Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

DOE PAGES

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; ...

2018-04-24

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

Controlled vapor crystal growth of N a 4 I r 3 O 8 : A three-dimensional quantum spin liquid candidate

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

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.

In this work, we report the successful bulk single-crystal growth of the hyperkagome lattice iridate Na 4Ir 3O 8 (Na438) by vapor transport using a sealed aluminum oxide tube as a container. Crystals were characterized by magnetization, x-ray diffraction, and energy-dispersive x-ray measurements, confirming their identity and properties. Single-crystal x-ray diffraction experiments revealed superlattice peaks indexed on a propagation vector q=(1/3,1/3,1/3) based on the cubic substructure with cell parameter a=8.986(1)Å. This superlattice is three-dimensional and fully coherent. Polarization analysis rules out spin and/or orbital order as the underlying origin of the modulation and points to long-range ordering of Na ionsmore » at the notionally disordered Na sites as a plausible origin for the observed superlattice.« less

Micropatterned photoalignment for wavefront controlled switchable optical devices

NASA Astrophysics Data System (ADS)

Glazar, Nikolaus

Photoalignment is a well-established technique for surface alignment of the liquid crystal director. Previously, chrome masks were necessary for patterned photoalignment but were difficult to use, costly, and inflexible. To extend the capabilities of photoalignment we built an automated maskless multi-domain photoalignment device based on a DMD (digital multimirror device) projection system. The device is capable of creating arbitrary photoalignment patterns with micron-sized features. Pancharatnam-Berry phase (PB-phase) is a geometric phase that arises from cyclic change of polarization state. By varying the azimuthal anchoring angle in a hybrid-aligned liquid crystal cell we can control the spatial variation of the PB-phase shift. Using our automated photoalignment device to align the liquid crystal arbitrary wave front manipulations are possible. The PB-phase shift effect is maximized when the cell is tuned to have a half-wave retardation and disappears at full-wave retardation, so the cell can be switched on and off by applying a voltage. Two wavefront controlled devices developed using this technique will be discussed: A switchable liquid crystal phase shift mask for creating sub-diffraction sized photolithographic features, and a transparent diffractive display that utilizes a switchable liquid crystal diffraction grating.

Liquid-phase explosive crystallization of electron-beam-evaporated a-Si films induced by flash lamp annealing

NASA Astrophysics Data System (ADS)

Ohdaira, Keisuke; Matsumura, Hideki

2013-01-01

We succeed in the formation of micrometer-order-thick polycrystalline silicon (poly-Si) films through the flash-lamp-induced liquid-phase explosive crystallization (EC) of precursor a-Si films prepared by electron-beam (EB) evaporation. The velocity of the explosive crystallization (vEC) is estimated to be ˜14 m/s, which is close to the velocity of the liquid-phase epitaxy (LPE) of Si at a temperature around the melting point of a-Si of 1418 K. Poly-Si films formed have micrometer-order-long grains stretched along a lateral crystallization direction, and X-ray diffraction (XRD) and electron diffraction pattern measurements reveal that grains in poly-Si films tend to have a particular orientation. These features are significantly different from our previous results: the formation of poly-Si films containing randomly-oriented 10-nm-sized fine grains formed from a-Si films prepared by catalytic chemical vapor deposition (Cat-CVD) or sputtering. One possible reason for the emergence of a different EC mode in EB-evaporated a-Si films is the suppression of solid-phase nucleation (SPN) during Flash Lamp Annealing (FLA) due to tensile stress which precursor a-Si films originally hold. Poly-Si films formed from EB-evaporated a-Si films would contribute to the realization of high-efficiency thin-film poly-Si solar cells because of large and oriented grains.

Modes of surface premelting in colloidal crystals composed of attractive particles

NASA Astrophysics Data System (ADS)

Li, Bo; Wang, Feng; Zhou, Di; Peng, Yi; Ni, Ran; Han, Yilong

2016-03-01

Crystal surfaces typically melt into a thin liquid layer at temperatures slightly below the melting point of the crystal. Such surface premelting is prevalent in all classes of solids and is important in a variety of metallurgical, geological and meteorological phenomena. Premelting has been studied using X-ray diffraction and differential scanning calorimetry, but the lack of single-particle resolution makes it hard to elucidate the underlying mechanisms. Colloids are good model systems for studying phase transitions because the thermal motions of individual micrometre-sized particles can be tracked directly using optical microscopy. Here we use colloidal spheres with tunable attractions to form equilibrium crystal-vapour interfaces, and study their surface premelting behaviour at the single-particle level. We find that monolayer colloidal crystals exhibit incomplete premelting at their perimeter, with a constant liquid-layer thickness. In contrast, two- and three-layer crystals exhibit conventional complete melting, with the thickness of the surface liquid diverging as the melting point is approached. The microstructures of the surface liquids differ in certain aspects from what would be predicted by conventional premelting theories. Incomplete premelting in the monolayer crystals is triggered by a bulk isostructural solid-solid transition and truncated by a mechanical instability that separately induces homogeneous melting within the bulk. This finding is in contrast to the conventional assumption that two-dimensional crystals melt heterogeneously from their free surfaces (that is, at the solid-vapour interface). The unexpected bulk melting that we observe for the monolayer crystals is accompanied by the formation of grain boundaries, which supports a previously proposed grain-boundary-mediated two-dimensional melting theory. The observed interplay between surface premelting, bulk melting and solid-solid transitions challenges existing theories of surface premelting and two-dimensional melting.

A roadmap to uranium ionic liquids: anti-crystal engineering.

PubMed

Yaprak, Damla; Spielberg, Eike T; Bäcker, Tobias; Richter, Mark; Mallick, Bert; Klein, Axel; Mudring, Anja-Verena

2014-05-19

In the search for uranium-based ionic liquids, tris(N,N-dialkyldithiocarbamato)uranylates have been synthesized as salts of the 1-butyl-3-methylimidazolium (C4mim) cation. As dithiocarbamate ligands binding to the UO2(2+) unit, tetra-, penta-, hexa-, and heptamethylenedithiocarbamates, N,N-diethyldithiocarbamate, N-methyl-N-propyldithiocarbamate, N-ethyl-N-propyldithiocarbamate, and N-methyl-N-butyldithiocarbamate have been explored. X-ray single-crystal diffraction allowed unambiguous structural characterization of all compounds except N-methyl-N-butyldithiocarbamate, which is obtained as a glassy material only. In addition, powder X-ray diffraction as well as vibrational and UV/Vis spectroscopy, supported by computational methods, were used to characterize the products. Differential scanning calorimetry was employed to investigate the phase-transition behavior depending on the N,N-dialkyldithiocarbamato ligand with the aim to establish structure-property relationships regarding the ionic liquid formation capability. Compounds with the least symmetric N,N-dialkyldithiocarbamato ligand and hence the least symmetric anions, tris(N-methyl-N-propyldithiocarbamato)uranylate, tris(N-ethyl-N-propyldithiocarbamato)uranylate, and tris(N-methyl-N-butyldithiocarbamato)uranylate, lead to the formation of (room-temperature) ionic liquids, which confirms that low-symmetry ions are indeed suitable to suppress crystallization. These materials combine low melting points, stable complex formation, and hydrophobicity and are therefore excellent candidates for nuclear fuel purification and recovery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A roadmap to uranium ionic liquids: Anti-crystal engineering

DOE PAGES

Yaprak, Damla; Spielberg, Eike T.; Bäcker, Tobias; ...

2014-04-15

In the search for uranium-based ionic liquids, tris(N,N-dialkyldithiocarbamato)uranylates have been synthesized as salts of the 1-butyl-3-methylimidazolium (C 4mim) cation. As dithiocarbamate ligands binding to the UO 2 2+ unit, tetra-, penta-, hexa-, and heptamethylenedithiocarbamates, N,N-diethyldithiocarbamate, N-methyl-N-propyldithiocarbamate, N-ethyl-N-propyldithiocarbamate, and N-methyl-N-butyldithiocarbamate have been explored. X-ray single-crystal diffraction allowed unambiguous structural characterization of all compounds except N-methyl-N-butyldithiocarbamate, which is obtained as a glassy material only. In addition, powder X-ray diffraction as well as vibrational and UV/Vis spectroscopy, supported by computational methods, were used to characterize the products. Differential scanning calorimetry was employed to investigate the phase-transition behavior depending on the N,N-dialkyldithiocarbamato ligand withmore » the aim to establish structure–property relationships regarding the ionic liquid formation capability. Compounds with the least symmetric N,N-dialkyldithiocarbamato ligand and hence the least symmetric anions, tris(N-methyl-N-propyldithiocarbamato)uranylate, tris(N-ethyl-N-propyldithiocarbamato)uranylate, and tris(N-methyl-N-butyldithiocarbamato)uranylate, lead to the formation of (room-temperature) ionic liquids, which confirms that low-symmetry ions are indeed suitable to suppress crystallization. As a result, these materials combine low melting points, stable complex formation, and hydrophobicity and are therefore excellent candidates for nuclear fuel purification and recovery.« less

In-line FINCH super resolution digital holographic fluorescence microscopy using a high efficiency transmission liquid crystal GRIN lens.

PubMed

Brooker, Gary; Siegel, Nisan; Rosen, Joseph; Hashimoto, Nobuyuki; Kurihara, Makoto; Tanabe, Ayano

2013-12-15

We report a new optical arrangement that creates high-efficiency, high-quality Fresnel incoherent correlation holography (FINCH) holograms using polarization sensitive transmission liquid crystal gradient index (TLCGRIN) diffractive lenses. In contrast, current universal practice in the field employs a reflective spatial light modulator (SLM) to separate sample and reference beams. Polarization sensitive TLCGRIN lenses enable a straight optical path, have >90% transmission efficiency, are not pixilated, and are free of many limitations of reflective SLM devices. For each sample point, two spherical beams created by a glass lens in combination with a polarization sensitive TLCGRIN lens interfere and create a hologram and resultant super resolution image.

Polyethylene nano crystalsomes formed at a curved liquid/liquid interface.

PubMed

Wang, Wenda; Staub, Mark C; Zhou, Tian; Smith, Derrick M; Qi, Hao; Laird, Eric D; Cheng, Shan; Li, Christopher Y

2017-12-21

Crystallization is incommensurate with nanoscale curved space due to the lack of three dimensional translational symmetry of the latter. Herein, we report the formation of single-crystal-like, nanosized polyethylene (PE) capsules using a miniemulsion solution crystallization method. The miniemulsion was formed at elevated temperatures using PE organic solution as the oil phase and sodium dodecyl sulfate as the surfactant. Subsequently, cooling the system stepwisely for controlled crystallization led to the formation of hollow, nanosized PE crystalline capsules, which are named as crystalsomes since they mimic the classical self-assembled structures such as liposome, polymersome and colloidosome. We show that the formation of the nanosized PE crystalsomes is driven by controlled crystallization at the curved liquid/liquid interface of the miniemulson droplet. The morphology, structure and mechanical properties of the PE crystalsomes were characterized using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and atomic force spectroscopy. Electron diffraction showed the single-crystal-like nature of the crystalsomes. The incommensurateness between the nanocurved interface and the crystalline packing led to reduced crystallinity and crystallite size of the PE crystalsome, as observed from the X-ray diffraction measurements. Moreover, directly quenching the emulsion below the spinodal line led to the formation of hierarchical porous PE crystalsomes due to the coupling of the PE crystallization and liquid/liquid phase separation. We anticipate that this unique crystalsome represents a new type of nanostructure that might be used as nanodrug carriers and ultrasound contrast agents.

Gelator-doped liquid-crystal phase grating with multistable and dynamic modes

NASA Astrophysics Data System (ADS)

Lin, Hui-Chi; Yang, Meng-Ru; Tsai, Sheng-Feng; Yan, Shih-Chiang

2014-01-01

We demonstrate a gelator-doped nematic liquid-crystal (LC) phase grating, which can be operated in both the multistable mode and the dynamic mode. Thermoreversible association and dissociation of the gelator molecules can vary and fix the multistable diffraction efficiencies of the gratings. A voltage (V) can also be applied to modulate dynamically the diffraction efficiencies of the grating, which behaves as a conventional LC grating. Experimental results show that the variations of the diffraction efficiencies in the multistable and dynamic modes are similar. The maximum diffraction efficiency is approximately 30% at V = 2 V.

Gelator-doped liquid-crystal phase grating with multistable and dynamic modes

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

Lin, Hui-Chi, E-mail: huichilin@nfu.edu.tw; Yang, Meng-Ru; Tsai, Sheng-Feng

2014-01-06

We demonstrate a gelator-doped nematic liquid-crystal (LC) phase grating, which can be operated in both the multistable mode and the dynamic mode. Thermoreversible association and dissociation of the gelator molecules can vary and fix the multistable diffraction efficiencies of the gratings. A voltage (V) can also be applied to modulate dynamically the diffraction efficiencies of the grating, which behaves as a conventional LC grating. Experimental results show that the variations of the diffraction efficiencies in the multistable and dynamic modes are similar. The maximum diffraction efficiency is approximately 30% at V = 2 V.

Ultra-fast switching blue phase liquid crystals diffraction grating stabilized by chiral monomer

NASA Astrophysics Data System (ADS)

Manda, Ramesh; Pagidi, Srinivas; Sarathi Bhattacharya, Surjya; Yoo, Hyesun; T, Arun Kumar; Lim, Young Jin; Lee, Seung Hee

2018-05-01

We have demonstrated an ultra-fast switching and efficient polymer stabilized blue phase liquid crystal (PS-BPLC) diffraction grating utilizing a chiral monomer. We have obtained a 0.5 ms response time by a novel polymer stabilization method which is three times faster than conventional PS-BPLC. In addition, the diffraction efficiency was improved 2% with a much wider phase range and the driving voltage to switch the device is reduced. The polarization properties of the diffracted beam are unaffected by this novel polymer stabilization. This device can be useful for future photonic applications.

Crystallisation of alpha-crustacyanin, the lobster carapace astaxanthin-protein: results from EURECA

NASA Astrophysics Data System (ADS)

Zagalsky, P. F.; Wright, C. E.; Parsons, M.

1995-08-01

Crystallisation of alpha-crustacyanin, the lobster carapace astaxanthin-protein was attempted under microgravity conditions in EURECA satellite using liquid-liquid diffusion with polyethyleneglycol (PEG) as precipitant; in a second reaction chamber phenol and dioxan were used as additives to prevent composite crystal growth. Crystals of alpha-crustacyanin grown under microgravity from PEG were larger than those grown terrestrially in the same apparatus under otherwise identical conditions. On retrieval, the crystals from PEG were shown to be composite and gave a powder diffraction pattern. The second reaction chamber showed leakage on retrieval and had also been subjected to rapid temperature variation during flight. Crystal fragments were nevertheless recovered but showed a powder diffraction pattern. It is concluded, certainly for liquid-liquid diffusion using PEG alone, that, for crustacyanin, although microgravity conditions resulted in an increase in dimensions of crystals, a measurable improvement in molecular ordering was not achieved.

Phase-Shifting Liquid Crystal Interferometers for Microgravity Fluid Physics

NASA Technical Reports Server (NTRS)

Griffin, DeVon W.; Marshall, Keneth L.

2002-01-01

The initial focus of this project was to eliminate both of these problems in the Liquid Crystal Point-Diffraction Interferometer (LCPDI). Progress toward that goal will be described, along with the demonstration of a phase shifting Liquid Crystal Shearing Interferometer (LCSI) that was developed as part of this work. The latest LCPDI, other than a lens to focus the light from a test section onto a diffracting microsphere within the interferometer and a collimated laser for illumination, the pink region contained within the glass plates on the rod-mounted platform is the complete interferometer. The total width is approximately 1.5 inches with 0.25 inches on each side for bonding the electrical leads. It is 1 inch high and there are only four diffracting microspheres within the interferometer. As a result, it is very easy to align, achieving the first goal. The liquid crystal electro-optical response time is a function of layer thickness, with thinner devices switching faster due to a reduction in long-range viscoelastic forces between the LC molecules. The LCPDI has a liquid crystal layer thickness of 10 microns, which is controlled by plastic or glass microspheres embedded in epoxy 'pads' at the corners of the device. The diffracting spheres are composed of polystyrene/divinyl benzene polymer with an initial diameter of 15 microns. The spheres deform slightly when the interferometer is assembled to conform to the spacing produced by the microsphere-filled epoxy spacer pads. While the speed of this interferometer has not yet been tested, previous LCPDIs fabricated at the Laboratory for Laser Energetics switched at a rate of approximately 3.3 Hz, a factor of 10 slower than desired. We anticipate better performance when the speed of these interferometers is tested since they are approximately three times thinner. Phase shifting in these devices is a function of the AC voltage level applied to the liquid crystal. As the voltage increases, the dye in the liquid crystal tends to become more transparent, thus introducing a rather large amount of error into the phase-shifting measurement. While that error can be greatly reduced by normalization, we prefer eliminating the source of the error. To that end, we have pursued development of a 'blend' of custom dyes that will not exhibit these properties. That goal has not yet been fully achieved. Guardalben, et al, presented a similar set of interferograms in a paper partially funded by this grant. Shearing interferometers are a second class of common path interferometers. Typically they consist of a thick glass plate optimized for equal reflection from the front and back surface. While not part of the original thrust of the project, through the course of laboratory work, we demonstrated a prototype of a shearing interferometer capable of phase shifting using a commercial liquid crystal retardation plate. A schematic of this liquid crystal shearing interferometer (LCSI) and a sample set of interferograms are in the reference. This work was also supported by the U.S. Department of Energy Office of Inertial Confinement Fusion under Cooperative Agreement No. DE-FC03-92SF19460, the University of Rochester, and the New York State Energy Research and Development Authority. The support of DOE does not constitute an endorsement by DOE of the views expressed in this article. Additional information is included in the original extended abstract.

Real-time observation of the isothermal crystallization kinetics in a deeply supercooled liquid

NASA Astrophysics Data System (ADS)

Zanatta, M.; Cormier, L.; Hennet, L.; Petrillo, C.; Sacchetti, F.

2017-03-01

Below the melting temperature Tm, crystals are the stable phase of typical elemental or molecular systems. However, cooling down a liquid below Tm, crystallization is anything but inevitable. The liquid can be supercooled, eventually forming a glass below the glass transition temperature Tg. Despite their long lifetimes and the presence of strong barriers that produces an apparent stability, supercooled liquids and glasses remain intrinsically a metastable state and thermodynamically unstable towards the crystal. Here we investigated the isothermal crystallization kinetics of the prototypical strong glassformer GeO2 in the deep supercooled liquid at 1100 K, about half-way between Tm and Tg. The crystallization process has been observed through time-resolved neutron diffraction for about three days. Data show a continuous reorganization of the amorphous structure towards the alpha-quartz phase with the final material composed by crystalline domains plunged into a low-density, residual amorphous matrix. A quantitative analysis of the diffraction patterns allows determining the time evolution of the relative fractions of crystal and amorphous, that was interpreted through an empirical model for the crystallization kinetics. This approach provides a very good description of the experimental data and identifies a predator-prey-like mechanism between crystal and amorphous, where the density variation acts as a blocking barrier.

Controllable light diffraction in woodpile photonic crystals filled with liquid crystal

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

Ho, Chih-Hua; Zeng, Hao; Wiersma, Diederik S.

2015-01-12

An approach to switching between different patterns of light beams transmitted through the woodpile photonic crystals filled with liquid crystals is proposed. The phase transition between the nematic and isotropic liquid crystal states leads to an observable variation of the spatial pattern transmitted through the photonic structure. The transmission profiles in the nematic phase also show polarization sensibility due to refractive index dependence on the field polarization. The experimental results are consistent with a numerical calculation by Finite Difference Time Domain method.

Analysis of holographic polymer-dispersed liquid crystals (HPDLCs) for tunable low frequency diffractive optical elements recording

NASA Astrophysics Data System (ADS)

Fernández, R.; Gallego, S.; Márquez, A.; Francés, J.; Martínez, F. J.; Pascual, I.; Beléndez, A.

2018-02-01

Holographic polymer dispersed liquid crystals (HPDLCs) are the result of the optimization of the photopolymer fabrication techniques. They are made by recording in a photopolymerization induced phase separation process (PIPS) in which the liquid crystal molecules diffuse to dark zones in the diffraction grating originated. Thanks to the addition of liquid crystal molecules to the composition, this material has a dynamic behavior by reorientation of the liquid crystal molecules applying an electrical field. In this sense, it is possible to use this material to make dynamic devices. In this work, we study the behavior of this material working in low frequencies with different spatial periods of blazed gratings, a sharp profile whose recording is possible thanks to the addition of a Holoeye LCoS-Pluto spatial light modulator with a resolution of 1920 × 1080 pixels (HD) and a pixel size of 8 × 8 μm2. This device allows us to have an accurate and dynamic control of the phase and amplitude of the recording beam.

The collection of MicroED data for macromolecular crystallography.

PubMed

Shi, Dan; Nannenga, Brent L; de la Cruz, M Jason; Liu, Jinyang; Sawtelle, Steven; Calero, Guillermo; Reyes, Francis E; Hattne, Johan; Gonen, Tamir

2016-05-01

The formation of large, well-ordered crystals for crystallographic experiments remains a crucial bottleneck to the structural understanding of many important biological systems. To help alleviate this problem in crystallography, we have developed the MicroED method for the collection of electron diffraction data from 3D microcrystals and nanocrystals of radiation-sensitive biological material. In this approach, liquid solutions containing protein microcrystals are deposited on carbon-coated electron microscopy grids and are vitrified by plunging them into liquid ethane. MicroED data are collected for each selected crystal using cryo-electron microscopy, in which the crystal is diffracted using very few electrons as the stage is continuously rotated. This protocol gives advice on how to identify microcrystals by light microscopy or by negative-stain electron microscopy in samples obtained from standard protein crystallization experiments. The protocol also includes information about custom-designed equipment for controlling crystal rotation and software for recording experimental parameters in diffraction image metadata. Identifying microcrystals, preparing samples and setting up the microscope for diffraction data collection take approximately half an hour for each step. Screening microcrystals for quality diffraction takes roughly an hour, and the collection of a single data set is ∼10 min in duration. Complete data sets and resulting high-resolution structures can be obtained from a single crystal or by merging data from multiple crystals.

The Influence of Surface Morphology and Diffraction Resolution of Canavalin Crystals

NASA Technical Reports Server (NTRS)

Plomp, M.; Thomas, B. R.; Day, J. S.; McPherson, A.; Chernov, A. A.; Malkin, A.

2003-01-01

Canavalin crystals grown from material purified and not purified by High Performance Liquid Chromatography were studied by atomic force microscopy and x-ray diffraction. After purification, resolution was improved from 2.55Angstroms to 2.22Angstroms and jagged isotropic spiral steps transformed into regular, well polygonized steps.

Polymer stabilized liquid crystals: Topology-mediated electro-optical behavior and applications

NASA Astrophysics Data System (ADS)

Weng, Libo

There has been a wide range of liquid crystal polymer composites that vary in polymer concentration from as little as 3 wt.% (polymer stabilized liquid crystal) to as high as 60 wt.% (polymer dispersed liquid crystals). In this dissertation, an approach of surface polymerization based on a low reactive monomer concentration about 1 wt.% is studied in various liquid crystal operation modes. The first part of dissertation describes the development of a vertical alignment (VA) mode with surface polymer stabilization, and the effects of structure-performance relationship of reactive monomers (RMs) and polymerization conditions on the electro-optical behaviors of the liquid crystal device has been explored. The polymer topography plays an important role in modifying and enhancing the electro-optical performance of stabilized liquid crystal alignment. The enabling surface-pinned polymer stabilized vertical alignment (PSVA) approach has led to the development of high-performance and fast-switching displays with controllable pretilt angle, increase in surface anchoring energy, high optical contrast and fast response time. The second part of the dissertation explores a PSVA mode with in-plane switching (IPS) and its application for high-efficiency and fast-switching phase gratings. The diffraction patterns and the electro-optical behaviors including diffraction efficiency and response time are characterized. The diffraction grating mechanism and performance have been validated by computer simulation. Finally, the advantages of surface polymerization approach such as good optical contrast and fast response time have been applied to the fringe-field switching (FFS) system. The concentration of reactive monomer on the electro-optical behavior of the FFS cells is optimized. The outstanding electro-optical results and mechanism of increase in surface anchoring strength are corroborated by the director field simulation. The density and topology of nanoscale polymer protrusions are analyzed and confirmed by morphological study. The developed high-performance polymer-stabilized fringe-field-switching (PS-FFS) could open new types of device applications.

Angular selectivity asymmetry of holograms recorded in near infrared sensitive liquid crystal photopolymerizable materials

NASA Astrophysics Data System (ADS)

Harbour, Steven; Galstian, Tigran; Akopyan, Rafik; Galstyan, Artur

2004-08-01

We have experimentally observed and theoretically explained the angular selectivity asymmetry in polymer dispersed liquid crystal holograms. Experiments are conducted in compounds with near infrared sensitivity. The coupled-wave theory is used to describe the diffraction properties of obtained anisotropic holographic gratings. Furthermore, the comparison of theory and experiments provides information about the optical axis direction that is defined by the average molecular orientation of the liquid crystal in the polymer matrix.

Electric-field responsive contrast agent based on liquid crystals and magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Mair, Lamar O.; Martinez-Miranda, Luz J.; Kurihara, Lynn K.; Nacev, Aleksandar; Hilaman, Ryan; Chowdhury, Sagar; Jafari, Sahar; Ijanaten, Said; da Silva, Claudian; Baker-McKee, James; Stepanov, Pavel Y.; Weinberg, Irving N.

2018-05-01

The properties of liquid crystal-magnetic nanoparticle composites have potential for sensing in the body. We study the response of a liquid crystal-magnetic nanoparticle (LC-MNP) composite to applied potentials of hundreds of volts per meter. Measuring samples using X-ray diffraction (XRD) and imaging composites using magnetic resonance imaging (MRI), we demonstrate that electric potentials applied across centimeter scale LC-MNP composite samples can be detected using XRD and MRI techniques.

Switchable electro-optic diffractive lens with high efficiency for ophthalmic applications

PubMed Central

Li, Guoqiang; Mathine, David L.; Valley, Pouria; Äyräs, Pekka; Haddock, Joshua N.; Giridhar, M. S.; Williby, Gregory; Schwiegerling, Jim; Meredith, Gerald R.; Kippelen, Bernard; Honkanen, Seppo; Peyghambarian, Nasser

2006-01-01

Presbyopia is an age-related loss of accommodation of the human eye that manifests itself as inability to shift focus from distant to near objects. Assuming no refractive error, presbyopes have clear vision of distant objects; they require reading glasses for viewing near objects. Area-divided bifocal lenses are one example of a treatment for this problem. However, the field of view is limited in such eyeglasses, requiring the user to gaze down to accomplish near-vision tasks and in some cases causing dizziness and discomfort. Here, we report on previously undescribed switchable, flat, liquid-crystal diffractive lenses that can adaptively change their focusing power. The operation of these spectacle lenses is based on electrical control of the refractive index of a 5-μm-thick layer of nematic liquid crystal using a circular array of photolithographically defined transparent electrodes. It operates with high transmission, low voltage (<2 Vrms), fast response (<1 sec), diffraction efficiency > 90%, small aberrations, and a power-failure-safe configuration. These results represent significant advance in state-of-the-art liquid-crystal diffractive lenses for vision care and other applications. They have the potential of revolutionizing the field of presbyopia correction when combined with automatic adjustable focusing power. PMID:16597675

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.

Birefringence Bragg Binary (3B) grating, quasi-Bragg grating and immersion gratings

NASA Astrophysics Data System (ADS)

Ebizuka, Noboru; Morita, Shin-ya; Yamagata, Yutaka; Sasaki, Minoru; Bianco, Andorea; Tanabe, Ayano; Hashimoto, Nobuyuki; Hirahara, Yasuhiro; Aoki, Wako

2014-07-01

A volume phase holographic (VPH) grating achieves high angular dispersion and very high diffraction efficiency for the first diffraction order and for S or P polarization. However the VPH grating could not achieve high diffraction efficiency for non-polarized light at a large diffraction angle because properties of diffraction efficiencies for S and P polarizations are different. Furthermore diffraction efficiency of the VPH grating extinguishes toward a higher diffraction order. A birefringence binary Bragg (3B) grating is a thick transmission grating with optically anisotropic material such as lithium niobate or liquid crystal. The 3B grating achieves diffraction efficiency up to 100% for non-polarized light by tuning of refractive indices for S and P polarizations, even in higher diffraction orders. We fabricated 3B grating with liquid crystal and evaluated the performance of the liquid crystal grating. A quasi-Bragg (QB) grating, which consists long rectangle mirrors aligned in parallel precisely such as a window shade, also achieves high diffraction efficiency toward higher orders. We fabricated QB grating by laminating of silica glass substrates and glued by pressure fusion of gold films. A quasi-Bragg immersion (QBI) grating has smooth mirror hypotenuse and reflector array inside the hypotenuse, instead of step-like grooves of a conventional immersion grating. An incident beam of the QBI grating reflects obliquely at a reflector, then reflects vertically at the mirror surface and reflects again at the same reflector. We are going to fabricate QBI gratings by laminating of mirror plates as similar to fabrication of the QB grating. We will also fabricate silicon and germanium immersion gratings with conventional step-like grooves by means of the latest diamond machining methods. We introduce characteristics and performance of these gratings.

Structural and conformational properties of 1-decyl-3-methylimidazolium tetrafluoroborate under high pressure

NASA Astrophysics Data System (ADS)

Chen, Liucheng; Li, Haining; Zhu, Xiang; Su, Lei; Yang, Kun; Yuan, Chaosheng; Yang, Guoqiang; Li, Xiaodong

2017-06-01

In situ crystalization of 1-decyl-3-methylimidazolium tetrafluoroborate ([C10MIM][BF4]) from melt has been investigated under high pressure up to 3.4 GPa at room temperature by using Raman spectroscopy and synchrotron X-ray diffraction measurement. Raman spectral analysis indicated that [C10MIM][BF4] experienced two successive phase transitions at about 0.3 GPa and 1.6 GPa. And the polymorphism was also discussed in view of the conformational isomerism of [C10MIM]+ cation between gauche and trans conformers. Notably, liquid-crystal and crystal-crystal phase transitions were further confirmed by synchrotron X-ray diffraction measurement. Moreover, it also indicated that high structural flexibility of the cations with long alkyl chain might have effect on the degree of disorder of pressure-induced crystallization for ionic liquids.

Discovery of a metastable Al20Sm4 phase

NASA Astrophysics Data System (ADS)

Ye, Z.; Zhang, F.; Sun, Y.; Mendelev, M. I.; Ott, R. T.; Park, E.; Besser, M. F.; Kramer, M. J.; Ding, Z.; Wang, C.-Z.; Ho, K.-M.

2015-03-01

We present an efficient genetic algorithm, integrated with experimental diffraction data, to solve a nanoscale metastable Al20Sm4 phase that evolves during crystallization of an amorphous magnetron sputtered Al90Sm10 alloy. The excellent match between calculated and experimental X-ray diffraction patterns confirms an accurate description of this metastable phase. Molecular dynamic simulations of crystal growth from the liquid phase predict the formation of disordered defects in the devitrified crystal.

2D-crystallization of Rhodococcus 20S proteasome at the liquid-liquid interface

NASA Astrophysics Data System (ADS)

Aoyama, Kazuhiro

1996-10-01

The 2D-crystallization method using the liquid-liquid interface between a aqueous phase (protein solution) and a thin organic liquid (dehydroabietylamine) layer has been applied to the Rhodococcus 20S proteasome. The 20S proteasome is known to be the core complex of the 26S proteasome, which is the central protease of the ubiquitin-dependent pathway. Two types of ordered arrays were obtained, both large enough for high resolution analysis by electron crystallography. The first one had a four-fold symmetry, whereas the second one was found out to be a hexagonally close-packed array. By image analysis based on a real space correlation averaging (CAV) technique, the close-packed array was found to be hexagonally packed, but the molecules had presumably rotational freedom. The four-fold array was found to be a true crystal with p4 symmetry. Lattice constants were a = b = 20.0 nm and α = 90°. The unit cell of this crystal contained two molecules. The diffraction pattern computed from the original picture showed spots up to (4, 5) that corresponds to 3.1 nm resolution. After applying an unbending procedure, the diffraction pattern showed spots extending to 1.8 nm resolution.

Quantitative performance of a polarization diffraction grating polarimeter encoded onto two liquid-crystal-on-silicon displays

NASA Astrophysics Data System (ADS)

Cofré, Aarón; Vargas, Asticio; Torres-Ruiz, Fabián A.; Campos, Juan; Lizana, Angel; del Mar Sánchez-López, María; Moreno, Ignacio

2017-11-01

We present a quantitative analysis of the performance of a complete snapshot polarimeter based on a polarization diffraction grating (PDGr). The PDGr is generated in a common path polarization interferometer with a Z optical architecture that uses two liquid-crystal on silicon (LCoS) displays to imprint two different phase-only diffraction gratings onto two orthogonal linear states of polarization. As a result, we obtain a programmable PDGr capable to act as a simultaneous polarization state generator (PSG), yielding diffraction orders with different states of polarization. The same system is also shown to operate as a polarization state analyzer (PSA), therefore useful for the realization of a snapshot polarimeter. We analyze its performance using quantitative metrics such as the conditional number, and verify its reliability for the detection of states of polarization.

Experimental evidence of low-density liquid water upon rapid decompression

PubMed Central

Lin, Chuanlong; Smith, Jesse S.; Sinogeikin, Stanislav V.; Shen, Guoyin

2018-01-01

Water is an extraordinary liquid, having a number of anomalous properties which become strongly enhanced in the supercooled region. Due to rapid crystallization of supercooled water, there exists a region that has been experimentally inaccessible for studying deeply supercooled bulk water. Using a rapid decompression technique integrated with in situ X-ray diffraction, we show that a high-pressure ice phase transforms to a low-density noncrystalline (LDN) form upon rapid release of pressure at temperatures of 140–165 K. The LDN subsequently crystallizes into ice-Ic through a diffusion-controlled process. Together with the change in crystallization rate with temperature, the experimental evidence indicates that the LDN is a low-density liquid (LDL). The measured X-ray diffraction data show that the LDL is tetrahedrally coordinated with the tetrahedral network fully developed and clearly linked to low-density amorphous ices. On the other hand, there is a distinct difference in structure between the LDL and supercooled water or liquid water in terms of the tetrahedral order parameter. PMID:29440411

Polar POLICRYPS diffractive structures generate cylindrical vector beams

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

Alj, Domenico; Caputo, Roberto, E-mail: roberto.caputo@fis.unical.it; Umeton, Cesare

2015-11-16

Local shaping of the polarization state of a light beam is appealing for a number of applications. This can be achieved by employing devices containing birefringent materials. In this article, we present one such enables converting a uniformly circularly polarized beam into a cylindrical vector beam (CVB). This device has been fabricated by exploiting the POLICRYPS (POlymer-LIquid CRYstals-Polymer-Slices) photocuring technique. It is a liquid-crystal-based optical diffraction grating featuring polar symmetry of the director alignment. We have characterized the resulting CVB profile and polarization for the cases of left and right circularly polarized incoming beams.

Evidence of monotropic hexatic tilted smectic phase in the phase sequence of ferroelectric liquid crystal

NASA Astrophysics Data System (ADS)

Różycka, Anna; Deptuch, Aleksandra; Jaworska-Gołąb, Teresa; Węgłowska, Dorota; Marzec, Monika

2018-02-01

Physical properties of a new ferroelectric liquid crystal have been studied by complementary methods: differential scanning calorimetry, polarizing optical microscopy, dielectric and X-ray diffraction. It was found that next to enantiotropic ferroelectric smectic C* phase, the monotropic smectic phase appears at cooling. X-ray diffraction measurements allowed to identify this phase as hexatic tilted smectic. Temperature dependence of spontaneous polarization, tilt angle of molecules and switching time were found in both liquid crystalline phases at cooling. Based on the dielectric results, the dielectric processes were identified as Goldstone mode in the smectic C* phase, whereas as the bond-orientation-like phason and the bulk domain mode in the monotropic hexatic tilted smectic phase.

Fast switchable ferroelectric liquid crystal gratings with two electro-optical modes

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

Ma, Ying; Srivastava, A. K., E-mail: abhishek-srivastava-lu@yahoo.co.in; Chigrinov, V. G.

In this article, we reveal a theoretical and experimental illustration of the Ferroelectric liquid crystal (FLC) grating fabricated by mean of patterned alignment based on photo-alignment. The complexity related to the mismatching of the predefined alignment domains on the top and bottom substrate has been avoided by incorporating only one side photo aligned substrate while the other substrate does not have any alignment layer. Depending on the easy axis in the said alignment domains and the azimuth plane of the impinging polarized light, the diffracting element can be tuned in two modes i.e. DIFF/OFF switchable and DIFF/TRANS switchable modes, whichmore » can be applied to different applications. The diffraction profile has been illustrated theoretically that fits well with the experimental finding and thus the proposed diffraction elements with fast response time and high diffraction efficiency could find application in many modern devices.« less

Electrically and spatially controllable PDLC phase gratings for diffraction and modulation of laser beams

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

Hadjichristov, Georgi B., E-mail: georgibh@issp.bas.bg; Marinov, Yordan G.; Petrov, Alexander G.

2016-03-25

We present a study on electrically- and spatially-controllable laser beam diffraction, electrooptic (EO) phase modulation, as well as amplitude-frequency EO modulation by single-layer microscale polymer-dispersed liquid crystal (PDLC) phase gratings (PDLC SLPGs) of interest for device applications. PDLC SLPGs were produced from nematic liquid crystal (LC) E7 in photo-curable NOA65 polymer. The wedge-formed PDLC SLPGs have a continuously variable thickness (2–25 µm). They contain LC droplets of diameters twice as the layer thickness, with a linear-gradient size distribution along the wedge. By applying alternating-current (AC) electric field, the PDLC SLPGs produce efficient: (i) diffraction splitting of transmitted laser beams; (ii)more » spatial redistribution of diffracted light intensity; (iii) optical phase modulation; (iv) amplitude-frequency modulation, all controllable by the driven AC field and the droplet size gradient.« less

Design considerations for a backlight with switchable viewing angles

NASA Astrophysics Data System (ADS)

Fujieda, Ichiro; Takagi, Yoshihiko; Rahadian, Fanny

2006-08-01

Small-sized liquid crystal displays are widely used for mobile applications such as cell phones. Electronic control of a viewing angle range is desired in order to maintain privacy for viewing in public as well as to provide wide viewing angles for solitary viewing. Conventionally, a polymer-dispersed liquid crystal (PDLC) panel is inserted between a backlight and a liquid crystal panel. The PDLC layer either transmits or scatters the light from the backlight, thus providing an electronic control of viewing angles. However, such a display system is obviously thick and expensive. Here, we propose to place an electronically-controlled, light-deflecting device between an LED and a light-guide of a backlight. For example, a liquid crystal lens is investigated for other applications and its focal length is controlled electronically. A liquid crystal phase grating either transmits or diffracts an incoming light depending on whether or not a periodic phase distribution is formed inside its liquid crystal layer. A bias applied to such a device will control the angular distribution of the light propagating inside a light-guide. Output couplers built in the light-guide extract the propagating light to outside. They can be V-shaped grooves, pyramids, or any other structures that can refract, reflect or diffract light. When any of such interactions occur, the output couplers translate the changes in the propagation angles into the angular distribution of the output light. Hence the viewing-angle characteristic can be switched. The designs of the output couplers and the LC devices are important for such a backlight system.

Color changing plasmonic surfaces utilizing liquid crystal (Conference Presentation)

NASA Astrophysics Data System (ADS)

Franklin, Daniel; Wu, Shin-Tson; Chanda, Debashis

2016-09-01

Plasmonic structural color has recently garnered significant interest as an alternative to the organic dyes standard in print media and liquid crystal displays. These nanostructured metallic systems can produce diffraction limited images, be made polarization dependent, and exhibit resistance to color bleaching. Perhaps even more advantageous, their optical characteristics can also be tuned, post-fabrication, by altering the surrounding media's refractive index parallel to the local plasmonic fields. A common material with which to achieve this is liquid crystal. By reorienting the liquid crystal molecules through external electric fields, the optical resonances of the plasmonic filters can be dynamically controlled. Demonstrations of this phenomenon, however, have been limited to modest shifts in plasmon resonance. Here, we report a liquid crystal-plasmonic system with an enhanced tuning range through the use of a shallow array of nano-wells and high birefringent liquid crystal. The continuous metallic nanostructure maximizes the overlap between plasmonic fields and liquid crystal while also allowing full reorientation of the liquid crystal upon an applied electric field. Sweeping over structural dimensions and voltages results in a color palette for these dynamic reflective pixels that can further be exploited to create color tunable images. These advances make plasmonic-liquid crystal systems more attractive candidates for filter, display, and other tunable optical technologies.

Programmable diffractive lens for ophthalmic application

NASA Astrophysics Data System (ADS)

Millán, María S.; Pérez-Cabré, Elisabet; Romero, Lenny A.; Ramírez, Natalia

2014-06-01

Pixelated liquid crystal displays have been widely used as spatial light modulators to implement programmable diffractive optical elements, particularly diffractive lenses. Many different applications of such components have been developed in information optics and optical processors that take advantage of their properties of great flexibility, easy and fast refreshment, and multiplexing capability in comparison with equivalent conventional refractive lenses. We explore the application of programmable diffractive lenses displayed on the pixelated screen of a liquid crystal on silicon spatial light modulator to ophthalmic optics. In particular, we consider the use of programmable diffractive lenses for the visual compensation of refractive errors (myopia, hypermetropia, astigmatism) and presbyopia. The principles of compensation are described and sketched using geometrical optics and paraxial ray tracing. For the proof of concept, a series of experiments with artificial eye in optical bench are conducted. We analyze the compensation precision in terms of optical power and compare the results with those obtained by means of conventional ophthalmic lenses. Practical considerations oriented to feasible applications are provided.

Ophthalmic compensation of visual ametropia based on a programmable diffractive lens

NASA Astrophysics Data System (ADS)

Millán, Maria S.; Pérez-Cabré, Elisabet; Romero, Lenny A.; Ramírez, Natalia

2013-11-01

Pixelated liquid crystal displays have been widely used as spatial light modulators to implement programmable diffractive optical elements (DOEs), particularly diffractive lenses. Many different applications of such components have been developed in information optics and optical processors that take advantage of their properties of great flexibility, easy and fast refreshment, and multiplexing capability in comparison with equivalent conventional refractive lenses. In this paper, we explore the application of programmable diffractive lenses displayed on the pixelated screen of a liquid crystal on silicon spatial light modulator (LCoS-SLM) to ophthalmic optics. In particular, we consider the use of programmable diffractive lenses for the visual compensation of some refractive errors (myopia, hyperopia). The theoretical principles of compensation are described and sketched using geometrical optics and paraxial ray tracing. A series of experiments with artificial eye in optical bench are conducted to analyze the compensation accuracy in terms of optical power and to compare the results with those obtained by means of conventional ophthalmic lenses. Practical considerations oriented to feasible applications are provided.

Ca-P spots modified zirconia by liquid precursor infiltration and the effect on osteoblast-like cell responses.

PubMed

Li, Yongmei; Liu, Yan; Zhang, Zutai; Zhuge, Ruishen; Ding, Ning; Tian, Yueming

2018-01-26

Ca-P spots modified zirconia by liquid precursor infiltration and the cell responses were investigated. Pre-sintered zirconia specimens were immersed in Ca-P precursor solution. After dense sintering, scanning electron microscopy showed Ca-P spots were formed on the zirconia and anchored with zirconia substrates. The distribution density was increased with the extension of immersion time. Energy dispersive spectrometer confirmed the stoichiometric Ca/P ratio was about 1.67. After hydrothermal treatment, Ca-P spots turned into rod crystals where diffraction peaks of tricalcium phosphate and hydroxyapatite were detected by X-ray diffraction, and Ca 2+ and PO 4 3- release decreased slightly (p>0.05). There was no significant decrease on three-point bending strength (p>0.05). Osteoblast-like MC3T3-E1 cells attached and spread well and showed higher proliferation on Ca-P spots modified zirconia (p<0.05), though its initial alkaline phosphatase activity was not significant high (p>0.05). In conclusion, Ca-P liquid precursor infiltration is a potential method to modify the zirconia ceramics for improving bioactivity.

Organic holographic polymer dispersed liquid crystal distributed feedback laser from different diffraction orders

NASA Astrophysics Data System (ADS)

Liu, Minghuan; Liu, Yonggang; Zhang, Guiyang; Peng, Zenghui; Li, Dayu; Ma, Ji; Xuan, Li

2016-11-01

Holographic polymer dispersed liquid crystal (HPDLC) based distributed feedback (DFB) lasers were prepared with poly (-methoxy-5-(2‧-ethyl-hexyloxy)-1,4-phenylene-vinylene) (MEH-PPV) film as the active medium layer. The HPDLC grating film was fabricated via holographic induced photopolymerization. The pure film spectra of MEH-PPV and the amplified spontaneous emission (ASE) spectrum were investigated. The laser device was single-longitudinal mode operation. The tunability of the HPDLC DFB laser was achieved by selecting different grating periods. The lasing performances were also characterized and compared from different diffraction orders. The lasing threshold increased with the diffraction order and the third order laser possessed the largest conversion efficiency in this device. The experimental results were in good agreement with the theoretical calculations.

Dynamic Self-Stiffening in Liquid Crystal Elastomers

PubMed Central

Agrawal, Aditya; Chipara, Alin C.; Shamoo, Yousif; Patra, Prabir K.; Carey, Brent J.; Ajayan, Pulickel M.; Chapman, Walter G.

2013-01-01

Biological tissues have the remarkable ability to remodel and repair in response to disease, injury, and mechanical stresses. Synthetic materials lack the complexity of biological tissues, and man-made materials which respond to external stresses through a permanent increase in stiffness are uncommon. Here, we report that polydomain nematic liquid crystal elastomers increase in stiffness by up to 90% when subjected to a low-amplitude (5%), repetitive (dynamic) compression. Elastomer stiffening is influenced by liquid crystal content, the presence of a nematic liquid crystal phase and the use of a dynamic as opposed to static deformation. Through rheological and X-ray diffraction measurements, stiffening can be attributed to a nematic director which rotates in response to dynamic compression. Stiffening under dynamic compression has not been previously observed in liquid crystal elastomers and may be useful for the development of self-healing materials or for the development of biocompatible, adaptive materials for tissue replacement. PMID:23612280

An Optically Isotropic Antiferroelectric Liquid Crystal (OI-AFLC) Display Mode Operating over a Wide Temperature Range using Ternary Bent-Core Liquid Crystal Mixtures

DOE PAGES

Bergquist, Leah; Zhang, Cuiyu; Ribeiro de Almeida, Roberta R.; ...

2017-02-07

Here, we report on the synthesis and characterization of bent-core liquid crystal (LC) compounds and the preparation of mixtures that provide an optically isotropic antiferroelectric (OI-AFLC) liquid crystal display mode over a very wide temperature interval and well below room temperature. From the collection of compounds synthesized during this study, we recognized that several ternary mixtures displayed a modulated SmC aP A phase down to below -40 °C and up to about 100 °C on both heating and cooling, as well as optical tilt angles in the transformed state of approximately 45° (optically isotropic state). The materials were fully characterizedmore » and their liquid crystal as well as electro-optical properties analyzed by polarized optical microscopy, differential scanning calorimetry, synchrotron X-ray diffraction, dielectric spectroscopy, and electro-optical tests.« less

An Optically Isotropic Antiferroelectric Liquid Crystal (OI-AFLC) Display Mode Operating over a Wide Temperature Range using Ternary Bent-Core Liquid Crystal Mixtures

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

Bergquist, Leah; Zhang, Cuiyu; Ribeiro de Almeida, Roberta R.

Here, we report on the synthesis and characterization of bent-core liquid crystal (LC) compounds and the preparation of mixtures that provide an optically isotropic antiferroelectric (OI-AFLC) liquid crystal display mode over a very wide temperature interval and well below room temperature. From the collection of compounds synthesized during this study, we recognized that several ternary mixtures displayed a modulated SmC aP A phase down to below -40 °C and up to about 100 °C on both heating and cooling, as well as optical tilt angles in the transformed state of approximately 45° (optically isotropic state). The materials were fully characterizedmore » and their liquid crystal as well as electro-optical properties analyzed by polarized optical microscopy, differential scanning calorimetry, synchrotron X-ray diffraction, dielectric spectroscopy, and electro-optical tests.« less

A simple method for evaluating the wavefront compensation error of diffractive liquid-crystal wavefront correctors.

PubMed

Cao, Zhaoliang; Mu, Quanquan; Hu, Lifa; Lu, Xinghai; Xuan, Li

2009-09-28

A simple method for evaluating the wavefront compensation error of diffractive liquid-crystal wavefront correctors (DLCWFCs) for atmospheric turbulence correction is reported. A simple formula which describes the relationship between pixel number, DLCWFC aperture, quantization level, and atmospheric coherence length was derived based on the calculated atmospheric turbulence wavefronts using Kolmogorov atmospheric turbulence theory. It was found that the pixel number across the DLCWFC aperture is a linear function of the telescope aperture and the quantization level, and it is an exponential function of the atmosphere coherence length. These results are useful for people using DLCWFCs in atmospheric turbulence correction for large-aperture telescopes.

Achromatic diffractive lens written onto a liquid crystal display.

PubMed

Márquez, A; Iemmi, C; Campos, J; Yzuel, M J

2006-02-01

We propose a programmable diffractive lens written onto a liquid crystal display (LCD) that is able to provide equal focal lengths for several wavelengths simultaneously. To achieve this goal it is necessary that the LCD operate in the phase-only regime simultaneously for the different wavelengths. We design the appropriate lens for each wavelength, and then the lenses are spatially multiplexed onto the LCD. Various multiplexing schemes have been analyzed, and the random scheme shows the best performance. We further show the possibility of finely tuning the chromaticity of the focal spot by changing the relative weights of the multiplexing among the various wavelengths.

A fast point-cloud computing method based on spatial symmetry of Fresnel field

NASA Astrophysics Data System (ADS)

Wang, Xiangxiang; Zhang, Kai; Shen, Chuan; Zhu, Wenliang; Wei, Sui

2017-10-01

Aiming at the great challenge for Computer Generated Hologram (CGH) duo to the production of high spatial-bandwidth product (SBP) is required in the real-time holographic video display systems. The paper is based on point-cloud method and it takes advantage of the propagating reversibility of Fresnel diffraction in the propagating direction and the fringe pattern of a point source, known as Gabor zone plate has spatial symmetry, so it can be used as a basis for fast calculation of diffraction field in CGH. A fast Fresnel CGH method based on the novel look-up table (N-LUT) method is proposed, the principle fringe patterns (PFPs) at the virtual plane is pre-calculated by the acceleration algorithm and be stored. Secondly, the Fresnel diffraction fringe pattern at dummy plane can be obtained. Finally, the Fresnel propagation from dummy plan to hologram plane. The simulation experiments and optical experiments based on Liquid Crystal On Silicon (LCOS) is setup to demonstrate the validity of the proposed method under the premise of ensuring the quality of 3D reconstruction the method proposed in the paper can be applied to shorten the computational time and improve computational efficiency.

Electrically tunable two-dimensional holographic polymer-dispersed liquid crystal grating with variable period

NASA Astrophysics Data System (ADS)

Wang, Kangni; Zheng, Jihong; Liu, Yourong; Gao, Hui; Zhuang, Songlin

2017-06-01

An electrically tunable two-dimensional (2D) holographic polymer-dispersed liquid crystal (H-PDLC) grating with variable period was fabricated by inserting a cylindrical lens in a conventional holographic interference beam. The interference between the plane wave and cylindrical wave resulting in varying intersection angles on the sample, combined with dual exposure along directions perpendicular to each other, generates a 2D H-PDLC grating with varied period. We have identified periods varying from 3.109 to 5.158 μm across a 16 mm width, with supporting theoretical equations for the period. The period exhibits a symmetrical square lattice in a diagonal direction, with an asymmetrical rectangular lattice in off-diagonal locations. With the first exposure at 2 s and the second exposure at 60 s, the phase separation between the prepolymer and liquid crystal was most evident. The diffraction properties and optic-electric characteristics were also studied. The diffraction efficiency of first-order light was observed to be 13.5% without external voltage, and the transmission efficiency of non-diffracted light was 78% with an applied voltage of 100 V. The proposed method provides the capability of generating period variation to the conventional holographic interference path, with potential application in diffractive optics such as tunable multi-wavelength organic lasing from a dye-doped 2D H-PDLC grating.

Molecular dynamics simulations of liquid silica crystallization.

PubMed

Niu, Haiyang; Piaggi, Pablo M; Invernizzi, Michele; Parrinello, Michele

2018-05-07

Silica is one of the most abundant minerals on Earth and is widely used in many fields. Investigating the crystallization of liquid silica by atomic simulations is of great importance to understand the crystallization mechanism; however, the high crystallization barrier and the tendency of silica to form glasses make such simulations very challenging. Here we have studied liquid silica crystallization to [Formula: see text]-cristobalite with metadynamics, using X-ray diffraction (XRD) peak intensities as collective variables. The frequent transitions between solid and liquid of the biased runs demonstrate the highly successful use of the XRD peak intensities as collective variables, which leads to the convergence of the free-energy surface. By calculating the difference in free energy, we have estimated the melting temperature of [Formula: see text]-cristobalite, which is in good agreement with the literature. The nucleation mechanism during the crystallization of liquid silica can be described by classical nucleation theory. Copyright © 2018 the Author(s). Published by PNAS.

Holographic Formation of Diffraction Elements for Transformation of Light Beams in Liquid Crystal - Photopolymer Compositions

NASA Astrophysics Data System (ADS)

Semkin, A. O.; Sharangovich, S. N.

2018-03-01

A theoretical model of holographic formation of diffractive optical elements for transformation of light beam field into Bessel-like fields in liquid crystal - photopolymer (LC-PPM) composite materials with a dyesensitizer is developed. Results of numerical modeling of kinetics ofvariation of the refractive index of a material in the process of formation with different relationships between the photopolymerization rates and diffusion processes are presented. Based on the results of numerical simulation, it is demonstrated that when the photopolarization process dominates, the diffractive element being formed is distorted. This leads to a change in the light field distribution at its output and consequently, to ineffective transformation of the reading beam. Thus, the necessity of optimizing of the recording conditions and of the prepolymeric composition to increase the transformation efficiency of light beam fields is demonstrated.

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids.

PubMed

Zipper, Lauren E; Aristide, Xavier; Bishop, Dylan P; Joshi, Ishita; Kharzeev, Julia; Patel, Krishna B; Santiago, Brianna M; Joshi, Karan; Dorsinvil, Kahille; Sweet, Robert M; Soares, Alexei S

2014-12-01

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under different conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63-82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. The results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.

Polymerization speed and diffractive experiments in polymer network LC test cells

NASA Astrophysics Data System (ADS)

Braun, Larissa; Gong, Zhen; Habibpourmoghadam, Atefeh; Schafforz, Samuel L.; Wolfram, Lukas; Lorenz, Alexander

2018-02-01

Polymer-network liquid crystals (LCs), where the response properties of a LC can be enhanced by the presence of a porous polymer network, are investigated. In the reported experiments, liquid crystals were doped with a small amount (< 10%) of photo-curable acrylate monomers. Samples with surface grafted photoinitiators, dissolvable photoinitiators, and samples with both kinds of photoinitiators were prepared. Both conventional (planar electrodes) and diffractive (interdigitated electrodes) test cells were used. These samples were exposed with a UV light source and changes of their capacitance were investigated with an LCR meter during exposure. Due to the presence of the in-situ generated polymer network, the electro-optic response properties of photo cured samples were enhanced. For example, their continuous phase modulation properties led to more localized responses in samples with interdigitated electrodes, which caused suppression of selected diffraction orders in the diffraction patterns recorded in polymer network LC samples. Moreover, capacitance changes were investigated during photopolymerization of a blue phase LC.

Blazed vector grating liquid crystal cells with photocrosslinkable polymeric alignment films fabricated by one-step polarizer rotation method

NASA Astrophysics Data System (ADS)

Kawai, Kotaro; Kuzuwata, Mitsuru; Sasaki, Tomoyuki; Noda, Kohei; Kawatsuki, Nobuhiro; Ono, Hiroshi

2014-12-01

Blazed vector grating liquid crystal (LC) cells, in which the directors of low-molar-mass LCs are antisymmetrically distributed, were fabricated by one-step exposure of an empty glass cell inner-coated with a photocrosslinkable polymer LC (PCLC) to UV light. By adopting a LC cell structure, twisted nematic (TN) and homogeneous (HOMO) alignments were obtained in the blazed vector grating LC cells. Moreover, the diffraction efficiency of the blazed vector grating LC cells was greatly improved by increasing the thickness of the device in comparison with that of a blazed vector grating with a thin film structure obtained in our previous study. In addition, the diffraction efficiency and polarization states of ±1st-order diffracted beams from the resultant blazed vector grating LC cells were controlled by designing a blazed pattern in the alignment films, and these diffraction properties were well explained on the basis of Jones calculus and the elastic continuum theory of nematic LCs.

Hidden Gratings in Holographic Liquid Crystal Polymer-Dispersed Liquid Crystal Films.

PubMed

De Sio, Luciano; Lloyd, Pamela F; Tabiryan, Nelson V; Bunning, Timothy J

2018-04-18

Dynamic diffraction gratings that are hidden in the field-off state are fabricated utilizing a room-temperature photocurable liquid crystal (LC) monomer and nematic LC (NLC) using holographic photopolymerization techniques. These holographic LC polymer-dispersed LCs (HLCPDLCs) are hidden because of the refractive index matching between the LC polymer and the NLC regions in the as-formed state (no E-field applied). Application of a moderate E-field (5 V/μm) generates a refractive index mismatch because of the NLC reorientation (along the E-field) generating high-diffraction efficiency transmission gratings. These dynamic gratings are characterized by morphological, optical, and electrooptical techniques. They exhibit a morphology made of oriented LC polymer regions (containing residual NLC) alternating with a two-phase region of an NLC and LC polymer. Unlike classic holographic polymer-dispersed LC gratings formed with a nonmesogenic monomer, there is index matching between the as-formed alternating regions of the grating. These HLCPDLCs exhibit broad band and high diffraction efficiency (≈90%) at the Bragg angle, are transparent to white light across the visible range because of the refractive index matching, and exhibit fast response times (1 ms). The ability of HLCPDLCs not to consume electrical power in the off state opens new possibilities for the realization of energy-efficient switchable photonic devices.

Wave-aberration control with a liquid crystal on silicon (LCOS) spatial phase modulator.

PubMed

Fernández, Enrique J; Prieto, Pedro M; Artal, Pablo

2009-06-22

Liquid crystal on Silicon (LCOS) spatial phase modulators offer enhanced possibilities for adaptive optics applications in terms of response velocity and fidelity. Unlike deformable mirrors, they present a capability for reproducing discontinuous phase profiles. This ability also allows an increase in the effective stroke of the device by means of phase wrapping. The latter is only limited by the diffraction related effects that become noticeable as the number of phase cycles increase. In this work we estimated the ranges of generation of the Zernike polynomials as a means for characterizing the performance of the device. Sets of images systematically degraded with the different Zernike polynomials generated using a LCOS phase modulator have been recorded and compared with their theoretical digital counterparts. For each Zernike mode, we have found that image degradation reaches a limit for a certain coefficient value; further increase in the aberration amount has no additional effect in image quality. This behavior is attributed to the intensification of the 0-order diffraction. These results have allowed determining the usable limits of the phase modulator virtually free from diffraction artifacts. The results are particularly important for visual simulation and ophthalmic testing applications, although they are equally interesting for any adaptive optics application with liquid crystal based devices.

Liquid-crystal science from 1888 to 1922: building a revolution.

PubMed

Mitov, Michel

2014-05-19

The saga of liquid crystals started with their discovery in 1888 by the botanist Friedrich Reinitzer, who unexpectedly observed "two melting points" for crystals extracted from the root of a carrot. At the end of the nineteenth century, most scientists did not believe in the existence of "liquid crystals" as promoted by the crystallographer Otto Lehmann. The controversies were very vivid; to the point that the recognition of mesomorphic states of matter by the scientific community required more than two decades. In the end, liquid crystals have changed our vision of matter by shattering the three-state paradigm. Since the mid-1970s, liquid crystals have revolutionized the worldwide information-display industry and now play a host of key roles in various technologies. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

About Small Streams and Shiny Rocks: Macromolecular Crystal Growth in Microfluidics

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark; Ferree, Darren; Spearing, Scott; Monaco, Lisa; Molho, Josh; Spaid, Michael; Brasseur, Mike; Curreri, Peter A. (Technical Monitor)

2002-01-01

We are developing a novel technique with which we have grown diffraction quality protein crystals in very small volumes, utilizing chip-based, microfluidic ("LabChip") technology. With this technology volumes smaller than achievable with any laboratory pipette can be dispensed with high accuracy. We have performed a feasibility study in which we crystallized several proteins with the aid of a LabChip device. The protein crystals are of excellent quality as shown by X-ray diffraction. The advantages of this new technology include improved accuracy of dispensing for small volumes, complete mixing of solution constituents without bubble formation, highly repeatable recipe and growth condition replication, and easy automation of the method. We have designed a first LabChip device specifically for protein crystallization in batch mode and can reliably dispense and mix from a range of solution constituents. We are currently testing this design. Upon completion additional crystallization techniques, such as vapor diffusion and liquid-liquid diffusion will be accommodated. Macromolecular crystallization using microfluidic technology is envisioned as a fully automated system, which will use the 'tele-science' concept of remote operation and will be developed into a research facility aboard the International Space Station.

Steady distribution structure of point defects near crystal-melt interface under pulling stop of CZ Si crystal

NASA Astrophysics Data System (ADS)

Abe, T.; Takahashi, T.; Shirai, K.

2017-02-01

In order to reveal a steady distribution structure of point defects of no growing Si on the solid-liquid interface, the crystals were grown at a high pulling rate, which Vs becomes predominant, and the pulling was suddenly stopped. After restoring the variations of the crystal by the pulling-stop, the crystals were then left in prolonged contact with the melt. Finally, the crystals were detached and rapidly cooled to freeze point defects and then a distribution of the point defects of the as-grown crystals was observed. As a result, a dislocation loop (DL) region, which is formed by the aggregation of interstitials (Is), was formed over the solid-liquid interface and was surrounded with a Vs-and-Is-free recombination region (Rc-region), although the entire crystals had been Vs rich in the beginning. It was also revealed that the crystal on the solid-liquid interface after the prolonged contact with the melt can partially have a Rc-region to be directly in contact with the melt, unlike a defect distribution of a solid-liquid interface that has been growing. This experimental result contradicts a hypothesis of Voronkov's diffusion model, which always assumes the equilibrium concentrations of Vs and Is as the boundary condition for distribution of point defects on the growth interface. The results were disscussed from a qualitative point of view of temperature distribution and thermal stress by the pulling-stop.

[Fine stereo structure for natural organic molecules, a preliminary study. II. Melting point influenced by structure factors].

PubMed

Lu, Y; Zheng, Q; Lu, D; Ma, P; Chen, Y

1995-06-01

Crystal structures of two compounds from Tripterygium wilfordii Hook f. have been determined by X-ray diffraction method. Structure factors influencing melting point of solid state have been analysed. Crystal class (or space group), recrystallization solvent, force between molecules and fine changes of molecular structures will all cause melting point changes of crystal substance.

Process for Encapsulating Protein Crystals

NASA Technical Reports Server (NTRS)

Morrison, Dennis R.; Mosier, Benjamin

2003-01-01

A process for growing protein crystals encapsulated within membranes has been invented. This process begins with the encapsulation of a nearly saturated aqueous protein solution inside semipermeable membranes to form microcapsules. The encapsulation is effected by use of special formulations of a dissolved protein and a surfactant in an aqueous first liquid phase, which is placed into contact with a second, immiscible liquid phase that contains one or more polymers that are insoluble in the first phase. The second phase becomes formed into the semipermeable membranes that surround microglobules of the first phase, thereby forming the microcapsules. Once formed, the microcapsules are then dehydrated osmotically by exposure to a concentrated salt or polymer solution. The dehydration forms supersaturated solutions inside the microcapsules, thereby enabling nucleation and growth of protein crystals inside the microcapsules. By suitable formulation of the polymer or salt solution and of other physical and chemical parameters, one can control the rate of transport of water out of the microcapsules through the membranes and thereby create physicochemical conditions that favor the growth, within each microcapsule, of one or a few large crystals suitable for analysis by x-ray diffraction. The membrane polymer can be formulated to consist of low-molecular-weight molecules that do not interfere with the x-ray diffraction analysis of the encapsulated crystals. During dehydration, an electrostatic field can be applied to exert additional control over the rate of dehydration. This protein-crystal-encapsulation process is expected to constitute the basis of protein-growth experiments to be performed on the space shuttle and the International Space Station. As envisioned, the experiments would involve the exposure of immiscible liquids to each other in sequences of steps under microgravitational conditions. The experiments are expected to contribute to knowledge of the precise conditions under which protein crystals form. By enhancing the ability to grow crystals suitable for x-ray diffraction analysis, this knowledge can be expected to benefit not only the space program but also medicine and the pharmaceutical industry.

Photo-Responsive Soft Ionic Crystals: Ion-Pairing Assemblies of Azobenzene Carboxylates.

PubMed

Yamakado, Ryohei; Hara, Mitsuo; Nagano, Shusaku; Seki, Takahiro; Maeda, Hiromitsu

2017-07-12

This report delineates the design and synthesis of negatively charged azobenzene derivatives that form photo-responsive ion-pairing assemblies. The azobenzene carboxylates possessing aliphatic chains were prepared as photo-responsive anions that promote the formation of ion-pairing dimension-controlled assemblies, including mesophases, when used in conjunction with a tetrabutylammonium (TBA) cation. The photo-responsive properties of the ion pairs and the precursory carboxylic acids in the bulk state were examined by polarized optical microscopy (POM) and X-ray diffraction (XRD), demonstrating that liquid crystal (LC)-liquid and crystal-liquid phase transitions occurred, depending on the number and lengths of the aliphatic chains of each assembly. An ion pair exhibited photo-induced crystal-crystal phase transitions upon switching between two irradiation wavelengths (365/436 nm). © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integrated crystal mounting and alignment system for high-throughput biological crystallography

DOEpatents

Nordmeyer, Robert A.; Snell, Gyorgy P.; Cornell, Earl W.; Kolbe, William F.; Yegian, Derek T.; Earnest, Thomas N.; Jaklevich, Joseph M.; Cork, Carl W.; Santarsiero, Bernard D.; Stevens, Raymond C.

2007-09-25

A method and apparatus for the transportation, remote and unattended mounting, and visual alignment and monitoring of protein crystals for synchrotron generated x-ray diffraction analysis. The protein samples are maintained at liquid nitrogen temperatures at all times: during shipment, before mounting, mounting, alignment, data acquisition and following removal. The samples must additionally be stably aligned to within a few microns at a point in space. The ability to accurately perform these tasks remotely and automatically leads to a significant increase in sample throughput and reliability for high-volume protein characterization efforts. Since the protein samples are placed in a shipping-compatible layered stack of sample cassettes each holding many samples, a large number of samples can be shipped in a single cryogenic shipping container.

Integrated crystal mounting and alignment system for high-throughput biological crystallography

DOEpatents

Nordmeyer, Robert A.; Snell, Gyorgy P.; Cornell, Earl W.; Kolbe, William; Yegian, Derek; Earnest, Thomas N.; Jaklevic, Joseph M.; Cork, Carl W.; Santarsiero, Bernard D.; Stevens, Raymond C.

2005-07-19

A method and apparatus for the transportation, remote and unattended mounting, and visual alignment and monitoring of protein crystals for synchrotron generated x-ray diffraction analysis. The protein samples are maintained at liquid nitrogen temperatures at all times: during shipment, before mounting, mounting, alignment, data acquisition and following removal. The samples must additionally be stably aligned to within a few microns at a point in space. The ability to accurately perform these tasks remotely and automatically leads to a significant increase in sample throughput and reliability for high-volume protein characterization efforts. Since the protein samples are placed in a shipping-compatible layered stack of sample cassettes each holding many samples, a large number of samples can be shipped in a single cryogenic shipping container.

A high throughput liquid crystal light shutter for unpolarized light using polymer polarization gratings

NASA Astrophysics Data System (ADS)

Komanduri, Ravi K.; Lawler, Kris F.; Escuti, Michael J.

2011-05-01

We report on a broadband, diffractive, light shutter with the ability to modulate unpolarized light. This polarizer-free approach employs a conventional liquid crystal (LC) switch, combined with broadband Polarization Gratings (PGs) formed with polymer LC materials. The thin-film PGs act as diffractive polarizing beam-splitters, while the LC switch operates on both orthogonal polarization states simultaneously. As an initial experimental proof-of- concept for unpolarized light with +/-7° aperture, we utilize a commercial twisted-nematic LC switch and our own polymer PGs to achieve a peak transmittance of 80% and peak contrast ratio of 230:1. We characterize the optoelectronic performance, discuss the limitations, and evaluate its use in potential nonmechanical shutter applications (imaging and non-imaging).

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids

PubMed Central

Zipper, Lauren E.; Aristide, Xavier; Bishop, Dylan P.; Joshi, Ishita; Kharzeev, Julia; Patel, Krishna B.; Santiago, Brianna M.; Joshi, Karan; Dorsinvil, Kahille; Sweet, Robert M.; Soares, Alexei S.

2014-01-01

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under different conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. The results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations. PMID:25484231

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids

DOE PAGES

Zipper, Lauren E.; Aristide, Xavier; Bishop, Dylan P.; ...

2014-11-28

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under differentmore » conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. Ultimately, the results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.« less

A finite element beam propagation method for simulation of liquid crystal devices.

PubMed

Vanbrabant, Pieter J M; Beeckman, Jeroen; Neyts, Kristiaan; James, Richard; Fernandez, F Anibal

2009-06-22

An efficient full-vectorial finite element beam propagation method is presented that uses higher order vector elements to calculate the wide angle propagation of an optical field through inhomogeneous, anisotropic optical materials such as liquid crystals. The full dielectric permittivity tensor is considered in solving Maxwell's equations. The wide applicability of the method is illustrated with different examples: the propagation of a laser beam in a uniaxial medium, the tunability of a directional coupler based on liquid crystals and the near-field diffraction of a plane wave in a structure containing micrometer scale variations in the transverse refractive index, similar to the pixels of a spatial light modulator.

X-Ray Diffraction and Imaging Study of Imperfections of Crystallized Lysozyme with Coherent X-Rays

NASA Technical Reports Server (NTRS)

Hu, Zheng-Wei; Chu, Y. S.; Lai, B.; Cai, Z.; Thomas, B. R.; Chernov, A. A.

2003-01-01

Phase-sensitive x-ray diffraction imaging and high angular-resolution diffraction combined with phase contrast radiographic imaging are employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in symmetric Laue case. The fill width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal is approximately 16.7 arcseconds, and defects, which include point defects, line defects, and microscopic domains, have been clearly observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front, and they have been found to originate mostly at a central growth area and occasionally at outer growth regions. Individual point defects trapped at a crystal nucleus are resolved in the images of high sensitivity to defects. Slow dehydration has led to the broadening of the 4 4 0 rocking curve by a factor of approximately 2.4. A significant change of the defect structure and configuration with drying has been revealed, which suggests the dehydration induced migration and evolution of dislocations and lattice rearrangements to reduce overall strain energy. The sufficient details of the observed defects shed light upon perfection, nucleation and growth, and properties of protein crystals.

A compensation method for the full phase retardance nonuniformity in phase-only liquid crystal on silicon spatial light modulators.

PubMed

Teng, Long; Pivnenko, Mike; Robertson, Brian; Zhang, Rong; Chu, Daping

2014-10-20

A simple and efficient compensation method for the full correction of both the anisotropic and isotropic nonuniformity of the light phase retardance in a liquid crystal (LC) layer is presented. This is achieved by accurate measurement of the spatial variation of the LC layer's thickness with the help of a calibrated liquid crystal wedge, rather than solely relying on the light intensity profile recorded using two crossed polarizers. Local phase retardance as a function of the applied voltage is calculated with its LC thickness and a set of reference data measured from the intensity of the reflected light using two crossed polarizers. Compensation of the corresponding phase nonuniformity is realized by applying adjusted local voltage signals for different grey levels. To demonstrate its effectiveness, the proposed method is applied to improve the performance of a phase-only liquid crystal on silicon (LCOS) spatial light modulator (SLM). The power of the first diffraction order measured with the binary phase gratings compensated by this method is compared with that compensated by the conventional crossed-polarizer method. The results show that the phase compensation method proposed here can increase the dynamic range of the first order diffraction power significantly from 15~21 dB to over 38 dB, while the crossed-polarizer method can only increase it to 23 dB.

Diketonylpyridinium Cations as a Support of New Ionic Liquid Crystals and Ion-Conductive Materials: Analysis of Counter-Ion Effects.

PubMed

Pastor, María Jesús; Cuerva, Cristián; Campo, José A; Schmidt, Rainer; Torres, María Rosario; Cano, Mercedes

2016-05-12

Ionic liquid crystals (ILCs) allow the combination of the high ionic conductivity of ionic liquids (ILs) with the supramolecular organization of liquid crystals (LCs). ILCs salts were obtained by the assembly of long-chained diketonylpyridinium cations of the type [HOO R(n)pyH ]⁺ and BF₄ - , ReO₄ - , NO₃ - , CF₃SO₃ - , CuCl₄ 2- counter-ions. We have studied the thermal behavior of five series of compounds by differential scanning calorimetry (DSC) and hot stage polarized light optical microscopy (POM). All materials show thermotropic mesomorphism as well as crystalline polymorphism. X-ray diffraction of the [HOO R(12)pyH ][ReO₄] crystal reveals a layered structure with alternating polar and apolar sublayers. The mesophases also exhibit a lamellar arrangement detected by variable temperature powder X-ray diffraction. The CuCl₄ 2- salts exhibit the best LC properties followed by the ReO₄ - ones due to low melting temperature and wide range of existence. The conductivity was probed for the mesophases in one species each from the ReO₄ - , and CuCl₄ 2- families, and for the solid phase in one of the non-mesomorphic Cl - salts. The highest ionic conductivity was found for the smectic mesophase of the ReO₄ - containing salt, whereas the solid phases of all salts were dominated by electronic contributions. The ionic conductivity may be favored by the mesophase lamellar structure.

Role of Molecular Structure on X-ray Diffraction in Thermotropic Uniaxial and Biaxial Nematic Liquid Crystal Phases

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

Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena

2009-08-27

X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution functionmore » is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.« less

Role of Molecular Structure on X-ray Diffraction in Uniaxial and Biaxial Phases of Thermotropic Liquid Crystals

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

Acharya, Bharat R.; Kang, Shin-Woong; Prasad, Veena

2009-04-29

X-ray diffraction is one of the most definitive methods to determine the structure of condensed matter phases, and it has been applied to unequivocally infer the structures of conventional calamitic and lyotropic liquid crystals. With the advent of bent-core and tetrapodic mesogens and the discovery of the biaxial nematic phase in them, the experimental results require more careful interpretation and analysis. Here, we present ab-initio calculations of X-ray diffraction patterns in the isotropic, uniaxial nematic, and biaxial nematic phases of bent-core mesogens. A simple Meier-Saupe-like molecular distribution function is employed to describe both aligned and unaligned mesophases. The distribution functionmore » is decomposed into two, polar and azimuthal, distribution functions to calculate the effect of the evolution of uniaxial and biaxial nematic orientational order. The calculations provide satisfactory semiquantitative interpretations of experimental results. The calculations presented here should provide a pathway to more refined and quantitative analysis of X-ray diffraction data from the biaxial nematic phase.« less

Experimental study of strong nonlinear-optics effects in liquid crystals

NASA Astrophysics Data System (ADS)

Darbin, S. D.; Arakelyan, S. M.; Cheung, M. M.; Shen, Y. R.

1984-07-01

Nonlinear optical effects that arise in nematic liquid crystals as a result of a change in the index of refraction induced by a laser field are considered. Since the resultant nonlinearity is extremely high, the approximation of perturbation theory cannot be used in calculations. However, the change in refractive index results mainly in phase advance as waves propagate through a thin film of liquid crystal, while the change of intensity is significant. Moreover, if there is no change in polarization of the pumping field, calculations are relatively simple. An investigation is made of the propagation of a cross sectionally bounded laser beam through a homeotropically oriented liquid crystal, giving rise to spatial phase modulation of emission. When the intensity of the laser beam exceeds a certain value, a system of aberation rings is observed in the output radiation. Effects of dynamic self-diffraction accompanying degenerate four-wave mixing when a change in refractive index is induced in a homeotropic liquid crystal film, and optical bistability in a nonlinear Fabry-Perot optical cavity, as well as generation of a self-oscillatory state in such a resonator are discussed.

Atomistic simulation of flow-induced crystallization at constant temperature

NASA Astrophysics Data System (ADS)

Baig, C.; Edwards, B. J.

2010-02-01

Semi-crystalline fibers, such as nylon, orlon, and spectra, play a crucial role in modern society in applications including clothing, medical devices, and aerospace technology. These applications rely on the enhanced properties that are generated in these fibers through the orientation and deformation of the constituent molecules of a molten liquid undergoing flow prior to crystallization; however, the atomistic mechanisms of flow-induced crystallization are not understood, and macroscopic theories that have been developed in the past to describe this behavior are semi-empirical. We present here the results of the first successful simulation of flow-induced crystallization at constant temperature using a nonequilibrium Monte Carlo algorithm for a short-chain polyethylene liquid. A phase transition between the liquid and crystalline phases was observed at a critical flow rate in elongational flow. The simulation results quantitatively matched experimental X-ray diffraction data of the crystalline phase. Examination of the configurational temperature generated under flow confirmed for the first time the hypothesis that flow-induced stresses within the liquid effectively raised the crystallization temperature of the liquid.

Physical properties of the Ce 2 M Al 7 Ge 4 heavy-fermion compounds ( M = Co , Ir , Ni , Pd )

DOE PAGES

Ghimire, N. J.; Cary, S. K.; Eley, S.; ...

2016-05-23

Here, we report the synthesis, crystal structure, and characterization by means of single-crystal x-ray diffraction, neutron powder diffraction, and magnetic, thermal, and transport measurements of the new heavy-fermion compounds Ce 2MAl 7Ge 4 (M=Co,Ir,Ni,Pd). These compounds crystallize in a noncentrosymmetric tetragonal space group Pmore » $$\\bar{4}$$2 1m, consisting of layers of square nets of Ce atoms separated by Ge-Al and M-Al-Ge blocks. Ce 2CoAl 7Ge 4,Ce 2IrAl 7Ge 4, and Ce 2NiAl 7Ge 4 order magnetically below TM=1.8, 1.6, and 0.8 K, respectively. There is no evidence of magnetic ordering in Ce 2PdAl 7Ge 4 down to 0.4 K. Furthermore, the small amount of entropy released in the magnetic state of Ce 2MAl 7Ge 4 (M = Co, Ir, Ni) and the reduced specific heat jump at T M suggest a strong Kondo interaction in these materials. Ce 2PdAl 7Ge 4 shows non-Fermi liquid behavior, possibly due to the presence of a nearby quantum critical point.« less

In situ Raman and synchrotron X-ray diffraction study on crystallization of Choline chloride/Urea deep eutectic solvent under high pressure

NASA Astrophysics Data System (ADS)

Yuan, Chaosheng; Chu, Kunkun; Li, Haining; Su, Lei; Yang, Kun; Wang, Yongqiang; Li, Xiaodong

2016-09-01

Pressure-induced crystallization of Choline chloride/Urea (ChCl/Urea) deep eutectic solvent (DES) has been investigated by in-situ Raman spectroscopy and synchrotron X-ray diffraction. The results indicated that high pressure crystals appeared at around 2.6 GPa, and the crystalline structure was different from that formed at ambient pressure. Upon increasing the pressure, the Nsbnd H stretching modes of Urea underwent dramatic change after liquid-solid transition. It appears that high pressures may enhance the hydrogen bonds formed between ChCl and Urea. P versus T phase diagram of ChCl/Urea DES was constructed, and the crystallization mechanism of ChCl/Urea DES was discussed in view of hydrogen bonds.

Manipulating terahertz wave by a magnetically tunable liquid crystal phase grating.

PubMed

Lin, Chia-Jen; Li, Yu-Tai; Hsieh, Cho-Fan; Pan, Ru-Pin; Pan, Ci-Ling

2008-03-03

This investigation demonstrates the feasibility of a magnetically tunable liquid crystal phase grating for the terahertz wave. The phase grating can be used as a beam splitter. The ratio of the zeroth and first-order diffracted THz-beams (0.3 THz) polarized in a direction perpendicular to that of the grooves of the grating can be tuned from 4:1 to 1:2. When the THz wave is polarized in any other direction, this device can be operated as a polarizing beam splitter.

Note: Laser beam scanning using a ferroelectric liquid crystal spatial light modulator

NASA Astrophysics Data System (ADS)

Das, Abhijit; Boruah, Bosanta R.

2014-04-01

In this work we describe laser beam scanning using a ferroelectric liquid crystal spatial light modulator. Commercially available ferroelectric liquid crystal spatial light modulators are capable of displaying 85 colored images in 1 s using a time dithering technique. Each colored image, in fact, comprises 24 single bit (black and white) images displayed sequentially. We have used each single bit image to write a binary phase hologram. For a collimated laser beam incident on the hologram, one of the diffracted beams can be made to travel along a user defined direction. We have constructed a beam scanner employing the above arrangement and demonstrated its use to scan a single laser beam in a laser scanning optical sectioning microscope setup.

Dielectric properties of nematic liquid crystal doped with Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Maleki, A.; Ara, M. H. Majles; Saboohi, F.

2017-04-01

The influence of Fe3O4 nanoparticles (NPs) on dielectric properties of planar and homeotropic oriented nematic liquid crystals (NLCs) were studied during the temperature interval of 298-322 °K. It was found that the dielectric permittivity was considerably increased by adding NPs mass percentages. The structural characterization of the synthesized NPs with the scale 14-18 nm has been analyzed by the X-ray diffraction and field-emission scanning electron microscopy results. The obtained dielectric anisotropy (?) and mean dielectric (?) have shown an immense increment in the value of 1% and 10% wt. NPs doped NLCs, respectively. These results were assigned to the strong dipole-dipole interaction between the superparamagnetic particles and the surrounding liquid crystal molecules.

Experimental Evidence of Low Density Liquid Water under Decompression

NASA Astrophysics Data System (ADS)

Shen, G.; Lin, C.; Sinogeikin, S. V.; Smith, J.

2017-12-01

Water is not only the most important substance for life, but also plays important roles in liquid science for its anomalous properties. It has been widely accepted that water's anomalies are not a result of simple thermal fluctuation, but are connected to the formation of various structural aggregates in the hydrogen bonding network. Among several proposed scenarios, one model of fluctuations between two different liquids has gradually gained traction. These two liquids are referred to as a low-density liquid (LDL) and a high-density liquid (HDL) with a coexistence line in the deeply supercooled regime at elevated pressure. The LDL-HDL transition ends with decreasing pressure at a liquid-liquid critical point (LLCP) with its Widom line extending to low pressures. Above the Widom line lies mostly HDL which is favored by entropy, while LDL, mostly lying below the Widom line, is favored by enthalpy in the tetrahedral hydrogen bonding network. The origin of water's anomalies can then be explained by the increase in structural fluctuations, as water is cooled down to deeply supercooled temperatures approaching the Widom line. Because both the LLCP and the LDL-HDL transition line lie in water's "no man's land" between the homogeneous nucleation temperature (TH, 232 K) and the crystallization temperature (TX, 150 K), the success of experiments exploring this region has been limited thus far. Using a rapid decompression technique integrated with in situ x-ray diffraction, we observe that a high-pressure ice phase transforms to a low-density noncrystalline (LDN) form upon rapid release of pressure at temperatures of 140-165K. The LDN subsequently crystallizes into ice-Ic through a diffusion-controlled process. The change in crystallization rate with temperature indicates that the LDN is a LDL with its tetrahedrally-coordinated network fully developed and clearly linked to low-density amorphous ices. The observation of the tetrahedral LDL supports the two-liquid model for water including the existence of a LLCP.

Crystallization kinetics and molecular mobility of an amorphous active pharmaceutical ingredient: A case study with Biclotymol.

PubMed

Schammé, Benjamin; Couvrat, Nicolas; Malpeli, Pascal; Delbreilh, Laurent; Dupray, Valérie; Dargent, Éric; Coquerel, Gérard

2015-07-25

The present case study focuses on the crystallization kinetics and molecular mobility of an amorphous mouth and throat drug namely Biclotymol, through differential scanning calorimetry (DSC), temperature resolved X-ray powder diffraction (TR-XRPD) and hot stage microscopy (HSM). Kinetics of crystallization above the glass transition through isothermal and non-isothermal cold crystallization were considered. Avrami model was used for isothermal crystallization process. Non-isothermal cold crystallization was investigated through Augis and Bennett model. Differences between crystallization processes have been ascribed to a site-saturated nucleation mechanism of the metastable form, confirmed by optical microscopy images. Regarding molecular mobility, a feature of molecular dynamics in glass-forming liquids as thermodynamic fragility index m was determined through calorimetric measurements. It turned out to be around m=100, describing Biclotymol as a fragile glass-former for Angell's classification. Relatively long-term stability of amorphous Biclotymol above Tg was analyzed indirectly by calorimetric monitoring to evaluate thermodynamic parameters and crystallization behavior of glassy Biclotymol. Within eight months of storage above Tg (T=Tg+2°C), amorphous Biclotymol does not show a strong inclination to crystallize and forms a relatively stable glass. This case study, involving a multidisciplinary approach, points out the importance of continuing looking for stability predictors. Copyright © 2015 Elsevier B.V. All rights reserved.

Low-Absorption Liquid Crystals for Infrared Beam Steering

DTIC Science & Technology

2013-10-22

Low absorption, MWIR, chlorinated liquid crystals, fluorination, FTIR, eutectic mixture, deuteration, nematic phase, birefringence, overtone...absorption compounds for LWIR and SWIR are also investigated. Key words: Low absorption, MWIR, chlorinated liquid crystals, fluorination, FTIR, eutectic ...the melting point significantly. We did careful investigation and formed a eutectic mixture consisting of five fluorinated compounds without any

Three-Dimensional Model of Holographic Formation of Inhomogeneous PPLC Diffraction Structures

NASA Astrophysics Data System (ADS)

Semkin, A. O.; Sharangovich, S. N.

2018-05-01

A three-dimensional theoretical model of holographic formation of inhomogeneous diffraction structures in composite photopolymer - liquid crystal materials is presented considering both the nonlinearity of recording and the amplitude-phase inhomogeneity of the recording light field. Based on the results of numerical simulation, the kinematics of formations of such structures and their spatial profile are investigated.

Flat liquid crystal diffractive lenses with variable focus and magnification

NASA Astrophysics Data System (ADS)

Valley, Pouria

Non-mechanical variable lenses are important for creating compact imaging devices. Various methods employing dielectrically actuated lenses, membrane lenses, and liquid crystal lenses were previously proposed [1-4]. In This dissertation the design, fabrication, and characterization of innovative flat tunable-focus liquid crystal diffractive lenses (LCDL) are presented. LCDL employ binary Fresnel zone electrodes fabricated on Indium-Tin-Oxide using conventional micro-photolithography. The light phase can be adjusted by varying the effective refractive index of a nematic liquid crystal sandwiched between the electrodes and a reference substrate. Using a proper voltage distribution across various electrodes the focal length can be changed between several discrete values. Electrodes are shunted such that the correct phase retardation step sequence is achieved. If the number of 2pi zone boundaries is increased by a factor of m the focal length is changed from f to f/m based on the digitized Fresnel zone equation: f = rm2/2mlambda, where r m is mth zone radius, and lambda is the wavelength. The chromatic aberration of the diffractive lens is addressed and corrected by adding a variable fluidic lens. These LCDL operate at very low voltage levels (+/-2.5V ac input), exhibit fast switching times (20-150 ms), can have large apertures (>10 mm), and small form factor, and are robust and insensitive to vibrations, gravity, and capillary effects that limit membrane and dielectrically actuated lenses. Several tests were performed on the LCDL including diffraction efficiency measurement, switching dynamics, and hybrid imaging with a refractive lens. Negative focal lengths are achieved by adjusting the voltages across electrodes. Using these lenses in combination, magnification can be changed and zoom lenses can be formed. These characteristics make LCDL a good candidate for a variety of applications including auto-focus and zoom lenses in compact imaging devices such as camera phones. A business plan centered on this technology was developed as part of the requirements for the minor in entrepreneurship from the Eller College of Management. An industrial analysis is presented in this study that involves product development, marketing, and financial analyses (Appendix I).

Solvent exchange in a metal–organic framework single crystal monitored by dynamic in situ X-ray diffraction

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

Cox, Jordan M.; Walton, Ian M.; Bateman, Gage

2017-07-25

Understanding the processes by which porous solid-state materials adsorb and release guest molecules would represent a significant step towards developing rational design principles for functional porous materials. To elucidate the process of liquid exchange in these materials, dynamicin situX-ray diffraction techniques have been developed which utilize liquid-phase chemical stimuli. Using these time-resolved diffraction techniques, the ethanol solvation process in a flexible metal–organic framework [Co(AIP)(bpy) 0.5(H 2O)]·2H 2O was examined. The measurements provide important insight into the nature of the chemical transformation in this system including the presence of a previously unreported neat ethanol solvate structure.

A Low Voltage Liquid Crystal Phase Grating with Switchable Diffraction Angles

PubMed Central

Chen, Haiwei; Tan, Guanjun; Huang, Yuge; Weng, Yishi; Choi, Tae-Hoon; Yoon, Tae-Hoon; Wu, Shin-Tson

2017-01-01

We demonstrate a simple yet high performance phase grating with switchable diffraction angles using a fringe field switching (FFS) liquid crystal (LC) cell. The LC rubbing angle is parallel to the FFS electrodes (i.e. α = 0°), leading to symmetric LC director distribution in a voltage-on state. Such a grating exhibits three unique features: 1) Two grating periods can be formed by controlling the applied voltage, resulting in switchable diffraction angles. In our design, the 1st diffraction order occurs at 4.3°, while the 2nd order appears at 8.6°. 2) The required voltage to achieve peak diffraction efficiency (η~32%) for the 1st order is only 4.4 V at λ = 633 nm as compared to 70 V for a conventional FFS-based phase grating in which α ≈ 7°, while the 2nd order (η~27%) is 15 V. 3). The measured rise and decay time for the 1st order is 7.62 ms and 6.75 ms, and for the 2nd order is 0.75 ms and 3.87 ms, respectively. To understand the physical mechanisms, we also perform device simulations. Good agreement between experiment and simulation is obtained. PMID:28054592

Growing Larger Crystals for Neutron Diffraction

NASA Technical Reports Server (NTRS)

Pusey, Marc

2003-01-01

Obtaining crystals of suitable size and high quality has been a major bottleneck in macromolecular crystallography. With the advent of advanced X-ray sources and methods the question of size has rapidly dwindled, almost to the point where if one can see the crystal then it was big enough. Quality is another issue, and major national and commercial efforts were established to take advantage of the microgravity environment in an effort to obtain higher quality crystals. Studies of the macromolecule crystallization process were carried out in many labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. While technological improvements are resulting in a diminishing of the minimum crystal size required, neutron diffraction structural studies still require considerably larger crystals, by several orders of magnitude, than X-ray studies. From a crystal growth physics perspective there is no reason why these 'large' crystals cannot be obtained: the question is generally more one of supply than limitations mechanism. This talk will discuss our laboratory s current model for macromolecule crystal growth, with highlights pertaining to the growth of crystals suitable for neutron diffraction studies.

Self-interferometric technique for visualization of phase patterns encoded onto a liquid-crystal display

NASA Astrophysics Data System (ADS)

Bentley, Joel B.; Davis, Jeffrey A.; Albero, Jorge; Moreno, Ignacio

2006-10-01

We report a new self-interferometric technique for visualizing phase patterns that are encoded onto a phase-only liquid-crystal display (LCD). In our approach, the LCD generates both the desired object beam as well as the reference beam. Normally the phase patterns are encoded with a phase depth of 2π radians, and all of the incident energy is diffracted into the first-order beam. However, by reducing this phase depth, we can generate an additional zero-order diffracted beam, which acts as the reference beam. We work at distances such that these two patterns spatially interfere, producing an interference pattern that displays the encoded phase pattern. This approach was used recently to display the phase vortices of helical Ince-Gaussian beams. Here we show additional experimental results and analyze the process.

Wide-field-of-view nanoscale Bragg liquid crystal polarization gratings

NASA Astrophysics Data System (ADS)

Xiang, Xiao; Kim, Jihwan; Escuti, Michael J.

2018-02-01

Here, we demonstrate a liquid crystal (LC) polymer Bragg polarization grating (PG) with large angular band- width and high efficiency in transmission-mode for 532 nm wavelength and 400 nm period. The field-of-view (FOV ) is increased significantly while preserving high diffraction efficiency by realizing a monolithic grating comprising two different slants. Using rigorous coupled-wave analysis simulation, we identified a structure with 48° FOV and 70% average first-order efficiency. We then experimentally fabricated and characterized the grating with a photo-aligned LC polymer network, also known as reactive mesogens. We measured 40° FOV and nearly 80% average diffraction efficiency. With this broadened and fairly uniform angular response, this wide FOV Bragg PG is a compelling option for large deflection-angle applications, including near-eye display in augmented reality systems, waveguide based illumination, and beam steering.

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

Limitation of Liquid Crystal on Silicon Spatial Light Modular for Holographic Three-dimensional Displays

NASA Technical Reports Server (NTRS)

Wang, Xinghua; Wang, Bin; Bos, Philip J.; Anderson, James E.; Kujawinska, Malgorzata; Pouch, John; Miranda, Feliz

2004-01-01

In a 3-D display system based on an opto-electronic reconstruction of a digitally recorded hologram, the field of view of such a system is limited by the spatial resolution of the liquid crystal on silicon (LCOS) spatial light modular (SLM) used to perform the opto-electronic reconstruction. In this article, the special resolution limitation of LCOS SLM associated with the fringe field effect and interpixel coupling is determined by the liquid crystal detector simulation and the Finite Difference Time Domain (FDTD) simulation. The diffraction efficiency loss associated with the imperfection in the phase profile is studied with an example of opto-electronic reconstruction of an amplitude object. A high spatial resolution LCOS SLM with a wide reconstruction angle is proposed.

Tuning the group delay of optical wave packets in liquid-crystal light valves

NASA Astrophysics Data System (ADS)

Bortolozzo, U.; Residori, S.; Huignard, J. P.

2009-05-01

By performing two-wave mixing experiments in a liquid-crystal light valve, optical pulses are slowed down to group velocities as slow as a few tenths of mm/s, corresponding to a very large group index. We present experiments and model of the slow-light process occurring in the liquid-crystal light valve, showing that this is characterized by multiple-beam diffraction in the Raman-Nath regime. Depending on the initial frequency detuning between pump and signal, the different output order beams are distinguished by different group delays. The group delay can be tuned by changing the main parameters of the experiment: the detuning between the pump and the input wave packet, the strength of the nonlinearity, and the intensity of the pump beam.

Colloidal crystal growth monitored by Bragg diffraction interference fringes.

PubMed

Bohn, Justin J; Tikhonov, Alexander; Asher, Sanford A

2010-10-15

We monitored the crystal growth kinetics of crystallization of a shear melted crystalline colloidal array (CCA). The fcc CCA heterogeneously nucleates at the flow cell wall surface. We examined the evolution of the (1 1 1) Bragg diffraction peak, and, for the first time, quantitatively monitored growth by measuring the temporal evolution of the Bragg diffraction interference fringes. Modeling of the evolution of the fringe patterns exposes the time dependence of the increasing crystal thickness. The initial diffusion-driven linear growth is followed by ripening-driven growth. Between 80 and 90 microM NaCl concentrations the fcc crystals first linearly grow at rates between 1.9 and 4.2 microm/s until they contact homogeneously nucleated crystals in the bulk. At lower salt concentrations interference fringes are not visible because the strong electrostatic interactions between particles result in high activation barriers, preventing defect annealing and leading to a lower crystal quality. The fcc crystals melt to a liquid phase at >90 microM NaCl concentrations. Increasing NaCl concentrations slow the fcc CCA growth rate consistent with the expectation of the classical Wilson-Frenkel growth theory. The final thickness of wall-nucleated CCA, that is determined by the competition between growth of heterogeneously and homogenously nucleated CCA, increases with higher NaCl concentrations. Copyright 2010 Elsevier Inc. All rights reserved.

Ultrasound liquid crystal lens

NASA Astrophysics Data System (ADS)

Shimizu, Yuki; Koyama, Daisuke; Fukui, Marina; Emoto, Akira; Nakamura, Kentaro; Matsukawa, Mami

2018-04-01

A variable-focus lens using a combination of liquid crystals and ultrasound is discussed. The lens uses a technique based on ultrasound vibration to control the molecular orientation of the liquid crystal. The lens structure is simple, with no mechanical moving parts and no transparent electrodes, which is helpful for device downsizing; the structure consists of a liquid crystal layer sandwiched between two glass substrates with a piezoelectric ring. The tens-of-kHz ultrasonic resonance flexural vibration used to excite the lens generates an acoustic radiation force on the liquid crystal layer to induce changes in the molecular orientation of the liquid crystal. The orientations of the liquid crystal molecules and the optical characteristics of the lens were investigated under ultrasound excitation. Clear optical images were observed through the lens, and the focal point could be controlled using the input voltage to the piezoelectric ring to give the lens its variable-focus action.

Electrically Reconfigurable Liquid Crystalline Mirrors (Postprint)

DTIC Science & Technology

2018-04-24

preparation of a structurally chiral polymer stabilizing network that enforces anchoring of a low-molar- mass liquid crystalline media with positive...crystals (LCs). The distinctive responses detailed here are enabled by the preparation of a structurally chiral polymer stabilizing network that enforces ...aerospace systems . Dynamic changes to optical material properties including absorption, diffraction, reflection, and scatter have been the subject to

Naturally occurring vapor-liquid-solid (VLS) Whisker growth of germanium sulfide

USGS Publications Warehouse

Finkelman, R.B.; Larson, R.R.; Dwornik, E.J.

1974-01-01

The first naturally occurring terrestrial example of vapor-liquid-solid (VLS) growth has been observed in condensates from gases released by burning coal in culm banks. Scanning electron microscopy, X-ray diffraction, and energy dispersive analysis indicate that the crystals consist of elongated rods (??? 100 ??m) of germanium sulfide capped by bulbs depleted in germanium. ?? 1974.

Metastable liquid-liquid transition in a molecular model of water

NASA Astrophysics Data System (ADS)

Palmer, Jeremy C.; Martelli, Fausto; Liu, Yang; Car, Roberto; Panagiotopoulos, Athanassios Z.; Debenedetti, Pablo G.

2014-06-01

Liquid water's isothermal compressibility and isobaric heat capacity, and the magnitude of its thermal expansion coefficient, increase sharply on cooling below the equilibrium freezing point. Many experimental, theoretical and computational studies have sought to understand the molecular origin and implications of this anomalous behaviour. Of the different theoretical scenarios put forward, one posits the existence of a first-order phase transition that involves two forms of liquid water and terminates at a critical point located at deeply supercooled conditions. Some experimental evidence is consistent with this hypothesis, but no definitive proof of a liquid-liquid transition in water has been obtained to date: rapid ice crystallization has so far prevented decisive measurements on deeply supercooled water, although this challenge has been overcome recently. Computer simulations are therefore crucial for exploring water's structure and behaviour in this regime, and have shown that some water models exhibit liquid-liquid transitions and others do not. However, recent work has argued that the liquid-liquid transition has been mistakenly interpreted, and is in fact a liquid-crystal transition in all atomistic models of water. Here we show, by studying the liquid-liquid transition in the ST2 model of water with the use of six advanced sampling methods to compute the free-energy surface, that two metastable liquid phases and a stable crystal phase exist at the same deeply supercooled thermodynamic condition, and that the transition between the two liquids satisfies the thermodynamic criteria of a first-order transition. We follow the rearrangement of water's coordination shell and topological ring structure along a thermodynamically reversible path from the low-density liquid to cubic ice. We also show that the system fluctuates freely between the two liquid phases rather than crystallizing. These findings provide unambiguous evidence for a liquid-liquid transition in the ST2 model of water, and point to the separation of time scales between crystallization and relaxation as being crucial for enabling it.

Metastable liquid-liquid transition in a molecular model of water.

PubMed

Palmer, Jeremy C; Martelli, Fausto; Liu, Yang; Car, Roberto; Panagiotopoulos, Athanassios Z; Debenedetti, Pablo G

2014-06-19

Liquid water's isothermal compressibility and isobaric heat capacity, and the magnitude of its thermal expansion coefficient, increase sharply on cooling below the equilibrium freezing point. Many experimental, theoretical and computational studies have sought to understand the molecular origin and implications of this anomalous behaviour. Of the different theoretical scenarios put forward, one posits the existence of a first-order phase transition that involves two forms of liquid water and terminates at a critical point located at deeply supercooled conditions. Some experimental evidence is consistent with this hypothesis, but no definitive proof of a liquid-liquid transition in water has been obtained to date: rapid ice crystallization has so far prevented decisive measurements on deeply supercooled water, although this challenge has been overcome recently. Computer simulations are therefore crucial for exploring water's structure and behaviour in this regime, and have shown that some water models exhibit liquid-liquid transitions and others do not. However, recent work has argued that the liquid-liquid transition has been mistakenly interpreted, and is in fact a liquid-crystal transition in all atomistic models of water. Here we show, by studying the liquid-liquid transition in the ST2 model of water with the use of six advanced sampling methods to compute the free-energy surface, that two metastable liquid phases and a stable crystal phase exist at the same deeply supercooled thermodynamic condition, and that the transition between the two liquids satisfies the thermodynamic criteria of a first-order transition. We follow the rearrangement of water's coordination shell and topological ring structure along a thermodynamically reversible path from the low-density liquid to cubic ice. We also show that the system fluctuates freely between the two liquid phases rather than crystallizing. These findings provide unambiguous evidence for a liquid-liquid transition in the ST2 model of water, and point to the separation of time scales between crystallization and relaxation as being crucial for enabling it.

Effect of 120 MeV Ag9+ ion irradiation of YCOB single crystals

NASA Astrophysics Data System (ADS)

Arun Kumar, R.; Dhanasekaran, R.

2012-09-01

Single crystals of yttrium calcium oxy borate (YCOB) grown from boron-tri-oxide flux were subjected to swift heavy ion irradiation using silver Ag9+ ions from the 15 UD Pelletron facility at Inter University Accelerator Center, New Delhi. The crystals were irradiated at 1 × 1013, 5 × 1013 and 1 × 1014 ions/cm2 fluences at room temperature and with 5 × 1013 ions/cm2 fluence at liquid nitrogen temperature. The pristine and the irradiated samples were characterized by glancing angle X-ray diffraction, UV-Vis-NIR and photoluminescence studies. From the characterization studies performed on the samples, it is inferred that the crystals irradiated at liquid nitrogen temperature had fewer defects compared to the crystals irradiated at room temperature and the defects increased when the ion fluence was increased at room temperature.

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids

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

Zipper, Lauren E.; Binghamton University, 4400 Vestal Parkway East, Vestal, NY 13902; Aristide, Xavier

This article describes the use of evaporation control lids that are fitted to crystallization plates to improve the reproducibility of trials using as little as 5 nl. The plate lids contain apertures which are large enough for the transfer of protein containing droplets, but small enough to greatly reduce the rate of evaporation during the time needed to prepare the plate. A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fittingmore » the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under different conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. The results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.« less

Diketonylpyridinium Cations as a Support of New Ionic Liquid Crystals and Ion-Conductive Materials: Analysis of Counter-Ion Effects

PubMed Central

Pastor, María Jesús; Cuerva, Cristián; Campo, José A.; Schmidt, Rainer; Torres, María Rosario; Cano, Mercedes

2016-01-01

Ionic liquid crystals (ILCs) allow the combination of the high ionic conductivity of ionic liquids (ILs) with the supramolecular organization of liquid crystals (LCs). ILCs salts were obtained by the assembly of long-chained diketonylpyridinium cations of the type [HOOR(n)pyH]+ and BF4−, ReO4−, NO3−, CF3SO3−, CuCl42− counter-ions. We have studied the thermal behavior of five series of compounds by differential scanning calorimetry (DSC) and hot stage polarized light optical microscopy (POM). All materials show thermotropic mesomorphism as well as crystalline polymorphism. X-ray diffraction of the [HOOR(12)pyH][ReO4] crystal reveals a layered structure with alternating polar and apolar sublayers. The mesophases also exhibit a lamellar arrangement detected by variable temperature powder X-ray diffraction. The CuCl42− salts exhibit the best LC properties followed by the ReO4− ones due to low melting temperature and wide range of existence. The conductivity was probed for the mesophases in one species each from the ReO4−, and CuCl42− families, and for the solid phase in one of the non-mesomorphic Cl− salts. The highest ionic conductivity was found for the smectic mesophase of the ReO4− containing salt, whereas the solid phases of all salts were dominated by electronic contributions. The ionic conductivity may be favored by the mesophase lamellar structure. PMID:28773485

Crystallization and preliminary crystallographic analysis of latent, active and recombinantly expressed aurone synthase, a polyphenol oxidase, from Coreopsis grandiflora

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

Molitor, Christian; Mauracher, Stephan Gerhard; Rompel, Annette, E-mail: annette.rompel@univie.ac.at

2015-05-22

Latent and active aurone synthase purified from petals of C. grandiflora (cgAUS1) were crystallized. The crystal quality of recombinantly expressed latent cgAUS1 was significantly improved by co-crystallization with the polyoxotungstate Na{sub 6}[TeW{sub 6}O{sub 24}] within the liquid–liquid phase-separation zone. Aurone synthase (AUS), a member of a novel group of plant polyphenol oxidases (PPOs), catalyzes the oxidative conversion of chalcones to aurones. Two active cgAUS1 (41.6 kDa) forms that differed in the level of phosphorylation or sulfation as well as the latent precursor form (58.9 kDa) were purified from the petals of Coreopsis grandiflora. The differing active cgAUS1 forms and themore » latent cgAUS1 as well as recombinantly expressed latent cgAUS1 were crystallized, resulting in six different crystal forms. The active forms crystallized in space groups P2{sub 1}2{sub 1}2{sub 1} and P12{sub 1}1 and diffracted to ∼1.65 Å resolution. Co-crystallization of active cgAUS1 with 1,4-resorcinol led to crystals belonging to space group P3{sub 1}21. The crystals of latent cgAUS1 belonged to space group P12{sub 1}1 and diffracted to 2.50 Å resolution. Co-crystallization of recombinantly expressed pro-AUS with the hexatungstotellurate(VI) salt Na{sub 6}[TeW{sub 6}O{sub 24}] within the liquid–liquid phase separation zone significantly improved the quality of the crystals compared with crystals obtained without hexatungstotellurate(VI)« less

Physical properties of new binary antiferroelectric liquid crystal mixtures

NASA Astrophysics Data System (ADS)

Fitas, Jakub; Jaworska-Gołąb, Teresa; Deptuch, Aleksandra; Tykarska, Marzena; Kurp, Katarzyna; Żurowska, Magdalena; Marzec, Monika

2018-02-01

Three newly prepared binary mixtures exhibiting chiral tilted smectic phases have been studied using differential scanning calorimetry, dielectric spectroscopy and electro-optic method, as well as X-ray diffraction. Broad temperature range of ferroelectric and antiferroelectric phases was detected in these mixtures and temperature dependence of spontaneous polarization, tilt angle and switching time were measured for all of them. It's occurred that all of the studied mixtures are orthoconic antiferroelectric liquid crystals. Based on the X-ray diffraction results, the temperature dependence of layer thickness in the paraelectric, ferroelectric and antiferroelectric phases was found. By using dielectric spectroscopy, Goldstone mode was identified in the ferroelectric phase, while antiphase fluctuations of azimuthal angle have been found in the antiferroelectric phase. Based on the results of the complementary methods, the transition temperatures were found as well as the order of the para-ferroelectric phase transition was determined as non-continuous one with critical parameter β equal to ca. 0.25.

LASER APPLICATIONS AND OTHER TOPICS IN QUANTUM ELECTRONICS: Influence of the layer thickness and concentration of dye molecules on the emission amplification in cholesteric liquid crystals

NASA Astrophysics Data System (ADS)

Alaverdyan, R. B.; Gevorgyan, A. A.; Chilingaryan, A. D.; Chilingaryan, Yu S.

2008-05-01

The propagation of light through a planar layer of a cholesteric liquid crystal doped with dye molecules is considered. The features of the emission spectra of the crystal are studied both in the absence and presence of dielectric boundaries. The increase in the emission intensity is investigated for different layer thicknesses and different concentrations of dye molecules. It is shown that an anomalously strong increase in the emission intensity with the diffraction intrinsic polarisation takes place in the case of a comparatively small crystal thickness and a relatively low concentration of dye molecules. The obtained results can be used for the development of miniature lasers with the circular polarisation of the fundamental radiation mode.

Tunable two-dimensional photonic crystals using liquid crystal infiltration

NASA Astrophysics Data System (ADS)

Leonard, S. W.; Mondia, J. P.; van Driel, H. M.; Toader, O.; John, S.; Busch, K.; Birner, A.; Gösele, U.; Lehmann, V.

2000-01-01

The photonic band gap of a two-dimensional photonic crystal is continuously tuned using the temperature dependent refractive index of a liquid crystal. Liquid crystal E7 was infiltrated into the air pores of a macroporous silicon photonic crystal with a triangular lattice pitch of 1.58 μm and a band gap wavelength range of 3.3-5.7 μm. After infiltration, the band gap for the H polarized field shifted dramatically to 4.4-6.0 μm while that of the E-polarized field collapsed. As the sample was heated to the nematic-isotropic phase transition temperature of the liquid crystal (59 °C), the short-wavelength band edge of the H gap shifted by as much as 70 nm while the long-wavelength edge was constant within experimental error. Band structure calculations incorporating the temperature dependence of the liquid crystal birefringence can account for our results and also point to an escaped-radial alignment of the liquid crystal in the nematic phase.

All-optical image processing with nonlinear liquid crystals

NASA Astrophysics Data System (ADS)

Hong, Kuan-Lun

Liquid crystals are fascinating materials because of several advantages such as large optical birefringence, dielectric anisotropic, and easily compatible to most kinds of materials. Compared to the electro-optical properties of liquid crystals widely applied in displays and switching application, transparency through most parts of wavelengths also makes liquid crystals a better candidate for all-optical processing. The fast response time of liquid crystals resulting from multiple nonlinear effects, such as thermal and density effect can even make real-time processing realized. In addition, blue phase liquid crystals with spontaneously self-assembled three dimensional cubic structures attracted academic attention. In my dissertation, I will divide the whole contents into six parts. In Chapter 1, a brief introduction of liquid crystals is presented, including the current progress and the classification of liquid crystals. Anisotropy and laser induced director axis reorientation is presented in Chapter 2. In Chapter 3, I will solve the electrostrictive coupled equation and analyze the laser induced thermal and density effect in both static and dynamic ways. Furthermore, a dynamic simulation of laser induced density fluctuation is proposed by applying finite element method. In Chapter 4, two image processing setups are presented. One is the intensity inversion experiment in which intensity dependent phase modulation is the mechanism. The other is the wavelength conversion experiment in which I can read the invisible image with a visible probe beam. Both experiments are accompanied with simulations to realize the matching between the theories and practical experiment results. In Chapter 5, optical properties of blue phase liquid crystals will be introduced and discussed. The results of grating diffractions and thermal refractive index gradient are presented in this chapter. In addition, fiber arrays imaging and switching with BPLCs will be included in this chapter. Finally, I will give a brief summary and mention a few future researches in Chapter 6.

Multi-level diffractive optics for single laser exposure fabrication of telecom-band diamond-like 3-dimensional photonic crystals.

PubMed

Chanda, Debashis; Abolghasemi, Ladan E; Haque, Moez; Ng, Mi Li; Herman, Peter R

2008-09-29

We present a novel multi-level diffractive optical element for diffractive optic near-field lithography based fabrication of large-area diamond-like photonic crystal structure in a single laser exposure step. A multi-level single-surface phase element was laser fabricated on a thin polymer film by two-photon polymerization. A quarter-period phase shift was designed into the phase elements to generate a 3D periodic intensity distribution of double basis diamond-like structure. Finite difference time domain calculation of near-field diffraction patterns and associated isointensity surfaces are corroborated by definitive demonstration of a diamond-like woodpile structure formed inside thick photoresist. A large number of layers provided a strong stopband in the telecom band that matched predictions of numerical band calculation. SEM and spectral observations indicate good structural uniformity over large exposure area that promises 3D photonic crystal devices with high optical quality for a wide range of motif shapes and symmetries. Optical sensing is demonstrated by spectral shifts of the Gamma-Zeta stopband under liquid emersion.

Lasing in a nematic liquid crystal cell with an interdigitated electrode system

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

Shtykov, N M; Palto, S P; Umanskii, B A

2015-04-30

Waveguide lasing in a layer of a dye-doped nematic liquid crystal has been observed. The liquid-crystal layer was sandwiched between a quartz substrate and a glass cover plate on whose surface was deposited an interdigitated electrode system. This system had a period of 3.75 μm and played a dual role, namely, it created a spatial periodicity of the waveguide medium refractive index (thus creating distributed feedback) and served as a diffraction grating coupling out a part of waveguide radiation into the glass cover plate. The distributed feedback ensured lasing in the 18th diffraction order for the TE modes and inmore » the 19th order for the TM modes of the waveguide. The generated radiation was observed at the exit from the glass plate end face at the angles to the waveguide plane of 33.1 ± 1.5° for TM modes and 21.8 ± 1.8° for TE modes. The intensity and position of the TE emission line showed no regular dependence on the voltage on the electrodes. In the case of TM radiation, an increase in the voltage led to a short-wavelength shift of the laser line and to a decrease in its intensity. (lasers)« less

Intangible pointlike tracers for liquid-crystal-based microsensors

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

Brasselet, Etienne; Juodkazis, Saulius

2010-12-15

We propose an optical detection technique for liquid-crystal-based sensors that is based on polarization-resolved tracking of optical singularities and does not rely on standard observation of light-intensity changes caused by modifications of the liquid crystal orientational ordering. It uses a natural two-dimensional network of polarization singularities embedded in the transverse cross section of a probe beam that passes through a liquid crystal sample, in our case, a nematic droplet held in laser tweezers. The identification and spatial evolution of such a topological fingerprint is retrieved from subwavelength polarization-resolved imaging, and the mechanical constraint exerted on the molecular ordering by themore » trapping beam itself is chosen as the control parameter. By restricting our analysis to one type of point singularity, C points, which correspond to location in space where the polarization azimuth is undefined, we show that polarization singularities appear as intangible pointlike tracers for liquid-crystal-based three-dimensional microsensors. The method has a superresolution potential and can be used to visualize changes at the nanoscale.« less

Study of structural and optical properties of YAG and Nd:YAG single crystals

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

Kostić, S.; Lazarević, Z.Ž., E-mail: lzorica@yahoo.com; Radojević, V.

2015-03-15

Highlights: • Transparent YAG and pale pink Nd:YAG single crystals were produced by the Czochralski technique. • Growth mechanisms and shape of the liquid/solid interface and incorporation of Nd{sup 3+} were studied. • The structure of the crystals was investigated by X-ray diffraction, Raman and IR spectroscopy. • The 15 Raman and 17 IR modes were observed. • The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. - Abstract: Yttrium aluminum garnet (YAG, Y{sub 3}Al{sub 5}O{sub 12}) and yttrium aluminum garnet doped with neodymium (Nd:YAG) single crystals were grown by the Czochralski technique. Themore » critical diameter and the critical rate of rotation were calculated. Suitable polishing and etching solutions were determined. As a result of our experiments, the transparent YAG and pale pink Nd:YAG single crystals were produced. The obtained crystals were studied by X-ray diffraction, Raman and IR spectroscopy. The crystal structure was confirmed by XRD. The 15 Raman and 17 IR modes were observed. The Raman and IR spectroscopy results are in accordance with X-ray diffraction analysis. The obtained YAG and Nd:YAG single crystals were without core and of good optical quality. The absence of a core was confirmed by viewing polished crystal slices. Also, it is important to emphasize that the obtained Nd:YAG single crystal has a concentration of 0.8 wt.% Nd{sup 3+} that is characteristic for laser materials.« less

Design and fabrication of a variable optical attenuator based on polymer-dispersed liquid crystal

NASA Astrophysics Data System (ADS)

She, Jun; Xu, Su; Tao, Tao; Wang, Qian

2005-02-01

In order to obtain a low polarization dependent loss (PDL) and a large attenuation range simultaneously, an optimal design and fabrication of a polymer-dispersed liquid crystal (PDLC) based variable optical attenuator (VOA) is presented. First, an optimal diameter of the liquid crystal droplets is determined by the anomalous diffraction approach (ADA). This optimal diameter gives maximal scattering and thus a large attenuation range is achieved with a relatively thin liquid crystal cell. Secondly, the fabrication of PDLC cell is carried out. The influence of the ultraviolet (UV) curing condition on the morphology of the LC droplets is investigated. For a given liquid crystal concentration, the optimal UV curing power is obtained after a series of statistically designed experiments. Finally, an optical configuration of the PDLC based VOA is presented. Measurements of the attenuation and the PDL are carried out with this configuration. The measured results show that the device has a typical attenuation range of 25dB. The corresponding PDL is nearly 1dB and the insertion loss is 1.8dB. The threshold voltage is 8Vrms and the saturation voltage is 40Vrms. From these measured results, one can see that the fabricated VOA based on PDLC is much more practical for optical communications as compared to the existing ones.

Synthesis of hexavalent molybdenum formo- and aceto-hydroxamates and deferoxamine via liquid-liquid metal partitioning

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

Breshears, Andrew T.; Brown, M. Alex; Bloom, Ira

We report a new method of crystal growth and synthesis based on liquid-liquid partitioning that allows for isolation and in-depth characterization of molybdenyl bis(formohydroxamate), Mo-FHA, molybdenyl bis(acetohydroxamate), Mo-AHA, and molybdenyl deferoxamine, Mo-DFO, for the first time. This novel approach affords shorter crystal growth time (hourly timeframe) without sacrificing crystal size or integrity when other methods of crystallization were unsuccessful. All three Mo complexes are characterized in solution via FTIR, NMR, UV-vis, and EXAFS spectroscopy. Mo-AHA and Mo-FHA structures are resolved by single crystal X-ray diffraction. Using the molybdenyl hydroxamate structural information, the speciation of Mo in a siderophore complex (Mo-DFO)more » is determined via complimentary spectroscopic methods and confirmed by DFT calculations. ESI-MS verifies that a complex of 1:1 molybdenum to deferoxamine is present in solution. Additionally, the Mo solution speciation in the precursor organic phase, MoO2(NO3)2HEH[EHP]2 (where HEH[EHP] is 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester), is characterized by FTIR and EXAFS spectroscopy as well as DFT calculations.« less

Three-dimensional reconstruction of the size and shape of protein microcrystals using Bragg coherent diffractive imaging

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

Coughlan, H. D.; Darmanin, C.; Kirkwood, H. J.

2016-03-14

Three-dimensional imaging of protein crystals during X-ray diffraction experiments opens up a range of possibilities for optimising crystal quality and gaining new insights into the fundamental processes that drive radiation damage. Obtaining this information at the appropriate lengthscales however is extremely challenging. One approach that has been recently demonstrated as a promising avenue for charactering the size and shape of protein crystals at nanometre lengthscales is Bragg Coherent Diffractive Imaging (BCDI). BCDI is a recently developed technique that is able to recover the phase of the continuous diffraction intensity signal around individual Bragg peaks. When data is collected at multiplemore » points on a rocking curve a Reciprocal Space Map (RSM) can be assembled and then inverted using BCDI to obtain a three-dimensional image of the crystal. The first demonstration of two-dimensional BCDI of protein crystals was reported by Boutet at al., recently this work was extended to the study of radiation damage of micron-sized crystals. Here we present the first three-dimensional reconstructions of a Lysozyme protein crystal using BDI. The results are validated against RSM and TEM data and have implications for both radiation damage studies and for developing new approaches to structure retrieval from micron-sized protein crystals.« less

Spatial resolution limitation of liquid crystal spatial light modulator

NASA Astrophysics Data System (ADS)

Wang, Xinghua; Wang, Bin; McManamon, Paul F., III; Pouch, John J.; Miranda, Felix A.; Anderson, James E.; Bos, Philip J.

2004-10-01

The effect of fringing electric fields in a liquid crystal (LC) Optical Phased Array (OPA), also referred to as a spatial light modulator (SLM), is a governing factor that determines the diffraction efficiency (DE) of the LC OPA for high resolution spatial phase modulation. In this article, the fringing field effect in a high resolution LC OPA is studied by accurate modeling the DE of the LC blazed gratings by LC director simulation and Finite Difference Time Domain (FDTD) simulation. Influence factors that contribute significantly to the DE are discussed. Such results provide fundamental understanding for high resolution LC devices.

Transmission electron microscopy as a tool for nanocrystal characterization pre- and post-injector

PubMed Central

Stevenson, H. P.; DePonte, D. P.; Makhov, A. M.; Conway, James F.; Zeldin, O. B.; Boutet, S.; Calero, G.; Cohen, A. E.

2014-01-01

Recent advancements at the Linac Coherent Light Source X-ray free-electron laser (XFEL) enabling successful serial femtosecond diffraction experiments using nanometre-sized crystals (NCs) have opened up the possibility of X-ray structure determination of proteins that produce only submicrometre crystals such as many membrane proteins. Careful crystal pre-characterization including compatibility testing of the sample delivery method is essential to ensure efficient use of the limited beamtime available at XFEL sources. This work demonstrates the utility of transmission electron microscopy for detecting and evaluating NCs within the carrier solutions of liquid injectors. The diffraction quality of these crystals may be assessed by examining the crystal lattice and by calculating the fast Fourier transform of the image. Injector reservoir solutions, as well as solutions collected post-injection, were evaluated for three types of protein NCs (i) the membrane protein PTHR1, (ii) the multi-protein complex Pol II-GFP and (iii) the soluble protein lysozyme. Our results indicate that the concentration and diffraction quality of NCs, particularly those with high solvent content and sensitivity to mechanical manipulation may be affected by the delivery process. PMID:24914151

A coronagraph based on two spatial light modulators for active amplitude apodizing and phase corrections

NASA Astrophysics Data System (ADS)

Dou, Jiangpei; Ren, Deqing; Zhang, Xi; Zhu, Yongtian; Zhao, Gang; Wu, Zhen; Chen, Rui; Liu, Chengchao; Yang, Feng; Yang, Chao

2014-08-01

Almost all high-contrast imaging coronagraphs proposed until now are based on passive coronagraph optical components. Recently, Ren and Zhu proposed for the first time a coronagraph that integrates a liquid crystal array (LCA) for the active pupil apodizing and a deformable mirror (DM) for the phase corrections. Here, for demonstration purpose, we present the initial test result of a coronagraphic system that is based on two liquid crystal spatial light modulators (SLM). In the system, one SLM is served as active pupil apodizing and amplitude correction to suppress the diffraction light; another SLM is used to correct the speckle noise that is caused by the wave-front distortions. In this way, both amplitude and phase error can be actively and efficiently compensated. In the test, we use the stochastic parallel gradient descent (SPGD) algorithm to control two SLMs, which is based on the point spread function (PSF) sensing and evaluation and optimized for a maximum contrast in the discovery area. Finally, it has demonstrated a contrast of 10-6 at an inner working angular distance of ~6.2 λ/D, which is a promising technique to be used for the direct imaging of young exoplanets on ground-based telescopes.

Investigation of the thermal and optical performance of a spatial light modulator with high average power picosecond laser exposure for materials processing applications

NASA Astrophysics Data System (ADS)

Zhu, G.; Whitehead, D.; Perrie, W.; Allegre, O. J.; Olle, V.; Li, Q.; Tang, Y.; Dawson, K.; Jin, Y.; Edwardson, S. P.; Li, L.; Dearden, G.

2018-03-01

Spatial light modulators (SLMs) addressed with computer generated holograms (CGHs) can create structured light fields on demand when an incident laser beam is diffracted by a phase CGH. The power handling limitations of these devices based on a liquid crystal layer has always been of some concern. With careful engineering of chip thermal management, we report the detailed optical phase and temperature response of a liquid cooled SLM exposed to picosecond laser powers up to 〈P〉  =  220 W at 1064 nm. This information is critical for determining device performance at high laser powers. SLM chip temperature rose linearly with incident laser exposure, increasing by only 5 °C at 〈P〉  =  220 W incident power, measured with a thermal imaging camera. Thermal response time with continuous exposure was 1-2 s. The optical phase response with incident power approaches 2π radians with average power up to 〈P〉  =  130 W, hence the operational limit, while above this power, liquid crystal thickness variations limit phase response to just over π radians. Modelling of the thermal and phase response with exposure is also presented, supporting experimental observations well. These remarkable performance characteristics show that liquid crystal based SLM technology is highly robust when efficiently cooled. High speed, multi-beam plasmonic surface micro-structuring at a rate R  =  8 cm2 s-1 is achieved on polished metal surfaces at 〈P〉  =  25 W exposure while diffractive, multi-beam surface ablation with average power 〈P〉  =100 W on stainless steel is demonstrated with ablation rate of ~4 mm3 min-1. However, above 130 W, first order diffraction efficiency drops significantly in accord with the observed operational limit. Continuous exposure for a period of 45 min at a laser power of 〈P〉  =  160 W did not result in any detectable drop in diffraction efficiency, confirmed afterwards by the efficient parallel beam processing at 〈P〉  =  100 W. Hence, no permanent changes in SLM phase response characteristics have been detected. This research work will help to accelerate the use of liquid crystal spatial light modulators for both scientific and ultra high throughput laser-materials micro-structuring applications.

Method of forming calthrate ice

DOEpatents

Hino, T.; Gorski, A.J.

1985-09-30

A method of forming clathrate ice in a supercooled water-based liquid contained in a vessel is disclosed. Initially, an oscillator device is located in the liquid in the vessel. The oscillator device is then oscillated ultransonically so that small crystals are formed in the liquid. Thes small crystals serve as seed crystals for ice formation in the liquid and thereby prevent supercooling of the liquid. Preferably, the oscillating device is controlled by a thermostat which initiates operation of the oscillator device when the temperature of the liquid is lowered to the freezing point. Thereafter, the operation of the oscillator device is terminated when ice is sensed in the liquid by an ice sensor.

Method of forming clathrate ice

DOEpatents

Hino, Toshiyuki; Gorski, Anthony J.

1987-01-01

A method of forming clathrate ice in a supercooled water-based liquid contained in a vessel is disclosed. Initially, an oscillator device is located in the liquid in the vessel. The oscillator device is then oscillated ultrasonically so that small crystals are formed in the liquid. These small crystals serve as seed crystals for ice formation in the liquid and thereby prevent supercooling of the liquid. Preferably, the oscillating device is controlled by a thermostat which initiates operation of the oscillator device when the temperature of the liquid is lowered to the freezing point. Thereafter, the operation of the oscillator device is terminated when ice is sensed in the liquid by an ice sensor.

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

Solvent screening for a hard-to-dissolve molecular crystal.

PubMed

Maiti, A; Pagoria, P F; Gash, A E; Han, T Y; Orme, C A; Gee, R H; Fried, L E

2008-09-01

Materials with a high-degree of inter- and intra-molecular hydrogen bonding generally have limited solubility in conventional organic solvents. This presents a problem for the dissolution, manipulation and purification of these materials. Using a state-of-the-art density-functional-theory based quantum chemical solvation model we systematically evaluated solvents for a known hydrogen-bonded molecular crystal. This, coupled with direct solubility measurements, uncovered a class of ionic liquids involving fluoride anions that possess more than two orders of magnitude higher solvation power as compared with the best conventional solvents. The crystal structure of one such ionic liquid, determined by X-ray diffraction spectroscopy, indicates that F- ions are stabilized through H-bonded chains with water. The presence of coordinating water in such ionic liquids seems to facilitate the dissolution process by keeping the chemical activity of the F- ions in check.

Crystallization in supercooled liquid Cu: Homogeneous nucleation and growth

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

E, J. C.; Key Laboratory of Advanced Technologies of Materials, Ministry of Education, Southwest Jiaotong University, Chengdu, Sichuan 610031; Wang, L.

2015-02-14

Homogeneous nucleation and growth during crystallization of supercooled liquid Cu are investigated with molecular dynamics simulations, and the microstructure is characterized with one- and two-dimensional x-ray diffraction. The resulting solids are single-crystal or nanocrystalline, containing various defects such as stacking faults, twins, fivefold twins, and grain boundaries; the microstructure is subject to thermal fluctuations and extent of supercooling. Fivefold twins form via sequential twinning from the solid-liquid interfaces. Critical nucleus size and nucleation rate at 31% supercooling are obtained from statistical runs with the mean first-passage time and survival probability methods, and are about 14 atoms and 10{sup 32} m{supmore » −3}s{sup −1}, respectively. The bulk growth dynamics are analyzed with the Johnson-Mehl-Avrami law and manifest three stages; the Avrami exponent varies in the range of 1–19, which also depends on thermal fluctuations and supercooling.« less

Comparing two tetraalkylammonium ionic liquids. II. Phase transitions.

PubMed

Lima, Thamires A; Paschoal, Vitor H; Faria, Luiz F O; Ribeiro, Mauro C C; Ferreira, Fabio F; Costa, Fanny N; Giles, Carlos

2016-06-14

Phase transitions of the ionic liquids n-butyl-trimethylammonium bis(trifluoromethanesulfonyl)imide, [N1114][NTf2], and methyl-tributylammonium bis(trifluoromethanesulfonyl)imide, [N1444][NTf2], were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) measurements, and Raman spectroscopy. XRD and Raman spectra were obtained as a function of temperature at atmospheric pressure, and also under high pressure at room temperature using a diamond anvil cell (DAC). [N1444][NTf2] experiences glass transition at low temperature, whereas [N1114][NTf2] crystallizes or not depending on the cooling rate. Both the ionic liquids exhibit glass transition under high pressure. XRD and low-frequency Raman spectra provide a consistent physical picture of structural ordering-disordering accompanying the thermal events of crystallization, glass transition, cold crystallization, pre-melting, and melting. Raman spectra in the high-frequency range of some specific cation and anion normal modes reveal conformational changes of the molecular structures along phase transitions.

Phase separations in mixtures of a liquid crystal and a nanocolloidal particle.

PubMed

Matsuyama, Akihiko

2009-11-28

We present a mean field theory to describe phase separations in mixtures of a liquid crystal and a nanocolloidal particle. By taking into account a nematic, a smectic A ordering of the liquid crystal, and a crystalline ordering of the nanoparticle, we calculate the phase diagrams on the temperature-concentration plane. We predict various phase separations, such as a smectic A-crystal phase separation and a smectic A-isotropic-crystal triple point, etc., depending on the interactions between the liquid crystal and the colloidal surface. Inside binodal curves, we find new unstable and metastable regions, which are important in the phase ordering dynamics. We also find a crystalline ordering of the nanoparticles dispersed in a smectic A phase and a nematic phase. The cooperative phenomena between liquid-crystalline ordering and crystalline ordering induce a variety of phase diagrams.

Liquid crystal true 3D displays for augmented reality applications

NASA Astrophysics Data System (ADS)

Li, Yan; Liu, Shuxin; Zhou, Pengcheng; Chen, Quanming; Su, Yikai

2018-02-01

Augmented reality (AR) technology, which integrates virtual computer-generated information into the real world scene, is believed to be the next-generation human-machine interface. However, most AR products adopt stereoscopic 3D display technique, which causes the accommodation-vergence conflict. To solve this problem, we have proposed two approaches. The first is a multi-planar volumetric display using fast switching polymer-stabilized liquid crystal (PSLC) films. By rapidly switching the films between scattering and transparent states while synchronizing with a high-speed projector, the 2D slices of a 3D volume could be displayed in time sequence. We delved into the research on developing high-performance PSLC films in both normal mode and reverse mode; moreover, we also realized the demonstration of four-depth AR images with correct accommodation cues. For the second approach, we realized a holographic AR display using digital blazed gratings and a 4f system to eliminate zero-order and higher-order noise. With a 4k liquid crystal on silicon device, we achieved a field of view (FOV) of 32 deg. Moreover, we designed a compact waveguidebased holographic 3D display. In the design, there are two holographic optical elements (HOEs), each of which functions as a diffractive grating and a Fresnel lens. Because of the grating effect, holographic 3D image light is coupled into and decoupled out of the waveguide by modifying incident angles. Because of the lens effect, the collimated zero order light is focused at a point, and got filtered out. The optical power of the second HOE also helps enlarge FOV.

Specific features of two diffraction schemes for a widely divergent X-ray beam

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

Avetyan, K. T.; Levonyan, L. V.; Semerjian, H. S.

2015-03-15

We investigated the specific features of two diffraction schemes for a widely divergent X-ray beam that use a circular diaphragm 30–50 μm in diameter as a point source of characteristic radiation. In one of the schemes, the diaphragm was set in front of the crystal (the diaphragm-crystal (d-c) scheme); in the other, it was installed behind the crystal (the crystal-diaphragm (c-d) scheme). It was established that the diffraction image in the c-d scheme is a topographic map of the investigated crystal area. In the d-c scheme at L = 2l (l and L are the distances between the crystal andmore » the diaphragm and between the photographic plate and the diaphragm, respectively), the branches of hyperbolas formed in this family of planes (hkl) by the characteristic K{sub α} and K{sub β} radiations, including higher order reflections, converge into one straight line. It is experimentally demonstrated that this convergence is very sensitive to structural inhomogeneities in the crystal under study.« less

Influence of the liquid crystal behaviour on the Langmuir and Langmuir-Blodgett film supramolecular architecture of an ionic liquid crystal.

PubMed

Pérez-Gregorio, Víctor; Giner, Ignacio; López, M Carmen; Gascón, Ignacio; Cavero, Emma; Giménez, Raquel

2012-06-01

A new luminescent ionic liquid crystal, called Ipz-2, has been synthesised and its mesophase behaviour and also at the air-liquid interface has been studied and compared with Ipz, another ionic pyrazole derivative, with a similar molecular structure, previously studied. The X-ray diffraction pattern shows that Ipz-2 exhibits hexagonal columnar mesomorphism, while Ipz adopts lamellar mesophases. Langmuir films of both compounds are flat and homogeneous at large areas per molecule, but create different supramolecular structures under further compression. Ipz-2 Langmuir films have been transferred onto solid substrates, and Atomic Force Microscopy (AFM) images of the Langmuir-Blodgett films have shown that large columnar structures hundreds of nm in diameter are formed on top of the initial monolayer, in contrast with well-defined trilayer LB films obtained for Ipz. Our results show that Ipz-2 has a tendency to stack in columnar arrangements both in liquid crystalline bulk and in Langmuir and Langmuir-Blodgett films. Copyright © 2012 Elsevier Inc. All rights reserved.

Purification and crystallization of the ABC-type transport substrate-binding protein OppA from Thermoanaerobacter tengcongensis

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

Gao, Jinlan; Li, Xiaolu; Tsinghua-Peking Joint Center for Life Sciences, Center for Structural Biology, School of Life Sciences, Tsinghua University, Beijing 100084, People's Republic of China

2012-06-22

Highlights: Black-Right-Pointing-Pointer We truncated the signal peptide of OppA{sub TTE0054} to make it express in Escherichia coli as a soluble protein. Black-Right-Pointing-Pointer Crystals of OppA{sub TTE0054} were grown by sitting-drop vapor diffusion method. Black-Right-Pointing-Pointer The crystal of OppA{sub TTE0054} diffracted to 2.25 A. -- Abstract: Di- and oligopeptide- binding protein OppAs play important roles in solute and nutrient uptake, sporulation, biofilm formation, cell wall muropeptides recycling, peptide-dependent quorum-sensing responses, adherence to host cells, and a variety of other biological processes. Soluble OppA from Thermoanaerobacter tengcongensis was expressed in Escherichia coli. The protein was found to be >95% pure with SDS-PAGEmore » after a series of purification steps and the purity was further verified by mass spectrometry. The protein was crystallized using the sitting-drop vapour-diffusion method with PEG 400 as the precipitant. Crystal diffraction extended to 2.25 A. The crystal belonged to space group C222{sub 1}, with unit-cell parameters of a = 69.395, b = 199.572, c = 131.673 A, and {alpha} = {beta} = {gamma} = 90 Degree-Sign .« less

The molecular and crystal structure of dextrans: a combined electron and X-ray diffraction study. II. A low temperature, hydrated polymorph.

PubMed

Guizard, C; Chanzy, H; Sarko, A

1985-06-05

The crystal and molecular structure of a dextran hydrate has been determined through combined electron and X-ray diffraction analysis, aided by stereochemical model refinement. A total of 65 hk0 electron diffraction intensities were measured on frozen single crystals held at the temperature of liquid nitrogen, to a resolution limit of 1.6 A. The X-ray intensities were measured from powder patterns recorded from collections of the single crystals. The structure crystallizes in a monoclinic unit cell with parameters a = 25.71 A, b = 10.21 A, c (chain axis) = 7.76 A and beta = 91.3 degrees. The space group is P2(1) with b axis unique. The unit cell contains six chains and eight water molecules, with three chains of the same polarity and four water molecules constituting the asymmetric unit. Along the chain direction the asymmetric unit is a dimer residue; however, the individual glucopyranose residues are very nearly related by a molecular 2-fold screw axis. The conformation of the chain is very similar to that in the anhydrous structure, but the chain packing differs in the two structures in that the rotational positions of the chains about the helix axes (the chain setting angles) are considerably different. The chains still pack in the form of sheets that are separated by water molecules. The difference in the chain setting angles between the anhydrous and hydrate structures corresponds to the angle between like unit cell axes observed in the diffraction diagrams recorded from hybrid crystals containing both polymorphs. Despite some beam damage effects, the structure was determined to a satisfactory degree of agreement, with the residuals R''(electron diffraction) = 0.258 and R(X-ray) = 0.127.

Aperiodic crystals and beyond.

PubMed

Grimm, Uwe

2015-06-01

Crystals are paradigms of ordered structures. While order was once seen as synonymous with lattice periodic arrangements, the discoveries of incommensurate crystals and quasicrystals led to a more general perception of crystalline order, encompassing both periodic and aperiodic crystals. The current definition of crystals rests on their essentially point-like diffraction. Considering a number of recently investigated toy systems, with particular emphasis on non-crystalline ordered structures, the limits of the current definition are explored.

Soft X-Ray Diffraction Microscopy of a Frozen Hydrated Yeast Cell

DOE PAGES

Huang, Xiaojing; Nelson, Johanna; Kirz, Janos; ...

2009-11-01

We report the first image of an intact, frozen hydrated eukaryotic cell using x-ray diffraction microscopy, or coherent x-ray diffraction imaging. By plunge freezing the specimen in liquid ethane and maintaining it below -170 °C, artifacts due to dehydration, ice crystallization, and radiation damage are greatly reduced. In this example, coherent diffraction data using 520 eV x rays were recorded and reconstructed to reveal a budding yeast cell at a resolution better than 25 nm. This demonstration represents an important step towards high resolution imaging of cells in their natural, hydrated state, without limitations imposed by x-ray optics.

Hydrogen bonds in concreto and in computro

NASA Astrophysics Data System (ADS)

Stouten, Pieter F. W.; Kroon, Jan

1988-07-01

Molecular dynamics simulations of liquid water and liquid methanol have been carried out. For both liquids an effective pair potential was used. The models were fitted to the heat of vaporization, pressure and various radial distribution functions resulting from diffraction experiments on liquids. In both simulations 216 molecules were put in a cubic periodical ☐. The system was loosely coupled to a temperature bath and to a pressure bath. Following an initial equilibration period relevant data were sampled during 15 ps. The distributions of oxygen—oxygen distances in hydrogen bonds obtained from the two simulations are essentially the same. The distribution obtained from crystal data is somewhat different: the maximum has about the same position, but the curve is much narrower, which can be expected merely from the fact that diffraction experiments only supply average atomic positions and hence average interatomic distances. When thermal motion is taken into account a closer likeness is observed.

Melt growth of organic 4-(2-Phenylisopropyl) phenol single crystal and its structural, thermal, dielectric permittivity and optical properties

NASA Astrophysics Data System (ADS)

Sadhasivam, S.; Rajesh, N. P.

2017-12-01

A nonlinear optical (NLO) organic crystal 4-(2-Phenylisopropyl) phenol has been grown by a top seeded melt growth technique. The melt growth kinetics of solid-liquid (molten) interface and facets formation in melt growth were studied. The melt grown crystal has the (001), (00 1 bar),(110)(1 bar 1 bar 0) ,(1 bar 20),(1 2 bar 0),(2 bar 10) and(2 1 bar 0) different morphological face. The morphological characteristics of melt grown crystal helps to better infer the kinetic influence of melt and hone growth of organic material. The rhombohedral lattice cell parameters were measured by single crystal X-ray diffraction. 4-(2-Phenylisopropyl) phenol crystallizes in space group of R 3 bar . Thermal study shows that solid to liquid transition occurring at 350 K and decomposes at 597 K. The grown crystal was optically transparent in the wavelength range of 300-1100 nm. The low dielectric constant (9-11) was measured in the [001] of 4-(2-Phenylisopropyl) phenol crystal.

Liquid crystal devices based on photoalignment and photopatterning materials

NASA Astrophysics Data System (ADS)

Chigrinov, Vladimir

2014-02-01

Liquid crystal (LC) display and photonics devices based on photo-alignment and photo-patterning LC cells are developed. A fast switchable grating based on ferroelectric liquid crystals and orthogonal planar alignment by means of photo alignments. Both 1D and 2D gratings have been constructed. The proposed diffracting element provides fast response time of around 20 μs, contrast of 7000:1 and high diffraction efficiency, at the electric field of 6V/μm. A switchable LC Fresnel zone lens was also developed with the efficiency of ~42% that can be further improved, and the switching time for the 3 μm thick cell is ~6.7 ms which is relatively fast in comparison of existing devices. Thus, because of the photoalignment technology the fabrication of Fresnel lens became considerably simpler than others. A thin high spatial resolution, photo-patterned micropolarizer array for complementary metal-oxide-semiconductor (CMOS) image sensors was implemented for the complete optical visualization of so called "invisible" objects, which are completely transparent (reflective) and colorless. Four Stokes parameters, which fully characterized the reflected light beam can be simultaneously detected using the array of photo-patterned polarizers on CMOS sensor plate. The cheap, high resolution photo-patterned LC matrix sensor was developed to be able successfully compete with the expensive and low reliable wire grid polarizer patterned arrays currently used for the purpose.

Amplification of interference color by using liquid crystal for protein detection

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

Zhu, Qingdi; Yang, Kun-Lin, E-mail: cheyk@nus.edu.sg

Micrometer-sized, periodic protein lines printed on a solid surface cause interference color which is invisible to the naked eye. However, the interference color can be amplified by using a thin layer of liquid crystal (LC) covered on the surface to form a phase diffraction grating. Strong interference color can thus be observed under ambient light. By using the LC-amplified interference color, we demonstrate naked-eye detection of a model protein—immunoglobulin G (IgG). Limit of detection can reach 20 μg/ml of IgG without using any instrumentation. This detection method is potentially useful for the development of low-cost and portable biosensors.

Determination of the absolute chirality of tellurium using resonant diffraction with circularly polarized x-rays.

PubMed

Tanaka, Y; Collins, S P; Lovesey, S W; Matsumami, M; Moriwaki, T; Shin, S

2010-03-31

Many proteins, sugars and pharmaceuticals crystallize into two forms that are mirror images of each other (enantiomers) like our right and left hands. Tellurium is one enantiomer having a space group pair, P3(1)21 (right-handed screw) and P3(2)21 (left-handed screw). X-ray diffraction with dispersion correction terms has been playing an important role in determining the handedness of enantiomers for a long time. However, this approach is not applicable for an elemental crystal such as tellurium or selenium. We have demonstrated that positive and negative circularly polarized x-rays at the resonant energy of tellurium can be used to absolutely distinguish right from left tellurium. This method is applicable to chiral motifs that occur in biomolecules, liquid crystals, ferroelectrics and antiferroelectrics, multiferroics, etc.

Freezing, melting and structure of ice in a hydrophilic nanopore.

PubMed

Moore, Emily B; de la Llave, Ezequiel; Welke, Kai; Scherlis, Damian A; Molinero, Valeria

2010-04-28

The nucleation, growth, structure and melting of ice in 3 nm diameter hydrophilic nanopores are studied through molecular dynamics simulations with the mW water model. The melting temperature of water in the pore was T(m)(pore) = 223 K, 51 K lower than the melting point of bulk water in the model and in excellent agreement with experimental determinations for 3 nm silica pores. Liquid and ice coexist in equilibrium at the melting point and down to temperatures as low as 180 K. Liquid water is located at the interface of the pore wall, increasing from one monolayer at the freezing temperature, T(f)(pore) = 195 K, to two monolayers a few degrees below T(m)(pore). Crystallization of ice in the pore occurs through homogeneous nucleation. At the freezing temperature, the critical nucleus contains approximately 75 to 100 molecules, with a radius of gyration similar to the radius of the pore. The critical nuclei contain features of both cubic and hexagonal ice, although stacking of hexagonal and cubic layers is not defined until the nuclei reach approximately 150 molecules. The structure of the confined ice is rich in stacking faults, in agreement with the interpretation of X-ray and neutron diffraction experiments. Though the presence of cubic layers is twice as prevalent as hexagonal ones, the crystals should not be considered defective Ic as sequences with more than three adjacent cubic (or hexagonal) layers are extremely rare in the confined ice.

Quantitative Interferometry in the Severe Acoustic Environment of Resonant Supersonic Jets

NASA Technical Reports Server (NTRS)

Mercer, Carolyn R.; Raman, Ganesh

1999-01-01

Understanding fundamental fluidic dynamic and acoustic processes in high-speed jets requires quantitative velocity, density and temperature measurements. In this paper we demonstrate a new, robust Liquid Crystal Point Diffraction Interferometer (LCPDI) that includes phase stepping and can provide accurate data even in the presence of intense acoustic fields. This novel common path interferometer (LCPDI) was developed to overcome difficulties with the Mach Zehnder interferometer in vibratory environments and is applied here to the case of a supersonic shock- containing jet. The environmentally insensitive LCPDI that is easy to align and capable of measuring optical wavefronts with high accuracy is briefly described, then integrated line of sight density data from the LCPDI for two underexpanded jets are presented.

Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

DOE PAGES

Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; ...

2015-06-27

Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here in this study, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallizationmore » conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.« less

Enhanced amplified spontaneous emission in a quantum dot-doped polymer-dispersed liquid crystal

NASA Astrophysics Data System (ADS)

Cao, Mingxuan; Zhang, Yating; Song, Xiaoxian; Che, Yongli; Zhang, Haiting; Yan, Chao; Dai, Haitao; Liu, Guang; Zhang, Guizhong; Yao, Jianquan

2016-07-01

Quantum dot-doped polymer-dispersed liquid crystals (QD-PDLCs) were prepared by photoinitiated polymerization and sealed in capillary tubes. The concentration of QDs in the PDLC was 1 wt%. Amplified spontaneous emission (ASE) of the quantum dot-doped polymer-dispersed liquid crystals was observed with 532 nm wavelength laser excitation. The threshold for ASE was 6 mJ cm-2, which is much lower than that for homogeneous quantum dot-doped polymer (25 mJ cm-2). The threshold for ASE was dramatically enhanced when the working temperature exceeded the clearing point of the liquid crystal; this result demonstrates that multi-scattering caused by the liquid crystals effectively improved the path length or dwell time of light in the gain region, which played a key role in decreasing the threshold for ASE.

Method for measuring surface shear stress magnitude and direction using liquid crystal coatings

NASA Technical Reports Server (NTRS)

Reda, Daniel C. (Inventor)

1995-01-01

A method is provided for determining surface shear magnitude and direction at every point on a surface. The surface is covered with a shear stress sensitive liquid crystal coating and illuminated by white light from a normal direction. A video camera is positioned at an oblique angle above the surface to observe the color of the liquid crystal at that angle. The shear magnitude and direction are derived from the color information. A method of calibrating the device is also provided.

A single-solenoid pulsed-magnet system for single-crystal scattering studies

NASA Astrophysics Data System (ADS)

Islam, Zahirul; Capatina, Dana; Ruff, Jacob P. C.; Das, Ritesh K.; Trakhtenberg, Emil; Nojiri, Hiroyuki; Narumi, Yasuo; Welp, Ulrich; Canfield, Paul C.

2012-03-01

We present a pulsed-magnet system that enables x-ray single-crystal diffraction in addition to powder and spectroscopic studies with the magnetic field applied on or close to the scattering plane. The apparatus consists of a single large-bore solenoid, cooled by liquid nitrogen. A second independent closed-cycle cryostat is used for cooling samples near liquid helium temperatures. Pulsed magnetic fields close to ˜30 T with a zero-to-peak-field rise time of ˜2.9 ms are generated by discharging a 40 kJ capacitor bank into the magnet coil. The unique characteristic of this instrument is the preservation of maximum scattering angle (˜23.6°) on the entrance and exit sides of the magnet bore by virtue of a novel double-funnel insert. This instrument will facilitate x-ray diffraction and spectroscopic studies that are impractical, if not impossible, to perform using split-pair and narrow-opening solenoid magnets. Furthermore, it offers a practical solution for preserving optical access in future higher-field pulsed magnets.

Holographic storage of three-dimensional image and data using photopolymer and polymer dispersed liquid crystal films

NASA Astrophysics Data System (ADS)

Gao, Hong-Yue; Liu, Pan; Zeng, Chao; Yao, Qiu-Xiang; Zheng, Zhiqiang; Liu, Jicheng; Zheng, Huadong; Yu, Ying-Jie; Zeng, Zhen-Xiang; Sun, Tao

2016-09-01

We present holographic storage of three-dimensional (3D) images and data in a photopolymer film without any applied electric field. Its absorption and diffraction efficiency are measured, and reflective analog hologram of real object and image of digital information are recorded in the films. The photopolymer is compared with polymer dispersed liquid crystals as holographic materials. Besides holographic diffraction efficiency of the former is little lower than that of the latter, this work demonstrates that the photopolymer is more suitable for analog hologram and big data permanent storage because of its high definition and no need of high voltage electric field. Therefore, our study proposes a potential holographic storage material to apply in large size static 3D holographic displays, including analog hologram displays, digital hologram prints, and holographic disks. Project supported by the National Natural Science Foundation of China (Grant Nos. 11474194, 11004037, and 61101176) and the Natural Science Foundation of Shanghai, China (Grant No. 14ZR1415500).

New Pyrazolium Salts as a Support for Ionic Liquid Crystals and Ionic Conductors.

PubMed

Pastor, María Jesús; Sánchez, Ignacio; Campo, José A; Schmidt, Rainer; Cano, Mercedes

2018-04-03

Ionic liquid crystals (ILCs) are a class of materials that combine the properties of liquid crystals (LCs) and ionic liquids (ILs). This type of materials is directed towards properties such as conductivity in ordered systems at different temperatures. In this work, we synthesize five new families of ILCs containing symmetrical and unsymmetrical substituted pyrazolium cations, with different alkyl long-chains, and anions such as Cl - , BF₄ - , ReO₄ - , p -CH₃-₆H₄SO₃ - (PTS) and CF₃SO₃ - (OTf). We study their thermal behavior by polarized light optical microscopy (POM) and differential scanning calorimetry (DSC). All of them, except those with OTf as counteranion, show thermotropic mesomorphism. The observations by POM reveal textures of lamellar mesophases. Those agree with the arrangement observed in the X-ray crystal structure of [H₂pz R(4),R(4) ][ReO₄]. The nature of the mesophases is also confirmed by variable temperature powder X-ray diffraction. On the other hand, the study of the dielectric properties at variable temperature in mesomorphic (Cl - and BF₄ - ) and non-mesomorphic (OTf) salts indicates that the supramolecular arrangement of the mesophase favors a greater ionic mobility and therefore ionic conductivity.

Effect of binder liquid type on spherical crystallization.

PubMed

Maghsoodi, Maryam; Hajipour, Ali

2014-11-01

Spherical crystallization is a process of formation of agglomerates of crystals held together by binder liquid. This research focused on understanding the effect of type of solvents used as binder liquid on the agglomeration of crystals. Carbamazepine and ethanol/water were used respectively as a model drug and crystallization system. Eight solvents as binder liquid including chloroform, dichloromethane, isopropyl acetate, ethyl acetate, n-hexane, dimethyl aniline, benzene and toluene were examined to better understand the relationship between the physical properties of the binder liquid and its ability to bring about the formation of the agglomerates. Moreover, the agglomerates obtained from effective solvents as binder liquid were evaluated in term of size, apparent particle density and compressive strength. In this study the clear trend was observed experimentally in the agglomerate formation as a function of physical properties of the binder liquid such as miscibility with crystallization system. Furthermore, the properties of obtained agglomerates such as size, apparent particle density and compressive strength were directly related to physical properties of effective binder liquids. RESULTS of this study offer a useful starting point for a conceptual framework to guide the selection of solvent systems for spherical crystallization.

Crystal defects in solar cells produced by the method of thermomigration

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

Lozovskii, V. N.; Lomov, A. A.; Lunin, L. S.

2017-03-15

The results of studying the crystal structure of regions in silicon, recrystallized during the course of thermomigration of the liquid Si–Al zone in the volume of the silicon substrate, are reported (similar regions doped with an acceptor impurity are used to obtain high-voltage solar cells). X-ray methods (including measurements of both diffraction-reflection curves and topograms) and also high-resolution electron microscopy indicate that single-crystal regions in the form of a series of thin strips or rectangular grids are formed as a result of the thermomigration of liquid zones. Dislocation half-loops are detected in the surface layers of the front and backmore » surfaces of the substrate. (311)-type defects are observed in the recrystallized regions.« less

Nucleation and Convection Effects in Protein Crystal Growth

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1997-01-01

Work during the second year under this grant (NAG8-1161) resulted in several major achievements. We have characterized protein impurities as well as microheterogeneities in the proteins hen egg white lysozyme and horse spleen apoferritin, and demonstrated the effects of these impurities on nucleation and crystallization. In particular, the purification of apoferritin resulted in crystals with an X-ray diffraction resolution of better than 1.8 A, i.e. a 1 A improvement over earlier work on the cubic form. Furthermore, we have shown, in association with studies of liquid-liquid phase separation, that depending on the growth conditions, lysozyme can produce all growth morphologies that have been observed with other proteins. Finally, in connection with our experimental and simulation work on growth step bunching, we have developed a system-dependent criterion for advantages and disadvantages of crystallization from solution under reduced gravity. In the following, these efforts are described in some detail.

Experiments with Cholesteric Liquid Crystals

ERIC Educational Resources Information Center

Fergason, James L.

1970-01-01

Describes laboratory experiments designed to demonstrate (1) the properties of cholesteric liquid crystals, (2) thermal mapping, (3) thermal diffusivity, (4) adiabatic expansion of rubber, and (5) measurement of radiated energy by a point source. Contains all of the information on materials and apparatus needed to perform the experiments.…

Tunable dichroic polarization beam splitter created by one-step holographic photoalignment using four-beam polarization interferometry

NASA Astrophysics Data System (ADS)

Kawai, Kotaro; Sakamoto, Moritsugu; Noda, Kohei; Sasaki, Tomoyuki; Kawatsuki, Nobuhiro; Ono, Hiroshi

2017-01-01

A tunable dichroic polarization beam splitter (tunable DPBS) simultaneously performs the follow functions: 1. Separation of a polarized incident beam into multiple pairs of orthogonally polarized beams; 2. Separation of the propagation direction of two wavelength incident beams after passing through the tunable DPBS; and 3. Control of both advanced polarization and wavelength separation capabilities by varying the temperature of the tunable DPBS. This novel complex optical property is realized by diffraction phenomena using a designed three-dimensional periodic structure of aligned liquid crystals in the tunable DPBS, which was fabricated quickly with precision in a one-step photoalignment using four-beam polarization interferometry. In experiments, we demonstrated that these diffraction properties are obtained by entering polarized beams of wavelengths 532 nm and 633 nm onto the tunable DPBS. These diffraction properties are described using the Jones calculus in a polarization propagation analysis. Of significance is that the aligned liquid crystal structure needed to obtain these diffraction properties was proposed based on a theoretical analysis, and these properties were then demonstrated experimentally. The tunable DPBS can perform several functions of a number of optical elements such as wave plates, polarization beam splitter, dichroic beam splitter, and tunable wavelength filter. Therefore, the tunable DPBS can contribute to greater miniaturization, sophistication, and cost reduction of optical systems used widely in applications, such as optical measurements, communications, and information processing.

Effect of erbium(III) oxide addition on thermal properties and crystallization behavior of some zinc-borate glasses

NASA Astrophysics Data System (ADS)

Borodi, G.; Bolundut, L. C.; Pascuta, P.

2017-12-01

The effect of replacing B2O3 with Er2O3 on the thermal properties and crystallization behaviour of B2O3-ZnO glasses were investigated by Differential Thermal Analysis (DTA) and X-ray Diffraction Analysis (XRD) measurements. DTA measurements reveal that the temperature of vitreous transition and the glass stability increase with the increasing in concentration the erbium ions added in the samples. The fragility index of the glasses increases also, when the dopant concentration from the studied samples increases. The glass was obtained from kinetically strong-glass-forming liquid (KS type glass). The most stable sample from the thermal point of view seems to be the sample that contains 10 mol% of Er2O3. The XRD patterns of the heat-treated samples at 860°C show new crystalline phases that contain erbium when the concentration of Er2O3 in the samples is higher than 3 mol%.

Lab-on-a-Chip Based Protein Crystallization

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark J.; Brasseur, Michael M.; Spearing, Scott F.; Whitaker, Ann F. (Technical Monitor)

2001-01-01

We are developing a novel technique with which we will grow protein crystals in very small volumes, utilizing chip-based, microfluidic ("LabChip") technology. This development, which is a collaborative effort between NASA's Marshall Space Flight Center and Caliper Technologies Corporation, promises a breakthrough in the field of protein crystal growth. Our initial results obtained from two model proteins, Lysozyme and Thaumatin, show that it is feasible to dispense and adequately mix protein and precipitant solutions on a nano-liter scale. The mixtures have shown crystal growth in volumes in the range of 10 nanoliters to 5 microliters. In addition, large diffraction quality crystals were obtained by this method. X-ray data from these crystals were shown to be of excellent quality. Our future efforts will include the further development of protein crystal growth with LabChip(trademark) technology for more complex systems. We will initially address the batch growth method, followed by the vapor diffusion method and the liquid-liquid diffusion method. The culmination of these chip developments is to lead to an on orbit protein crystallization facility on the International Space Station. Structural biologists will be invited to utilize the on orbit Iterative Biological Crystallization facility to grow high quality macromolecular crystals in microgravity.

Advection of nematic liquid crystals by chaotic flow

NASA Astrophysics Data System (ADS)

O'Náraigh, Lennon

2017-04-01

Consideration is given to the effects of inhomogeneous shear flow (both regular and chaotic) on nematic liquid crystals in a planar geometry. The Landau-de Gennes equation coupled to an externally prescribed flow field is the basis for the study: this is solved numerically in a periodic spatial domain. The focus is on a limiting case where the advection is passive, such that variations in the liquid-crystal properties do not feed back into the equation for the fluid velocity. The main tool for analyzing the results (both with and without flow) is the identification of the fixed points of the dynamical equations without flow, which are relevant (to varying degrees) when flow is introduced. The fixed points are classified as stable/unstable and further as either uniaxial or biaxial. Various models of passive shear flow are investigated. When tumbling is present, the flow is shown to have a strong effect on the liquid-crystal morphology; however, the main focus herein is on the case without tumbling. Accordingly, the main result of the work is that only the biaxial fixed point survives as a solution of the Q-tensor dynamics under the imposition of a general flow field. This is because the Q-tensor experiences not only transport due to advection but also co-rotation relative to the local vorticity field. A second result is that all families of fixed points survive for certain specific velocity fields, which we classify. We single out for close study those velocity fields for which the influence of co-rotation effectively vanishes along the Lagrangian trajectories of the imposed velocity field. In this scenario, the system exhibits coarsening arrest, whereby the liquid-crystal domains are "frozen in" to the flow structures, and the growth in their size is thus limited.

Thermally induced lamellar reorganization and thickening in spherical poly (L-lactic acid) crystalsome

NASA Astrophysics Data System (ADS)

Staub, Mark; Qi, Hao; Li, Christopher

Understanding fundamental aspects of spherical crystals is important for a variety of applications such as encapsulation and drug delivery. The curved nature of these crystals gives rise to differences in key crystallographic concepts such as grain boundaries and defect formation when compared to flat crystals. This curved crystallography is difficult to study experimentally, especially at the nanoscale. Our group has recently shown how an oil in water miniemulsion can be used to direct the crystallization of poly (L-lactic acid) (PLLA) at a curved liquid/liquid interface. This produces nanosized, polymer single-crystal-like capsules termed crystalsomes with increased stability and mechanical properties compared with non-crystalline counterparts. This system will serve as our model for examining spherical crystallography. In this work, combined wide angle X-ray diffraction, Atomic force microscopy, and differential scanning calorimetry is employed to examine how the curved interface effects crystal thickening and reorganization compared to flat PLLA crystals. The influence of degree of curvature on these processes is also studied by examining crystalsomes with differing diameters.

In vacuo X-ray data collection from graphene-wrapped protein crystals.

PubMed

Warren, Anna J; Crawshaw, Adam D; Trincao, Jose; Aller, Pierre; Alcock, Simon; Nistea, Ioana; Salgado, Paula S; Evans, Gwyndaf

2015-10-01

The measurement of diffraction data from macromolecular crystal samples held in vacuo holds the promise of a very low X-ray background and zero absorption of incident and scattered beams, leading to better data and the potential for accessing very long X-ray wavelengths (>3 Å) for native sulfur phasing. Maintaining the hydration of protein crystals under vacuum is achieved by the use of liquid jets, as with serial data collection at free-electron lasers, or is side-stepped by cryocooling the samples, as implemented at new synchrotron beamlines. Graphene has been shown to protect crystals from dehydration by creating an extremely thin layer that is impermeable to any exchanges with the environment. Furthermore, owing to its hydrophobicity, most of the aqueous solution surrounding the crystal is excluded during sample preparation, thus eliminating most of the background caused by liquid. Here, it is shown that high-quality data can be recorded at room temperature from graphene-wrapped protein crystals in a rough vacuum. Furthermore, it was observed that graphene protects crystals exposed to different relative humidities and a chemically harsh environment.

Purification and crystal growth of NPB via imidazolium based ionic liquids

NASA Astrophysics Data System (ADS)

Oh, Yong-Taeg; Shin, Dong-Chan

2018-04-01

Here we report the production of high purity and crystallinity organic electronic material of NPB (N,N‧-Di-[(1-naphthyl)-N,N‧-diphenyl]-1,1‧-biphenyl-4,4‧-diamine (C44H32N2) through solution recrystallization within imidazolium based ionic liquids. When low purity NPB was recrystallized at 170 °C within C8MIM[TFSI], its purity was drastically improved from 82% to 99.92%. These recrystallized NPB crystals showed 0.040° FWHM (Full Width Half Maximum) of X-ray (1 1 1) diffraction peak. Such small FWHM angle indicates single-crystal like crystallinity. Initial NPB powder was dissolved at 100 °C and recrystallized at temperature above 110 °C. At higher temperature of 170 °C, a small number of bigger crystals were formed compared to those at 110 °C. This can be well explained by the classical nucleation and growth theory. Therefore, solution recrystallization process using ionic liquid might be promising for mass production of organic electronic materials by replacing the widely-used sublimation purification method.

Kinetics and equilibria of lysozyme precipitation and crystallization in concentrated ammonium sulfate solutions.

PubMed

Cheng, Yu-Chia; Lobo, Raul F; Sandler, Stanley I; Lenhoff, Abraham M

2006-05-05

The kinetics and thermodynamics of lysozyme precipitation in ammonium sulfate solutions at pH 4 and 8 and room temperature were studied. X-ray powder diffraction (XRD) was used to characterize the structure of lysozyme precipitates. It was found that, if sufficient time was allowed, microcrystals developed following an induction period after initial lysozyme precipitation, even up to ionic strengths of 8 m and at acidic pH, where lysozyme is refractory to crystallization in ammonium sulfate. The full set of precipitation and crystallization data allowed construction of a phase diagram of lysozyme, showing the ammonium sulfate dependence. It suggests that precipitation may reflect a frustrated metastable liquid-liquid phase separation, which would allow this process to be understood within the framework of the generic phase diagram for proteins. The results also demonstrate that XRD, more frequently used for characterizing inorganic and organic polycrystalline materials, is useful both in characterizing the presence of crystals in the dense phase and in verifying the crystal form of proteins.

Nematic Liquid-Crystal Colloids

PubMed Central

Muševič, Igor

2017-01-01

This article provides a concise review of a new state of colloidal matter called nematic liquid-crystal colloids. These colloids are obtained by dispersing microparticles of different shapes in a nematic liquid crystal that acts as a solvent for the dispersed particles. The microparticles induce a local deformation of the liquid crystal, which then generates topological defects and long-range forces between the neighboring particles. The colloidal forces in nematic colloids are much stronger than the forces in ordinary colloids in isotropic solvents, exceeding thousands of kBT per micrometer-sized particle. Of special interest are the topological defects in nematic colloids, which appear in many fascinating forms, such as singular points, closed loops, multitudes of interlinked and knotted loops or soliton-like structures. The richness of the topological phenomena and the possibility to design and control topological defects with laser tweezers make colloids in nematic liquid crystals an excellent playground for testing the basic theorems of topology. PMID:29295574

Liquid crystals of carbon nanotubes and graphene.

PubMed

Zakri, Cécile; Blanc, Christophe; Grelet, Eric; Zamora-Ledezma, Camilo; Puech, Nicolas; Anglaret, Eric; Poulin, Philippe

2013-04-13

Liquid crystal ordering is an opportunity to develop novel materials and applications with spontaneously aligned nanotubes or graphene particles. Nevertheless, achieving high orientational order parameter and large monodomains remains a challenge. In addition, our restricted knowledge of the structure of the currently available materials is a limitation for fundamental studies and future applications. This paper presents recent methodologies that have been developed to achieve large monodomains of nematic liquid crystals. These allow quantification and increase of their order parameters. Nematic ordering provides an efficient way to prepare conductive films that exhibit anisotropic properties. In particular, it is shown how the electrical conductivity anisotropy increases with the order parameter of the nematic liquid crystal. The order parameter can be tuned by controlling the length and entanglement of the nanotubes. In the second part of the paper, recent results on graphene liquid crystals are reported. The possibility to obtain water-based liquid crystals stabilized by surfactant molecules is demonstrated. Structural and thermodynamic characterizations provide indirect but statistical information on the dimensions of the graphene flakes. From a general point of view, this work presents experimental approaches to optimize the use of nanocarbons as liquid crystals and provides new methodologies for the still challenging characterization of such materials.

The putative liquid-liquid transition is a liquid-solid transition in atomistic models of water

NASA Astrophysics Data System (ADS)

Limmer, David T.; Chandler, David

2011-10-01

We use numerical simulation to examine the possibility of a reversible liquid-liquid transition in supercooled water and related systems. In particular, for two atomistic models of water, we have computed free energies as functions of multiple order parameters, where one is density and another distinguishes crystal from liquid. For a range of temperatures and pressures, separate free energy basins for liquid and crystal are found, conditions of phase coexistence between these phases are demonstrated, and time scales for equilibration are determined. We find that at no range of temperatures and pressures is there more than a single liquid basin, even at conditions where amorphous behavior is unstable with respect to the crystal. We find a similar result for a related model of silicon. This result excludes the possibility of the proposed liquid-liquid critical point for the models we have studied. Further, we argue that behaviors others have attributed to a liquid-liquid transition in water and related systems are in fact reflections of transitions between liquid and crystal.

Improved crystal orientation and physical properties from single-shot XFEL stills

DOE PAGES

Sauter, Nicholas K.; Hattne, Johan; Brewster, Aaron S.; ...

2014-11-28

X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factors from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model themore » diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg's law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographic R factors and sharpening anomalous differences that are near the level of the noise.« less

Improved crystal orientation and physical properties from single-shot XFEL stills

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

Sauter, Nicholas K.; Hattne, Johan; Brewster, Aaron S.

X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factors from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model themore » diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg's law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographic R factors and sharpening anomalous differences that are near the level of the noise.« less

Compression Freezing Kinetics of Water to Ice VII

DOE PAGES

Gleason, A. E.; Bolme, C. A.; Galtier, E.; ...

2017-07-11

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Compression Freezing Kinetics of Water to Ice VII

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

Gleason, A. E.; Bolme, C. A.; Galtier, E.

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

Comparing two tetraalkylammonium ionic liquids. II. Phase transitions

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

Lima, Thamires A.; Paschoal, Vitor H.; Faria, Luiz F. O.

Phase transitions of the ionic liquids n-butyl-trimethylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1114}][NTf{sub 2}], and methyl-tributylammonium bis(trifluoromethanesulfonyl)imide, [N{sub 1444}][NTf{sub 2}], were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) measurements, and Raman spectroscopy. XRD and Raman spectra were obtained as a function of temperature at atmospheric pressure, and also under high pressure at room temperature using a diamond anvil cell (DAC). [N{sub 1444}][NTf{sub 2}] experiences glass transition at low temperature, whereas [N{sub 1114}][NTf{sub 2}] crystallizes or not depending on the cooling rate. Both the ionic liquids exhibit glass transition under high pressure. XRD and low-frequency Raman spectra provide a consistent physical picturemore » of structural ordering-disordering accompanying the thermal events of crystallization, glass transition, cold crystallization, pre-melting, and melting. Raman spectra in the high-frequency range of some specific cation and anion normal modes reveal conformational changes of the molecular structures along phase transitions.« less

Ultraslow Phase Transitions in an Anion-Anion Hydrogen-Bonded Ionic Liquid.

PubMed

Faria, Luiz F O; Lima, Thamires A; Ferreira, Fabio F; Ribeiro, Mauro C C

2018-02-15

A Raman spectroscopy study of 1-ethyl-3-methylimidazolium hydrogen sulfate, [C 2 C 1 im][HSO 4 ], as a function of temperature, has been performed to reveal the role played by anion-anion hydrogen bond on the phase transitions of this ionic liquid. Anion-anion hydrogen bonding implies high viscosity, good glass-forming ability, and also moderate fragility of [C 2 C 1 im][HSO 4 ] in comparison with other ionic liquids. Heating [C 2 C 1 im][HSO 4 ] from the glassy phase results in cold crystallization at ∼245 K. A solid-solid transition (crystal I → crystal II) is barely discernible in calorimetric measurements at typical heating rates, but it is clearly revealed by Raman spectroscopy and X-ray diffraction. Raman spectroscopy indicates that crystal I has extended ([HSO 4 ] - ) n chains of hydrogen-bonded anions but crystal II has not. Raman spectra recorded at isothermal condition show the ultraslow dynamics of cold crystallization, solid-solid transition, and continuous melting of [C 2 C 1 im][HSO 4 ]. A brief comparison is also provided between [C 2 C 1 im][HSO 4 ] and [C 4 C 1 im][HSO 4 ], as Raman spectroscopy shows that the latter does not form the crystalline phase with extended anion-anion chains.

Holographic Gratings for Slow-Neutron Optics

PubMed Central

Klepp, Juergen; Pruner, Christian; Tomita, Yasuo; Geltenbort, Peter; Drevenšek-Olenik, Irena; Gyergyek, Saso; Kohlbrecher, Joachim; Fally, Martin

2012-01-01

Recent progress in the development of holographic gratings for neutron-optics applications is reviewed. We summarize the properties of gratings recorded in deuterated (poly)methylmethacrylate, holographic polymer-dispersed liquid crystals and nanoparticle-polymer composites revealed by diffraction experiments with slow neutrons. Existing and anticipated neutron-optical instrumentations based on holographic gratings are discussed.

Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature.

PubMed

Tsujino, Soichiro; Tomizaki, Takashi

2016-05-06

Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography.

Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature

NASA Astrophysics Data System (ADS)

Tsujino, Soichiro; Tomizaki, Takashi

2016-05-01

Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography.

Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature

PubMed Central

Tsujino, Soichiro; Tomizaki, Takashi

2016-01-01

Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography. PMID:27150272

Phase Adaptation and Correction by Adaptive Optics

NASA Astrophysics Data System (ADS)

Tiziani, Hans J.

2010-04-01

Adaptive optical elements and systems for imaging or laser beam propagation are used for some time in particular in astronomy, where the image quality is degraded by atmospheric turbulence. In astronomical telescopes a deformable mirror is frequently used to compensate wavefront-errors due to deformations of the large mirror, vibrations as well as turbulence and hence to increase the image quality. In the last few years interesting elements like Spatial Light Modulators, SLM's, such as photorefractive crystals, liquid crystals and micro mirrors and membrane mirrors were introduced. The development of liquid crystals and micro mirrors was driven by data projectors as consumer products. They contain typically a matrix of individually addressable pixels of liquid crystals and flip mirrors respectively or more recently piston mirrors for special applications. Pixel sizes are in the order of a few microns and therefore also appropriate as active diffractive elements in digital holography or miniature masks. Although liquid crystals are mainly optimized for intensity modulation; they can be used for phase modulation. Adaptive optics is a technology for beam shaping and wavefront adaptation. The application of spatial light modulators for wavefront adaptation and correction and defect analysis as well as sensing will be discussed. Dynamic digital holograms are generated with liquid crystal devices (LCD) and used for wavefront correction as well as for beam shaping and phase manipulation, for instance. Furthermore, adaptive optics is very useful to extend the measuring range of wavefront sensors and for the wavefront adaptation in order to measure and compare the shape of high precision aspherical surfaces.

Pressure-induced structural change in liquid GaIn eutectic alloy.

PubMed

Yu, Q; Ahmad, A S; Ståhl, K; Wang, X D; Su, Y; Glazyrin, K; Liermann, H P; Franz, H; Cao, Q P; Zhang, D X; Jiang, J Z

2017-04-25

Synchrotron x-ray diffraction reveals a pressure induced crystallization at about 3.4 GPa and a polymorphic transition near 10.3 GPa when compressed a liquid GaIn eutectic alloy up to ~13 GPa at room temperature in a diamond anvil cell. Upon decompression, the high pressure crystalline phase remains almost unchanged until it transforms to the liquid state at around 2.3 GPa. The ab initio molecular dynamics calculations can reproduce the low pressure crystallization and give some hints on the understanding of the transition between the liquid and the crystalline phase on the atomic level. The calculated pair correlation function g(r) shows a non-uniform contraction reflected by the different compressibility between the short (1st shell) and the intermediate (2nd to 4th shells). It is concluded that the pressure-induced liquid-crystalline phase transformation likely arises from the changes in local atomic packing of the nearest neighbors as well as electronic structures at the transition pressure.

Ice-Crystal Fallstreaks from Supercooled Liquid Water Parent Clouds

NASA Technical Reports Server (NTRS)

Campbell, James R.; O'C. Starr, David; Welton, Ellsworth J.; Spinhirne, James D.; Ferrare, Richard A.

2003-01-01

On 31 December 2001, ice-crystal fallstreaks (e.g., cirrus uncinus, or colloquially "Mare's Tails") from supercooled liquid water parent clouds were observed by ground-based lidars pointed vertically from the Atmospheric Radiation Measurement Southern Great Plains (SGP) facility near Lamont, Oklahoma. The incidence of liquid phase cloud with apparent ice-phase precipitation is investigated. Scenarios for mixed-phase particle nucleation, and fallstreak formation and sustenance are discussed. The observations are unique in the context of the historical reverence given to the commonly observed c h s uncinus fallstreak (wholly ice) versus this seemingly contradictory coincidence of liquid water begetting ice-crystal streaks.

Anisotropic Light Diffraction by Ultrasound in Crystals with Strong Acoustic Anisotropy

NASA Astrophysics Data System (ADS)

Voloshin, Andrey S.; Balakshy, Vladimir I.

In modern acousto-optics, crystalline materials are used predominantly for manufacturing acousto-optic instruments. Among these materials, such crystals as paratellurite, tellurium, calomel, TAS and some others occupy a prominent place, which are distinguished by exceptionally large anisotropy of acoustic properties. In this work, the influence of acoustic beam energy walk-off on characteristics of Bragg diffraction of light is studied by the example of tellurium crystal. It is shown that the walk-off can substantially change angular and frequency ranges, resulting in their narrowing or broadening subject to position of the operating point in the Bragg angle frequency characteristic. Coefficients of broadening are introduced for characterization of this effect.

X-ray shearing interferometer

DOEpatents

Koch, Jeffrey A [Livermore, CA

2003-07-08

An x-ray interferometer for analyzing high density plasmas and optically opaque materials includes a point-like x-ray source for providing a broadband x-ray source. The x-rays are directed through a target material and then are reflected by a high-quality ellipsoidally-bent imaging crystal to a diffraction grating disposed at 1.times. magnification. A spherically-bent imaging crystal is employed when the x-rays that are incident on the crystal surface are normal to that surface. The diffraction grating produces multiple beams which interfere with one another to produce an interference pattern which contains information about the target. A detector is disposed at the position of the image of the target produced by the interfering beams.

Creation of vector beams from a polarization diffraction grating using a programmable liquid crystal spatial light modulator and a q-plate

NASA Astrophysics Data System (ADS)

Badham, Katherine Emily

This thesis presents the ability of complete polarization control of light to create a polarization diffraction grating (PDG). This system has the ability to create diffracted light with each order having a separate high-order polarization state in one location on the optical axis. First, an external Excel program is used to create a grating phase profile from userspecified target diffraction orders. High-order vector beams in this PDG are created using a combination of two devices---a liquid crystal spatial light modulator (LC-SLM) manufactured by Seiko Epson, and a tunable q -plate from Citizen Holdings Co. The transmissive SLM is positioned in an optical setup with a reflective architecture allowing control over both the horizontal and vertical components of the laser beam. The SLM has its LC director oriented vertically only affecting the vertically polarized state, however, the optical setup allows modulation of both vertical and horizontal components by the use of a quarter-wave plate (QWP) and a mirror to rotate the polarizations 90 degrees. Each half of the SLM is encoded with an anisotropic phase-only diffraction grating which are superimposed to create a select number of orders with the desired polarization states and equally distributed intensity. The technique of polarimetry is used to confirm the polarization state of each diffraction order. The q-plate is an inhomogeneous birefringent waveplate which has the ability to convert zero-order vector beams into first-order vector beams. The physical placement of this device into the system converts the orders with zero-order polarization states to first-order polarization states. The light vector patterns of each diffraction order confirm which first-order polarization state of is produced. A specially made PDG sextuplicator is encoded onto the SLM to generate six diffraction orders with separate states of polarization.

In-situ study of crystallization kinetics in ternary bulk metallic glass alloys with different glass forming abilities

DOE PAGES

Lan, Si; Wei, Xiaoya; Zhou, Jie; ...

2014-11-18

In-situ transmission electron microcopy and time-resolved neutron diffraction were used to study crystallization kinetics of two ternary bulk metallic glasses during isothermal annealing in the supercooled liquid region. It is found that the crystallization of Zr 56Cu 36Al 8, an average glass former, follows continuous nucleation and growth, while that of Zr 46Cu 46Al 8, a better glass former, is characterized by site-saturated nucleation, followed by slow growth. Possible mechanisms for the observed differences and the relationship to the glass forming ability are discussed.

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Rotator Phases of n-Heptane under High Pressure: Raman Scattering and X-ray Diffraction Studies

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

C Ma; Q Zhou; F Li

2011-12-31

We performed high-pressure Raman scattering and angle-dispersive synchrotron X-ray diffraction measurements on n-heptane at room temperature. It has been found that n-heptane undergoes a liquid to rotator phase III (R{sub III}) transition at 1.2 GPa and then transforms into another rotator phase R{sub IV} at about 3 GPa. As the pressure reaches 7.5 GPa, a transition from an orientationally disordered R{sub IV} phase to an ordered crystalline state starts and is completed around 14.5 GPa. Our results clearly present the high-pressure phase transition sequence (liquid-R{sub III}-R{sub IV}-crystal) of n-heptane, similar to that of normal alkanes.

Three-dimensionally modulated anisotropic structure for diffractive optical elements created by one-step three-beam polarization holographic photoalignment

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

Kawai, Kotaro, E-mail: s135016@stn.nagaokaut.ac.jp; Sakamoto, Moritsugu; Noda, Kohei

2016-03-28

A diffractive optical element with a three-dimensional liquid crystal (LC) alignment structure for advanced control of polarized beams was fabricated by a highly efficient one-step photoalignment method. This study is of great significance because different two-dimensional continuous and complex alignment patterns can be produced on two alignment films by simultaneously irradiating an empty glass cell composed of two unaligned photocrosslinkable polymer LC films with three-beam polarized interference beam. The polarization azimuth, ellipticity, and rotation direction of the diffracted beams from the resultant LC grating widely varied depending on the two-dimensional diffracted position and the polarization states of the incident beams.more » These polarization diffraction properties are well explained by theoretical analysis based on Jones calculus.« less

New Pyrazolium Salts as a Support for Ionic Liquid Crystals and Ionic Conductors

PubMed Central

Pastor, María Jesús; Sánchez, Ignacio; Schmidt, Rainer; Cano, Mercedes

2018-01-01

Ionic liquid crystals (ILCs) are a class of materials that combine the properties of liquid crystals (LCs) and ionic liquids (ILs). This type of materials is directed towards properties such as conductivity in ordered systems at different temperatures. In this work, we synthesize five new families of ILCs containing symmetrical and unsymmetrical substituted pyrazolium cations, with different alkyl long-chains, and anions such as Cl−, BF4−, ReO4−, p-CH3-6H4SO3− (PTS) and CF3SO3− (OTf). We study their thermal behavior by polarized light optical microscopy (POM) and differential scanning calorimetry (DSC). All of them, except those with OTf as counteranion, show thermotropic mesomorphism. The observations by POM reveal textures of lamellar mesophases. Those agree with the arrangement observed in the X-ray crystal structure of [H2pzR(4),R(4)][ReO4]. The nature of the mesophases is also confirmed by variable temperature powder X-ray diffraction. On the other hand, the study of the dielectric properties at variable temperature in mesomorphic (Cl− and BF4−) and non-mesomorphic (OTf) salts indicates that the supramolecular arrangement of the mesophase favors a greater ionic mobility and therefore ionic conductivity. PMID:29614030

Preparation of Monodomain Liquid Crystal Elastomers and Liquid Crystal Elastomer Nanocomposites.

PubMed

Kim, Hojin; Zhu, Bohan; Chen, Huiying; Adetiba, Oluwatomiyin; Agrawal, Aditya; Ajayan, Pulickel; Jacot, Jeffrey G; Verduzco, Rafael

2016-02-06

LCEs are shape-responsive materials with fully reversible shape change and potential applications in medicine, tissue engineering, artificial muscles, and as soft robots. Here, we demonstrate the preparation of shape-responsive liquid crystal elastomers (LCEs) and LCE nanocomposites along with characterization of their shape-responsiveness, mechanical properties, and microstructure. Two types of LCEs - polysiloxane-based and epoxy-based - are synthesized, aligned, and characterized. Polysiloxane-based LCEs are prepared through two crosslinking steps, the second under an applied load, resulting in monodomain LCEs. Polysiloxane LCE nanocomposites are prepared through the addition of conductive carbon black nanoparticles, both throughout the bulk of the LCE and to the LCE surface. Epoxy-based LCEs are prepared through a reversible esterification reaction. Epoxy-based LCEs are aligned through the application of a uniaxial load at elevated (160 °C) temperatures. Aligned LCEs and LCE nanocomposites are characterized with respect to reversible strain, mechanical stiffness, and liquid crystal ordering using a combination of imaging, two-dimensional X-ray diffraction measurements, differential scanning calorimetry, and dynamic mechanical analysis. LCEs and LCE nanocomposites can be stimulated with heat and/or electrical potential to controllably generate strains in cell culture media, and we demonstrate the application of LCEs as shape-responsive substrates for cell culture using a custom-made apparatus.

Nonlinear-Optical Correction of Aberrations in Imaging Telescopes Based on a Diffraction Structure on the Primary Mirror

DTIC Science & Technology

1998-01-01

48 f) Metal and semiconductor thin- film systems ................ 48 3.3.2. Methods of formation of interference field for recording the hologram...in others - dynamic holograms [27,29,30,33] based either on photorefractive crystals [27,33], or on liquid -crystal spatial light modulators (SLM...variations of the primary mirror’s curvature, which can be caused, e.g., by thermal effects or by inaccuracy in adjustment of the elastic thin- film mirror

The growth of dislocation-free crystals of benzil

NASA Astrophysics Data System (ADS)

Katoh, K.; Kato, N.

1985-11-01

Dislocation-free crystals of benzil have been obtained by repeated Czochralski growth and have been characterized using X-ray diffraction topography. At each stage of growth, the parts containing the defects were etched off and the rest was used for the seed in the next growth. The growth behaviour could be interpreted in connection with the shape of the solid-liquid interface. The double image of the screw dislocation could be explained elementarily and it was concluded that the Burgers vector was c/3.

Large-size TlBr single crystal growth and defect study

NASA Astrophysics Data System (ADS)

Zhang, Mingzhi; Zheng, Zhiping; Chen, Zheng; Zhang, Sen; Luo, Wei; Fu, Qiuyun

2018-04-01

Thallium bromide (TlBr) is an attractive semiconductor material for fabrication of radiation detectors due to its high photon stopping power originating from its high atomic number, wide band gap and high resistivity. In this paper the vertical Bridgman method was used for crystal growth and TlBr single crystals with diameter of 15 mm were grown. X-ray diffraction (XRD) was used to identify phase and orientation. Electron backscatter diffraction (EBSD) was used to investigate crystal microstructure and crystallographic orientation. The optical and electric performance of the crystal was characterized by infrared (IR) transmittance spectra and I-V measurement. The types of point defects in the crystals were investigated by thermally stimulated current (TSC) spectra and positron annihilation spectroscopy (PAS). Four types of defects, with ionization energy of each defect fitting as follows: 0.1308, 0.1540, 0.3822 and 0.538 eV, were confirmed from the TSC result. The PAS result showed that there were Tl vacancies in the crystal.

Data collection strategies for time-resolved X-ray free-electron laser diffraction, and 2-color methods

PubMed Central

Li, Chufeng; Schmidt, Kevin; Spence, John C.

2015-01-01

We compare three schemes for time-resolved X-ray diffraction from protein nanocrystals using an X-ray free-electron laser. We find expressions for the errors in structure factor measurement using the Monte Carlo pump-probe method of data analysis with a liquid jet, the fixed sample pump-probe (goniometer) method (both diffract-and-destroy, and below the safe damage dose), and a proposed two-color method. Here, an optical pump pulse arrives between X-ray pulses of slightly different energies which hit the same nanocrystal, using a weak first X-ray pulse which does not damage the sample. (Radiation damage is outrun in the other cases.) This two-color method, in which separated Bragg spots are impressed on the same detector readout, eliminates stochastic fluctuations in crystal size, shape, and orientation and is found to require two orders of magnitude fewer diffraction patterns than the currently used Monte Carlo liquid jet method, for 1% accuracy. Expressions are given for errors in structure factor measurement for the four approaches, and detailed simulations provided for cathepsin B and IC3 crystals. While the error is independent of the number of shots for the dose-limited goniometer method, it falls off inversely as the square root of the number of shots for the two-color and Monte Carlo methods, with a much smaller pre-factor for the two-color mode, when the first shot is below the damage threshold. PMID:26798813

The Landau-de Gennes approach revisited: A minimal self-consistent microscopic theory for spatially inhomogeneous nematic liquid crystals

NASA Astrophysics Data System (ADS)

Gârlea, Ioana C.; Mulder, Bela M.

2017-12-01

We design a novel microscopic mean-field theory of inhomogeneous nematic liquid crystals formulated entirely in terms of the tensor order parameter field. It combines the virtues of the Landau-de Gennes approach in allowing both the direction and magnitude of the local order to vary, with a self-consistent treatment of the local free-energy valid beyond the small order parameter limit. As a proof of principle, we apply this theory to the well-studied problem of a colloid dispersed in a nematic liquid crystal by including a tunable wall coupling term. For the two-dimensional case, we investigate the organization of the liquid crystal and the position of the point defects as a function of the strength of the coupling constant.

Field lens multiplexing in holographic 3D displays by using Bragg diffraction based volume gratings

NASA Astrophysics Data System (ADS)

Fütterer, G.

2016-11-01

Applications, which can profit from holographic 3D displays, are the visualization of 3D data, computer-integrated manufacturing, 3D teleconferencing and mobile infotainment. However, one problem of holographic 3D displays, which are e.g. based on space bandwidth limited reconstruction of wave segments, is to realize a small form factor. Another problem is to provide a reasonable large volume for the user placement, which means to provide an acceptable freedom of movement. Both problems should be solved without decreasing the image quality of virtual and real object points, which are generated within the 3D display volume. A diffractive optical design using thick hologram gratings, which can be referred to as Bragg diffraction based volume gratings, can provide a small form factor and high definition natural viewing experience of 3D objects. A large collimated wave can be provided by an anamorphic backlight unit. The complex valued spatial light modulator add local curvatures to the wave field he is illuminated with. The modulated wave field is focused onto to the user plane by using a volume grating based field lens. Active type liquid crystal gratings provide 1D fine tracking of approximately +/- 8° deg. Diffractive multiplex has to be implemented for each color and for a set of focus functions providing coarse tracking. Boundary conditions of the diffractive multiplexing are explained. This is done in regards to the display layout and by using the coupled wave theory (CWT). Aspects of diffractive cross talk and its suppression will be discussed including longitudinal apodized volume gratings.

Theoretical model of a polarization diffractive elements for the light beams conversion holographic formation in PDLCs

NASA Astrophysics Data System (ADS)

Sharangovich, Sergey N.; Semkin, Artem O.

2017-12-01

In this work a theoretical model of the holographic formation of the polarization diffractive optical elements for the transformation of Gaussian light beams into Bessel-like ones in polymer-dispersed liquid crystals (PDLC) is developed. The model is based on solving the equations of photo-induced Fredericks transition processes for polarization diffractive elements formation by orthogonally polarized light beams with inhomogeneous amplitude and phase profiles. The results of numerical simulation of the material's dielectric tensor changing due to the structure's formation process are presented for various recording beams' polarization states. Based on the results of numerical simulation, the ability to form the diffractive optical elements for light beams transformation by the polarization holography methods is shown.

Identification of polymer stabilized blue-phase liquid crystal display by chromaticity diagram

NASA Astrophysics Data System (ADS)

Lan, Yi-Fen; Tsai, Cheng-Yeh; Wang, Ling-Yung; Ku, Po-Jen; Huang, Tai-Hsiang; Liu, Chu-Yu; Sugiura, Norio

2012-04-01

We reported an identification method of blue phase liquid crystal (BPLC) display status by using Commission International de l'Éclairage (CIE) chromaticity diagram. The BPLC was injected into in-plane-switch (IPS) cell, polymer stabilized (PS) by ultraviolet cured process and analyzed by luminance colorimeter. The results of CIE chromaticity diagram showed a remarkable turning point when polymer stabilized blue phase liquid crystal II (PSBPLC-II) formed in the IPS cell. A mechanism of CIE chromaticity diagram identify PSBPLC display status was proposed, and we believe this finding will be useful to application and production of PSBPLC display.

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

NASA Technical Reports Server (NTRS)

Park, Yoonjoon; Choi, Sang Hyouk; King, Glen C.; Elliott, James R.; Dimarcantonio, Albert L.

2010-01-01

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Forming a three-dimensional porous organic network via solid-state explosion of organic single crystals.

PubMed

Bae, Seo-Yoon; Kim, Dongwook; Shin, Dongbin; Mahmood, Javeed; Jeon, In-Yup; Jung, Sun-Min; Shin, Sun-Hee; Kim, Seok-Jin; Park, Noejung; Lah, Myoung Soo; Baek, Jong-Beom

2017-11-17

Solid-state reaction of organic molecules holds a considerable advantage over liquid-phase processes in the manufacturing industry. However, the research progress in exploring this benefit is largely staggering, which leaves few liquid-phase systems to work with. Here, we show a synthetic protocol for the formation of a three-dimensional porous organic network via solid-state explosion of organic single crystals. The explosive reaction is realized by the Bergman reaction (cycloaromatization) of three enediyne groups on 2,3,6,7,14,15-hexaethynyl-9,10-dihydro-9,10-[1,2]benzenoanthracene. The origin of the explosion is systematically studied using single-crystal X-ray diffraction and differential scanning calorimetry, along with high-speed camera and density functional theory calculations. The results suggest that the solid-state explosion is triggered by an abrupt change in lattice energy induced by release of primer molecules in the 2,3,6,7,14,15-hexaethynyl-9,10-dihydro-9,10-[1,2]benzenoanthracene crystal lattice.

Observing in space and time the ephemeral nucleation of liquid-to-crystal phase transitions.

PubMed

Yoo, Byung-Kuk; Kwon, Oh-Hoon; Liu, Haihua; Tang, Jau; Zewail, Ahmed H

2015-10-19

The phase transition of crystalline ordering is a general phenomenon, but its evolution in space and time requires microscopic probes for visualization. Here we report direct imaging of the transformation of amorphous titanium dioxide nanofilm, from the liquid state, passing through the nucleation step and finally to the ordered crystal phase. Single-pulse transient diffraction profiles at different times provide the structural transformation and the specific degree of crystallinity (η) in the evolution process. It is found that the temporal behaviour of η exhibits unique 'two-step' dynamics, with a robust 'plateau' that extends over a microsecond; the rate constants vary by two orders of magnitude. Such behaviour reflects the presence of intermediate structure(s) that are the precursor of the ordered crystal state. Theoretically, we extend the well-known Johnson-Mehl-Avrami-Kolmogorov equation, which describes the isothermal process with a stretched-exponential function, but here over the range of times covering the melt-to-crystal transformation.

Lasing in a three-dimensional photonic crystal of the liquid crystal blue phase II.

PubMed

Cao, Wenyi; Muñoz, Antonio; Palffy-Muhoray, Peter; Taheri, Bahman

2002-10-01

Photonic-bandgap materials, with periodicity in one, two or three dimensions, offer control of spontaneous emission and photon localization. Low-threshold lasing has been demonstrated in two-dimensional photonic-bandgap materials, both with distributed feedback and defect modes. Liquid crystals with chiral constituents exhibit mesophases with modulated ground states. Helical cholesterics are one-dimensional, whereas blue phases are three-dimensional self-assembled photonic-bandgap structures. Although mirrorless lasing was predicted and observed in one-dimensional helical cholesteric materials and chiral ferroelectric smectic materials, it is of great interest to probe light confinement in three dimensions. Here, we report the first observations of lasing in three-dimensional photonic crystals, in the cholesteric blue phase II. Our results show that distributed feedback is realized in three dimensions, resulting in almost diffraction-limited lasing with significantly lower thresholds than in one dimension. In addition to mirrorless lasing, these self-assembled soft photonic-bandgap materials may also be useful for waveguiding, switching and sensing applications.

Overview: Experimental studies of crystal nucleation: Metals and colloids.

PubMed

Herlach, Dieter M; Palberg, Thomas; Klassen, Ina; Klein, Stefan; Kobold, Raphael

2016-12-07

Crystallization is one of the most important phase transformations of first order. In the case of metals and alloys, the liquid phase is the parent phase of materials production. The conditions of the crystallization process control the as-solidified material in its chemical and physical properties. Nucleation initiates the crystallization of a liquid. It selects the crystallographic phase, stable or meta-stable. Its detailed knowledge is therefore mandatory for the design of materials. We present techniques of containerless processing for nucleation studies of metals and alloys. Experimental results demonstrate the power of these methods not only for crystal nucleation of stable solids but in particular also for investigations of crystal nucleation of metastable solids at extreme undercooling. This concerns the physical nature of heterogeneous versus homogeneous nucleation and nucleation of phases nucleated under non-equilibrium conditions. The results are analyzed within classical nucleation theory that defines the activation energy of homogeneous nucleation in terms of the interfacial energy and the difference of Gibbs free energies of solid and liquid. The interfacial energy acts as barrier for the nucleation process. Its experimental determination is difficult in the case of metals. In the second part of this work we therefore explore the potential of colloidal suspensions as model systems for the crystallization process. The nucleation process of colloids is observed in situ by optical observation and ultra-small angle X-ray diffraction using high intensity synchrotron radiation. It allows an unambiguous discrimination of homogeneous and heterogeneous nucleation as well as the determination of the interfacial free energy of the solid-liquid interface. Our results are used to construct Turnbull plots of colloids, which are discussed in relation to Turnbull plots of metals and support the hypothesis that colloids are useful model systems to investigate crystal nucleation.

Improved crystal orientation and physical properties from single-shot XFEL stills

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

Sauter, Nicholas K., E-mail: nksauter@lbl.gov; Hattne, Johan; Brewster, Aaron S.

X-ray free-electron laser crystallography relies on the collection of still-shot diffraction patterns. New methods are developed for optimal modeling of the crystals’ orientations and mosaic block properties. X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factorsmore » from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model the diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg’s law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographic R factors and sharpening anomalous differences that are near the level of the noise.« less

Lead(ii) soaps: crystal structures, polymorphism, and solid and liquid mesophases.

PubMed

Martínez-Casado, F J; Ramos-Riesco, M; Rodríguez-Cheda, J A; Redondo-Yélamos, M I; Garrido, L; Fernández-Martínez, A; García-Barriocanal, J; da Silva, I; Durán-Olivencia, M; Poulain, A

2017-07-05

The long-chain members of the lead(ii) alkanoate series or soaps, from octanoate to octadecanoate, have been thoroughly characterized by means of XRD, PDF analysis, DSC, FTIR, ssNMR and other techniques, in all their phases and mesophases. The crystal structures at room temperature of all of the members of the series are now solved, showing the existence of two polymorphic forms in the room temperature crystal phase, different to short and long-chain members. Only nonanoate and decanoate present both forms, and this polymorphism is proven to be monotropic. At higher temperature, these compounds present a solid mesophase, defined as rotator, a liquid crystal phase and a liquid phase, all of which have a similar local arrangement. Since some lead(ii) soaps appear as degradation compounds in oil paintings, the solved crystal structures of lead(ii) soaps can now be used as fingerprints for their detection using X-ray diffraction. Pair distribution function analysis on these compounds is very similar in the same phases and mesophases for the different members, showing the same short range order. This observation suggests that this technique could also be used in the detection of these compounds in disordered phases or in the initial stages of formation in paintings.

Asymmetric flavone-based liquid crystals: synthesis and properties

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

Timmons, Daren J.; Jordan, Abraham J.; Kirchon, Angelo A.

2017-02-01

A series of flavones (n-F) substituted at the 4', and 6 positions was prepared, characterised by NMR (1H,13C), HRMS, and studied for liquid crystal properties. The 4'-alkoxy,6-methoxyflavones (4-F–16-F) exhibit varying ranges of nematic and smectic A phases as evidenced by polarised optical microscopy and differential scanning calorimetry (DSC). As the tail length is increased, the smectic phase becomes more prevalent. Smectic phases for (8-F–16-F) were further analysed by powder X-ray diffraction (XRD), and the rate of structural transformations was explored by combined DSC/XRD studies. Flavonol 6-F–OH was also prepared but no mesogenic behaviour was observed. The molecular structures of 6-Fmore » and 6-F–OH were determined by single-crystal XRD and help to explain the differences in material properties. Additionally, fluorescence and electrochemical studies were conducted on solutions of n-F.« less

Structural analysis of as-deposited and annealed low-temperature gallium arsenide

NASA Astrophysics Data System (ADS)

Matyi, R. J.; Melloch, M. R.; Woodall, J. M.

1993-04-01

The structure of GaAs grown at low substrate temperatures (LT-GaAs) by molecular beam epitaxy has been studied using high resolution X-ray diffraction methods. Double crystal rocking curves from the as-deposited LT-GaAs show well defined interference fringes, indicating a high level of structural perfection. Triple crystal diffraction analysis of the as-deposited sample showed significantly less diffuse scattering near the LT-GaAs 004 reciprocal lattice point compared with the substrate 004 reciprocal lattice point, suggesting that despite the incorporation of approximately 1% excess arsenic, the epitaxial layer had superior crystalline perfection than did the GaAs substrate. Triple crystal scans of annealed LT-GaAs showed an increase in the integrated diffuse intensity by approximately a factor of three as the anneal temperature was increased from 700 to 900°C. Analogous to the effects of SiO2 precipitates in annealed Czochralski silicon, the diffuse intensity is attributed to distortions in the epitaxial LT-GaAs lattice by arsenic precipitates.

Stabilized high-accuracy correction of ocular aberrations with liquid crystal on silicon spatial light modulator in adaptive optics retinal imaging system.

PubMed

Huang, Hongxin; Inoue, Takashi; Tanaka, Hiroshi

2011-08-01

We studied the long-term optical performance of an adaptive optics scanning laser ophthalmoscope that uses a liquid crystal on silicon spatial light modulator to correct ocular aberrations. The system achieved good compensation of aberrations while acquiring images of fine retinal structures, excepting during sudden eye movements. The residual wavefront aberrations collected over several minutes in several situations were statistically analyzed. The mean values of the root-mean-square residual wavefront errors were 23-30 nm, and for around 91-94% of the effective time the errors were below the Marechal criterion for diffraction limited imaging. The ability to axially shift the imaging plane to different retinal depths was also demonstrated.

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.

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol.

PubMed

Fili, S; Valmas, A; Norrman, M; Schluckebier, G; Beckers, D; Degen, T; Wright, J; Fitch, A; Gozzo, F; Giannopoulou, A E; Karavassili, F; Margiolaki, I

2015-09-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50-8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs.

Human insulin polymorphism upon ligand binding and pH variation: the case of 4-ethylresorcinol

PubMed Central

Fili, S.; Valmas, A.; Norrman, M.; Schluckebier, G.; Beckers, D.; Degen, T.; Wright, J.; Fitch, A.; Gozzo, F.; Giannopoulou, A. E.; Karavassili, F.; Margiolaki, I.

2015-01-01

This study focuses on the effects of the organic ligand 4-ethylresorcinol on the crystal structure of human insulin using powder X-ray crystallography. For this purpose, systematic crystallization experiments have been conducted in the presence of the organic ligand and zinc ions within the pH range 4.50–8.20, while observing crystallization behaviour around the isoelectric point of insulin. High-throughput crystal screening was performed using a laboratory X-ray diffraction system. The most representative samples were selected for synchrotron X-ray diffraction measurements, which took place at the European Synchrotron Radiation Facility (ESRF) and the Swiss Light Source (SLS). Four different crystalline polymorphs have been identified. Among these, two new phases with monoclinic symmetry have been found, which are targets for the future development of microcrystalline insulin drugs. PMID:26306195

Structural studies of crystalline forms of triamterene with carboxylic acid, GRAS and API molecules

PubMed Central

Rehman, Abida

2018-01-01

Pharmaceutical salt solvates (dimethyl sulfoxide, DMSO) of the drug triamterene with the coformers acetic, succinic, adipic, pimelic, azelaic and nicotinic acid and ibuprofen are prepared by liquid-assisted grinding and solvent-evaporative crystallization. The modified ΔpK a rule as proposed by Cruz-Cabeza [(2012 ▸). CrystEngComm, 14, 6362–6365] is in close agreement with the results of this study. All adducts were characterized by X-ray diffraction and thermal analytical techniques, including single-crystal X-ray diffraction, powder X-ray diffraction, differential scanning calorimetry and thermal gravimetric analysis. Hydrogen-bonded motifs combined to form a variety of extended tapes and sheets. Analysis of the crystal structures showed that all adducts existed as salt solvates and contained the amino­pyridinium–carboxyl­ate heterodimer, except for the solvate containing triamterene, ibuprofen and DMSO, as a result of the presence of a strong and stable hemitriamterenium duplex. A search of the Cambridge Structural Database (CSD 5.36, Version 1.18) to determine the frequency of occurrence of the putative supramolecular synthons found in this study showed good agreement with previous work. PMID:29755747

Beam steering for virtual/augmented reality displays with a cycloidal diffractive waveplate.

PubMed

Chen, Haiwei; Weng, Yishi; Xu, Daming; Tabiryan, Nelson V; Wu, Shin-Tson

2016-04-04

We proposed a switchable beam steering device with cycloidal diffractive waveplate (CDW) for eye tracking in a virtual reality (VR) or augmented reality (AR) display system. Such a CDW diffracts the incident circularly polarized light to the first order with over 95% efficiency. To convert the input linearly polarized light to right-handed or left-handed circular polarization, we developed a broadband polarization switch consisting of a twisted nematic liquid crystal cell and an achromatic quarter-wave retardation film. By cascading 2-3 CDWs together, multiple diffraction angles can be achieved. To suppress the color dispersion, we proposed two approaches to obtain the same diffraction angle for red, green, and blue LEDs-based full color displays. Our device exhibits several advantages, such as high diffraction efficiency, fast response time, low power consumption, and low cost. It holds promise for the emerging VR/AR displays.

Photoalignment and resulting holographic vector grating formation in composites of low molecular weight liquid crystals and photoreactive liquid crystalline polymers

NASA Astrophysics Data System (ADS)

Sasaki, Tomoyuki; Shoho, Takashi; Goto, Kohei; Noda, Kohei; Kawatsuki, Nobuhiro; Ono, Hiroshi

2015-08-01

Polarization holographic gratings were formed in liquid crystal (LC) cells fabricated from a mixture of low molecular weight nematic LC and a photoreactive liquid crystalline polymer (PLCP) with 4-(4-methoxycinnamoyloxy)biphenyl side groups. The diffraction properties of the gratings were analyzed using theoretical models which were determined based on the polarization patterns of the polarization holography. The results demonstrated that vector gratings comprised of periodic orientation distributions of the LC molecule were induced in the cells based on the axis-selective photoreaction of the PLCP. The vector gratings were erased by applying a sufficiently high voltage to the cells and then were reformed with no hysteresis after the voltage was removed. This phenomenon suggested that the PLCP molecules were stabilized based on the axis-selective photocrosslink reaction and that the LC molecules were aligned by the photocrosslinked PLCP. This LC composite with axis-selective photoreactivity is useful for various optical applications, because of their stability, transparency, and response to applied voltage.

High-throughput crystallization screening.

PubMed

Skarina, Tatiana; Xu, Xiaohui; Evdokimova, Elena; Savchenko, Alexei

2014-01-01

Protein structure determination by X-ray crystallography is dependent on obtaining a single protein crystal suitable for diffraction data collection. Due to this requirement, protein crystallization represents a key step in protein structure determination. The conditions for protein crystallization have to be determined empirically for each protein, making this step also a bottleneck in the structure determination process. Typical protein crystallization practice involves parallel setup and monitoring of a considerable number of individual protein crystallization experiments (also called crystallization trials). In these trials the aliquots of purified protein are mixed with a range of solutions composed of a precipitating agent, buffer, and sometimes an additive that have been previously successful in prompting protein crystallization. The individual chemical conditions in which a particular protein shows signs of crystallization are used as a starting point for further crystallization experiments. The goal is optimizing the formation of individual protein crystals of sufficient size and quality to make them suitable for diffraction data collection. Thus the composition of the primary crystallization screen is critical for successful crystallization.Systematic analysis of crystallization experiments carried out on several hundred proteins as part of large-scale structural genomics efforts allowed the optimization of the protein crystallization protocol and identification of a minimal set of 96 crystallization solutions (the "TRAP" screen) that, in our experience, led to crystallization of the maximum number of proteins.

Liquid crystal nanocomposites produced by mixtures of hydrogen bonded achiral liquid crystals and functionalized carbon nanotubes

NASA Astrophysics Data System (ADS)

Katranchev, B.; Petrov, M.; Keskinova, E.; Naradikian, H.; Rafailov, P. M.; Dettlaff-Weglikowska, U.; Spassov, T.

2014-12-01

The liquid crystalline (LC) nature of alkyloxybenzoic acids is preserved after adding of any mesogenic or non-mesogenic compound through hydrogen bonding. However, this noncovalent interaction provokes a sizable effect on the physical properties as, e. g. melting point and mesomorphic states. In the present work we investigate nanocomposites, prepared by mixture of the eighth homologue of p-n-alkyloxybenzoic acids (8OBA) with single-walled carbon nanotubes (SWCNT) with the purpose to modify the optical properties of the liquid crystal. We exercise optical control on the LC system by inserting SWCNT specially functionalized by carboxylic groups. Since the liquid crystalline state combines order and mobility at the molecular (nanoscale) level, molecular modification can lead to different macroscopical nanocomposite symmetry. The thermal properties of the functionalized nanocomposite are confirmed by DSC analyses. The mechanism of the interaction between surface-treated nanoparticles (functionalized nanotubes) and the liquid crystal 8OBA bent- dimer molecules is briefly discussed.

[Physicochemical properties of suplatast tosilate racemate and enantiomers].

PubMed

Ushio, T; Endo, K; Yamamoto, K

1996-11-01

The physicochemical properties of the enantiomer and racemates of suplatast tosilate (ST) were investigated by means of infrared spectroscopy, solid-state 13C CP/MAS NMR spectroscopy, thermal analysis, and X-ray diffraction analysis, and by measuring the solubility and hygroscopy. The infrared and NMR spectra and X-ray diffraction pattern of the enantiomer were distinctly different from those of the racemate. The melting point of the enantiomer was lower than that of the racemate by 5 degrees C, while the solubility of the enantiomer was 1.3 times higher than that of the racemate. The hygroscopic rate of the enantiomer was greater than that of the racemate. These results suggested that ST was classified into a racemic compound crystal. Furthermore, by comparing the relative peak intensity ratios on X-ray diffraction patterns of the crystals with various optical purities prepared by recrystallization, it was found that a mixture of racemic compound crystals and either of racemic mixture crystals or racemic solid solutions was obtained by recrystallization of ST in the content of 0 to 64%ee, while the recrystallization of ST in the content of more than 64%ee led to the formation of racemic mixture crystals or racemic solid solutions.

Light-scattering study of a polymer nematic liquid crystal

NASA Astrophysics Data System (ADS)

Taratuta, Victor G.; Hurd, Alan J.; Meyer, Robert B.

1985-07-01

We study the relaxation of thermally excited orientation fluctuations in a polymer nematic liquid crystal using photon correlation spectroscopy. The material studied is poly-γ-benzyl glutamate at a concentration just above the isotropic to nematic transition point. The relaxation rates of elastic deformation modes exhibit large anisotropies. Quantitative measurements of ratios of Frank elastic constants and Leslie viscosities are described.

Electrodeposition of CdSe on GaAs and InP substrates

NASA Astrophysics Data System (ADS)

Etcheberry, A.; Cachet, H.; Cortes, R.; Froment, M.

2001-06-01

Epitaxial CdSe layers have been electrodeposited on the (1 0 0) and ( 1¯ 1¯ 1¯) faces of GaAs and InP single crystals. Chemical composition and crystalline quality of CdSe have been studied by X-photoelectron spectroscopy, reflection high energy electron diffraction and X-ray diffraction. Influence of the substrate has been pointed out.

Optical properties and diffraction effects in opal photonic crystals.

PubMed

Balestreri, Alessandra; Andreani, Lucio Claudio; Agio, Mario

2006-09-01

Optical properties of fcc opals oriented along the [111] direction are calculated by means of a scattering-matrix approach based on approximating each sphere with cylindrical slices. The use of a plane-wave basis in each layer allows distinguishing zero-order reflection and transmission from higher-order (diffraction) spectra. Optical spectra at large values of the angle of incidence indicate the presence of diffraction effects and of polarization mixing along the LW orientation. Reflectance and transmittance in the high-energy region show a rich spectral dependence and compare reasonably well with recent experimental observations on polystyrene opals. Diffraction spectra as a function of the number of layers display an oscillatory behavior, pointing to the existence of a Pendellösung phenomenon, related to the exchange of energy between two propagating modes in the investigated three-dimensional photonic crystal. This phenomenon could be observed in transmittance experiments on high-quality opals with controlled thickness.

Feasibility of one-shot-per-crystal structure determination using Laue diffraction

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

Cornaby, Sterling; CHESS; Szebenyi, Doletha M. E.

Structure determination was successfully carried out using single Laue exposures from a group of lysozyme crystals. The Laue method may be a viable option for collection of one-shot-per-crystal data from microcrystals. Crystal size is an important factor in determining the number of diffraction patterns which may be obtained from a protein crystal before severe radiation damage sets in. As crystal dimensions decrease this number is reduced, eventually falling to one, at which point a complete data set must be assembled using data from multiple crystals. When only a single exposure is to be collected from each crystal, the polychromatic Lauemore » technique may be preferable to monochromatic methods owing to its simultaneous recording of a large number of fully recorded reflections per image. To assess the feasibility of solving structures using single Laue images from multiple crystals, data were collected using a ‘pink’ beam at the CHESS D1 station from groups of lysozyme crystals with dimensions of the order of 20–30 µm mounted on MicroMesh grids. Single-shot Laue data were used for structure determination by molecular replacement and correct solutions were obtained even when as few as five crystals were used.« less

Comparative study of crystallization process in metallic melts using ab initio molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Debela, Tekalign T.; Wang, X. D.; Cao, Q. P.; Zhang, D. X.; Jiang, J. Z.

2017-05-01

The crystallization process of liquid metals is studied using ab initio molecular dynamics simulations. The evolution of short-range order during quenching in Pb and Zn liquids is compared with body-centered cubic (bcc) Nb and V, and hexagonal closed-packed (hcp) Mg. We found that the fraction and type of the short-range order depends on the system under consideration, in which the icosahedral symmetry seems to dominate in the body-centered cubic metals. Although the local atomic structures in stable liquids are similar, liquid hcp-like Zn, bcc-like Nb and V can be deeply supercooled far below its melting point before crystallization while the supercooled temperature range in liquid Pb is limited. Further investigations into the nucleation process reveal the process of polymorph selection. In the body-centered cubic systems, the polymorph selection occurs in the supercooled state before the nucleation is initiated, while in the closed-packed systems it starts at the time of onset of crystallization. Atoms with bcc-like lattices in all studied supercooled liquids are always detected before the polymorph selection. It is also found that the bond orientational ordering is strongly correlated with the crystallization process in supercooled Zn and Pb liquids.

Mercury sulphide dimorphism in glasses

DOE PAGES

Kassem, Mohammad; Sokolov, Anton; Cuisset, Arnault; ...

2016-05-23

Crystals usually exist in several polymorphic forms in different domains of the P,T-diagram. Glasses and liquids also reveal density- or entropy-driven polyamorphism when e.g. an amorphous molecular solid or liquid transforms into a network polymorph. Using pulsed neutron and high-energy X-ray diffraction, we show that mercury sulphide exists simultaneously in two polymorphic modifications in a glass network forming chain-like and tetrahedral motifs. DFT simulations of 4-fold coordinated mercury species and RMC modelling of high-resolution diffraction data provide additional details on local Hg environment and connectivity implying the (HgS2/2)m oligomeric chains (1 m 6) are acting as a network former whilemore » the HgS4/4-related mixed agglomerated units behave as a modifier« less

X-ray Diffraction from Membrane Protein Nanocrystals

PubMed Central

Hunter, M.S.; DePonte, D.P.; Shapiro, D.A.; Kirian, R.A.; Wang, X.; Starodub, D.; Marchesini, S.; Weierstall, U.; Doak, R.B.; Spence, J.C.H.; Fromme, P.

2011-01-01

Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane proteins is <300. To develop new concepts for membrane protein structure determination, we have explored the serial nanocrystallography method, in which fully hydrated protein nanocrystals are delivered to an x-ray beam within a liquid jet at room temperature. As a model system, we have collected x-ray powder diffraction data from the integral membrane protein Photosystem I, which consists of 36 subunits and 381 cofactors. Data were collected from crystals ranging in size from 100 nm to 2 μm. The results demonstrate that there are membrane protein crystals that contain <100 unit cells (200 total molecules) and that 3D crystals of membrane proteins, which contain <200 molecules, may be suitable for structural investigation. Serial nanocrystallography overcomes the problem of x-ray damage, which is currently one of the major limitations for x-ray structure determination of small crystals. By combining serial nanocrystallography with x-ray free-electron laser sources in the future, it may be possible to produce molecular-resolution electron-density maps using membrane protein crystals that contain only a few hundred or thousand unit cells. PMID:21190672

Pseudo-transient heat transfer in vertical Bridgman crystal growth of semi-transparent materials

NASA Astrophysics Data System (ADS)

Barvinschi, F.; Nicoara, I.; Santailler, J. L.; Duffar, T.

1998-11-01

The temperature distribution and the solid-liquid interface shape during semi-transparent crystal growth have been studied by modelling a vertical Bridgman technique, using a pseudo-transient approximation in an ideal configuration. The heat transfer equation and the boundary conditions have been solved by the finite-element method. It has been pointed out that the optical absorption coefficients of the liquid and solid phases have a major effect on the thermal field, especially on the shape and location of the crystallization interface.

Application of dot-matrix illumination of liquid crystal phase space light modulator in 3D imaging of APD array

NASA Astrophysics Data System (ADS)

Wang, Shuai; Sun, Huayan; Guo, Huichao

2018-01-01

Aiming at the problem of beam scanning in low-resolution APD array in three-dimensional imaging, a method of beam scanning with liquid crystal phase-space optical modulator is proposed to realize high-resolution imaging by low-resolution APD array. First, a liquid crystal phase spatial light modulator is used to generate a beam array and then a beam array is scanned. Since the sub-beam divergence angle in the beam array is smaller than the field angle of a single pixel in the APD array, the APD's pixels respond only to the three-dimensional information of the beam illumination position. Through the scanning of the beam array, a single pixel is used to collect the target three-dimensional information multiple times, thereby improving the resolution of the APD detector. Finally, MATLAB is used to simulate the algorithm in this paper by using two-dimensional scalar diffraction theory, which realizes the splitting and scanning with a resolution of 5 x 5. The feasibility is verified theoretically.

Growth, crystalline perfection, spectral, thermal and theoretical studies on imidazolium L-tartrate crystals.

PubMed

Meena, K; Muthu, K; Meenatchi, V; Rajasekar, M; Bhagavannarayana, G; Meenakshisundaram, S P

2014-04-24

Transparent optical quality single crystals of imidazolium L-tartrate (IMLT) were grown by conventional slow evaporation solution growth technique. Crystal structure of the as-grown IMLT was determined by single crystal X-ray diffraction analysis. Thermal analysis reveals the purity of the crystal and the sample is stable up to the melting point. Good transmittance in the visible region is observed and the band gap energy is estimated using diffuse reflectance data by the application of Kubelka-Munk algorithm. The powder X-ray diffraction study reveals the crystallinity of the as-grown crystal and it is compared with that of the experimental one. An additional peak in high resolution X-ray diffraction (HRXRD) indicates the presence of an internal structural low angle boundary. Second harmonic generation (SHG) activity of IMLT is significant as estimated by Kurtz and Perry powder technique. HOMO-LUMO energies and first-order molecular hyperpolarizability of IMLT have been evaluated using density functional theory (DFT) employing B3LYP functional and 6-31G(d,p) basis set. The optimized geometry closely resembles the ORTEP. The vibrational patterns present in the molecule are confirmed by FT-IR coinciding with theoretical patterns. Copyright © 2014 Elsevier B.V. All rights reserved.

Anthracene + Pyrene Solid Mixtures: Eutectic and Azeotropic Character

PubMed Central

Rice, James W.; Fu, Jinxia; Suuberg, Eric M.

2010-01-01

To better characterize the thermodynamic behavior of a binary polycyclic aromatic hydrocarbon mixture, thermochemical and vapor pressure experiments were used to examine the phase behavior of the anthracene (1) + pyrene (2) system. A solid-liquid phase diagram was mapped for the mixture. A eutectic point occurs at 404 K at x1 = 0.22. A model based on eutectic formation can be used to predict the enthalpy of fusion associated with the mixture. For mixtures that contain x1 < 0.90, the enthalpy of fusion is near that of pure pyrene. This and X-ray diffraction results indicate that mixtures of anthracene and pyrene have pyrene-like crystal structures and energetics until the composition nears that of pure anthracene. Solid-vapor equilibrium studies show that mixtures of anthracene and pyrene form solid azeotropes at x1 of 0.03 and 0.14. Additionally, mixtures at x1 = 0.99 sublime at the vapor pressure of pure anthracene, suggesting that anthracene behavior is not significantly influenced by x2 = 0.01 in the crystal structure. PMID:21116474

Melting Curve of Molecular Crystal GeI4

NASA Astrophysics Data System (ADS)

Fuchizaki, Kazuhiro; Hamaya, Nozomu

2014-07-01

In situ synchrotron x-ray diffraction measurements were carried out to determine the melting curve of the molecular crystal GeI4. We found that the melting line rapidly increases with a pressure up to about 3 GPa, at which it abruptly breaks. Such a strong nonlinear shape of the melting curve can be approximately captured by the Kumari-Dass-Kechin equation. The parameters involved in the equation could be determined from the equation of state for the crystalline phase, which was also established in the present study. The melting curve predicted from the equation approaches the actual melting curve as the degree of approximation involved in obtaining the equation is improved. However, the treatment is justifiable only if the slope of the melting curve is everywhere continuous. We believe that this is not the case for GeI4's melting line at the breakpoint, as inferred from the nature of breakdown of the Kraut-Kennedy and the Magalinskii-Zubov relationships.The breakpoint may then be a triple point among the crystalline phase and two possible liquid phases.

X-ray imaging crystal spectrometer for extended X-ray sources

DOEpatents

Bitter, Manfred L.; Fraenkel, Ben; Gorman, James L.; Hill, Kenneth W.; Roquemore, A. Lane; Stodiek, Wolfgang; von Goeler, Schweickhard E.

2001-01-01

Spherically or toroidally curved, double focusing crystals are used in a spectrometer for X-ray diagnostics of an extended X-ray source such as a hot plasma produced in a tokomak fusion experiment to provide spatially and temporally resolved data on plasma parameters using the imaging properties for Bragg angles near 45. For a Bragg angle of 45.degree., the spherical crystal focuses a bundle of near parallel X-rays (the cross section of which is determined by the cross section of the crystal) from the plasma to a point on a detector, with parallel rays inclined to the main plain of diffraction focused to different points on the detector. Thus, it is possible to radially image the plasma X-ray emission in different wavelengths simultaneously with a single crystal.

Preparation and Optical Properties of Spherical Inverse Opals by Liquid Phase Deposition Using Spherical Colloidal Crystals

NASA Astrophysics Data System (ADS)

Aoi, Y.; Tominaga, T.

2013-03-01

Titanium dioxide (TiO2) inverse opals in spherical shape were prepared by liquid phase deposition (LPD) using spherical colloidal crystals as templates. Spherical colloidal crystals were produced by ink-jet drying technique. Aqueous emulsion droplets that contain polystyrene latex particles were ejected into air and dried. Closely packed colloidal crystals with spherical shape were obtained. The obtained spherical colloidal crystals were used as templates for the LPD. The templates were dispersed in the deposition solution of the LPD, i.e. a mixed solution of ammonium hexafluorotitanate and boric acid and reacted for 4 h at 30 °C. After the LPD process, the interstitial spaces of the spherical colloidal crystals were completely filled with titanium oxide. Subsequent heat treatment resulted in removal of templates and spherical titanium dioxide inverse opals. The spherical shape of the template was retained. SEM observations indicated that the periodic ordered voids were surrounded by titanium dioxide. The optical reflectance spectra indicated that the optical properties of the spherical titanium dioxide inverse opals were due to Bragg diffractions from the ordered structure. Filling in the voids of the inverse opals with different solvents caused remarkable changes in the reflectance peak.

Pixel-level tunable liquid crystal lenses for auto-stereoscopic display

NASA Astrophysics Data System (ADS)

Li, Kun; Robertson, Brian; Pivnenko, Mike; Chu, Daping; Zhou, Jiong; Yao, Jun

2014-02-01

Mobile video and gaming are now widely used, and delivery of a glass-free 3D experience is of both research and development interest. The key drawbacks of a conventional 3D display based on a static lenticular lenslet array and parallax barriers are low resolution, limited viewing angle and reduced brightness, mainly because of the need of multiple-pixels for each object point. This study describes the concept and performance of pixel-level cylindrical liquid crystal (LC) lenses, which are designed to steer light to the left and right eye sequentially to form stereo parallax. The width of the LC lenses can be as small as 20-30 μm, so that the associated auto-stereoscopic display will have the same resolution as the 2D display panel in use. Such a thin sheet of tunable LC lens array can be applied directly on existing mobile displays, and can deliver 3D viewing experience while maintaining 2D viewing capability. Transparent electrodes were laser patterned to achieve the single pixel lens resolution, and a high birefringent LC material was used to realise a large diffraction angle for a wide field of view. Simulation was carried out to model the intensity profile at the viewing plane and optimise the lens array based on the measured LC phase profile. The measured viewing angle and intensity profile were compared with the simulation results.

On the Fringe Field of Wide Angle LC Optical Phased Array

NASA Technical Reports Server (NTRS)

Wang, Xighua; Wang, Bin; Bos, Philip J.; Anderson, James E.; Pouch, John; Miranda, Felix; McManamon, Paul F.

2004-01-01

For free space laser communication, light weighted large deployable optics is a critical component for the transmitter. However, such an optical element will introduce large aberrations due to the fact that the surface figure of the large optics is susceptable to deformation in the space environment. We propose to use a high-resolution liquid crystal spatial light modulator to correct for wavefront aberrations introduced by the primary optical element, and to achieve very fine beam steering and shaping at the same time. A 2-D optical phased array (OPA) antenna based on a Liquid Crystal on Silicon (LCOS) spatial light modulator is described. This device offers a combination of low cost, high resolution, high accuracy, high diffraction efficiency at video speed. To quantitatively understand the influence factor of the different design parameters, a computer simulation of the device is given by the 2-D director simulation and the Finite Difference Time domain (FDTD) simulation. For the 1-D OPA, we define the maximum steering angle to have a grating period of 8 pixel/reset scheme; as for larger steering angles than this criterion, the diffraction efficiency drops dramatically. In this case, the diffraction efficiency of 0.86 and the Strehl ratio of 0.9 are obtained in the simulation. The performance of the device in achieving high resolution wavefront correction and beam steering is also characterized experimentally.

Statistical foundations of liquid-crystal theory: II: Macroscopic balance laws.

PubMed

Seguin, Brian; Fried, Eliot

2013-01-01

Working on a state space determined by considering a discrete system of rigid rods, we use nonequilibrium statistical mechanics to derive macroscopic balance laws for liquid crystals. A probability function that satisfies the Liouville equation serves as the starting point for deriving each macroscopic balance. The terms appearing in the derived balances are interpreted as expected values and explicit formulas for these terms are obtained. Among the list of derived balances appear two, the tensor moment of inertia balance and the mesofluctuation balance, that are not standard in previously proposed macroscopic theories for liquid crystals but which have precedents in other theories for structured media.

Statistical foundations of liquid-crystal theory

PubMed Central

Seguin, Brian; Fried, Eliot

2013-01-01

Working on a state space determined by considering a discrete system of rigid rods, we use nonequilibrium statistical mechanics to derive macroscopic balance laws for liquid crystals. A probability function that satisfies the Liouville equation serves as the starting point for deriving each macroscopic balance. The terms appearing in the derived balances are interpreted as expected values and explicit formulas for these terms are obtained. Among the list of derived balances appear two, the tensor moment of inertia balance and the mesofluctuation balance, that are not standard in previously proposed macroscopic theories for liquid crystals but which have precedents in other theories for structured media. PMID:23554513

Field-induced phase transitions in chiral smectic liquid crystals studied by the constant current method

NASA Astrophysics Data System (ADS)

H, Dhaouadi; R, Zgueb; O, Riahi; F, Trabelsi; T, Othman

2016-05-01

In ferroelectric liquid crystals, phase transitions can be induced by an electric field. The current constant method allows these transition to be quickly localized and thus the (E,T) phase diagram of the studied product can be obtained. In this work, we make a slight modification to the measurement principles based on this method. This modification allows the characteristic parameters of ferroelectric liquid crystal to be quantitatively measured. The use of a current square signal highlights a phenomenon of ferroelectric hysteresis with remnant polarization at null field, which points out an effect of memory in this compound.

The role of the “Casimir force analogue” at the microscopic processes of crystallization and melting

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

Chuvildeev, V.N., E-mail: chuvildeev@gmail.com; Semenycheva, A.V., E-mail: avsemenycheva@gmail.com

Melting (crystallization), a phase transition from a crystalline solid to a liquid state, is a common phenomenon in nature. We suggest a new factor, “the Casimir force analogue”, to describe mechanisms of melting and crystallization. The Casimir force analogue is a force occurring between the surfaces of solid and liquid phases of metals caused by different energy density of phonons of these phases. It explains abrupt changes in geometry and thermodynamic parameters at a melting point. “The Casimir force analogue” helps to estimate latent melting heat and to gain an insight into a solid–liquid transition problem.

The role of the "Casimir force analogue" at the microscopic processes of crystallization and melting

NASA Astrophysics Data System (ADS)

Chuvildeev, V. N.; Semenycheva, A. V.

2016-10-01

Melting (crystallization), a phase transition from a crystalline solid to a liquid state, is a common phenomenon in nature. We suggest a new factor, "the Casimir force analogue", to describe mechanisms of melting and crystallization. The Casimir force analogue is a force occurring between the surfaces of solid and liquid phases of metals caused by different energy density of phonons of these phases. It explains abrupt changes in geometry and thermodynamic parameters at a melting point. "The Casimir force analogue" helps to estimate latent melting heat and to gain an insight into a solid-liquid transition problem.

The liquid wood heat flow and material properties as a function of temperature

NASA Astrophysics Data System (ADS)

Mazurchevici, Simona; Quadrini, Fabrizio; Nedelcu, Dumitru

2018-03-01

There are three types of ‘liquid wood’, Arbofill, Arboblend and Arboform and will replace plastics materials in the near future taking into account the biodegradability and higher properties versus common used plastics materials. In order to get more information about the materials properties of ‘liquid wood’ the granules and samples obtained by injection molding were studied using Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) for Arboform L,V3 Nature-‘liquid wood’ (A-LW) and Arboform L, V3 Nature reinforced with Aramid Fibers (A-LWAF).In case of A-LW granule studied, the DSC analysis presents that at 97 °C appears an endoderm peak which represents the crystallization of the material, at 175 °C the exoderm peak which means the melting point of the material. After the tested granule cooling period of time this one was tested again and the endoderm peak disappears, which means that crystallization of material disappeared. The melting point of the second test decreases slightly at 174.6 °C. Also, the new test shows that at 61.7 °C the glass transition temperature appears and the melting point slightly decreases. In case of A-LW samples the DSC analyses shows that the melting point increased by 2.77 °C compared to the melting point of Arboform granule. The material behavior is more or less the same without the crystallization area.

Melting point suppression in new lanthanoid(III) ionic liquids by trapping of kinetic polymorphs: an in situ synchrotron powder diffraction study.

PubMed

Chesman, Anthony S R; Yang, Mei; Mallick, Bert; Ross, Tamsyn M; Gass, Ian A; Deacon, Glen B; Batten, Stuart R; Mudring, Anja-Verena

2012-01-04

The complexes (N(4444))(3)[Ln(dcnm)(6)] (Ln = La-Nd, Sm; N(4444) = tetrabutylammonium) display a decrease in the melting point upon fast cooling from a melt, which is shown by in situ synchrotron based X-ray powder diffraction to be due to the formation of a second, less thermodynamically stable, polymorph. This journal is © The Royal Society of Chemistry 2012

AsS melt under pressure: one substance, three liquids.

PubMed

Brazhkin, V V; Katayama, Y; Kondrin, M V; Hattori, T; Lyapin, A G; Saitoh, H

2008-04-11

An in situ high-temperature--high-pressure study of liquid chalcogenide AsS by x-ray diffraction, resistivity measurements, and quenching from melt is presented. The obtained data provide direct evidence for the existence in the melt under compression of two transformations: one is from a moderate-viscosity molecular liquid to a high-viscosity nonmetallic polymerized liquid at P approximately 1.6-2.2 GPa; the other is from the latter to a low-viscosity metallic liquid at P approximately 4.6-4.8 GPa. Upon rapid cooling, molecular and metallic liquids crystallize to normal and high-pressure phases, respectively, while a polymerized liquid is easily quenched to a new AsS glass. General aspects of multiple phase transitions in liquid AsS, including relations to the phase diagram of the respective crystalline, are discussed.

Crystalline Colloidal Arrays in Polymer Matrices

NASA Technical Reports Server (NTRS)

Sunkara, Hari B.; Penn, B. G.; Frazier, D. O.; Ramachandran, N.

1997-01-01

Crystalline Colloidal Arrays (CCA, also known as colloidal crystals), composed of aqueous or nonaqueous dispersions of self-assembled nanosized polymer colloidal spheres, are emerging toward the development of advanced optical devices for technological applications. The spontaneous self assembly of polymer spheres in a dielectric medium results from the electrostatic repulsive interaction between particles of uniform size and charge distribution. In a way similar to atomic crystals that diffract X-rays, CCA dispersions in thin quartz cells selectively and efficiently Bragg diffract the incident visible light. The reason for this diffraction is because the lattice (body or face centered cubic) spacing is on the order of the wavelength of visible light. Unlike the atomic crystals that diffract a fixed wavelength, colloidal crystals in principle, depending on the particle size, particle number and charge density, can diffract W, Vis or IR light. Therefore, the CCA dispersions can be used as laser filters. Besides, the diffraction intensity depends on the refractive index mismatch between polymer spheres and dielectric medium; therefore, it is possible to modulate incident light intensities by manipulating the index of either the spheres or the medium. Our interest in CCA is in the fabrication of all-optical devices such as optical switches, limiters, and spatial light modulators for optical signal processing. The two major requirements from a materials standpoint are the incorporation of suitable nonlinear optical materials (NLO) into polymer spheres which will allow us to alter the refractive index of the spheres by intense laser radiation, and preparation of solid CCA filters which can resist laser damage. The fabrication of solid composite filters not only has the advantage that the films are easier to handle, but also the arrays in solid films are more robust than in liquid media. In this paper, we report the photopolymerization process used to trap CCA in polymer matrices, the factors which affect the optical diffraction qualities of resulting polymer films, and methods to improve the efficiencies of solid optical filters. Before this, we also present the experimental demonstration, of controlling the optical diffraction intensities from aqueous CCA dispersions by varying the temperature, which establishes the feasibility of fabricating all-optical switching devices with nonlinear periodic array structures.

Erasing no-man’s land by thermodynamically stabilizing the liquid-liquid transition in tetrahedral particles

NASA Astrophysics Data System (ADS)

Smallenburg, Frank; Filion, Laura; Sciortino, Francesco

2014-09-01

One of the most controversial hypotheses for explaining the origin of the thermodynamic anomalies characterizing liquid water postulates the presence of a metastable second-order liquid-liquid critical point located in the `no-man’s land’. In this scenario, two liquids with distinct local structure emerge near the critical temperature. Unfortunately, as spontaneous crystallization is rapid in this region, experimental support for this hypothesis relies on significant extrapolations, either from the metastable liquid or from amorphous solid water. Although the liquid-liquid transition is expected to feature in many tetrahedrally coordinated liquids, including silicon, carbon and silica, even numerical studies of atomic and molecular models have been unable to conclusively prove the existence of this transition. Here we provide such evidence for a model in which it is possible to continuously tune the softness of the interparticle interaction and the flexibility of the bonds, the key ingredients controlling the existence of the critical point. We show that conditions exist where the full coexistence is thermodynamically stable with respect to crystallization. Our work offers a basis for designing colloidal analogues of water exhibiting liquid-liquid transitions in equilibrium, opening the way for experimental confirmation of the original hypothesis.

Interpretation of small-angle diffraction experiments on opal-like photonic crystals

NASA Astrophysics Data System (ADS)

Marlow, F.; Muldarisnur, M.; Sharifi, P.; Zabel, H.

2011-08-01

Comprehensive structural information on artificial opals involving the deviations from the strongly dominating face-centered cubic structure is still missing. Recent structure investigations with neutrons and synchrotron sources have shown a high degree of order but also a number of unexpected scattering features. Here, we point out that the exclusion of the allowed 002-type diffraction peaks by a small atomic form factor is not obvious and that surface scattering has to be included as a possible source for the diffraction peaks. Our neutron diffraction data indicate that surface scattering is the main reason for the smallest-angle peaks in the diffraction patterns.

Quick measurement of crystal truncation rod profiles in simultaneous multi-wavelength dispersive mode

NASA Astrophysics Data System (ADS)

Matsushita, T.; Takahashi, T.; Shirasawa, T.; Arakawa, E.; Toyokawa, H.; Tajiri, H.

2011-11-01

To conduct time-resolved measurements in the wide momentum transfer (q = 4π sinθ/λ, θ: the glancing angle of the x-ray beam, λ: x-ray wavelength) range of interest, we developed a method that can simultaneously measure the whole profile of x-ray diffraction and crystal truncation rod scattering of interest with no need of rotation of the specimen, detector, and monochromator crystal during the measurement. With a curved crystal polychromator (Si 111 diffraction), a horizontally convergent x-ray beam having a one-to-one correlation between wavelength (energy: 16.24-23.0 keV) and direction is produced. The convergent x-ray beam components of different wavelengths are incident on the specimen in a geometry where θ is the same for all the x-ray components and are diffracted within corresponding vertical scattering planes by a specimen ([GaAs(12ML)/AlAs(8 ML)]50 on GaAs(001) substrate) placed at the focal point. Although θ is the same for all the directions, q continuously varies because λ changes as a function of direction. The normalized horizontal intensity distribution across the beam, as measured using a two-dimensional pixel array detector downstream of the specimen, represents the reflectivity curve profile both near to and far from the Bragg point. As for the crystal truncation rod scattering around the 002 reflection, the diffraction profile from the Bragg peak down to reflectivity of 1.0 × 10-9 was measured with a sufficient data collection time (1000-2000 s). With data collection times of 100, 10, 1.0, and 0.1 s, profiles down to a reflectivity of ˜6 × 10-9, ˜2 × 10-8, ˜8 × 10-8, and ˜8 × 10-7 were measured, respectively. To demonstrate the time-resolving capability of the system, reflectivity curves were measured with time resolutions of 1.0 s while rotating the specimen. We have also measured the diffraction profile around the 113 reflection in the non-specular reflection geometry.

Crystal structure, spectrum character and explosive property of a new cocrystal CL-20/DNT

NASA Astrophysics Data System (ADS)

Liu, Ke; Zhang, Gao; Luan, Jieyu; Chen, Zhiqun; Su, Pengfei; Shu, Yuanjie

2016-04-01

A new cocrystal explosive of 2,4,6,8,10,12-hexanitrohexaazaiso-wurtzitane(CL-20) and 2,5-dinitrotoluene(DNT) in a molar ratio of 1:2 has been prepared by slow solvent evaporation method. Crystal structure of the cocrystal characterized by single crystal X-ray diffraction (SXRD) reveals that the cocrystal is formed by intermolecular hydrogen bond interactions and belongs to the triclinic system with P-1 group. Moreover, the obivious differences of powder X-ray diffraction (PXRD) patterns, infrared spectroscopy and Raman spectroscopy confirm that the intermolecular interactions have great influence for the crystal structure and formation of cocrystal. The cocrystal exhibits a lower impact height of 44 cm, suggesting a substantial reduction of sensitivity in comparison with CL-20. And thermal test results showed cocrystal obtains a lower melting point than DNT, which means huge advantages in blasting engineering.

Time-resolved structural dynamics of thin metal films heated with femtosecond optical pulses.

PubMed

Chen, Jie; Chen, Wei-Kan; Tang, Jau; Rentzepis, Peter M

2011-11-22

We utilize 100 fs optical pulses to induce ultrafast disorder of 35- to 150-nm thick single Au(111) crystals and observe the subsequent structural evolution using 0.6-ps, 8.04-keV X-ray pulses. Monitoring the picosecond time-dependent modulation of the X-ray diffraction intensity, width, and shift, we have measured directly electron/phonon coupling, phonon/lattice interaction, and a histogram of the lattice disorder evolution, such as lattice breath due to a pressure wave propagating at sonic velocity, lattice melting, and recrystallization, including mosaic formation. Results of theoretical simulations agree and support the experimental data of the lattice/liquid phase transition process. These time-resolved X-ray diffraction data provide a detailed description of all the significant processes induced by ultrafast laser pulses impinging on thin metallic single crystals.

Dacarbazine.

PubMed

Al-Badr, Abdullah A; Alodhaib, Mansour M

2016-01-01

Dacarbazine is a cell cycle nonspecific antineoplastic alkylating agent used in the treatment of metastatic malignant melanoma. This chapter contains the descriptions of the drug: nomenclature, formulae, chemical structure, elemental composition, and appearance. The uses and applications of dacarbazine and the methods that were used for its preparation are reported. The methods which were used for the physical characterization of the drug are ionization constant, solubility, X-ray powder diffraction pattern, crystal structure, melting point, and differential scanning calorimetry. The profile contains the spectra of the drug: ultraviolet spectrum, vibrational spectrum, nuclear magnetic resonance spectra, and mass spectrum. The compendial methods of analysis for dacarbazine include the United States Pharmacopeia methods, British Pharmacopeia methods, and International Pharmacopeia methods. Other reported methods that are used for the analysis of the drug are high-performance liquid chromatography, high-performance liquid chromatography-mass spectrometry, and polarography. Metabolism, pharmacokinetics, and stability studies on dacarbazine are also included. Reviews of some analytical methods and physicochemical properties of the drug as well as the most important enzymes that are involved in the prodrug activation are provided. Sixty-four references are listed at the end of this monograph. © 2016 Elsevier Inc. All rights reserved.

Ultra-stiff large-area carpets of carbon nanotubes

NASA Astrophysics Data System (ADS)

Meysami, Seyyed Shayan; Dallas, Panagiotis; Britton, Jude; Lozano, Juan G.; Murdock, Adrian T.; Ferraro, Claudio; Gutierrez, Eduardo Saiz; Rijnveld, Niek; Holdway, Philip; Porfyrakis, Kyriakos; Grobert, Nicole

2016-06-01

Herewith, we report the influence of post-synthesis heat treatment (<=2350 °C and plasma temperatures) on the crystal structure, defect density, purity, alignment and dispersibility of free-standing large-area (several cm2) carpets of ultra-long (several mm) vertically aligned multi-wall carbon nanotubes (VA-MWCNTs). VA-MWCNTs were produced in large quantities (20-30 g per batch) using a semi-scaled-up aerosol-assisted chemical vapour deposition (AACVD) setup. Electron and X-ray diffraction showed that the heat treatment at 2350 °C under inert atmosphere purifies, removes residual catalyst particles, and partially aligns adjacent single crystals (crystallites) in polycrystalline MWCNTs. The purification and improvement in the crystallites alignment within the MWCNTs resulted in reduced dispersibility of the VA-MWCNTs in liquid media. High-resolution microscopy revealed that the crystallinity is improved in scales of few tens of nanometres while the point defects remain largely unaffected. The heat treatment also had a marked benefit on the mechanical properties of the carpets. For the first time, we report compression moduli as high as 120 MPa for VA-MWCNT carpets, i.e. an order of magnitude higher than previously reported figures. The application of higher temperatures (arc-discharge plasma, >=4000 °C) resulted in the formation of a novel graphite-matrix composite reinforced with CVD and arc-discharge-like carbon nanotubes.Herewith, we report the influence of post-synthesis heat treatment (<=2350 °C and plasma temperatures) on the crystal structure, defect density, purity, alignment and dispersibility of free-standing large-area (several cm2) carpets of ultra-long (several mm) vertically aligned multi-wall carbon nanotubes (VA-MWCNTs). VA-MWCNTs were produced in large quantities (20-30 g per batch) using a semi-scaled-up aerosol-assisted chemical vapour deposition (AACVD) setup. Electron and X-ray diffraction showed that the heat treatment at 2350 °C under inert atmosphere purifies, removes residual catalyst particles, and partially aligns adjacent single crystals (crystallites) in polycrystalline MWCNTs. The purification and improvement in the crystallites alignment within the MWCNTs resulted in reduced dispersibility of the VA-MWCNTs in liquid media. High-resolution microscopy revealed that the crystallinity is improved in scales of few tens of nanometres while the point defects remain largely unaffected. The heat treatment also had a marked benefit on the mechanical properties of the carpets. For the first time, we report compression moduli as high as 120 MPa for VA-MWCNT carpets, i.e. an order of magnitude higher than previously reported figures. The application of higher temperatures (arc-discharge plasma, >=4000 °C) resulted in the formation of a novel graphite-matrix composite reinforced with CVD and arc-discharge-like carbon nanotubes. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01660j

Programmable liquid crystal waveplate polarization gratings as elements for polarimetric and interference applications

NASA Astrophysics Data System (ADS)

Moreno, I.; Davis, J. A.

2010-06-01

We review the use of a parallel aligned nematic liquid crystal spatial light modulator as a very useful and flexible device for polarimetric and interferometric applications. The device acts as a programmable pixelated waveplate, and the encoding of a linear grating permits its use as a polarization beam splitter. When a grating with a reduced period is encoded, the diffracted beams are spatially separated and the device can be used for polarimetric analysis. On the contrary when a large period grating is displayed, the beams are not spatially separated, and they are useful to realize a common path interferometric system with polarization sensitivity. The flexibility offered by the programmability of the display allows non-conventional uses, including the analysis of light beams with structured spatial polarizations.

Diffraction Efficiency of Thin Film Holographic Beam Steering Devices

NASA Technical Reports Server (NTRS)

Titus, Charles M.; Pouch, John; Nguyen, Hung; Miranda, Felix; Bos, Philip J.

2003-01-01

Dynamic holography has been demonstrated as a method for correcting aberrations in space deployable optics, and can also be used to achieve high-resolution beam steering in the same environment. In this paper, we consider some of the factors affecting the efficiency of these devices. Specifically, the effect on the efficiency of a highly collimated beam from the number of discrete phase steps per period is considered for a blazed thin film beam steering grating. The effect of the number of discrete phase steps per period on steering resolution is also considered. We also present some result of Finite-Difference Time-Domain (FDTD) calculations of light propagating through liquid crystal "blazed" gratings. Liquid crystal gratings are shown to spatially modulate both the phase and amplitude of the propagating light.

Smectic Layer Origami via Preprogrammed Photoalignment.

PubMed

Ma, Ling-Ling; Tang, Ming-Jie; Hu, Wei; Cui, Ze-Qun; Ge, Shi-Jun; Chen, Peng; Chen, Lu-Jian; Qian, Hao; Chi, Li-Feng; Lu, Yan-Qing

2017-04-01

Hierarchical architecture is of vital importance in soft materials. Focal conic domains (FCDs) of smectic liquid crystals, characterized by an ordered lamellar structure, attract intensive attention. Simultaneously tailoring the geometry and clustering characteristics of FCDs remains a challenge. Here, the 3D smectic layer origami via a 2D preprogrammed photoalignment film is accomplished. Full control of hierarchical superstructures is demonstrated, including the domain size, shape, and orientation, and the lattice symmetry of fragmented toric FCDs. The unique symmetry breaking of resultant superstructures combined with the optical anisotropy of the liquid crystals induces an intriguing polarization-dependent diffraction. This work broadens the scientific understanding of self-assembled soft materials and may inspire new opportunities for advanced functional materials and devices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystal pathologies in macromolecular crystallography.

PubMed

Dauter, Zbigniew; Jaskólski, Mariusz

Macromolecules, such as proteins or nucleic acids, form crystals with a large volume fraction of water, ~50% on average. Apart from typical physical defects and rather trivial poor quality problems, macromolecular crystals, as essentially any crystals, can also suffer from several kinds of pathologies, in which everything seems to be perfect, except that from the structural point of view the interpretation may be very difficult, sometimes even impossible. A frequent nuisance is pseudosymmetry, or non-crystallographic symmetry (NCS), which is particularly nasty when it has translational character. Lattice-translocation defects, also called order-disorder twinning (OD-twinning), occur when molecules are packed regularly in layers but the layers are stacked (without rotation) in two (or more) discrete modes, with a unique translocation vector. Crystal twinning arises when twin domains have different orientations, incompatible with the symmetry of the crystal structure. There are also crystals in which the periodic (lattice) order is broken or absent altogether. When the strict short-range translational order from one unit cell to the next is lost but the long-range order is restored by a periodic modulation, we have a modulated crystal structure. In quasicrystals (not observed for macromolecules yet), the periodic order (in 3D space) is lost completely and the diffraction pattern (which is still discrete) cannot be even indexed using three hkl indices. In addition, there are other physical defects and phenomena (such as high mosaicity, diffraction anisotropy, diffuse scattering, etc.) which make diffraction data processing and structure solution difficult or even impossible.

Adjustable liquid aperture to eliminate undesirable light in holographic projection.

PubMed

Wang, Di; Liu, Chao; Li, Lei; Zhou, Xin; Wang, Qiong-Hua

2016-02-08

In this paper, we propose an adjustable liquid aperture to eliminate the undesirable light in a holographic projection. The aperture is based on hydrodynamic actuation. A chamber is formed with a cylindrical tube. A black droplet is filled in the sidewall of the cylinder tube and the outside space is the transparent oil which is immiscible with the black droplet. An ultrathin glass sheet is attached on the bottom substrate of the device and a black shading film is secured to the central area of the glass sheet. By changing the volume of the black droplet, the black droplet will move to the middle or sidewall due to hydrodynamic actuation, so the device can be used as an adjustable aperture. A divergent spherical wave and a solid lens are used to separate the focus planes of the reconstructed image and diffraction beams induced by the liquid crystal on silicon in the holographic projection. Then the aperture is used to eliminate the diffraction beams by adjusting the size of the liquid aperture and the holographic projection does not have undesirable light.

Studies of fatty acid composition, physicochemical and thermal properties, and crystallization behavior of mango kernel fats from various Thai varieties.

PubMed

Sonwai, Sopark; Ponprachanuvut, Punnee

2014-01-01

Mango kernel fat (MKF) has received attention in recent years due to the resemblance between its characteristics and those of cocoa butter (CB). In this work, fatty acid (FA) composition, physicochemical and thermal properties and crystallization behavior of MKFs obtained from four varieties of Thai mangoes: Keaw-Morakot (KM), Keaw-Sawoey (KS), Nam-Dokmai (ND) and Aok-Rong (AR), were characterized. The fat content of the mango kernels was 6.40, 5.78, 5.73 and 7.74% (dry basis) for KM, KS, ND and AR, respectively. The analysis of FA composition revealed that all four cultivars had oleic and stearic acids as the main FA components with ND and AR exhibiting highest and lowest stearic acid content, respectively. ND had the highest slip melting point and solid fat content (SFC) followed by KS, KM and AR. All fat samples exhibited high SFC at 20℃ and below. They melted slowly as the temperature increased and became complete liquids as the temperature approached 35°C. During static isothermal crystallization at 20°C, ND displayed the highest Avrami rate constant k followed by KS, KM and AR, indicating that the crystallization was fastest for ND and slowest for AR. The Avrami exponent n of all samples ranged from 0.89 to 1.73. The x-ray diffraction analysis showed that all MKFs crystallized into a mixture of pseudo-β', β', sub-β and β structures with β' being the predominant polymorph. Finally, the crystals of the kernel fats from all mango varieties exhibited spherulitic morphology.

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

Andreev, A L; Andreeva, T B; Kompanets, I N

We have studied the method for suppressing speckle noise in patterns produced by a laser based on a fast-response electro-optical cell with a ferroelectric liquid crystal (FLC) in which helicoid is absent, i.e., compensated for. The character of smectic layer deformation in an electric field is considered along with the mechanism of spatially inhomogeneous phase modulation of a laser beam passing through the cell which is accompanied by the destruction of phase relations in the beam. Advantages of a helix-free FLC cell are pointed out as compared to helical crystal cells studied previously. (liquid crystal devices)

Structural and microstructural description of the glacial state in triphenyl phosphite from powder synchrotron X-ray diffraction data and Raman scattering investigations

NASA Astrophysics Data System (ADS)

Derollez, P.; Hernandez, O.; Hédoux, A.; Guinet, Y.; Masson, O.; Lefebvre, J.; Descamps, M.

2004-06-01

The structure and microstructure (refinement of the isotropic size and microstrain parameters) of the glacial state in triphenyl phosphite (TPP, P(OC 6H 5) 3) transformed at 222K have been determined from powder synchrotron X-ray diffraction data through a Rietveld and a Le Bail refinement, respectively. It is shown that the glacial state is composed of crystallites of the stable crystal phase coexisting with non-transformed supercooled liquid, the apparent size of the crystallites—depending on the aging temperature at which the glacial state is isothermally formed, [Phys. Rev. B 60 (1999) 9390]—being equal to 329.2(2) Å at 222K. The molecular conformation is slightly less mirror-symmetric than the one in the crystal state, and correlatively only one of the two unusual weak intermolecular C-H⋯O hydrogen bonds already observed in the latter state is encountered in the glacial one. Additional Raman scattering investigations confirm the previous result and reveal in addition that no hydrogen bonding interaction is observed neither in the glass nor in the liquid states.

A Quartz Crystal Microbalance dew point sensor without frequency measurement.

PubMed

Wang, Guohua; Zhang, Weishuo; Wang, Shuo; Sun, Jinglin

2014-11-01

This work deals with the design of a dew point sensor based on Quartz Crystal Microbalance (QCM) without measuring the frequency. This idea is inspired by the fact that the Colpitts oscillation circuit will stop oscillating when the QCM works in the liquid media. The quartz crystal and the electrode are designed through the finite element simulation and the stop oscillating experiment is conducted to verify the sensibility. Moreover, the measurement result is calibrated to approach the true value. At last a series of dew points at the same temperature is measured with the designed sensor. Results show that the designed dew point sensor is able to detect the dew point with the proper accuracy.

A quartz crystal microbalance dew point sensor without frequency measurement

NASA Astrophysics Data System (ADS)

Wang, Guohua; Zhang, Weishuo; Wang, Shuo; Sun, Jinglin

2014-11-01

This work deals with the design of a dew point sensor based on Quartz Crystal Microbalance (QCM) without measuring the frequency. This idea is inspired by the fact that the Colpitts oscillation circuit will stop oscillating when the QCM works in the liquid media. The quartz crystal and the electrode are designed through the finite element simulation and the stop oscillating experiment is conducted to verify the sensibility. Moreover, the measurement result is calibrated to approach the true value. At last a series of dew points at the same temperature is measured with the designed sensor. Results show that the designed dew point sensor is able to detect the dew point with the proper accuracy.

Single-shot mega-electronvolt ultrafast electron diffraction for structure dynamic studies of warm dense matter

NASA Astrophysics Data System (ADS)

Mo, M. Z.; Shen, X.; Chen, Z.; Li, R. K.; Dunning, M.; Sokolowski-Tinten, K.; Zheng, Q.; Weathersby, S. P.; Reid, A. H.; Coffee, R.; Makasyuk, I.; Edstrom, S.; McCormick, D.; Jobe, K.; Hast, C.; Glenzer, S. H.; Wang, X.

2016-11-01

We have developed a single-shot mega-electronvolt ultrafast-electron-diffraction system to measure the structural dynamics of warm dense matter. The electron probe in this system is featured by a kinetic energy of 3.2 MeV and a total charge of 20 fC, with the FWHM pulse duration and spot size at sample of 350 fs and 120 μm respectively. We demonstrate its unique capability by visualizing the atomic structural changes of warm dense gold formed from a laser-excited 35-nm freestanding single-crystal gold foil. The temporal evolution of the Bragg peak intensity and of the liquid signal during solid-liquid phase transition are quantitatively determined. This experimental capability opens up an exciting opportunity to unravel the atomic dynamics of structural phase transitions in warm dense matter regime.

Neutron diffraction, specific heat and magnetization studies on Nd{sub 2}CuTiO{sub 6}

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

Rayaprol, S., E-mail: sudhindra@csr.res.in; Kaushik, S. D.; Kumar, Naresh

2016-05-23

Structural and physical properties of a double-perovskite compound, Nd{sub 2}CuTiO{sub 6} have been studied using neutron diffraction, magnetization and specific heat measurements. The compound crystallizes in an orthorhombic structure in space group Pnma. The interesting observation we make here is that, though no long range magnetic order is observed between 2 and 300 K, the low temperature specific heat and magnetic susceptibility behavior exhibits non-Fermi liquid like behavior in this insulating compound. The magnetization and specific heat data are presented and discussed in light of these observations.

Evidence for SrHo2O4 and SrDy2O4 as model J1-J2 zigzag chain materials

NASA Astrophysics Data System (ADS)

Fennell, A.; Pomjakushin, V. Y.; Uldry, A.; Delley, B.; Prévost, B.; Désilets-Benoit, A.; Bianchi, A. D.; Bewley, R. I.; Hansen, B. R.; Klimczuk, T.; Cava, R. J.; Kenzelmann, M.

2014-06-01

Neutron diffraction and inelastic spectroscopy is used to characterize the magnetic Hamiltonian of SrHo2O4 and SrDy2O4. Through a detailed computation of the crystal-field levels we find site-dependent anisotropic single-ion magnetism in both materials, and diffraction measurements show the presence of strong one-dimensional spin correlations. Our measurements indicate that competing interactions of the zigzag chain, combined with frustrated interchain interactions, play a crucial role in stabilizing spin-liquid type correlations in this series.

Recording polarization gratings with a standing spiral wave

NASA Astrophysics Data System (ADS)

Vernon, Jonathan P.; Serak, Svetlana V.; Hakobyan, Rafik S.; Aleksanyan, Artur K.; Tondiglia, Vincent P.; White, Timothy J.; Bunning, Timothy J.; Tabiryan, Nelson V.

2013-11-01

A scalable and robust methodology for writing cycloidal modulation patterns of optical axis orientation in photosensitive surface alignment layers is demonstrated. Counterpropagating circularly polarized beams, generated by reflection of the input beam from a cholesteric liquid crystal, direct local surface orientation in a photosensitive surface. Purposely introducing a slight angle between the input beam and the photosensitive surface normal introduces a grating period/orientation that is readily controlled and templated. The resulting cycloidal diffractive waveplates offer utility in technologies requiring diffraction over a broad range of angles/wavelengths. This simple methodology of forming polarization gratings offers advantages over conventional fabrication techniques.

Behavior of Sn atoms in GeSn thin films during thermal annealing: Ex-situ and in-situ observations

NASA Astrophysics Data System (ADS)

Takase, Ryohei; Ishimaru, Manabu; Uchida, Noriyuki; Maeda, Tatsuro; Sato, Kazuhisa; Lieten, Ruben R.; Locquet, Jean-Pierre

2016-12-01

Thermally induced crystallization processes for amorphous GeSn thin films with Sn concentrations beyond the solubility limit of the bulk crystal Ge-Sn binary system have been examined by X-ray photoelectron spectroscopy, grazing incidence X-ray diffraction, and (scanning) transmission electron microscopy. We paid special attention to the behavior of Sn before and after recrystallization. In the as-deposited specimens, Sn atoms were homogeneously distributed in an amorphous matrix. Prior to crystallization, an amorphous-to-amorphous phase transformation associated with the rearrangement of Sn atoms was observed during heat treatment; this transformation is reversible with respect to temperature. Remarkable recrystallization occurred at temperatures above 400 °C, and Sn atoms were ejected from the crystallized GeSn matrix. The segregation of Sn became more pronounced with increasing annealing temperature, and the ejected Sn existed as a liquid phase. It was found that the molten Sn remains as a supercooled liquid below the eutectic temperature of the Ge-Sn binary system during the cooling process, and finally, β-Sn precipitates were formed at ambient temperature.

Adsorption of gentian violet dyes in aqueous solution on microporous AlPOs molecular sieves synthesized by ionothermal method

NASA Astrophysics Data System (ADS)

Fortas, W.; Djelad, A.; Hasnaoui, M. A.; Sassi, M.; Bengueddach, A.

2018-02-01

In this work, AlPO-34, like-chabazite (CHA) zeolite, was ionothermally prepared using the ionic liquid (IL), 1-ethyl-3-methylimidazolium chloride [EMIMCl], as solvent. The solids obtained were characterized by x-ray powder diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FTIR), thermal analysis (TG) and nitrogen adsorption/desorption at 77.3 K. The results show that the ionic liquid is occluded in the AlPO-34 framework and consequently it acts also as a structure-directing agent. The variation of chemical composition led to AlPO-34 materials with different crystal sizes and morphologies. The well crystallized AlPO-34 material was used as adsorbent for Crystal Violet (CV) dye removal from aqueous solutions. The effect of adsorption parameters such as pH and initial concentration were investigated. It was found that adsorption dyes is favorable at pH = 6. The adsorption isotherm data follow the Langmuir equation in which parameters are calculated. The selected AlPO-34 sample exhibited a high crystal violet dye removal of 46.08 mg g-1 at pH = 6.

Crystal structure and properties of tetragonal EuAg{sub 4}In{sub 8} grown by metal flux technique

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

Subbarao, Udumula; Sarkar, Sumanta; Peter, Sebastian C., E-mail: sebastiancp@jncasr.ac.in

The compound EuAg{sub 4}In{sub 8} has been obtained as single crystals in high yield from reactions run in liquid indium. X-ray diffraction on single crystals suggests that EuAg{sub 4}In{sub 8} crystallizes in the CeMn{sub 4}Al{sub 8} structure type, tetragonal space group I4/mmm with lattice constants a=b=9.7937(2) Å and c=5.7492(2) Å. Crystal structure of EuAg{sub 4}In{sub 8} is composed of pseudo Frank–Kasper cages occupied by one europium atom in each ring, which are shared through the corner along the ab plane resulting in a three dimensional network. The magnetic susceptibility of EuAg{sub 4}In{sub 8} was measured in the temperature range 2–300more » K, which obeyed Curie–Weiss law above 50 K. Magnetic moment value calculated from the fitting indicates the presence of divalent europium, which was confirmed by X-ray absorption near edge spectroscopy. Electrical resistivity measurements suggest that EuAg{sub 4}In{sub 8} is metallic in nature with a probable Fermi liquid behavior at low temperature. - Graphical abstract: The tetragonal EuAg{sub 4}In{sub 8} has been grown as single crystals from reactions run in liquid indium. Magnetic and XANES measurements suggest divalent nature of Eu and resistivity measurements suggest metallic nature. - Highlights: • EuAg{sub 4}In{sub 8} phase having tetragonal phase is grown by metal flux technique. • Magnetic and XANES measurements exhibit divalent nature of Eu in EuAg{sub 4}In{sub 8}. • Resistivity measurement suggests metallic nature and probable Fermi liquid behavior.« less

Colorimetric qualification of shear sensitive liquid crystal coatings

NASA Technical Reports Server (NTRS)

Muratore, Joseph J., Jr.

1993-01-01

The work that has been done to date on the Shear Sensitive Liquid Crystal Project demonstrated that cholesteric liquid crystal coatings respond to both the direction and magnitude of a shearing force. The response of the coating is to selectively scatter incident white light into a spectrum of colors. Discernible color changes at a fixed angle of observation and illumination are the result of an applied shear stress. The intention was to be able to convert these observable color patterns from a flow visualization technique into a quantitative tool. One of the earlier intentions was to be able to use liquid crystals in dynamic flow fields. This was assumed possible because liquid crystals had made it possible to visualize transients in surface shear forces. Although the transients were visualized by color changes to an order one micro second, the time response of a coating to align to a shearing force is dependent on the magnitude of the change between its initial and final states. Unfortunately, the response is not instantaneous. It is for this reason any future attempt at quantifying the magnitude and directions of a shearing force are limited to surface shear stress vector fields in three dimensional steady state flows. This limitation does not significantly detract from the utility of liquid crystal coatings. The measurement of skin friction in the study of transition on wings, prediction of drag forces, performance assessment, and the investigation of boundary layer behavior is of great importance in aerodynamics. There exist numerous examples of techniques for the measurement of surface shear stress. Most techniques require arduous calibrations and necessitate extensive preparation of the receiving surfaces. However, the main draw back of instruments such as Preston tubes, hot films, buried wire gages, and floating element balances is that they only provide a point measurement. The advantages of capturing global shear data would be appreciable when compared with conventional point measurement sensors. It has yet to be determined if a repeatable correlation exists between the measured color of a liquid crystal coating and the magnitude/directional components of a shear vector imposed onto it.

Hetero-phase fluctuations in the pre-melting region in ionic crystals

NASA Astrophysics Data System (ADS)

Matsunaga, S.; Tamaki, S.

2008-06-01

The theory of the pre-melting phenomena in ionic crystals on the basis of the concept of the hetero phase fluctuation has been applied to KCl and AgCl crystal. The large scale molecular dynamics simulations (MD) in KCl and AgCl crystals are also performed to examine the ionic configuration in premelting region in the vicinity of their melting points. The size of the liquid like clusters are estimated by the theory and MD. The structural features of liquid like clusters are discussed by MD results using the Lindemann instability condition. The ionic conductivities in the pre-melting region are also discussed on the same theoretical basis.

The Stanford Automated Mounter: Enabling High-Throughput Protein Crystal Screening at SSRL

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

Smith, C.A.; Cohen, A.E.

2009-05-26

The macromolecular crystallography experiment lends itself perfectly to high-throughput technologies. The initial steps including the expression, purification, and crystallization of protein crystals, along with some of the later steps involving data processing and structure determination have all been automated to the point where some of the last remaining bottlenecks in the process have been crystal mounting, crystal screening, and data collection. At the Stanford Synchrotron Radiation Laboratory, a National User Facility that provides extremely brilliant X-ray photon beams for use in materials science, environmental science, and structural biology research, the incorporation of advanced robotics has enabled crystals to be screenedmore » in a true high-throughput fashion, thus dramatically accelerating the final steps. Up to 288 frozen crystals can be mounted by the beamline robot (the Stanford Auto-Mounting System) and screened for diffraction quality in a matter of hours without intervention. The best quality crystals can then be remounted for the collection of complete X-ray diffraction data sets. Furthermore, the entire screening and data collection experiment can be controlled from the experimenter's home laboratory by means of advanced software tools that enable network-based control of the highly automated beamlines.« less

Real-time molecular scale observation of crystal formation.

PubMed

Schreiber, Roy E; Houben, Lothar; Wolf, Sharon G; Leitus, Gregory; Lang, Zhong-Ling; Carbó, Jorge J; Poblet, Josep M; Neumann, Ronny

2017-04-01

How molecules in solution form crystal nuclei, which then grow into large crystals, is a poorly understood phenomenon. The classical mechanism of homogeneous crystal nucleation proceeds via the spontaneous random aggregation of species from liquid or solution. However, a non-classical mechanism suggests the formation of an amorphous dense phase that reorders to form stable crystal nuclei. So far it has remained an experimental challenge to observe the formation of crystal nuclei from five to thirty molecules. Here, using polyoxometallates, we show that the formation of small crystal nuclei is observable by cryogenic transmission electron microscopy. We observe both classical and non-classical nucleation processes, depending on the identity of the cation present. The experiments verify theoretical studies that suggest non-classical nucleation is the lower of the two energy pathways. The arrangement in just a seven-molecule proto-crystal matches the order found by X-ray diffraction of a single bulk crystal, which demonstrates that the same structure was formed in each case.

Talbot effect of quasi-periodic grating.

PubMed

Zhang, Chong; Zhang, Wei; Li, Furui; Wang, Junhong; Teng, Shuyun

2013-07-20

Theoretic and experimental studies of the Talbot effect of quasi-periodic gratings are performed in this paper. The diffractions of periodic and quasi-periodic square aperture arrays in Fresnel fields are analyzed according to the scalar diffraction theory. The expressions of the diffraction intensities of two types of quasi-periodic gratings are deduced. Talbot images of the quasi-periodic gratings are predicted to appear at multiple certain distances. The quasi-periodic square aperture arrays are produced with the aid of a liquid crystal light modulator, and the self-images of the quasi-periodic gratings are measured successfully in the experiment. This study indicates that even a structure in short-range disorder may take on the self-imaging effect in a Fresnel field.

Crystallinity properties and crystallization behavior of chocolate fat blends.

PubMed

da Silva, Thais Lomonaco Teodoro; Grimaldi, Renato; Calligaris, Guilherme Andrade; Cardoso, Lisandro Pavie; Gonçalves, Lireny Aparecida Guaraldo

2017-06-01

Cocoa butter (CB) provides unique crystallization characteristics to chocolates and confectionary products; hence, it is an important value-add product. However, other alternative fats that minimally affect the crystallization behaviour of chocolates and confectionary products are now being increasingly used. This study analyzed the crystallization behaviour of CB, cocoa butter substitutes (CBSs), and their blends. Blends were prepared using CBS concentrations: 5, 10, 15, 20 and 37.5%. CB, CBS, and their blends were evaluated by following analysis: solid fat content, isothermal analysis, polarized light microscopic, thermal behaviour, X-ray diffraction and consistency. Crystallization analysis showed an incompatibility between the 2 fats, with a reduction in the crystallinity and increase in liquid content in all the blends. Eutectic crystallization at 20 °C was only observed for the blend containing 20% CBSs. This was considered as a positive result because previous studies have indicated that CBS concentration in CB blends should not be more than 5%.

Small-angle light scattering symmetry breaking in polymer-dispersed liquid crystal films with inhomogeneous electrically controlled interface anchoring

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

Loiko, V. A., E-mail: loiko@ifanbel.bas-net.by; Konkolovich, A. V.; Zyryanov, V. Ya.

2017-03-15

We have described the method of analyzing and reporting on the results of calculation of the small-angle structure of radiation scattered by a polymer-dispersed liquid crystal film with electrically controlled interfacial anchoring. The method is based on the interference approximation of the wave scattering theory and the hard disk model. Scattering from an individual liquid crystal droplet has been described using the anomalous diffraction approximation extended to the case of droplets with uniform and nonuniform interface anchoring at the droplet–polymer boundary. The director field structure in an individual droplet is determined from the solution of the problem of minimizing themore » volume density of the free energy. The electrooptical effect of symmetry breaking in the angular distribution of scattered radiation has been analyzed. This effect means that the intensities of radiation scattered within angles +θ{sub s} and–θ{sub s} relative to the direction of illumination in the scattering plane can be different. The effect is of the interference origin and is associated with asymmetry of the phase shift of the wavefront of an incident wave from individual parts of the droplet, which appears due to asymmetry of the director field structure in the droplet, caused by nonuniform anchoring of liquid crystal molecules with the polymer on its surface. This effect is analyzed in the case of normal illumination of the film depending on the interfacial anchoring at the liquid crystal–polymer interface, the orientation of the optical axes of droplets, their concentration, sizes, anisometry, and polydispersity.« less

Hidden topological constellations and polyvalent charges in chiral nematic droplets

NASA Astrophysics Data System (ADS)

Posnjak, Gregor; Čopar, Simon; Muševič, Igor

2017-02-01

Topology has an increasingly important role in the physics of condensed matter, quantum systems, material science, photonics and biology, with spectacular realizations of topological concepts in liquid crystals. Here we report on long-lived hidden topological states in thermally quenched, chiral nematic droplets, formed from string-like, triangular and polyhedral constellations of monovalent and polyvalent singular point defects. These topological defects are regularly packed into a spherical liquid volume and stabilized by the elastic energy barrier due to the helical structure and confinement of the liquid crystal in the micro-sphere. We observe, for the first time, topological three-dimensional point defects of the quantized hedgehog charge q=-2, -3. These higher-charge defects act as ideal polyvalent artificial atoms, binding the defects into polyhedral constellations representing topological molecules.

Hidden topological constellations and polyvalent charges in chiral nematic droplets

PubMed Central

Posnjak, Gregor; Čopar, Simon; Muševič, Igor

2017-01-01

Topology has an increasingly important role in the physics of condensed matter, quantum systems, material science, photonics and biology, with spectacular realizations of topological concepts in liquid crystals. Here we report on long-lived hidden topological states in thermally quenched, chiral nematic droplets, formed from string-like, triangular and polyhedral constellations of monovalent and polyvalent singular point defects. These topological defects are regularly packed into a spherical liquid volume and stabilized by the elastic energy barrier due to the helical structure and confinement of the liquid crystal in the micro-sphere. We observe, for the first time, topological three-dimensional point defects of the quantized hedgehog charge q=−2, −3. These higher-charge defects act as ideal polyvalent artificial atoms, binding the defects into polyhedral constellations representing topological molecules. PMID:28220770

Controlled dehydration improves the diffraction quality of two RNA crystals.

PubMed

Park, HaJeung; Tran, Tuan; Lee, Jun Hyuck; Park, Hyun; Disney, Matthew D

2016-11-03

Post-crystallization dehydration methods, applying either vapor diffusion or humidity control devices, have been widely used to improve the diffraction quality of protein crystals. Despite the fact that RNA crystals tend to diffract poorly, there is a dearth of reports on the application of dehydration methods to improve the diffraction quality of RNA crystals. We use dehydration techniques with a Free Mounting System (FMS, a humidity control device) to recover the poor diffraction quality of RNA crystals. These approaches were applied to RNA constructs that model various RNA-mediated repeat expansion disorders. The method we describe herein could serve as a general tool to improve diffraction quality of RNA crystals to facilitate structure determinations.

Macromolecular Crystal Growth by Means of Microfluidics

NASA Technical Reports Server (NTRS)

vanderWoerd, Mark; Ferree, Darren; Spearing, Scott; Monaco, Lisa; Molho, Josh; Spaid, Michael; Brasseur, Mike; Curreri, Peter A. (Technical Monitor)

2002-01-01

We have performed a feasibility study in which we show that chip-based, microfluidic (LabChip(TM)) technology is suitable for protein crystal growth. This technology allows for accurate and reliable dispensing and mixing of very small volumes while minimizing bubble formation in the crystallization mixture. The amount of (protein) solution remaining after completion of an experiment is minimal, which makes this technique efficient and attractive for use with proteins, which are difficult or expensive to obtain. The nature of LabChip(TM) technology renders it highly amenable to automation. Protein crystals obtained in our initial feasibility studies were of excellent quality as determined by X-ray diffraction. Subsequent to the feasibility study, we designed and produced the first LabChip(TM) device specifically for protein crystallization in batch mode. It can reliably dispense and mix from a range of solution constituents into two independent growth wells. We are currently testing this design to prove its efficacy for protein crystallization optimization experiments. In the near future we will expand our design to incorporate up to 10 growth wells per LabChip(TM) device. Upon completion, additional crystallization techniques such as vapor diffusion and liquid-liquid diffusion will be accommodated. Macromolecular crystallization using microfluidic technology is envisioned as a fully automated system, which will use the 'tele-science' concept of remote operation and will be developed into a research facility for the International Space Station as well as on the ground.

FAST TRACK COMMUNICATION: Gas liquid phase coexistence in a tetrahedral patchy particle model

NASA Astrophysics Data System (ADS)

Romano, Flavio; Tartaglia, Piero; Sciortino, Francesco

2007-08-01

We evaluate the location of the gas-liquid coexistence line and of the associated critical point for the primitive model for water (PMW), introduced by Kolafa and Nezbeda (1987 Mol. Phys. 61 161). Besides being a simple model for a molecular network forming liquid, the PMW is representative of patchy proteins and novel colloidal particles interacting with localized directional short-range attractions. We show that the gas-liquid phase separation is metastable, i.e. it takes place in the region of the phase diagram where the crystal phase is thermodynamically favoured, as in the case of particles interacting via short-range attractive spherical potentials. We do not observe crystallization close to the critical point. The region of gas-liquid instability of this patchy model is significantly reduced as compared to that from equivalent models of spherically interacting particles, confirming the possibility of observing kinetic arrest in a homogeneous sample driven by bonding as opposed to packing.

Quasi two-dimensional astigmatic solitons in soft chiral metastructures

NASA Astrophysics Data System (ADS)

Laudyn, Urszula A.; Jung, Paweł S.; Karpierz, Mirosław A.; Assanto, Gaetano

2016-03-01

We investigate a non-homogeneous layered structure encompassing dual spatial dispersion: continuous diffraction in one transverse dimension and discrete diffraction in the orthogonal one. Such dual diffraction can be balanced out by one and the same nonlinear response, giving rise to light self-confinement into astigmatic spatial solitons: self-focusing can compensate for the spreading of a bell-shaped beam, leading to quasi-2D solitary wavepackets which result from 1D transverse self-localization combined with a discrete soliton. We demonstrate such intensity-dependent beam trapping in chiral soft matter, exhibiting one-dimensional discrete diffraction along the helical axis and one-dimensional continuous diffraction in the orthogonal plane. In nematic liquid crystals with suitable birefringence and chiral arrangement, the reorientational nonlinearity is shown to support bell-shaped solitary waves with simple astigmatism dependent on the medium birefringence as well as on the dual diffraction of the input wavepacket. The observations are in agreement with a nonlinear nonlocal model for the all-optical response.

Erasing no-man's land by thermodynamically stabilizing the liquid-liquid transition in tetrahedral particles.

PubMed

Smallenburg, Frank; Filion, Laura; Sciortino, Francesco

2014-09-01

One of the most controversial hypotheses for explaining the origin of the thermodynamic anomalies characterizing liquid water postulates the presence of a metastable second-order liquid-liquid critical point [1] located in the "no-man's land" [2]. In this scenario, two liquids with distinct local structure emerge near the critical temperature. Unfortunately, since spontaneous crystallization is rapid in this region, experimental support for this hypothesis relies on significant extrapolations, either from the metastable liquid or from amorphous solid water [3, 4]. Although the liquid-liquid transition is expected to feature in many tetrahedrally coordinated liquids, including silicon [5], carbon [6] and silica, even numerical studies of atomic and molecular models have been unable to conclusively prove the existence of this transition. Here we provide such evidence for a model in which it is possible to continuously tune the softness of the interparticle interaction and the flexibility of the bonds, the key ingredients controlling the existence of the critical point. We show that conditions exist where the full coexistence is thermodynamically stable with respect to crystallization. Our work offers a basis for designing colloidal analogues of water exhibiting liquid-liquid transitions in equilibrium, opening the way for experimental confirmation of the original hypothesis.

Depth-enhanced three-dimensional-two-dimensional convertible display based on modified integral imaging.

PubMed

Park, Jae-Hyeung; Kim, Hak-Rin; Kim, Yunhee; Kim, Joohwan; Hong, Jisoo; Lee, Sin-Doo; Lee, Byoungho

2004-12-01

A depth-enhanced three-dimensional-two-dimensional convertible display that uses a polymer-dispersed liquid crystal based on the principle of integral imaging is proposed. In the proposed method, a lens array is located behind a transmission-type display panel to form an array of point-light sources, and a polymer-dispersed liquid crystal is electrically controlled to pass or to scatter light coming from these point-light sources. Therefore, three-dimensional-two-dimensional conversion is accomplished electrically without any mechanical movement. Moreover, the nonimaging structure of the proposed method increases the expressible depth range considerably. We explain the method of operation and present experimental results.

Synchrotron Study on Crystallization Kinetics of Milk Fat under Shear Flow

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

Mazzanti, G.; Marangoni, A; Idziak, S

A detailed synchrotron X-ray diffraction study on the kinetics of crystallization of anhydrous milk fat (AMF) and milk fat triacylglycerols (MFT) was done in a Couette cell at 17 C, 17.5 C and 20 C under shear rates between 0 and 2880 s-1. We observed shear-induced acceleration of the transition from phase ? to ?? and the presence of crystalline orientation, but no effect of shear on the onset time of phase ? was observed. A two stage regime was observed for the growth of phase ??. The first stage follows a series-parallel system of differential equations describing the conversionmore » between liquid and crystalline phases. The second stage follows a diffusion-controlled regime. These mechanisms are consistent with the crystalline orientation, the growth of the crystalline domains and the observed displacement of the diffraction peak positions. The absence of the polar lipids explains the faster kinetics of MFT.« less

Broadband integrated mid infrared light sources as enabling technology for point of care mid-infrared spectroscopy

DTIC Science & Technology

2017-08-20

liquid crystal cell was successfully employed as an active q-switching element in the same type of chip lasers. The short laser pulses that were...switched mode-locked (QML) operation of those chip lasers. Further, a novel nematic liquid crystal cell was successfully employed as an active q... gas spectroscopy and environmental monitoring, areas that hold immense significance and importance. However, laser source development at these

Phase relations of iron and iron nickel alloys up to 300 GPa: Implications for composition and structure of the Earth's inner core

NASA Astrophysics Data System (ADS)

Kuwayama, Yasuhiro; Hirose, Kei; Sata, Nagayoshi; Ohishi, Yasuo

2008-09-01

We have investigated the phase relations of iron and iron-nickel alloys with 18 to 50 wt.% Ni up to over 300 GPa using a laser-heated diamond-anvil cell. The synchrotron X-ray diffraction measurements show the wide stability of hcp-iron up to 301 GPa and 2000 K and 319 GPa and 300 K without phase transition to dhcp, orthorhombic, or bcc phases. On the other hand, the incorporation of nickel has a remarkable effect on expanding the stability field of fcc phase. The geometry of the temperature-composition phase diagram of iron-nickel alloys suggests that the hcp-fcc-liquid triple point is located at 10 to 20 wt.% Ni at the pressure of the inner core boundary. The fcc phase could crystallize depending on the nickel and silicon contents in the Earth's core, both of which are fcc stabilizer.

Phase behavior in quaternary ammonium ionic liquid-propanol solutions: Hydrophobicity, molecular conformations, and isomer effects

NASA Astrophysics Data System (ADS)

Abe, Hiroshi; Kohki, Erica; Nakada, Ayumu; Kishimura, Hiroaki

2017-07-01

In ionic liquids (ILs), the effects of a quaternary ammonium cation containing a hydroxyl group were investigated and compared with the effect of a standard quaternary ammonium cation. The cation possessing a hydroxyl group is choline, Chol+, and the anion is bis(trifluoromethylsulfonyl)imide, TFSI-. Crystal polymorphism of pure [Chol][TFSI] was observed upon both cooling and heating by simultaneous X-ray diffraction and differential scanning calorimetry measurements. In contrast, [N3111][TFSI] (N3111+: N-trimethyl-N-propylammonium), a standard IL, demonstrated simple crystallization upon cooling. By adding 1-propanol or 2-propanol, the phase behaviors of the [Chol][TFSI]-based and [N3111][TFSI]-based mixtures were clearly distinguished. By Raman spectroscopy, the TFSI- anion conformers in the liquid state were shown to vary according to the propanol concentration, propanol isomer, and type of cation. The anomalous behaviors of pure [Chol][TFSI] and its mixtures are derived from hydrogen bonding of the hydroxyl group of Chol+ cation coupled with the hydrophobicity and packing efficiency of propanol.

Cluster self-organization of nanotubes in a nematic phase: The percolation behavior and appearance of optical singularities

NASA Astrophysics Data System (ADS)

Ponevchinsky, V. V.; Goncharuk, A. I.; Vasil'Ev, V. I.; Lebovka, N. I.; Soskin, M. S.

2010-03-01

The structural features, as well as the optical and electrophysical properties of a 5CB nematic liquid crystal with additions of multilayer carbon nanotubes, have been investigated in the concentration range C = 0.0025-0.1 wt %. The self-aggregation of nanotubes into clusters with a fractal structure occurs in the liquid crystal. At 0.025 wt %, the clusters are merged, initiating the percolation transition of the composite to a state with a high electric conductivity. The strong interaction of 5CB molecules with the surface of nanotube clusters is responsible for the formation of micron surface liquid crystal layers with an irregular field of elastic stresses and a complex structure of birefringence. They are easily observed in a polarization microscope and visualize directly invisible submicron nanotube aggregates. Their transverse size increases when an electric field is applied to the liquid crystal cell. Two mechanisms of the generation of optical singularities in the passing laser beam have been revealed. Optical vortices appear in the speckle fields of laser radiation scattered at the indented boundaries of the nanotube clusters, whereas the birefringence of the beam in surface liquid-crystal layers is accompanied by the appearance of polarization C points.

Study of solid/liquid and solid/gas interfaces in Cu-isoleucine complex by surface X-ray diffraction

NASA Astrophysics Data System (ADS)

Ferrer, Pilar; Rubio-Zuazo, Juan; Castro, German R.

2013-02-01

The enzymes could be understood like structures formed by amino acids bonded with metals, which act as active sites. The research on the coordination of metal-amino acid complexes will bring light on the behavior of metal enzymes, due to the close relation existing between the atomic structure and the functionality. The Cu-isoleucine bond is considered as a good model system to attain a better insight into the characteristics of naturally occurring copper metalloproteins. The surface structure of metal-amino acid complex could be considered as a more realistic model for real systems under biologic working conditions, since the molecular packing is decreased. In the surface, the structural constrains are reduced, keeping the structural capability of surface complex to change as a function of the surrounding environment. In this work, we present a surface X-ray diffraction study on Cu-isoleucine complex under different ambient conditions. Cu(Ile)2 crystals of about 5 mm × 5 mm × 1 mm have been growth, by seeding method in a supersaturated solution, presenting a surface of high quality. The sample for the surface diffraction study was mounted on a cell specially designed for solid/liquid or solid/gas interface analysis. The Cu-isoleucine crystal was measured under a protective dry N2 gas flow and in contact with a saturated metal amino acid solution. The bulk and the surface signals were compared, showing different atomic structures. In both cases, from surface diffraction data, it is observed that the atomic structure of the top layer undergoes a clear structural deformation. A non-uniform surface relaxation is observed producing an inhomogeneous displacement of the surface atoms towards the surface normal.

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

Salud, J.; Lopez, D.O.; Barrio, M.

The experimental two-component phase diagram between the orientationally disordered crystals 2-amino-2-methyl-1,3-propanediol (AMP) and 1,1,1-tris(hydroxymethyl)propane (PG) has been established from room temperature to the liquid state using thermal analysis and X-ray powder diffraction techniques. The intermolecular interactions in the orientationally disordered mixed crystals of the mentioned system and other related two-component systems are discussed by analyzing the evolution of the packing coefficient as a function of the composition. A thermodynamic analysis of the presented phase diagram and the redetermined AMP/NPG (2,2-dimethyl-1,3-propanediol) is reported on the basis of the enthalpy-entropy compensation theory.

Effects of elongation on the phase behavior of the Gay-Berne fluid

NASA Astrophysics Data System (ADS)

Brown, Julian T.; Allen, Michael P.; Martín del Río, Elvira; Miguel, Enrique De

1998-06-01

In this paper we present a computer simulation study of the phase behavior of the Gay-Berne liquid crystal model, concentrating on the effects of varying the molecular elongation κ. We study a range of length-to-width parameters 3<=κ<=4, using a variety of molecular dynamics and Monte Carlo techniques, obtaining a guide to the phase behavior for each shape studied. We observe vapor (V), isotropic liquid (I), nematic (N), smectic-A (SA) and smectic-B (SB) liquid crystal phases. Within the small range of elongation studied, the phase diagram shows significant changes. On increasing κ, the liquid-vapor critical point moves to lower temperature until it falls below the I-SB coexistence line, around κ=3.4, where liquid-vapor coexistence proves hard to establish. The liquid-vapor critical point seems to be completely absent at κ=4.0. Another dramatic effect is the growth of a stable SA ``island'' in the phase diagram at elongations slightly above κ=3.0. The SA range extends to both higher and lower temperatures as κ is increased. Also as κ is increased, the I-N transition is seen to move to lower density (and pressure) at given temperature. The lowest temperature at which the nematic phase is stable does not vary dramatically with κ. On cooling, no SB-crystal transition can be identified in the equation of state for any of these elongations; we suggest that, on the basis of simulation evidence, SB and crystal are really the same phase for these models.

Absence of Jahn-Teller transition in the hexagonal Ba 3CuSb 2O 9 single crystal

DOE PAGES

Katayama, Naoyuki; Kimura, Kenta; Han, Yibo; ...

2015-07-13

With decreasing temperature, liquids generally freeze into a solid state, losing entropy in the process. However, exceptions to this trend exist, such as quantum liquids, which may remain unfrozen down to absolute zero owing to strong quantum entanglement effects that stabilize a disordered state with zero entropy. Examples of such liquids include Bose-Einstein condensation of cold atoms, superconductivity, quantum Hall state of electron systems, and quantum spin liquid state in the frustrated magnets. Furthermore, recent studies have clarified the possibility of another exotic quantum liquid state based on the spin-orbital entanglement in FeSc2S4. To confirm this exotic ground state, experimentsmore » based on single-crystalline samples are essential. However, no such single-crystal study has been reported to date. Here, we report, to our knowledge, the first single-crystal study on the spin-orbital liquid candidate, 6H-Ba3CuSb2O9, and we have confirmed the absence of an orbital frozen state. In strongly correlated electron systems, orbital ordering usually appears at high temperatures in a process accompanied by a lattice deformation, called a static Jahn-Teller distortion. By combining synchrotron X-ray diffraction, electron spin resonance, Raman spectroscopy, and ultrasound measurements, we find that the static Jahn-Teller distortion is absent in the present material, which indicates that orbital ordering is suppressed down to the lowest temperatures measured. Lastly, we discuss how such an unusual feature is realized with the help of spin degree of freedom, leading to a spin-orbital entangled quantum liquid state.« less

New infrared-sensitive photopolymer materials for information storage and processing

NASA Astrophysics Data System (ADS)

Nagtegaele, Patrice; Galstian, Tigran V.

2001-11-01

In response to the increasing demand of information systems, we need new materials with high performance for storage and processing applications. Available on the market optical storage materials present very useful characteristics but are still limited in the visible spectrum and are expansive. Recently, we have developed holographic polymer dispersed liquid crystal (H-PDLC) materials sensitive in the near infrared region (800 nm to 850 nm). These compounds are based on acrylate monomers and different liquid crystals (LC) and allow highly efficient in-situ recording of holographic optical elements using infra red lasers. Diffraction efficiency above 95% is demonstrated. Photosensitivity of the material, its dark ­development and photochemical stability of recorded gratings are investigated. The angular and spectral selectivities of gratings, recorded in these films are examined for recovering the refractive index modulation profile.

Pattern formation in a liquid-crystal light valve with feedback, including polarization, saturation, and internal threshold effects

NASA Astrophysics Data System (ADS)

Neubecker, R.; Oppo, G.-L.; Thuering, B.; Tschudi, T.

1995-07-01

The use of liquid-crystal light valves (LCLV's) as nonlinear elements in diffractive optical systems with feedback leads to the formation of a variety of optical patterns. The spectrum of possible spatial instabilities is shown to be even richer when the LCLV's capability for polarization modulation is utilized and internal threshold and saturation effects are considered. We derive a model for the feedback system based on a realistic description of the LCLV's internal function and coupling to a polarizer. Thresholds of pattern formation are compared to the common Kerr-type approximation and show transitions involving rolls, squares, hexagons, and tiled patterns. Numerical and experimental results confirm our theoretical predictions and unveil how patterns and their typical length scales can be easily controlled by changes of the parameters.

Developments in the Implementation of Acoustic Droplet Ejection for Protein Crystallography.

PubMed

Wu, Ping; Noland, Cameron; Ultsch, Mark; Edwards, Bonnie; Harris, David; Mayer, Robert; Harris, Seth F

2016-02-01

Acoustic droplet ejection (ADE) enables crystallization experiments at the low-nanoliter scale, resulting in rapid vapor diffusion equilibration dynamics and efficient reagent usage in the empirical discovery of structure-enabling protein crystallization conditions. We extend our validation of this technology applied to the diverse physicochemical property space of aqueous crystallization reagents where dynamic fluid analysis coupled to ADE aids in accurate and precise dispensations. Addition of crystallization seed stocks, chemical additives, or small-molecule ligands effectively modulates crystallization, and we here provide examples in optimization of crystal morphology and diffraction quality by the acoustic delivery of ultra-small volumes of these cofactors. Additional applications are discussed, including set up of in situ proteolysis and alternate geometries of crystallization that leverage the small scale afforded by acoustic delivery. Finally, we describe parameters of a system of automation in which the acoustic liquid handler is integrated with a robotic arm, plate centrifuge, peeler, sealer, and stacks, which allows unattended high-throughput crystallization experimentation. © 2015 Society for Laboratory Automation and Screening.

Protein crystal growth results from the United States Microgravity Laboratory-1 mission

NASA Technical Reports Server (NTRS)

Delucas, Lawrence J.; Moore, K. M.; Vanderwoerd, M.; Bray, T. L.; Smith, C.; Carson, M.; Narayana, S. V. L.; Rosenblum, W. M.; Carter, D.; Clark, A. D, Jr.

1994-01-01

Protein crystal growth experiments have been performed by this laboratory on 18 Space Shuttle missions since April, 1985. In addition, a number of microgravity experiments also have been performed and reported by other investigators. These Space Shuttle missions have been used to grow crystals of a variety of proteins using vapor diffusion, liquid diffusion, and temperature-induced crystallization techniques. The United States Microgravity Laboratory - 1 mission (USML-1, June 25 - July 9, 1992) was a Spacelab mission dedicated to experiments involved in materials processing. New protein crystal growth hardware was developed to allow in orbit examination of initial crystal growth results, the knowledge from which was used on subsequent days to prepare new crystal growth experiments. In addition, new seeding hardware and techniques were tested as well as techniques that would prepare crystals for analysis by x-ray diffraction, a capability projected for the planned Space Station. Hardware that was specifically developed for the USML-1 mission will be discussed along with the experimental results from this mission.

Controlled In Meso Phase Crystallization – A Method for the Structural Investigation of Membrane Proteins

PubMed Central

Kubicek, Jan; Schlesinger, Ramona; Baeken, Christian; Büldt, Georg; Schäfer, Frank; Labahn, Jörg

2012-01-01

We investigated in meso crystallization of membrane proteins to develop a fast screening technology which combines features of the well established classical vapor diffusion experiment with the batch meso phase crystallization, but without premixing of protein and monoolein. It inherits the advantages of both methods, namely (i) the stabilization of membrane proteins in the meso phase, (ii) the control of hydration level and additive concentration by vapor diffusion. The new technology (iii) significantly simplifies in meso crystallization experiments and allows the use of standard liquid handling robots suitable for 96 well formats. CIMP crystallization furthermore allows (iv) direct monitoring of phase transformation and crystallization events. Bacteriorhodopsin (BR) crystals of high quality and diffraction up to 1.3 Å resolution have been obtained in this approach. CIMP and the developed consumables and protocols have been successfully applied to obtain crystals of sensory rhodopsin II (SRII) from Halobacterium salinarum for the first time. PMID:22536388

Retrieving cirrus microphysical properties from stellar aureoles

NASA Astrophysics Data System (ADS)

DeVore, J. G.; Kristl, J. A.; Rappaport, S. A.

2013-06-01

The aureoles around stars caused by thin cirrus limit nighttime measurement opportunities for ground-based astronomy, but can provide information on high-altitude ice crystals for climate research. In this paper we attempt to demonstrate quantitatively how this works. Aureole profiles can be followed out to ~0.2° from stars and ~0.5° from Jupiter. Interpretation of diffracted starlight is similar to that for sunlight, but emphasizes larger particles. Stellar diffraction profiles are very distinctive, typically being approximately flat out to a critical angle followed by gradually steepening power-law falloff with slope less steep than -3. Using the relationship between the phase function for diffraction and the average Fourier transform of the projected area of complex ice crystals, we show that defining particle size in terms of average projected area normal to the propagation direction of the starlight leads to a simple, analytic approximation representing large-particle diffraction that is nearly independent of crystal habit. A similar analytic approximation for the diffraction aureole allows it to be separated from the point spread function and the sky background. Multiple scattering is deconvolved using the Hankel transform leading to the diffraction phase function. Application of constrained numerical inversion to the phase function then yields a solution for the particle size distribution in the range between ~50 μm and ~400 μm. Stellar aureole measurements can provide one of the very few, as well as least expensive, methods for retrieving cirrus microphysical properties from ground-based observations.

A graphite crystal polarimeter for stellar X-ray astronomy.

NASA Technical Reports Server (NTRS)

Weisskopf, M. C.; Berthelsdorf, R.; Epstein, G.; Linke, R.; Mitchell, D.; Novick, R.; Wolff, R. S.

1972-01-01

The first crystal X-ray polarimeter to be used for X-ray astronomy is described. Polarization is measured by modulation of the X rays diffracted at an average 45 deg glancing angle from large, curved graphite crystal panels as these rotate about an axis parallel to the incident X-ray flux. Arrangement of the crystal panels, the design of the detector, and the signal-processing circuitry were optimized to minimize systematic effects produced by off-axis pointing of the rocket and cosmic ray induced events. The in-flight performance of the instrument in relation to the observed background signal is discussed.

Observation of Weyl points

Science.gov Websites

copolymers, liquid crystals. Experimental observation of Weyl points First public annoucement on 11 Feburary Vishwanath from University of California, Berkeley. "Experimental Observation of Weyl Semimetals" ; Published by Science on 16 July, 2015. "Experimental observation of Weyl points" Featured on the

Pyrolysis result of polyethylene waste as fuel for solid oxide fuel cell with samarium doped-ceria (SDC)-carbonate as electrolyte

NASA Astrophysics Data System (ADS)

Syahputra, R. J. E.; Rahmawati, F.; Prameswari, A. P.; Saktian, R.

2017-02-01

In this research, the result of pyrolysis on polyethylene was used as fuel for a solid oxide fuel cell (SOFC). The pyrolysis result is a liquid which consists of hydrocarbon chains. According to GC-MS analysis, the hydrocarbons mainly consist of C7 to C20 hydrocarbon chain. Then, the liquid was applied to a single cell of NSDC-L | NSDC | NSDC-L. NSDC is a composite SDC (samarium doped-ceria) with sodium carbonate. Meanwhile, NSDC-L is a composite of NSDC with LiNiCuO (LNC). NSDC and LNC were analyzed by X-ray diffraction to understand their crystal structure. The result shows that presence of carbonate did not change the crystal structure of SDC. SEM EDX analysis for fuel cell before and after being loaded with polyethylene oil to get information of element diffusion to the electrolyte. Meanwhile, the conductivity properties were investigated through impedance measurement. The presence of carbonate even increases the electrical conductivity. The single cell test with the pyrolysis result of polyethylene at 300 - 600 °C, found that the highest power density is at 600 °C with the maximum power density of 0.14 mW/cm2 and open circuit voltage of 0.4 Volt. Elemental analysis at three point spots of single cell NDSC-L |NSDC|NSDC-L found that a migration of ions was occurred during fuel operation at 300 - 600 °C.

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.

Single-shot mega-electronvolt ultrafast electron diffraction for structure dynamic studies of warm dense matter

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

Mo, M. Z., E-mail: mmo09@slac.stanford.edu; Shen, X.; Chen, Z.

We have developed a single-shot mega-electronvolt ultrafast-electron-diffraction system to measure the structural dynamics of warm dense matter. The electron probe in this system is featured by a kinetic energy of 3.2 MeV and a total charge of 20 fC, with the FWHM pulse duration and spot size at sample of 350 fs and 120 μm respectively. We demonstrate its unique capability by visualizing the atomic structural changes of warm dense gold formed from a laser-excited 35-nm freestanding single-crystal gold foil. The temporal evolution of the Bragg peak intensity and of the liquid signal during solid-liquid phase transition are quantitatively determined.more » This experimental capability opens up an exciting opportunity to unravel the atomic dynamics of structural phase transitions in warm dense matter regime.« less

Single-shot mega-electronvolt ultrafast electron diffraction for structure dynamic studies of warm dense matter

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

Mo, M. Z.; Shen, X.; Chen, Z.

We have developed a single-shot mega-electronvolt ultrafast-electron-diffraction system to measure the structural dynamics of warm dense matter. The electron probe in this system is featured by a kinetic energy of 3.2 MeV and a total charge of 20 fC, with the FWHM pulse duration and spot size at sample of 350 fs and 120 µm respectively. We demonstrate its unique capability by visualizing the atomic structural changes of warm dense gold formed from a laser-excited 35-nm freestanding single-crystal gold foil. The temporal evolution of the Bragg peak intensity and of the liquid signal during solid-liquid phase transition are quantitatively determined.more » This experimental capability opens up an exciting opportunity to unravel the atomic dynamics of structural phase transitions in warm dense matter regime« less

Single-shot mega-electronvolt ultrafast electron diffraction for structure dynamic studies of warm dense matter

DOE PAGES

Mo, M. Z.; Shen, X.; Chen, Z.; ...

2016-08-04

We have developed a single-shot mega-electronvolt ultrafast-electron-diffraction system to measure the structural dynamics of warm dense matter. The electron probe in this system is featured by a kinetic energy of 3.2 MeV and a total charge of 20 fC, with the FWHM pulse duration and spot size at sample of 350 fs and 120 µm respectively. We demonstrate its unique capability by visualizing the atomic structural changes of warm dense gold formed from a laser-excited 35-nm freestanding single-crystal gold foil. The temporal evolution of the Bragg peak intensity and of the liquid signal during solid-liquid phase transition are quantitatively determined.more » This experimental capability opens up an exciting opportunity to unravel the atomic dynamics of structural phase transitions in warm dense matter regime« less

Direct Measurement of Water States in Cryopreserved Cells Reveals Tolerance toward Ice Crystallization

PubMed Central

Huebinger, Jan; Han, Hong-Mei; Hofnagel, Oliver; Vetter, Ingrid R.; Bastiaens, Philippe I.H.; Grabenbauer, Markus

2016-01-01

Complex living systems such as mammalian cells can be arrested in a solid phase by ultrarapid cooling. This allows for precise observation of cellular structures as well as cryopreservation of cells. The state of water, the main constituent of biological samples, is crucial for the success of cryogenic applications. Water exhibits many different solid states. If it is cooled extremely rapidly, liquid water turns into amorphous ice, also called vitreous water, a glassy and amorphous solid. For cryo-preservation, the vitrification of cells is believed to be mandatory for cell survival after freezing. Intracellular ice crystallization is assumed to be lethal, but experimental data on the state of water during cryopreservation are lacking. To better understand the water conditions in cells subjected to freezing protocols, we chose to directly analyze their subcellular water states by cryo-electron microscopy and tomography, cryoelectron diffraction, and x-ray diffraction both in the cryofixed state and after warming to different temperatures. By correlating the survival rates of cells with their respective water states during cryopreservation, we found that survival is less dependent on ice-crystal formation than expected. Using high-resolution cryo-imaging, we were able to directly show that cells tolerate crystallization of extra- and intracellular water. However, if warming is too slow, many small ice crystals will recrystallize into fewer but bigger crystals, which is lethal. The applied cryoprotective agents determine which crystal size is tolerable. This suggests that cryoprotectants can act by inhibiting crystallization or recrystallization, but they also increase the tolerance toward ice-crystal growth. PMID:26541066

Structural studies of homoisoflavonoids: NMR spectroscopy, X-ray diffraction, and theoretical calculations

NASA Astrophysics Data System (ADS)

Sievänen, Elina; Toušek, Jaromír; Lunerová, Kamila; Marek, Jaromír; Jankovská, Dagmar; Dvorská, Margita; Marek, Radek

2010-08-01

In this article we present a detailed structural investigation for five homoisoflavonoids, molecules important from the pharmacological point of view. For studying the electron distribution as well as its influence on the physicochemical properties, NMR spectroscopy, X-ray diffraction, and theoretical calculations have been used. Nuclear magnetic shieldings obtained by using DFT calculations for optimized molecular geometries are correlated with the experimentally determined chemical shifts. The theoretical data are well in agreement with the experimental values. The single crystal X-ray structures of homoisoflavonoid derivatives 1, 3, and 4 have been solved. The molecular geometries and crystal packing determined by X-ray diffraction are used for characterizing the intermolecular interactions. Electron distribution is crucial for the stability of radicals and hence the antioxidant efficiency of flavonoid structures. The hydrogen bonding governs the formation of complexes of homoisoflavonoids with biological targets.

Crystal Structure Variations of Sn Nanoparticles upon Heating

NASA Astrophysics Data System (ADS)

Mittal, Jagjiwan; Lin, Kwang-Lung

2018-04-01

Structural changes in Sn nanoparticles during heating below the melting point have been investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD) analysis, electron diffraction (ED), and high-resolution transmission electron microscopy (HRTEM). DSC revealed that the heat required to melt the nanoparticles (28.43 J/g) was about half compared with Sn metal (52.80 J/g), which was attributed to the large surface energy contribution for the nanoparticles. ED and XRD analyses of the Sn nanoparticles revealed increased intensity for crystal planes having large interplaner distances compared with regular crystal planes with increasing heat treatment temperature (HTT). HRTEM revealed an increase in interlayer spacing at the surface and near joints between nanoparticles with the HTT, leading to an amorphous structure of nanoparticles at the surface at 220°C. These results highlight the changes that occur in the morphology and crystal structure of Sn nanoparticles at the surface and in the interior with increase of the heat treatment temperature.

Chromonic liquid crystalline nematic phase exhibited in binary mixture of two liquid crystals

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

Govindaiah, T. N., E-mail: tngovi.phy@gmail.com; Sreepad, H. R.; Sridhar, K. N.

2015-06-24

A binary mixture of abietic acid and orthophosphoric acid (H{sub 3}PO{sub 4}) exhibits co-existence of biphasic region of Nematic+Isotropic (N+I), lyotropic Nematic (ND) and Smectic-G (SmG) phases. The mixture exhibits N+I, N and SmG phases at different concentrations and at different temperatures. Mixtures with all concentrations of abietic acid exhibit I→N+I→N→SmG phases sequentially when the specimen is cooled from its isotropic melt. These phases have been characterized by using differential scanning calorimetric, X-ray diffraction, and optical texture studies.

X-ray characterization of curved crystals for hard x-ray astronomy

NASA Astrophysics Data System (ADS)

Buffagni, Elisa; Bonnini, Elisa; Ferrari, Claudio; Virgilli, Enrico; Frontera, Filippo

2015-05-01

Among the methods to focus photons the diffraction in crystals results as one of the most effective for high energy photons. An assembling of properly oriented crystals can form a lens able to focus x-rays at high energy via Laue diffraction in transmission geometry; this is a Laue lens. The x-ray diffraction theory provides that the maximum diffraction efficiency is achieved in ideal mosaic crystals, but real mosaic crystals show diffraction efficiencies several times lower than the ideal case due to technological problems. An alternative and convenient approach is the use of curved crystals. We have recently optimized an efficient method based on the surface damage of crystals to produce self-standing uniformly curved Si, GaAs and Ge tiles of thickness up to 2-3 mm and curvature radii R down to a few meters. We show that, for curved diffracting planes, such crystals have a diffraction efficiency nearly forty times higher than the diffraction efficiency of perfect similar flat crystals, thus very close to that of ideal mosaic crystals. Moreover, in an alternative configuration where the diffracting planes are perpendicular to the curved ones, a focusing effect occurs and will be shown. These results were obtained for several energies between 17 and 120 keV with lab sources or at high energy facilities such as LARIX at Ferrara (Italy), ESRF at Grenoble (France), and ANKA at Karlsruhe (Germany).

On the correlation between hydrogen bonding and melting points in the inositols

PubMed Central

Bekö, Sándor L.; Alig, Edith; Schmidt, Martin U.; van de Streek, Jacco

2014-01-01

Inositol, 1,2,3,4,5,6-hexahydroxycyclohexane, exists in nine stereoisomers with different crystal structures and melting points. In a previous paper on the relationship between the melting points of the inositols and the hydrogen-bonding patterns in their crystal structures [Simperler et al. (2006 ▶). CrystEngComm 8, 589], it was noted that although all inositol crystal structures known at that time contained 12 hydrogen bonds per molecule, their melting points span a large range of about 170 °C. Our preliminary investigations suggested that the highest melting point must be corrected for the effect of molecular symmetry, and that the three lowest melting points may need to be revised. This prompted a full investigation, with additional experiments on six of the nine inositols. Thirteen new phases were discovered; for all of these their crystal structures were examined. The crystal structures of eight ordered phases could be determined, of which seven were obtained from laboratory X-ray powder diffraction data. Five additional phases turned out to be rotator phases and only their unit cells could be determined. Two previously unknown melting points were measured, as well as most enthalpies of melting. Several previously reported melting points were shown to be solid-to-solid phase transitions or decomposition points. Our experiments have revealed a complex picture of phases, rotator phases and phase transitions, in which a simple correlation between melting points and hydrogen-bonding patterns is not feasible. PMID:25075320

Crystal structure and thermal expansion of a CsCe 2Cl 7 scintillator

DOE PAGES

Zhuravleva, M.; Lindsey, A.; Chakoumakos, B. C.; ...

2015-04-06

Here we used single-crystal X-ray diffraction data to determine crystal structure of CsCe 2Cl 7. It crystallizes in a P112 1/b space group with a = 19.352(1) Å, b = 19.352(1) Å, c = 14.838(1) Å, γ = 119.87(2) ° , and V = 4818.6(5) Å 3. Differential scanning calorimetry measurements combined with the structural evolution of CsCe 2Cl 7 via X-ray diffractometry over a temperature range from room temperature to the melting point indicates no obvious intermediate solid-solid phase transitions. The anisotropy in the average linear coefficient of thermal expansion of the a axis (21.3 10 -6/ °C) withmore » respect to the b and c axes (27.0 10 -6/ °C) was determined through lattice parameter refinement of the temperature dependent diffraction patterns. Lastly, these findings suggest that the reported cracking behavior during melt growth of CsCe 2Cl 7 bulk crystals using conventional Bridgman and Czochralski techniques may be largely attributed to the anisotropy in thermal expansion.« less

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.

Characterization of racemic species of chiral drugs using thermal analysis, thermodynamic calculation, and structural studies.

PubMed

Li, Z J; Zell, M T; Munson, E J; Grant, D J

1999-03-01

The identification of the racemic species, as a racemic compound, a racemic conglomerate, or a racemic solid solution (pseudoracemate), is crucial for rationalizing the potential for resolution of racemates by crystallization. The melting points and enthalpies of fusion of a number of chiral drugs and their salts were measured by differential scanning calorimetry. Based on a thermodynamic cycle involving the solid and liquid phases of the enantiomers and racemic species, the enthalpy, entropy and Gibbs free energy of the racemic species were derived from the thermal data. The Gibbs free energy of formation, is always negative for a racemic compound, if it can exist, and the contribution from the entropy of mixing in the liquid state to the free energy of formation is the driving force for the process. For a racemic conglomerate, the entropy of mixing in the liquid state is close to the ideal value of R ln 2 (1.38 cal.mol-1. K-1). Pseudoracemates behave differently from the other two types of racemic species. When the melting points of the racemic species is about 30 K below that of the homochiral species, is approximately zero, indicating that the racemic compound and racemic conglomerate possess similar relative stabilities. The powder X-ray diffraction patterns and 13C solid-state nuclear magnetic resonance spectra are valuable for revealing structural differences between a racemic compound and a racemic conglomerate. Thermodynamic prediction, thermal analysis, and structural study are in excellent agreement for identifying the nature of the racemic species.

Tunable liquid crystal photonic devices

NASA Astrophysics Data System (ADS)

Fan, Yun-Hsing

2005-07-01

Liquid crystal (LC)-based adaptive optics are important for information processing, optical interconnections, photonics, integrated optics, and optical communications due to their tunable optical properties. In this dissertation, we describe novel liquid crystal photonic devices. In Chap. 3, we demonstrate a novel electrically tunable-efficiency Fresnel lens which is devised for the first time using nanoscale PDLC. The tunable Fresnel lens is very desirable to eliminate the need of external spatial light modulator. The nanoscale LC devices are polarization independent and exhibit a fast response time. Because of the small droplet sizes, the operating voltage is higher than 100 Vrms. To lower the driving voltage, in Chap. 2 and Chap. 3, we have investigated tunable Fresnel lens using polymer-network liquid crystal (PNLC) and phase-separated composite film (PSCOF). The operating voltage is below 12 Vrms. The PNLC and PSCOF devices are polarization dependent. To overcome this shortcoming, stacking two cells with orthogonal alignment directions is a possibility. Using PNLC, we also demonstrated LC blazed grating. The diffraction efficiency of these devices is continuously controlled by the electric field. We also develop a system with continuously tunable focal length. A conventional mechanical zooming system is bulky and power hungry. In Chap. 4, we developed an electrically tunable-focus flat LC spherical lens and microlens array. A huge tunable range from 0.6 m to infinity is achieved by the applied voltage. In Chap. 5, we describe a LC microlens array whose focal length can be switched from positive to negative by the applied voltage. The fast response time feature of our LC microlens array will be very helpful in developing 3-D animated images. In Chap. 6, we demonstrate polymer network liquid crystals for switchable polarizers and optical shutters. The use of dual-frequency liquid crystal and special driving scheme leads to a sub-millisecond response time. In Chap. 7, for the first time, we demonstrate a fast-response and scattering-free homogeneously-aligned PNLC light modulator. The PNLC response time is ˜300x faster than that of a pure LC mixture. The PNLC cell also holds promise for mid and long infrared applications where response time is a critical issue.

Self-organization processes and topological defects in nanolayers in a nematic liquid crystal

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

Chuvyrov, A. N.; Girfanova, F. M.; Mal'tsev, I. S.

Atomic force microscopy is used to study the self-organization processes that occur during the formation of topological defects in nanomolecular layers in a nematic liquid crystal with the homeotropic orientation of its molecules with respect to the substrate. In this case, a smectic monolayer with a thickness of one molecule length (about 2.2 nm) forms on the substrate, and a nanomolecular layer of a nematic liquid crystal forms above this monolayer. In such virtually two-dimensional layers, numerous different nanoclusters, namely, hut structures, pyramids, raft structures with symmetry C{sub nm} (where n = 2, 4, 5, 6, 7, ?, {infinity}), cones,more » and nanopools, form [1]. They have a regular shape close to the geometry of solid crystals. Modulated linear structures and topological point defects appear spontaneously in the nanopools and raft structures.« less

Apparatus for use in examining the lattice of a semiconductor wafer by X-ray diffraction

NASA Technical Reports Server (NTRS)

Parker, D. L.; Porter, W. A. (Inventor)

1978-01-01

An improved apparatus for examining the crystal lattice of a semiconductor wafer utilizing X-ray diffraction techniques was presented. The apparatus is employed in a method which includes the step of recording the image of a wafer supported in a bent configuration conforming to a compound curve, produced through the use of a vacuum chuck provided for an X-ray camera. The entire surface thereof is illuminated simultaneously by a beam of incident X-rays which are projected from a distant point-source and satisfy conditions of the Bragg Law for all points on the surface of the water.

Novel diffraction gratings for next generation spectrographs with high spectral dispersion

NASA Astrophysics Data System (ADS)

Ebizuka, N.; Okamoto, T.; Hosobata, T.; Yamagata, Y.; Sasaki, M.; Uomoto, M.; Shimatsu, T.; Sato, S.; Hashimoto, N.; Tanaka, I.; Hattori, T.; Ozaki, S.; Aoki, W.

2016-07-01

As a transmission grating, a surface-relief (SR) grating with sawtooth shaped ridges and volume phase holographic (VPH) grating are widely used for instruments of astronomical observations. However the SR grating is difficult to achieve high diffraction efficiency at high angular dispersion, and the VPH grating has low diffraction efficiency in high diffraction orders. We propose novel gratings that solve these problems. We introduce the hybrid grism which combines a high refractive index prism with a replicated transmission grating, which has sawtooth shaped ridges of an acute apex angle. The birefringence VPH (B-VPH) grating which contains an anisotropic medium, such as a liquid crystal, achieves diffraction efficiency up to 100% at the first diffraction order for natural polarization and for circular polarization. The quasi-Bragg (QB) grating which consists of long rectangular mirrors aligned in parallel precisely, like a window blind, achieves diffraction efficiency of 60% or more in higher than the 4th diffraction order. The volume binary (VB) grating with narrow grooves also achieves diffraction efficiency of 60% or more in higher than the 6th diffraction order. The reflector facet transmission (RFT) grating which is a SR grating with sawtooth shaped ridges of an acute apex angle achieves diffraction efficiency up to 80% in higher than the 4th diffraction order.

Dynamics anomaly in high-density amorphous ice between 0.7 and 1.1 GPa

NASA Astrophysics Data System (ADS)

Handle, Philip H.; Loerting, Thomas

2016-02-01

We studied high-density amorphous ices between 0.004 and 1.6 GPa by isobaric in situ volumetry and by subsequent ex situ x-ray diffraction and differential scanning calorimetry at 1 bar. Our observations indicate two processes, namely, relaxation in the amorphous matrix and crystallization, taking place at well-separated time scales. For this reason, we are able to report rate constants of crystallization kX and glass-transition temperatures Tg in an unprecedented pressure range. Tg's agree within ±3 K with earlier work in the small pressure range where there is overlap. Both Tg and kX show a pressure anomaly between 0.7 and 1.1 GPa, namely, a kX minimum and a Tg maximum. This anomalous pressure dependence suggests a continuous phase transition from high- (HDA) to very-high-density amorphous ice (VHDA) and faster hydrogen bond dynamics in VHDA. We speculate this phenomenology can be rationalized by invoking the crossing of a Widom line between 0.7 and 1.1 GPa emanating from a low-lying HDA-VHDA critical point. Furthermore, we interpret the volumetric relaxation of the amorphous matrix to be accompanied by viscosity change to explain the findings such that the liquid state can be accessed prior to the crystallization temperature TX at <0.4 GPa and >0.8 GPa.

In meso in situ serial X-ray crystallography of soluble and membrane proteins at cryogenic temperatures

PubMed Central

Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Howe, Nicole; Vogeley, Lutz; Liu, Xiangyu; Warshamanage, Rangana; Weinert, Tobias; Panepucci, Ezequiel; Kobilka, Brian; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

2016-01-01

Here, a method for presenting crystals of soluble and membrane proteins growing in the lipid cubic or sponge phase for in situ diffraction data collection at cryogenic temperatures is introduced. The method dispenses with the need for the technically demanding and inefficient crystal-harvesting step that is an integral part of the lipid cubic phase or in meso method of growing crystals. Crystals are dispersed in a bolus of mesophase sandwiched between thin plastic windows. The bolus contains tens to hundreds of crystals, visible with an in-line microscope at macromolecular crystallography synchrotron beamlines and suitably disposed for conventional or serial crystallographic data collection. Wells containing the crystal-laden boluses are removed individually from hermetically sealed glass plates in which crystallization occurs, affixed to pins on goniometer bases and excess precipitant is removed from around the mesophase. The wells are snap-cooled in liquid nitrogen, stored and shipped in Dewars, and manually or robotically mounted on a goniometer in a cryostream for diffraction data collection at 100 K, as is performed routinely with standard, loop-harvested crystals. The method is a variant on the recently introduced in meso in situ serial crystallography (IMISX) method that enables crystallo­graphic measurements at cryogenic temperatures where crystal lifetimes are enormously enhanced whilst reducing protein consumption dramatically. The new approach has been used to generate high-resolution crystal structures of a G-protein-coupled receptor, α-helical and β-barrel transporters and an enzyme as model integral membrane proteins. Insulin and lysozyme were used as test soluble proteins. The quality of the data that can be generated by this method was attested to by performing sulfur and bromine SAD phasing with two of the test proteins. PMID:26894538

Laser-directed hierarchical assembly of liquid crystal defects and control of optical phase singularities

PubMed Central

Ackerman, Paul J.; Qi, Zhiyuan; Lin, Yiheng; Twombly, Christopher W.; Laviada, Mauricio J.; Lansac, Yves; Smalyukh, Ivan I.

2012-01-01

Topological defect lines are ubiquitous and important in a wide variety of fascinating phenomena and theories in many fields ranging from materials science to early-universe cosmology, and to engineering of laser beams. However, they are typically hard to control in a reliable manner. Here we describe facile erasable “optical drawing” of self-assembled defect clusters in liquid crystals. These quadrupolar defect clusters, stabilized by the medium's chirality and the tendency to form twisted configurations, are shaped into arbitrary two-dimensional patterns, including reconfigurable phase gratings capable of generating and controlling optical phase singularities in laser beams. Our findings bridge the studies of defects in condensed matter physics and optics and may enable applications in data storage, singular optics, displays, electro-optic devices, diffraction gratings, as well as in both optically- and electrically-addressed pixel-free spatial light modulators. PMID:22679553

Laser-Directed Hierarchical Assembly of Liquid Crystal Defects and Control of Optical Phase Singularities

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

Ackerman, P. J.; Qi, Z. Y.; Lin, Y. H.

2012-06-07

Topological defect lines are ubiquitous and important in a wide variety of fascinating phenomena and theories in many fields ranging from materials science to early-universe cosmology, and to engineering of laser beams. However, they are typically hard to control in a reliable manner. Here we describe facile erasable 'optical drawing' of self-assembled defect clusters in liquid crystals. These quadrupolar defect clusters, stabilized by the medium's chirality and the tendency to form twisted configurations, are shaped into arbitrary two-dimensional patterns, including reconfigurable phase gratings capable of generating and controlling optical phase singularities in laser beams. Our findings bridge the studies ofmore » defects in condensed matter physics and optics and may enable applications in data storage, singular optics, displays, electro-optic devices, diffraction gratings, as well as in both optically- and electrically-addressed pixel-free spatial light modulators.« less

Research on the liquid crystal adaptive optics system for human retinal imaging

NASA Astrophysics Data System (ADS)

Zhang, Lei; Tong, Shoufeng; Song, Yansong; Zhao, Xin

2013-12-01

The blood vessels only in Human eye retinal can be observed directly. Many diseases that are not obvious in their early symptom can be diagnosed through observing the changes of distal micro blood vessel. In order to obtain the high resolution human retinal images,an adaptive optical system for correcting the aberration of the human eye was designed by using the Shack-Hartmann wavefront sensor and the Liquid Crystal Spatial Light Modulator(LCLSM) .For a subject eye with 8m-1 (8D)myopia, the wavefront error is reduced to 0.084 λ PV and 0.12 λRMS after adaptive optics(AO) correction ,which has reached diffraction limit.The results show that the LCLSM based AO system has the ability of correcting the aberration of the human eye efficiently,and making the blurred photoreceptor cell to clearly image on a CCD camera.

An electrically tunable plenoptic camera using a liquid crystal microlens array.

PubMed

Lei, Yu; Tong, Qing; Zhang, Xinyu; Sang, Hongshi; Ji, An; Xie, Changsheng

2015-05-01

Plenoptic cameras generally employ a microlens array positioned between the main lens and the image sensor to capture the three-dimensional target radiation in the visible range. Because the focal length of common refractive or diffractive microlenses is fixed, the depth of field (DOF) is limited so as to restrict their imaging capability. In this paper, we propose a new plenoptic camera using a liquid crystal microlens array (LCMLA) with electrically tunable focal length. The developed LCMLA is fabricated by traditional photolithography and standard microelectronic techniques, and then, its focusing performance is experimentally presented. The fabricated LCMLA is directly integrated with an image sensor to construct a prototyped LCMLA-based plenoptic camera for acquiring raw radiation of targets. Our experiments demonstrate that the focused region of the LCMLA-based plenoptic camera can be shifted efficiently through electrically tuning the LCMLA used, which is equivalent to the extension of the DOF.

An electrically tunable plenoptic camera using a liquid crystal microlens array

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

Lei, Yu; School of Automation, Huazhong University of Science and Technology, Wuhan 430074; Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074

2015-05-15

Plenoptic cameras generally employ a microlens array positioned between the main lens and the image sensor to capture the three-dimensional target radiation in the visible range. Because the focal length of common refractive or diffractive microlenses is fixed, the depth of field (DOF) is limited so as to restrict their imaging capability. In this paper, we propose a new plenoptic camera using a liquid crystal microlens array (LCMLA) with electrically tunable focal length. The developed LCMLA is fabricated by traditional photolithography and standard microelectronic techniques, and then, its focusing performance is experimentally presented. The fabricated LCMLA is directly integrated withmore » an image sensor to construct a prototyped LCMLA-based plenoptic camera for acquiring raw radiation of targets. Our experiments demonstrate that the focused region of the LCMLA-based plenoptic camera can be shifted efficiently through electrically tuning the LCMLA used, which is equivalent to the extension of the DOF.« less

Electro-optical properties of low viscosity driven holographic polymer dispersed liquid crystals

NASA Astrophysics Data System (ADS)

Moon, K. R.; Bae, S. Y.; Kim, B. K.

2015-04-01

Relative diffraction efficiency (RDE), operating voltage, and response times are most important performance characteristics of holographic polymer dispersed liquid crystals (HPDLC). Two types of triallyl isocyanurate (TI) having different structures were incorporated into the conventional transmission grating of HPDLC. Premix viscosity decreased by 13-18% with up to 3% TI, beyond which it increased. TI eliminated induction period and augmented initial grating formation rate at all contents. Saturation RDE increased over 200% while threshold voltage and rise time decreased to about half and 2/3, respectively up to 3% TI, beyond which the tendencies were reversed. Among the two TIs, low viscosity monomer (TA) showed high RDE, while high miscibility monomer (TE) low characteristic voltages and short response times. It is concluded that grating formation is largely favored by low viscosity, while interface tensions and electro-optical performances by miscibility at similar viscosities.

An electrically tunable plenoptic camera using a liquid crystal microlens array

NASA Astrophysics Data System (ADS)

Lei, Yu; Tong, Qing; Zhang, Xinyu; Sang, Hongshi; Ji, An; Xie, Changsheng

2015-05-01

Plenoptic cameras generally employ a microlens array positioned between the main lens and the image sensor to capture the three-dimensional target radiation in the visible range. Because the focal length of common refractive or diffractive microlenses is fixed, the depth of field (DOF) is limited so as to restrict their imaging capability. In this paper, we propose a new plenoptic camera using a liquid crystal microlens array (LCMLA) with electrically tunable focal length. The developed LCMLA is fabricated by traditional photolithography and standard microelectronic techniques, and then, its focusing performance is experimentally presented. The fabricated LCMLA is directly integrated with an image sensor to construct a prototyped LCMLA-based plenoptic camera for acquiring raw radiation of targets. Our experiments demonstrate that the focused region of the LCMLA-based plenoptic camera can be shifted efficiently through electrically tuning the LCMLA used, which is equivalent to the extension of the DOF.

Three-dimensional textures and defects of soft material layering revealed by thermal sublimation.

PubMed

Yoon, Dong Ki; Kim, Yun Ho; Kim, Dae Seok; Oh, Seong Dae; Smalyukh, Ivan I; Clark, Noel A; Jung, Hee-Tae

2013-11-26

Layering is found and exploited in a variety of soft material systems, ranging from complex macromolecular self-assemblies to block copolymer and small-molecule liquid crystals. Because the control of layer structure is required for applications and characterization, and because defects reveal key features of the symmetries of layered phases, a variety of techniques have been developed for the study of soft-layer structure and defects, including X-ray diffraction and visualization using optical transmission and fluorescence confocal polarizing microscopy, atomic force microscopy, and SEM and transmission electron microscopy, including freeze-fracture transmission electron microscopy. Here, it is shown that thermal sublimation can be usefully combined with such techniques to enable visualization of the 3D structure of soft materials. Sequential sublimation removes material in a stepwise fashion, leaving a remnant layer structure largely unchanged and viewable using SEM, as demonstrated here using a lamellar smectic liquid crystal.

Mesomorphic phase transitions of 3F7HPhF studied by complementary methods

NASA Astrophysics Data System (ADS)

Deptuch, Aleksandra; Jaworska-Gołąb, Teresa; Marzec, Monika; Pociecha, Damian; Fitas, Jakub; Żurowska, Magdalena; Tykarska, Marzena; Hooper, James

2018-02-01

Physical properties and the phase sequence of (S)-4‧-(1-methylheptyloxycarbonyl)biphenyl-4-yl 4-[7-(2,2,3,3,4,4,4-heptafluorobutoxy) heptyl-1-oxy]-2-fluorobenzoate exhibiting the liquid crystalline paraelectric smectic A*, ferroelectric smectic C* and antiferroelectric smectic CA* phases were studied by complementary methods in the temperature range from -125 to 120 °C. Differential scanning calorimetry measurements together with polarizing optical microscopy provided the phase sequence, including the glass transition and a cold crystallization. X-ray diffraction was used to obtain the unit-cell parameters of the crystal phase, as well as the layer thickness and correlation length in the liquid crystalline smectic phases. The tilt angle was found to reach 45°, as determined from the measurements of the layer thickness and molecular modeling. Relaxation processes in the smectic phases and the fragility parameter were studied using frequency-domain dielectric spectroscopy.

Phononic crystal diffraction gratings

NASA Astrophysics Data System (ADS)

Moiseyenko, Rayisa P.; Herbison, Sarah; Declercq, Nico F.; Laude, Vincent

2012-02-01

When a phononic crystal is interrogated by an external source of acoustic waves, there is necessarily a phenomenon of diffraction occurring on the external enclosing surfaces. Indeed, these external surfaces are periodic and the resulting acoustic diffraction grating has a periodicity that depends on the orientation of the phononic crystal. This work presents a combined experimental and theoretical study on the diffraction of bulk ultrasonic waves on the external surfaces of a 2D phononic crystal that consists of a triangular lattice of steel rods in a water matrix. The results of transmission experiments are compared with theoretical band structures obtained with the finite-element method. Angular spectrograms (showing frequency as a function of angle) determined from diffraction experiments are then compared with finite-element simulations of diffraction occurring on the surfaces of the crystal. The experimental results show that the diffraction that occurs on its external surfaces is highly frequency-dependent and has a definite relation with the Bloch modes of the phononic crystal. In particular, a strong influence of the presence of bandgaps and deaf bands on the diffraction efficiency is found. This observation opens perspectives for the design of efficient phononic crystal diffraction gratings.

Synthesis and magnetic properties of the high-pressure scheelite-type GdCrO{sub 4} polymorph

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

Dos santos-Garcia, A.J., E-mail: adossant@quim.ucm.es; Climent-Pascual, E.; Gallardo-Amores, J.M.

The scheelite-type polymorph of GdCrO{sub 4} has been obtained from the corresponding zircon-type compound under high pressure and temperature conditions, namely 4 GPa and 803 K. The crystal structure has been determined by X-ray powder diffraction. This GdCrO{sub 4} scheelite crystallizes in a tetragonal symmetry with space group I4{sub 1}/a (No. 88, Z=4), a=5.0501(1) A, c=11.4533(2) A and V=292.099(7) A{sup 3}. The thermal decomposition leads to the formation of the zircon-polymorph as intermediate phase at 773 K to end in the corresponding GdCrO{sub 3} distorted perovskite-structure at higher temperatures. Magnetic susceptibility and magnetization measurements suggest the existence of long-range antiferromagneticmore » interactions which have been also confirmed from specific heat measurements. Neutron powder diffraction data reveal the simultaneous antiferromagnetic Gd{sup 3+} and Cr{sup 5+} ordering in the scheelite-type GdCrO{sub 4} with a T{sub N}{approx}20 K. The magnetic propagation vector was found to be k=(0 0 0). Combined with group theory analysis, the best neutron powder diffraction fit was obtained with a collinear antiferromagnetic coupling in which the m{sub Cr{sup 5}{sup +}} and m{sub Gd{sup 3}{sup +}} magnetic moments are confined in the tetragonal basal plane according to the mixed representation {Gamma}{sub 6} Circled-Plus {Gamma}{sub 8}. Thermal decomposition of the GdCrO{sub 4} high pressure polymorph, from the scheelite-type through the zircon-type structure as intermediate to end in the GdCrO{sub 3} perovskite. Highlights: Black-Right-Pointing-Pointer New high pressure GdCrO{sub 4} polymorph crystallizing in the scheelite type structure. Black-Right-Pointing-Pointer It is an antiferromagnet with a metamagnetic transition at low magnetic fields. Black-Right-Pointing-Pointer We have determined its magnetic structure from powder neutron diffraction data. Black-Right-Pointing-Pointer Otherwise, the room pressure zircon-polymorph is a ferromagnet. Black-Right-Pointing-Pointer The paper will be a great contribution in the study of 3d-4f magnetic interactions.« less

Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

PubMed

Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

2014-03-17

A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

New structure type in the mixed-valent compound YbCu4Ga8.

PubMed

Subbarao, Udumula; Gutmann, Matthias J; Peter, Sebastian C

2013-02-18

The new compound YbCu(4)Ga(8) was obtained as large single crystals in high yield from reactions run in liquid gallium. Preliminary investigations suggest that YbCu(4)Ga(8) crystallizes in the CeMn(4)Al(8) structure type, tetragonal space group I4/mmm, and lattice constants are a = b = 8.6529(4) Å and c = 5.3976(11) Å. However, a detailed single-crystal XRD revealed a tripling of the c axis and crystallizing in a new structure type with lattice constants of a = b = 8.6529(4) Å and c = 15.465(1) Å. The structural model was further confirmed by neutron diffraction measurements on high-quality single crystal. The crystal structure of YbCu(4)Ga(8) is composed of pseudo-Frank-Kasper cages occupying one ytterbium atom in each ring which are shared through the corner along the ab plane, resulting in a three-dimensional network. The magnetic susceptibility of YbCu(4)Ga(8) investigated in the temperature range 2-300 K showed Curie-Weiss law behavior above 100 K, and the experimentally measured magnetic moment indicates mixed-valent ytterbium. Electrical resistivity measurements show the metallic nature of the compound. At low temperatures, variation of ρ as a function of T indicates a possible Fermi-liquid state at low temperatures.

Promoting crystallisation of the Salmonella enteritidis fimbriae 14 pilin SefD using deuterium oxide

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

Liu, Bing; Garnett, James A.; Lee, Wei-chao

Highlights: Black-Right-Pointing-Pointer The benefits of D{sub 2}O in screening for crystallisation was explored. Black-Right-Pointing-Pointer The crystal structures of the SefD pilin in both H{sub 2}O and D{sub 2}O reveal differences. Black-Right-Pointing-Pointer Crystallisation improvements are explained by altered interactions in D{sub 2}O crystals. Black-Right-Pointing-Pointer D{sub 2}O is useful additive in sparse-matrix screening for crystallisation. -- Abstract: The use of heavy water (D{sub 2}O) as a solvent is commonplace in many spectroscopic techniques for the study of biological macromolecules. A significant deuterium isotope effect exists where hydrogen-bonding is important, such as in protein stability, dynamics and assembly. Here we illustrate the usemore » of D{sub 2}O in additive screening for the production of reproducible diffraction-quality crystals for the Salmonella enteritidis fimbriae 14 (SEF14) putative tip adhesin, SefD.« less

Liquid Crystal on Silicon Wavefront Corrector

NASA Technical Reports Server (NTRS)

Pouch, John; Miranda, Felix; Wang, Xinghua; Bos, Philip, J.

2004-01-01

A low cost, high resolution, liquid crystal on silicon, spatial light modulator has been developed for the correction of huge aberrations in an optical system where the polarization dependence and the chromatic nature are tolerated. However, the overall system performance suggests that this device is also suitable for real time correction of aberration in human eyes. This device has a resolution of 1024 x 768, and is driven by an XGA display driver. The effective stroke length of the device is 700 nm and 2000 nm for the visible and IR regions of the device, respectively. The response speeds are 50 Hz and 5 Hz, respectively, which are fast enough for real time adaptive optics for aberrations in human eyes. By modulating a wavefront of 2 pi, this device can correct for arbitrary high order wavefront aberrations since the 2-D pixel array is independently controlled by the driver. The high resolution and high accuracy of the device allow for diffraction limited correction of the tip and tilt or defocus without an additional correction loop. We have shown that for every wave of aberration, an 8 step blazed grating is required to achieve high diffraction efficiency around 80%. In light of this, up to 125 waves peak to valley of tip and tilt can be corrected if we choose the simplest aberration. Corrections of 34 waves of aberration, including high order Zernicke terms in a high magnification telescope, to diffraction limited performance (residual wavefront aberration less than 1/30 lambda at 632.8 nm) have been observed at high efficiency.

Syntheses, structures and luminescent properties of two novel Zn (II) coordination polymers

NASA Astrophysics Data System (ADS)

Huang, Ya-Ru; Gao, Ling-Ling; Wang, Xiao-Qing; Fan, Li-Ming; Hu, Tuo-Ping

2018-02-01

Two new coordination polymers, namely [Zn(TZMB)]n (1) and {[Zn(TZMB)](H2TZMB)]·(C2H5OH)0.5(H2O)2.5}n (2), (H2TZMB = 4,4‧-(1H-1,2,4-triazol-1-yl)methylene-bis(benzonic acid), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analysis, elemental analysis (EA), IR spectrum analysis (IR), powder X-ray diffraction (PXRD), and thermogravimetric (TG) analysis. Single X-ray diffraction analysis reveals that complex 1 is a 3D 3,6-connected net with the point symbol of (6110.84)(63)2 and complex 2 is a 2D 3-connected net with the point symbol of (63). Furthermore, luminescent properties of complexes 1 and 2 were also investigated in detail.

Microscopic structural change in a liquid Fe-C alloy of ~5 GPa

DOE PAGES

Shibazaki, Yuki; Kono, Yoshio; Fei, Yingwei

2015-07-04

The structure of a liquid Fe-3.5 wt% C alloy is examined for up to 7.2 GPa via multiangle energy-dispersive X-ray diffraction using a Paris-Edinburgh type large-volume press. X-ray diffraction data show clear changes in the pressure-dependent peak positions of structure factor and reduced pair distribution function at 5GPa. These results suggest that the liquid Fe-3.5wt%C alloys change structurally at approximately 5GPa. This finding serves as a microscopic explanation for the alloy’s previously observed density change at the same pressure. The pressure dependencies of the nearest and second neighbor distances of the liquid Fe-3.5 wt% C alloy are similar to thosemore » of liquid Fe which exhibits a structural change near the bcc-fcc-liquid triple point (5.2GPa and 1991 K). Here, similarities between Fe-3.5wt% C and Fe suggest that a density change also occurs in liquid Fe and that this structural change extends to other Fe-light element alloys.« less

The role of ultrasound in controlling the liquid-liquid phase separation and nucleation of vanillin polymorphs I and II

NASA Astrophysics Data System (ADS)

Parimaladevi, P.; Supriya, S.; Srinivasan, K.

2018-02-01

The influence of ultrasound on liquid-liquid phase separation (LLPS) and polymorphism of vanillin in aqueous solution has been investigated for the first time by varying the ultrasonic parameters such as power, pulse rate and insonation time at ambient condition. Results reveal that the application of ultrasound controls the impact of LLPS and accelerates the nucleation of vanillin within a short period at lower levels of ultrasonic process parameters, and also enhances the quality of the nucleated crystals. Moreover, the application of ultrasound induces the nucleation of rare and metastable polymorph of vanillin Form II in aqueous solution. But, at higher levels of power, pulse rate and insonation time, the rate of LLPS is found increased and the quality of the crystals becomes deteriorated. Morphology of the nucleated polymorphs were identified through optical microscopy and confirmed by optical goniometry. The internal structure and thermal stability of the grown stable Form I and metastable Form II of vanillin were confirmed through powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) analyses. Further, results suggest that the ultrasound has profound effect in controlling the LLPS and nucleation of vanillin polymorphs in aqueous solution.

Growth and characterization of an organic single crystal: 2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide

NASA Astrophysics Data System (ADS)

Senthil, K.; Kalainathan, S.; Ruban Kumar, A.

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. 1H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker’s hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal.

Growth and characterization of an organic single crystal: 2-[2-(4-diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide.

PubMed

Senthil, K; Kalainathan, S; Ruban Kumar, A

2014-05-05

Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. (1)H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker's hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal. Copyright © 2014 Elsevier B.V. All rights reserved.

Polymer-directed crystallization of atorvastatin.

PubMed

Choi, Hyemin; Lee, Hyeseung; Lee, Min Kyung; Lee, Jonghwi

2012-08-01

Living organisms secrete minerals composed of peptides and proteins, resulting in "mesocrystals" of three-dimensional-assembled composite structures. Recently, this biomimetic polymer-directed crystallization technique has been widely applied to inorganic materials, although it has seldom been used with drugs. In this study, the technique was applied to the drowning-out crystallization of atorvastatin using various polymers. Nucleation and growth at optimized conditions successfully produced composite crystals with significant polymer contents and unusual characteristics. Atorvastatin composite crystals containing polyethylene glycol, polyacrylic acid, polyethylene imine, and chitosan showed a markedly decreased melting point and heat of fusion, improved stability, and sustained-release patterns. The use of hydroxypropyl cellulose yielded a unique combination of enhanced in vitro release and improved drug stability under a forced degradation condition. The formation hypothesis of unique mesocrystal structures was strongly supported by an X-ray diffraction pattern and substantial melting point reduction. This polymer-directed crystallization technique offers a novel and effective way, different from the solid dispersion approach, to engineer the release, stability, and processability of drug crystals. Copyright © 2012 Wiley Periodicals, Inc.

Alkyltributylphosphonium chloride ionic liquids: synthesis, physicochemical properties and crystal structure.

PubMed

Adamová, Gabriela; Gardas, Ramesh L; Nieuwenhuyzen, Mark; Puga, Alberto V; Rebelo, Luís Paulo N; Robertson, Allan J; Seddon, Kenneth R

2012-07-21

A series of alkyltributylphosphonium chloride ionic liquids, prepared from tributylphosphine and the respective 1-chloroalkane, C(n)H(2n+1)Cl (where n = 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12 or 14), is reported. This work is a continuation of an extended series of tetraalkylphosphonium ionic liquids, where the focus is on the variability of n and its impact on the physical properties, such as melting points/glass transitions, thermal stability, density and viscosity. Experimental density and viscosity data were interpreted using QPSR and group contribution methods and the crystal structure of propyl(tributyl)phosphonium chloride is detailed.

Retinal axial focusing and multi-layer imaging with a liquid crystal adaptive optics camera

NASA Astrophysics Data System (ADS)

Liu, Rui-Xue; Zheng, Xian-Liang; Li, Da-Yu; Xia, Ming-Liang; Hu, Li-Fa; Cao, Zhao-Liang; Mu, Quan-Quan; Xuan, Li

2014-09-01

With the help of adaptive optics (AO) technology, cellular level imaging of living human retina can be achieved. Aiming to reduce distressing feelings and to avoid potential drug induced diseases, we attempted to image retina with dilated pupil and froze accommodation without drugs. An optimized liquid crystal adaptive optics camera was adopted for retinal imaging. A novel eye stared system was used for stimulating accommodation and fixating imaging area. Illumination sources and imaging camera kept linkage for focusing and imaging different layers. Four subjects with diverse degree of myopia were imaged. Based on the optical properties of the human eye, the eye stared system reduced the defocus to less than the typical ocular depth of focus. In this way, the illumination light can be projected on certain retina layer precisely. Since that the defocus had been compensated by the eye stared system, the adopted 512 × 512 liquid crystal spatial light modulator (LC-SLM) corrector provided the crucial spatial fidelity to fully compensate high-order aberrations. The Strehl ratio of a subject with -8 diopter myopia was improved to 0.78, which was nearly close to diffraction-limited imaging. By finely adjusting the axial displacement of illumination sources and imaging camera, cone photoreceptors, blood vessels and nerve fiber layer were clearly imaged successfully.

Liquid crystal based optical platform for the detection of Pb2+ ions using NiFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Zehra, Saman; Gul, Iftikhar Hussain; Hussain, Zakir

2018-06-01

A simple, sensitive, selective and real time detection protocol was developed for Pb2+ ions in water using liquid crystals (LCs). In this method, NiFe2O4 nanoparticles were synthesized using chemical co-precipitation method. Crystallite size, morphological, functional groups and magnetization studies were confirmed using X-ray diffraction, Scanning Electron Microscopy, and Fourier transform infrared spectroscopy techniques, respectively. The nanoparticles were mono dispersed with average particle size of 20 ± 2 nm. The surfactant stabilized magnetic nanoparticles were incubated in liquid crystal based sensor system for the detection of Pb+2 ions. The bright to dark transition of LC was observed through optical microscope. When this system was further immersed with a solution containing Pb2+ ions, it caused homeotropic to planar orientation of LC. This interaction is attributed to the presence of abundant hydroxyl groups in such as M-OH, Fe-OH on the surface of spinel ferrites nanoparticles. These groups interact with metal ions at aqueous interface, causing disruption in LCs orientation giving bright texture. This sensor showed higher selectivity towards Pb2+ ions. The detection limit was estimated to be 100 ppb. The cheap and effective protocol reported here should make promising development of LC based sensor for lead ion detection.

Femtosecond X-ray Diffraction From Two-Dimensional Protein Crystals

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

Frank, Matthias; Carlson, David B.; Hunter, Mark

2014-02-28

Here we present femtosecond x-ray diffraction patterns from two-dimensional (2-D) protein crystals using an x-ray free electron laser (XFEL). To date it has not been possible to acquire x-ray diffraction from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permits a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy methodology at the Linac Coherent Light Source, we observed Bragg diffraction to better than 8.5 Å resolution for two different 2-D protein crystal samples that were maintained at room temperature. These proof-of-principle results show promisemore » for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.« less

Neutron diffraction study of water freezing on aircraft engine combustor soot.

PubMed

Tishkova, V; Demirdjian, B; Ferry, D; Johnson, M

2011-12-14

The study of the formation of condensation trails and cirrus clouds on aircraft emitted soot particles is important because of its possible effects on climate. In the present work we studied the freezing of water on aircraft engine combustor (AEC) soot particles under conditions of pressure and temperature similar to the upper troposphere. The microstructure of the AEC soot was found to be heterogeneous containing both primary particles of soot and metallic impurities (Fe, Cu, and Al). We also observed various surface functional groups such as oxygen-containing groups, including sulfate ions, that can act as active sites for water adsorption. Here we studied the formation of ice on the AEC soot particles by using neutron diffraction. We found that for low amount of adsorbed water, cooling even up to 215 K did not lead to the formation of hexagonal ice. Whereas, larger amount of adsorbed water led to the coexistence of liquid water (or amorphous ice) and hexagonal ice (I(h)); 60% of the adsorbed water was in the form of ice I(h) at 255 K. Annealing of the system led to the improvement of the crystal quality of hexagonal ice crystals as demonstrated from neutron diffraction.

Solubility of carbamazepine co-crystals in ethanolic solution

NASA Astrophysics Data System (ADS)

Ramle, Noor Ashila; Rahim, Syarifah Abd; Anuar, Nornizar; El-Hadad, Omar

2017-08-01

The study aimed to determine the solubility of carbamazepine (CBZ) co-crystals formed from co-crystal formers (CCFs) of nicotinamide (NIC), saccharin (SAC), succinic acid (SUC) and fumaric acid (FUM) at various temperatures (25-50°C). High Performance Liquid Chromatography (HPLC) was used to determine the solubility and the X-Ray Powder Diffraction was used to characterize the crystals. The solubility of CBZ-NIC and CBZ-FUM co-crystals were found to be higher than the solubility of the CBZ for the range of studied temperatures. However, opposite findings was obtained for CBZ-SUC co-crystal as its solubility is lower than the solubility of CBZ. Different trend was found for CBZ-SAC co-crystal in which for temperature lower than 40°C, the solubility of CBZ crystal is higher than the CBZ-SAC co-crystal. The solubility of CBZ-SAC co-crystal is higher than the solubility of CBZ at a temperature above 40°C. CBZ co-crystals with NIC and FUM have shown to increase the solubility of CBZ by solubility ratio of 1.95 and 1.24 respectively. However, the CBZ co-crystal with SAC was found to have similar solubility value as the CBZ.

Nature of the anomalies in the supercooled liquid state of the mW model of water.

PubMed

Holten, Vincent; Limmer, David T; Molinero, Valeria; Anisimov, Mikhail A

2013-05-07

The thermodynamic properties of the supercooled liquid state of the mW model of water show anomalous behavior. Like in real water, the heat capacity and compressibility sharply increase upon supercooling. One of the possible explanations of these anomalies, the existence of a second (liquid-liquid) critical point, is not supported by simulations for this model. In this work, we reproduce the anomalies of the mW model with two thermodynamic scenarios: one based on a non-ideal "mixture" with two different types of local order of the water molecules, and one based on weak crystallization theory. We show that both descriptions accurately reproduce the model's basic thermodynamic properties. However, the coupling constant required for the power laws implied by weak crystallization theory is too large relative to the regular backgrounds, contradicting assumptions of weak crystallization theory. Fluctuation corrections outside the scope of this work would be necessary to fit the forms predicted by weak crystallization theory. For the two-state approach, the direct computation of the low-density fraction of molecules in the mW model is in agreement with the prediction of the phenomenological equation of state. The non-ideality of the "mixture" of the two states never becomes strong enough to cause liquid-liquid phase separation, also in agreement with simulation results.

Nature of the anomalies in the supercooled liquid state of the mW model of water

NASA Astrophysics Data System (ADS)

Holten, Vincent; Limmer, David T.; Molinero, Valeria; Anisimov, Mikhail A.

2013-05-01

The thermodynamic properties of the supercooled liquid state of the mW model of water show anomalous behavior. Like in real water, the heat capacity and compressibility sharply increase upon supercooling. One of the possible explanations of these anomalies, the existence of a second (liquid-liquid) critical point, is not supported by simulations for this model. In this work, we reproduce the anomalies of the mW model with two thermodynamic scenarios: one based on a non-ideal "mixture" with two different types of local order of the water molecules, and one based on weak crystallization theory. We show that both descriptions accurately reproduce the model's basic thermodynamic properties. However, the coupling constant required for the power laws implied by weak crystallization theory is too large relative to the regular backgrounds, contradicting assumptions of weak crystallization theory. Fluctuation corrections outside the scope of this work would be necessary to fit the forms predicted by weak crystallization theory. For the two-state approach, the direct computation of the low-density fraction of molecules in the mW model is in agreement with the prediction of the phenomenological equation of state. The non-ideality of the "mixture" of the two states never becomes strong enough to cause liquid-liquid phase separation, also in agreement with simulation results.

Diffraction Correlation to Reconstruct Highly Strained Particles

NASA Astrophysics Data System (ADS)

Brown, Douglas; Harder, Ross; Clark, Jesse; Kim, J. W.; Kiefer, Boris; Fullerton, Eric; Shpyrko, Oleg; Fohtung, Edwin

2015-03-01

Through the use of coherent x-ray diffraction a three-dimensional diffraction pattern of a highly strained nano-crystal can be recorded in reciprocal space by a detector. Only the intensities are recorded, resulting in a loss of the complex phase. The recorded diffraction pattern therefore requires computational processing to reconstruct the density and complex distribution of the diffracted nano-crystal. For highly strained crystals, standard methods using HIO and ER algorithms are no longer sufficient to reconstruct the diffraction pattern. Our solution is to correlate the symmetry in reciprocal space to generate an a priori shape constraint to guide the computational reconstruction of the diffraction pattern. This approach has improved the ability to accurately reconstruct highly strained nano-crystals.

Impact of Heterogeneity and Lattice Bond Strength on DNA Triangle Crystal Growth.

PubMed

Stahl, Evi; Praetorius, Florian; de Oliveira Mann, Carina C; Hopfner, Karl-Peter; Dietz, Hendrik

2016-09-07

One key goal of DNA nanotechnology is the bottom-up construction of macroscopic crystalline materials. Beyond applications in fields such as photonics or plasmonics, DNA-based crystal matrices could possibly facilitate the diffraction-based structural analysis of guest molecules. Seeman and co-workers reported in 2009 the first designed crystal matrices based on a 38 kDa DNA triangle that was composed of seven chains. The crystal lattice was stabilized, unprecedentedly, by Watson-Crick base pairing. However, 3D crystallization of larger designed DNA objects that include more chains such as DNA origami remains an unsolved problem. Larger objects would offer more degrees of freedom and design options with respect to tailoring lattice geometry and for positioning other objects within a crystal lattice. The greater rigidity of multilayer DNA origami could also positively influence the diffractive properties of crystals composed of such particles. Here, we rationally explore the role of heterogeneity and Watson-Crick interaction strengths in crystal growth using 40 variants of the original DNA triangle as model multichain objects. Crystal growth of the triangle was remarkably robust despite massive chemical, geometrical, and thermodynamical sample heterogeneity that we introduced, but the crystal growth sensitively depended on the sequences of base pairs next to the Watson-Crick sticky ends of the triangle. Our results point to weak lattice interactions and high concentrations as decisive factors for achieving productive crystallization, while sample heterogeneity and impurities played a minor role.

Optical determination of crystal phase in semiconductor nanocrystals

PubMed Central

Lim, Sung Jun; Schleife, André; Smith, Andrew M.

2017-01-01

Optical, electronic and structural properties of nanocrystals fundamentally derive from crystal phase. This is especially important for polymorphic II–VI, III–V and I-III-VI2 semiconductor materials such as cadmium selenide, which exist as two stable phases, cubic and hexagonal, each with distinct properties. However, standard crystallographic characterization through diffraction yields ambiguous phase signatures when nanocrystals are small or polytypic. Moreover, diffraction methods are low-throughput, incompatible with solution samples and require large sample quantities. Here we report the identification of unambiguous optical signatures of cubic and hexagonal phases in II–VI nanocrystals using absorption spectroscopy and first-principles electronic-structure theory. High-energy spectral features allow rapid identification of phase, even in small nanocrystals (∼2 nm), and may help predict polytypic nanocrystals from differential phase contributions. These theoretical and experimental insights provide simple and accurate optical crystallographic analysis for liquid-dispersed nanomaterials, to improve the precision of nanocrystal engineering and improve our understanding of nanocrystal reactions. PMID:28513577

Crystals for astronomical X-ray spectroscopy

NASA Technical Reports Server (NTRS)

Burek, A.

1976-01-01

Crystal spectrometric properties and the factors that affect their measurement are discussed. Theoretical and experimental results on KAP are summarized and theoretical results based on the dynamical theory of X-ray diffraction are given for the acid phthalates as well as for the commonly used planes of ADP, PET and EDDT. Anomalous dispersion is found to be important for understanding the details of crystal Bragg reflection properties at long X-ray wavelengths and some important effects are pointed out. The theory of anomalous dispersion is applied to explain the anomalous reflectivity exhibited by KAP at 23.3 A.

Anisotropic stress inhibits crystallization in Cu-Zr glass-forming liquids

NASA Astrophysics Data System (ADS)

Pang, H. H.; Bi, Q. L.; Huang, H. S.; Lü, Y. J.

2017-12-01

Liquids attain a metastable state without crystallizing by cooling rapidly to a given temperature below the melting point. With increasing supercooling, the nucleation rate would show an increase based on the prediction of the classical nucleation theory. It is generally thought that the nucleation rate will reach the maximum upon approaching the glass transition temperature, Tg, for glass-forming liquids. We report that there exists a supercooled region above Tg in which the crystallization has actually been severely suppressed. Our molecular dynamics simulations show that the growth of embryos in the supercooled Cu60Zr40 melt is subjected to a strong anisotropic stress associated with the dynamic heterogeneity. Its long-range effect drives the embryo to grow into a ramified morphology so that the interface energy dominates over the embryo growth, leading to the suppression of nucleation.

Grazing-incidence X-ray diffraction from a crystal with subsurface defects

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

Gaevskii, A. Yu., E-mail: transilv@mail.ru; Golentus, I. E.

2015-03-15

The diffraction of X rays incident on a crystal surface under grazing angles under conditions of total external reflection has been investigated. An approach is proposed in which exact solutions to the dynamic problem of grazing-incidence diffraction in an ideal crystal are used as initial functions to calculate the diffuse component of diffraction in a crystal with defects. The diffuse component of diffraction is calculated for a crystal with surface defects of a dilatation-center type. Exact formulas of the continuum theory which take into account the mirror-image forces are used for defect-induced atomic displacements. Scattering intensity maps near Bragg peaksmore » are constructed for different scan modes, and the conditions for detecting primarily the diffuse component are determined. The results of dynamic calculations of grazing-incidence diffraction in defect-containing crystals are compared with calculations in the kinematic approximation.« less

Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

NASA Technical Reports Server (NTRS)

Judge, R. A.; Kephart, R.; Leardi, R.; Myles, D. A.; Snell, E. H.; vanderWoerd, M.; Curreri, Peter A. (Technical Monitor)

2002-01-01

A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

Optical-diffraction method for determining crystal orientation

DOEpatents

Sopori, B.L.

1982-05-07

Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

Effects of ionic liquid to water ratio as a composite medium for the synthesis of LiFePO4 for battery

NASA Astrophysics Data System (ADS)

Tith, Rany; Dutta, Jaydeep; Jung, Kichang; Martinez-Morales, Alfredo A.

2017-05-01

LiFePO4 is a highly researched cathode material that serves as an alternative material for traditional commercial lithiumion batteries such as LiCoO2. Currently, there are a number of different methods to synthesize LiFePO4 including: hydrothermal, solid state, spray pyrolysis, and coprecipitation. Our proposed method has the potential to provide an ecologically friendly and economically competitive way to synthesize LiFePO4 by utilizing ionic liquid and water, as a composite synthesis medium. The addition of water to ionic liquid can be beneficial as it can act as a mineralizer to bring insoluble precursors to form LiFePO4 seed crystals. Furthermore, this method provides the possibility of recycling the ionic liquid for repeated synthesis processes. In this work, we study the effects of ionic liquid to water ratio on the crystallinity and morphology of the synthesized material. Our group was able to conclude a reaction medium utilizing a ratio of equal parts of 1-ethyl-3-methyl imidazolium trifluoromethane sulfonate (EMIM Otf) and water, or a slightly favored ionic liquid ratio, increases the efficacy of the synthesis route. Crystallinity and purity was determined by X-ray diffraction (XRD), scanning electron microscopy (SEM) was used to determine morphology and crystal sizes, and energy dispersion spectroscopy (EDX) was used for elemental analysis.

Crystallization and preliminary X-ray analysis of the ergothioneine-biosynthetic methyltransferase EgtD.

PubMed

Vit, Allegra; Misson, Laëtitia; Blankenfeldt, Wulf; Seebeck, Florian Peter

2014-05-01

Ergothioneine is an amino-acid betaine derivative of histidine that was discovered more than one century ago. Despite significant research pointing to a function in oxidative stress defence, the exact mechanisms of action of ergothioneine remain elusive. Although both humans and bacterial pathogens such as Mycobacterium tuberculosis seem to depend on ergothioneine, humans are devoid of the corresponding biosynthetic enzymes. Therefore, its biosynthesis may emerge as potential drug target in the development of novel therapeutics against tuberculosis. The recent identification of ergothioneine-biosynthetic genes in M. smegmatis enables a more systematic study of its biology. The pathway is initiated by EgtD, a SAM-dependent methyltransferase that catalyzes a trimethylation reaction of histidine to give N(α),N(α),N(α)-trimethylhistidine. Here, the recombinant production, purification and crystallization of EgtD are reported. Crystals of native EgtD diffracted to 2.35 Å resolution at a synchrotron beamline, whereas crystals of seleno-L-methionine-labelled protein diffracted to 1.75 Å resolution and produced a significant anomalous signal to 2.77 Å resolution at the K edge. All of the crystals belonged to space group P212121, with two EgtD monomers in the asymmetric unit.

Synthesis and carbon-13 NMR studies of liquid crystals

NASA Astrophysics Data System (ADS)

Sun, Hong

2000-08-01

The orientation of different segments of 4'-cyanophenyl 4-heptylbenzoate (7CPB) has been investigated using 13C NMR. The method of proton encoded local field (PELF) spectroscopy was used in combination with off-magic-angle spinning (OMAS) of the sample. High-resolution 2D spectra were obtained and the order parameters were calculated from the spectra. Linear relationships between the obtained order parameters and anisotropic chemical shifts determined by 1D 13C NMR were established and semi-empirical parameters were obtained. A 1:2 mixture of 7CPB and its chain-perfluorinated analog (7PFCPB) shows interesting phase behavior with changing of temperature. The mixture was studied by the use of 13C NMR and polarizing optical microscopy. The order parameters of 7CPB in the smectic A phase of the mixture were calculated using the semi-empirical parameters obtained by the 2D NMR method. Eight series of liquid crystals containing an electron- donating group at one end of a conjugated system and an electron-withdrawing group at the other end have been synthesized. The electron-donating group is 4- n-alkylpiperazinyl group, the electron- withdrawing group is nitro group and the conjugated system is diphenyldiazene with zero, one or two substituents on the phenyl rings. The substituents are -F, -Cl, and -CH3. Two series of compounds with cyano group as electron-withdrawing group were also synthesized. Most of the compounds synthesized are nematogenic and exhibit rather broad liquid crystalline ranges. The effects of the lateral substituents on the optical absorption and phase transition temperatures are correlated with their nature and position of substitution. Birefringence, dielectric anisotropy, elastic constant ratio and rise time of the liquid crystals were carried out using 10 wt% LC mixtures in E7. It has been found that lateral substituents have subtle effects on the properties. The presence of lateral substituents depresses melting points and clearing points of the liquid crystals. All the liquid crystals synthesized in this work have relatively large values of birefiringence, although the dielectric anisotropy values were not as high as desired. The incorporation of a fluorine atom onto the position neighboring the nitro group enhances the conjugation of the push-pull system and liquid crystals with better physical properties were obtained.

Optical devices combining an organic semiconductor crystal with a two-dimensional inorganic diffraction grating

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

Kitazawa, Takenori; Yamao, Takeshi, E-mail: yamao@kit.ac.jp; Hotta, Shu

2016-02-01

We have fabricated optical devices using an organic semiconductor crystal as an emission layer in combination with a two-dimensional (2D) inorganic diffraction grating used as an optical cavity. We formed the inorganic diffraction grating by wet etching of aluminum-doped zinc oxide (AZO) under a 2D cyclic olefin copolymer (COC) diffraction grating used as a mask. The COC diffraction grating was fabricated by nanoimprint lithography. The AZO diffraction grating was composed of convex prominences arranged in a triangular lattice. The organic crystal placed on the AZO diffraction grating indicated narrowed peaks in its emission spectrum under ultraviolet light excitation. These aremore » detected parallel to the crystal plane. The peaks were shifted by rotating the optical devices around the normal to the crystal plane, which reflected the rotational symmetries of the triangular lattice through 60°.« less

Modified Bridgman-Stockbarger growth and characterization of LiInSe{sub 2} single crystal

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

Vijayakumar, P., E-mail: ramasamyp@ssn.edu.in; Magesh, M., E-mail: ramasamyp@ssn.edu.in; Arunkumar, A., E-mail: ramasamyp@ssn.edu.in

2014-04-24

The LiInSe{sub 2} polycrystalline materials were successfully synthesized from melt and temperature oscillation method. 8 mm diameter and 32 mm length single crystal was grown from Bridgman-Stockbarger method with steady ampoule rotation. Crystalline phase was confirmed by powder XRD pattern. Thermo gravimetric and differential thermal analysis confirms that the melting point of the grown crystal is 897°C. Rutherford backscattering analysis (RBS) gives the crystal composition as Li{sub 0.8}In{sub 1.16}Se{sub 2.04}. The crystalline perfection of the grown crystal was analyzed by High resolution X-ray diffraction measurements (HRXRD). The electrical properties of the grown crystal were analyzed by Hall effect measurements andmore » it confirms the n-type semiconducting nature.« less

USAXS analysis of concentration-dependent self-assembling of polymer-brush-modified nanoparticles in ionic liquid: [I] concentrated-brush regime

NASA Astrophysics Data System (ADS)

Nakanishi, Yohei; Ishige, Ryohei; Ogawa, Hiroki; Sakakibara, Keita; Ohno, Kohji; Morinaga, Takashi; Sato, Takaya; Kanaya, Toshiji; Tsujii, Yoshinobu

2018-03-01

Using ultra-small angle X-ray scattering (USAXS), we analyzed the higher-order structures of nanoparticles with a concentrated brush of an ionic liquid (IL)-type polymer (concentrated-polymer-brush-modified silica particle; PSiP) in an IL and the structure of the swollen shell layer of PSiP. Homogeneous mixtures of PSiP and IL were successfully prepared by the solvent-casting method involving the slow evaporation of a volatile solvent, which enabled a systematic study over an exceptionally wide range of compositions. Different diffraction patterns as a function of PSiP concentration were observed in the USAXS images of the mixtures. At suitably low PSiP concentrations, the USAXS intensity profile was analyzed using the Percus-Yevick model by matching the contrast between the shell layer and IL, and the swollen structure of the shell and "effective diameter" of the PSiP were evaluated. This result confirms that under sufficiently low pressures below and near the liquid/crystal-threshold concentration, the studied PSiP can be well described using the "hard sphere" model in colloidal science. Above the threshold concentration, the PSiP forms higher-order structures. The analysis of diffraction patterns revealed structural changes from disorder to random hexagonal-closed-packing and then face-centered-cubic as the PSiP concentration increased. These results are discussed in terms of thermodynamically stable "hard" and/or "semi-soft" colloidal crystals, wherein the swollen layer of the concentrated polymer brush and its structure play an important role.

Interaction of copper with dinitrogen tetroxide in 1-butyl-3-methylimidazolium-based ionic liquids.

PubMed

Morozov, I V; Deeva, E B; Glazunova, T Yu; Troyanov, S I; Guseinov, F I; Kustov, L M

2017-03-27

Ionic liquids that are stable toward oxidation and nitration and are based on the 1-n-butyl-3-methylimidazolium cation (BMIm + ) can be used as solvents and reaction media for copper dissolution in liquid dinitrogen tetraoxide N 2 O 4 . The ionic liquid not only favors the dissociation of N 2 O 4 into NO + and NO 3 - , but also takes part in the formation of different crystalline products. Thus, NO[BF 4 ], NO[Cu(NO 3 ) 3 ] and (BMIm) 2 [Cu 2 (CF 3 COO) 6 ] were prepared using (BMIm)A, A - = [BF 4 ] - , (CF 3 SO 2 ) 2 N - , CF 3 COO - , respectively. The formation of a certain product is determined by the nature of the anion A - and the relative solubility of the reaction products in the ionic liquid. Crystals of NO[BF 4 ] were also prepared directly from a mixture of N 2 O 4 and BMImBF 4 . According to XRD single-crystal structure analysis, the structure of NO[BF 4 ] consists of tetrahedral [BF 4 ] - anions and nitrosonium NO + cations; the formation of these ions prove the heterolytic dissociation of N 2 O 4 dissolved in the ionic liquid. The crystal structure of the earlier unknown binuclear copper trifluoroacetate (BMIm) 2 [Cu 2 (CF 3 COO) 6 ] were determined by X-ray diffraction. The peculiarity of this dimer compared to the majority of known dimeric copper(ii) carboxylates is the unusually long CuCu distance (3.15 Å), with Cu(ii) ions demonstrating an atypical coordination of a distorted trigonal bipyramid formed by five O atoms of five trifluoroacetate groups.

Dynamic X-ray diffraction sampling for protein crystal positioning

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

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

DOE PAGES

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; ...

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction,more » significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Furthermore, by usingin situtwo-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.« less

Dynamic X-ray diffraction sampling for protein crystal positioning

PubMed Central

Scarborough, Nicole M.; Godaliyadda, G. M. Dilshan P.; Ye, Dong Hye; Kissick, David J.; Zhang, Shijie; Newman, Justin A.; Sheedlo, Michael J.; Chowdhury, Azhad U.; Fischetti, Robert F.; Das, Chittaranjan; Buzzard, Gregery T.; Bouman, Charles A.; Simpson, Garth J.

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations. PMID:28009558

Dynamic X-ray diffraction sampling for protein crystal positioning.

PubMed

Scarborough, Nicole M; Godaliyadda, G M Dilshan P; Ye, Dong Hye; Kissick, David J; Zhang, Shijie; Newman, Justin A; Sheedlo, Michael J; Chowdhury, Azhad U; Fischetti, Robert F; Das, Chittaranjan; Buzzard, Gregery T; Bouman, Charles A; Simpson, Garth J

2017-01-01

A sparse supervised learning approach for dynamic sampling (SLADS) is described for dose reduction in diffraction-based protein crystal positioning. Crystal centering is typically a prerequisite for macromolecular diffraction at synchrotron facilities, with X-ray diffraction mapping growing in popularity as a mechanism for localization. In X-ray raster scanning, diffraction is used to identify the crystal positions based on the detection of Bragg-like peaks in the scattering patterns; however, this additional X-ray exposure may result in detectable damage to the crystal prior to data collection. Dynamic sampling, in which preceding measurements inform the next most information-rich location to probe for image reconstruction, significantly reduced the X-ray dose experienced by protein crystals during positioning by diffraction raster scanning. The SLADS algorithm implemented herein is designed for single-pixel measurements and can select a new location to measure. In each step of SLADS, the algorithm selects the pixel, which, when measured, maximizes the expected reduction in distortion given previous measurements. Ground-truth diffraction data were obtained for a 5 µm-diameter beam and SLADS reconstructed the image sampling 31% of the total volume and only 9% of the interior of the crystal greatly reducing the X-ray dosage on the crystal. Using in situ two-photon-excited fluorescence microscopy measurements as a surrogate for diffraction imaging with a 1 µm-diameter beam, the SLADS algorithm enabled image reconstruction from a 7% sampling of the total volume and 12% sampling of the interior of the crystal. When implemented into the beamline at Argonne National Laboratory, without ground-truth images, an acceptable reconstruction was obtained with 3% of the image sampled and approximately 5% of the crystal. The incorporation of SLADS into X-ray diffraction acquisitions has the potential to significantly minimize the impact of X-ray exposure on the crystal by limiting the dose and area exposed for image reconstruction and crystal positioning using data collection hardware present in most macromolecular crystallography end-stations.

Optical and structural properties of colloidal zirconia nanoparticles prepared by arc discharge in liquid

NASA Astrophysics Data System (ADS)

Peymani forooshani, Reza; Poursalehi, Reza; Yourdkhani, Amin

2018-01-01

Zirconia is one of the important ceramic materials with unique properties such as high melting point, high ionic conductivity, high mechanical properties and low thermal conductivity. Therefore, zirconia is one of the useful materials in refractories, thermal barriers, cutting tools, oxygen sensors electrolytes, catalysis, catalyst supports and solid oxide fuel cells. Recently, direct current (DC) arc discharge is extensively employed to synthesis of metal oxide nanostructures in liquid environments. The aim of this work is the synthesis of colloidal zirconia nanoparticles by DC arc discharge method in water as a medium. Arc discharge was ignited between two pure zirconium electrodes in water. Optical and structural properties of prepared colloidal nanoparticles were investigated. Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and UV-visible spectroscopy, were employed for characterization of particle size, morphology, crystal structure and optical properties, respectively. SEM images demonstrate that the nanoparticles are spherical in shape with an average size lower than 38 nm. The XRD patterns of the nanoparticles were consistent with tetragonal and monoclinic zirconia crystal structures. The optical transmission spectra of the colloidal solution show optical characteristic of zirconia nanoparticles as a wide band gap semiconductor with no absorption peak in visible wavelength with the considerable amount of oxygen deficiency. Oxidation of colloidal nanoparticles in water could be explained via reaction with either dissociated oxygen from water in hot plasma region or with dissolved oxygen in water. The results provide a simple and flexible method for preparation of zirconia nanoparticles with a capability of mass production without environmental footprints.

High resolution x-ray diffraction analysis of annealed low-temperature gallium arsenide

NASA Astrophysics Data System (ADS)

Matyi, R. J.; Melloch, M. R.; Woodall, J. M.

1992-05-01

High resolution x-ray diffraction methods have been used to characterize GaAs grown at low substrate temperatures by molecular beam epitaxy and to examine the effects of post-growth annealing on the structure of the layers. Double crystal rocking curves from the as-deposited epitaxial layer show well-defined interference fringes, indicating a high level of structural perfection despite the presence of excess arsenic. Annealing at temperatures from 700 to 900 °C resulted in a decrease in the perpendicular lattice mismatch between the GaAs grown at low temperature and the substrate from 0.133% to 0.016% and a decrease (but not total elimination) of the visibility of the interference fringes. Triple-crystal diffraction scans around the 004 point in reciprocal space exhibited an increase in the apparent mosaic spread of the epitaxial layer with increasing anneal temperature. The observations are explained in terms of the growth of arsenic precipitates in the epitaxial layer.

Current trends in protein crystallization.

PubMed

Gavira, José A

2016-07-15

Proteins belong to the most complex colloidal system in terms of their physicochemical properties, size and conformational-flexibility. This complexity contributes to their great sensitivity to any external change and dictate the uncertainty of crystallization. The need of 3D models to understand their functionality and interaction mechanisms with other neighbouring (macro)molecules has driven the tremendous effort put into the field of crystallography that has also permeated other fields trying to shed some light into reluctant-to-crystallize proteins. This review is aimed at revising protein crystallization from a regular-laboratory point of view. It is also devoted to highlight the latest developments and achievements to produce, identify and deliver high-quality protein crystals for XFEL, Micro-ED or neutron diffraction. The low likelihood of protein crystallization is rationalized by considering the intrinsic polypeptide nature (folded state, surface charge, etc) followed by a description of the standard crystallization methods (batch, vapour diffusion and counter-diffusion), including high throughput advances. Other methodologies aimed at determining protein features in solution (NMR, SAS, DLS) or to gather structural information from single particles such as Cryo-EM are also discussed. Finally, current approaches showing the convergence of different structural biology techniques and the cross-methodologies adaptation to tackle the most difficult problems, are presented. Current advances in biomacromolecules crystallization, from nano crystals for XFEL and Micro-ED to large crystals for neutron diffraction, are covered with special emphasis in methodologies applicable at laboratory scale. Copyright © 2015 Elsevier Inc. All rights reserved.

Premelting phenomena in pseudo-binary ionic crystals

NASA Astrophysics Data System (ADS)

Matsunaga, Shigeki

2010-04-01

The theory of the premelting phenomena in ionic crystals on the basis of the concept of the heterophase fluctuation has been applied to the pseudo-binary ionic crystals, KCl-NaCl, AgBr-AgCl and AgBr-CuBr systems. Molecular dynamics simulations (MD) have been performed to examine the ionic configurations in their premelting region in the vicinity of their melting points. Liquid-like clusters have been observed in the results of MD utilizing the Lindemann instability condition. The sizes of liquid-like clusters have been estimated by theory and MD. The characteristics of the dynamical behavior of ions in the premelting region have been examined by the mean square displacement and the velocity correlation functions.

Transrotational Crystals Revealed by TEM in Crystallizing Amorphous Films: New Solid State Order or Novel Extended Imperfection?

NASA Astrophysics Data System (ADS)

Kolosov, Vladimir Yu.

2011-03-01

Uunusual transrotational structure is presented for crystal growth in thin amorphous films. Experimental results have been obtained for the microcrystals of different chemical nature (oxides, chalcogenides, metals and alloys) grown in thin films prepared by various methods. Basically we used transmission electron microscopy (TEM): our original bend contour technique combined with selected area diffraction (HREM, EDX and CBED used in due cases as well as AFM). The unusual phenomenon (also traced inside TEM in situ) resides in strong (up to the whole rotation per micrometer) regular internal bending of crystal lattice planes (transrotation) in a growing crystal. As a result permanent rotation of the lattice orientation (realized round an axis lying in the film plane) is revealed by TEM. Different geometries of transrotational nanostructures are described: cylindrical, ellipsoidal, etc. Such crystal with transrotational atom periodicity resembles ideal single crystal enclosed in a curved space. Transrotational crystals can be considered as endless 2.5 D analogy of nanotubes, nanonions. Transrotation is strongly increasing as the film gets thinner in the range 100-15 nm. Transrotations supplement well known dislocations (in crystals) and disclinations (in liquid crystals). Support of RF Ministry of Education and Science is acknowledged.

Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

NASA Astrophysics Data System (ADS)

Ma, Zhenye; Li, Cheng; Wu, Rujun; Chen, Rizhi; Gu, Zhenggui

2009-10-01

In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.

Isolation of isoelectrically pure cholera toxin for crystallization

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

Spangler, B.D.; Westbrook, E.M.

1989-01-01

We have determined that the failure of cholera toxin to crystallize well results from its isoelectric heterogeneity, which is probably due to a post-translational process such as deamidation of its B subunit. Every sample of cholera toxin we have examined from commercial or academic suppliers has been heterogeneous; heterogeneous cholera toxin does not crystallize satisfactorily. We have overcome this problem by using ion-exchange fast protein liquid chromatography (FPLC) to obtain an isoelectrically homogeneous species of cholera toxin. Homogeneous cholera toxin crystallizes readily, forming single, nonmosaic crystals suitable for x-ray diffraction studies. For this process, protein was applied to a MonoQmore » ion-exchange column, then eluted with an isocratic low salt buffer followed by a linear salt gradient (0-100 mM NaCl). Column fractions were analyzed on isoelectric focusing gels, and those fractions containing the desired homogeneous species were pooled and concentrated. Crystals formed within 24 to 48 hours in a MOPS/PEG buffer, which made use of slow isoelectric precipitation to induce crystallization. 23 refs., 6 figs.« less

Ultrasonic irradiation-assisted synthesis of Bi2S3 nanoparticles in aqueous ionic liquid at ambient condition.

PubMed

de la Parra-Arciniega, Salomé M; Garcia-Gomez, Nora A; Garza-Tovar, Lorena L; García-Gutiérrez, Domingo I; Sánchez, Eduardo M

2017-05-01

In this work, an easy, fast and environmentally friendly method to obtain Bi 2 S 3 nanostructures with sphere-like morphology is introduced. The promising material was successfully synthesized by a sonochemical route in 20% 1-ethyl-3-methylimidazolium ethyl sulfate [EMIM][EtSO 4 ] ionic liquid solution (IL). Morphological studies by electron microscopy (SEM and TEM) show that the use of IL in the synthesis of Bi 2 S 3 favors the formation of nanocrystals non-agglomerated. Micro Raman and energy dispersive X-ray spectroscopy (EDXS) were used to determine the composition and purity of the synthesized material. X-ray powder diffraction (XRD) and selective area electron diffraction (SAED) revealed that ultrasonic radiation accelerated the crystallization of Bi 2 S 3 into orthorhombic bismuthinite structure. The band gap calculated from the diffuse reflectance spectra (DRS) was found to be 1.5eV. Copyright © 2016 Elsevier B.V. All rights reserved.

Chaos and Beyond in a Water Filled Ultrasonic Resonance System

NASA Technical Reports Server (NTRS)

Lazlo, Adler; Yost, W.; Cantrell, John H.

2013-01-01

Finite amplitude ultrasonic wave resonances in a one-dimensional liquid-filled cavity, formed by a narrow band transducer and a plane reflector, are reported. The resonances are observed to include not only the expected harmonic and subharmonic signals (1,2) but chaotic signals as well. The generation mechanism requires attaining a threshold value of the driving amplitude that the liquid-filled cavity system becomes sufficiently nonlinear in response. The nonlinear features of the system were recently investigated via the construction of an ultrasonic interferometer having optical precision. The transducers were compressional, undamped quartz and lithium niobate crystals having the frequency range 1-10 MHz, driven by a high power amplifier. Both an optical diffraction system to characterize the diffraction pattern of laser light normally incident to the cavity and a receiving transducer attached to an aligned reflector with lapped flat and parallel surfaces were used to assess the generated resonance response in the cavity. At least 5 regions of excitation are identified.

Template-free solution approach to synthesize CdS dendrites with SCN based ionic liquid

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

Li, Kangfeng; Li, Jiajia; Cheng, Xianyi

2011-07-15

Highlights: {yields} Template-free solution approach to synthesize CdS hierarchical dendrites. {yields} The 1-butyl-3-methlyimidazole thiocyanate ([BMIM][SCN]) plays doubly functional roles in the progress. {yields} The CdS hierarchical dendrites exhibit a more intense emission at 710 nm belongs to infrared band. -- Abstract: Cadmium sulfide dendrites were synthesized by a facile hydrothermal treatment from CdCl{sub 2} and ionic liquid 1-butyl-3-methlyimidazole thiocyanate acted both as sulfur source and surfactant. The product was characterized by means of X-ray powder diffraction and scanning electron microscopy. X-ray powder diffraction studies indicated that the product was well-crystallized hexagonal phase of CdS, and the scanning electron microscopy imagesmore » showed that the obtained powders consisted of a wealth of well-defined CdS dendritic microstructures with a pronounced trunk and highly ordered branches. The UV-Vis and photoluminescence spectroscopy measurements were taken as well. The possible formation mechanism of CdS dendrites was simply proposed in the end.« less

Origin of melting point depression for rare gas solids confined in carbon pores

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

Morishige, Kunimitsu, E-mail: morishi@chem.ous.ac.jp; Kataoka, Takaaki

To obtain insights into the mechanism of the melting-point depression of rare gas solids confined in crystalline carbon pores, we examined the freezing and melting behavior of Xe and Ar confined to the crystalline pores of ordered mesoporous carbons as well as compressed exfoliated graphite compared to the amorphous pores of ordered mesoporous silicas, by means of X-ray diffraction. For the Xe and Ar confined to the crystalline carbon pores, there was no appreciable thermal hysteresis between freezing and melting. Furthermore, the position of the main diffraction peak did not change appreciably on freezing and melting. This strongly suggests thatmore » the liquids confined in the carbon pores form a multilayered structure parallel to the smooth walls. For the Xe and Ar confined to the amorphous silica pores, on the other hand, the position of the main diffraction peak shifted into higher scattering angle on freezing suggested that the density of the confined solid is distinctly larger than for the confined liquid. Using compressed exfoliated graphite with carbon walls of higher crystallinity, we observed that three-dimensional (3D) microcrystals of Xe confined in the slit-shaped pores melted to leave the unmelted bilayers on the pore walls below the bulk triple point. The lattice spacing of the 3D microcrystals confined is larger by ∼0.7% than that of the bilayer next to the pore walls in the vicinity of the melting point.« less

A novel inert crystal delivery medium for serial femtosecond crystallography

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

Conrad, Chelsie E.; Basu, Shibom; James, Daniel

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5 Å resolution using 300 µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

A novel inert crystal delivery medium for serial femtosecond crystallography

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

Conrad, Chelsie E.; Basu, Shibom; James, Daniel

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5Å resolution using 300µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

A novel inert crystal delivery medium for serial femtosecond crystallography

DOE PAGES

Conrad, Chelsie E.; Basu, Shibom; James, Daniel; ...

2015-06-30

Serial femtosecond crystallography (SFX) has opened a new era in crystallography by permitting nearly damage-free, room-temperature structure determination of challenging proteins such as membrane proteins. In SFX, femtosecond X-ray free-electron laser pulses produce diffraction snapshots from nanocrystals and microcrystals delivered in a liquid jet, which leads to high protein consumption. A slow-moving stream of agarose has been developed as a new crystal delivery medium for SFX. It has low background scattering, is compatible with both soluble and membrane proteins, and can deliver the protein crystals at a wide range of temperatures down to 4°C. Using this crystal-laden agarose stream, themore » structure of a multi-subunit complex, phycocyanin, was solved to 2.5 Å resolution using 300 µg of microcrystals embedded into the agarose medium post-crystallization. The agarose delivery method reduces protein consumption by at least 100-fold and has the potential to be used for a diverse population of proteins, including membrane protein complexes.« less

High-throughput and in situ EDXRD investigation on the formation of two new metal aminoethylphosphonates - Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) and Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O

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

Schmidt, Corinna; Feyand, Mark; Rothkirch, Andre

2012-04-15

The system Ca{sup 2+}/2-aminoethylphosphonic acid/H{sub 2}O/NaOH was systematically investigated using high-throughput methods. The experiments led to one new compound Ca(O{sub 3}PC{sub 2} H{sub 4}NH{sub 2}) (1) and the crystal structure was determined using in house X-ray powder diffraction data (monoclinic, P2{sub 1}/c, a=9.7753(3), b=6.4931(2), c=8.4473(2) A, {beta}=106.46(2) Degree-Sign , V=514.20(2) A{sup 3}, Z=4). The formation of 1 was investigated by in situ energy dispersive X-ray diffraction measurements (EDXRD) at beamline F3 at HASYLAB (light source DORIS III), DESY, Hamburg. An intermediate, Ca(OH)(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3}){center_dot}2H{sub 2}O (2), was observed and could be isolated from the reaction mixture at ambientmore » temperatures by quenching the reaction. The crystal structure of 2 was determined from XRPD data using synchrotron radiation (monoclinic, P2{sub 1}/m, a=11.2193(7), b=7.1488(3), c=5.0635(2) A, {beta}=100.13(4) Degree-Sign , V=399.78(3) A{sup 3}, Z=2). - Graphical abstarct: The detailed in situ energy dispersive X-ray diffraction (EDXRD) investigation on the formation of the new inorganic-organic hybrid compound Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) leads to the discovery of a new crystalline intermediate phase. Both crystal structures were elucidated using X-ray powder diffraction data. Highlights: Black-Right-Pointing-Pointer High-throughput investigation led to new metal aminoethylphosphonate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}). Black-Right-Pointing-Pointer The formation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 2}) was followed by in situ EDXRD measurements. Black-Right-Pointing-Pointer The crystalline intermediate Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was discovered. Black-Right-Pointing-Pointer Isolation of Ca(O{sub 3}PC{sub 2}H{sub 4}NH{sub 3})(OH){center_dot}2H{sub 2}O was accomplished by quenching experiments. Black-Right-Pointing-Pointer The structures were determined using X-ray powder diffraction data.« less

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Growth and characterization of a new nonlinear optical organic crystal: 2,4,6-Trimethylacetanilide

NASA Astrophysics Data System (ADS)

Upadhyaya, V.; Prabhu, Sharada G.

2015-09-01

A new nonlinear optical organic material, 2,4,6-trimethylacetanilide (246TMAA), also known as N-[2,4,6- trimethylphenyl]acetamide, has been synthesized and grown as a single crystal by the slow evaporation technique by organic solvents. The grown crystals have been characterized by morphology study. The crystals are prismatic. Surface examination shows granular dendritic pattern in optical micrograph. The Scanning Electron Micrograph shows the layered growth of the crystal. The Differential Scanning Calorimeter plot shows no phase change until melting point (219°C). The density of the crystals is 1.1g/cc and the crystals are soft. The crystals are transparent in the visible region and in the ultra-violet region till 280 nm. 246TMAA crystallizes with 2 molecules in a monoclinic unit cell in the noncentrosymmetric point group m, space group Pn. Refractive indices of this optically biaxial crystal along the three crystallophysical axes have been measured at 633 nm. The optical second harmonic generation efficiency of the crystal at 1064 nm is about half that of the urea crystal, measured by powder method using Nd:YAG laser. The results show that the 246TMAA crystal can efficiently be used for up-conversion of infrared radiation into visible green light. The powder X-ray diffraction spectrum of the crystal has been obtained.

Glass-to-cryogenic-liquid transitions in aqueous solutions suggested by crack healing

PubMed Central

Kim, Chae Un; Tate, Mark W.; Gruner, Sol M.

2015-01-01

Observation of theorized glass-to-liquid transitions between low-density amorphous (LDA) and high-density amorphous (HDA) water states had been stymied by rapid crystallization below the homogeneous water nucleation temperature (∼235 K at 0.1 MPa). We report optical and X-ray observations suggestive of glass-to-liquid transitions in these states. Crack healing, indicative of liquid, occurs when LDA ice transforms to cubic ice at 160 K, and when HDA ice transforms to the LDA state at temperatures as low as 120 K. X-ray diffraction study of the HDA to LDA transition clearly shows the characteristics of a first-order transition. Study of the glass-to-liquid transitions in nanoconfined aqueous solutions shows them to be independent of the solute concentrations, suggesting that they represent an intrinsic property of water. These findings support theories that LDA and HDA ice are thermodynamically distinct and that they are continuously connected to two different liquid states of water. PMID:26351671

An aggregation-volume-bias Monte Carlo investigation on the condensation of a Lennard-Jones vapor below the triple point and crystal nucleation in cluster systems: an in-depth evaluation of the classical nucleation theory.

PubMed

Chen, Bin; Kim, Hyunmi; Keasler, Samuel J; Nellas, Ricky B

2008-04-03

The aggregation-volume-bias Monte Carlo based simulation technique, which has led to our recent success in vapor-liquid nucleation research, was extended to the study of crystal nucleation processes. In contrast to conventional bulk-phase techniques, this method deals with crystal nucleation events in cluster systems. This approach was applied to the crystal nucleation of Lennard-Jonesium under a wide range of undercooling conditions from 35% to 13% below the triple point. It was found that crystal nucleation in these model clusters proceeds initially via a vapor-liquid like aggregation followed by the formation of crystals inside the aggregates. The separation of these two stages of nucleation is distinct except at deeper undercooling conditions where the crystal nucleation barrier was found to diminish. The simulation results obtained for these two nucleation steps are separately compared to the classical nucleation theory (CNT). For the vapor-liquid nucleation step, the CNT was shown to provide a reasonable description of the critical cluster size but overestimate the barrier heights, consistent with previous simulation studies. On the contrary, for the crystal nucleation step, nearly perfect agreement with the barrier heights was found between the simulations and the CNT. For the critical cluster size, the comparison is more difficult as the simulation data were found to be sensitive to the definition of the solid cluster, but a stringent criterion and lower undercooling conditions generally lead to results closer with the CNT. Additional simulations at undercooling conditions of 40% or above indicate a nearly barrierless transition from the liquid to crystalline-like structure for sufficiently large clusters, which leads to further departure of the barrier height predicted by the CNT from the simulation data for the aggregation step. This is consistent with the latest experimental results on argon that show an unusually large underestimation of the nucleation rate by the CNT toward deep undercooling conditions.

Heterogeneous nucleation in a glass-forming alloy

NASA Astrophysics Data System (ADS)

Wall, J. J.; Liu, C. T.; Rhim, W.-K.; Li, J. J. Z.; Liaw, P. K.; Choo, H.; Johnson, W. L.

2008-06-01

Nucleation in the undercooled liquid state in the bulk metallic glass-forming composition Zr52.5Cu17.9Ni14.6Al10Ti5 (VIT-105), produced using high purity (PA) and commercial purity (CA) raw materials was investigated using electrostatic levitation and ex situ neutron diffraction. The CA material was observed to have a lower density than the PA sample and crystallized at relatively shallow undercooling. The densities of the samples at temperatures above the solidus showed an oxygen-dependent hysteresis associated with the state change, indicating the presence of oxygen-stabilized intermetallics. The PA alloy exhibited three distinct crystallization modes dependent on the thermal history of the melt, one of which showed a net volume expansion.

Preferred orientations of laterally grown silicon films over amorphous substrates using the vapor-liquid-solid technique

NASA Astrophysics Data System (ADS)

LeBoeuf, J. L.; Brodusch, N.; Gauvin, R.; Quitoriano, N. J.

2014-12-01

A novel method has been optimized so that adhesion layers are no longer needed to reliably deposit patterned gold structures on amorphous substrates. Using this technique allows for the fabrication of amorphous oxide templates known as micro-crucibles, which confine a vapor-liquid-solid (VLS) catalyst of nominally pure gold to a specific geometry. Within these confined templates of amorphous materials, faceted silicon crystals have been grown laterally. The novel deposition technique, which enables the nominally pure gold catalyst, involves the undercutting of an initial chromium adhesion layer. Using electron backscatter diffraction it was found that silicon nucleated in these micro-crucibles were 30% single crystals, 45% potentially twinned crystals and 25% polycrystals for the experimental conditions used. Single, potentially twinned, and polycrystals all had an aversion to growth with the {1 0 0} surface parallel to the amorphous substrate. Closer analysis of grain boundaries of potentially twinned and polycrystalline samples revealed that the overwhelming majority of them were of the 60° Σ3 coherent twin boundary type. The large amount of coherent twin boundaries present in the grown, two-dimensional silicon crystals suggest that lateral VLS growth occurs very close to thermodynamic equilibrium. It is suggested that free energy fluctuations during growth or cooling, and impurities were the causes for this twinning.

Spherical quartz crystals investigated with synchrotron radiation

DOE PAGES

Pereira, N. R.; Macrander, A. T.; Hill, K. W.; ...

2015-10-27

The quality of x-ray spectra and images obtained from plasmas with spherically bent crystals depends in part on the crystal's x-ray diffraction across the entire crystal surface. We employ the energy selectivity and high intensity of synchrotron radiation to examine typical spherical crystals from alpha-quartz for their diffraction quality, in a perpendicular geometry that is particularly convenient to examine sagittal focusing. The crystal's local diffraction is not ideal: the most noticeable problems come from isolated regions that so far have failed to correlate with visible imperfections. In conclusion, excluding diffraction from such problem spots has little effect on the focusmore » beyond a decrease in background.« less

Total reflection infrared spectroscopy of water-ice and frozen aqueous NaCl solutions.

PubMed

Walker, Rachel L; Searles, Keith; Willard, Jesse A; Michelsen, Rebecca R H

2013-12-28

Liquid-like and liquid water at and near the surface of water-ice and frozen aqueous sodium chloride films were observed using attenuated total reflection infrared spectroscopy (ATR-IR). The concentration of NaCl ranged from 0.0001 to 0.01 M and the temperature varied from the melting point of water down to 256 K. The amount of liquid brine at the interface of the frozen films with the germanium ATR crystal increased with salt concentration and temperature. Experimental spectra are compared to reflection spectra calculated for a simplified morphology of a uniform liquid layer between the germanium crystal and the frozen film. This morphology allows for the amount of liquid observed in an experimental spectrum to be converted to the thickness of a homogenous layer with an equivalent amount of liquid. These equivalent thickness ranges from a nanometer for water-ice at 260 K to 170 nm for 0.01 M NaCl close to the melting point. The amounts of brine observed are over an order of magnitude less than the total liquid predicted by equilibrium thermodynamic models, implying that the vast majority of the liquid fraction of frozen solutions may be found in internal inclusions, grain boundaries, and the like. Thus, the amount of liquid and the solutes dissolved in them that are available to react with atmospheric gases on the surfaces of snow and ice are not well described by thermodynamic equilibrium models which assume the liquid phase is located entirely at the surface.

Mesomorphic behaviors of a series of heterocyclic thiophene-imine-ester-based liquid crystals

NASA Astrophysics Data System (ADS)

Foo, K.-L.; Ha, S.-T.; Yeap, G. Y.; Lee, S. L.

2018-05-01

The synthesis and characterization of a series of heterocyclic liquid crystal, 4-{[(thiophen-2-yl)methylidene]amino}phenyl 4-alkoxybenzoates possessing even number of carbon atoms at the alkoxy chain (CnH2n+1O-, n = 6, 8, 10, 12, 14, 16, 18) are reported. The molecular structures of title compounds were elucidated using Fourier-transform infrared spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopic techniques along with mass spectrometric analysis. The phase behavior of these compounds was characterized and studied by differential scanning calorimetry and polarizing optical microscopy. All members exhibited enantiotropic nematic phase except for the highest member (n = 18) which is a non-mesogen. Influence of alkoxy chain length on the transition temperatures of crystal-to-nematic (melting point) and nematic-to-isotropic (clearing point) was studied. Nematic phase range was found to increase from n = 6 to n = 10, then it started to descend from n = 12 to n = 16 and finally the nematic phase disappeared when n changed to 18.

Sunlight-switchable light shutter fabricated using liquid crystals doped with push-pull azobenzene.

PubMed

Oh, Seung-Won; Baek, Jong-Min; Yoon, Tae-Hoon

2016-11-14

We propose a sunlight-switchable light shutter using liquid crystal/polymer composite doped with push-pull azobenzene. The proposed light shutter is switchable between the translucent and transparent states by application of an electric field or by UV irradiation. Switching by UV irradiation is based on the change of the liquid crystal (LC) clearing point by the photo-isomerization effect of push-pull azobenzene. Under sunlight, the light shutter can be switched from the translucent to the transparent state by the nematic-isotropic phase transition of the LC domains triggered by trans-cis photo-isomerization of the push-pull azobenzene molecules. When the amount of sunlight is low because of cloud cover or when there is no sunlight at sunset, the light shutter rapidly relaxes from its transparent state back to its initial translucent state by the isotropic-nematic phase transition induced by cis-trans back-isomerization of the push-pull azobenzene molecules.

Topological transformations of Hopf solitons in chiral ferromagnets and liquid crystals.

PubMed

Tai, Jung-Shen B; Ackerman, Paul J; Smalyukh, Ivan I

2018-01-30

Liquid crystals are widely known for their facile responses to external fields, which forms a basis of the modern information display technology. However, switching of molecular alignment field configurations typically involves topologically trivial structures, although singular line and point defects often appear as short-lived transient states. Here, we demonstrate electric and magnetic switching of nonsingular solitonic structures in chiral nematic and ferromagnetic liquid crystals. These topological soliton structures are characterized by Hopf indices, integers corresponding to the numbers of times that closed-loop-like spatial regions (dubbed "preimages") of two different single orientations of rod-like molecules or magnetization are linked with each other. We show that both dielectric and ferromagnetic response of the studied material systems allow for stabilizing a host of topological solitons with different Hopf indices. The field transformations during such switching are continuous when Hopf indices remain unchanged, even when involving transformations of preimages, but discontinuous otherwise.

Optical Simulation and Fabrication of Pancharatnam (Geometric) Phase Devices from Liquid Crystals

NASA Astrophysics Data System (ADS)

Gao, Kun

Pancharatnam made clear the concept of a phase-only device based on changes in the polarization state of light. A device of this type is sometimes called a circular polarization grating because of the polarization states of interfering light beams used to fabricate it by polarization holography. Here, we will call it a Pancharatnam (geometric) phase device to emphasize the fact that the phase of diffracted light does not have a discontinuous periodic profile but changes continuously. In this dissertation, using simulations and experiments, we have successfully demonstrated a 90% diffraction efficiency based on the Pancharatnam phase deflector (PPD) with the dual-twist structure. Unlike the conventional Pancharatnam phase deflector (c-PPD) limited to small diffraction angles, our work demonstrates that a device with a structural periodicity near the wavelength of light is highly efficient at deflecting light to large angles. Also, from a similar fabrication procedure, we have made an ultra-compact non-mechanical zoom lens system based on the Pancharatnam phase lens (PPL) with a low f-number and high efficiency. The wavelength dependence on the image quality is evaluated and shown to be satisfactory from red light to near-infrared machine vision systems. A demonstration device is shown with a 4x zoom ratio at a 633 nm wavelength. The unique characteristic of these devices is made possible through the use of azo-dye photoalignment materials to align a liquid crystal polymer (reactive mesogens). Furthermore, the proposed dual-twist design and fabrication opens the possibility for making a high-efficiency beam-steering device, a lens with an f-number less than 1.0, as well as a wide range of other potential applications in the optical and display industry. The details of simulation, fabrication, and characterization of these devices are shown in this dissertation.

Mechanisms of differentiation in the Skaergaard magma chamber

NASA Astrophysics Data System (ADS)

Tegner, C.; Lesher, C. E.; Holness, M. B.; Jakobsen, J. K.; Salmonsen, L. P.; Humphreys, M. C. S.; Thy, P.

2012-04-01

The Skaergaard intrusion is a superb natural laboratory for studying mechanisms of magma chamber differentiation. The magnificent exposures and new systematic sample sets of rocks that solidified inwards from the roof, walls and floor of the chamber provide means to test the relative roles of crystal settling, diffusion, convection, liquid immiscibility and compaction in different regions of the chamber and in opposite positions relative to gravity. Examination of the melt inclusions and interstitial pockets has demonstrated that a large portion of intrusion crystallized from an emulsified magma chamber composed of immiscible silica- and iron-rich melts. The similarity of ratios of elements with opposite partitioning between the immiscible melts (e.g. P and Rb) in wall, floor and roof rocks, however, indicate that large-scale separation did not occur. Yet, on a smaller scale of metres to hundred of metres and close to the interface between the roof and floor rocks (the Sandwich Horizon), irregular layers and pods of granophyre hosted by extremely iron-rich cumulates point to some separation of the two liquid phases. Similar proportions of the primocryst (cumulus) minerals in roof, wall and floor rocks indicate that crystal settling was not an important mechanism. Likewise, the lack of fractionation of elements with different behavior indicate that diffusion and fluid-driven metasomatism played relatively minor roles. Compositional convection and/or compaction within the solidifying crystal mush boundary layer are likely the most important mechanisms. A correlation of low trapped liquid fractions (calculated from strongly incompatible elements) in floor rocks with high fractionation density (the density difference between the crystal framework and the liquid) indicate that compaction is the dominating process in expelling evolved liquid from the crystal mush layer. This is supported by high and variable trapped liquid contents in the roof rocks, where gravity-driven compaction will not work.

Synthesis, growth, structural, spectral, thermal, chemical etching, linear and nonlinear optical and mechanical studies of an organic single crystal 4-chloro 4-nitrostilbene (CONS): a potential NLO material.

PubMed

Dinakaran, Paul M; Kalainathan, S

2013-07-01

4-Chloro 4-nitrostilbene (CONS) a new organic nonlinear optical material has been synthesized. Employing slow evaporation method, good optical quality single crystals (dimensions up to 6×2×3 mm(3)) have been grown using ethyl methyl ketone (EMK) as a solvent. The grown crystals have been subjected to various characterizations such as single crystal X-ray diffraction, powder XRD, Fourier Transform Infrared spectroscopy (FTIR), proton NMR, solid UV absorption, SHG studies. Single crystal X-ray diffraction reveals that the crystal system belongs to monoclinic with noncentrosymmetric space group P21. The UV-Vis absorption spectrum has been recorded and found that the cut off wavelength is 380 nm. Functional groups and the structure of the title compound have been confirmed by FTIR and (1)H NMR spectroscopic analyses respectively. Molecular mass of the CONS confirmed by the high resolution mass spectral analysis .The thermal behavior of the grown crystal has been studied by TG/DTA analysis and it shows the melting point is at 188.66 °C. Dislocations and growth pattern present in the grown crystal revealed by the etching study. The mechanical strength of the CONS crystal has been studied by Vicker's hardness measurement. The SHG efficiency of the grown crystal has been determined by Kurtz and Perry powder test which revealed that the CONS crystal (327 mV) has 15 times greater efficiency than that of KDP (21.7 mV). Copyright © 2013 Elsevier B.V. All rights reserved.

Atomistic simulation of solid-liquid coexistence for molecular systems: application to triazole and benzene.

PubMed

Eike, David M; Maginn, Edward J

2006-04-28

A method recently developed to rigorously determine solid-liquid equilibrium using a free-energy-based analysis has been extended to analyze multiatom molecular systems. This method is based on using a pseudosupercritical transformation path to reversibly transform between solid and liquid phases. Integration along this path yields the free energy difference at a single state point, which can then be used to determine the free energy difference as a function of temperature and therefore locate the coexistence temperature at a fixed pressure. The primary extension reported here is the introduction of an external potential field capable of inducing center of mass order along with secondary orientational order for molecules. The method is used to calculate the melting point of 1-H-1,2,4-triazole and benzene. Despite the fact that the triazole model gives accurate bulk densities for the liquid and crystal phases, it is found to do a poor job of reproducing the experimental crystal structure and heat of fusion. Consequently, it yields a melting point that is 100 K lower than the experimental value. On the other hand, the benzene model has been parametrized extensively to match a wide range of properties and yields a melting point that is only 20 K lower than the experimental value. Previous work in which a simple "direct heating" method was used actually found that the melting point of the benzene model was 50 K higher than the experimental value. This demonstrates the importance of using proper free energy methods to compute phase behavior. It also shows that the melting point is a very sensitive measure of force field quality that should be considered in parametrization efforts. The method described here provides a relatively simple approach for computing melting points of molecular systems.

Crystal nucleation and metastable bcc phase in charged colloids: A molecular dynamics study

NASA Astrophysics Data System (ADS)

Ji, Xinqiang; Sun, Zhiwei; Ouyang, Wenze; Xu, Shenghua

2018-05-01

The dynamic process of homogenous nucleation in charged colloids is investigated by brute-force molecular dynamics simulation. To check if the liquid-solid transition will pass through metastable bcc, simulations are performed at the state points that definitely lie in the phase region of thermodynamically stable fcc. The simulation results confirm that, in all of these cases, the preordered precursors, acting as the seeds of nucleation, always have predominant bcc symmetry consistent with Ostwald's step rule and the Alexander-McTague mechanism. However, the polymorph selection is not straightforward because the crystal structures formed are not often determined by the symmetry of intermediate precursors but have different characters under different state points. The region of the state point where bcc crystal structures of large enough size are formed during crystallization is narrow, which gives a reasonable explanation as to why the metastable bcc phase in charged colloidal suspensions is rarely detected in macroscopic experiments.

Lasing and Longitudinal Cavity Modes in Photo-Pumped Deep Ultraviolet AlGaN Heterostructures

DTIC Science & Technology

2013-04-29

of the structures were intentionally doped. The AlGaN composition was determined by triple -axis high-resolution X-ray diffraction measurements. Cross...threshold can be achieved on single crystal AlN substrates. This achievement serves as a starting point towards realizing electrically pumped sub-300 nm UV

Crystal growth, spectral, structural and optical studies of π-conjugated stilbazolium crystal: 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate.

PubMed

Krishna Kumar, M; Sudhahar, S; Bhagavannarayana, G; Mohan Kumar, R

2014-05-05

Nonlinear optical (NLO) organic compound, 4-bromobenzaldehyde-4'-N'-methylstilbazolium tosylate was synthesized by reflux method. The formation of molecular complex was confirmed from (1)H NMR, FT-IR and FT-Raman spectral analyses. The single crystals were grown by slow evaporation solution growth method and the crystal structure and atomic packing of grown crystal was identified. The morphology and growth axis of grown crystal were determined. The crystal perfection was analyzed using high resolution X-ray diffraction study on (001) plane. Thermal stability, decomposition stages and melting point of the grown crystal were analyzed. The optical absorption coefficient (α) and energy band gap (E(g)) of the crystal were determined using UV-visible absorption studies. Second harmonic generation efficiency of the grown crystal was examined by Kurtz powder method with different particle size using 1064 nm laser. Laser induced damage threshold study was carried out for the grown crystal using Nd:YAG laser. Copyright © 2014 Elsevier B.V. All rights reserved.

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

NASA Technical Reports Server (NTRS)

Stojanoff, Vivian; Boggon, Titus; Helliwell, John R.; Judge, Russell; Olczak, Alex; Snell, Edward H.; Siddons, D. Peter; Rose, M. Franklin (Technical Monitor)

2000-01-01

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

A multi-cone x-ray imaging Bragg crystal spectrometer

DOE PAGES

Bitter, M.; Hill, K. W.; Gao, Lan; ...

2016-08-26

This article describes a new x-ray imaging Bragg crystal spectrometer, which—in combination with a streak camera or a gated strip detector—can be used for time-resolved measurements of x-ray line spectra at the National Ignition Facility and other high power laser facilities. The main advantage of this instrument is that it produces perfect images of a point source for each wavelength in a selectable spectral range and that the detector plane can be perpendicular to the crystal surface or inclined by an arbitrary angle with respect to the crystal surface. Furthermore, these unique imaging properties are obtained by bending the x-raymore » diffracting crystal into a certain shape, which is generated by arranging multiple cones with different aperture angles on a common nodal line.« less

Structural properties of Y2O3–Al2O3 liquids and glasses: An overview

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

Wilding, Martin C.; Wilson, Mark; McMillan, Paul F.

2015-01-01

Liquids in the system Y2O3- Al2O3 have been the subject of considerable study because of the reported occurrence of a first-order density and entropy-driven liquid-liquid phase transition (LLPT) in the supercooled liquid state. The observations have become controversial because of the presence of crystalline material that can be formed simultaneously and that can mask the nucleation and growth of the lower density liquid. The previous work is summarized here along with arguments for and against the different viewpoints. Also two studies have been undertaken to investigate the LLPT in this refractory system with emphasis on determining the structure of unequivocallymore » amorphous materials. These include the in situ high energy X-ray diffraction (HEXRD) of supercooled Y2O3 - Al2O3 liquids and the low frequency vibrational dynamics of recovered glasses. Manybody molecular dynamics simulations are also used to interpret the results of both studies. The HEXRD measurements, combined with aerodynamic levitation and rapid data acquisition techniques, show that for the 20 mol% Y2O3 (i.e. AlY20) liquid there is a shift in the position of the first peak in the diffraction pattern over a narrow temperature range (2100-1800 K) prior to crystallization. Microbeam Raman spectroscopy measurements made on AlY20 glasses clearly show contrasting spectra in the low frequency part of the spectrum for low(LDA) and high-density (HDA) glassy regions. The molecular dynamics simulations identify contrasting coordination environments around oxygen anions for the high- (HDL) and low-density (LDL) liquids. (C) 2014 Elsevier B.V. All rights reserved.« less

Structural properties of Y 2O 3–Al 2O 3 liquids and glasses: An overview

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

Wilding, Martin C.; Wilson, Mark; McMillan, Paul F.

2015-01-01

Liquids in the system Y 2O 3–Al 2O 3 have been the subject of considerable study because of the reported occurrence of a first-order density and entropy-driven liquid-liquid phase transition (LLPT) in the supercooled liquid state. The observations have become controversial because of the presence of crystalline material that can be formed simultaneously and that can mask the nucleation and growth of the lower density liquid. The previous work is summarized here along with arguments for and against the different viewpoints. Also two studies have been undertaken to investigate the LLPT in this refractory system with emphasis on determining themore » structure of unequivocally amorphous materials. These include the in situ high energy X-ray diffraction (HEXRD) of supercooled Y 2O 3–Al 2O 3 liquids and the low frequency vibrational dynamics of recovered glasses. Manybody molecular dynamics simulations are also used to interpret the results of both studies. The HEXRD measurements, combined with aerodynamic levitation and rapid data acquisition techniques, show that for the 20 mol% Y 2O 3 (i.e. AlY20) liquid there is a shift in the position of the first peak in the diffraction pattern over a narrow temperature range (2100-1800 K) prior to crystallization. Microbeam Raman spectroscopy measurements made on AlY20 glasses clearly show contrasting spectra in the low frequency part of the spectrum for low(LDA) and high-density (HDA) glassy regions. The molecular dynamics simulations identify contrasting coordination environments around oxygen anions for the high- (HDL) and low-density (LDL) liquids. (C) 2014 Elsevier B.V. All rights reserved.« less

On-axis programmable microscope using liquid crystal spatial light modulator

NASA Astrophysics Data System (ADS)

García-Martínez, Pascuala; Martínez, José Luís.; Moreno, Ignacio

2017-06-01

Spatial light modulators (SLM) are currently used in many applications in optical microscopy and imaging. One of the most promising methods is the use of liquid crystal displays (LCD) as programmable phase diffractive optical elements (DOE) placed in the Fourier plane giving access to the spatial frequencies which can be phased shifted individually, allowing to emulate a wealth of contrast enhancing methods for both amplitude and phase samples. We use phase and polarization modulation of LCD to implement an on-axis microscope optical system. The LCD used are Hamamatsu liquid crystal on silicon (LCOS) SLM free of flicker, thus showing a full profit of the SLM space bandwidth, as opposed to optical systems in the literature forced to work off-axis due to the strong zero-order component. Taking benefits of the phase modulation of the LCOS we have implemented different microscopic imaging operations, such as high-pass and low-pass filtering in parallel using programmable blazed gratings. Moreover, we are able to control polarization modulation to display two orthogonal linear state of polarization images than can be subtracted or added by changing the period of the blazed grating. In that sense, Differential Interference Contrast (DIC) microscopy can be easily done by generating two images exploiting the polarization splitting properties when a blazed grating is displayed in the SLM. Biological microscopy samples are also used.

High-density grids for efficient data collection from multiple crystals

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

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

High-density grids for efficient data collection from multiple crystals

PubMed Central

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; Barnes, Christopher O.; Bonagura, Christopher A.; Brehmer, Winnie; Brunger, Axel T.; Calero, Guillermo; Caradoc-Davies, Tom T.; Chatterjee, Ruchira; Degrado, William F.; Fraser, James S.; Ibrahim, Mohamed; Kern, Jan; Kobilka, Brian K.; Kruse, Andrew C.; Larsson, Karl M.; Lemke, Heinrik T.; Lyubimov, Artem Y.; Manglik, Aashish; McPhillips, Scott E.; Norgren, Erik; Pang, Siew S.; Soltis, S. M.; Song, Jinhu; Thomaston, Jessica; Tsai, Yingssu; Weis, William I.; Woldeyes, Rahel A.; Yachandra, Vittal; Yano, Junko; Zouni, Athina; Cohen, Aina E.

2016-01-01

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassette or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into the Blu-Ice/DCSS experimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. Crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures. PMID:26894529

High-density grids for efficient data collection from multiple crystals

DOE PAGES

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; ...

2015-11-03

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

Crystallization and preliminary X-ray diffraction study of the protealysin precursor belonging to the peptidase family M4

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

Gromova, T. Yu., E-mail: duk@img.ras.ru; Demidyuk, I. V.; Kostrov, S. V.

2008-09-15

A protealysin precursor (the enzyme of the peptidase family M4) was crystallized for the first time. The crystal-growth conditions were found, and single crystals of the protein with dimensions of 0.3-0.5 mm were grown. The preliminary X-ray diffraction study of the enzyme was performed. The protealysin precursor was shown to crystallize in two crystal modifications suitable for the X-ray diffraction study of the three-dimensional structure of the protein molecule at atomic resolution.

Birefringent coherent diffraction imaging

NASA Astrophysics Data System (ADS)

Karpov, Dmitry; dos Santos Rolo, Tomy; Rich, Hannah; Kryuchkov, Yuriy; Kiefer, Boris; Fohtung, E.

2016-10-01

Directional dependence of the index of refraction contains a wealth of information about anisotropic optical properties in semiconducting and insulating materials. Here we present a novel high-resolution lens-less technique that uses birefringence as a contrast mechanism to map the index of refraction and dielectric permittivity in optically anisotropic materials. We applied this approach successfully to a liquid crystal polymer film using polarized light from helium neon laser. This approach is scalable to imaging with diffraction-limited resolution, a prospect rapidly becoming a reality in view of emergent brilliant X-ray sources. Applications of this novel imaging technique are in disruptive technologies, including novel electronic devices, in which both charge and spin carry information as in multiferroic materials and photonic materials such as light modulators and optical storage.

Ionic liquid catalyzed one-pot multi-component synthesis, characterization and antibacterial activity of novel chromeno[2,3-d]pyrimidin-8-amine derivatives

NASA Astrophysics Data System (ADS)

Kanakaraju, Sankari; Prasanna, Bethanamudi; Basavoju, Srinivas; Chandramouli, G. V. P.

2012-06-01

An efficient, simple and convenient method for the one-pot multi-component synthesis of novel chromeno[2,3-d]pyrimidin-8-amine derivatives has been accomplished by starting from α-naphthol, aryl aldehydes, malononitrile and NH4Cl. The reaction has been catalyzed by 1-butyl-3-methylimidazolium tetrafluoroborate [bmim]BF4 ionic liquid. The newly synthesized compounds were characterized by IR, 1H NMR, 13C NMR, mass spectra, and elemental analysis. The structure of compound 4a was confirmed by single-crystal X-ray diffraction. All the synthesized compounds were evaluated for their in vitro antibacterial activity.

Compression driven 2D nematic phase in a columnar Langmuir monolayer

NASA Astrophysics Data System (ADS)

El Abed, A.; Goldmann, M.

2012-08-01

Langmuir films of pyramidic liquid crystals were studied using surface pressure versus molecular area isotherms and synchrotron grazing incidence X-ray diffraction. The used molecule, named 3BCN/14, consists of a pyramidal central core to which are bound symmetrically six lateral C14 alkyl chains. These molecules spread spontaneously at the air-water interface in a metastable side-on phase which relax rapidly upon compression towards a stable edge-on phase. Our results suggest that the new edge-on phase consists of an in-plane organization of columns which are made of about 11 stacked edge-on molecules. This structure remains stable after several expansion-compression cycles. Comparing these results with those obtained previously on two other pyramidic liquid crystals with shorter and longer lateral alkyl chains, C9 and C15 respectively, we attribute the formation of the obtained 2D nematic phase to a suitable lateral chains length which allow for the establishing of strong short smectic order within of the 3BCN/14 columns.

Analysis of multiple internal reflections in a parallel aligned liquid crystal on silicon SLM.

PubMed

Martínez, José Luis; Moreno, Ignacio; del Mar Sánchez-López, María; Vargas, Asticio; García-Martínez, Pascuala

2014-10-20

Multiple internal reflection effects on the optical modulation of a commercial reflective parallel-aligned liquid-crystal on silicon (PAL-LCoS) spatial light modulator (SLM) are analyzed. The display is illuminated with different wavelengths and different angles of incidence. Non-negligible Fabry-Perot (FP) effect is observed due to the sandwiched LC layer structure. A simplified physical model that quantitatively accounts for the observed phenomena is proposed. It is shown how the expected pure phase modulation response is substantially modified in the following aspects: 1) a coupled amplitude modulation, 2) a non-linear behavior of the phase modulation, 3) some amount of unmodulated light, and 4) a reduction of the effective phase modulation as the angle of incidence increases. Finally, it is shown that multiple reflections can be useful since the effect of a displayed diffraction grating is doubled on a beam that is reflected twice through the LC layer, thus rendering gratings with doubled phase modulation depth.

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

Cuttitta, Christina M.; Ericson, Daniel L.; Scalia, Alexander

Acoustic droplet ejection (ADE) is an emerging technology with broad applications in serial crystallography such as growing, improving and manipulating protein crystals. One application of this technology is to gently transfer crystals onto MiTeGen micromeshes with minimal solvent. Once mounted on a micromesh, each crystal can be combined with different chemicals such as crystal-improving additives or a fragment library. Acoustic crystal mounting is fast (2.33 transfers s -1) and all transfers occur in a sealed environment that is in vapor equilibrium with the mother liquor. Here, a system is presented to retain crystals near the ejection point and away frommore » the inaccessible dead volume at the bottom of the well by placing the crystals on a concave agarose pedestal (CAP) with the same chemical composition as the crystal mother liquor. The bowl-shaped CAP is impenetrable to crystals. Consequently, gravity will gently move the crystals into the optimal location for acoustic ejection. It is demonstrated that an agarose pedestal of this type is compatible with most commercially available crystallization conditions and that protein crystals are readily transferred from the agarose pedestal onto micromeshes with no loss in diffraction quality. It is also shown that crystals can be grown directly on CAPs, which avoids the need to transfer the crystals from the hanging drop to a CAP. This technology has been used to combine thermolysin and lysozyme crystals with an assortment of anomalously scattering heavy atoms. The results point towards a fast nanolitre method for crystal mounting and high-throughput screening.« less

Polymorphism in R-tamsulosin (an alpha blocker): The unexpected manifestation of a sulfonamide⋯o-diethoxybenzene heterosynthon

NASA Astrophysics Data System (ADS)

Nanubolu, Jagadeesh Babu; Sridhar, Balasubramanian; Ravikumar, Krishnan

2014-12-01

A two point Nsbnd H⋯O dimer or an infinite catemer are the most preferred motifs/synthons for sulfonamide structures. Such synthons are known to be so robust that they are only disrupted in the presence of highly activated O acceptors such as pyridine-N-oxide and sulfoxide. We demonstrate in this article that a multi-point synthon offered by much weaker ethoxy O and amine N acceptors can however strongly compete and disrupt the robust sulfonamide homosynthons. This has been illustrated with the synthon analysis in three polymorphic crystal structures of R-tamsulosin, an active drug used in the treatment of Benign Prostatic Hyperplasia (BPH) and its hydrochloride salt. These crystalline solids are characterized by Single crystal X-ray diffraction (SC-XRD), powder X-ray diffraction (PXRD), Fourier Transform Infrared (FT-IR) and Raman spectroscopy. Forms I, II of the free base and hydrochloride salt crystallize in the monoclinic P21, C2, and P21 space groups respectively with two molecules in the asymmetric unit (Z‧ = 2), whereas, form III of freebase crystallize in the orthorhombic P212121 space group with Z‧ = 1. Remarkably, all four crystal structures contain a totally unexpected sulfonamide⋯o-diethoxybenzene heterosynthon. The multi-point motifs observed in polymorphs are relatively stronger than those in the hydrochloride salt because of the gauche conformation of the tamsulosin linker chain which renders an additional hydrogen bond interaction with amine N acceptor, and resemble the crown ether sulfonamide recognition pattern. Observation of this new heterosynthon offers potential scope in the design of pharmaceutical cocrystals for sulfonamide bearing drug molecules. The present study also presents a detailed hydrogen bond motif analysis in 310 primary sulfonamide structures culled from the latest version of Cambridge Structural Database (CSD). The role of various competing groups is discussed in the context of understanding the most recurring sulfonamide homo and heterosynthons.

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

Zhao, Haishuang; Krysiak, Yaşar; Hoffmann, Kristin

The crystal structure and disorder phenomena of Al{sub 4}B{sub 2}O{sub 9}, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al{sub 4}B{sub 2}O{sub 9}, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO{sub 6} octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along themore » b axis are observed. Analysis of the modulation pattern implies a mean superstructure (AAB) with a threefold b axis, where B corresponds to an A layer shifted by ½a and ½c. Diffraction patterns simulated for the AAB sequence including additional stacking disorder are in good agreement with experimental electron diffraction patterns. - Graphical abstract: Crystal structure and disorder phenomena of B-rich Al{sub 4}B{sub 2}O{sub 9} studied by automated electron diffraction tomography (ADT) and described by diffraction simulation using DISCUS. - Highlights: • Ab-initio structure solution by electron diffraction from single nanocrystals. • Detected modulation corresponding mainly to three-fold superstructure. • Diffuse diffraction streaks caused by stacking faults in disordered crystals. • Observed streaks explained by simulated electron diffraction patterns.« less

Optical Anisotropy of Photonic Crystals of Cubic Symmetry Induced by Multiple Diffraction of Light

NASA Astrophysics Data System (ADS)

Ukleev, T. A.; Shevchenko, N. N.; Iurasova, D. I.; Sel'kin, A. V.

2018-05-01

The optical spectra of Bragg reflection from opal-like photonic crystals under conditions of the resonant enhancement of the multiple diffraction of light have been studied experimentally and theoretically using the photonic crystal structures prepared of monodisperse polystyrene globules. It is shown that the reflection signal registered in mutually orthogonal configurations of the polarizer and analyzer is related to the intrinsic optical anisotropy of the crystals and is a specific manifestation of the multiple Bragg diffraction in three-dimensional photonic crystals.

Orientational order and rotational relaxation in the plastic crystal phase of tetrahedral molecules.

PubMed

Rey, Rossend

2008-01-17

A methodology recently introduced to describe orientational order in liquid carbon tetrachloride is extended to the plastic crystal phase of XY4 molecules. The notion that liquid and plastic crystal phases are germane regarding orientational order is confirmed for short intermolecular distances but is seen to fail beyond, as long range orientational correlations are found for the simulated solid phase. It is argued that, if real, such a phenomenon may not to be accessible with direct (diffraction) methods due to the high molecular symmetry. This behavior is linked to the existence of preferential orientation with respect to the fcc crystalline network defined by the centers of mass. It is found that the dominant class accounts, at most, for one-third of all configurations, with a feeble dependence on temperature. Finally, the issue of rotational relaxation is also addressed, with an excellent agreement with experimental measures. It is shown that relaxation is nonhomogeneous in the picosecond range, with a slight dispersion of decay times depending on the initial orientational class. The results reported mainly correspond to neopentane over a wide temperature range, although results for carbon tetrachloride are included, as well.

Effect of Interface Shape and Magnetic Field on the Microstructure of Bulk Ge:Ga

NASA Technical Reports Server (NTRS)

Cobb, S. D.; Szofran, F. R.; Volz, M. P.

1999-01-01

Thermal and compositional gradients induced during the growth process contribute significantly to the development of defects in the solidified boule. Thermal gradients and the solid-liquid interface shape can be greatly effected by ampoule material. Compositional gradients are strongly influenced by interface curvature and convective flow in the liquid. Results of this investigation illustrate the combined influences of interface shape and convective fluid flow. An applied magnetic field was used to reduce the effects of convective fluid flow in the electrically conductive melt during directional solidification. Several 8 mm diameter boules of Ga-doped Ge were grown at different field strengths, up to 5 Tesla, in four different ampoule materials. Compositional profiles indicate mass transfer conditions ranged from completely mixed to diffusion controlled. The influence of convection in the melt on the developing crystal microstructure and defect density was investigated as a function of field strength and ampoule material. Chemical etching and electron backscattered electron diffraction were used to map the crystal structure of each boule along the center plane. Dislocation etch pit densities were measured for each boule. Results show the influence of magnetic field strength and ampoule material on overall crystal quality.

Third-order nonlinear electro-optic measurements in the smectic-? phase

NASA Astrophysics Data System (ADS)

Nowicka, Kamila; Bielejewska, Natalia

2018-02-01

The chiral smectic subphase with three-layer structure, ?, is now of great interest from the point of view of device technologies such as multistate or symmetric switching. We report that the unique nonlinear electro-optic response can serve as precise mark of the phase transition into three-layer structure. The problem is illustrated with the first and third harmonic electro-optic spectra. Furthermore, the characteristic response of the helical liquid crystal phases correlated with particular collective modes using the Debye-type relaxation method for the well-known prototype liquid crystal material (MHPOBC) are presented.

European Scientific Notes. Volume 35. Number 1.

DTIC Science & Technology

1981-01-31

thermotropic polymers, primar- formed smectic phases. She also studied ily with aromatic polyesters. Dr. R.W. the orientation of liquid crystal ...booster synchrotron and Linac are switched studies of crystals where a very good off and the electrons are allowed to approximation to a point source...compounds in the temperature Cr in a MgO host crystal in magnetic range of 1 to 25 K and as a function of fields up to 2*S T at temperatures between

Improving the diffraction of apoA-IV crystals through extreme dehydration.

PubMed

Deng, Xiaodi; Davidson, W Sean; Thompson, Thomas B

2012-01-01

Apolipoproteins are the protein component of high-density lipoproteins (HDL), which are necessary for mobilizing lipid-like molecules throughout the body. Apolipoproteins undergo self-association, especially at higher concentrations, making them difficult to crystallize. Here, the crystallization and diffraction of the core fragment of apolipoprotein A-IV (apoA-IV), consisting of residues 64-335, is presented. ApoA-IV(64-335) crystallized readily in a variety of hexagonal (P6) morphologies with similar unit-cell parameters, all containing a long axis of nearly 550 Å in length. Preliminary diffraction experiments with the different crystal morphologies all resulted in limited streaky diffraction to 3.5 Å resolution. Crystal dehydration was applied to the different morphologies with variable success and was also used as a quality indicator of crystal-growth conditions. The results show that the morphologies that withstood the most extreme dehydration conditions showed the greatest improvement in diffraction. One morphology in particular was able to withstand dehydration in 60% PEG 3350 for over 12 h, which resulted in well defined intensities to 2.7 Å resolution. These results suggest that the approach of integrating dehydration with variation in crystal-growth conditions might be a general technique to optimize diffraction. © 2012 International Union of Crystallography. All rights reserved.

Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements

DOE PAGES

Hofmann, Felix; Phillips, Nicholas W.; Harder, Ross J.; ...

2017-08-08

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here, in this paper, a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focusedmore » ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Lastly, our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.« less

Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements

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

Hofmann, Felix; Phillips, Nicholas W.; Harder, Ross J.

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here, in this paper, a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focusedmore » ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Lastly, our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.« less

Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements.

PubMed

Hofmann, Felix; Phillips, Nicholas W; Harder, Ross J; Liu, Wenjun; Clark, Jesse N; Robinson, Ian K; Abbey, Brian

2017-09-01

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focused ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.

Micro-beam Laue Alignment of Multi-Reflection Bragg Coherent Diffraction Imaging Measurements

PubMed Central

Hofmann, Felix; Phillips, Nicholas W.; Harder, Ross J.; Liu, Wenjun; Clark, Jesse N.; Robinson, Ian K.; Abbey, Brian

2017-01-01

Multi-reflection Bragg coherent diffraction imaging has the potential to allow 3D resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here we demonstrate a different approach, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focussed ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples. PMID:28862628

Local Order-Disorder Transition Driving by Structural Heterogeneity in a Benzyl Functionalized Ionic Liquid.

PubMed

Faria, Luiz F O; Paschoal, Vitor H; Lima, Thamires A; Ferreira, Fabio F; Freitas, Rafael S; Ribeiro, Mauro C C

2017-10-26

A local order-disorder transition has been disclosed in the thermophysical behavior of the ionic liquid 1-benzyl-3-methylimidazolium dicyanamide, [Bzmim][N(CN) 2 ], and its microscopic nature revealed by spectroscopic techniques. Differential scanning calorimetry and specific heat measurements show a thermal event of small enthalpy variation taking place in the range 250-260 K, which is not due to crystallization or melting. Molecular dynamic simulations and X-ray diffraction measurements have been used to discuss the segregation of domains in the liquid structure of [Bzmim][N(CN) 2 ]. Raman and NMR spectroscopy measurements as a function of temperature indicate that the microscopic origin of the event observed in the calorimetric measurements comes from structural rearrangement involving the benzyl group. The results indicate that the characteristic structural heterogeneity allow for rearrangements within local domains implying the good glass-forming ability for the low viscosity ionic liquid [Bzmim][N(CN) 2 ]. This work sheds light on our understanding of the microscopic origin behind complex thermal behavior of ionic liquids.

Crystallization and preliminary X-ray analysis of the ergothioneine-biosynthetic methyltransferase EgtD

PubMed Central

Vit, Allegra; Misson, Laëtitia; Blankenfeldt, Wulf; Seebeck, Florian Peter

2014-01-01

Ergothioneine is an amino-acid betaine derivative of histidine that was discovered more than one century ago. Despite significant research pointing to a function in oxidative stress defence, the exact mechanisms of action of ergothioneine remain elusive. Although both humans and bacterial pathogens such as Mycobacterium tuberculosis seem to depend on ergothioneine, humans are devoid of the corresponding biosynthetic enzymes. Therefore, its biosyn­thesis may emerge as potential drug target in the development of novel therapeutics against tuberculosis. The recent identification of ergothioneine-biosynthetic genes in M. smegmatis enables a more systematic study of its biology. The pathway is initiated by EgtD, a SAM-dependent methyltransferase that catalyzes a trimethylation reaction of histidine to give N(α),N(α),N(α)-trimethylhistidine. Here, the recombinant production, purification and crystallization of EgtD are reported. Crystals of native EgtD diffracted to 2.35 Å resolution at a synchrotron beamline, whereas crystals of seleno-l-methionine-labelled protein diffracted to 1.75 Å resolution and produced a significant anomalous signal to 2.77 Å resolution at the K edge. All of the crystals belonged to space group P212121, with two EgtD monomers in the asymmetric unit. PMID:24817736

Mesoscopic monodisperse ferromagnetic colloids enable magnetically controlled photonic crystals.

PubMed

Xu, Xiangling; Majetich, Sara A; Asher, Sanford A

2002-11-20

We report here the first synthesis of mesoscopic, monodisperse particles which contain nanoscopic inclusions of ferromagnetic cobalt ferrites. These monodisperse ferromagnetic composite particles readily self-assemble into magnetically responsive photonic crystals that efficiently Bragg diffract incident light. Magnetic fields can be used to control the photonic crystal orientation and, thus, the diffracted wavelength. We demonstrate the use of these ferromagnetic particles to fabricate magneto-optical diffracting fluids and magnetically switchable diffracting mirrors.

Inclined monochromator for high heat-load synchrotron x-ray radiation

DOEpatents

Khounsary, A.M.

1994-02-15

A double crystal monochromator is described including two identical, parallel crystals, each of which is cut such that the normal to the diffraction planes of interest makes an angle less than 90 degrees with the surface normal. Diffraction is symmetric, regardless of whether the crystals are symmetrically or asymmetrically cut, enabling operation of the monochromator with a fixed plane of diffraction. As a result of the inclination of the crystal surface, an incident beam has a footprint area which is elongated both vertically and horizontally when compared to that of the conventional monochromator, reducing the heat flux of the incident beam and enabling more efficient surface cooling. Because after inclination of the crystal only a fraction of thermal distortion lies in the diffraction plane, slope errors and the resultant misorientation of the diffracted beam are reduced. 11 figures.

Inclined monochromator for high heat-load synchrotron x-ray radiation

DOEpatents

Khounsary, Ali M.

1994-01-01

A double crystal monochromator including two identical, parallel crystals, each of which is cut such that the normal to the diffraction planes of interest makes an angle less than 90 degrees with the surface normal. Diffraction is symmetric, regardless of whether the crystals are symmetrically or asymmetrically cut, enabling operation of the monochromator with a fixed plane of diffraction. As a result of the inclination of the crystal surface, an incident beam has a footprint area which is elongated both vertically and horizontally when compared to that of the conventional monochromator, reducing the heat flux of the incident beam and enabling more efficient surface cooling. Because after inclination of the crystal only a fraction of thermal distortion lies in the diffraction plane, slope errors and the resultant misorientation of the diffracted beam are reduced.

Phase-field crystal simulation facet and branch crystal growth

NASA Astrophysics Data System (ADS)

Chen, Zhi; Wang, Zhaoyang; Gu, Xinrui; Chen, Yufei; Hao, Limei; de Wit, Jos; Jin, Kexin

2018-05-01

Phase-field crystal model with one mode is introduced to describe morphological transition. The relationship between growth morphology and smooth density distribution was investigated. The results indicate that the pattern selection of dendrite growth is caused by the competition between interface energy anisotropy and interface kinetic anisotropy based on the 2D phase diagram. When the calculation time increases, the crystal grows to secondary dendrite at the dimensionless undercooling equal to - 0.4. Moreover, when noise is introduced in the growth progress, the symmetry is broken in the growth mode, and there becomes irregular fractal-like growth morphology. Furthermore, the single crystal shape develops into polycrystalline when the noise amplitude is large enough. When the dimensionless undercooling is less than - 0.3, the noise has a significant effect on the growth shape. In addition, the growth velocity of crystal near to liquid phase line is slow, while the shape far away from the liquid adapts to fast growth. Based on the simulation results, the method was proved to be effective, and it can easily obtain different crystal shapes by choosing the different points in 2D phase diagram.

Water polygons in high-resolution protein crystal structures.

PubMed

Lee, Jonas; Kim, Sung-Hou

2009-07-01

We have analyzed the interstitial water (ISW) structures in 1500 protein crystal structures deposited in the Protein Data Bank that have greater than 1.5 A resolution with less than 90% sequence similarity with each other. We observed varieties of polygonal water structures composed of three to eight water molecules. These polygons may represent the time- and space-averaged structures of "stable" water oligomers present in liquid water, and their presence as well as relative population may be relevant in understanding physical properties of liquid water at a given temperature. On an average, 13% of ISWs are localized enough to be visible by X-ray diffraction. Of those, averages of 78% are water molecules in the first water layer on the protein surface. Of the localized ISWs beyond the first layer, almost half of them form water polygons such as trigons, tetragons, as well as expected pentagons, hexagons, higher polygons, partial dodecahedrons, and disordered networks. Most of the octagons and nanogons are formed by fusion of smaller polygons. The trigons are most commonly observed. We suggest that our observation provides an experimental basis for including these water polygon structures in correlating and predicting various water properties in liquid state.

Water polygons in high-resolution protein crystal structures

PubMed Central

Lee, Jonas; Kim, Sung-Hou

2009-01-01

We have analyzed the interstitial water (ISW) structures in 1500 protein crystal structures deposited in the Protein Data Bank that have greater than 1.5 Å resolution with less than 90% sequence similarity with each other. We observed varieties of polygonal water structures composed of three to eight water molecules. These polygons may represent the time- and space-averaged structures of “stable” water oligomers present in liquid water, and their presence as well as relative population may be relevant in understanding physical properties of liquid water at a given temperature. On an average, 13% of ISWs are localized enough to be visible by X-ray diffraction. Of those, averages of 78% are water molecules in the first water layer on the protein surface. Of the localized ISWs beyond the first layer, almost half of them form water polygons such as trigons, tetragons, as well as expected pentagons, hexagons, higher polygons, partial dodecahedrons, and disordered networks. Most of the octagons and nanogons are formed by fusion of smaller polygons. The trigons are most commonly observed. We suggest that our observation provides an experimental basis for including these water polygon structures in correlating and predicting various water properties in liquid state. PMID:19551896

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

NASA Technical Reports Server (NTRS)

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

1999-01-01

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

Dicyanamide Salts that Adopt Smectic, Columnar, or Bicontinuous Cubic Liquid-Crystalline Mesophases.

PubMed

Park, Geonhui; Goossens, Karel; Shin, Tae Joo; Bielawski, Christopher W

2018-04-25

Although dicyanamide (i.e., [N(CN) 2 ] - ) has been commonly used to obtain low-viscosity, halogen-free, room-temperature ionic liquids, liquid-crystalline salts containing such anions have remained virtually unexplored. Here we report a series of amphiphilic dicyanamide salts that, depending on their structures and compositions, adopt smectic, columnar, or bicontinuous cubic thermotropic liquid-crystalline mesophases, even at room temperature in some cases. Their thermal properties were explored by polarized light optical microscopy, differential scanning calorimetry, thermogravimetric analysis (including evolved gas analysis), and variable-temperature synchrotron X-ray diffraction. Comparison of the thermal phase characteristics of these new liquid-crystalline salts featuring "V-shaped" [N(CN) 2 ] - anions with those of structural analogues containing [SCN] - , [BF 4 ] - , [PF 6 ] - , or [CF 3 SO 3 ] - anions indicated that not only the size of the counterion but also its shape should be considered in the development of mesomorphic salts. Collectively, these discoveries may be expected to facilitate the design of thermotropic ionic liquid crystals that form inverted-type bicontinuous cubic and other sophisticated liquid-crystalline phases. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Influence of Hydrogen Bond on Thermal and Phase Transitions of Binary Complex Liquid Crystals

NASA Astrophysics Data System (ADS)

Vijayakumar, V. N.; Rajasekaran, T. R.; Baskar, K.

2017-12-01

A novel supramolecular liquid crystal (LC) is synthesized from the binary complex of 4-decyloxy benzoic acid and cholesteryl acetate. Fourier transform infrared (FTIR) spectroscopic study confirms the formation of intermolecular hydrogen bond between the mesogens. Various mesophases and corresponding textural changes in the complex are observed by comparing with its constituents through polarizing optical microscopic (POM) studies. The thermal stability factor of smectic phase for present complex is calculated. An interesting observation of present work is that investigation of extended thermal span of mesomorphic phases, decreased enthalpy, a nematic phase with a high clearing point and a low melting point. This is due to an arrangement of molecular reorientations and the development of new associations by hydrogen bonding. Optical tilt angle for smectic C phase is determined and the same is fitted to a power law.

Chloride influence on the formation of lanthanum hexaboride: An in-situ diffraction study

DOE PAGES

Mattox, Tracy M.; Groome, Chloe; Doran, Andrew; ...

2018-01-31

LaB 6 has been a material of interest for decades due to its thermionic emission, plasmonic properties, and low work function, and researchers continue to discover new properties even now. In order to meet growing interest in customizing these properties, it is important to gain better control over the system and a better understanding of the fundamental mechanism of LaB 6 crystal growth and formation. Traditional synthetic methods require very high temperatures, at which point crystallization happens too quickly to be readily studied. Our discovery that LaB 6 may be made using lower temperatures has made it possible to slowmore » down crystal formation enough for lattice growth to be observed. Here, we report an in situ diffraction study of the reaction between LaCl 3 and NaBH 4 . In observing the evolution of the (1 1 1), (1 1 0), and (2 0 0) lattice planes of LaB 6, we have discovered that the Cl of LaCl3 has a strong influence on crystal formation, and that excess Cl, temperature and heating rate may all be used as tools to control the LaB 6 final product.« less

Chloride influence on the formation of lanthanum hexaboride: An in-situ diffraction study

NASA Astrophysics Data System (ADS)

Mattox, Tracy M.; Groome, Chloe; Doran, Andrew; Beavers, Christine M.; Urban, Jeffrey J.

2018-03-01

LaB6 has been a material of interest for decades due to its thermionic emission, plasmonic properties, and low work function, and researchers continue to discover new properties even now. In order to meet growing interest in customizing these properties, it is important to gain better control over the system and a better understanding of the fundamental mechanism of LaB6 crystal growth and formation. Traditional synthetic methods require very high temperatures, at which point crystallization happens too quickly to be readily studied. Our discovery that LaB6 may be made using lower temperatures has made it possible to slow down crystal formation enough for lattice growth to be observed. We report here an in situ diffraction study of the reaction between LaCl3 and NaBH4. In observing the evolution of the (1 1 1), (1 1 0), and (2 0 0) lattice planes of LaB6, we have discovered that the Cl of LaCl3 has a strong influence on crystal formation, and that excess Cl, temperature and heating rate may all be used as tools to control the LaB6 final product.

Time-resolved X-ray diffraction microprobe studies of the conversion of cellulose I to ethylenediamine-cellulose I

PubMed Central

Nishiyama, Yoshiharu; Wada, Masahisa; Hanson, B. Leif

2012-01-01

Structural changes during the treatment of films of highly crystalline microfibers of Cladophora cellulose with ethylenediamine (EDA) have been studied by time-resolved X-ray microprobe diffraction methods. As EDA penetrates the sample and converts cellulose I to EDA-cellulose I, the measured profile widths of reflections reveal changes in the shapes and average dimensions of cellulose I and EDA-cellulose I crystals. The (200) direction of cellulose I is most resistant to EDA penetration, with EDA penetrating most effectively at the hydrophilic edges of the hydrogen bonded sheets of cellulose chains. Most of the cellulose chains in the initial crystals of cellulose I are incorporated into crystals of EDA-cellulose I. The size of the emerging EDA-cellulose I crystals is limited to about half of their size in cellulose I, most likely due to strains introduced by the penetration of EDA molecules. There is no evidence of any gradual structural transition from cellulose I to EDA-cellulose I involving a continuously changing intermediate phase. Rather, the results point to a rapid transition to EDA-cellulose I in regions of the microfibrils that have been penetrated by EDA. PMID:22693365

Chloride influence on the formation of lanthanum hexaboride: An in-situ diffraction study

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

Mattox, Tracy M.; Groome, Chloe; Doran, Andrew

LaB 6 has been a material of interest for decades due to its thermionic emission, plasmonic properties, and low work function, and researchers continue to discover new properties even now. In order to meet growing interest in customizing these properties, it is important to gain better control over the system and a better understanding of the fundamental mechanism of LaB 6 crystal growth and formation. Traditional synthetic methods require very high temperatures, at which point crystallization happens too quickly to be readily studied. Our discovery that LaB 6 may be made using lower temperatures has made it possible to slowmore » down crystal formation enough for lattice growth to be observed. Here, we report an in situ diffraction study of the reaction between LaCl 3 and NaBH 4 . In observing the evolution of the (1 1 1), (1 1 0), and (2 0 0) lattice planes of LaB 6, we have discovered that the Cl of LaCl3 has a strong influence on crystal formation, and that excess Cl, temperature and heating rate may all be used as tools to control the LaB 6 final product.« less

Stokes parameter studies of spontaneous emission from chiral nematic liquid crystals as a one-dimensional photonic stopband crystal: experiment and theory.

PubMed

Woon, Kai L; O'Neill, Mary; Richards, Gary J; Aldred, Matthew P; Kelly, Stephen M

2005-04-01

The helical structure of uniformly aligned chiral nematic liquid crystals results in a photonic stopband for only one sense of circular polarization. The spectroscopic Stokes polarimeter is used to analyze spontaneous emission in the stopband. Highly polarized photoluminescence is found and the polarization properties vary with the excitation wavelength. Spontaneous emission is enhanced at the stopband edge and this Purcell effect is greater on excitation at wavelengths where the absorption coefficient is low. This is interpreted as greater overlap between the excited molecules and the electrical modal field of the resonant modes at the stopband edge. Photoluminescence detected from the excitation face of the liquid crystal cell is less polarized because of photon tunneling. Fermi's golden rule in conjunction with Stokes vectors is used to model the polarization of emission taking multiple reflections at the interfaces of the cell into account. The discrepancy between the experiment and the theoretical model is interpreted as direct experimental evidence that virtual photons, which originate from zero point fluctuations of quantum space, are randomly polarized.

The nucleation and growth mechanism of Ni-Sn eutectic in a single crystal superalloy

NASA Astrophysics Data System (ADS)

Jiang, Weiguo; Wang, Li; Li, Xiangwei; Lou, Langhong

2017-12-01

The microstructure of single crystal superalloy with and without tin layer on the surface of as-cast and heat-treatment state was investigated by optical microscope (OM) and scanning electron microscopy (SEM). The composition of different regions on the surface was tested by energy dispersive X-ray (EDS). The reaction intermetallic compound (IMC) formed in the heat treatment process was confirmed by X-ray diffraction (XRD). The orientations of different microstructure in samples as heat treatment state were determined by electron back-scattering diffraction (EBSD) method. The porosity location in the interdendritic region was observed by X-ray computed tomography (XCT). The experiment results showed that the remained Sn on the surface of the superalloy reacted with Ni, and then formed Ni3Sn4 in the as-cast state. Sn enriched by diffusion along the porosity located in the interdendritic region and γ + γ‧ (contain a little of Sn) eutectic and Ni3Sn2 formed in single crystal superalloy during heat treatment, and the recalescence behaviors were found. Ni3Sn2 nucleated independently in the cooled liquid at the front of (γ + γ‧) (Sn) eutectic. The nucleation and growth mechanism of the eutectic and Ni3Sn2 IMC during heat treatment was discussed in the present paper.

Layered water in crystal interfaces as source for bone viscoelasticity: arguments from a multiscale approach

PubMed Central

Eberhardsteiner, Lukas; Hellmich, Christian; Scheiner, Stefan

2012-01-01

Extracellular bone material can be characterised as a nanocomposite where, in a liquid environment, nanometre-sized hydroxyapatite crystals precipitate within as well as between long fibre-like collagen fibrils (with diameters in the 100 nm range), as evidenced from neutron diffraction and transmission electron microscopy. Accordingly, these crystals are referred to as ‘interfibrillar mineral’ and ‘extrafibrillar mineral’, respectively. From a topological viewpoint, it is probable that the mineralisations start on the surfaces of the collagen fibrils (‘mineral-encrusted fibrils’), from where the crystals grow both into the fibril and into the extrafibrillar space. Since the mineral concentration depends on the pore spaces within the fibrils and between the fibrils (there is more space between them), the majority of the crystals (but clearly not all of them) typically lie in the extrafibrillar space. There, larger crystal agglomerations or clusters, spanning tens to hundreds of nanometers, develop in the course of mineralisation, and the micromechanics community has identified the pivotal role, which this extrafibrillar mineral plays for tissue elasticity. In such extrafibrillar crystal agglomerates, single crystals are stuck together, their surfaces being covered with very thin water layers. Recently, the latter have caught our interest regarding strength properties (Fritsch et al. 2009 J Theor Biol. 260(2): 230–252) – we have identified these water layers as weak interfaces in the extrafibrillar mineral of bone. Rate-independent gliding effects of crystals along the aforementioned interfaces, once an elastic threshold is surpassed, can be related to overall elastoplastic material behaviour of the hierarchical material ‘bone’. Extending this idea, the present paper is devoted to viscous gliding along these interfaces, expressing itself, at the macroscale, in the well-known experimentally evidenced phenomenon of bone viscoelasticity. In this context, a multiscale homogenisation scheme is extended to viscoelasticity, mineral-cluster-specific creep parameters are identified from three-point bending tests on hydrated bone samples, and the model is validated by statistically and physically independent experiments on partially dried samples. We expect this model to be relevant when it comes to prediction of time-dependent phenomena, e.g. in the context of bone remodelling. PMID:22563708

Layered water in crystal interfaces as source for bone viscoelasticity: arguments from a multiscale approach.

PubMed

Eberhardsteiner, Lukas; Hellmich, Christian; Scheiner, Stefan

2014-01-01

Extracellular bone material can be characterised as a nanocomposite where, in a liquid environment, nanometre-sized hydroxyapatite crystals precipitate within as well as between long fibre-like collagen fibrils (with diameters in the 100 nm range), as evidenced from neutron diffraction and transmission electron microscopy. Accordingly, these crystals are referred to as 'interfibrillar mineral' and 'extrafibrillar mineral', respectively. From a topological viewpoint, it is probable that the mineralisations start on the surfaces of the collagen fibrils ('mineral-encrusted fibrils'), from where the crystals grow both into the fibril and into the extrafibrillar space. Since the mineral concentration depends on the pore spaces within the fibrils and between the fibrils (there is more space between them), the majority of the crystals (but clearly not all of them) typically lie in the extrafibrillar space. There, larger crystal agglomerations or clusters, spanning tens to hundreds of nanometers, develop in the course of mineralisation, and the micromechanics community has identified the pivotal role, which this extrafibrillar mineral plays for tissue elasticity. In such extrafibrillar crystal agglomerates, single crystals are stuck together, their surfaces being covered with very thin water layers. Recently, the latter have caught our interest regarding strength properties (Fritsch et al. 2009 J Theor Biol. 260(2): 230-252) - we have identified these water layers as weak interfaces in the extrafibrillar mineral of bone. Rate-independent gliding effects of crystals along the aforementioned interfaces, once an elastic threshold is surpassed, can be related to overall elastoplastic material behaviour of the hierarchical material 'bone'. Extending this idea, the present paper is devoted to viscous gliding along these interfaces, expressing itself, at the macroscale, in the well-known experimentally evidenced phenomenon of bone viscoelasticity. In this context, a multiscale homogenisation scheme is extended to viscoelasticity, mineral-cluster-specific creep parameters are identified from three-point bending tests on hydrated bone samples, and the model is validated by statistically and physically independent experiments on partially dried samples. We expect this model to be relevant when it comes to prediction of time-dependent phenomena, e.g. in the context of bone remodelling.

Total reflection infrared spectroscopy of water-ice and frozen aqueous NaCl solutions

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

Walker, Rachel L.; Searles, Keith; Willard, Jesse A.

2013-12-28

Liquid-like and liquid water at and near the surface of water-ice and frozen aqueous sodium chloride films were observed using attenuated total reflection infrared spectroscopy (ATR-IR). The concentration of NaCl ranged from 0.0001 to 0.01 M and the temperature varied from the melting point of water down to 256 K. The amount of liquid brine at the interface of the frozen films with the germanium ATR crystal increased with salt concentration and temperature. Experimental spectra are compared to reflection spectra calculated for a simplified morphology of a uniform liquid layer between the germanium crystal and the frozen film. This morphologymore » allows for the amount of liquid observed in an experimental spectrum to be converted to the thickness of a homogenous layer with an equivalent amount of liquid. These equivalent thickness ranges from a nanometer for water-ice at 260 K to 170 nm for 0.01 M NaCl close to the melting point. The amounts of brine observed are over an order of magnitude less than the total liquid predicted by equilibrium thermodynamic models, implying that the vast majority of the liquid fraction of frozen solutions may be found in internal inclusions, grain boundaries, and the like. Thus, the amount of liquid and the solutes dissolved in them that are available to react with atmospheric gases on the surfaces of snow and ice are not well described by thermodynamic equilibrium models which assume the liquid phase is located entirely at the surface.« less

Diffractive-refractive optics: X-ray splitter.

PubMed

Hrdý, Jaromír

2010-01-01

The possibility of splitting a thin (e.g. undulator) X-ray beam based on diffraction-refraction effects is discussed. The beam is diffracted from a crystal whose diffracting surface has the shape of a roof with the ridge lying in the plane of diffraction. The crystal is cut asymmetrically. One half of the beam impinges on the left-hand part of the roof and the other half impinges on the right-hand side of the roof. Owing to refraction the left part of the beam is deviated to the left whereas the right part is deviated to the right. The device proposed consists of two channel-cut crystals with roof-like diffraction surfaces; the crystals are set in a dispersive position. The separation of the beams after splitting is calculated at a distance of 10 m from the crystals for various asymmetry and inclination angles. It is shown that such a splitting may be utilized for long beamlines. Advantages and disadvantages of this method are discussed.

Optical, mechanical and thermal behaviors of Nitrilotriacetic acid single crystal

NASA Astrophysics Data System (ADS)

Deepa, B.; Philominathan, P.

2017-11-01

An organic nonlinear single crystal of Nitrilotriacetic acid (NTAA) was grown for the first time by employing a simple slow evaporation technique. Single crystal X-ray diffraction (XRD) analysis reveals that the grown crystal belongs to the monoclinic system with noncentrosymmetric space group CC. Fourier transform infrared (FTIR) spectral study ascertains the presence of functional groups in NTAA. The molecular structure of the grown crystal was confirmed by Nuclear Magnetic Resonance (NMR) spectral analysis. The optical parameters such as transmittance, absorption coefficient and band gap were calculated from UV-Visible and fluorescence studies. Dielectric measurements were carried out for different frequency and temperature. The mechanical strength of the grown crystal was measured using Vickers microhardness test. The high thermal stability and the melting point of the grown crystal were also estimated using thermogravimetric (TGA) and differential thermal analyses (DTA). The confirmation of the grown crystals belonging to nonlinear optical crystals was performed by Kurtz-Perry technique and found as suitable candidate for optoelectronics applications.

Habit control of deuterated potassium dihydrogen phosphate crystal for laser applications

NASA Astrophysics Data System (ADS)

Guzman, L. A.; Suzuki, M.; Fujimoto, Y.; Fujioka, K.

2016-03-01

In this study we investigate the habit of partially deuterated potassium dihydrogen phosphate (DKDP) crystals in the presence of Al3+ ions. We have grown single DKDP crystals in (50wt% and 80wt%) partially deuterated solutions and in solutions doped with Al3+ ions (2 ppm) by the point-seed rapid growth technique at controlled supercooling (ΔT=10°C). The growth length of each crystal face was measured and the aspect ratio was calculated. We found that crystals grown in partially deuterated solutions are similar in aspect ratio, while, crystals grown in deuterated solutions doped with Al3+ ions showed a relative change in aspect ratio, the crystal increased in size in the pyramidal direction (vertical axis direction). Crystal characteristics were also analyzed by X-ray diffraction, FTIR and Raman spectroscopy. We have speculated that the relative habit modification is due to a probably adsorption and inclusions of Al3+ ions in the prismatic section of the crystal.

Effects of alkyl chain length and anion size on thermal and structural properties for 1-alkyl-3-methylimidazolium hexafluorocomplex salts (C(x)MImAF6, x = 14, 16 and 18; A = P, As, Sb, Nb and Ta).

PubMed

Xu, Fei; Matsumoto, Kazuhiko; Hagiwara, Rika

2012-03-28

A series of 1-alkyl-3-methylimidazolium hexafluorocomplex salts (C(x)MImAF(6), x = 14, 16 and 18, A = P, As, Sb, Nb and Ta) have been characterized by thermal analysis, X-ray diffraction and polarized optical microscopy. A liquid crystalline mesophase is observed for all the C(16)MIm and C(18)MIm salts. The C(14)MIm(+) cation gives a liquid crystalline mesophase only with PF(6)(-). The temperature range of the liquid crystalline mesophase increases with an increase in alkyl chain length or with decrease in anion size. Single-crystal X-ray diffraction revealed that all the C(18)MImAF(6) salts (A = P, As, Sb, Nb and Ta) are isostructural with each other in the crystalline phase and have a layered structure. The interdigitated alkyl chain of the cation has a bent shape like a spoon near the imidazolium ring in the crystalline phase at -100 °C and is tilted with respect to the sheets of the imidazolium headgroups and anions. An increase of temperature increases the ratio of an all-trans conformation to the bent conformation in the crystalline phase. X-ray diffraction and polarized optical microscopy suggested that the liquid crystalline mesophase has a smectic A(2) structure. The interlayer distance increases with a decrease in the anion size since the smaller anion has a stronger coulombic interaction with the imidazolium headgroup, resulting in the decrease of the interdigitated part to give a larger layer spacing.

Optics of short-pitch deformed-helix ferroelectric liquid crystals: Symmetries, exceptional points, and polarization-resolved angular patterns

NASA Astrophysics Data System (ADS)

Kiselev, Alexei D.; Chigrinov, Vladimir G.

2014-10-01

In order to explore electric-field-induced transformations of polarization singularities in the polarization-resolved angular (conoscopic) patterns emerging after deformed-helix ferroelectric liquid crystal (DHFLC) cells with subwavelength helix pitch, we combine the transfer matrix formalism with the results for the effective dielectric tensor of biaxial FLCs evaluated using an improved technique of averaging over distorted helical structures. Within the framework of the transfer matrix method, we deduce a number of symmetry relations and show that the symmetry axis of L lines (curves of linear polarization) is directed along the major in-plane optical axis which rotates under the action of the electric field. When the angle between this axis and the polarization plane of incident linearly polarized light is above its critical value, the C points (points of circular polarization) appear in the form of symmetrically arranged chains of densely packed star-monstar pairs. We also emphasize the role of phase singularities of a different kind and discuss the enhanced electro-optic response of DHFLCs near the exceptional point where the condition of zero-field isotropy is fulfilled.

Growth and characterization of Methyl 2-amino-5-bromobenzoate crystal for NLO applications

NASA Astrophysics Data System (ADS)

Parthasarathy, M.; Gopalakrishnan, R.

2012-11-01

Good quality single crystal of organic Methyl 2-amino-5-bromobenzoate (M2A5B) was grown using slow evaporation solution growth technique. The grown crystal was confirmed by single crystal X-ray diffraction. The functional groups and vibrational frequencies were identified using FT-IR and FT-Raman spectral analyses. The presence of hydrogen and carbon atoms in the grown sample was confirmed with proton and carbon NMR spectral studies. The optical energy band gap of the title compound is found to be 2.7 eV from the optical transmission spectra. The refractive indices nx, ny, and nz were found to be 1.569, 1.587 and 1.600, respectively using Brewster's angle method. The melting point of the material obtained with melting point apparatus is 74 °C. Thermal stability of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The mechanical behaviour of the grown crystal was analyzed with Vicker's microhardness tester. The particle size dependent second harmonic generation efficiency for M2A5B was evaluated by Kurtz-Perry powder method using Nd:YAG laser, which established the existence of phase matching.

Synthesis of Ga 2O 3 chains with closely spaced knots connected by nanowires

NASA Astrophysics Data System (ADS)

Dai, L.; You, L. P.; Duan, X. F.; Lian, W. C.; Qin, G. G.

2004-07-01

Chains of closely spaced metal or semiconductor particles have potential applications in optoelectronics and single electron devices. We report, for the first time, the synthesis of Ga 2O 3 chains with closely spaced knots connected by nanowires using the thermal evaporation method with a specially designed quartz boat. The Ga 2O 3 chains grew only on the Si substrates where Au catalyst or Ga droplets were coated. The average diameter of the knots is about 450 nm and that of the nanowires is about 50 nm. The selected area electron diffraction of either a knot or a connecting nanowire includes two sets of overlapped single crystal electron diffraction patterns which belong to the [1 0 2] and [1 0 1¯] crystal zone axes of the monoclinic β-Ga 2O 3 phase, respectively. The knot and its neighbor nanowire have the common ( 2¯ 0 1) growth planes at their interface. A mechanism model for the Ga 2O 3 chains synthesis based on the vapor-liquid-solid mechanism is discussed.

Synchrotron X-ray reciprocal-space mapping, topography and diffraction resolution studies of macromolecular crystal quality.

PubMed

Boggon, T J; Helliwell, J R; Judge, R A; Olczak, A; Siddons, D P; Snell, E H; Stojanoff, V

2000-07-01

A comprehensive study of microgravity and ground-grown chicken egg-white lysozyme crystals is presented using synchrotron X-ray reciprocal-space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed reduced intrinsic mosaicities on average, but no differences in terms of strain over their ground-grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the ground-control case only a small volume of the crystal contributed to the intensity at the diffraction peak. The techniques prove to be highly complementary, with the reciprocal-space mapping providing a quantitative measure of the crystal mosaicity and strain (or variation in lattice spacing) and the topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out at the synchrotron.

Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin

PubMed Central

Jaimohan, S. M.; Naresh, M. D.; Arumugam, V.; Mandal, A. B.

2009-01-01

Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemo­globins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 Å resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 Å, β = 109.35°. Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit. PMID:19851014

Purification, crystallization and preliminary X-ray diffraction studies of parakeet (Psittacula krameri) haemoglobin.

PubMed

Jaimohan, S M; Naresh, M D; Arumugam, V; Mandal, A B

2009-10-01

Birds often show efficient oxygen management in order to meet the special demands of their metabolism. However, the structural studies of avian haemoglobins (Hbs) are inadequate for complete understanding of the mechanism involved. Towards this end, purification, crystallization and preliminary X-ray diffraction studies have been carried out for parakeet Hb. Parakeet Hb was crystallized as the met form in low-salt buffered conditions after extracting haemoglobin from crude blood by microcentrifugation and purifying the sample by column chromatography. Good-quality crystals were grown from 10% PEG 3350 and a crystal diffracted to about 2.8 A resolution. Preliminary diffraction data showed that the Hb crystal belonged to the monoclinic system (space group C2), with unit-cell parameters a = 110.68, b = 64.27, c = 56.40 A, beta = 109.35 degrees . Matthews volume analysis indicated that the crystals contained a half-tetramer in the asymmetric unit.

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

NASA Technical Reports Server (NTRS)

Boggon, T. J.; Helliwell, J. R.; Judge, Russell A.; Siddons, D. P.; Snell, Edward H.; Stojanoff, V.

2000-01-01

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Elucidations on the Reciprocal Lattice and the Ewald Sphere

ERIC Educational Resources Information Center

Foadi, J.; Evans, G.

2008-01-01

The reciprocal lattice is derived through the Fourier transform of a generic crystal lattice, as done previously in the literature. A few key derivations are this time handled in detail, and the connection with x-ray diffraction is clearly pointed out. The Ewald sphere is subsequently thoroughly explained and a few comments on its representation…

Synthesis and Crystal Structure Study of 2’-Se-Adenosine-Derivatized DNA

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

Sheng, J.; Salon, J; Gan, J

2010-01-01

The selenium derivatization of nucleic acids is a novel and promising strategy for 3D structure determination of nucleic acids. Selenium can serve as an excellent anomalous scattering center to solve the phase problem, which is one of the two major bottlenecks in macromolecule X-ray crystallography. The other major bottleneck is crystallization. It has been demonstrated that the incorporated selenium functionality at the 2'-positions of the nucleosides and nucleotides is stable and does not cause significant structure perturbation. Furthermore, it was observed that the 2'-Se-derivatization could facilitate crystallization of oligonucleotides with fast crystal growth and high diffraction quality. Herein, we describemore » a convenient synthesis of the 2'-Se-adenosine phosphoramidite, and report the first synthesis and X-ray crystal structure determination of the DNA containing the 2'-Se-A derivatization. The 3D structure of 2'-Se-A-DNA decamer [5'-GTACGCGT(2'-Se-A)C-3']{sub 2} was determined at 1.75 {angstrom} resolution, the 2'-Se-functionality points to the minor groove, and the Se-modified and native structures are virtually identical. Moreover, we have observed that the 2'-Se-A modification can greatly facilitate the crystal growth with high diffraction quality. In conjunction with the crystallization facilitation by the 2'-Se-U and 2'-Se-T, this novel observation on the 2'-Se-A functionality suggests that the 2'-Se moiety is sole responsible for the crystallization facilitation and the identity of nucleobases does not influence the crystal growth significantly.« less

Phase development in the Bi 2Sr 2CaCu 2O y system . Effects of oxygen pressure

NASA Astrophysics Data System (ADS)

List, F. A.; Hsu, H.; Cavin, O. B.; Porter, W. D.; Hubbard, C. R.; Kroeger, D. M.

1992-11-01

Studies have been undertaken using thermal analysis, in conjunction with high-temperature and room temperature X-ray diffraction, fraction, to elucidate phase relationships during thermal processing of thick films of initially phase pure Bi 2Sr 2CaCu 2O y (2212) on silver substrates in various oxygen-containing atmospheres (0.001 to 100% O 2). Exothermic events on cooling at 10°C/min from a partially liquid state vary with oxygen partial pressure and can be grouped into three sets (I-III). Set I is prominent for 0.001% and 0.1% O 2 in the range of 740-775°C and is believed to be associated with the crystallization of a Cu-free ∼ Bi 5Sr 3Ca 1 oxide phase. Set II results from the crystallization of 2212; it is observed for p(O 2)≥1.0% in the temperature range 800-870°C. Set III appears for 21% and 100% O 2 in the temperature range 880-910°C, and its origin is not clear from the results of this study. Subsequent room temperature X-ray diffraction from these samples suggests that in general high oxygen partial pressures (100% O 2) tend to favor the formation of Bi 2Sr 2CuO 6 (2201), whereas low oxygen partial pressures (0.001-0.1% O 2) lead to the formation of a Cu-free, Bi-Sr-Ca oxide phase. The 2212 phase forms at this cooling rate predominantly for intermediate oxygen partial pressures (7.6-21% O 2). High-temperature X-ray diffraction during cooling (2°C/h) from the partially liquid state shows a pronounced dependence of the order of evolution of crystalline 2212 and 2201 phases on p(O 2). For an oxygen partial pressure of 1.0% the formation of 2212 precedes that of 2201, whereas for 0.01% O 2 2201 crystallizes at a higher temperature than 2212. The implications of these results pertaining to thermal processing of thick 2212 films are discussed.

Suppressed Release of Clarithromycin from Tablets by Crystalline Phase Transition of Metastable Polymorph Form I.

PubMed

Fujiki, Sadahiro; Watanabe, Narumi; Iwao, Yasunori; Noguchi, Shuji; Mizoguchi, Midori; Iwamura, Takeru; Itai, Shigeru

2015-08-01

The pharmaceutical properties of clarithromycin (CAM) tablets containing the metastable form I of crystalline CAM were investigated. Although the dissolution rate of form I was higher than that of stable form II, the release of CAM from form I tablet was delayed. Disintegration test and liquid penetration test showed that the disintegration of the tablet delayed because of the slow penetration of an external solution into form I tablet. Investigation by scanning electron microscopy revealed that the surface of form I tablet was covered with fine needle-shaped crystals following an exposure to the external solution. These crystals were identified as form IV crystals by powder X-ray diffraction. The phenomenon that CAM releases from tablet was inhibited by fine crystals spontaneously formed on the tablet surface could be applied to the design of sustained-release formulation systems with high CAM contents by minimizing the amount of functional excipients. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Microporous Cd(II) metal-organic framework as fluorescent sensor for nitroaromatic explosives at the sub-ppm level

NASA Astrophysics Data System (ADS)

Wang, Xing-Po; Han, Lu-Lu; Wang, Zhi; Guo, Ling-Yu; Sun, Di

2016-03-01

A novel Cd(II) metal-organic framework (MOF) based on a rigid biphenyltetracarboxylic acid, [Cd4(bptc)2(DMA)4(H2O)2·4DMA] (1) was successfully synthesized under the solvothermal condition and characterized by single-crystal X-ray diffraction and further consolidated by elemental analyses, powder X-ray diffraction (PXRD), infrared spectra (IR) and luminescent measurements. Single crystal X-ray diffraction analysis reveals that compound 1 is 4-connected PtS (Point symbol: {42·84}) network based on [Cd2(COO)4] secondary building units (SBUs). Its inherent porous and emissive characteristics make them to be a suitable fluorescent probe to sense small solvents and nitroaromatic explosives. Compound 1 shows obviously solvent-dependent emissive behaviors, especially for acetone with very high fluorescence quenching effect. Moreover, compound 1 displays excellent sensing of nitroaromatic explosives at sub-ppm level, giving a detection limit of 0.43 ppm and 0.37 ppm for nitrobenzene (NB) and p-nitrotoluene (PNT), respectively. This shows this Cd(II) MOF can be used as fluorescence probe for the detection of nitroaromatic explosives.

High pressure effects on U L 3 x-ray absorption in partial fluorescence yield mode and single crystal x-ray diffraction in the heavy fermion compound UCd 11

DOE PAGES

Nasreen, Farzana; Antonio, Daniel; VanGennep, Derrick; ...

2016-02-15

© 2016 IOP Publishing Ltd. We report a study of high pressure x-ray absorption (XAS) performed in the partial fluorescence yield mode (PFY) at the U L 3 edge (0-28.2 GPa) and single crystal x-ray diffraction (SXD) (0-20 GPa) on the UCd 11 heavy fermion compound at room temperature. Under compression, the PFY-XAS results show that the white line is shifted by +4.1(3) eV at the highest applied pressure of 28.2 GPa indicating delocalization of the 5f electrons. The increase in full width at half maxima and decrease in relative amplitude of the white line with respect to the edgemore » jump point towards 6d band broadening under high pressure. A bulk modulus of K 0 = 62(1) GPa and its pressure derivative, = 4.9(2) was determined from high pressure SXD results. Both the PFY-XAS and diffraction results do not show any sign of a structural phase transition in the applied pressure range.« less

Raman scattering and X-ray powder diffraction studies of hydrate layered perovskites: dirubidium aquapentafluoromanganate(III) and dipotassium aquapentafluoroferrate(III)

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

Galicka, Karolina; Slodczyk, Aneta; Ratuszna, Alicja

2004-06-08

The structural and vibrational properties of above mentioned crystals were determined using X-ray powder diffraction and Raman scattering experiments. At room temperature hydrate layered perovskites: Rb{sub 2}MnF{sub 5}{center_dot}H{sub 2}O and K{sub 2}FeF{sub 5}{center_dot}H{sub 2}O exhibit orthorhombic--Cmcm (D{sub 2h}{sup 17}) and monoclinic--C2/c (C{sub 2h}{sup 6}) symmetry. Their structure is built up of MnF{sub 6} or FeF{sub 5}{center_dot}H{sub 2}O octahedra forming trans-linked zig-zag chains or hydrogen bonded zig-zag chains along the major crystallographic direction [0 0 1], respectively. To confirm crystal structures and to describe lattice dynamics of these compounds the vibrational normal modes (in {gamma} point of first Brillouin zone) weremore » calculated on the base of the group theory analysis and compared with the spectra obtained from Raman scattering experiments. A relatively good reliability was obtained for both X-ray powder diffraction and Raman scattering.« less

Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture.

PubMed

Padrela, Luis; de Azevedo, Edmundo Gomes; Velaga, Sitaram P

2012-08-01

The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product. The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods. Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550 mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0-100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG). The IND-SAC cocrystal calibration curve showed excellent linearity (R(2) = 0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R(2) = 0.9981). The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method. The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.

Crystal structure of tin(IV) chloride octa­hydrate

PubMed Central

Hennings, Erik; Schmidt, Horst; Voigt, Wolfgang

2014-01-01

The title compound, [SnCl4(H2O)2]·6H2O, was crystallized according to the solid–liquid phase diagram at lower temperatures. It is built-up of SnCl4(H2O)2 octa­hedral units (point group symmetry 2) and lattice water mol­ecules. An intricate three-dimensional network of O—H⋯O and O—H⋯Cl hydrogen bonds between the complex molecules and the lattice water molecules is formed in the crystal structure. PMID:25552971

New solid state forms of antineoplastic 5-fluorouracil with anthelmintic piperazine

NASA Astrophysics Data System (ADS)

Moisescu-Goia, C.; Muresan-Pop, M.; Simon, V.

2017-12-01

The aim of the present study was to asses the formation of solid forms between the 5-fluorouracil chemotherapy drug and the anthelmintic piperazine. Two new solid forms of antineoplastic agent 5-fluorouracil with anthelmintic piperazine were obtained by liquid assisted ball milling and slurry crystallization methods. The Nsbnd H hydrogen bonding donors and C = O hydrogen bonding acceptors of 5-fluorouracil allow to form co-crystals with other drugs delivering improved properties for medical applications, as proved for other compounds of pharmaceutical interest. Both new solid forms were investigated using X-ray powder diffraction (XRD), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) spectroscopy. The XRD results show that by both methods were successfully synthesized new solid forms of 5-fluorouracil with piperazine. According to FTIR results the form prepared by lichid assisted grinding process was obtained as co-crystal and the other one, prepared by slurry method, resulted as a salt.

Crystallization studies and dielectric properties of (Ba0.7Sr0.3)TiO3 in bariumaluminosilicate glass

NASA Astrophysics Data System (ADS)

Divya, P. V.; Vignesh, G.; Kumar, V.

2007-12-01

Ferroelectric glass-ceramics with a basic composition (1 - y)(Ba0.70Sr0.30)TiO3 : y(BaO : Al2O3 : 2SiO2) have been synthesized by the sol-gel method. The major crystalline phase is the perovskite. The crystallization of the ferroelectric phase in the glass matrix have been studied using differential thermal analysis and x-ray diffraction and the kinetic parameters characterizing the crystallization have been determined using an Arrhenius model. Glass contents <= 5 mol% promoted liquid phase sintering, which reduced the sintering temperature to 1250 °C. The dielectric permittivity of the glass-ceramic samples decreased and the ferroelectric-paraelectric phase transition became more diffuse with increasing glass content. The dielectric connectivity of the ferroelectric phase in the composite have also been investigated and are reported.

Reduction of glycine particle size by impinging jet crystallization.

PubMed

Tari, Tímea; Fekete, Zoltán; Szabó-Révész, Piroska; Aigner, Zoltán

2015-01-15

The parameters of crystallization processes determine the habit and particle size distribution of the products. A narrow particle size distribution and a small average particle size are crucial for the bioavailability of poorly water-soluble pharmacons. Thus, particle size reduction is often required during crystallization processes. Impinging jet crystallization is a method that results in a product with a reduced particle size due to the homogeneous and high degree of supersaturation at the impingement point. In this work, the applicability of the impinging jet technique as a new approach in crystallization was investigated for the antisolvent crystallization of glycine. A factorial design was applied to choose the relevant crystallization factors. The results were analysed by means of a statistical program. The particle size distribution of the crystallized products was investigated with a laser diffraction particle size analyser. The roundness and morphology were determined with the use of a light microscopic image analysis system and a scanning electron microscope. Polymorphism was characterized by differential scanning calorimetry and powder X-ray diffraction. Headspace gas chromatography was utilized to determine the residual solvent content. Impinging jet crystallization proved to reduce the particle size of glycine. The particle size distribution was appropriate, and the average particle size was an order of magnitude smaller (d(0.5)=8-35 μm) than that achieved with conventional crystallization (d(0.5)=82-680 μm). The polymorphic forms of the products were influenced by the solvent ratio. The quantity of residual solvent in the crystallized products was in compliance with the requirements of the International Conference on Harmonization. Copyright © 2014 Elsevier B.V. All rights reserved.

Unique isothermal crystallization behavior of novel polyphenylene sulfide/inorganic fullerene-like WS2 nanocomposites.

PubMed

Naffakh, Mohammed; Marco, Carlos; Gómez, Marián A; Jiménez, Ignacio

2008-11-27

The isothermal crystallization of polyphenylene sulfide (PPS) nanocomposites with inorganic fullerene-like tungsten disulfide nanoparticles (IF-WS2) has been studied from a thermal and morphological point of view, using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), polarized optical microscopy (POM) and time-resolved synchrotron X-ray diffraction. All the analyses revealed that the incorporation of the IF-WS2 altered significantly the crystallization behavior of PPS, in a way strongly dependent with the nanocomposite composition. The addition of IF-WS2 in 0.1 wt % proportion retarded the crystallization of PPS by increasing its fold surface free energy in a 10%. However, addition of the nanoparticles in excess of 1 wt % results in a promotion of the crystallization rate with reduction of the fold surface free energy to half the value of pure PPS.

Observing the overall rocking motion of a protein in a crystal

NASA Astrophysics Data System (ADS)

Ma, Peixiang; Xue, Yi; Coquelle, Nicolas; Haller, Jens D.; Yuwen, Tairan; Ayala, Isabel; Mikhailovskii, Oleg; Willbold, Dieter; Colletier, Jacques-Philippe; Skrynnikov, Nikolai R.; Schanda, Paul

2015-10-01

The large majority of three-dimensional structures of biological macromolecules have been determined by X-ray diffraction of crystalline samples. High-resolution structure determination crucially depends on the homogeneity of the protein crystal. Overall `rocking' motion of molecules in the crystal is expected to influence diffraction quality, and such motion may therefore affect the process of solving crystal structures. Yet, so far overall molecular motion has not directly been observed in protein crystals, and the timescale of such dynamics remains unclear. Here we use solid-state NMR, X-ray diffraction methods and μs-long molecular dynamics simulations to directly characterize the rigid-body motion of a protein in different crystal forms. For ubiquitin crystals investigated in this study we determine the range of possible correlation times of rocking motion, 0.1-100 μs. The amplitude of rocking varies from one crystal form to another and is correlated with the resolution obtainable in X-ray diffraction experiments.

Acoustic transfer of protein crystals from agarose pedestals to micromeshes for high-throughput screening

PubMed Central

Cuttitta, Christina M.; Ericson, Daniel L.; Scalia, Alexander; Roessler, Christian G.; Teplitsky, Ella; Joshi, Karan; Campos, Olven; Agarwal, Rakhi; Allaire, Marc; Orville, Allen M.; Sweet, Robert M.; Soares, Alexei S.

2015-01-01

Acoustic droplet ejection (ADE) is an emerging technology with broad applications in serial crystallography such as growing, improving and manipulating protein crystals. One application of this technology is to gently transfer crystals onto MiTeGen micromeshes with minimal solvent. Once mounted on a micromesh, each crystal can be combined with different chemicals such as crystal-improving additives or a fragment library. Acoustic crystal mounting is fast (2.33 transfers s−1) and all transfers occur in a sealed environment that is in vapor equilibrium with the mother liquor. Here, a system is presented to retain crystals near the ejection point and away from the inaccessible dead volume at the bottom of the well by placing the crystals on a concave agarose pedestal (CAP) with the same chemical composition as the crystal mother liquor. The bowl-shaped CAP is impenetrable to crystals. Consequently, gravity will gently move the crystals into the optimal location for acoustic ejection. It is demonstrated that an agarose pedestal of this type is compatible with most commercially available crystallization conditions and that protein crystals are readily transferred from the agarose pedestal onto micromeshes with no loss in diffraction quality. It is also shown that crystals can be grown directly on CAPs, which avoids the need to transfer the crystals from the hanging drop to a CAP. This technology has been used to combine thermolysin and lysozyme crystals with an assortment of anomalously scattering heavy atoms. The results point towards a fast nanolitre method for crystal mounting and high-throughput screening. PMID:25615864

Acoustic transfer of protein crystals from agarose pedestals to micromeshes for high-throughput screening

DOE PAGES

Cuttitta, Christina M.; Ericson, Daniel L.; Scalia, Alexander; ...

2014-06-01

Acoustic droplet ejection (ADE) is an emerging technology with broad applications in serial crystallography such as growing, improving and manipulating protein crystals. One application of this technology is to gently transfer crystals onto MiTeGen micromeshes with minimal solvent. Once mounted on a micromesh, each crystal can be combined with different chemicals such as crystal-improving additives or a fragment library. Acoustic crystal mounting is fast (2.33 transfers s -1) and all transfers occur in a sealed environment that is in vapor equilibrium with the mother liquor. Here, a system is presented to retain crystals near the ejection point and away frommore » the inaccessible dead volume at the bottom of the well by placing the crystals on a concave agarose pedestal (CAP) with the same chemical composition as the crystal mother liquor. The bowl-shaped CAP is impenetrable to crystals. Consequently, gravity will gently move the crystals into the optimal location for acoustic ejection. It is demonstrated that an agarose pedestal of this type is compatible with most commercially available crystallization conditions and that protein crystals are readily transferred from the agarose pedestal onto micromeshes with no loss in diffraction quality. It is also shown that crystals can be grown directly on CAPs, which avoids the need to transfer the crystals from the hanging drop to a CAP. This technology has been used to combine thermolysin and lysozyme crystals with an assortment of anomalously scattering heavy atoms. The results point towards a fast nanolitre method for crystal mounting and high-throughput screening.« less

Hemispherical Laue camera

DOEpatents

Li, James C. M.; Chu, Sungnee G.

1980-01-01

A hemispherical Laue camera comprises a crystal sample mount for positioning a sample to be analyzed at the center of sphere of a hemispherical, X-radiation sensitive film cassette, a collimator, a stationary or rotating sample mount and a set of standard spherical projection spheres. X-radiation generated from an external source is directed through the collimator to impinge onto the single crystal sample on the stationary mount. The diffracted beam is recorded on the hemispherical X-radiation sensitive film mounted inside the hemispherical film cassette in either transmission or back-reflection geometry. The distances travelled by X-radiation diffracted from the crystal to the hemispherical film are the same for all crystal planes which satisfy Bragg's Law. The recorded diffraction spots or Laue spots on the film thereby preserve both the symmetry information of the crystal structure and the relative intensities which are directly related to the relative structure factors of the crystal orientations. The diffraction pattern on the exposed film is compared with the known diffraction pattern on one of the standard spherical projection spheres for a specific crystal structure to determine the orientation of the crystal sample. By replacing the stationary sample support with a rotating sample mount, the hemispherical Laue camera can be used for crystal structure determination in a manner previously provided in conventional Debye-Scherrer cameras.

Goniometer-based femtosecond X-ray diffraction of mutant 30S ribosomal subunit crystals

DOE PAGES

Dao, E. Han; Sierra, Raymond G.; Laksmono, Hartawan; ...

2015-04-30

In this work, we collected radiation-damage-free data from a set of cryo-cooled crystals for a novel 30S ribosomal subunit mutant using goniometer-based femtosecond crystallography. Crystal quality assessment for these samples was conducted at the X-ray Pump Probe end-station of the Linac Coherent Light Source (LCLS) using recently introduced goniometer-based instrumentation. These 30S subunit crystals were genetically engineered to omit a 26-residue protein, Thx, which is present in the wild-type Thermus thermophilus 30S ribosomal subunit. We are primarily interested in elucidating the contribution of this ribosomal protein to the overall 30S subunit structure. To assess the viability of this study, femtosecondmore » X-ray diffraction patterns from these crystals were recorded at the LCLS during a protein crystal screening beam time. During our data collection, we successfully observed diffraction from these difficult-to-grow 30S ribosomal subunit crystals. Most of our crystals were found to diffract to low resolution, while one crystal diffracted to 3.2 Å resolution. These data suggest the feasibility of pursuing high-resolution data collection as well as the need to improve sample preparation and handling in order to collect a complete radiation-damage-free data set using an X-ray Free Electron Laser.« less

Phase separation and crystallization process of amorphous Fe{sub 78}B{sub 12}Si{sub 9}Ni{sub 1} alloy

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

Mukhgalin, V. V.; Lad’yanov, V. I.

2015-08-17

The influence of the melt heat treatment on the structure and crystallization process of the rapidly quenched amorphous Fe{sub 78}B{sub 12}Si{sub 9}Ni{sub 1} alloys have been investigated by means of x-ray diffraction, DSC and TEM. Amorphous phase separation has been observed in the alloys quenched after the preliminary high temperature heat treatment of the liquid alloy (heating above 1400°C). Comparative analysis of the pair distribution functions demonstrates that this phase separation accompanied by a changes in the local atomic arrangement. It has been found that crystallization process at heating is strongly dependent on the initial amorphous phase structure - homogeneousmore » or phase separated. In the last case crystallization goes through the formation of a new metastable hexagonal phase [a=12.2849(9) Ǻ, c=7.6657(8) Ǻ]. At the same time the activation energy for crystallization (Ea) reduces from 555 to 475 kJ mole{sup −1}.« less

Six-axis multi-anvil press for high-pressure, high-temperature neutron diffraction experiments

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

Sano-Furukawa, A., E-mail: sano.asami@jaea.go.jp; Hattori, T.; J-PARC Center, Japan Atomic Energy Agency, Ibaraki 319-1195

2014-11-15

We developed a six-axis multi-anvil press, ATSUHIME, for high-pressure and high-temperature in situ time-of-flight neutron powder diffraction experiments. The press has six orthogonally oriented hydraulic rams that operate individually to compress a cubic sample assembly. Experiments indicate that the press can generate pressures up to 9.3 GPa and temperatures up to 2000 K using a 6-6-type cell assembly, with available sample volume of about 50 mm{sup 3}. Using a 6-8-type cell assembly, the available conditions expand to 16 GPa and 1273 K. Because the six-axis press has no guide blocks, there is sufficient space around the sample to use themore » aperture for diffraction and place an incident slit, radial collimators, and a neutron imaging camera close to the sample. Combination of the six-axis press and the collimation devices realized high-quality diffraction pattern with no contamination from the heater or the sample container surrounding the sample. This press constitutes a new tool for using neutron diffraction to study the structures of crystals and liquids under high pressures and temperatures.« less

Dynamical effects in Bragg coherent x-ray diffraction imaging of finite crystals

NASA Astrophysics Data System (ADS)

Shabalin, A. G.; Yefanov, O. M.; Nosik, V. L.; Bushuev, V. A.; Vartanyants, I. A.

2017-08-01

We present simulations of Bragg coherent x-ray diffractive imaging (CXDI) data from finite crystals in the frame of the dynamical theory of x-ray diffraction. The developed approach is based on a numerical solution of modified Takagi-Taupin equations and can be applied for modeling of a broad range of x-ray diffraction experiments with finite three-dimensional crystals of arbitrary shape also in the presence of strain. We performed simulations for nanocrystals of a cubic and hemispherical shape of different sizes and provided a detailed analysis of artifacts in the Bragg CXDI reconstructions introduced by the dynamical diffraction. Based on our theoretical analysis we developed an analytical procedure to treat effects of refraction and absorption in the reconstruction. Our results elucidate limitations for the kinematical approach in the Bragg CXDI and suggest a natural criterion to distinguish between kinematical and dynamical cases in coherent x-ray diffraction on a finite crystal.

Supercritical Anomalies and the Widom Line for the Isostructural Phase Transition in Solids

NASA Astrophysics Data System (ADS)

Tareyeva, E. E.; Fomin, Yu. D.; Tsiok, E. N.; Ryzhov, V. N.

2018-01-01

The representation of the Widom line as a line of maximums of the correlation length and a whole set of thermodynamic response functions above the critical point were introduced to describe anomalies observed in water above the hypothetical critical point of the liquid-liquid transition. The supercritical region for the gas-liquid transition was also described later in terms of the Widom line. It is natural to assume that an analogue of the Widom line also exists in the supercritical region for the first-order isostructural transition in crystals, which ends at a critical point. We use a simple semiphenomenological model, close in spirit the van der Waals theory, to study the properties of the new Widom line. We calculate the thermodynamic response functions above the critical point of the isostructural transition and find their maximums determining the Widom line position.

Dielectric Anistropy and Elastic Constants Near the Nematic-Smectic A Transition

NASA Astrophysics Data System (ADS)

Visco, Angelo; Mahmood, Rizwan; Zapien, Donald

The present work examines the behavior of dielectric anisotropy and the elastic constants associated with the deformation of liquid crystal molecules under the influence of an AC electric field and measured by an Automatic Liquid Crystal Tester (ALCT). The systems investigated are of various concentrations of 5CB (4-Cyano-4'-pentylbiphenyl) and 8CB (4-octyl-4'-cyanobiphenyl) liquid crystal as a function of temperature. These studies are important due to the complexity of the coupling between the orientational (nematic) and positional (smectic A) order parameters that can drive this transition to be either continuous or discontinuous. Theoretically, NA transition is weakly first order due to nematic director fluctuations in semctic A phase. This is similar to the transition from normal to superconductor. Thus, there exists a triple point similar to He3/He4 mixtures. Moreover, despite more than four decades of intense work, our understanding of this complex and interesting problem remains unclear. The funding for the project was provided by Slippery Rock University (2015-2016).

Control over phase separation and nucleation using a laser-tweezing potential

NASA Astrophysics Data System (ADS)

Walton, Finlay; Wynne, Klaas

2018-05-01

Control over the nucleation of new phases is highly desirable but elusive. Even though there is a long history of crystallization engineering by varying physicochemical parameters, controlling which polymorph crystallizes or whether a molecule crystallizes or forms an amorphous precipitate is still a poorly understood practice. Although there are now numerous examples of control using laser-induced nucleation, the absence of physical understanding is preventing progress. Here we show that the proximity of a liquid-liquid critical point or the corresponding binodal line can be used by a laser-tweezing potential to induce concentration gradients. A simple theoretical model shows that the stored electromagnetic energy of the laser beam produces a free-energy potential that forces phase separation or triggers the nucleation of a new phase. Experiments in a liquid mixture using a low-power laser diode confirm the effect. Phase separation and nucleation using a laser-tweezing potential explains the physics behind non-photochemical laser-induced nucleation and suggests new ways of manipulating matter.

Melting relations in the Fe-S-Si system at high pressure and temperature: implications for the planetary core

NASA Astrophysics Data System (ADS)

Sakairi, Takanori; Ohtani, Eiji; Kamada, Seiji; Sakai, Takeshi; Sakamaki, Tatsuya; Hirao, Naohisa

2017-12-01

The phase and melting relations in the Fe-S-Si system were determined up to 60 GPa by using a double-sided laser-heated diamond anvil cell combined with X-ray diffraction. On the basis of the X-ray diffraction patterns, we confirmed that hcp/fcc Fe-Si alloys and Fe3S are stable phases under subsolidus conditions in the Fe-S-Si system. Both solidus and liquidus temperatures are significantly lower than the melting temperature of pure Fe and both increase with pressure. The slopes of the Fe-S-Si liquidus and solidus curves determined here are smaller than the adiabatic temperature gradients of the liquid cores of Mercury and Mars. Thus, crystallization of their cores started at the core-mantle boundary region.

Invited Review Article: Development of crystal lenses for energetic photons

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

Smither, Robert K.

2014-08-15

This paper follows the development of crystal diffraction lenses designed to focus energetic photons. It begins with the search for a solution to the astrophysics problem of how to detect weak astrophysics sources of gamma rays and x-rays. This led to the basic designs for a lens and to the understanding of basic limitations of lens design. The discussion of the development of crystal diffraction lenses is divided into two parts: lenses using crystals with mosaic structure, and lenses that use crystals with curved crystal planes. This second group divides into two sub-groups: (1) Curved crystals that are used tomore » increase the acceptance angle of the diffraction of a monochromatic beam and to increase the energy bandwidth of the diffraction. (2) Curved crystals used to focus gamma ray beams. The paper describes how these two types of crystals affect the design of the corresponding crystal lenses in different fields: astrophysics, medical imaging, detection of weak, distant, gamma-ray sources, etc. The designs of crystal lenses for these applications are given in enough detail to allow the reader to design a lens for his own application.« less

Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystals

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

Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D.; Wu, M.

2014-11-15

This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals thatmore » we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.« less

Enhanced magnetic hysteresis in Ni-Mn-Ga single crystal and its influence on magnetic shape memory effect

NASA Astrophysics Data System (ADS)

Heczko, O.; Drahokoupil, J.; Straka, L.

2015-05-01

Enhanced magnetic hysteresis due to boron doping in combination with magnetic shape memory effect in Ni-Mn-Ga single crystal results in new interesting functionality of magnetic shape memory (MSM) alloys such as mechanical demagnetization. In Ni50.0Mn28.5Ga21.5 single crystal, the boron doping increased magnetic coercivity from few Oe to 270 Oe while not affecting the transformation behavior and 10 M martensite structure. However, the magnetic field needed for MSM effect also increased in doped sample. The magnetic behavior is compared to undoped single crystal of similar composition. The evidence from the X-ray diffraction, magnetic domain structure, magnetization loops, and temperature evolution of the magnetic coercivity points out that the enhanced hysteresis is caused by stress-induced anisotropy.

Overcoming a hemihedral twinning problem in tetrahydrofolate-dependent O -demethylase crystals by the microseeding method

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

Harada, Ayaka; Sato, Yukari; Kamimura, Naofumi

2016-11-30

A tetrahydrofolate-dependentO-demethylase, LigM, from Sphingobiumsp. SYK-6 was crystallized by the hanging-drop vapour-diffusion method. However, the obtained P3 121 orP3 221 crystals, which diffracted to 2.5–3.3 Å resolution, were hemihedrally twinned. To overcome the twinning problem, microseeding using P3 121/P3 2 21 crystals as microseeds was performed with optimization of the reservoir conditions. As a result, another crystal form was obtained. The newly obtained crystal diffracted to 2.5–3.0 Å resolution and belonged to space group P2 12 12, with unit-cell parametersa= 102.0,b= 117.3,c = 128.1 Å. The P2 12 12 crystals diffracted to better than 2.0 Å resolution after optimizing themore » cryoconditions. Phasing using the single anomalous diffraction method was successful at 3.0 Å resolution with a Pt-derivative crystal. This experience suggested that microseeding is an effective method to overcome the twinning problem, even when twinned crystals are utilized as microseeds.« less

Thermodynamics of freezing and melting

PubMed Central

Pedersen, Ulf R.; Costigliola, Lorenzo; Bailey, Nicholas P.; Schrøder, Thomas B.; Dyre, Jeppe C.

2016-01-01

Although the freezing of liquids and melting of crystals are fundamental for many areas of the sciences, even simple properties like the temperature–pressure relation along the melting line cannot be predicted today. Here we present a theory in which properties of the coexisting crystal and liquid phases at a single thermodynamic state point provide the basis for calculating the pressure, density and entropy of fusion as functions of temperature along the melting line, as well as the variation along this line of the reduced crystalline vibrational mean-square displacement (the Lindemann ratio), and the liquid's diffusion constant and viscosity. The framework developed, which applies for the sizable class of systems characterized by hidden scale invariance, is validated by computer simulations of the standard 12-6 Lennard-Jones system. PMID:27530064

The structure of and origin of nodular chromite from the Troodos ophiolite, Cyprus, revealed using high-resolution X-ray computed tomography and electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Prichard, H. M.; Barnes, S. J.; Godel, B.; Reddy, S. M.; Vukmanovic, Z.; Halfpenny, A.; Neary, C. R.; Fisher, P. C.

2015-03-01

Nodular chromite is a characteristic feature of ophiolitic podiform chromitite and there has been much debate about how it forms. Nodular chromite from the Troodos ophiolite in Cyprus is unusual in that it contains skeletal crystals enclosed within the centres of the nodules and interstitial to them. 3D imaging and electron backscatter diffraction have shown that the skeletal crystals within the nodules are single crystals that are surrounded by a rim of polycrystalline chromite. 3D analysis reveals that the skeletal crystals are partially or completely formed cage or hopper structures elongated along the < 111 > axis. The rim is composed of a patchwork of chromite grains that are truncated on the outer edge of the rim. The skeletal crystals formed first from a magma supersaturated in chromite and silicate minerals crystallised from melt trapped between the chromite skeletal crystal blades as they grew. The formation of skeletal crystals was followed by a crystallisation event which formed a silicate-poor rim of chromite grains around the skeletal crystals. These crystals show a weak preferred orientation related to the orientation of the core skeletal crystal implying that they formed by nucleation and growth on this core, and did not form by random mechanical aggregation. Patches of equilibrium adcumulate textures within the rim attest to in situ development of such textures. The nodules were subsequently exposed to chromite undersaturated magma resulting in dissolution, recorded by truncated grain boundaries in the rim and a smooth outer surface to the nodule. None of these stages of formation require a turbulent magma. Lastly the nodules impinged on each other causing local deformation at points of contact.

Structural Study of Liquid Lithium Niobate by Neutron Diffraction Role of the Li Atom in the Clustering Near Solidification

NASA Astrophysics Data System (ADS)

Andonov, P.; Fischer, H. E.; Palleau, P.; Kimura, S.

2001-05-01

The structure of liquid LiNbO3 has been investigated by neutron diffraction using samples with different isotopic composition of lithium. The intensity scattered by these samples has been measured for momentum transfers 0.4 Å-1 T> 1500 K, which include the undercooling domain. From an analysis of the correlation functions Gij(r) of the atomic pairs Li-Li, Li-Nb, Li-O and their structural evolutions, given by Δ Gi-j (r) = Gi-j(r)1500 -Gi-j(r)1550 made with reference to the crystalline LiNbO3 ferroelectric structure, it was possible to confirm a local ordering similar to that of the crystal. The presence of clusters (groupings of NbO3 octahedra) is confirmed. Both regular and irregular N b06 octahedra are observed in the liquid near solidification. With its high mobil­ity in the melt, the Li atom plays an important role in the clustering: the Li-O and Li-Nb bonds make possible the staking of four octahedra groups into clusters of eight octahedra or more. The Li-Li bonds join these groups. The diameter of the clusters is a least 22 Å in the undercooling regime.

Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

PubMed

Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

2004-03-01

In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

Surface-treated self-standing curved crystals as high-efficiency elements for X- and γ-ray optics: theory and experiment.

PubMed

Bonnini, Elisa; Buffagni, Elisa; Zappettini, Andrea; Doyle, Stephen; Ferrari, Claudio

2015-06-01

The efficiency of a Laue lens for X- and γ-ray focusing in the energy range 60-600 keV is closely linked to the diffraction efficiency of the single crystals composing the lens. A powerful focusing system is crucial for applications like medical imaging and X-ray astronomy where wide beams must be focused. Mosaic crystals with a high density, such as Cu or Au, and bent crystals with curved diffracting planes (CDPs) are considered for the realization of a focusing system for γ-rays, owing to their high diffraction efficiency in a predetermined angular range. In this work, a comparison of the efficiency of CDP crystals and Cu and Au mosaic crystals was performed on the basis of the theory of X-ray diffraction. Si, GaAs and Ge CDP crystals with optimized thicknesses and moderate radii of curvature of several tens of metres demonstrate comparable or superior performance with respect to the higher atomic number mosaic crystals generally used. In order to increase the efficiency of the lens further, a stack of several CDP crystals is proposed as an optical element. CDP crystals were obtained by a surface-damage method, and a stack of two surface-damaged bent Si crystals was prepared and tested. Rocking curves of the stack were performed with synchrotron radiation at 19 keV to check the lattice alignment: they exhibited only one diffraction peak.