction experiments. The heterogeneous crystallization is characterized by a kinetic behavior that is far from that expected, according to the classical nucleation theory. We demonstrate that the evolution of the crystallinity is characterized by an Avrami exponent largely smaller than 1. Finally, nanocrystals exhibiting a size significantly below their Bohr radius are obtained and the number of these nanocrystals increases during isothermal treatment, whereas their mean size remains quasi-constant.

The evolution of structural and chemical heterogeneity during rapid solidification at gas atomization

NASA Astrophysics Data System (ADS)

Golod, V. M.; Sufiiarov, V. Sh

2017-04-01

Gas atomization is a high-performance process for manufacturing superfine metal powders. Formation of the powder particles takes place primarily through the fragmentation of alloy melt flow with high-pressure inert gas, which leads to the formation of non-uniform sized micron-scale particles and subsequent their rapid solidification due to heat exchange with gas environment. The article presents results of computer modeling of crystallization process, simulation and experimental studies of the cellular-dendrite structure formation and microsegregation in different size particles. It presents results of adaptation of the approach for local nonequilibrium solidification to conditions of crystallization at gas atomization, detected border values of the particle size at which it is possible a manifestation of diffusionless crystallization.

Key to enhance thermoelectric performance by controlling crystal size of strontium titanate

NASA Astrophysics Data System (ADS)

Wang, Jun; Ye, Xinxin; Yaer, Xinba; Wu, Yin; Zhang, Boyu; Miao, Lei

2015-09-01

One-step molten salt synthesis process was introduced to fabricate nano to micrometer sized SrTiO3 powders in which effects of synthesis temperature, oxide-to-flux ratios and raw materials on the generation of SrTiO3 powders were examined. 100 nm or above sized pure SrTiO3 particles were obtained at relatively lower temperature of 900∘C. Micro-sized rhombohedral crystals with a maximum size of approximately 12 μm were obtained from SrCO3 or Sr(NO3)2 strontium source with 1:1 O/S ratio. Controlled crystal size and morphology of Nb-doped SrTiO3 particles are prepared by using this method to confirm the performance of thermoelectric properties. The Seebeck coefficient obtained is significantly high when compared with the reported data, and the high ratio of nano particles in the sample has a positive effect on the increase of Seebeck coefficient too, which is likely due to the energy filtering effect at large numbers of grain boundaries resulting from largely distributed structure.

Effect of dislocation pile-up on size-dependent yield strength in finite single-crystal micro-samples

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

Pan, Bo; Shibutani, Yoji, E-mail: sibutani@mech.eng.osaka-u.ac.jp; Zhang, Xu

2015-07-07

Recent research has explained that the steeply increasing yield strength in metals depends on decreasing sample size. In this work, we derive a statistical physical model of the yield strength of finite single-crystal micro-pillars that depends on single-ended dislocation pile-up inside the micro-pillars. We show that this size effect can be explained almost completely by considering the stochastic lengths of the dislocation source and the dislocation pile-up length in the single-crystal micro-pillars. The Hall–Petch-type relation holds even in a microscale single-crystal, which is characterized by its dislocation source lengths. Our quantitative conclusions suggest that the number of dislocation sources andmore » pile-ups are significant factors for the size effect. They also indicate that starvation of dislocation sources is another reason for the size effect. Moreover, we investigated the explicit relationship between the stacking fault energy and the dislocation “pile-up” effect inside the sample: materials with low stacking fault energy exhibit an obvious dislocation pile-up effect. Our proposed physical model predicts a sample strength that agrees well with experimental data, and our model can give a more precise prediction than the current single arm source model, especially for materials with low stacking fault energy.« less

Size-dependent and tunable crystallization of GeSbTe phase-change nanoparticles

NASA Astrophysics Data System (ADS)

Chen, Bin; Ten Brink, Gert H.; Palasantzas, George; Kooi, Bart J.

2016-12-01

Chalcogenide-based nanostructured phase-change materials (PCMs) are considered promising building blocks for non-volatile memory due to their high write and read speeds, high data-storage density, and low power consumption. Top-down fabrication of PCM nanoparticles (NPs), however, often results in damage and deterioration of their useful properties. Gas-phase condensation based on magnetron sputtering offers an attractive and straightforward solution to continuously down-scale the PCMs into sub-lithographic sizes. Here we unprecedentedly present the size dependence of crystallization for Ge2Sb2Te5 (GST) NPs, whose production is currently highly challenging for chemical synthesis or top-down fabrication. Both amorphous and crystalline NPs have been produced with excellent size and composition control with average diameters varying between 8 and 17 nm. The size-dependent crystallization of these NPs was carefully analyzed through in-situ heating in a transmission electron microscope, where the crystallization temperatures (Tc) decrease when the NPs become smaller. Moreover, methane incorporation has been observed as an effective method to enhance the amorphous phase stability of the NPs. This work therefore elucidates that GST NPs synthesized by gas-phase condensation with tailored properties are promising alternatives in designing phase-change memories constrained by optical lithography limitations.

Oxygen isotope geochemistry of mafic magmas at Mt. Vesuvius

NASA Astrophysics Data System (ADS)

Dallai, Luigi; Raffaello, Cioni; Chiara, Boschi; Claudia, D'oriano

2010-05-01

Pumice and scoria from different eruptive layers of Mt. Vesuvius volcanic products contain mafic minerals consisting of High-Fo olivine and Diopsidic Pyroxene. These phases were crystallized in unerupted trachibasaltic to tephritic magmas, and were brought to surface by large phonolitic/tephri-phonolitic (e.g. Avellino and Pompei) and/or of tephritic and phono-tephritic (Pollena) eruptions. A large set of these mm-sized crystals was accurately separated from selected juvenile material and measured for their chemical compositions (EPMA, Laser Ablation ICP-MS) and 18O/16O ratios (conventional laser fluorination) to constrain the nature and evolution of the primary magmas at Mt. Vesuvius. Uncontaminated mantle δ18O values are hardly recovered in Italian Quaternary magmas, mostly due to the widespread occurrence of crustal contamination of the primary melts during their ascent to the surface (e.g. Alban Hills, Ernici Mts., and Aeolian Islands). At Mt. Vesuvius, measured olivine and clinopyroxene share quite homogeneous chemical compositions (Olivine Fo 85-90 ; Diopside En 45-48, respectively), and represent phases crystallized in near primary mafic magmas. Trace element composition constrains the near primary nature of the phases. Published data on volatile content of melt inclusions hosted in these crystals reveal the coexistence of dissolved water and carbon dioxide, and a minimum trapping pressure around 200-300 MPa, suggesting that crystal growth occurred in a reservoir at about 8-10 km depth. Recently, experimental data have suggested massive carbonate assimilation (up to about 20%) to derive potassic alkali magmas from trachybasaltic melts. Accordingly, the δ18O variability and the trace element content of the studied minerals suggest possible contamination of primary melts by an O-isotope enriched, REE-poor contaminant like the limestone of Vesuvius basement. Low, nearly primitive δ18O values are observed for olivine from Pompeii eruption, although still above the range of typical mantle minerals. The δ18Oolivine and δ18Ocpxof the minerals from all the studied eruptions define variable degrees of carbonate interaction and magma crystallization for the different eruptions, and possibly within the same eruption, and show evidence of oxygen isotope equilibrium at high temperature. However, energy-constrained AFC model suggest that carbonate assimilation was limited. On the basis of our data, we suggest that interaction between magma and a fluxing, decarbonation-derived CO2 fluid may be partly accounted for the measured O-isotope compositions.

Orbital processing of high-quality CdTe compound semiconductors

NASA Technical Reports Server (NTRS)

Larson, David J., Jr.; Alexander, J. I. D.; Gillies, D.; Carlson, F. M.; Wu, J.; Black, D.

1994-01-01

CdZnTe crystals were grown in one-g and in micro-g for comparative analysis. The two micro-g crystals were grown in the Crystal Growth Furnace during the First United States Microgravity Laboratory mission (USML-1). The samples were analyzed for chemical homogeneity, structural perfection, and optoelectronic performance (infrared transmission). Fourier Transform Infrared (FTIR) transmission of both ground and flight materials showed that the infrared transmission was close to theoretical, 63% versus 66%, suggesting that the material was close to the stochiometric composition during both the ground and flight experiments. Infrared microscopy confirmed that the principal precipitates were Te and their size (1-10 microns) and density suggested that the primary flight and ground base samples experienced similar cooling rates. Macrosegregation was predicted, using scaling analysis, to be low even in one-g crystals and this was confirmed experimentally, with nearly diffusion controlled growth achieved even in the partial mixing regime on the ground. Radial segregation was monitored in the flight samples and was found to vary with fraction solidified, but was disturbed due to the asymmetric grvitational and thermal fields experienced by the flight samples. The flight samples, however, were found to be much higher in structural perfection than the ground samples produced in the same furnace under identical growth conditions except for the gravitational level. Rocking curve widths were found to be substantially reduced, from 20/35 (one-g) to 9/20 (micro-g) for the best regions of the crystals. The full width at half maximum (FWHM) of 9 arc seconds is as good as the best reported terrestrially for this material. The ground samples were found to have a fully developed mosaic structure consisting of subgrains, whereas the flight sample dislocations were discrete and no mosaic substructure was evident. The defect density was reduced from 50-100,000 (one-g) to 500-25000 EPD (micro-g). These results were confirmed using rocking curve analysis, synchrotron topography, and etch pit analysis. The low dislocation density is thought to have resulted from the near-absence of hydrostatic pressure which allowed the melt to solidify with minimum or no wall contact, resulting in very low stress being exerted on the crystal during growth or during post-solidification cooling.

Calculated photonic structures for infrared emittance control

NASA Astrophysics Data System (ADS)

Rung, Andreas; Ribbing, Carl G.

2002-06-01

Using an available program package based on the transfer-matrix method, we calculated the photonic band structure for two different structures: a quasi-three-dimensional crystal of square air rods in a high-index matrix and an opal structure of high-index spheres in a matrix of low index, epsilon = 1.5. The high index used is representative of gallium arsenide in the thermal infrared range. The geometric parameters of the rod dimension, sphere radius, and lattice constants were chosen to give total reflectance for normal incidence, i.e., minimum thermal emittance, in either one of the two infrared atmospheric windows. For these four photonic crystals, the bulk reflectance spectra and the wavelength-averaged thermal emittance as a function of crystal thickness were calculated. The results reveal that potentially useful thermal signature suppression is obtained for crystals as thin as 20-50 mum, i.e., comparable with that of a paint layer.

Study on growth techniques and macro defects of large-size Nd:YAG laser crystal

NASA Astrophysics Data System (ADS)

Quan, Jiliang; Yang, Xin; Yang, Mingming; Ma, Decai; Huang, Jinqiang; Zhu, Yunzhong; Wang, Biao

2018-02-01

Large-size neodymium-doped yttrium aluminum garnet (Nd:YAG) single crystals were grown by the Czochralski method. The extinction ratio and wavefront distortion of the crystal were tested to determine the optical homogeneity. Moreover, under different growth conditions, the macro defects of inclusion, striations, and cracking in the as-grown Nd:YAG crystals were analyzed. Specifically, the inclusion defects were characterized using scanning electron microscopy and energy dispersive spectroscopy. The stresses of growth striations and cracking were studied via a parallel plane polariscope. These results demonstrate that improper growth parameters and temperature fields can enhance defects significantly. Thus, by adjusting the growth parameters and optimizing the thermal environment, high-optical-quality Nd:YAG crystals with a diameter of 80 mm and a total length of 400 mm have been obtained successfully.

Phase behavior of binary and polydisperse suspensions of compressible microgels controlled by selective particle deswelling

NASA Astrophysics Data System (ADS)

Scotti, A.; Gasser, U.; Herman, E. S.; Han, Jun; Menzel, A.; Lyon, L. A.; Fernandez-Nieves, A.

2017-09-01

We investigate the phase behavior of suspensions of poly(N -isopropylacrylamide) (pNIPAM) microgels with either bimodal or polydisperse size distribution. We observe a shift of the fluid-crystal transition to higher concentrations depending on the polydispersity or the fraction of large particles in suspension. Crystallization is observed up to polydispersities as high as 18.5%, and up to a number fraction of large particles of 29% in bidisperse suspensions. The crystal structure is random hexagonal close-packed as in monodisperse pNIPAM microgel suspensions. We explain our experimental results by considering the effect of bound counterions. Above a critical particle concentration, these cause deswelling of the largest microgels, which are the softest, changing the size distribution of the suspension and enabling crystal formation in conditions where incompressible particles would not crystallize.

Crystal imperfection studies of pure and silicon substituted hydroxyapatite using Raman and XRD.

PubMed

Zou, Shuo; Huang, Jie; Best, Serena; Bonfield, William

2005-12-01

Hydroxyapatite (HA) is important in biomedical applications because of its chemical similarity to the mineral content of bone and its consequent bioactivity. Silicon substitution into the hydroxyapatite crystal lattice was found to enhance its bioactivity both in vitro and in vivo [1, 2]. However, the mechanism for the enhancement is still not well understood. In this paper, the crystal imperfections introduced by silicon substitution were studied using XRD and Raman spectroscopy. It was found that silicon substitution did not introduce microstrain, but deceased the crystal size in the hk0 direction. Three new vibration modes and peak broadening were observed in Raman spectra following silicon incorporation. The imperfections introduced by silicon substitution may play a role in enhancing bioactivity. A phenomenological relationship between the width of the PO4 v1 peak and crystal size was established.

Novel fluorescence adjustable photonic crystal materials

NASA Astrophysics Data System (ADS)

Zhu, Cheng; Liu, Xiaoxia; Ni, Yaru; Fang, Jiaojiao; Fang, Liang; Lu, Chunhua; Xu, Zhongzi

2017-11-01

Novel photonic crystal materials (PCMs) with adjustable fluorescence were fabricated by distributing organic fluorescent powders of Yb0.2Er0.4Tm0.4(TTA)3Phen into the opal structures of self-assembled silica photonic crystals (PCs). Via removing the silica solution in a constant speed, PCs with controllable thicknesses and different periodic sizes were obtained on glass slides. Yb0.2Er0.4Tm0.4(TTA)3Phen powders were subsequently distributed into the opal structures. The structures and optical properties of the prepared PCMs were investigated. Finite-difference-time-domain (FDTD) calculation was used to further analyze the electric field distributions in PCs with different periodic sizes while the relation between periodic sizes and fluorescent spectra of PCMs was discussed. The results showed that the emission color of the PCMs under irradiation of 980 nm laser can be easily adjusted from green to blue by increasing the periodic size from 250 to 450 nm.

The "New Polyethylene Glycol Dilemma": Polyethylene Glycol Impurities and Their Paradox Role in mAb Crystallization.

PubMed

Hildebrandt, Christian; Joos, Lea; Saedler, Rainer; Winter, Gerhard

2015-06-01

Polyethylene glycols (PEG) represent the most successful and frequently applied class of excipients used for protein crystallization. PEG auto-oxidation and formation of impurities such as peroxides and formaldehydes that foster protein drug degradation is known. However, their effect on mAb crystallization has not been studied in detail before. During the present study, a model IgG1 antibody (mAb1) was crystallized in PEG solutions. Aggregate formation was observed during crystallization and storage that was ascribed to PEG degradation products. Reduction of peroxide and formaldehyde levels prior to crystallization by vacuum and freeze-drying was investigated for its effect on protein degradation. Vacuum drying was superior in removal of peroxides but inferior in reducing formaldehyde residues. Consequently, double purification allowed extensive removal of both impurities. Applying of purified PEG led to 50% lower aggregate fractions. Surprisingly, PEG double purification or addition of methionine prior to crystallization prevented crystal formation. With increased PEG concentration or spiking with peroxides and formaldehydes, crystal formation could be recovered again. With these results, we demonstrate that minimum amounts of oxidizing impurities and thus in consequence chemically altered proteins are vital to initiate mAb1 crystallization. The present study calls PEG as good precipitant for therapeutic biopharmaceuticals into question. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Economic analysis of crystal growth in space

NASA Technical Reports Server (NTRS)

Ulrich, D. R.; Chung, A. M.; Yan, C. S.; Mccreight, L. R.

1972-01-01

Many advanced electronic technologies and devices for the 1980's are based on sophisticated compound single crystals, i.e. ceramic oxides and compound semiconductors. Space processing of these electronic crystals with maximum perfection, purity, and size is suggested. No ecomonic or technical justification was found for the growth of silicon single crystals for solid state electronic devices in space.

Imaging System For Measuring Macromolecule Crystal Growth Rates in Microgravity

NASA Technical Reports Server (NTRS)

Corder, Eric L.; Briscoe, Jeri

2004-01-01

In order to determine how macromolecule crystal quality improvement in microgravity is related to crystal growth characteristics, a team of scientists and engineers at NASA's Marshal Space Flight Center (MSFC) developed flight hardware capable of measuring the crystal growth rates of a population of crystals growing under the same conditions. As crystal growth rate is defined as the change or delta in a defined dimension or length (L) of crystal over time, the hardware was named Delta-L. Delta-L consists of three sub assemblies: a fluid unit including a temperature-controlled growth cell, an imaging unit, and a control unit (consisting of a Data Acquisition and Control Unit (DACU), and a thermal control unit). 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. This paper will describe the Delta-L imaging system. The Delta-L imaging system was designed to locate, resolve, and capture images of up to 10 individual crystals ranging in size from 10 to 500 microns with a point-to-point accuracy of +/- 2.0 microns within a quartz growth cell observation area of 20 mm x 10 mm x 1 mm. The optical imaging system is comprised of a video microscope camera mounted on computer controlled translation stages. The 3-axis translation stages and control units provide crewmembers the ability to search throughout the growth cell observation area for crystals forming in size of approximately 10 microns. Once the crewmember has selected ten crystals of interest, the growth of these crystals is tracked until the size reaches approximately 500 microns. In order to resolve these crystals an optical system with a magnification of 10X was designed. A black and white NTSC camera was utilized with a 20X microscope objective and a 0.5X custom designed relay lens with an inline light to meet the magnification requirement. The design allows a 500 pm crystal to be viewed in the vertical dimension on a standard NTSC monitor (4:3 aspect ratio). Images of the 10 crystals are collected periodically and stored in sets by the DACU.

New water soluble heterometallic complex showing unpredicted coordination modes of EDTA

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

Mudsainiyan, R.K., E-mail: mudsainiyanrk@gmail.com; Jassal, A.K.; Chawla, S.K., E-mail: sukhvinder.k.chawla@gmail.com

2015-10-15

A mesoporous 3D polymeric complex (I) having formula ([Zr(IV)O-μ{sup 3}-(EDTA)Fe(III)OH]·H{sub 2}O){sub n} has been crystallized and characterized by various techniques. Single-crystal X-ray diffraction analysis revealed that complex (I) crystallized in chiral monoclinic space group Cc (space group no. 9) with unexpected coordination modes of EDTA and mixture of two transition metal ions. In this complex, the coordination number of Zr(IV) ion is seven where four carboxylate oxygen atoms, two nitrogen atoms, one oxide atom are coordinating with Zr(IV). Fe(III) is four coordinated and its coordination environment is composed of three different carboxylic oxygen atoms from three different EDTA and onemore » oxygen atom of –OH group. The structure consists of 4-c and 16-c (2-nodal) net with new topology and point symbol for net is (3{sup 36}·4{sup 54}·5{sup 30})·(3{sup 6}). TGA study and XRPD pattern showed that the coordination polymer is quite stable even after losing water molecule and –OH ion. Quenching behavior in fluorescence of ligand is observed by complexation with transition metal ions is due to n–π⁎ transition. The SEM micrograph shows the morphology of complex (I) exhibits spherical shape with size ranging from 50 to 280 nm. The minimum N{sub 2} (S{sub BET}=8.7693 m{sup 2}/g) and a maximum amount of H{sub 2} (high surface area=1044.86 m{sup 2}/g (STP)) could be adsorbed at 77 K. From DLS study, zeta potential is calculated i.e. −7.94 shows the negative charges on the surface of complex. Hirshfeld surface analysis and fingerprint plots revealed influence of weak or non bonding interactions in crystal packing of complex. - Graphical abstract: The complex (I) crystallized with unexpected coordination modes of EDTA having 4-c, 16-c net with new topology and point symbol is (3{sup 36}·4{sup 54}·5{sup 30})·(3{sup 6}). TGA study and XRPD pattern proved its stability with high preference of H{sub 2} uptake by complex. - Highlights: • 3D complex having unexpected coordination modes of EDTA with Zr(IV) and Fe(III). • The structure consists of 4-c and 16-c (2-nodal) net with new topology. • Reasonable S{sub BET} (8.7693 m{sup 2}/g) but high H{sub 2} uptake (1044.86 m{sup 2}/g) due to limited pore size. • Quenching behavior due to n–π⁎ transition by complexation with transition metal ions. • From DLS study, zeta potential value is −7.94.« less

Structuring β-Ga2O3 photonic crystal photocatalyst for efficient degradation of organic pollutants.

PubMed

Li, Xiaofang; Zhen, Xiuzheng; Meng, Sugang; Xian, Jiangjun; Shao, Yu; Fu, Xianzhi; Li, Danzhen

2013-09-03

Coupling photocatalysts with photonic crystals structure is based on the unique property of photonic crystals in confining, controlling, and manipulating the incident photons. This combination enhances the light absorption in photocatalysts and thus greatly improves their photocatalytic performance. In this study, Ga2O3 photonic crystals with well-arranged skeleton structures were prepared via a dip-coating infiltration method. The positions of the electronic band absorption for Ga2O3 photonic crystals could be made to locate on the red edge, on the blue edge, and away from the edge of their photonic band gaps by changing the pore sizes of the samples, respectively. Particularly, the electronic band absorption of the Ga2O3 photonic crystal with a pore size of 135 nm was enhanced more than other samples by making it locate on the red edge of its photonic band gap, which was confirmed by the higher instantaneous photocurrent and photocatalytic activity for the degradation of various organic pollutants under ultraviolet light irradiation. Furthermore, the degradation mechanism over Ga2O3 photonic crystals was discussed. The design of Ga2O3 photonic crystals presents a prospective application of photonic crystals in photocatalysis to address light harvesting and quantum efficiency problems through manipulating photons or constructing photonic crystal structure as groundwork.

Crystallization of sodium chloride from a concentrated calcium chloride-potassium chloride-sodium chloride solution in a CMSMPR crystallizer: Observation of crystal size distribution and model validation

NASA Astrophysics Data System (ADS)

Choi, Byung Sang

Compared to overwhelming technical data available in other advanced technologies, knowledge about particle technology, especially in particle synthesis from a solution, is still poor due to the lack of available equipment to study crystallization phenomena in a crystallizer. Recent technical advances in particle size measurement such as Coulter counter and laser light scattering have made in/ex situ study of some of particle synthesis, i.e., growth, attrition, and aggregation, possible with simple systems. Even with these advancements in measurement technology, to grasp fully the crystallization phenomena requires further theoretical and technical advances in understanding such particle synthesis mechanisms. Therefore, it is the motive of this work to establish the general processing parameters and to produce rigorous experimental data with reliable performance and characterization that rigorously account for the crystallization phenomena of nucleation, growth, aggregation, and breakage including their variations with time and space in a controlled continuous mixed-suspension mixed-product removal (CMSMPR) crystallizer. This dissertation reports the results and achievements in the following areas: (1) experimental programs to support the development and validation of the phenomenological models and generation of laboratory data for the purpose of testing, refining, and validating the crystallization process, (2) development of laboratory well-mixed crystallizer system and experimental protocols to generate crystal size distribution (CSD) data, (3) the effects of feed solution concentration, crystallization temperature, feed flow rate, and mixing speed, as well as different types of mixers resulting in the evolution of CSDs with time from a concentrated brine solution, (4) with statistically designed experiments the effects of processing variables on the resultant particle structure and CSD at steady state were quantified and related to each of those operating conditions by studying the detailed crystallization processes, such as nucleation, growth, and breakage, as well as agglomeration. The purification of CaCl2 solution involving the crystallization of NaCl from the solution mixture of CaCl2, KCl, and NaCl as shipped from Dow Chemical, Ludington, in a CMSMPR crystallizer was studied as our model system because of its nucleation and crystal growth tendencies with less agglomeration. This project also generated a significant body of experimental data that are available at URL that is http://www.che.utah.edu/˜ring/CrystallizationWeb.

Bubble migration in a compacting crystal-liquid mush

NASA Astrophysics Data System (ADS)

Boudreau, Alan

2016-04-01

Recent theoretical models have suggested that bubbles are unlikely to undergo significant migration in a compaction crystal mush by capillary invasion while the system remains partly molten. To test this, experiments of bubble migration during compaction in a crystal-liquid mush were modeled using deformable foam crystals in corn syrup in a volumetric burette, compacted with rods of varying weights. A bubble source was provided by sodium bicarbonate (Alka-Seltzer®). Large bubbles (>several crystal sizes) are pinched by the compacting matrix and become overpressured and deformed as the bubbles experience a load change from hydrostatic to lithostatic. Once they begin to move, they move much faster than the compaction-driven liquid. Bubbles that are about the same size as the crystals but larger than the narrower pore throats move by deformation or breaking into smaller bubbles as they are forced through pore restrictions. Bubbles that are less than the typical pore diameter generally move with the liquid: The liquid + bubble mixture behaves as a single phase with a lower density than the bubble-free liquid, and as a consequence it rises faster than bubble-free liquid and allows for faster compaction. The overpressure required to force a bubble through the matrix (max grain size = 5 mm) is modest, about 5 %, and it is estimated that for a grain size of 1 mm, the required overpressure would be about 25 %. Using apatite distribution in a Stillwater olivine gabbro as an analog for bubble nucleation and growth, it is suggested that relatively large bubbles initially nucleate and grow in liquid-rich channels that develop late in the compaction history. Overpressure from compaction allows bubbles to rise higher into hotter parts of the crystal pile, where they redissolve and increase the volatile content of the liquid over what it would have without the bubble migration, leading to progressively earlier vapor saturation during crystallization of the interstitial liquid. Bubbles can also move rapidly by `surfing' on porosity waves that can develop in a compacting mush.

An evaluation of adhesive sample holders for advanced crystallographic experiments

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

Mazzorana, Marco; Sanchez-Weatherby, Juan, E-mail: juan.sanchez-weatherby@diamond.ac.uk; Sandy, James

Commercially available adhesives have been evaluated for crystal mounting when undertaking complex macromolecular crystallography experiments. Here, their use as tools for advanced sample mounting and cryoprotection is assessed and their suitability for room-temperature data-collection and humidity-controlled studies is investigated. The hydration state of macromolecular crystals often affects their overall order and, ultimately, the quality of the X-ray diffraction pattern that they produce. Post-crystallization techniques that alter the solvent content of a crystal may induce rearrangement within the three-dimensional array making up the crystal, possibly resulting in more ordered packing. The hydration state of a crystal can be manipulated by exposingmore » it to a stream of air at controlled relative humidity in which the crystal can equilibrate. This approach provides a way of exploring crystal hydration space to assess the diffraction capabilities of existing crystals. A key requirement of these experiments is to expose the crystal directly to the dehydrating environment by having the minimum amount of residual mother liquor around it. This is usually achieved by placing the crystal on a flat porous support (Kapton mesh) and removing excess liquid by wicking. Here, an alternative approach is considered whereby crystals are harvested using adhesives that capture naked crystals directly from their crystallization drop, reducing the process to a one-step procedure. The impact of using adhesives to ease the harvesting of different types of crystals is presented together with their contribution to background scattering and their usefulness in dehydration experiments. It is concluded that adhesive supports represent a valuable tool for mounting macromolecular crystals to be used in humidity-controlled experiments and to improve signal-to-noise ratios in diffraction experiments, and how they can protect crystals from modifications in the sample environment is discussed.« less

Quantitative Research on the Minimum Wage

ERIC Educational Resources Information Center

Goldfarb, Robert S.

1975-01-01

The article reviews recent research examining the impact of minimum wage requirements on the size and distribution of teenage employment and earnings. The studies measure income distribution, employment levels and effect on unemployment. (MW)

Anatase TiO2 single crystals with dominant {0 0 1} facets: Synthesis, shape-control mechanism and photocatalytic activity

NASA Astrophysics Data System (ADS)

Tong, Huifen; Zhou, Yingying; Chang, Gang; Li, Pai; Zhu, Ruizhi; He, Yunbin

2018-06-01

Anatase TiO2 micro-crystals with 51% surface exposing highly active {0 0 1} facets are prepared by hydrothermal synthesis using TiF4 as Ti resource and HF as morphology control agent. In addition, anatase TiO2 single crystals exposing large {0 0 1} crystal facets are facilely synthesized with "green" NaF plus HCl replacing HF for the morphology control. A series of comparative experiments are carried out for separately studying the effects of F- and H+ concentrations on the growth of TiO2 crystals, which have not been understood very much in depth so far. The results indicate that both F- and H+ synergistically affect the synthesis of truncated anatase octahedrons, where F- is preferentially adsorbed on the {0 0 1} facets resulting in lateral growth of these facets and H+ adjusts the growth rate of anatase TiO2 along different orientations by tuning the hydrolysis rate. Based on this information, anatase TiO2 single crystals with small size (1.3 μm) and large exposure of {0 0 1} facets (45%) are successfully prepared under optimal conditions ([H+]/[F-] = 20:1). Photocatalytic activities of the as-prepared products toward methylene blue photo-degradation are further tested. It is revealed that both crystal size and percentage of {0 0 1} facets are decisive for the photocatalytic performance, and the crystals with a small size (1.3 μm) and large exposure of {0 0 1} facets (45%) are catalytically most active. This work has clarified the main factors that control the growth process and morphology of anatase TiO2 single crystals for achieving superior photocatalytic properties.

Imaging transport phenomena during lysozyme protein crystal growth by the hanging drop technique

NASA Astrophysics Data System (ADS)

Sethia Gupta, Anamika; Gupta, Rajive; Panigrahi, P. K.; Muralidhar, K.

2013-06-01

The present study reports the transport process that occurs during the growth of lysozyme protein crystals by the hanging drop technique. A rainbow schlieren technique has been employed for imaging changes in salt concentration. A one dimensional color filter is used to record the deflection of the light beam. An optical microscope and an X-ray crystallography unit are used to characterize the size, tetragonal shape and Bravais lattice constants of the grown crystals. A parametric study on the effect of drop composition, drop size, reservoir height and number of drops on the crystal size and quality is reported. Changes in refractive index are not large enough to create a meaningful schlieren image in the air gap between the drop and the reservoir. However, condensation of fresh water over the reservoir solution creates large changes in the concentration of NaCl, giving rise to clear color patterns in the schlieren images. These have been analyzed to obtain salt concentration profiles near the free surface of the reservoir solution as a function of time. The diffusion of fresh water into the reservoir solution at the early stages of crystal growth followed by the mass flux of salt from the bulk solution towards the free surface has been recorded. The overall crystal growth process can be classified into two regimes, as demarcated by the changes in slope of salt concentration within the reservoir. The salt concentration in the reservoir equilibrates at long times when the crystallization process is complete. Thus, transport processes in the reservoir emerge as the route to monitor protein crystal growth in the hanging drop configuration. Results show that crystal growth rate is faster for a higher lysozyme concentration, smaller drops, and larger reservoir heights.

Time-evolution of grain size distributions in random nucleation and growth crystallization processes

NASA Astrophysics Data System (ADS)

Teran, Anthony V.; Bill, Andreas; Bergmann, Ralf B.

2010-02-01

We study the time dependence of the grain size distribution N(r,t) during crystallization of a d -dimensional solid. A partial differential equation, including a source term for nuclei and a growth law for grains, is solved analytically for any dimension d . We discuss solutions obtained for processes described by the Kolmogorov-Avrami-Mehl-Johnson model for random nucleation and growth (RNG). Nucleation and growth are set on the same footing, which leads to a time-dependent decay of both effective rates. We analyze in detail how model parameters, the dimensionality of the crystallization process, and time influence the shape of the distribution. The calculations show that the dynamics of the effective nucleation and effective growth rates play an essential role in determining the final form of the distribution obtained at full crystallization. We demonstrate that for one class of nucleation and growth rates, the distribution evolves in time into the logarithmic-normal (lognormal) form discussed earlier by Bergmann and Bill [J. Cryst. Growth 310, 3135 (2008)]. We also obtain an analytical expression for the finite maximal grain size at all times. The theory allows for the description of a variety of RNG crystallization processes in thin films and bulk materials. Expressions useful for experimental data analysis are presented for the grain size distribution and the moments in terms of fundamental and measurable parameters of the model.

Surface phase separation, dewetting feature size, and crystal morphology in thin films of polystyrene/poly(ε-caprolactone) blend.

PubMed

Ma, Meng; He, Zhoukun; Li, Yuhan; Chen, Feng; Wang, Ke; Zhang, Qing; Deng, Hua; Fu, Qiang

2012-12-01

Thin films of polystyrene (PS)/poly(ε-caprolactone) (PCL) blends were prepared by spin-coating and characterized by tapping mode force microscopy (AFM). Effects of the relative concentration of PS in polymer solution on the surface phase separation and dewetting feature size of the blend films were systematically studied. Due to the coupling of phase separation, dewetting, and crystallization of the blend films with the evaporation of solvent during spin-coating, different size of PS islands decorated with various PCL crystal structures including spherulite-like, flat-on individual lamellae, and flat-on dendritic crystal were obtained in the blend films by changing the film composition. The average distance of PS islands was shown to increase with the relative concentration of PS in casting solution. For a given ratio of PS/PCL, the feature size of PS appeared to increase linearly with the square of PS concentration while the PCL concentration only determined the crystal morphology of the blend films with no influence on the upper PS domain features. This is explained in terms of vertical phase separation and spinodal dewetting of the PS rich layer from the underlying PCL rich layer, leading to the upper PS dewetting process and the underlying PCL crystalline process to be mutually independent. Copyright © 2012 Elsevier Inc. All rights reserved.

Thermal conductivity of tungsten: Effects of plasma-related structural defects from molecular-dynamics simulations

NASA Astrophysics Data System (ADS)

Hu, Lin; Wirth, Brian D.; Maroudas, Dimitrios

2017-08-01

We report results on the lattice thermal conductivities of tungsten single crystals containing nanoscale-sized pores or voids and helium (He) nanobubbles as a function of void/bubble size and gas pressure in the He bubbles based on molecular-dynamics simulations. For reference, we calculated lattice thermal conductivities of perfect tungsten single crystals along different crystallographic directions at room temperature and found them to be about 10% of the overall thermal conductivity of tungsten with a weak dependence on the heat flux direction. The presence of nanoscale voids in the crystal causes a significant reduction in its lattice thermal conductivity, which decreases with increasing void size. Filling the voids with He to form He nanobubbles and increasing the bubble pressure leads to further significant reduction of the tungsten lattice thermal conductivity, down to ˜20% of that of the perfect crystal. The anisotropy in heat conduction remains weak for tungsten single crystals containing nanoscale-sized voids and He nanobubbles throughout the pressure range examined. Analysis of the pressure and atomic displacement fields in the crystalline region that surrounds the He nanobubbles reveals that the significant reduction of tungsten lattice thermal conductivity in this region is due to phonon scattering from the nanobubbles, as well as lattice deformation around the nanobubbles and formation of lattice imperfections at higher bubble pressure.

Crystal Face Distributions and Surface Site Densities of Two Synthetic Goethites: Implications for Adsorption Capacities as a Function of Particle Size.

PubMed

Livi, Kenneth J T; Villalobos, Mario; Leary, Rowan; Varela, Maria; Barnard, Jon; Villacís-García, Milton; Zanella, Rodolfo; Goodridge, Anna; Midgley, Paul

2017-09-12

Two synthetic goethites of varying crystal size distributions were analyzed by BET, conventional TEM, cryo-TEM, atomic resolution STEM and HRTEM, and electron tomography in order to determine the effects of crystal size, shape, and atomic scale surface roughness on their adsorption capacities. The two samples were determined by BET to have very different site densities based on Cr VI adsorption experiments. Model specific surface areas generated from TEM observations showed that, based on size and shape, there should be little difference in their adsorption capacities. Electron tomography revealed that both samples crystallized with an asymmetric {101} tablet habit. STEM and HRTEM images showed a significant increase in atomic-scale surface roughness of the larger goethite. This difference in roughness was quantified based on measurements of relative abundances of crystal faces {101} and {201} for the two goethites, and a reactive surface site density was calculated for each goethite. Singly coordinated sites on face {210} are 2.5 more dense than on face {101}, and the larger goethite showed an average total of 36% {210} as compared to 14% for the smaller goethite. This difference explains the considerably larger adsorption capacitiy of the larger goethite vs the smaller sample and points toward the necessity of knowing the atomic scale surface structure in predicting mineral adsorption processes.

Use of a miniature diamond-anvil cell in high-pressure single-crystal neutron Laue diffraction

PubMed Central

Binns, Jack; Kamenev, Konstantin V.; McIntyre, Garry J.; Moggach, Stephen A.; Parsons, Simon

2016-01-01

The first high-pressure neutron diffraction study in a miniature diamond-anvil cell of a single crystal of size typical for X-ray diffraction is reported. This is made possible by modern Laue diffraction using a large solid-angle image-plate detector. An unexpected finding is that even reflections whose diffracted beams pass through the cell body are reliably observed, albeit with some attenuation. The cell body does limit the range of usable incident angles, but the crystallographic completeness for a high-symmetry unit cell is only slightly less than for a data collection without the cell. Data collections for two sizes of hexamine single crystals, with and without the pressure cell, and at 300 and 150 K, show that sample size and temperature are the most important factors that influence data quality. Despite the smaller crystal size and dominant parasitic scattering from the diamond-anvil cell, the data collected allow a full anisotropic refinement of hexamine with bond lengths and angles that agree with literature data within experimental error. This technique is shown to be suitable for low-symmetry crystals, and in these cases the transmission of diffracted beams through the cell body results in much higher completeness values than are possible with X-rays. The way is now open for joint X-ray and neutron studies on the same sample under identical conditions. PMID:27158503

High-temperature crystallization of nanocrystals into three-dimensional superlattices.

PubMed

Wu, Liheng; Willis, Joshua J; McKay, Ian Salmon; Diroll, Benjamin T; Qin, Jian; Cargnello, Matteo; Tassone, Christopher J

2017-08-10

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single- and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) of micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. The rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.

High-temperature crystallization of nanocrystals into three-dimensional superlattices

NASA Astrophysics Data System (ADS)

Wu, Liheng; Willis, Joshua J.; McKay, Ian Salmon; Diroll, Benjamin T.; Qin, Jian; Cargnello, Matteo; Tassone, Christopher J.

2017-08-01

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single- and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) of micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. The rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.

A Hierarchical Modeling Study of the Interactions Among Turbulence, Cloud Microphysics, and Radiative Transfer in the Evolution of Cirrus Clouds

NASA Technical Reports Server (NTRS)

Curry, Judith; Khvorostyanov, V. I.

2005-01-01

This project used a hierarchy of cloud resolving models to address the following science issues of relevance to CRYSTAL-FACE: What ice crystal nucleation mechanisms are active in the different types of cirrus clouds in the Florida area and how do these different nucleation processes influence the evolution of the cloud system and the upper tropospheric humidity? How does the feedback between supersaturation and nucleation impact the evolution of the cloud? What is the relative importance of the large-scale vertical motion and the turbulent motions in the evolution of the crystal size spectra? How does the size spectra impact the life-cycle of the cloud, stratospheric dehydration, and cloud radiative forcing? What is the nature of the turbulence and waves in the upper troposphere generated by precipitating deep convective cloud systems? How do cirrus microphysical and optical properties vary with the small-scale dynamics? How do turbulence and waves in the upper troposphere influence the cross-tropopause mixing and stratospheric and upper tropospheric humidity? The models used in this study were: 2-D hydrostatic model with explicit microphysics that can account for 30 size bins for both the droplet and crystal size spectra. Notably, a new ice crystal nucleation scheme has been incorporated into the model. Parcel model with explicit microphysics, for developing and evaluating microphysical parameterizations. Single column model for testing bulk microphysics parameterizations

Quantitative control of CaCO3 growth on quartz crystal microbalance sensors as a signal amplification method.

PubMed

Wu, Congcong; Sun, Zhaomei; Liu, Li-Shang

2017-07-10

The surface crystallization of CaCO 3 on gold was monitored by a quartz crystal microbalance (QCM). Quantitative control of the grown crystals was realized by adjusting the ratio of two functional groups, -N(CH 3 ) 3 and -COOH, on SAMs. Crystals with uniform size, morphology and polymorphism were obtained. The amount of crystals formed was found to increase with an increase in the -COOH group. The proposed quantitative control of crystallization can be an effective mass amplification strategy for QCM to enhance its assay sensitivity.

A comparison between protein crystals grown with vapor diffusion methods in microgravity and protein crystals using a gel liquid-liquid diffusion ground-based method

NASA Technical Reports Server (NTRS)

Miller, Teresa Y.; He, Xiao-Min; Carter, Daniel C.

1992-01-01

Crystals of human serum albumin have been successfully grown in a variety of gels using crystallization conditions otherwise equivalent to those utilized in the popular hanging-drop vapor-equilibrium method. Preliminary comparisons of gel grown crystals with crystals grown by the vapor diffusion method via both ground-based and microgravity methods indicate that crystals superior in size and quality may be grown by limiting solutal convection. Preliminary X-ray diffraction statistics are presented.

Advances in food crystallization.

PubMed

Hartel, Richard W

2013-01-01

Crystals often play an important role in food product quality and shelf life. Controlling crystallization to obtain the desired crystal content, size distribution, shape, and polymorph is key to manufacturing products with desired functionality and shelf life. Technical developments in the field have improved the tools with which we study and characterize crystals in foods. These developments also help our understanding of the physico-chemical phenomena that govern crystallization and improve our ability to control it during processing and storage. In this review, some of the more important recent developments in measuring and controlling crystallization are discussed.

Effects of increasing size and changing europium activator concentration in KCaI3 scintillator crystals

NASA Astrophysics Data System (ADS)

Lindsey, Adam C.; Zhuravleva, Mariya; Wu, Yuntao; Stand, Luis; Loyd, Matthew; Gokhale, Sasmit; Koschan, Merry; Melcher, Charles L.

2016-09-01

KCaI3:Eu crystals have been identified as very promising for use in spectroscopic detector applications related to nuclear nonproliferation and domestic security efforts. Initial studies have shown for small crystals a few mm3 in size with 3% europium dopant concentration, a high light yield of >70,000 ph/MeV and energy resolution of ≈3% at 662 keV is attainable which is comparable with the highest performance scintillators discovered. In this work, single crystals of KCaI3 with a range of Eu2+ doping between 0 and 5 at% substituting for Ca2+ were grown at 22 mm diameter and their performance for gamma-ray spectroscopy studied. Comparisons among crystals approximately Ø22 mm×22 mm (8.4 cm3 or ≈0.5 in3) provide a more accurate understanding of how scintillation performance changes with Eu doping and increased crystal size. KCaI3 in the undoped form is shown to be a highly efficient intrinsic scintillator with a defect-related emission at 404 nm which coexists with the Eu2+ 5d-4f emission in low dopant concentrations and is completely re-absorbed in more heavily doped crystals. For larger crystals, effects from self-absorption due to Eu activation become more evident by a near doubling of decay time for 0.5 in3 crystals as the activator is increased from 0.5 to 5.0 at% Eu. Comparisons of pulse-height spectra obtained for Ø22 mm×22 mm cylinders with varying Eu concentration suggests best performance is achieved using lower Eu additions closer to 0.5-1.0 at%. Using a modified crystal packaging featuring an offset reflector geometry, 0.5 in3 crystals of KCaI3:Eu can attain under 4% energy resolution at 662 keV.

The modification of generalized uncertainty principle applied in the detection technique of femtosecond laser

NASA Astrophysics Data System (ADS)

Li, Ziyi

2017-12-01

Generalized uncertainty principle (GUP), also known as the generalized uncertainty relationship, is the modified form of the classical Heisenberg’s Uncertainty Principle in special cases. When we apply quantum gravity theories such as the string theory, the theoretical results suggested that there should be a “minimum length of observation”, which is about the size of the Planck-scale (10-35m). Taking into account the basic scale of existence, we need to fix a new common form of Heisenberg’s uncertainty principle in the thermodynamic system and make effective corrections to statistical physical questions concerning about the quantum density of states. Especially for the condition at high temperature and high energy levels, generalized uncertainty calculations have a disruptive impact on classical statistical physical theories but the present theory of Femtosecond laser is still established on the classical Heisenberg’s Uncertainty Principle. In order to improve the detective accuracy and temporal resolution of the Femtosecond laser, we applied the modified form of generalized uncertainty principle to the wavelength, energy and pulse time of Femtosecond laser in our work. And we designed three typical systems from micro to macro size to estimate the feasibility of our theoretical model and method, respectively in the chemical solution condition, crystal lattice condition and nuclear fission reactor condition.

Wax encapsulation of water-soluble compounds for application in foods.

PubMed

Mellema, M; Van Benthum, W A J; Boer, B; Von Harras, J; Visser, A

2006-11-01

Water-soluble ingredients have been successfully encapsulated in wax using two preparation techniques. The first technique ('solid preparation') leads to relatively large wax particles. The second technique ('liquid preparation') leads to relatively small wax particles immersed in vegetable oil. On the first technique: stable encapsulation of water-soluble colourants (dissolved at low concentration in water) has been achieved making use of beeswax and PGPR. The leakage from the capsules, for instance of size 2 mm, is about 30% after 16 weeks storage in water at room temperature. To form such capsules a minimum wax mass of 40% relative to the total mass is needed. High amounts of salt or acids at the inside water phase causes more leaking, probably because of the osmotic pressure difference. Osmotic matching of inner and outer phase can lead to a dramatic reduction in leakage. Fat capsules are less suitable to incorporate water soluble colourants. The reason for this could be a difference in crystal structure (fat is less ductile and more brittle). On the second technique: stable encapsulation of water-soluble colourants (encapsulated in solid wax particles) has been achieved making use of carnauba wax. The leakage from the capsules, for instance of size 250 mm, is about 40% after 1 weeks storage in water at room temperature.

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

Terai, Tsuyoshi; Itoh, Yoichi; Oasa, Yumiko

We present a measurement of H{sub 2}O ice crystallinity on the surface of trans-neptunian objects with near-infrared narrow-band imaging. The newly developed photometric technique allows us to efficiently determine the strength of a 1.65 μ m absorption feature in crystalline H{sub 2}O ice. Our data for three large objects—Haumea, Quaoar, and Orcus—which are known to contain crystalline H{sub 2}O ice on the surfaces, show a reasonable result with high fractions of the crystalline phase. It can also be pointed out that if the grain size of H{sub 2}O ice is larger than ∼20 μ m, the crystallinities of these objectsmore » are obviously below 1.0, which suggests the presence of the amorphous phase. In particular, Orcus exhibits a high abundance of amorphous H{sub 2}O ice compared to Haumea and Quaoar, possibly indicating a correlation between the bulk density of the bodies and the degree of surface crystallization. We also found the presence of crystalline H{sub 2}O ice on Typhon and 2008 AP{sub 129}, both of which are smaller than the minimum size limit for inducing cryovolcanism as well as a transition from amorphous to crystalline phase through thermal evolution due to the decay of long-lived isotopes.« less

Single crystals of selected titanates and tungstates

NASA Technical Reports Server (NTRS)

Loiacono, G. M.

1972-01-01

The compound preparation and crystal growth of a number of mixed titanate compositions was investigated. None of the compounds studied were found to melt congruently and therefore, crystal growth was extremely difficult. Various single crystal preparation methods always resulted in mixed phases from which 1-2 mm size crystals could be separated. It is concluded from this study that before successful single crystal growth can be accomplished, a detailed study of the phase diagrams in each of the systems of interest must be completed.

Light scattering by hexagonal ice crystals with distributed inclusions

NASA Astrophysics Data System (ADS)

Panetta, R. Lee; Zhang, Jia-Ning; Bi, Lei; Yang, Ping; Tang, Guanlin

2016-07-01

Inclusions of air bubbles or soot particles have significant effects on the single-scattering properties of ice crystals, effects that in turn have significant impacts on the radiation budget of an atmosphere containing the crystals. This study investigates some of the single-scattering effects in the case of hexagonal ice crystals, including effects on the backscattering depolarization ratio, a quantity of practical importance in the interpretation of lidar observations. One distinguishing feature of the study is an investigation of scattering properties at a visible wavelength for a crystal with size parameter (x) above 100, a size regime where one expects some agreement between exact methods and geometrical optics methods. This expectation is generally borne out in a test comparison of how the sensitivity of scattering properties to the distribution of a given volume fraction of included air is represented using (i) an approximate Monte Carlo Ray Tracing (MCRT) method and (ii) a numerically exact pseudo-spectral time-domain (PSTD) method. Another distinguishing feature of the study is a close examination, using the numerically exact Invariant-Imbedding T-Matrix (II-TM) method, of how some optical properties of importance to satellite remote sensing vary as the volume fraction of inclusions and size of crystal are varied. Although such an investigation of properties in the x>100 regime faces serious computational burdens that force a large number of idealizations and simplifications in the study, the results nevertheless provide an intriguing glimpse of what is evidently a quite complex sensitivity of optical scattering properties to inclusions of air or soot as volume fraction and size parameter are varied.

Computer Modeling of Non-Isothermal Crystallization

NASA Technical Reports Server (NTRS)

Kelton, K. F.; Narayan, K. Lakshmi; Levine, L. E.; Cull, T. C.; Ray, C. S.

1996-01-01

A realistic computer model for simulating isothermal and non-isothermal phase transformations proceeding by homogeneous and heterogeneous nucleation and interface-limited growth is presented. A new treatment for particle size effects on the crystallization kinetics is developed and is incorporated into the numerical model. Time-dependent nucleation rates, size-dependent growth rates, and surface crystallization are also included. Model predictions are compared with experimental measurements of DSC/DTA peak parameters for the crystallization of lithium disilicate glass as a function of particle size, Pt doping levels, and water content. The quantitative agreement that is demonstrated indicates that the numerical model can be used to extract key kinetic data from easily obtained calorimetric data. The model can also be used to probe nucleation and growth behavior in regimes that are otherwise inaccessible. Based on a fit to data, an earlier prediction that the time-dependent nucleation rate in a DSC/DTA scan can rise above the steady-state value at a temperature higher than the peak in the steady-state rate is demonstrated.

Strength and fatigue properties of three-step sintered dense nanocrystal hydroxyapatite bioceramics

NASA Astrophysics Data System (ADS)

Guo, Wen-Guang; Qiu, Zhi-Ye; Cui, Han; Wang, Chang-Ming; Zhang, Xiao-Jun; Lee, In-Seop; Dong, Yu-Qi; Cui, Fu-Zhai

2013-06-01

Dense hydroxyapatite (HA) ceramic is a promising material for hard tissue repair due to its unique physical properties and biologic properties. However, the brittleness and low compressive strength of traditional HA ceramics limited their applications, because previous sintering methods produced HA ceramics with crystal sizes greater than nanometer range. In this study, nano-sized HA powder was employed to fabricate dense nanocrystal HA ceramic by high pressure molding, and followed by a three-step sintering process. The phase composition, microstructure, crystal dimension and crystal shape of the sintered ceramic were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties of the HA ceramic were tested, and cytocompatibility was evaluated. The phase of the sintered ceramic was pure HA, and the crystal size was about 200 nm. The compressive strength and elastic modulus of the HA ceramic were comparable to human cortical bone, especially the good fatigue strength overcame brittleness of traditional sintered HA ceramics. Cell attachment experiment also demonstrated that the ceramics had a good cytocompatibility.

Fabrication of crystals from single metal atoms

PubMed Central

Barry, Nicolas P. E.; Pitto-Barry, Anaïs; Sanchez, Ana M.; Dove, Andrew P.; Procter, Richard J.; Soldevila-Barreda, Joan J.; Kirby, Nigel; Hands-Portman, Ian; Smith, Corinne J.; O’Reilly, Rachel K.; Beanland, Richard; Sadler, Peter J.

2014-01-01

Metal nanocrystals offer new concepts for the design of nanodevices with a range of potential applications. Currently the formation of metal nanocrystals cannot be controlled at the level of individual atoms. Here we describe a new general method for the fabrication of multi-heteroatom-doped graphitic matrices decorated with very small, ångström-sized, three-dimensional (3D)-metal crystals of defined size. We irradiate boron-rich precious-metal-encapsulated self-spreading polymer micelles with electrons and produce, in real time, a doped graphitic support on which individual osmium atoms hop and migrate to form 3D-nanocrystals, as small as 15 Å in diameter, within 1 h. Crystal growth can be observed, quantified and controlled in real time. We also synthesize the first examples of mixed ruthenium–osmium 3D-nanocrystals. This technology not only allows the production of ångström-sized homo- and hetero-crystals, but also provides new experimental insight into the dynamics of nanocrystals and pathways for their assembly from single atoms. PMID:24861089

7 CFR 51.3198 - Size classifications.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 2 2012-01-01 2012-01-01 false Size classifications. 51.3198 Section 51.3198... STANDARDS) United States Standards for Grades of Bermuda-Granex-Grano Type Onions Size Classifications § 51.3198 Size classifications. Size shall be specified in connection with the grade in terms of minimum...

7 CFR 51.3198 - Size classifications.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Size classifications. 51.3198 Section 51.3198... STANDARDS) United States Standards for Grades of Bermuda-Granex-Grano Type Onions Size Classifications § 51.3198 Size classifications. Size shall be specified in connection with the grade in terms of minimum...

7 CFR 51.3198 - Size classifications.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Size classifications. 51.3198 Section 51.3198... STANDARDS) United States Standards for Grades of Bermuda-Granex-Grano Type Onions Size Classifications § 51.3198 Size classifications. Size shall be specified in connection with the grade in terms of minimum...

Plant ice-binding (antifreeze) proteins

USDA-ARS?s Scientific Manuscript database

Proteins that determine the temperature at which ice crystals will form in water-based solutions in cells and tissues, that bind to growing ice crystals, thus affecting their size, and that impact ice re-crystallization have been widely-documented and studied in many plant, bacterial, fungal, insect...

Low-Temperature Growth of Two-Dimensional Layered Chalcogenide Crystals on Liquid.

PubMed

Zhou, Yubing; Deng, Bing; Zhou, Yu; Ren, Xibiao; Yin, Jianbo; Jin, Chuanhong; Liu, Zhongfan; Peng, Hailin

2016-03-09

The growth of high-quality two-dimensional (2D) layered chalcogenide crystals is highly important for practical applications in future electronics, optoelectronics, and photonics. Current route for the synthesis of 2D chalcogenide crystals by vapor deposition method mainly involves an energy intensive high-temperature growth process on solid substrates, often suffering from inhomogeneous nucleation density and grain size distribution. Here, we first demonstrate a facile vapor-phase synthesis of large-area high-quality 2D layered chalcogenide crystals on liquid metal surface with relatively low surface energy at a growth temperature as low as ∼100 °C. Uniform and large-domain-sized 2D crystals of GaSe and GaxIn1-xSe were grown on liquid metal surface even supported on a polyimide film. As-grown 2D GaSe crystals have been fabricated to flexible photodetectors, showing high photoresponse and excellent flexibility. Our strategy of energy-sustainable low-temperature growth on liquid metal surface may open a route to the synthesis of high-quality 2D crystals of Ga-, In-, Bi-, Hg-, Pb-, or Sn-based chalcogenides and halides.

Probabilistic approach to lysozyme crystal nucleation kinetics.

PubMed

Dimitrov, Ivaylo L; Hodzhaoglu, Feyzim V; Koleva, Dobryana P

2015-09-01

Nucleation of lysozyme crystals in quiescent solutions at a regime of progressive nucleation is investigated under an optical microscope at conditions of constant supersaturation. A method based on the stochastic nature of crystal nucleation and using discrete time sampling of small solution volumes for the presence or absence of detectable crystals is developed. It allows probabilities for crystal detection to be experimentally estimated. One hundred single samplings were used for each probability determination for 18 time intervals and six lysozyme concentrations. Fitting of a particular probability function to experimentally obtained data made possible the direct evaluation of stationary rates for lysozyme crystal nucleation, the time for growth of supernuclei to a detectable size and probability distribution of nucleation times. Obtained stationary nucleation rates were then used for the calculation of other nucleation parameters, such as the kinetic nucleation factor, nucleus size, work for nucleus formation and effective specific surface energy of the nucleus. The experimental method itself is simple and adaptable and can be used for crystal nucleation studies of arbitrary soluble substances with known solubility at particular solution conditions.

On the use of big-bang method to generate low-energy structures of atomic clusters modeled with pair potentials of different ranges.

PubMed

Marques, J M C; Pais, A A C C; Abreu, P E

2012-02-05

The efficiency of the so-called big-bang method for the optimization of atomic clusters is analysed in detail for Morse pair potentials with different ranges; here, we have used Morse potentials with four different ranges, from long- ρ = 3) to short-ranged ρ = 14) interactions. Specifically, we study the efficacy of the method in discovering low-energy structures, including the putative global minimum, as a function of the potential range and the cluster size. A new global minimum structure for long-ranged ρ = 3) Morse potential at the cluster size of n= 240 is reported. The present results are useful to assess the maximum cluster size for each type of interaction where the global minimum can be discovered with a limited number of big-bang trials. Copyright © 2011 Wiley Periodicals, Inc.

Characterization of Large Volume CLYC Scintillators for Nuclear Security Applications

NASA Astrophysics Data System (ADS)

Soundara-Pandian, Lakshmi; Tower, J.; Hines, C.; O'Dougherty, P.; Glodo, J.; Shah, K.

2017-07-01

We report on our development of large volume Cs2LiYCl6 (CLYC) detectors for nuclear security applications. Three-inch diameter boules have been grown and 3-in right cylinders have been fabricated. Crystals containing either >95% 6Li or >99% 7Li have been grown for applications specific to thermal or fast neutron detection, respectively. We evaluated their gamma and neutron detection properties and the performance is as good as small size crystals. Gamma and neutron efficiencies were measured for large crystals and compared with smaller size crystals. With their excellent performance characteristics, and the ability to detect fast neutrons, CLYC detectors are excellent triple-mode scintillators for use in handheld and backpack instruments for nuclear security applications.

Impact of minimum catch size on the population viability of Strombus gigas (Mesogastropoda: Strombidae) in Quintana Roo, Mexico.

PubMed

Peel, Joanne R; Mandujano, María del Carmen

2014-12-01

The queen conch Strombus gigas represents one of the most important fishery resources of the Caribbean but heavy fishing pressure has led to the depletion of stocks throughout the region, causing the inclusion of this species into CITES Appendix II and IUCN's Red-List. In Mexico, the queen conch is managed through a minimum fishing size of 200 mm shell length and a fishing quota which usually represents 50% of the adult biomass. The objectives of this study were to determine the intrinsic population growth rate of the queen conch population of Xel-Ha, Quintana Roo, Mexico, and to assess the effects of a regulated fishing impact, simulating the extraction of 50% adult biomass on the population density. We used three different minimum size criteria to demonstrate the effects of minimum catch size on the population density and discuss biological implications. Demographic data was obtained through capture-mark-recapture sampling, collecting all animals encountered during three hours, by three divers, at four different sampling sites of the Xel-Ha inlet. The conch population was sampled each month between 2005 and 2006, and bimonthly between 2006 and 2011, tagging a total of 8,292 animals. Shell length and lip thickness were determined for each individual. The average shell length for conch with formed lip in Xel-Ha was 209.39 ± 14.18 mm and the median 210 mm. Half of the sampled conch with lip ranged between 200 mm and 219 mm shell length. Assuming that the presence of the lip is an indicator for sexual maturity, it can be concluded that many animals may form their lip at greater shell lengths than 200 mm and ought to be considered immature. Estimation of relative adult abundance and densities varied greatly depending on the criteria employed for adult classification. When using a minimum fishing size of 200 mm shell length, between 26.2% and up to 54.8% of the population qualified as adults, which represented a simulated fishing impact of almost one third of the population. When conch extraction was simulated using a classification criteria based on lip thickness, it had a much smaller impact on the population density. We concluded that the best management strategy for S. gigas is a minimum fishing size based on a lip thickness, since it has lower impact on the population density, and given that selective fishing pressure based on size may lead to the appearance of small adult individuals with reduced fecundity. Furthermore, based on the reproductive biology and the results of the simulated fishing, we suggest a minimum lip thickness of ≥ 15 mm, which ensures the protection of reproductive stages, reduces the risk of overfishing, leading to non-viable density reduction.

Fox-7 for Insensitive Boosters

DTIC Science & Technology

2010-08-01

cavitation , and therefore nucleation, to occur at each frequency. As well as producing ultrasound at different frequencies, the method of delivery of...processing techniques using ultrasound , designed to optimise FOX-7 crystal size and morphology to improve booster formulations, and results from these...7 booster formulations. Also included are particle processing techniques using ultrasound , designed to optimise FOX-7 crystal size and morphology

Estimation of representative elementary volume for DNAPL saturation and DNAPL-water interfacial areas in 2D heterogeneous porous media

NASA Astrophysics Data System (ADS)

Wu, Ming; Cheng, Zhou; Wu, Jianfeng; Wu, Jichun

2017-06-01

Representative elementary volume (REV) is important to determine properties of porous media and those involved in migration of contaminants especially dense nonaqueous phase liquids (DNAPLs) in subsurface environment. In this study, an experiment of long-term migration of the commonly used DNAPL, perchloroethylene (PCE), is performed in a two dimensional (2D) sandbox where several system variables including porosity, PCE saturation (Soil) and PCE-water interfacial area (AOW) are accurately quantified by light transmission techniques over the entire PCE migration process. Moreover, the REVs for these system variables are estimated by a criterion of relative gradient error (εgi) and results indicate that the frequency of minimum porosity-REV size closely follows a Gaussian distribution in the range of 2.0 mm and 8.0 mm. As experiment proceeds in PCE infiltration process, the frequency and cumulative frequency of both minimum Soil-REV and minimum AOW-REV sizes change their shapes from the irregular and random to the regular and smooth. When experiment comes into redistribution process, the cumulative frequency of minimum Soil-REV size reveals a linear positive correlation, while frequency of minimum AOW-REV size tends to a Gaussian distribution in the range of 2.0 mm-7.0 mm and appears a peak value in 13.0 mm-14.0 mm. Undoubtedly, this study will facilitate the quantification of REVs for materials and fluid properties in a rapid, handy and economical manner, which helps enhance our understanding of porous media and DNAPL properties at micro scale, as well as the accuracy of DNAPL contamination modeling at field-scale.

Template-Directed Crystallization of High Energy Materials

DTIC Science & Technology

2014-04-01

objectives of this grant were to (a) examine the solution crystallization of RDX , HMX and CL-20 from a variety of solvents, withdetailed analysis of...crystal nucleation templates and (c) to assess the growth of RDX , HMX and CL-20 on these templates. High explosives, crystallization, RDX , CL-20...crystallization of RDX , HMX and CL-20 from a variety of solvents, with detailed analysis of their phase, size, and morphological properties; (b) to

Modeling ultrasonic compression wave absorption during the seeded crystallization of copper (II) sulphate pentahydrate from aqueous solution.

PubMed

Marshall, Thomas; Challis, Richard E; Holmes, Andrew K; Tebbutt, John S

2002-11-01

Ultrasonic compression wave absorption is investigated as a means to monitor the seeded crystallization of copper (II) sulphate pentahydrate from aqueous solution. Simple models are applied to predict crystal yield, crystal size distribution, and the changing nature of the continuous phase. The Allegra-Hawley scattering formulation is used to simulate ultrasonic absorption as crystallization proceeds. Experiments confirm that simulated attenuation is in agreement with measured results.

Biofilm formation by environmental isolates of Salmonella and their sensitivity to natural antimicrobials

USDA-ARS?s Scientific Manuscript database

We evaluated 15 Salmonella isolates; S. Derby (2), S. Infantis (4), and S. Typhimurium (9) from conventional swine farm environment (soil and lagoon) for biofilm formation. Biofilm forming ability was determined by 96-well microtitre plate Crystal-Violet and Minimum Biofilm Eradication Concentration...

Extraordinary wavelength reduction in terahertz graphene-cladded photonic crystal slabs

PubMed Central

Williamson, Ian A. D.; Mousavi, S. Hossein; Wang, Zheng

2016-01-01

Photonic crystal slabs have been widely used in nanophotonics for light confinement, dispersion engineering, nonlinearity enhancement, and other unusual effects arising from their structural periodicity. Sub-micron device sizes and mode volumes are routine for silicon-based photonic crystal slabs, however spectrally they are limited to operate in the near infrared. Here, we show that two single-layer graphene sheets allow silicon photonic crystal slabs with submicron periodicity to operate in the terahertz regime, with an extreme 100× wavelength reduction from graphene’s large kinetic inductance. The atomically thin graphene further leads to excellent out-of-plane confinement, and consequently photonic-crystal-slab band structures that closely resemble those of ideal two-dimensional photonic crystals, with broad band gaps even when the slab thickness approaches zero. The overall photonic band structure not only scales with the graphene Fermi level, but more importantly scales to lower frequencies with reduced slab thickness. Just like ideal 2D photonic crystals, graphene-cladded photonic crystal slabs confine light along line defects, forming waveguides with the propagation lengths on the order of tens of lattice constants. The proposed structure opens up the possibility to dramatically reduce the size of terahertz photonic systems by orders of magnitude. PMID:27143314

Probing Zeolite Crystal Architecture and Structural Imperfections using Differently Sized Fluorescent Organic Probe Molecules.

PubMed

Hendriks, Frank C; Schmidt, Joel E; Rombouts, Jeroen A; Lammertsma, Koop; Bruijnincx, Pieter C A; Weckhuysen, Bert M

2017-05-05

A micro-spectroscopic method has been developed to probe the accessibility of zeolite crystals using a series of fluorescent 4-(4-diethylaminostyryl)-1-methylpyridinium iodide (DAMPI) probes of increasing molecular size. Staining large zeolite crystals with MFI (ZSM-5) topology and subsequent mapping of the resulting fluorescence using confocal fluorescence microscopy reveal differences in structural integrity: the 90° intergrowth sections of MFI crystals are prone to develop structural imperfections, which act as entrance routes for the probes into the zeolite crystal. Polarization-dependent measurements provide evidence for the probe molecule's alignment within the MFI zeolite pore system. The developed method was extended to BEA (Beta) crystals, showing that the previously observed hourglass pattern is a general feature of BEA crystals with this morphology. Furthermore, the probes can accurately identify at which crystal faces of BEA straight or sinusoidal pores open to the surface. The results show this method can spatially resolve the architecture-dependent internal pore structure of microporous materials, which is difficult to assess using other characterization techniques such as X-ray diffraction. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

Evaluation of AQUI-S(TM) (efficacy and minimum toxic concentration) as a fish anaesthetic/sedative for public aquaculture in the United States

USGS Publications Warehouse

Stehly, G.R.; Gingerich, W.H.

1999-01-01

A preliminary evaluation of efficacy and minimum toxic concentration of AQUI-S(TM), a fish anaesthetic/sedative, was determined in two size classes of six species of fish important to US public aquaculture (bluegill, channel catfish, lake trout, rainbow trout, walleye and yellow perch). In addition, efficacy and minimum toxic concentration were determined in juvenile-young adult (fish aged 1 year or older) rainbow trout acclimated to water at 7 ??C, 12 ??C and 17 ??C. Testing concentrations were based on determinations made with range-finding studies for both efficacy and minimum toxic concentration. Most of the tested juvenile-young adult fish species were induced in 3 min or less at a nominal AQUI-S(TM) concentration of 20 mg L-1. In juvenile-young adult fish, the minimum toxic concentration was at least 2.5 times the selected efficacious concentration. Three out of five species of fry-fingerlings (1.25-12.5 cm in length and < 1 year old) were induced in ??? 4.1 min at a nominal concentration of 20 mg L-1 AQUI-S(TM), with the other two species requiring nominal concentrations of 25 and 35 mg L-1 for similar times of induction. Recovery times were ??? 7.3 rain for all species in the two size classes. In fry-fingerlings, the minimum toxic concentration was at least 1.4 times the selected efficacious concentration. There appeared to be little relationship between size of fish and concentrations or times to induction, recovery times and minimum toxic concentration. The times required for induction and for recovery were increased in rainbow trout as the acclimation temperature was reduced.

Silicon Carbide From a Carbon Nodule in the Canyon Diablo Meteorite

NASA Astrophysics Data System (ADS)

Leung, I. S.; Winston, R.

2011-12-01

The Canyon Diablo Meteorite fell in the Arizona desert 50,000 years ago, giving rise to the well-preserved Meteor Crater. Irons of various sizes were scattered around the crater rim and on the surrounding plains. We studied a rusty specimen containing a carbon nodule. We dug out small blocks of sooty carbon by means of a sharp tungsten carbide tip. These carbon materials contain traces of silicon carbide (SiC) and diamond/lonsdaleite. We report here our findigs of two groups of SiC grains. (1) Relatively large crystals, about 80-90 microns in size. Their colors are in shades of blue, green and neutral. One of the grains are composed of a cluster of 3 crystals of the 3C polytype, whereas, 7 other individual crystals are of hexagonal structure. All crystals in this group have dark, rounded resorption rims. (2) Small crystals, about 30-50 microns in size. They are pale blue in color, and they lack dark-colored rims. These two distinct groups probably have different modes of origin. The large crystals seem to be early-formed, but had been reheated or partially melted, as indicated by the bead-like rims. The complexities displayed by these SiC crystals might have resulted from a long residence time in the meteorite while it was still in space. Their origin might be akin to that of SiC occurring in carbonaceous chondrites and interplanetary dust particles.

Shaping plasmon beams via the controlled illumination of finite-size plasmonic crystals

PubMed Central

Bouillard, J.-S.; Segovia, P.; Dickson, W.; Wurtz, G. A.; Zayats, A. V.

2014-01-01

Plasmonic crystals provide many passive and active optical functionalities, including enhanced sensing, optical nonlinearities, light extraction from LEDs and coupling to and from subwavelength waveguides. Here we study, both experimentally and numerically, the coherent control of SPP beam excitation in finite size plasmonic crystals under focussed illumination. The correct combination of the illuminating spot size, its position relative to the plasmonic crystal, wavelength and polarisation enables the efficient shaping and directionality of SPP beam launching. We show that under strongly focussed illumination, the illuminated part of the crystal acts as an antenna, launching surface plasmon waves which are subsequently filtered by the surrounding periodic lattice. Changing the illumination conditions provides rich opportunities to engineer the SPP emission pattern. This offers an alternative technique to actively modulate and control plasmonic signals, either via micro- and nano-electromechanical switches or with electro- and all-optical beam steering which have direct implications for the development of new integrated nanophotonic devices, such as plasmonic couplers and switches and on-chip signal demultiplexing. This approach can be generalised to all kinds of surface waves, either for the coupling and discrimination of light in planar dielectric waveguides or the generation and control of non-diffractive SPP beams. PMID:25429786

Modeling of a Turbofan Engine with Ice Crystal Ingestion in the NASA Propulsion System Laboratory

NASA Technical Reports Server (NTRS)

Veres, Joseph P.; Jorgenson, Philip C. E.; Jones, Scott M.; Nili, Samaun

2017-01-01

The main focus of this study is to apply a computational tool for the flow analysis of the turbine engine that has been tested with ice crystal ingestion in the Propulsion Systems Laboratory (PSL) at NASA Glenn Research Center. The PSL has been used to test a highly instrumented Honeywell ALF502R-5A (LF11) turbofan engine at simulated altitude operating conditions. Test data analysis with an engine cycle code and a compressor flow code was conducted to determine the values of key icing parameters, that can indicate the risk of ice accretion, which can lead to engine rollback (un-commanded loss of engine thrust). The full engine aerothermodynamic performance was modeled with the Honeywell Customer Deck specifically created for the ALF502R-5A engine. The mean-line compressor flow analysis code, which includes a code that models the state of the ice crystal, was used to model the air flow through the fan-core and low pressure compressor. The results of the compressor flow analyses included calculations of the ice-water flow rate to air flow rate ratio (IWAR), the local static wet bulb temperature, and the particle melt ratio throughout the flow field. It was found that the assumed particle size had a large effect on the particle melt ratio, and on the local wet bulb temperature. In this study the particle size was varied parametrically to produce a non-zero calculated melt ratio in the exit guide vane (EGV) region of the low pressure compressor (LPC) for the data points that experienced a growth of blockage there, and a subsequent engine called rollback (CRB). At data points where the engine experienced a CRB having the lowest wet bulb temperature of 492 degrees Rankine at the EGV trailing edge, the smallest particle size that produced a non-zero melt ratio (between 3 percent - 4 percent) was on the order of 1 micron. This value of melt ratio was utilized as the target for all other subsequent data points analyzed, while the particle size was varied from 1 micron - 9.5 microns to achieve the target melt ratio. For data points that did not experience a CRB which had static wet bulb temperatures in the EGV region below 492 degrees Rankine, a non-zero melt ratio could not be achieved even with a 1 micron ice particle size. The highest value of static wet bulb temperature for data points that experienced engine CRB was 498 degrees Rankine with a particle size of 9.5 microns. Based on this study of the LF11 engine test data, the range of static wet bulb temperature at the EGV exit for engine CRB was in the narrow range of 492 degrees Rankine - 498 degrees Rankine , while the minimum value of IWAR was 0.002. The rate of blockage growth due to ice accretion and boundary layer growth was estimated by scaling from a known blockage growth rate that was determined in a previous study. These results obtained from the LF11 engine analysis formed the basis of a unique “icing wedge.”

Fiber based photonic-crystal acoustic sensor

NASA Astrophysics Data System (ADS)

Kilic, Onur

Photonic-crystal slabs are two-dimensional photonic crystals etched into a dielectric layer such as silicon. Standard micro fabrication techniques can be employed to manufacture these structures, which makes it feasible to produce them in large areas, usually an important criterion for practical applications. An appealing feature of these structures is that they can be employed as free-space optical devices such as broadband reflectors. The small thickness of the slab (usually in the vicinity of half a micron) also makes it deflectable. These combined optical and mechanical properties make it possible to employ photonic-crystal slabs in a range of practical applications, including displacement sensors, which in turn can be used for example to detect acoustic waves. An additional benefit of employing a photonic-crystal slab is that it is possible to tailor its optical and mechanical properties by adjusting the geometrical parameters of the structure such as hole radius or shape, pitch, and the slab thickness. By altering the hole radius and pitch, it is possible to make broadband reflectors or sharp transmission filters out of these structures. Adjusting the thickness also affects its deformability, making it possible to make broadband mirrors compliant to acoustic waves. Altering the hole shape, for example by introducing an asymmetry, extends the functionalities of photonic-crystal slabs even further. Breaking the symmetry by introducing asymmetric holes enables polarization-sensitive devices such as retarders, polarization beam splitters, and photonic crystals with additional non-degenerate resonances useful for increased sensitivity in sensors. All these practical advantages of photonic-crystal slabs makes them suitable as key components in micromachined sensor applications. We report one such example of an application of photonic-crystal slabs in the form of a micromachined acoustic sensor. It consists of a Fabry-Perot interferometer made of a photonic-crystal reflector embedded in a compliant silicon diaphragm placed at the tip of a single-mode fiber. Measurements in air indicate that this sensor has a relatively uniform frequency response up to at least 50 kHz, which is at least one order of magnitude higher than existing all-fiber acoustic sensors. This sensor was also shown to be able to detect pressures as low as 18 muPa/Hz 1/2. This limit is four orders of magnitude lower than in similar types of acoustic fiber sensors that are based on a deflectable diaphragm at the fiber end. This significant improvement is to a large extent due to the higher reflectivity of the reflectors, which is itself due to the use of a photonic crystal. Through a modification in the design, such a sensor can also be used in water. In addition to the high compliance of the diaphragm, the advantage for using the photonic-crystal slab is that the holes provide a venting channel for pressure equalization. As a result, the hydrophone can be employed in deep-sea applications without suffering from the high static pressure. Measurements in water over the range of 10 kHz-50 kHz show that this hydrophone has a minimum detectable pressure of only 10 muPa/Hz1/2, close to the ambient thermal-noise level. A model was developed to show that after optimization to ocean acoustics, the sensor has a theoretical minimum detectable pressure that follows the minimum ambient noise spectrum of the ocean in the bandwidth of 1 Hz-100 kHz. This makes this sensor extremely broadband compared to commercial fiber hydrophones, which are bulky and poorly responsive to frequencies above a few hundred Hz, since they require a long length of fiber. By placing several such sensors with different acoustic power ranges within a single sensor chip, this hydrophone is capable of exhibiting a dynamic range in the excess of 200 dB (1010).

Assessing SPO techniques to constrain magma flow: Examples from sills of the Karoo Igneous Province, South Africa

NASA Astrophysics Data System (ADS)

Hoyer, Lauren; Watkeys, Michael K.

2015-08-01

Shape ellipsoids that define the petrofabrics of plagioclase in Jurassic Karoo dolerite sills in KwaZulu-Natal, South Africa are rigorously constrained using the long axis lengths of plagioclase crystals and ellipse incompatibility. This has been undertaken in order to determine the most effective technique to determine petrofabrics when using the SPO-2003 programme (Launeau and Robin, 2005). The technique of segmenting an image for analysis is scrutinised and as a process is found redundant. A grain size threshold is defined to assist with the varying grain sizes observed within and between sills. Where grains exceed the 0.2 mm size threshold, images should be acquired at a high magnification (i.e., 10 × magnification). Petrofabrics are determined using the foliation and the lineation of the ellipsoid as defined by the maximum and minimum principal axes (respectively) of the resultant ellipsoid. Samples with strongly prolate fabrics are isolated allowing further constraint on the petrofabric to be made. Once the efficacy of the petrofabric determination process has been determined, the resultant foliations (and lineations) then elucidate the most accurate petrofabric attainable. The most accurate petrofabrics will be determined by using the correct magnification when the images are obtained and to run the analyses without segmenting the image. The fabrics of the upper and lower contacts of the Karoo dolerite sills are analysed in detail using these techniques and the fabrics are used as a proxy for magma flow.

Theory of Dust Voids in Plasmas

NASA Technical Reports Server (NTRS)

Goree, J.; Morfill, G. E.; Tsytovich, V. N.; Vladimirov, S. V.

1999-01-01

Dusty plasmas in a gas discharge often feature a stable void, i.e., a dust-free region inside the dust cloud. This occurs under conditions relevant to both plasma processing discharges and plasma crystal experiments. The void results from a balance of the electrostatic and ion drag forces on a dust particle. The ion drag force is driven by a flow of ions outward from an ionization source and toward the surrounding dust cloud, which has a negative space charge. In equilibrium the force balance for dust particles requires that the boundary with the dust cloud be sharp, provided that the particles are cold and monodispersive. Numerical solutions of the one-dimensional nonlinear fluid equations are carried out including dust charging and dust-neutral collisions, but not ion-neutral collisions. The regions of parameter space that allow stable void equilibria are identified. There is a minimum ionization rate that can sustain a void. Spatial profiles of plasma parameters in the void are reported. In the absence of ion-neutral collisions, the ion flow enters the dust cloud's edge at Mach number M = 1. Phase diagrams for expanding or contracting voids reveal a stationary point corresponding to a single stable equilibrium void size, provided the ionization rate is constant. Large voids contract and small voids expand until they attain this stationary void size. On the other hand, if the ionization rate is not constant, the void size can oscillate. Results are compared to recent laboratory and microgravity experiments.

Computational analysis of particle reinforced viscoelastic polymer nanocomposites - statistical study of representative volume element

NASA Astrophysics Data System (ADS)

Hu, Anqi; Li, Xiaolin; Ajdari, Amin; Jiang, Bing; Burkhart, Craig; Chen, Wei; Brinson, L. Catherine

2018-05-01

The concept of representative volume element (RVE) is widely used to determine the effective material properties of random heterogeneous materials. In the present work, the RVE is investigated for the viscoelastic response of particle-reinforced polymer nanocomposites in the frequency domain. The smallest RVE size and the minimum number of realizations at a given volume size for both structural and mechanical properties are determined for a given precision using the concept of margin of error. It is concluded that using the mean of many realizations of a small RVE instead of a single large RVE can retain the desired precision of a result with much lower computational cost (up to three orders of magnitude reduced computation time) for the property of interest. Both the smallest RVE size and the minimum number of realizations for a microstructure with higher volume fraction (VF) are larger compared to those of one with lower VF at the same desired precision. Similarly, a clustered structure is shown to require a larger minimum RVE size as well as a larger number of realizations at a given volume size compared to the well-dispersed microstructures.

Non-Isothermal Calorimetric Studies of the Crystallization of Lithium Disilicate Glass

NASA Technical Reports Server (NTRS)

Ray, C. S.; Day, D. E.; Huang, W.; Narayan, K. Lakshmi; Cull, T. S.; Kelton, K. F.

1996-01-01

The influence of preannealing treatments on the polymorphic crystallization of lithium disilicate glasses is examined. As expected, glasses heated at different rates through the temperature range where there is significant nucleation develop widely different numbers of nuclei. This can dramatically influence the stability and transformation characteristics of the annealed glass. Non-isothermal differential scanning calorimetry (DSC) and differential thermal analysis (DTA) measurements are demonstrated to be useful to probe the nucleation behavior. The first systematic investigations of particle size effects on the non-isothermal transformation behavior are presented and discussed. Based on DTA and microscopy experiments, we show that small particles of lithium disilicate glasses crystallize primarily by surface crystallization. The relative importance of surface versus volume crystallization is examined by varying particle size, by introducing nucleating agents and by exposing glasses to atmospheres of different water content. These data are analyzed quantitatively using a numerical model developed in a second paper following in this volume.

Repeated growth and bubbling transfer of graphene with millimetre-size single-crystal grains using platinum.

PubMed

Gao, Libo; Ren, Wencai; Xu, Huilong; Jin, Li; Wang, Zhenxing; Ma, Teng; Ma, Lai-Peng; Zhang, Zhiyong; Fu, Qiang; Peng, Lian-Mao; Bao, Xinhe; Cheng, Hui-Ming

2012-02-28

Large single-crystal graphene is highly desired and important for the applications of graphene in electronics, as grain boundaries between graphene grains markedly degrade its quality and properties. Here we report the growth of millimetre-sized hexagonal single-crystal graphene and graphene films joined from such grains on Pt by ambient-pressure chemical vapour deposition. We report a bubbling method to transfer these single graphene grains and graphene films to arbitrary substrate, which is nondestructive not only to graphene, but also to the Pt substrates. The Pt substrates can be repeatedly used for graphene growth. The graphene shows high crystal quality with the reported lowest wrinkle height of 0.8 nm and a carrier mobility of greater than 7,100 cm(2) V(-1) s(-1) under ambient conditions. The repeatable growth of graphene with large single-crystal grains on Pt and its nondestructive transfer may enable various applications.

Repeated growth and bubbling transfer of graphene with millimetre-size single-crystal grains using platinum

PubMed Central

Gao, Libo; Ren, Wencai; Xu, Huilong; Jin, Li; Wang, Zhenxing; Ma, Teng; Ma, Lai-Peng; Zhang, Zhiyong; Fu, Qiang; Peng, Lian-Mao; Bao, Xinhe; Cheng, Hui-Ming

2012-01-01

Large single-crystal graphene is highly desired and important for the applications of graphene in electronics, as grain boundaries between graphene grains markedly degrade its quality and properties. Here we report the growth of millimetre-sized hexagonal single-crystal graphene and graphene films joined from such grains on Pt by ambient-pressure chemical vapour deposition. We report a bubbling method to transfer these single graphene grains and graphene films to arbitrary substrate, which is nondestructive not only to graphene, but also to the Pt substrates. The Pt substrates can be repeatedly used for graphene growth. The graphene shows high crystal quality with the reported lowest wrinkle height of 0.8 nm and a carrier mobility of greater than 7,100 cm2 V−1 s−1 under ambient conditions. The repeatable growth of graphene with large single-crystal grains on Pt and its nondestructive transfer may enable various applications. PMID:22426220

Simplified numerical approach for estimation of effective segregation coefficient at the melt/crystal interface

NASA Astrophysics Data System (ADS)

Prostomolotov, A. I.; Verezub, N. A.; Voloshin, A. E.

2014-09-01

A thermo-gravitational convection and impurity transfer in the melt were investigated using a simplified numerical model for Bridgman GaSb(Te) crystal growth in microgravity conditions. Simplifications were as follows: flat melt/crystal interface, fixed melt sizes and only lateral ampoule heating. Calculations were carried out by Ansys®Fluent® code employing a two-dimensional Navier-Stokes-Boussinesq and heat and mass transfer equations in a coordinate system moving with the melt/crystal interface. The parametric dependence of the effective segregation coefficient Keff at the melt/crystal interface was studied for various ampoule sizes and for microgravity conditions. For the uprising one-vortex flow, the resulting dependences were presented as Keff vs. Vmax-the maximum velocity value. These dependences were compared with the formulas by Burton-Prim-Slichter's, Ostrogorsky-Muller's, as well as with the semi-analytical solutions.

Precise Manipulation and Patterning of Protein Crystals for Macromolecular Crystallography Using Surface Acoustic Waves.

PubMed

Guo, Feng; Zhou, Weijie; Li, Peng; Mao, Zhangming; Yennawar, Neela H; French, Jarrod B; Huang, Tony Jun

2015-06-01

Advances in modern X-ray sources and detector technology have made it possible for crystallographers to collect usable data on crystals of only a few micrometers or less in size. Despite these developments, sample handling techniques have significantly lagged behind and often prevent the full realization of current beamline capabilities. In order to address this shortcoming, a surface acoustic wave-based method for manipulating and patterning crystals is developed. This method, which does not damage the fragile protein crystals, can precisely manipulate and pattern micrometer and submicrometer-sized crystals for data collection and screening. The technique is robust, inexpensive, and easy to implement. This method not only promises to significantly increase efficiency and throughput of both conventional and serial crystallography experiments, but will also make it possible to collect data on samples that were previously intractable. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-destructive crystal size determination in geological samples of archaeological use by means of infrared spectroscopy.

PubMed

Olivares, M; Larrañaga, A; Irazola, M; Sarmiento, A; Murelaga, X; Etxebarria, N

2012-08-30

The determination of crystal size of chert samples can provide suitable information about the raw material used for the manufacture of archeological items. X-ray diffraction (XRD) has been widely used for this purpose in several scientific areas. However, the historical value of archeological pieces makes this procedure sometimes unfeasible and thus, non-invasive new analytical approaches are required. In this sense, a new method was developed relating the crystal size obtained by means of XRD and infrared spectroscopy (IR) using partial least squares regression. The IR spectra collected from a large amount of different geological chert samples of archeological use were pre-processed following different treatments (i.e., derivatization or sample-wise normalization) to obtain the best regression model. The full cross-validation was satisfactorily validated using real samples and the experimental root mean standard error of precision value was 165 Å whereas the average precision of the estimated size value was 3%. The features of infrared bands were also evaluated in order to know the background of the prediction ability. In the studied case, the variance in the model was associated to the differences in the characteristic stretching and bending infrared bands of SiO(2). Based on this fact, it would be feasible to estimate the crystal size if it is built beforehand a chemometric model relating the size measured by standard methods and the IR spectra. Copyright © 2012 Elsevier B.V. All rights reserved.

General equations for the motions of ice crystals and water drops in gravitational and electric fields

NASA Technical Reports Server (NTRS)

Nisbet, John S.

1988-01-01

General equations for the Reynolds number of a variety of types of ice crystals and water drops are given in terms of the Davies, Bond, and Knudsen numbers. The equations are in terms of the basic physical parameters of the system and are valid for calculating velocities in gravitational and electric fields over a very wide range of sizes and atmospheric conditions. The equations are asymptotically matched at the bottom and top of the size spectrum, useful when checking large computer codes. A numerical system for specifying the dimensional properties of ice crystals is introduced. Within the limits imposed by such variables as particle density, which have large deviations, the accuracy of velocities appears to be within 10 percent over the entire range of sizes of interest.

Controlled crystallization of the lipophilic drug fenofibrate during freeze-drying: elucidation of the mechanism by in-line Raman spectroscopy.

PubMed

de Waard, Hans; De Beer, Thomas; Hinrichs, Wouter L J; Vervaet, Chris; Remon, Jean-Paul; Frijlink, Henderik W

2010-12-01

We developed a novel process, "controlled crystallization during freeze-drying" to produce drug nanocrystals of poorly water-soluble drugs. This process involves freeze-drying at a relatively high temperature of a drug and a matrix material from a mixture of tertiary butyl alcohol and water, resulting in drug nanocrystals incorporated in a matrix. The aim of this study was to elucidate the mechanisms that determine the size of the drug crystals. Fenofibrate was used as a model lipophilic drug. To monitor the crystallization during freeze-drying, a Raman probe was placed just above the sample in the freeze-dryer. These in-line Raman spectroscopy measurements clearly revealed when the different components crystallized during freeze-drying. The solvents crystallized only during the freezing step, while the solutes only crystallized after the temperature was increased, but before drying started. Although the solutes crystallized only after the freezing step, both the freezing rate and the shelf temperature were critical parameters that determined the final crystal size. At a higher freezing rate, smaller interstitial spaces containing the freeze-concentrated fraction were formed, resulting in smaller drug crystals (based on dissolution data). On the other hand, when the solutes crystallized at a lower shelf temperature, the degree of supersaturation is higher, resulting in a higher nucleation rate and consequently more and therefore smaller crystals. In conclusion, for the model drug fenofibrate, a high freezing rate and a relatively low crystallization temperature resulted in the smallest crystals and therefore the highest dissolution rate.

Method of making macrocrystalline or single crystal semiconductor material

NASA Technical Reports Server (NTRS)

Shlichta, P. J. (Inventor); Holliday, R. J. (Inventor)

1986-01-01

A macrocrystalline or single crystal semiconductive material is formed from a primary substrate including a single crystal or several very large crystals of a relatively low melting material. This primary substrate is deposited on a base such as steel or ceramic, and it may be formed from such metals as zinc, cadmium, germanium, aluminum, tin, lead, copper, brass, magnesium silicide, or magnesium stannide. These materials generally have a melting point below about 1000 C and form on the base crystals the size of fingernails or greater. The primary substrate has an epitaxial relationship with a subsequently applied layer of material, and because of this epitaxial relationship, the material deposited on the primary substrate will have essentially the same crystal size as the crystals in the primary substrate. If required, successive layers are formed, each of a material which has an epitaxial relationship with the previously deposited layer, until a layer is formed which has an epitaxial relationship with the semiconductive material. This layer is referred to as the epitaxial substrate, and its crystals serve as sites for the growth of large crystals of semiconductive material. The primary substrate is passivated to remove or otherwise convert it into a stable or nonreactive state prior to deposition of the seconductive material.

Ensemble Weight Enumerators for Protograph LDPC Codes

NASA Technical Reports Server (NTRS)

Divsalar, Dariush

2006-01-01

Recently LDPC codes with projected graph, or protograph structures have been proposed. In this paper, finite length ensemble weight enumerators for LDPC codes with protograph structures are obtained. Asymptotic results are derived as the block size goes to infinity. In particular we are interested in obtaining ensemble average weight enumerators for protograph LDPC codes which have minimum distance that grows linearly with block size. As with irregular ensembles, linear minimum distance property is sensitive to the proportion of degree-2 variable nodes. In this paper the derived results on ensemble weight enumerators show that linear minimum distance condition on degree distribution of unstructured irregular LDPC codes is a sufficient but not a necessary condition for protograph LDPC codes.

Crystallization of aqueous inorganic-malonic acid particles: nucleation rates, dependence on size, and dependence on the ammonium-to-sulfate ratio.

PubMed

Parsons, Matthew T; Riffell, Jenna L; Bertram, Allan K

2006-07-06

Using an electrodynamic balance, we determined the relative humidity (RH) at which aqueous inorganic-malonic acid particles crystallized, with ammonium sulfate ((NH(4))(2)SO(4)), letovicite ((NH(4))(3)H(SO(4))(2)), or ammonium bisulfate (NH(4)HSO(4)) as the inorganic component. The results for (NH(4))(2)SO(4)-malonic acid particles and (NH(4))(3)H(SO(4))(2)-malonic acid particles show that malonic acid decreases the crystallization RH of the inorganic particles by less than 7% RH when the dry malonic acid mole fraction is less than 0.25. At a dry malonic acid mole fraction of about 0.5, the presence of malonic acid can decrease the crystallization RH of the inorganic particles by up to 35% RH. For the NH(4)HSO(4)-malonic acid particles, the presence of malonic acid does not significantly modify the crystallization RH of the inorganic particles for the entire range of dry malonic acid mole fractions studied; in all cases, either the particles did not crystallize or the crystallization RH was close to 0% RH. Size dependent measurements show that the crystallization RH of aqueous (NH(4))(2)SO(4) particles is not a strong function of particle volume. However, for aqueous (NH(4))(2)SO(4)-malonic acid particles (with dry malonic acid mole fraction = 0.36), the crystallization RH is a stronger function of particle volume, with the crystallization RH decreasing by 6 +/- 3% RH when the particle volume decreases by an order of magnitude. To our knowledge, these are the first size dependent measurements of the crystallization RH of atmospherically relevant inorganic-organic particles. These results suggest that for certain organic mole fractions the particle size and observation time need to be considered when extrapolating laboratory crystallization results to atmospheric scenarios. For aqueous (NH(4))(2)SO(4) particles, the homogeneous nucleation rate data are a strong function of RH, but for aqueous (NH(4))(2)SO(4)-malonic acid particles (with dry organic mole fraction = 0.36), the rates are not as dependent on RH. The homogeneous nucleation rates for aqueous (NH(4))(2)SO(4) particles were parametrized using classical nucleation theory, and from this analysis we determined that the interfacial surface tension between the crystalline ammonium sulfate critical nucleus and an aqueous ammonium sulfate solution is between 0.053 and 0.070 J m(-2).

Crystal Growth of Undoped and Doped ZnSe

NASA Technical Reports Server (NTRS)

Davis, Swanson L.; Chen, K.-T.; George, M. A.; Shi, D. T.; Collins, W. E.; Burger, Arnold

1997-01-01

The surface morphology of freshly cleaved ZnSe single crystal grown by the physical vapor transport (PVT) method was investigated by Atomic Force Microscopy (AFM) and the results were correlated with Differential Scanning Calorimetry (DSC) data. Selenium precipitates have been revealed in undoped doped ZnSe crystals having a size of about 50 nm. A transition temperature around 221 C in the DSC measurements is interpreted as the eutectic temperature of Se-saturated ZnSe. The AFM images of doped ZnSe also show that possible Cr clusters are uniformly distributed and they have an estimated size of about 6 nm.

A model predicting the evolution of ice particle size spectra and radiative properties of cirrus clouds. Part 2: Dependence of absorption and extinction on ice crystal morphology

NASA Technical Reports Server (NTRS)

Mitchell, David L.; Arnott, W. Patrick

1994-01-01

This study builds upon the microphysical modeling described in Part 1 by deriving formulations for the extinction and absorption coefficients in terms of the size distribution parameters predicted from the micro-physical model. The optical depth and single scatter albedo of a cirrus cloud can then be determined, which, along with the asymmetry parameter, are the input parameters needed by cloud radiation models. Through the use of anomalous diffraction theory, analytical expressions were developed describing the absorption and extinction coefficients and the single scatter albedo as functions of size distribution parameters, ice crystal shapes (or habits), wavelength, and refractive index. The extinction coefficient was formulated in terms of the projected area of the size distribution, while the absorption coefficient was formulated in terms of both the projected area and mass of the size distribution. These properties were formulated as explicit functions of ice crystal geometry and were not based on an 'effective radius.' Based on simulations of the second cirrus case study described in Part 1, absorption coefficients predicted in the near infrared for hexagonal columns and rosettes were up to 47% and 71% lower, respectively, than absorption coefficients predicted by using equivalent area spheres. This resulted in single scatter albedos in the near-infrared that were considerably greater than those predicted by the equivalent area sphere method. Reflectances in this region should therefore be underestimated using the equivalent area sphere approach. Cloud optical depth was found to depend on ice crystal habit. When the simulated cirrus cloud contained only bullet rosettes, the optical depth was 142% greater than when the cloud contained only hexagonal columns. This increase produced a doubling in cloud albedo. In the near-infrared (IR), the single scatter albedo also exhibited a significant dependence on ice crystal habit. More research is needed on the geometrical properties of ice crystals before the influence of ice crystal shape on cirrus radiative properties can be adequately understood. This study provides a way of coupling the radiative properties of absorption, extinction, and single scatter albedo to the microphysical properties of cirrus clouds. The dependence of extinction and absorption on ice crystal shape was not just due to geometrical differences between crystal types, but was also due to the effect these differences had on the evolution of ice particle size spectra. The ice particle growth model in Part 1 and the radiative properties treated here are based on analytical formulations, and thus represent a computationally efficient means of modeling the microphysical and radiative properties of cirrus clouds.

A hetero-micro-seeding strategy for readily crystallizing closely related protein variants.

PubMed

Islam, Mohammad M; Kuroda, Yutaka

2017-11-04

Protein crystallization remains difficult to rationalize and screening for optimal crystallization conditions is a tedious and time consuming procedure. Here, we report a hetero-micro-seeding strategy for producing high resolution crystals of closely related protein variants, where micro crystals from a readily crystallized variant are used as seeds to develop crystals of other variants less amenable to crystallization. We applied this strategy to Bovine Pancreatic Trypsin Inhibitor (BPTI) variants, which would not crystallize using standard crystallization practice. Out of six variants in our analysis, only one called BPTI-[5,55]A14G formed well behaving crystals; and the remaining five (A14GA38G, A14GA38V, A14GA38L, A14GA38I, and A14GA38K) could be crystallized only using micro-seeds from the BPTI-[5,55]A14G crystal. All hetero-seeded crystals diffracted at high resolution with minimum mosaicity, retaining the same space group and cell dimension. Moreover, hetero-micro-seeding did not introduce any biases into the mutant's structure toward the seed structure, as demonstrated by A14GA38I structures solved using micro-seeds from A14GA38G, A14GA38L and A14GA38I. Though hetero-micro-seeding is a simple and almost naïve strategy, this is the first direct demonstration of its workability. We believe that hetero-micro-seeding, which is contrasting with the popular idea that crystallization requires highly purified proteins, could contribute a new tool for rapidly solving protein structures in mutational analysis studies. Copyright © 2017 Elsevier Inc. All rights reserved.

Quartz c-axis orientation patterns in fracture cement as a measure of fracture opening rate and a validation tool for fracture pattern models

DOE PAGES

Ukar, Estibalitz; Laubach, Stephen E.; Marrett, Randall

2016-03-09

Here, we evaluate a published model for crystal growth patterns in quartz cement in sandstone fractures by comparing crystal fracture-spanning predictions to quartz c-axis orientation distributions measured by electron backscatter diffraction (EBSD) of spanning quartz deposits. Samples from eight subvertical opening-mode fractures in four sandstone formations, the Jurassic– Cretaceous Nikanassin Formation, northwestern Alberta Foothills (Canada), Cretaceous Mesaverde Group (USA; Cozzette Sandstone Member of the Iles Formation), Piceance Basin, Colorado (USA), and upper Jurassic–lower Cretaceous Cotton Valley Group (Taylor sandstone) and overlying Travis Peak Formation, east Texas, have similar quartzose composition and grain size but contain fractures with different temperature historiesmore » and opening rates based on fluid inclusion assemblages and burial history. Spherical statistical analysis shows that, in agreement with model predictions, bridging crystals have a preferred orientation with c-axis orientations at a high angle to fracture walls. The second form of validation is for spanning potential that depends on the size of cut substrate grains. Using measured cut substrate grain sizes and c-axis orientations of spanning bridges, we calculated the required orientation for the smallest cut grain to span the maximum gap size and the required orientation of the crystal with the least spanning potential to form overgrowths that span across maximum measured gap sizes. We find that within a 10° error all spanning crystals conform to model predictions. Using crystals with the lowest spanning potential based on crystallographic orientation (c-axis parallel to fracture wall) and a temperature range for fracture opening measured from fluid inclusion assemblages, we calculate maximum fracture opening rates that allow crystals to span. These rates are comparable to those derived independently from fracture temperature histories based on burial history and multiple sequential fluid inclusion assemblages. Results support the R. Lander and S. Laubach model, which predicts that for quartz deposited synchronously with fracture opening, spanning potential, or likelihood of quartz deposits that are thick enough to span between fracture walls, depends on temperature history, fracture opening rate, size of opening increments, and size, mineralogy, and crystallographic orientation of substrates in the fracture wall (transected grains). Results suggest that EBSD maps, which can be more rapidly acquired than measurement of tens to hundreds of fluid inclusion assemblages, can provide a useful measure of relative opening rates within populations of quartz-filled fractures formed under sedimentary basin conditions. Such data are useful for evaluating fracture pattern development models.« less

Quartz c-axis orientation patterns in fracture cement as a measure of fracture opening rate and a validation tool for fracture pattern models

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

Ukar, Estibalitz; Laubach, Stephen E.; Marrett, Randall

Here, we evaluate a published model for crystal growth patterns in quartz cement in sandstone fractures by comparing crystal fracture-spanning predictions to quartz c-axis orientation distributions measured by electron backscatter diffraction (EBSD) of spanning quartz deposits. Samples from eight subvertical opening-mode fractures in four sandstone formations, the Jurassic– Cretaceous Nikanassin Formation, northwestern Alberta Foothills (Canada), Cretaceous Mesaverde Group (USA; Cozzette Sandstone Member of the Iles Formation), Piceance Basin, Colorado (USA), and upper Jurassic–lower Cretaceous Cotton Valley Group (Taylor sandstone) and overlying Travis Peak Formation, east Texas, have similar quartzose composition and grain size but contain fractures with different temperature historiesmore » and opening rates based on fluid inclusion assemblages and burial history. Spherical statistical analysis shows that, in agreement with model predictions, bridging crystals have a preferred orientation with c-axis orientations at a high angle to fracture walls. The second form of validation is for spanning potential that depends on the size of cut substrate grains. Using measured cut substrate grain sizes and c-axis orientations of spanning bridges, we calculated the required orientation for the smallest cut grain to span the maximum gap size and the required orientation of the crystal with the least spanning potential to form overgrowths that span across maximum measured gap sizes. We find that within a 10° error all spanning crystals conform to model predictions. Using crystals with the lowest spanning potential based on crystallographic orientation (c-axis parallel to fracture wall) and a temperature range for fracture opening measured from fluid inclusion assemblages, we calculate maximum fracture opening rates that allow crystals to span. These rates are comparable to those derived independently from fracture temperature histories based on burial history and multiple sequential fluid inclusion assemblages. Results support the R. Lander and S. Laubach model, which predicts that for quartz deposited synchronously with fracture opening, spanning potential, or likelihood of quartz deposits that are thick enough to span between fracture walls, depends on temperature history, fracture opening rate, size of opening increments, and size, mineralogy, and crystallographic orientation of substrates in the fracture wall (transected grains). Results suggest that EBSD maps, which can be more rapidly acquired than measurement of tens to hundreds of fluid inclusion assemblages, can provide a useful measure of relative opening rates within populations of quartz-filled fractures formed under sedimentary basin conditions. Such data are useful for evaluating fracture pattern development models.« less

Towards true 3D textural analysis; using your crystal mush wisely.

NASA Astrophysics Data System (ADS)

Jerram, D. A.; Morgan, D. J.; Pankhurst, M. J.

2014-12-01

The crystal cargo that is found in volcanic and plutonic rocks contains a wealth of information about magmatic mush processes, crystallisation history, crystal entrainment and recycling. Phenocryst populations predominantly record episodes of growth/nucleation and bulk geochemical changes within an evolving crystal-melt body. Ante- and xeno-crysts provide useful clues to the nature of mush interaction with wall rock and with principal magma(s). Furthermore, crystal evolutions (core to rim) record pathways through pressure, temperature and compositional space. These can often illustrate complex recycling within systems, describing the plumbing architecture. Understanding this architecture underpins our knowledge of how igneous systems can interact with the crust, grow, freeze, re-mobilise and prime for eruption. Initially, 2D studies produced corrected 3D crystal size distributions to help provide information about nucleation and residence times. It immediately became clear that crystal shape is an important factor in determining the confidence placed upon 3D reconstructions of 2D data. Additionally studies utilised serial sections of medium- to coarse-grain-size populations which allowed 3D reconstruction using modelling software to be improved, since size and shape etc. can be directly constrained. Finally the advent of textural studies using X-ray tomography has revolutionised the way in which we can inspect the crystal cargo in mushy systems, allowing us to image in great detail crystal packing arrangements, 3D CSDs, shapes and orientations etc. The latest most innovative studies use X-ray micro-computed tomography to rapidly characterise chemical populations within the crystal cargo, adding a further dimension to this approach, and implies the ability to untangle magmatic chemical components to better understand their individual and combined evolution. In this contribution key examples of the different types of textural analysis techniques in 2D and 3D, including texture movie animations, are used from both plutonic and volcanic systems to highlight the roll of this approach towards a goal of true 3D textural analysis.

Type, origin, and reservoir characteristics of dolostones of the Ordovician Majiagou Group, Ordos, North China Platform

NASA Astrophysics Data System (ADS)

Feng Zengzhao; Zhang Yongsheng; Jin Zhenkui

1998-06-01

Dolostones are well developed in the Ordovician Majiagou Group in the Ordos area, North China Platform. These dolostones can be divided into four types: mud-sized to silt-sized crystalline dolostones not associated with gypsum and halite beds (type I), mud-sized to silt-sized crystalline dolostones associated with gypsum and halite beds (type II), mottled silt-sized to very fine sand-sized crystalline dolostones (fine saccharoidal dolostones) (type III), and mottled coarse silt-sized to fine sand-sized crystalline dolostones (coarse saccharoidal dolostones) (type IV). Type I dolostones consist of mud-sized to silt-sized dolomite crystals. Laminar stromatolites, ripple marks, mud cracks and birdseyes are common. Such dolostones are not associated with gypsum and halite beds, but lath-shaped pseudomorphs after gypsum are common. The ordering of dolomites averages 0.59, and molar concentration of CaCO 3 averages 51.44%. δ13C averages -0.8‰ (PDB Standard), δ18O averages -2.9‰, δCe averages 0.83. The above characteristics suggest that type I dolostones result from penecontemporaneous dolomitization of lime mud on supratidal flat environments by hypersaline sea water. Type II dolostones mainly consist of mud-sized to silt-sized dolomite crystals. They are commonly well laminated but show no desiccation structures. Such dolostones are intercalated within laminated gypsum and halite beds or are intermixed with them. Such dolostones resulted from dolomitization of lime mud by hypersaline sea water in gypsum and halite precipitating lagoons. Type III dolostones consist of coarse silt-sized to very fine sand-sized dolomite crystals. They commonly underlie type I dolostones and grade downwards to dolomite-mottled limestones and pure limestones. The ordering of dolomites averages 0.63, and molar concentration of CaCO 3 averages 55.64%. δ13C averages -0.2‰, δ18O averages -3.3‰, δCe averages 1.24. Such dolostones resulted from reflux dolomitization by hypersaline sea water. Type IV dolostones consist of coarse-silt-sized to fine-sand-sized dolomite crystals. In such dolostones, stylolites are cut by dolomite crystals. Fluid inclusions are present, and the homogenization temperature commonly ranges from 104°C to 203°C. The ordering of dolomites averages 0.85, and molar concentration of CaCO 3 averages 50.65%. δ13C averages 0.6‰, δ18O averages -7.4‰, and δCe averages 1.16. Such dolostones resulted from deep burial dolomitization. In the Ordos area, type I and II dolostones modified by palaeokarstification are the major gas reservoir rocks of the Ordos Gas Field at present. Type IV dolostones show good reservoir characteristics and may also be potential reservoir rocks.

46 CFR 76.10-90 - Installations contracted for prior to May 26, 1965.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Not over Minimum number of pumps Minimum hose and hydrant size, inches Nozzle orifice size, inches Length of hose, feet 100 4,000 2 1 11/2 1 5/8 1 50 4,000 3 1 11/2 1 5/8 1 50 1 May use 50 feet of 21/2-inch hose with 7/8-inch nozzles for exterior stations. May use 75 feet of 11/2-inch hose with 5/8-inch...

Evaluation of alternative model selection criteria in the analysis of unimodal response curves using CART

USGS Publications Warehouse

Ribic, C.A.; Miller, T.W.

1998-01-01

We investigated CART performance with a unimodal response curve for one continuous response and four continuous explanatory variables, where two variables were important (ie directly related to the response) and the other two were not. We explored performance under three relationship strengths and two explanatory variable conditions: equal importance and one variable four times as important as the other. We compared CART variable selection performance using three tree-selection rules ('minimum risk', 'minimum risk complexity', 'one standard error') to stepwise polynomial ordinary least squares (OLS) under four sample size conditions. The one-standard-error and minimum-risk-complexity methods performed about as well as stepwise OLS with large sample sizes when the relationship was strong. With weaker relationships, equally important explanatory variables and larger sample sizes, the one-standard-error and minimum-risk-complexity rules performed better than stepwise OLS. With weaker relationships and explanatory variables of unequal importance, tree-structured methods did not perform as well as stepwise OLS. Comparing performance within tree-structured methods, with a strong relationship and equally important explanatory variables, the one-standard-error-rule was more likely to choose the correct model than were the other tree-selection rules 1) with weaker relationships and equally important explanatory variables; and 2) under all relationship strengths when explanatory variables were of unequal importance and sample sizes were lower.

Growth of urea crystals by physical vapor transport

NASA Technical Reports Server (NTRS)

Feigelson, R. S.; Route, R. K.; Kao, T.-M.

1985-01-01

This work demonstrates that high optical quality crystals of urea can be grown by the physical vapor transport method. The unique features of this method are compared with growth from methanol/water solutions. High growth rates, exceeding 2.5 mm/day, were achieved, and cm-size optical quality single crystals were obtained. Details of the growth technique and the physical properties of the crystals are presented.

Synthesis of nanoparticles in a flame aerosol reactor with independent and strict control of their size, crystal phase and morphology

NASA Astrophysics Data System (ADS)

Jiang, Jingkun; Chen, Da-Ren; Biswas, Pratim

2007-07-01

A flame aerosol reactor (FLAR) was developed to synthesize nanoparticles with desired properties (crystal phase and size) that could be independently controlled. The methodology was demonstrated for TiO2 nanoparticles, and this is the first time that large sets of samples with the same size but different crystal phases (six different ratios of anatase to rutile in this work) were synthesized. The degree of TiO2 nanoparticle agglomeration was determined by comparing the primary particle size distribution measured by scanning electron microscopy (SEM) to the mobility-based particle size distribution measured by online scanning mobility particle spectrometry (SMPS). By controlling the flame aerosol reactor conditions, both spherical unagglomerated particles and highly agglomerated particles were produced. To produce monodisperse nanoparticles, a high throughput multi-stage differential mobility analyser (MDMA) was used in series with the flame aerosol reactor. Nearly monodisperse nanoparticles (geometric standard deviation less than 1.05) could be collected in sufficient mass quantities (of the order of 10 mg) in reasonable time (1 h) that could be used in other studies such as determination of functionality or biological effects as a function of size.

Protein Crystallization

NASA Technical Reports Server (NTRS)

Chernov, Alexander A.

2005-01-01

Nucleation, growth and perfection of protein crystals will be overviewed along with crystal mechanical properties. The knowledge is based on experiments using optical and force crystals behave similar to inorganic crystals, though with a difference in orders of magnitude in growing parameters. For example, the low incorporation rate of large biomolecules requires up to 100 times larger supersaturation to grow protein, rather than inorganic crystals. Nucleation is often poorly reproducible, partly because of turbulence accompanying the mixing of precipitant with protein solution. Light scattering reveals fluctuations of molecular cluster size, its growth, surface energies and increased clustering as protein ages. Growth most often occurs layer-by-layer resulting in faceted crystals. New molecular layer on crystal face is terminated by a step where molecular incorporation occurs. Quantitative data on the incorporation rate will be discussed. Rounded crystals with molecularly disordered interfaces will be explained. Defects in crystals compromise the x-ray diffraction resolution crucially needed to find the 3D atomic structure of biomolecules. The defects are immobile so that birth defects stay forever. All lattice defects known for inorganics are revealed in protein crystals. Contribution of molecular conformations to lattice disorder is important, but not studied. This contribution may be enhanced by stress field from other defects. Homologous impurities (e.g., dimers, acetylated molecules) are trapped more willingly by a growing crystal than foreign protein impurities. The trapped impurities induce internal stress eliminated in crystals exceeding a critical size (part of mni for ferritin, lysozyme). Lesser impurities are trapped from stagnant, as compared to the flowing, solution. Freezing may induce much more defects unless quickly amorphysizing intracrystalline water.

Protograph based LDPC codes with minimum distance linearly growing with block size

NASA Technical Reports Server (NTRS)

Divsalar, Dariush; Jones, Christopher; Dolinar, Sam; Thorpe, Jeremy

2005-01-01

We propose several LDPC code constructions that simultaneously achieve good threshold and error floor performance. Minimum distance is shown to grow linearly with block size (similar to regular codes of variable degree at least 3) by considering ensemble average weight enumerators. Our constructions are based on projected graph, or protograph, structures that support high-speed decoder implementations. As with irregular ensembles, our constructions are sensitive to the proportion of degree-2 variable nodes. A code with too few such nodes tends to have an iterative decoding threshold that is far from the capacity threshold. A code with too many such nodes tends to not exhibit a minimum distance that grows linearly in block length. In this paper we also show that precoding can be used to lower the threshold of regular LDPC codes. The decoding thresholds of the proposed codes, which have linearly increasing minimum distance in block size, outperform that of regular LDPC codes. Furthermore, a family of low to high rate codes, with thresholds that adhere closely to their respective channel capacity thresholds, is presented. Simulation results for a few example codes show that the proposed codes have low error floors as well as good threshold SNFt performance.

Determination of Minimum Training Sample Size for Microarray-Based Cancer Outcome Prediction–An Empirical Assessment

PubMed Central

Cheng, Ningtao; Wu, Leihong; Cheng, Yiyu

2013-01-01

The promise of microarray technology in providing prediction classifiers for cancer outcome estimation has been confirmed by a number of demonstrable successes. However, the reliability of prediction results relies heavily on the accuracy of statistical parameters involved in classifiers. It cannot be reliably estimated with only a small number of training samples. Therefore, it is of vital importance to determine the minimum number of training samples and to ensure the clinical value of microarrays in cancer outcome prediction. We evaluated the impact of training sample size on model performance extensively based on 3 large-scale cancer microarray datasets provided by the second phase of MicroArray Quality Control project (MAQC-II). An SSNR-based (scale of signal-to-noise ratio) protocol was proposed in this study for minimum training sample size determination. External validation results based on another 3 cancer datasets confirmed that the SSNR-based approach could not only determine the minimum number of training samples efficiently, but also provide a valuable strategy for estimating the underlying performance of classifiers in advance. Once translated into clinical routine applications, the SSNR-based protocol would provide great convenience in microarray-based cancer outcome prediction in improving classifier reliability. PMID:23861920

Application of the Maximum Amplitude-Early Rise Correlation to Cycle 23

NASA Technical Reports Server (NTRS)

Willson, Robert M.; Hathaway, David H.

2004-01-01

On the basis of the maximum amplitude-early rise correlation, cycle 23 could have been predicted to be about the size of the mean cycle as early as 12 mo following cycle minimum. Indeed, estimates for the size of cycle 23 throughout its rise consistently suggested a maximum amplitude that would not differ appreciably from the mean cycle, contrary to predictions based on precursor information. Because cycle 23 s average slope during the rising portion of the solar cycle measured 2.4, computed as the difference between the conventional maximum (120.8) and minimum (8) amplitudes divided by the ascent duration in months (47), statistically speaking, it should be a cycle of shorter period. Hence, conventional sunspot minimum for cycle 24 should occur before December 2006, probably near July 2006 (+/-4 mo). However, if cycle 23 proves to be a statistical outlier, then conventional sunspot minimum for cycle 24 would be delayed until after July 2007, probably near December 2007 (+/-4 mo). In anticipation of cycle 24, a chart and table are provided for easy monitoring of the nearness and size of its maximum amplitude once onset has occurred (with respect to the mean cycle and using the updated maximum amplitude-early rise relationship).

Crystallite size strain analysis of nanocrystalline La0.7Sr0.3MnO3 perovskite by Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Verma, Narendra Kumar; Singh, Chandra Bhal; Singh, Akhilesh Kumar

2018-04-01

The nanocrystalline Sr-doped LaMnO3 (La0.7Sr0.3MnO3 = LSMO) perovskite manganites having different crystallite size were synthesized using the nitrate-glycine auto-combustion method. The phase purity of the manganites was checked by X-ray diffraction (XRD) measurement. The XRD patterns of the sample reveal that La0.7S0.3MnO3 crystallizes into rhombohedral crystal structure with space group R-3c. The size-dependence of structural lattice parameters have been investigated with the help of Rietveld refinement. The structural parameters increase as a function of crystallite size. The crystallite-size and internal strain as a function of crystallite-size have been calculated using Williamson-Hall plot.

No support for Heincke's law in hagfish (Myxinidae): lack of an association between body size and the depth of species occurrence.

PubMed

Schumacher, E L; Owens, B D; Uyeno, T A; Clark, A J; Reece, J S

2017-08-01

This study tests for interspecific evidence of Heincke's law among hagfishes and advances the field of research on body size and depth of occurrence in fishes by including a phylogenetic correction and by examining depth in four ways: maximum depth, minimum depth, mean depth of recorded specimens and the average of maximum and minimum depths of occurrence. Results yield no evidence for Heincke's law in hagfishes, no phylogenetic signal for the depth at which species occur, but moderate to weak phylogenetic signal for body size, suggesting that phylogeny may play a role in determining body size in this group. © 2017 The Fisheries Society of the British Isles.

Aerosol-Cloud Interactions during Tropical Deep Convection: Evidence for the Importance of Free Tropospheric Aerosols

NASA Technical Reports Server (NTRS)

Ackerman, A.; Jensen, E.; Stevens, D.; Wang, D.; Heymsfield, A.; Miloshevich, L.; Twohy, C.; Poellot, M.; VanReken, T.; Fridland, Ann

2003-01-01

NASA's 2002 CRYSTAL-FACE field experiment focused on the formation and evolution of tropical cirrus cloud systems in southern Florida. Multiple aircraft extensively sampled cumulonimbus dynamical and microphysical properties, as well as characterizing ambient aerosol populations both inside and outside the full depth of the convective column. On July 18, unique measurements were taken when a powerful updraft was traversed directly by aircraft, providing a window into the primary source region of cumulonimbus anvil crystals. Observations of the updraft, entered at approximately l0 km altitude and -34 C, indicated more than 200 cloud particles per mL at vertical velocities exceeding 20 m/s and the presence of significant condensation nuclei and liquid water within the core. In this work, aerosol and cloud phase observations are integrated by simulating the updraft conditions using a large-eddy resolving model with 3 explicit multiphase microphysics, including treatment of size-resolved aerosol fields, aerosol activation and freezing, and evaporation of cloud particles back to the aerosol phase. Simulations were initialized with observed thermodynamic and aerosol size distributions profiles and convection was driven by surface fluxes assimilated from the ARPS forecast model. Model results are consistent with the conclusions that most crystals are homogeneously frozen droplets and that entrained free tropospheric aerosols may contribute a significant fraction of the crystals. Thus most anvil crystals appear to be formed aloft in updraft cores, well above cloud base. These conclusions are supported by observations of hydrometeor size distribution made while traversing the dore, as well as aerosol and cloud particle size distributions generally observed by aircraft below 4km and crystal properties generally observed by aircraft above 12km.

Random lasing in dye-doped polymer dispersed liquid crystal film

NASA Astrophysics Data System (ADS)

Wu, Rina; Shi, Rui-xin; Wu, Xiaojiao; Wu, Jie; Dai, Qin

2016-09-01

A dye-doped polymer-dispersed liquid crystal film was designed and fabricated, and random lasing action was studied. A mixture of laser dye, nematic liquid crystal, chiral dopant, and PVA was used to prepare the dye-doped polymer-dispersed liquid crystal film by means of microcapsules. Scanning electron microscopy analysis showed that most liquid crystal droplets in the polymer matrix ranged from 30 μm to 40 μm, the size of the liquid crystal droplets was small. Under frequency doubled 532 nm Nd:YAG laser-pumped optical excitation, a plurality of discrete and sharp random laser radiation peaks could be measured in the range of 575-590 nm. The line-width of the lasing peak was 0.2 nm and the threshold of the random lasing was 9 mJ. Under heating, the emission peaks of random lasing disappeared. By detecting the emission light spot energy distribution, the mechanism of radiation was found to be random lasing. The random lasing radiation mechanism was then analyzed and discussed. Experimental results indicated that the size of the liquid crystal droplets is the decisive factor that influences the lasing mechanism. The surface anchor role can be ignored when the size of the liquid crystal droplets in the polymer matrix is small, which is beneficial to form multiple scattering. The transmission path of photons is similar to that in a ring cavity, providing feedback to obtain random lasing output. Project supported by the National Natural Science Foundation of China (Grant No. 61378042), the Colleges and Universities in Liaoning Province Outstanding Young Scholars Growth Plans, China (Grant No. LJQ2015093), and Shenyang Ligong University Laser and Optical Information of Liaoning Province Key Laboratory Open Funds, China.

DAST single-nanometer crystal preparation using a substrate-supported rapid evaporation crystallization method.

PubMed

Tian, Tian; Cai, Bin; Sugihara, Okihiro

2016-12-07

A substrate-supported rapid evaporation crystallization (SSREC) method was used to develop a highly nonlinear optical material, 4-N,N-dimethylamino-4'-N'-methyl-stilbazolium tosylate (DAST), which satisfies the Rayleigh scattering requirement for the fabrication of highly transparent composites. DAST nanocrystals have a second harmonic generation active crystal structure and a high signal-to-noise ratio second harmonic generation signal when excited by using a 1064 nm cw laser. The nanocrystals also possess size-dependent UV-vis absorption and fluorescence behavior which is not seen in the bulk state. SSREC offers a very convenient means of nanocrystal size control for fabricating nonlinear optical nanomaterials, and the unique properties of these DAST NCs provide potential applications in the fields of lasing, fluorescence probes, and other nonlinear optical photonics.

Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

NASA Astrophysics Data System (ADS)

Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

2017-06-01

The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.

High-temperature crystallization of nanocrystals into three-dimensional superlattices

DOE PAGES

Wu, Liheng; Willis, Joshua J.; McKay, Ian Salmon; ...

2017-07-31

Crystallization of colloidal nanocrystals into superlattices represents a practical bottom-up process with which to create ordered metamaterials with emergent functionalities. With precise control over the size, shape and composition of individual nanocrystals, various single-and multi-component nanocrystal superlattices have been produced, the lattice structures and chemical compositions of which can be accurately engineered. Nanocrystal superlattices are typically prepared by carefully controlling the assembly process through solvent evaporation or destabilization or through DNA-guided crystallization. Slow solvent evaporation or cooling of nanocrystal solutions (over hours or days) is the key element for successful crystallization processes. Here we report the rapid growth (seconds) ofmore » micrometre-sized, face-centred-cubic, three-dimensional nanocrystal superlattices during colloidal synthesis at high temperatures (more than 230 degrees Celsius). Using in situ small-angle X-ray scattering, we observe continuous growth of individual nanocrystals within the lattices, which results in simultaneous lattice expansion and fine nanocrystal size control due to the superlattice templates. Thermodynamic models demonstrate that balanced attractive and repulsive interparticle interactions dictated by the ligand coverage on nanocrystal surfaces and nanocrystal core size are responsible for the crystallization process. The interparticle interactions can also be controlled to form different superlattice structures, such as hexagonal close-packed lattices. In conclusion, the rational assembly of various nanocrystal systems into novel materials is thus facilitated for both fundamental research and for practical applications in the fields of magnetics, electronics and catalysis.« less

Automated protein crystal growth facility

NASA Astrophysics Data System (ADS)

Donald, Stacey

A customer for the protein crystal growth facility fills the specially designed chamber with the correct solutions, fills the syringes with their quenching solutions, and submits the data needed for the proper growth of their crystal. To make sure that the chambers and syringes are filled correctly, a NASA representative may assist the customer. The data needed is the approximate growth time, the growth temperature, and the desired crystal size, but this data can be changed anytime from the ground, if needed. The chambers are gathered and placed into numbered slots in special drawers. Then, data is entered into a computer for each of the chambers. Technicians map out when each chamber's growth should be activated so that all of the chambers have enough time to grow. All of this data is up-linked to the space station when the previous growth session is over. Anti-vibrational containers need to be constructed for the high forces encountered during the lift off and the landing of the space shuttle, and though our team has not designed these containers, we do not feel that there is any reason why a suitable one could not be made. When the shuttle reaches the space station, an astronaut removes a drawer of quenched chambers from the growth facility and inserts a drawer of new chambers. All twelve of the drawers can be replaced in this fashion. The optical disks can also be removed this way. The old drawers are stored for the trip back to earth. Once inside the growth facility, a chamber is removed by the robot and placed in one of 144 active sites at a time previously picked by a technician. Growth begins when the chamber is inserted into an active site. Then, the sensing system starts to determine the size of the protein crystal. All during the crystal's growth, the customer can view the crystal and read all of the crystal's data, such as growth rate and crystal size. When the sensing system determines that the crystal has reached the predetermined size, the robot is told to pick up a syringe filled with the correct quenchant solution and inject it into the chamber to stop the crystal growth. The chamber is then removed from the active site and placed into its original storage slot.

Automated protein crystal growth facility

NASA Technical Reports Server (NTRS)

Donald, Stacey

1994-01-01

A customer for the protein crystal growth facility fills the specially designed chamber with the correct solutions, fills the syringes with their quenching solutions, and submits the data needed for the proper growth of their crystal. To make sure that the chambers and syringes are filled correctly, a NASA representative may assist the customer. The data needed is the approximate growth time, the growth temperature, and the desired crystal size, but this data can be changed anytime from the ground, if needed. The chambers are gathered and placed into numbered slots in special drawers. Then, data is entered into a computer for each of the chambers. Technicians map out when each chamber's growth should be activated so that all of the chambers have enough time to grow. All of this data is up-linked to the space station when the previous growth session is over. Anti-vibrational containers need to be constructed for the high forces encountered during the lift off and the landing of the space shuttle, and though our team has not designed these containers, we do not feel that there is any reason why a suitable one could not be made. When the shuttle reaches the space station, an astronaut removes a drawer of quenched chambers from the growth facility and inserts a drawer of new chambers. All twelve of the drawers can be replaced in this fashion. The optical disks can also be removed this way. The old drawers are stored for the trip back to earth. Once inside the growth facility, a chamber is removed by the robot and placed in one of 144 active sites at a time previously picked by a technician. Growth begins when the chamber is inserted into an active site. Then, the sensing system starts to determine the size of the protein crystal. All during the crystal's growth, the customer can view the crystal and read all of the crystal's data, such as growth rate and crystal size. When the sensing system determines that the crystal has reached the predetermined size, the robot is told to pick up a syringe filled with the correct quenchant solution and inject it into the chamber to stop the crystal growth. The chamber is then removed from the active site and placed into its original storage slot. Another chamber is then placed into the active site and the process is repeated in all of the active sites until all of the chambers have complted their growth. After ninety days (the scheduled time between shuttle visits), the crystal growth is completed, and the old drawers are replaced with new ones. Once the customer extracts the crystals, the chambers are retrieved for future customers.