Workman-Reynolds freezing potential measurements between ice and dilute salt solutions for single ice crystal faces.

PubMed

Wilson, P W; Haymet, A D J

2008-09-18

Workman-Reynolds freezing potentials have been measured for the first time across the interface between single crystals of ice 1h and dilute electrolyte solutions. The measured electric potential is a strictly nonequilibrium phenomenon and a function of the concentration of salt, freezing rate, orientation of the ice crystal, and time. When all these factors are controlled, the voltage is reproducible to the extent expected with ice growth experiments. Zero voltage is obtained with no growth or melting. For rapidly grown ice 1h basal plane in contact with a solution of 10 (-4) M NaCl the maximum voltage exceeds 30 V and decreases to zero at both high and low salt concentrations. These single-crystal experiments explain much of the data captured on this remarkable phenomenon since 1948.

High Pressure Single Crystal Diffraction at PX 2

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

Zhang, Dongzhou; Dera, Przemyslaw K.; Eng, Peter J.

2017-01-01

In this report, we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell at the GSECARS 13-BM-C beamline at the Advanced Photon Source. ATREX and RSV programs are used to analyze the data.

Inelastic neutron scattering experiments with the monochromatic imaging mode of the RITA-II spectrometer

NASA Astrophysics Data System (ADS)

Bahl, C. R. H.; Lefmann, K.; Abrahamsen, A. B.; Rønnow, H. M.; Saxild, F.; Jensen, T. B. S.; Udby, L.; Andersen, N. H.; Christensen, N. B.; Jakobsen, H. S.; Larsen, T.; Häfliger, P. S.; Streule, S.; Niedermayer, Ch.

2006-05-01

Recently a monochromatic multiple data taking mode has been demonstrated for diffraction experiments using a RITA type cold neutron spectrometer with a multi-bladed analyser and a position-sensitive detector. Here, we show how this mode can be used in combination with a flexible radial collimator to perform real inelastic neutron scattering experiments. We present the results from inelastic powder, single crystal dispersion and single crystal constant energy mapping experiments. The advantages and complications of performing these experiments are discussed along with a comparison between the imaging mode and the traditional monochromatic focussing mode.

Shock Hugoniot of single crystal copper

NASA Astrophysics Data System (ADS)

Chau, R.; Stölken, J.; Asoka-Kumar, P.; Kumar, M.; Holmes, N. C.

2010-01-01

The shock Hugoniot of single crystal copper is reported for stresses below 66 GPa. Symmetric impact experiments were used to measure the Hugoniots of three different crystal orientations of copper, [100], [110], and [111]. The photonic doppler velocimetry (PDV) diagnostic was adapted into a very high precision time of arrival detector for these experiments. The measured Hugoniots along all three crystal directions were nearly identical to the experimental Hugoniot for polycrystalline Cu. The predicted orientation dependence of the Hugoniot from molecular dynamics calculations was not observed. At the lowest stresses, the sound speed in Cu was extracted from the PDV data. The measured sound speeds are in agreement with values calculated from the elastic constants for Cu.

Modeling Nonlinear Elastic-plastic Behavior of RDX Single Crystals During Indentation

DTIC Science & Technology

2012-01-01

single crystals has also been probed using shock experiments (6, 12) and molecular dynamics simulations (12–14). RDX undergoes a polymorphic phase...Patterson, J.; Dreger, Z.; Gupta, Y. Shock-wave Induced Phase Transition in RDX Single Crystals. J. Phys. Chem. B 2007, 111, 10897–10904. 17. Bedrov, D...and Volume Compression of β - HMX and RDX . In Proc. Int. Symp. High Dynamic Pressures; Commissariat a l’Energie Atomique: Paris, 1978; pp 3–8. 24

Electrically driven quantum light emission in electromechanically tuneable photonic crystal cavities

NASA Astrophysics Data System (ADS)

Petruzzella, M.; Pagliano, F. M.; Zobenica, Ž.; Birindelli, S.; Cotrufo, M.; van Otten, F. W. M.; van der Heijden, R. W.; Fiore, A.

2017-12-01

A single quantum dot deterministically coupled to a photonic crystal environment constitutes an indispensable elementary unit to both generate and manipulate single-photons in next-generation quantum photonic circuits. To date, the scaling of the number of these quantum nodes on a fully integrated chip has been prevented by the use of optical pumping strategies that require a bulky off-chip laser along with the lack of methods to control the energies of nano-cavities and emitters. Here, we concurrently overcome these limitations by demonstrating electrical injection of single excitonic lines within a nano-electro-mechanically tuneable photonic crystal cavity. When an electrically driven dot line is brought into resonance with a photonic crystal mode, its emission rate is enhanced. Anti-bunching experiments reveal the quantum nature of these on-demand sources emitting in the telecom range. These results represent an important step forward in the realization of integrated quantum optics experiments featuring multiple electrically triggered Purcell-enhanced single-photon sources embedded in a reconfigurable semiconductor architecture.

Anisotropic constitutive modeling for nickel base single crystal superalloys using a crystallographic approach

NASA Technical Reports Server (NTRS)

Stouffer, D. C.; Sheh, M. Y.

1988-01-01

A micromechanical model based on crystallographic slip theory was formulated for nickel-base single crystal superalloys. The current equations include both drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments have been conducted to evaluate the effect of back stress in single crystals. The results showed that (1) the back stress is orientation dependent; and (2) the back stress state variable in the inelastic flow equation is necessary for predicting anelastic behavior of the material. The model also demonstrated improved fatigue predictive capability. Model predictions and experimental data are presented for single crystal superalloy Rene N4 at 982 C.

Thermal, mechanical, optical and conductivity studies of a novel NLO active L-phenylalanine L-phenylalaninium dihydrogenphosphate single crystal

NASA Astrophysics Data System (ADS)

Sujatha, T.; Cyrac Peter, A.; Vimalan, M.; Merline Shyla, J.; Madhavan, J.

2010-08-01

An efficient, novel, semi-organic, nonlinear optical (NLO) material L-phenylalanine L-phenylalaninium dihydrogenphosphate (LPADHP), single crystal of dimension 11×5×2 mm 3, has been grown by the slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to monoclinic system with the space group P2 1. The functional groups present in the crystal were confirmed by the Fourier transform infrared technique. Optical absorption spectrum shows that the material possesses very low absorption in the entire visible region. Thermal analysis confirmed that the crystal is thermally stable up to 161 °C. The frequency dependent dielectric properties of the grown crystal were studied for various temperatures. The second harmonic generation (SHG) efficiency of the grown crystal is 1.2 times greater than that of the potassium dihydrogenphosphate (KDP) single crystal. The laser induced surface damage threshold for the grown crystal was found to be 6.3 GW cm -2 with Nd:YAG laser assembly AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

Single-drop optimization of protein crystallization.

PubMed

Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

2012-08-01

A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline.

X-ray spectrometer based on a bent diamond crystal for high repetition rate free-electron laser applications

DOE PAGES

Boesenberg, Ulrike; Samoylova, Liubov; Roth, Thomas; ...

2017-02-03

A precise spectral characterization of every single pulse is required in many x-ray free-electron laser (XFEL) experiments due to the fluctuating spectral content of self-amplified spontaneous emission (SASE) beams. Bent single-crystal spectrometers can provide sufficient spectral resolution to resolve the SASE spikes while also covering the full SASE bandwidth. To better withstand the high heat load induced by the 4.5 MHz repetition rate of pulses at the forthcoming European XFEL facility, a spectrometer based on single-crystal diamond has been developed. Here, we report a direct comparison of the diamond spectrometer with its Si counterpart in experiments performed at the Linacmore » Coherent Light Source.« less

Single crystals of metal solid solutions

NASA Technical Reports Server (NTRS)

Miller, J. F.; Austin, A. E.; Richard, N.; Griesenauer, N. M.; Moak, D. P.; Mehrabian, M. R.; Gelles, S. H.

1974-01-01

The following definitions were sought in the research on single crystals of metal solid solutions: (1) the influence of convection and/or gravity present during crystallization on the substructure of a metal solid solution; (2) the influence of a magnetic field applied during crystallization on the substructure of a metal solid solution; and (3) requirements for a space flight experiment to verify the results. Growth conditions for the selected silver-zinc alloy system are described, along with pertinent technical and experimental details of the project.

Introducing single-crystal scattering and optical potentials into MCNPX: Predicting neutron emission from a convoluted moderator

DOE PAGES

Gallmeier, F. X.; Iverson, E. B.; Lu, W.; ...

2016-01-08

Neutron transport simulation codes are an indispensable tool used for the design and construction of modern neutron scattering facilities and instrumentation. It has become increasingly clear that some neutron instrumentation has started to exploit physics that is not well-modelled by the existing codes. Particularly, the transport of neutrons through single crystals and across interfaces in MCNP(X), Geant4 and other codes ignores scattering from oriented crystals and refractive effects, and yet these are essential ingredients for the performance of monochromators and ultra-cold neutron transport respectively (to mention but two examples). In light of these developments, we have extended the MCNPX codemore » to include a single-crystal neutron scattering model and neutron reflection/refraction physics. Furthermore, we have also generated silicon scattering kernels for single crystals of definable orientation with respect to an incoming neutron beam. As a first test of these new tools, we have chosen to model the recently developed convoluted moderator concept, in which a moderating material is interleaved with layers of perfect crystals to provide an exit path for neutrons moderated to energies below the crystal s Bragg cut off at locations deep within the moderator. Studies of simple cylindrical convoluted moderator systems of 100 mm diameter and composed of polyethylene and single crystal silicon were performed with the upgraded MCNPX code and reproduced the magnitude of effects seen in experiments compared to homogeneous moderator systems. Applying different material properties for refraction and reflection, and by replacing the silicon in the models with voids, we show that the emission enhancements seen in recent experiments are primarily caused by the transparency of the silicon/void layers. Finally the convoluted moderator experiments described by Iverson et al. were simulated and we find satisfactory agreement between the measurement and the results of simulations performed using the tools we have developed.« less

Methodology Developed for Modeling the Fatigue Crack Growth Behavior of Single-Crystal, Nickel-Base Superalloys

NASA Technical Reports Server (NTRS)

1996-01-01

Because of their superior high-temperature properties, gas generator turbine airfoils made of single-crystal, nickel-base superalloys are fast becoming the standard equipment on today's advanced, high-performance aerospace engines. The increased temperature capabilities of these airfoils has allowed for a significant increase in the operating temperatures in turbine sections, resulting in superior propulsion performance and greater efficiencies. However, the previously developed methodologies for life-prediction models are based on experience with polycrystalline alloys and may not be applicable to single-crystal alloys under certain operating conditions. One of the main areas where behavior differences between single-crystal and polycrystalline alloys are readily apparent is subcritical fatigue crack growth (FCG). The NASA Lewis Research Center's work in this area enables accurate prediction of the subcritical fatigue crack growth behavior in single-crystal, nickel-based superalloys at elevated temperatures.

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

Scanning electron microscope study of polytetrafluoroethylene sliding on aluminum single crystals

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Buckley, D. H.

1973-01-01

Friction experiments were conducted in air with polytetrafluoroethylene (PTFE) sliding on aluminum single crystals. Mechanical scoring of the crystals with (110) and (100) orientations was observed with a single pass of the PTFE slider. No scoring was observed on the (111). The degree of scoring of the crystals is related to the hardness, with the hardest surface (111) showing no damage and the softest surface (110) showing the most severe scoring. Scoring is caused by work-hardened pieces of aluminum which, as a consequence of the adhesion between PTFE and aluminum, were pulled out of the bulk and became embedded in the PTFE polymer.

Isothermal dendritic growth: A low gravity experiment

NASA Technical Reports Server (NTRS)

Glicksman, M. E.; Hahn, R. C.; Lograsso, T. A.; Rubinstein, E. R.; Selleck, M. E.; Winsa, E.

1988-01-01

The Isothermal Dendritic Growth Experiment is an active crystal growth experiment designed to test dendritic growth theory at low undercoolings where convection prohibits such studies at 1 g. The experiment will be essentially autonomous, though limited in-flight interaction through a computer interface is planned. One of the key components of the apparatus will be a crystal growth chamber capable of achieving oriented single crystal dendritic growth. Recent work indicates that seeding the chamber with a crystal of the proper orientation will not, in and of itself, be sufficient to meet this requirement. Additional flight hardware and software required for the STS flight experiment are currently being developed at NASA Lewis Research Center and at Rensselaer Polytechnic Institute.

Anisotropic constitutive modeling for nickel-base single crystal superalloys. Ph.D. Thesis

NASA Technical Reports Server (NTRS)

Sheh, Michael Y.

1988-01-01

An anisotropic constitutive model was developed based on crystallographic slip theory for nickel base single crystal superalloys. The constitutive equations developed utilizes drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments were conducted to evaluate the existence of back stress in single crystal superalloy Rene N4 at 982 C. The results suggest that: (1) the back stress is orientation dependent; and (2) the back stress state variable is required for the current model to predict material anelastic recovery behavior. The model was evaluated for its predictive capability on single crystal material behavior including orientation dependent stress-strain response, tension/compression asymmetry, strain rate sensitivity, anelastic recovery behavior, cyclic hardening and softening, stress relaxation, creep and associated crystal lattice rotation. Limitation and future development needs are discussed.

Phoenito experiments: combining the strengths of commercial crystallization automation.

PubMed

Newman, Janet; Pham, Tam M; Peat, Thomas S

2008-11-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines.

Phoenito experiments: combining the strengths of commercial crystallization automation

PubMed Central

Newman, Janet; Pham, Tam M.; Peat, Thomas S.

2008-01-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines. PMID:18997323

Structural and electronic evolution of Cr[subscript 2]O[subscript 3] on compression to 55 GPa

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

Dera, Przemyslaw; Lavina, Barbara; Meng, Yue

2016-08-15

Synchrotron single-crystal x-ray diffraction experiments have been performed on corundum-type Cr{sub 2}O{sub 3} up to a pressure of 55 GPa in Ne and He pressure transmitting media. Diffraction experiments were complemented by measurements of optical absorption spectra with single crystal samples up to 60 GPa. Results of the diffraction data analysis rule out the earlier reported monoclinic distortion at 15-30 GPa, but indicate evidence of two discontinuous transitions of electronic or magnetic nature, most likely associated with a change in magnetic ordering and charge transfer. The compression mechanism established from single crystal refinements indicates much smaller distortion of the Cr{supmore » 3+} coordination environment than was previously assumed.« less

Microgravity

NASA Image and Video Library

2001-01-24

Experiments with colloidal solutions of plastic microspheres suspended in a liquid serve as models of how molecules interact and form crystals. For the Dynamics of Colloidal Disorder-Order Transition (CDOT) experiment, Paul Chaikin of Princeton University has identified effects that are attributable to Earth's gravity and demonstrated that experiments are needed in the microgravity of orbit. Space experiments have produced unexpected dendritic (snowflake-like) structures. To date, the largest hard sphere crystal grown is a 3 mm single crystal grown at the cool end of a ground sample. At least two more additional flight experiments are plarned aboard the International Space Station. This image is from a video downlink.

Results of the TTF-TCNQ and the calcium carbonate crystallization on the Long Duration Exposure Facility

NASA Technical Reports Server (NTRS)

Nielsen, Kjeld Flemming; Lind, M. David

1992-01-01

Experiment A0139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit five years with crystal growth solutions for lead sulfide, calcium carbonate, and TTF-TCNQ. Although temperature data was lost, the experimental program had been working since the valves in all containers had been opened. All four experiments produced crystals of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X ray investigations as well as conductivity measurements on long duration space grown TTF-TCNQ crystals will be presented. Comparisons will be made with our previous space solution growth experiments. The TTF-TCNQ crystals are no longer of the highest interest, so this activity has been terminated in favor of calcium carbonate and calcium phosphate crystallizations.

Properties of pure single crystals of actinide compounds

NASA Astrophysics Data System (ADS)

Vogt, O.

1989-07-01

Actinide research started with substances of poor quality and a multitude of "unexplainable" results mostly found on powder samples of doubtful quality exerted some pressure on the crystal growers. As an example we may mention the measurements on UP. Type I antiferromagnetism was found below 123 K by neutron diffraction experiments on powdered samples. At 23 K another transition becomes apparent in susceptibility measurements. The change of the magnetic moments associated with this transition remained unexplained. It was only after the discovery of multi k structures in other actinide compounds that the need was seen to perform even inelastic neutron diffraction experiments on single crystals so that finally the true nature of the transition in UP could be revealed. NpAs is another illustrative example for the fact that sometimes it takes decades to get a clear understanding for things even so simple as macroscopic magnetic properties. The main reason for the need of single crystals is certainly the anisotropy of the magnetic moment encountered in all actinide compounds. Self-heating effects may prevent research on big crystals or might call for isotopic purity of certain samples.

Growth of Si spherical crystals and the surface oxidation (M-9)

NASA Technical Reports Server (NTRS)

Nishinaga, Tatau

1993-01-01

Nearly 90 percent of semiconductor devices are produced with Si single crystals as the starting materials. For instance, the integrated circuits (IC), which are used in almost all electronic equipments such as TV, tape recorders, audio amplifiers, etc., are made after various processings of Si single crystal wafers. In these wafers, the same controlled amounts of impurities are added and the uniformities in their distributions are extremely important. Growth under microgravity makes it possible to eliminate the buoyancy-driven convection in the melt, which is one of the main origins of convections which results in non-uniformity of the impurity. Another source of convection is known as Marangoni convection which is driven on the free surface when a temperature gradient occurs. One of the merits of microgravity experimentation is that the detailed study of this convection becomes possible. Another important advantage of microgravity is that growth of crystals without a crucible is possible. This makes it possible to study melt growth without the strain which is usually introduced on the ground. Nevertheless, we should repeat and analyze many growth experiments in space to get reliable results. However, since in the FMPT, the time for the experiment is limited, we plan to carry out two kinds of very simple and basic experiments as the first step for the semiconductor growth experiment. In the first experiment, we use single crystal Si sphere as the starting material and as shown, this sphere is heated in the furnace at a slightly higher temperature than the melting point. After the melting front moves nearly half way to its center, the temperature is decreased to stop the melting and to start the growth from the seed for which we use the unmelted solid party of the sphere. The sphere is centered by quartz protuberances inside of the quartz crucible. There exists the possibility of temperature fluctuations being introduced when the molten sphere occasionally touches the protuberances. The total time needed for the melting and the growth processes is estimated to be 30 minutes. Infrared emission from the sphere is monitored in order to prevent the accidental loss of the central solid core. The schematical illustration of the second experient is shown. A single crystal, Si rod is used as the starting material. In the first stage, the rod is melted from one end to obtain a liquid sphere. In the second stage, the single crystal is grown by decreasing the temperature from the unmelted part of the rod which is used as the seed. The second experient somewhat resembles the Czochralski method used on the ground; however, in the space experiment, no crucible is employed and the temperature uniformity is much superior. In both experiments, phosphorous is doped to allow observation of the change in the shape of the liquid solid interface during crystal growth and the impurity striations, if any.

Spacelab 3 vapor crystal growth experiment

NASA Technical Reports Server (NTRS)

Schnepple, W.; Vandenberg, L.; Skinner, N.; Ortale, C.

1987-01-01

The Space Shuttle Challenger, with Spacelab 3 as its payload, was launched into orbit April 29, 1985. The mission, number 51-B, emphasized materials processing in space, although a wide variety of experiments in other disciplines were also carried onboard. One of the materials processing experiments on this flight is described, specifically the growth of single crystals of mercuric iodide by physical vapor transport.

A methodology to determine the elastic moduli of crystals by matching experimental and simulated lattice strain pole figures using discrete harmonics

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

Wielewski, Euan; Boyce, Donald E.; Park, Jun-Sang

Determining reliable single crystal material parameters for complex polycrystalline materials is a significant challenge for the materials community. In this work, a novel methodology for determining those parameters is outlined and successfully applied to the titanium alloy, Ti-6Al-4V. Utilizing the results from a lattice strain pole figure experiment conducted at the Cornell High Energy Synchrotron Source, an iterative approach is used to optimize the single crystal elastic moduli by comparing experimental and simulated lattice strain pole figures at discrete load steps during a uniaxial tensile test. Due to the large number of unique measurements taken during the experiments, comparisons weremore » made by using the discrete spherical harmonic modes of both the experimental and simulated lattice strain pole figures, allowing the complete pole figures to be used to determine the single crystal elastic moduli. (C) 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.« less

Template-directed control of crystal morphologies.

PubMed

Meldrum, Fiona C; Ludwigs, Sabine

2007-02-12

Biominerals are characterised by unique morphologies, and it is a long-term synthetic goal to reproduce these synthetically. We here apply a range of templating routes to investigate whether a fascinating category of biominerals, the single crystals with complex forms, can be produced using simple synthetic methods. Macroporous crystals with sponge-like morphologies identical to that of sea urchin skeletal plates were produced on templating with a sponge-like polymer membrane. Similarly, patterning of individual crystal faces was achieved from the micrometer to nanometer scale through crystallisation on colloidal particle monolayers and patterned polymer thin films. These experiments demonstrate the versatility of a templating approach to producing single crystals with unique morphologies.

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.

Cryogenic motion performances of a piezoelectric single crystal micromotor

NASA Astrophysics Data System (ADS)

Li, Xiaotian; Wu, Yuting; Chen, Zhijiang; Wei, Xiaoyong; Luo, Haosu; Dong, Shuxiang

2014-04-01

This study investigates the cryogenic performances of a millimeter-size piezoelectric ultrasonic linear micromotor. The piezoelectric vibrator of the micromotor is made of Pb(In1/2Nb1/2)O3 -Pb(Mg1/3Nb2/3)-PbTiO3 single crystal and operated in first-bending wobbling mode. Experiments show that the piezoelectric single crystal micromotor works effectively even at extremely low temperature of -175 °C, although its resonance peaks vary with temperature significantly. This work confirms the feasibility of cryogenic operation of the piezo-micromotor, which is meaningful for aerospace or superconducting microwave application.

Performance study of single undoped CsI crystals for the Mu2e experiment

NASA Astrophysics Data System (ADS)

Donghia, R.; Mu2e Calorimeter Group

2016-03-01

The Mu2e experiment at Fermilab aims to measure the neutrinoless muon-to-electron conversion, which is a charged-lepton flavor-violating process. The goal of the experiment is to reach a single event sensitivity of 2.5 × 10^{-17} , to set an upper limit on the muon conversion rate at 6.7 × 10^{-17} in a three-year run. For this purpose, the Mu2e detector is designed to identify electrons from muon conversion and reduce the background to a negligible level. It consists of a low-mass straw tracker and a pure CsI crystal calorimeter. In this paper, the performance of undoped CsI single crystal is reported. Crystals from many vendors have been characterized by determining their Light Yield (LY) and Longitudinal Response Uniformity (LRU), when read with a UV extended PMT, and their time resolution when coupled to a silicon photomultiplier. The crystals show a LY of ˜100 photoelectrons per MeV when wrapped with Tyvek and coupled to the PMT without optical grease. The LRU is well represented by a linear slope that is on average 0.6%/cm. Both measurements have been performed using a ^{22} Na source. The timing performance has been evaluated exploiting cosmic rays, with MPPC readout. A timing resolution lower than 400ps has been achieved (at ˜20{ MeV} , which is the energy released by a minimum ionizing particle in the crystal).

Electron Induced Conductivity of Al2O3 as Pertaining to Thermionic Integrated Circuits.

DTIC Science & Technology

1985-12-01

No.6, pp. 4450-4456, December 1983. 18. Pomerantz, M. A., Shatas, R. A. and Marshall, 3. F., "Electrical Conductivity Induced in MgO Crystals by 1.3...Experiments were conducted to measure the electron induced conductivity CEIC) of single crystal sapphire (A120 ) and poly-crystalline alumina (A1203 ). The...induced conductivity (EIC) of single crystal sapphire (A li2O-) and poly-crystalline alumina (Alzz2O. The EIC is generated when the samples are bombarded

Mounting a thermocouple of type E onto a Cu single crystal for use in a magnetically sensitive environment below 77 K

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

Potzuweit, Alexander; Schaffner, Anuschka; Jänsch, Heinz Julius, E-mail: heinz.jaensch@physik.uni-marburg.de

2014-09-01

Type E thermocouples show magnetic effects at liquid nitrogen temperature and below. This may cause trouble in experiments that are sensitive to magnetic stray fields like nuclear magnetic resonance, photoemission or high resolution electron energy loss spectroscopy. Here, a solution for the temperature measurement of a single crystal is presented. The authors weld a copper rod onto the back side of the single crystal, thereby relocating the sensitive sample from the thermocouple attachment position. They show that it is possible to measure the crystal temperature at the end of the rod while significantly reducing the ferromagnetic influence due to themore » increased distance.« less

Results of the TTF-TCNQ- and the calcium carbonate-crystallization on the Long Duration Exposure Facility

NASA Technical Reports Server (NTRS)

Nielsen, Kjeld Flemming; Lind, M. David

1991-01-01

Experiment AO139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit for five years with crystal growth solutions for lead sulfide, calcium carbonate, and tetra thiafulvalene- tetra cyanoquino methane (TTF-TCNQ). The LDEF was in excellent condition after the long orbital stay, and although the temperature data was lost, the experiment program had been working since the valves in all containers were opened. All four experiments produced crystals; however, they were of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X-ray investigations as well as conductivity measurements on the long duration space grown TTF-TCNQ crystals are presented, and pictures of the calcium carbonate are shown. Comparisons are made with previous space solution growth experiments on the European Spacelab Mission and the Apollo-Soyuz Test Project.

Synthesis, high-resolution NMR spectroscopic analysis, and single-crystal X-ray diffraction of isoxazoline tetracycles.

PubMed

Fascio, Mirta L; Alvarez-Larena, Angel; D'Accorso, Norma B

2002-11-29

Three isoxazoline tetracycles were obtained enantiomerically pure by intramolecular 1,3-dipolar cycloaddition. The characterization of the new compounds was performed by high-resolution 1H and 13C NMR spectroscopy. The relative configuration of the new chiral centers was determined by NOESY experiments and confirmed by single-crystal X-ray structural analysis.

A new sample environment for cryogenic nuclear resonance scattering experiments on single crystals and microsamples at P01, PETRA III

NASA Astrophysics Data System (ADS)

Rackwitz, Sergej; Faus, Isabelle; Schmitz, Markus; Kelm, Harald; Krüger, Hans-Jörg; Andersson, K. Kristoffer; Hersleth, Hans-Petter; Achterhold, Klaus; Schlage, Kai; Wille, Hans-Christian; Schünemann, Volker; Wolny, Juliusz A.

2014-04-01

In order to carry out orientation dependent nuclear resonance scattering (NRS) experiments on small single crystals of e.g. iron proteins and/or chemical complexes but also on surfaces and other micrometer-sized samples a 2-circle goniometer including sample positioning optics has been installed at beamline P01, PETRA III, DESY, Hamburg. This sample environment is now available for all users of this beamline. Sample cooling is performed with a cryogenic gas stream which allows NRS measurements in the temperature range from 80 up to 400 K. In a first test this new sample environment has been used in order to investigate the orientation dependence of the nuclear inelastic scattering (NIS) signature of (i) a dinuclear iron(II) spin crossover (SCO) system and (ii) a hydrogen peroxide treated metmyoglobin single crystal.

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Helliwell, John R.; Snell, Edward H.; Chayen, Naomi E.; Judge, Russell A.; Boggon, Titus J.; Pusey, M. L.; Rose, M. Franklin (Technical Monitor)

2000-01-01

The first protein crystallization experiment in microgravity was launched in April, 1981 and used Germany's Technologische Experimente unter Schwerelosigkeit (TEXUS 3) sounding rocket. The protein P-galactosidase (molecular weight 465Kda) was chosen as the sample with a liquid-liquid diffusion growth method. A sliding device brought the protein, buffer and salt solution into contact when microgravity was reached. The sounding rocket gave six minutes of microgravity time with a cine camera and schlieren optics used to monitor the experiment, a single growth cell. In microgravity a strictly laminar diffusion process was observed in contrast to the turbulent convection seen on the ground. Several single crystals, approx 100micron in length, were formed in the flight which were of inferior but of comparable visual quality to those grown on the ground over several days. A second experiment using the same protocol but with solutions cooled to -8C (kept liquid with glycerol antifreeze) again showed laminar diffusion. The science of macromolecular structural crystallography involves crystallization of the macromolecule followed by use of the crystal for X-ray diffraction experiments to determine the three dimensional structure of the macromolecule. Neutron protein crystallography is employed for elucidation of H/D exchange and for improved definition of the bound solvent (D20). The structural information enables an understanding of how the molecule functions with important potential for rational drug design, improved efficiency of industrial enzymes and agricultural chemical development. The removal of turbulent convection and sedimentation in microgravity, and the assumption that higher quality crystals will be produced, has given rise to the growing number of crystallization experiments now flown. Many experiments can be flown in a small volume with simple, largely automated, equipment - an ideal combination for a microgravity experiment. The term "protein crystal growth" is often historically used to describe these microgravity experiments. This is somewhat inaccurate as the field involves the study of many varied biological molecules including viruses, proteins, DNA, RNA and complexes of those structures. For this reason we use the term macromolecular crystal growth. In this chapter we review a series of diagnostic microgravity crystal growth experiments carried out principally using the European Space Agency (ESA) Advanced Protein Crystallization Facility (APCF). We also review related research, both experimental and theoretical, on the aspects of microgravity fluid physics that affect microgravity protein crystal growth. Our experiments have revealed some surprises that were not initially expected. We discuss them here in the context of practical lessons learnt and how to maximize the limited microgravity opportunities available.

Neutron and X-ray investigations of the Jahn–Teller switch in partially deuterated ammonium copper Tutton salt, (NH 4 ) 2 [Cu(H 2 O) 6 ](SO 4 ) 2

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

Jørgensen, Mads R. V.; Piccoli, Paula M. B.; Hathwar, Venkatesha R.

2017-01-31

The structural phase transition accompanied by a Jahn–Teller switch has been studied over a range of H/D ratios in (NH 4) 2[Cu(H 2O) 6](SO 4) 2(ACTS). In particular, single-crystal neutron diffraction investigations of crystals with deuteration in the range 50 to 82% are shown to be consistent with previous electron paramagnetic resonance (EPR) experiments exhibiting a phase boundary at 50% deuteration under ambient pressure. Polycrystalline samples show that the two phases can co-exist. In addition, single-crystal neutron and polycrystalline X-ray diffraction pressure experiments show a shift to lower pressure at 60% deuterationversusprevious measurements at 100% deuteration.

Mesoscale martensitic transformation in single crystals of topological defects

PubMed Central

Martínez-González, José A.; Ramírez-Hernández, Abelardo; Zhou, Ye; Sadati, Monirosadat; Zhang, Rui; Nealey, Paul F.; de Pablo, Juan J.

2017-01-01

Liquid-crystal blue phases (BPs) are highly ordered at two levels. Molecules exhibit orientational order at nanometer length scales, while chirality leads to ordered arrays of double-twisted cylinders over micrometer scales. Past studies of polycrystalline BPs were challenged by the existence of grain boundaries between randomly oriented crystalline nanodomains. Here, the nucleation of BPs is controlled with precision by relying on chemically nanopatterned surfaces, leading to macroscopic single-crystal BP specimens where the dynamics of mesocrystal formation can be directly observed. Theory and experiments show that transitions between two BPs having a different network structure proceed through local reorganization of the crystalline array, without diffusion of the double-twisted cylinders. In solid crystals, martensitic transformations between crystal structures involve the concerted motion of a few atoms, without diffusion. The transformation between BPs, where crystal features arise in the submicron regime, is found to be martensitic in nature when one considers the collective behavior of the double-twist cylinders. Single-crystal BPs are shown to offer fertile grounds for the study of directed crystal nucleation and the controlled growth of soft matter. PMID:28874557

Protein Crystal Growth (PCG) experiment aboard mission STS-66

NASA Technical Reports Server (NTRS)

2000-01-01

On the Space Shuttle Orbiter Atlantis' middeck, Astronaut Joseph R. Tarner, mission specialist, works at an area amidst several lockers which support the Protein Crystal Growth (PCG) experiment during the STS-66 mission. This particular section is called the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES). Together with the Vapor Diffusion Apparatus (VDA), housed in Single Locker Thermal Enclosure (SLTES), the COS/TES represents the continuing research into the structure of proteins and other macromolecules such as viruses.

Tunable bandgap in hybrid perovskite CH{sub 3}NH{sub 3}Pb(Br{sub 3−y}X{sub y}) single crystals and photodetector applications

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

Wang, L.; Duan, R. F.; Huang, F.

We report the synthesis of CH{sub 3}NH{sub 3}Pb(Br{sub 3−y}X{sub y}) (X=Cl and I) single crystals via a stepwise temperature control approach. High-quality CH{sub 3}NH{sub 3}Pb(Br{sub 3−y}X{sub y}) crystals with a tunable bandgap from 1.92 eV to 2.53 eV have been prepared successfully in this way. And further experiments revealed the influence of halogen content and preparation temperature on the structural and optical properties of these crystals. It is observed that chlorine can lower the critical nucleation energy, which results in crystallizing at lower temperature with the chlorine content increasing, while the nucleation energy increases slowly with increasing iodine content. Moreover,more » in contrast to Frank–van der Merwe growth with low heating rate, high heating rate leads to a mass of small size single crystals and Stranski-Krastanov growth. The single crystals with tunable band gap and impressive characteristics enable us to fabricate high performance photodetectors for different wavelengths.« less

Valence-band and core-level photoemission study of single-crystal Bi2CaSr2Cu2O8 superconductors

NASA Astrophysics Data System (ADS)

Shen, Z.-X.; Lindberg, P. A. P.; Wells, B. O.; Mitzi, D. B.; Lindau, I.; Spicer, W. E.; Kapitulnik, A.

1988-12-01

High-quality single crystals of Bi2CaSr2Cu2O8 superconductors have been prepared and cleaved in ultrahigh vacuum. Low-energy electron diffraction measurements show that the surface structure is consistent with the bulk crystal structure. Ultraviolet photoemission and x-ray photoemission experiments were performed on these well-characterized sample surfaces. The valence-band and the core-level spectra obtained from the single-crystal surfaces are in agreement with spectra recorded from polycrystalline samples, justifying earlier results from polycrystalline samples. Cu satellites are observed both in the valence band and Cu 2p core level, signaling the strong correlation among the Cu 3d electrons. The O 1s core-level data exhibit a sharp, single peak at 529-eV binding energy without any clear satellite structures.

Electro-optic Modulation in Single-crystal Film of DAST Measured at 1.55 microns

NASA Astrophysics Data System (ADS)

Titus, Jitto; Swamy, Rajendra; Govindan Kutty, Srivatsa; Khatavkar, Sanchit; Thakur, Mrinal

2003-03-01

Exceptionally large electro-optic coefficient and high-speed modulation at 750 nm in DAST single-crystal film has been recently reported.[1] In this presentation, our measurement of electro-optic modulation in DAST single-crystal film at 1.55 microns will be discussed. The single-crystal film was prepared by the modified shear method. The modulation measurement was performed in the transverse configuration using the field-induced birefringence method. A semiconductor laser was used for this experiment. The light beam was propagated perpendicular to the film and the modulation was recorded for an ac field applied along the dipole axis on the film. About 6.5at a low field leading to a magnitude of the electro-optic coefficient (r11) of about 200 pm/V at 1.55 microns. 1. M. Thakur, A. Mishra, J. Titus and A.C. Ahyi, APL, 81 3738 (2002).

Thermal, optical, mechanical and electrical properties of a novel NLO active L-phenylalanine L-phenylalaninium perchlorate single crystals

NASA Astrophysics Data System (ADS)

Cyrac Peter, A.; Vimalan, M.; Sagayaraj, P.; Madhavan, J.

2010-01-01

Single crystals of L-phenylalanine L-phenylalaninium perchlorate (LPAPCl), a semiorganic nonlinear (NLO) material have been successfully grown up to a size of 14 mm×5 mm×3 mm. The lattice parameters of the grown crystals are determined by single crystal XRD. The UV-Vis-NIR spectrum of LPAPCl show less optical absorption in the entire visible region. Nonlinear optical study reveals that the SHG efficiency of LPAPCl is nearly 1.4 times that of KDP. The laser damage density is found to be 7.4 GW/cm 2. The crystals are subjected to microhardness studies and the variation of the microhardness with the applied load is studied. The response of dielectric constant in the frequency region of 50 Hz to 5 MHz has been investigated. AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

Rock-magnetic properties of single zircon crystals sampled from the Tanzawa tonalitic pluton, central Japan

NASA Astrophysics Data System (ADS)

Sato, Masahiko; Yamamoto, Shinji; Yamamoto, Yuhji; Okada, Yoshihiro; Ohno, Masao; Tsunakawa, Hideo; Maruyama, Shigenori

2015-09-01

This paper reports on the rock-magnetic properties of single zircon crystals, which are essential for future work establishing the reliable paleointensity method using single zircon crystals. Zircon crystals used in this study were sampled from the Nakagawa River, which crosses the Tanzawa tonalitic pluton in central Japan. Rock-magnetic measurements were conducted on 1037 grains of zircons, but many of these measurements are below the limits of the sensitivity of the magnetometers employed. Isothermal remanent magnetizations (IRMs) of 876 zircon crystal are below the practical resolution of this study; we infer that these crystals contain no or only minute quantities of ferromagnetic minerals. The other zircon crystals contain enough magnetic minerals to be measured in the DC SQUID magnetometer. For 81 zircon crystals, IRM intensities ( M IRM) are larger than 4 × 10-12 Am2, while natural remanent magnetization (NRM) intensities ( M NRM) are below 4 × 10-12 Am2, indicating that these crystals are inappropriate for the paleomagnetic study. For the samples that had values of M NRM ≥ 4 × 10-12 Am2 and M IRM ≥ 4 × 10-12 Am2 (80 zircons), combining the rock-magnetic parameter, we proposed the sample-selection criteria for future study of paleointensity experiments using single zircon crystals. In the case that the samples had high coercivity ( B c) values (>10 mT) or high M NRM/ M IRM values (>~0.1), main remanence carriers are probably pyrrhotite and these samples are inappropriate for the paleointensity study. In the case that the samples had low B c values (<10 mT) and low M NRM/ M IRM values (<~0.1), main remanence carriers seem to be nearly pure magnetite with pseudo-single-domain grain sizes, and these samples are expected to appropriate for the paleointensity study. Total thermoremanent magnetization (TRM) acquisition experiments were also carried out for 12 samples satisfying the above criteria. The TRM intensity was comparable with that of NRM, and a rough estimation of the paleointensity using NRM/TRM ratios shows field intensities consistent with the average geomagnetic field intensity at the Tanzawa tonalitic pluton for last 5 Myr.

Tunable and mode-locked laser action of Cr4+ in codoped forsterite Cr, Sc:Mg2SiO4

NASA Astrophysics Data System (ADS)

Sanina, V. V.; Mitrokhin, V. P.; Subbotin, K. A.; Lis, D. A.; Lis, O. N.; Ivanov, A. A.; Zharikov, E. V.

2018-01-01

The laser oscillation of tetravalent chromium and scandium codoped forsterite Cr4+,Sc:Mg2SiO4 single crystal has been demonstrated for the first time for continuous wave, tunable and mode-locked regimes. For comparison, the laser experiments have also been performed in the same configuration with the reference forsterite single crystal solely doped by chromium. The aim of scandium codoping is to inhibit the formation of parasitic trivalent chromium in the crystal. The crystal with scandium demonstrates a wider tuning range, lower lasing threshold and wider mode-locked lasing spectrum than those of the reference crystal, although the total lasing efficiency achieved by both crystals is nearly the same. The obtained results are discussed.

Structure-phase state and mechanical properties of surface layers in titanium nikelide single crystals after shock mechanical treatment

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

Surikova, N., E-mail: surikova@ispms.tsc.ru; Panin, V., E-mail: paninve@ispms.tsc.ru; Vlasov, I.

2015-10-27

The influence of ultrasonic shock surface treatment (USST) on refine structure and mechanical characteristics of surface layers and deformation behaviour of volume samples of TiNi(Fe, Mo) shape memory effect alloy single crystals is studied using optical and transmission electron microscope, X-ray diffraction, nanoindentation, mechanical attrition testing and experiments on uniaxial tension.

Structure-phase state and mechanical properties of surface layers in titanium nikelide single crystals after shock mechanical treatment

NASA Astrophysics Data System (ADS)

Surikova, N.; Panin, V.; Vlasov, I.; Narkevich, N.; Surikov, N.; Tolmachev, A.

2015-10-01

The influence of ultrasonic shock surface treatment (USST) on refine structure and mechanical characteristics of surface layers and deformation behaviour of volume samples of TiNi(Fe, Mo) shape memory effect alloy single crystals is studied using optical and transmission electron microscope, X-ray diffraction, nanoindentation, mechanical attrition testing and experiments on uniaxial tension.

Identification and Control of Gravity Related Defect Formation During Melt Growth of Electro-Optic Single Crystals Bismuth Silicate(Bi12SiO20)

NASA Technical Reports Server (NTRS)

Becia, Piotr; Wiegel, Michaela E. K.

2004-01-01

A research carried out under Award Number NAG8-1487 was aimed at to the design, conduct and analysis of experiments directed at the identification and control of gravitational effects on crystal growth, segregation and defect formation in the Sillenite system: bismuth silicate (Bi(12)SiO(20)). Correlation analyses was conducted in order to establish the influence of gravity related defects introduced during crystal growth on critical, application specific properties. Achievement of the states objective was conducted during the period from Feb. 01, 1998 to Dec. 31, 2003 with the following anticipated milestones: 1. Establishment of capabilities for (a) reproducible Czochralski and Bridgman-type growth of BSO single crystals and (b) for comprehensive analysis of crystalline and chemical defects as well as for selective property characterization of grown crystals (year 1). 2. Design and execution of critical space growth experiment(s) based on analyses of prefatory space results (experiments aimed at establishing the viability of planned approaches and procedures) and on unresolved issues related to growth, segregation and defect formation associated with conventional growth in Bridgman geometries. Comparative analysis of growth under conventional and under mu-g conditions; identification of gravity related defect formation during conventional Bridgman growth and formulation of approaches for their control (years 2 and 3). Development of charge confinement system which permits growth interface demarcation (in a mu-g environment) as well as minimization of confinement related stress and contamination during growth; design of complementary mu-g growth experiments aimed at quantitative mu-g growth and segregation analyses (year 4). 3. Conduct of quantitative mu-g growth experiments directed at: (a) identification and control of gravity related crystalline and chemical defect formation during single crystal growth of Bi(12)SiO(20) and at (b) defect engineering -the development of approaches to the controlled generation during crystal growth of specified point defects in homogeneous distribution (year 5). The proposed research places focus on a class of materials which have outstanding electrical and optical properties but have so far failed to reach their potential, primarily because of our inability to control adequately their stoichiometry and crystal defect formation as well as confinement related contamination and lattice stress.

Diamond turning of Si and Ge single crystals

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

Blake, P.; Scattergood, R.O.

Single-point diamond turning studies have been completed on Si and Ge crystals. A new process model was developed for diamond turning which is based on a critical depth of cut for plastic flow-to-brittle fracture transitions. This concept, when combined with the actual machining geometry for single-point turning, predicts that {open_quotes}ductile{close_quotes} machining is a combined action of plasticity and fracture. Interrupted cutting experiments also provide a meant to directly measure the critical depth parameter for given machining conditions.

Precipitation of thin-film organic single crystals by a novel crystal growth method using electrospray and ionic liquid film

NASA Astrophysics Data System (ADS)

Ueda, Hiroyuki; Takeuchi, Keita; Kikuchi, Akihiko

2018-04-01

We report an organic single crystal growth technique, which uses a nonvolatile liquid thin film as a crystal growth field and supplies fine droplets containing solute from the surface of the liquid thin film uniformly and continuously by electrospray deposition. Here, we investigated the relationships between the solute concentration of the supplied solution and the morphology and size of precipitated crystals for four types of fluorescent organic low molecule material [tris(8-hydroxyquinoline)aluminum (Alq3), 2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole (PBD), N,N‧-bis(3-methylphenyl)-N,N‧-diphenylbenzidine (TPD), and N,N-bis(naphthalene-1-yl)-N,N-diphenyl-benzidine (NPB)] using an ionic liquid as the nonvolatile liquid. As the concentration of the supplied solution decreased, the morphology of precipitated crystals changed from dendritic or leaf shape to platelike one. At the solution concentration of 0.1 mg/ml, relatively large platelike single crystals with a diagonal length of over 100 µm were obtained for all types of material. In the experiment using ionic liquid and dioctyl sebacate as nonvolatile liquids, it was confirmed that there is a clear positive correlation between the maximum volume of the precipitated single crystal and the solubility of solute under the same solution supply conditions.

Operation condition for continuous anti-solvent crystallization of CBZ-SAC cocrystal considering deposition risk of undesired crystals

NASA Astrophysics Data System (ADS)

Nishimaru, Momoko; Nakasa, Miku; Kudo, Shoji; Takiyama, Hiroshi

2017-07-01

Crystallization operation of cocrystal production has deposition risk of undesired crystals. Simultaneously, continuous manufacturing processes are focused on. In this study, conditions for continuous cocrystallization considering risk reduction of undesired crystals deposition were investigated on the view point of thermodynamics and kinetics. The anti-solvent cocrystallization was carried out in four-component system of carbamazepine, saccharin, methanol and water. From the preliminary batch experiment, the relationships among undesired crystal deposition, solution composition decided by mixing ratio of solutions, and residence time for the crystals were considered, and then the conditions of continuous experiment were decided. Under these conditions, the continuous experiment was carried out. The XRD patterns of obtained crystals in the continuous experiment showed that desired cocrystals were obtained without undesired crystals. This experimental result was evaluated by using multi-component phase diagrams from the view point of the operation point's movement. From the evaluation, it was found that there is a certain operation condition which the operation point is fixed with time in the specific domain without the deposition risk of undesired single component crystals. It means the possibility of continuous production of cocrystals without deposition risk of undesired crystals was confirmed by using multi-component phase diagrams.

Plagioclase nucleation and growth kinetics in a hydrous basaltic melt by decompression experiments

NASA Astrophysics Data System (ADS)

Arzilli, Fabio; Agostini, C.; Landi, P.; Fortunati, A.; Mancini, L.; Carroll, M. R.

2015-12-01

Isothermal single-step decompression experiments (at temperature of 1075 °C and pressure between 5 and 50 MPa) were used to study the crystallization kinetics of plagioclase in hydrous high-K basaltic melts as a function of pressure, effective undercooling (Δ T eff) and time. Single-step decompression causes water exsolution and a consequent increase in the plagioclase liquidus, thus imposing an effective undercooling (Δ T eff), accompanied by increased melt viscosity. Here, we show that the decompression process acts directly on viscosity and thermodynamic energy barriers (such as interfacial-free energy), controlling the nucleation process and favoring the formation of homogeneous nuclei also at high pressure (low effective undercoolings). In fact, this study shows that similar crystal number densities ( N a) can be obtained both at low and high pressure (between 5 and 50 MPa), whereas crystal growth processes are favored at low pressures (5-10 MPa). The main evidence of this study is that the crystallization of plagioclase in decompressed high-K basalts is more rapid than that in rhyolitic melts on similar timescales. The onset of the crystallization process during experiments was characterized by an initial nucleation event within the first hour of the experiment, which produced the largest amount of plagioclase. This nucleation event, at short experimental duration, can produce a dramatic change in crystal number density ( N a) and crystal fraction ( ϕ), triggering a significant textural evolution in only 1 h. In natural systems, this may affect the magma rheology and eruptive dynamics on very short time scales.

Low-stress pressure solution experiments on halite single-crystals

NASA Astrophysics Data System (ADS)

Martin, Brigitte; Röller, Klaus; Stöckhert, Bernhard

1999-07-01

Pressure solution experiments on halite single-crystals in saturated solution were carried out at atmospheric pressure under uniaxial stress ranging from 0.1 to 2.0 MPa and at temperatures of 303 and 323 K. The experiments were performed in ceramic loading rigs with damp-proofed sample chambers. The low uniaxial stress is applied by loading the piston with steel weights ranging from 0.5 to 5.0 kg. The position of the piston is measured by an electronic displacement transducer, connected to a data acquisition system. Deviations caused by fluctuations of temperature and output voltage of the power supply are corrected after data acquisition. The halite cubes {100} with edge dimensions of 3-9 mm are prepared by cleaving and placed with a (100) cleavage face on the (001) face of a muscovite single-crystal (10×10×0.1 mm), a polished quartz (0001) plate, or another halite crystal oriented to form a 45° twist boundary. The four free (100) faces of the halite cube are in contact with the surrounding NaCl solution. The initial displacement rate of the piston after flooding of the system and loading is up to 50.0 μm/day, attributed to smoothing of the halite face and elimination of point contacts with high stress concentration. Within 2 to 3 days this stage grades into steady-state displacement with rates of 0.1-2.0 μm/day. In some experiments stages of higher displacement rates (2.0-5.0 μm/day) lasting for 3-5 days are observed episodically, with intervals of 10-15 days. These cycles appear not to be triggered by external events. Experiments with a dry mica-halite interface, carried out for comparison at the same temperature and at an uniaxial stress of 2 MPa, result in a displacement rate below the limits of detection. This rules out a significant contribution of crystal plastic deformation in the wet experiments. The experimental results show no simple correlation between displacement rate and magnitude of uniaxial stress, crystal size, type of the interface, and temperature. At the given conditions, convergence at a single interface due to pressure solution is apparently not a steady-state process. The alternating stages of lower and higher displacement rates observed in many experiments suggest that the mechanisms of transport or dissolution may change spontaneously during the experiment. It is possible that the process itself leads to an unstable configuration causing episodic changes.

A crystallographic model for the tensile and fatigue response for Rene N4 at 982 C

NASA Technical Reports Server (NTRS)

Sheh, M. Y.; Stouffer, D. C.

1990-01-01

An anisotropic constitutive model based on crystallographic slip theory was formulated for nickel-base single-crystal superalloys. The current equations include both drag stress and back stress state variables to model the local inelastic flow. Specially designed experiments have been conducted to evaluate the existence of back stress in single crystals. The results showed that the back stress effect of reverse inelastic flow on the unloading stress is orientation-dependent, and a back stress state variable in the inelastic flow equation is necessary for predicting inelastic behavior. Model correlations and predictions of experimental data are presented for the single crystal superalloy Rene N4 at 982 C.

Experimental Research Into Generation of Acoustic Emission Signals in the Process of Friction of Hadfield Steel Single Crystals

NASA Astrophysics Data System (ADS)

Lychagin, D. V.; Filippov, A. V.; Novitskaia, O. S.; Kolubaev, E. A.; Sizova, O. V.

2016-08-01

The results of experimental research into dry sliding friction of Hadfield steel single crystals involving registration of acoustic emission are presented in the paper. The images of friction surfaces of Hadfield steel single crystals and wear grooves of the counterbody surface made after completion of three serial experiments conducted under similar conditions and friction regimes are given. The relation of the acoustic emission waveform envelope to the changing friction factor is revealed. Amplitude-frequency characteristics of acoustic emission signal frames are determined on the base of Fast Fourier Transform and Short Time Fourier Transform during the run-in stage of tribounits and in the process of stable friction.

Electrooptic crystal growth and properties

NASA Astrophysics Data System (ADS)

1994-02-01

A new member in the tungsten-bronze family of ferroelectric lead potassium niobate (PKN), with general formula Pb(1-x)K(2x)Nb2O6, has been grown as bulk single crystal. Growth of PKN with charge composition x = 0.23 has been achieved using the Czochralski technique of crystal pulling. Large diameter boules were grown in platinum crucibles at temperatures between 1280 and 1300 C. Crystallographic studies were conducted using x ray diffraction techniques. The samples were characterized for ferroelectric properties between 25 and 600 C and for optical absorption. This paper presents the crystal synthesis and the results of ferroelectric and optical characterization. Bulk single crystals of potassium tantalate niobate, KTa(1-x)Nb(x)O3, ferroelectric with different values of Ta/Nb ratios have been grown by temperature gradient transport technique (TGTT). A second attached paper presents the results of the crystal growth experiments, ferroelectric characterization techniques, and properties of potassium tantalate niobate crystals.

Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

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

Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil

2016-07-27

We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity andmore » spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.« less

Development of single crystal membranes

NASA Technical Reports Server (NTRS)

Stormont, R. W.; Cocks, F. H.

1972-01-01

The design and construction of a high pressure crystal growth chamber was accomplished which would allow the growth of crystals under inert gas pressures of 2 MN/sq m (300 psi). A novel crystal growth technique called EFG was used to grow tubes and rods of the hollandite compounds, BaMgTi7O16, K2MgTi7O16, and tubes of sodium beta-alumina, sodium magnesium-alumina, and potassium beta-alumina. Rods and tubes grown are characterized using metallographic and X-ray diffraction techniques. The hollandite compounds are found to be two or three-phase, composed of coarse grained orientated crystallites. Single crystal c-axis tubes of sodium beta-alumina were grown from melts containing excess sodium oxide. Additional experiments demonstrated that crystals of magnesia doped beta-alumina and potassium beta-alumina also can be achieved by this EFG technique.

One-step fabrication of porous GaN crystal membrane and its application in energy storage

NASA Astrophysics Data System (ADS)

Zhang, Lei; Wang, Shouzhi; Shao, Yongliang; Wu, Yongzhong; Sun, Changlong; Huo, Qin; Zhang, Baoguo; Hu, Haixiao; Hao, Xiaopeng

2017-03-01

Single-crystal gallium nitride (GaN) membranes have great potential for a variety of applications. However, fabrication of single-crystalline GaN membranes remains a challenge owing to its chemical inertness and mechanical hardness. This study prepares large-area, free-standing, and single-crystalline porous GaN membranes using a one-step high-temperature annealing technique for the first time. A promising separation model is proposed through a comprehensive study that combines thermodynamic theories analysis and experiments. Porous GaN crystal membrane is processed into supercapacitors, which exhibit stable cycling life, high-rate capability, and ultrahigh power density, to complete proof-of-concept demonstration of new energy storage application. Our results contribute to the study of GaN crystal membranes into a new stage related to the elelctrochemical energy storage application.

Directed self-assembly of liquid crystalline blue-phases into ideal single-crystals

NASA Astrophysics Data System (ADS)

Martínez-González, Jose A.; Li, Xiao; Sadati, Monirosadat; Zhou, Ye; Zhang, Rui; Nealey, Paul F.; de Pablo, Juan J.

2017-06-01

Chiral nematic liquid crystals are known to form blue phases--liquid states of matter that exhibit ordered cubic arrangements of topological defects. Blue-phase specimens, however, are generally polycrystalline, consisting of randomly oriented domains that limit their performance in applications. A strategy that relies on nano-patterned substrates is presented here for preparation of stable, macroscopic single-crystal blue-phase materials. Different template designs are conceived to exert control over different planes of the blue-phase lattice orientation with respect to the underlying substrate. Experiments are then used to demonstrate that it is indeed possible to create stable single-crystal blue-phase domains with the desired orientation over large regions. These results provide a potential avenue to fully exploit the electro-optical properties of blue phases, which have been hindered by the existence of grain boundaries.

The effect of tailor-made additives on crystal growth of methyl paraben: Experiments and modelling

NASA Astrophysics Data System (ADS)

Cai, Zhihui; Liu, Yong; Song, Yang; Guan, Guoqiang; Jiang, Yanbin

2017-03-01

In this study, methyl paraben (MP) was selected as the model component, and acetaminophen (APAP), p-methyl acetanilide (PMAA) and acetanilide (ACET), which share the similar molecular structure as MP, were selected as the three tailor-made additives to study the effect of tailor-made additives on the crystal growth of MP. HPLC results indicated that the MP crystals induced by the three additives contained MP only. Photographs of the single crystals prepared indicated that the morphology of the MP crystals was greatly changed by the additives, but PXRD and single crystal diffraction results illustrated that the MP crystals were the same polymorph only with different crystal habits, and no new crystal form was found compared with other references. To investigate the effect of the additives on the crystal growth, the interaction between additives and facets was discussed in detail using the DFT methods and MD simulations. The results showed that APAP, PMAA and ACET would be selectively adsorbed on the growth surfaces of the crystal facets, which induced the change in MP crystal habits.

Intrinsic Josephson junctions in mesas and ultrathin BSCCO single crystals: Ultimate control of shape and dimensions

NASA Astrophysics Data System (ADS)

Yurgens, A.; You, L. X.; Torstensson, M.; Winkler, D.

2007-09-01

We describe experiments which are only possible through an ultimate control of sample shape and dimensions down to nanometer scale whereby transport measurements can be done in various restricted geometries. We use photolithography patterning together with a flip-chip technique to isolate very thin (d ∼ 100 nm) pieces of Bi2Sr2CaCu2O8+δ (BSCCO) single crystals. Ar-ion milling allows us to further thin these crystals down to a few nanometers in a controlled way. With decreasing thickness below two to three unit cells, the superconducting transition temperature gradually decreases to zero and the in-plane resistivity increases to large values indicating the existence of a superconductor-insulator transition in these ultrathin single crystals. In a refined technique, a precise control of the etching depth from both sides of the crystal makes it possible to form stacks of intrinsic Josephson junctions (IJJs) inside the ultrathin single crystals. The stacks can be tailor-made to any microscopic height (0-9 nm < d), i.e. enclosing a specific number of IJJs (0-6). In certain geometries, by feeding current into the topmost Cu2O4-layer of a mesa on the surface of a BSCCO single crystal, we measured the critical value of this current by detecting a sharp upturn or break in the current-voltage characteristics. From this, we estimate the sheet critical current density of a single Cu2O4 plane to be ∼0.3-0.7 A/cm at 4.5 K, corresponding to a bulk current density of ∼2-5 MA/cm2. These values are among the largest ever reported for BSCCO single crystals, thin-films and tapes.

Concentration and structure inhomogeneities in GaSb(Si) single crystals grown at different heat and mass transfer conditions

NASA Astrophysics Data System (ADS)

Serebryakov, Yu. A.; Prokhorov, I. A.; Vlasov, V. N.; Korobeynikova, E. N.; Zakharov, B. G.; Shul'pina, I. L.; Marchenko, M. P.; Fryazinov, I. V.

2007-06-01

Results of ground-based experiments on crystallization of gallium antimonide on the POLIZON facility carried out within the framework of space experiment preparation aboard FOTON satellite are submitted. Technical and technological opportunities of suppression of disturbing factors for improvement of quality of grown crystals in space are substantiated. Features of formation of concentration and structure inhomogeneities in GaSb:Si crystals grown under non-stationary and stationary convection conditions are investigated. Experimental data about structure and dopant distribution inhomogeneities are discussed taking into account results of numerical researches of GaSb:Si crystallization. Also earlier received results of modeling of GaSb:Te crystallization under close temperature conditions are used. Correlation between computational and experimental data is shown. The data on intensity of flows close to crystallization front are received at which non-stationary or stationary conditions of crystallization are realized. The forecast for space conditions is made. The influence of a rotating magnetic field on convection in melt for application in space experiment projected is investigated.

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

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

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

2007-12-12

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

Shock compression experiments on Lithium Deuteride (LiD) single crystals

DOE PAGES

Knudson, M. D.; Desjarlais, M. P.; Lemke, R. W.

2016-12-21

Shock compression experiments in the few hundred GPa (multi-Mabr) regime were performed on Lithium Deuteride (LiD) single crystals. This study utilized the high velocity flyer plate capability of the Sandia Z Machine to perform impact experiments at flyer plate velocities in the range of 17-32 km/s. Measurements included pressure, density, and temperature between ~200-600 GPa along the Principal Hugoniot – the locus of end states achievable through compression by large amplitude shock waves – as well as pressure and density of re - shock states up to ~900 GPa. Lastly, the experimental measurements are compared with recent density functional theorymore » calculations as well as a new tabular equation of state developed at Los Alamos National Labs.« less

Astronaut Scott Parazynski works with PCG experiment on middeck

NASA Image and Video Library

1994-11-14

STS066-13-029 (3-14 Nov 1994) --- On the Space Shuttle Atlantis' mid-deck, astronaut Scott E. Parazynski, mission specialist, works at one of two areas onboard the Shuttle which support the Protein Crystal Growth (PCG) experiment. This particular section is called the Vapor Diffusion Apparatus (VDA), housed in a Single Locker Thermal Enclosure (STES). Together with the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES) the VDA represents the continuing research into the structures of proteins and other macromolecules such as viruses. In addition to using the microgravity of space to grow high-quality protein crystals for structural analyses, the experiments are expected to help develop technologies and methods to improve the protein crystallization process on Earth as well as in space.

Coilable single crystal fibers of doped-YAG for high power laser applications

NASA Astrophysics Data System (ADS)

Maxwell, Gisele; Soleimani, Nazila; Ponting, Bennett; Gebremichael, Eminet

2013-05-01

Single crystal fibers are an intermediate between laser crystals and doped glass fibers. They can combine the advantages of both by guiding laser light and matching the efficiencies found in bulk crystals, making them ideal candidates for high-power laser and fiber laser applications. In particular, a very interesting feature of single crystal fiber is that they can generate high power in the eye-safe range (Er:YAG) with a high efficiency, opening new possibilities for portable directed energy weapons. This work focuses on the growth of a flexible fiber with a core of dopant (Er, Nd, Yb, etc…) that will exhibit good waveguiding properties. Direct growth or a combination of growth and cladding experiments are described. We have, to date, demonstrated the growth of a flexible foot long 45 microns doped YAG fiber. Scattering loss measurements at visible wavelengths along with dopant profile characterization are also presented. Laser characterization for these fibers is in progress.

Shock and Microstructural Characterization of the α-ω Phase Transition in Titanium Crystals

NASA Astrophysics Data System (ADS)

Morrow, Benjamin M.; Rigg, Paulo A.; Jones, David R.; Addessio, Francis L.; Trujillo, Carl P.; Saavedra, Ramon A.; Martinez, Daniel T.; Cerreta, Ellen K.

2017-12-01

A multicrystal comprised of a small number of large crystals of high-purity titanium and a [0001] oriented high-purity single crystal titanium sample were shock loaded using gas gun plate impact experiments. Tests were performed at stresses above the α {-}ω phase transition stress (for high-purity polycrystalline specimens) to observe the behavior of oriented crystals under similar conditions. Post-mortem characterization of the shocked microstructure was conducted on the single crystal sample to measure textures, and quantify phases and twinning. The apparent activation of plastic and transformation mechanisms was dependent upon crystal orientation. Specifically, the [0001] crystal showed a higher Hugoniot elastic limit than the [10\\bar{1}0] or [3\\bar{1}\\bar{4}4] orientations. The slope of velocity as a function of time was lower in the [0001] orientation than the other orientations during plastic deformation, indicating sluggish transformation kinetics for the α to ω phase transition for the [0001] oriented crystal. Microtexture measurements of a recovered [0001] oriented single crystal revealed the presence of retained ω phase after unloading, with orientations of the constituent phase fractions indicative of the forward α → ω transition, rather than the reverse ω → α transition, suggesting that the material never achieved a state of 100% ω phase.

Substructure based modeling of nickel single crystals cycled at low plastic strain amplitudes

NASA Astrophysics Data System (ADS)

Zhou, Dong

In this dissertation a meso-scale, substructure-based, composite single crystal model is fully developed from the simple uniaxial model to the 3-D finite element method (FEM) model with explicit substructures and further with substructure evolution parameters, to simulate the completely reversed, strain controlled, low plastic strain amplitude cyclic deformation of nickel single crystals. Rate-dependent viscoplasticity and Armstrong-Frederick type kinematic hardening rules are applied to substructures on slip systems in the model to describe the kinematic hardening behavior of crystals. Three explicit substructure components are assumed in the composite single crystal model, namely "loop patches" and "channels" which are aligned in parallel in a "vein matrix," and persistent slip bands (PSBs) connected in series with the vein matrix. A magnetic domain rotation model is presented to describe the reverse magnetostriction of single crystal nickel. Kinematic hardening parameters are obtained by fitting responses to experimental data in the uniaxial model, and the validity of uniaxial assumption is verified in the 3-D FEM model with explicit substructures. With information gathered from experiments, all control parameters in the model including hardening parameters, volume fraction of loop patches and PSBs, and variation of Young's modulus etc. are correlated to cumulative plastic strain and/or plastic strain amplitude; and the whole cyclic deformation history of single crystal nickel at low plastic strain amplitudes is simulated in the uniaxial model. Then these parameters are implanted in the 3-D FEM model to simulate the formation of PSB bands. A resolved shear stress criterion is set to trigger the formation of PSBs, and stress perturbation in the specimen is obtained by several elements assigned with PSB material properties a priori. Displacement increment, plastic strain amplitude control and overall stress-strain monitor and output are carried out in the user subroutine DISP and URDFIL of ABAQUS, respectively, while constitutive formulations of the FEM model are coded and implemented in UMAT. The results of the simulations are compared to experiments. This model verified the validity of Winter's two-phase model and Taylor's uniform stress assumption, explored substructure evolution and "intrinsic" behavior in substructures and successfully simulated the process of PSB band formation and propagation.

High-Q/V Monolithic Diamond Microdisks Fabricated with Quasi-isotropic Etching.

PubMed

Khanaliloo, Behzad; Mitchell, Matthew; Hryciw, Aaron C; Barclay, Paul E

2015-08-12

Optical microcavities enhance light-matter interactions and are essential for many experiments in solid state quantum optics, optomechanics, and nonlinear optics. Single crystal diamond microcavities are particularly sought after for applications involving diamond quantum emitters, such as nitrogen vacancy centers, and for experiments that benefit from diamond's excellent optical and mechanical properties. Light-matter coupling rates in experiments involving microcavities typically scale with Q/V, where Q and V are the microcavity quality-factor and mode-volume, respectively. Here we demonstrate that microdisk whispering gallery mode cavities with high Q/V can be fabricated directly from bulk single crystal diamond. By using a quasi-isotropic oxygen plasma to etch along diamond crystal planes and undercut passivated diamond structures, we create monolithic diamond microdisks. Fiber taper based measurements show that these devices support TE- and TM-like optical modes with Q > 1.1 × 10(5) and V < 11(λ/n) (3) at a wavelength of 1.5 μm.

Diagnosing the Internal Architecture of Zeolite Ferrierite

PubMed Central

Schmidt, Joel E.; Hendriks, Frank C.; Lutz, Martin; Post, L. Christiaan; Fu, Donglong

2017-01-01

Abstract Large crystals of zeolite ferrierite (FER) are important model systems for spatially resolved catalysis and diffusion studies, though there is considerable variation in crystal habit depending on the chemical composition and employed synthesis conditions. A synergistic combination of techniques has been applied, including single crystal X‐ray diffraction, high‐temperature in situ confocal fluorescence microscopy, fluorescent probe molecules, wide‐field microscopy and atomic force microscopy to unravel the internal architecture of three distinct FER zeolites. Pyrolyzed template species can be used as markers for the 8‐membered ring direction as they are trapped in the terraced roof of the FER crystals. This happens as the materials grow in a layer‐by‐layer, defect‐free manner normal to the large crystal surface, and leads to a facile method to diagnose the pore system orientation, which avoids tedious single crystal X‐ray diffraction experiments. PMID:28809081

Correlation of the superconducting transition to oxygen stoichiometry in single-crystal Ba1-xKxBiO3-y

NASA Astrophysics Data System (ADS)

Mosley, W. D.; Dykes, J. W.; Klavins, P.; Shelton, R. N.; Sterne, P. A.; Howell, R. H.

1993-07-01

Temperature-dependent positron-lifetime experiments have been performed from room temperature to 15 K on single crystals of the oxide superconductor Ba1-xKxBiO3-y. Results indicate that the filling of oxygen vacancies has a marked impact on the superconducting properties of this system. Cation defect concentrations were below the detectable limit of positron-annihilation-analysis techniques in this material, which is in sharp contrast to identical studies on polycrystalline samples. We find that the positron lifetime in these electrochemically deposited single crystals is determined by the oxygen stoichiometry of the lattice, but there is no experimental signature of strong positron localization. By performing a subsequent oxygen anneal on the crystals, the superconducting transition is sharpened and the onset is raised. The observed change in positron lifetime associated with this annealing procedure is in quantitative agreement with theory.

Directed Self-Assembly of Liquid Crystalline Blue-Phases into Ideal Single-Crystals

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

Martinez-Gonzalez, Jose A.; Li, Xiao; Sadati, Monirosadat

Chiral nematic liquid crystals are known to form blue phases—liquid states of matter that exhibit ordered cubic arrangements of topological defects. Blue-phase specimens, however, are generally polycrystalline, consisting of randomly oriented domains that limit their performance in applications. A strategy that relies on nano-patterned substrates is presented here for preparation of stable, macroscopic single-crystal blue-phase materials. Different template designs are conceived to exert control over different planes of the blue-phase lattice orientation with respect to the underlying substrate. Experiments are then used to demonstrate that it is indeed possible to create stable single-crystal blue-phase domains with the desired orientation overmore » large regions. Lastly, these results provide a potential avenue to fully exploit the electro-optical properties of blue phases, which have been hindered by the existence of grain boundaries.« less

Directed Self-Assembly of Liquid Crystalline Blue-Phases into Ideal Single-Crystals

DOE PAGES

Martinez-Gonzalez, Jose A.; Li, Xiao; Sadati, Monirosadat; ...

2017-06-16

Chiral nematic liquid crystals are known to form blue phases—liquid states of matter that exhibit ordered cubic arrangements of topological defects. Blue-phase specimens, however, are generally polycrystalline, consisting of randomly oriented domains that limit their performance in applications. A strategy that relies on nano-patterned substrates is presented here for preparation of stable, macroscopic single-crystal blue-phase materials. Different template designs are conceived to exert control over different planes of the blue-phase lattice orientation with respect to the underlying substrate. Experiments are then used to demonstrate that it is indeed possible to create stable single-crystal blue-phase domains with the desired orientation overmore » large regions. Lastly, these results provide a potential avenue to fully exploit the electro-optical properties of blue phases, which have been hindered by the existence of grain boundaries.« less

Spall response of single-crystal copper

NASA Astrophysics Data System (ADS)

Turley, W. D.; Fensin, S. J.; Hixson, R. S.; Jones, D. R.; La Lone, B. M.; Stevens, G. D.; Thomas, S. A.; Veeser, L. R.

2018-02-01

We performed a series of systematic spall experiments on single-crystal copper in an effort to determine and isolate the effects of crystal orientation, peak stress, and unloading strain rate on the tensile spall strength. Strain rates ranging from 0.62 to 2.2 × 106 s-1 and peak shock stresses in the 5-14 GPa range, with one additional experiment near 50 GPa, were explored as part of this work. Gun-driven impactors, called flyer plates, generated flat top shocks followed by spall. This work highlights the effect of crystal anisotropy on the spall strength by showing that the spall strength decreases in the following order: [100], [110], and [111]. Over the range of stresses and strain rates explored, the spall strength of [100] copper depends strongly on both the strain rate and shock stress. Except at the very highest shock stress, the results for the [100] orientation show linear relationships between the spall strength and both the applied compressive stress and the strain rate. In addition, hydrodynamic computer code simulations of the spall experiments were performed to calculate the relationship between the strain rate near the spall plane in the target and the rate of free surface velocity release during the pullback. As expected, strain rates at the spall plane are much higher than the strain rates estimated from the free surface velocity release rate. We have begun soft recovery experiments and molecular dynamics calculations to understand the unusual recompression observed in the spall signature for [100] crystals.

Experimental Investigation of Orthoenstatite Single Crystal Rheology

NASA Astrophysics Data System (ADS)

fraysse, G.; Girard, J.; Holyoke, C. W.; Raterron, P.

2013-12-01

The plasticity of enstatite, upper mantle second most abundant mineral, is still poorly constrained, mostly because of its high-temperature (T) transformation into proto- and clino-enstatite at low pressure (P). Mackwell (1991, GRL, 18, 2027) reports a pioneer study of protoenstatite (Pbcn) single-crystal rheology, but the results do not directly apply to the orthorhombic (Pbca) mantle phase. Ohuchi et al. (2011, Contri. Mineral. Petrol , 161, 961) carried out deformation experiments at P=1.3 GPa on oriented orthoenstatite crystals, investigating the activity of [001](100) and [001](010) dislocation slip systems; they report the first rheological laws for orthoenstatite crystals. However, strain and stress were indirectly constrained in their experiments, which questioned whether steady state conditions of deformation were achieved. Also, data reported for [001](100) slip system were obtained after specimens had transformed by twinning into clinoenstatite. We report here new data from deformation experiments carried out at high T and P ranging from 3.5 to 6.2 GPa on natural Fe-bearing enstatite single crystals, using the Deformation-DIA apparatus (D-DIA) that equipped the X17B2 beamline of the NSLS (NY, USA). The applied stress and specimen strain rates were measured in situ by X-ray diffraction and imaging techniques (e.g., Raterron & Merkel, 2009, J. Sync. Rad., 16, 748; Raterron et al., 2013, Rev. Sci. Instr., 84, 043906). Three specimen orientations were tested: i) with the compression direction along [101]c crystallographic direction, which forms a 45° angle with both [100] and [001] axes, to investigate [001](100) slip-system activity; ii) along [011]c direction to investigate [001](010) system activity; iii) and along enstatite [125] axis, to activate both slip systems together. Crystals were deformed two by two, to compare slip system activities, or against enstatite aggregates or orientated olivine crystals of known rheology for comparison. Run products microstructures were investigated by transmission electron microscopy. Despite a significant hardening with P, enstatite [001](100) slip system is found to be the easiest system at mantle P and T. Furthermore, orthoenstatite crystals exhibit a higher sensitivity to stress than olivine crystals, i.e. a higher n exponent in classical power laws. At the low stress level prevailing in the Earth mantle, enstatite crystals are thus harder than olivine crystals.

Thick silicon growth techniques

NASA Technical Reports Server (NTRS)

Bates, H. E.; Mlavsky, A. I.; Jewett, D. N.

1973-01-01

Hall mobility measurements on a number of single crystal silicon ribbons grown from graphite dies have shown some ribbons to have mobilities consistent with their resistivities. The behavior of other ribbons appears to be explained by the introduction of impurities of the opposite sign. Growth of a small single crystal silicon ribbon has been achieved from a beryllia dia. Residual internal stresses of the order of 7 to 18,000 psi have been determined to exist in some silicon ribbon, particularly those grown at rates in excess of 1 in./min. Growth experiments have continued toward definition of a configuration and parameters to provide a reasonable yield of single crystal ribbons. High vacuum outgassing of graphite dies and evacuation and backfilling of growth chambers have provided significant improvements in surface quality of ribbons grown from graphite dies.

Additive Manufacturing of Single-Crystal Superalloy CMSX-4 Through Scanning Laser Epitaxy: Computational Modeling, Experimental Process Development, and Process Parameter Optimization

NASA Astrophysics Data System (ADS)

Basak, Amrita; Acharya, Ranadip; Das, Suman

2016-08-01

This paper focuses on additive manufacturing (AM) of single-crystal (SX) nickel-based superalloy CMSX-4 through scanning laser epitaxy (SLE). SLE, a powder bed fusion-based AM process was explored for the purpose of producing crack-free, dense deposits of CMSX-4 on top of similar chemistry investment-cast substrates. Optical microscopy and scanning electron microscopy (SEM) investigations revealed the presence of dendritic microstructures that consisted of fine γ' precipitates within the γ matrix in the deposit region. Computational fluid dynamics (CFD)-based process modeling, statistical design of experiments (DoE), and microstructural characterization techniques were combined to produce metallurgically bonded single-crystal deposits of more than 500 μm height in a single pass along the entire length of the substrate. A customized quantitative metallography based image analysis technique was employed for automatic extraction of various deposit quality metrics from the digital cross-sectional micrographs. The processing parameters were varied, and optimal processing windows were identified to obtain good quality deposits. The results reported here represent one of the few successes obtained in producing single-crystal epitaxial deposits through a powder bed fusion-based metal AM process and thus demonstrate the potential of SLE to repair and manufacture single-crystal hot section components of gas turbine systems from nickel-based superalloy powders.

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

PubMed

Klijn, Marieke E; Hubbuch, Jürgen

2018-04-27

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

Fabrication of a single sub-micron pore spanning a single crystal (100) diamond membrane and impact on particle translocation [Particle translocation through a single crystal diamond pore fabricated by electron beam induced chemical etching

DOE PAGES

Webb, Jennifer R.; Martin, Aiden A.; Johnson, Robert P.; ...

2017-06-21

The fabrication of sub-micron pores in single crystal diamond membranes, which span the entirety of the membrane, is described for the first time, and the translocation properties of polymeric particles through the pore investigated. The pores are produced using a combination of laser micromachining to form the membrane and electron beam induced etching to form the pore. Single crystal diamond as the membrane material, has the advantages of chemical stability and durability, does not hydrate and swell, has outstanding electrical properties that facilitate fast, low noise current-time measurements and is optically transparent for combined optical-conductance sensing. The resulting pores aremore » characterized individually using both conductance measurements, employing a microcapillary electrochemical setup, and electron microscopy. Proof-of-concept experiments to sense charged polystyrene particles as they are electrophoretically driven through a single diamond pore are performed, and the impact of this new pore material on particle translocation is explored. As a result, these findings reveal the potential of diamond as a platform for pore-based sensing technologies and pave the way for the fabrication of single nanopores which span the entirety of a diamond membrane.« less

Fabrication of a single sub-micron pore spanning a single crystal (100) diamond membrane and impact on particle translocation [Particle translocation through a single crystal diamond pore fabricated by electron beam induced chemical etching

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

Webb, Jennifer R.; Martin, Aiden A.; Johnson, Robert P.

The fabrication of sub-micron pores in single crystal diamond membranes, which span the entirety of the membrane, is described for the first time, and the translocation properties of polymeric particles through the pore investigated. The pores are produced using a combination of laser micromachining to form the membrane and electron beam induced etching to form the pore. Single crystal diamond as the membrane material, has the advantages of chemical stability and durability, does not hydrate and swell, has outstanding electrical properties that facilitate fast, low noise current-time measurements and is optically transparent for combined optical-conductance sensing. The resulting pores aremore » characterized individually using both conductance measurements, employing a microcapillary electrochemical setup, and electron microscopy. Proof-of-concept experiments to sense charged polystyrene particles as they are electrophoretically driven through a single diamond pore are performed, and the impact of this new pore material on particle translocation is explored. As a result, these findings reveal the potential of diamond as a platform for pore-based sensing technologies and pave the way for the fabrication of single nanopores which span the entirety of a diamond membrane.« less

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.

Fretting Fatigue of Single Crystal/Polycrystalline Nickel Subjected to Blade/Disk Contact Loading

NASA Astrophysics Data System (ADS)

Matlik, J. F.; Murthy, H.; Farris, T. N.

2002-01-01

Fretting fatigue describes the formation and growth of cracks at the edge-of-contact of nominally clamped components subjected to cyclic loading. Components that are known to be subject to fretting fatigue include riveted lap joints and blade/disk contacts in launch vehicle turbomachinery. Recent efforts have shown that conventional mechanics tools, both fatigue and fracture based, can be used to model fretting fatigue experiments leading to successful life predictions. In particular, experiments involving contact load configurations similar to those that occur in the blade/disk connection of gas turbine engines have been performed extensively. Predictions of fretting fatigue life have been compared favorably to experimental observations [1]. Recent efforts are aimed at performing experiments at higher temperatures as shown in the photograph below along with a sample fracture surface. The talk will describe the status of these experiments as will as model developments relevant to the single crystal material properties.

Biotechnology Science Experiments on Mir

NASA Technical Reports Server (NTRS)

Kroes, Roger L.

1999-01-01

This paper describes the microgravity biotechnology experiments carried out on the Shuttle/Mir program. Four experiments investigated the growth of protein crystals, and three investigated cellular growth. Many hundreds of protein samples were processed using four different techniques. The objective of these experiments was to determine optimum conditions for the growth of very high quality single crystals to be used for structure determination. The Biotechnology System (BTS) was used to process the three cell growth investigations. The samples processed by these experiments were: bovine chondrocytes, human renal epithelial cells, and human breast cancer cells and endothelial cells. The objective was to determine the unique properties of cell aggregates produced in the microgravity environment.

The deformation mechanisms and size effects of single-crystal magnesium

NASA Astrophysics Data System (ADS)

Byer, Cynthia M.

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

Friction and wear of tin and tin alloys from minus 100 C to 150 C

NASA Technical Reports Server (NTRS)

Buckley, D. H.

1975-01-01

Sliding friction experiments were conducted with an iron (110) single-crystal pin sliding on single and polycrystalline tin and tin alloys. Specimens were examined at various ambient temperatures from -100 to 150 C. Applied loads varied from 1 to 50 grams, and sliding velocity was constant at 0.7 mm/min. Results indicate that the crystal transformation of tin influences the friction coefficient. Friction was higher for the diamond structure (gray tin) than it was for the body-centered tetragonal structure (white tin). Bismuth arrested the crystal transformation, which resulted in constant friction over the temperature range -100 to 150 C. Both copper and aluminum enhanced the kinetics of transformation, with aluminum producing a nearly twofold change in friction with the crystal transformation.

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

Li, Xiao; Martínez-González, José A.; Hernández-Ortiz, Juan P.

Liquid crystal blue phases (BPs) are highly ordered at two levels. Molecules exhibit orientational order at nanometer length scales, while chirality leads to ordered arrays of doubletwisted cylinders over micrometer scales. Past studies of polycrystalline BPs were challenged by grain boundaries between randomly oriented crystalline nanodomains. Here, the nucleation of BPs is controlled with considerable precision by relying on chemically nano-patterned surfaces, leading to macroscopic single-crystal BP specimens where the dynamics of meso-crystal formation can be directly observed. Theory and experiments show that transitions between two BPs having a different network structure proceed through local re-organization of the crystalline array,more » without diffusion of the double twisted cylinders. In solid crystals, martensitic transformations between crystal structures involve the concerted motion of a few atoms, without diffusion. The transformation between BPs, where crystal features arise in the sub-micron regime, is found to be martensitic in nature, with the diffusion-less feature associated to the collective behavior of the double twist cylinders. Single-crystal BPs are shown to offer fertile grounds for the study of directed crystal-nucleation and the controlled growth of soft matter.« less

Characterisation of irradiation-induced defects in ZnO single crystals

NASA Astrophysics Data System (ADS)

Prochazka, I.; Cizek, J.; Lukac, F.; Melikhova, O.; Valenta, J.; Havranek, V.; Anwand, W.; Skuratov, V. A.; Strukova, T. S.

2016-01-01

Positron annihilation spectroscopy (PAS) combined with optical methods was employed for characterisation of defects in the hydrothermally grown ZnO single crystals irradiated by 167 MeV Xe26+ ions to fluences ranged from 3×1012 to 1×1014 cm-2. The positron lifetime (LT), Doppler broadening as well as slow-positron implantation spectroscopy (SPIS) techniques were involved. The ab-initio theoretical calculations were utilised for interpretation of LT results. The optical transmission and photoluminescence measurements were conducted, too. The virgin ZnO crystal exhibited a single component LT spectrum with a lifetime of 182 ps which is attributed to saturated positron trapping in Zn vacancies associated with hydrogen atoms unintentionally introduced into the crystal during the crystal growth. The Xe ion irradiated ZnO crystals have shown an additional component with a longer lifetime of ≈ 360 ps which comes from irradiation-induced larger defects equivalent in size to clusters of ≈10 to 12 vacancies. The concentrations of these clusters were estimated on the basis of combined LT and SPIS data. The PAS data were correlated with irradiation induced changes seen in the optical spectroscopy experiments.

Laser materials processing facility

NASA Technical Reports Server (NTRS)

Haggerty, J. S.

1982-01-01

The laser materials processing facility and its capabilities are described. A CO2 laser with continuous wave, repetitive pulse, and shaped power-time cycles is employed. The laser heated crystal growth station was used to produce metal and metal oxide single crystals and for cutting and shaping experiments using Si3N4 to displace diamond shaping processes.

Crystallization of Magma. CEGS Programs Publication Number 14.

ERIC Educational Resources Information Center

Berry, R. W.

Crystallization of Magma is one of a series of single-topic problem modules intended for use in undergraduate geology and earth science courses. Through problems and observations based on two sets of experiments, this module leads to an understanding of how an igneous rock can form from molten material. Environmental factors responsible for…

Containerless processing of single crystals in low-G environment

NASA Technical Reports Server (NTRS)

Walter, H. U.

1974-01-01

Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.

Anisotropic Thermoelectric Devices Made from Single-Crystal Semimetal Microwires in Glass Coating

NASA Astrophysics Data System (ADS)

Konopko, L. A.; Nikolaeva, A. A.; Kobylianskaya, A. K.; Huber, T. E.

2018-06-01

Thermoelectric heat conversion based on the Seebeck and Peltier effects generated at the junction between two materials of type- n and type- p is well known. Here, we present a demonstration of an unconventional thermoelectric energy conversion that is based on a single element made of an anisotropic material. In such materials, a heat flow generates a transverse thermoelectric electric field lying across the heat flow. Potentially, in applications involving miniature devices, the anisotropic thermoelectric (AT) effect has the advantage over traditional thermoelectrics that it simplifies the thermoelectric generator architecture. This is because the generator can be made of a single thermoelectric material without the complexity of a series of contacts forming a pile. A feature of anisotropic thermoelectrics is that the thermoelectric voltage is proportional to the element length and inversely proportional to the effective thickness. The AT effect has been demonstrated with artificial anisotropic thin film consisting of layers of alternating thermoelectric type, but there has been no demonstration of this effect in a long single-crystal. Electronic transport measurements have shown that the semimetal bismuth is highly anisotropic. We have prepared an experimental sample consisting of a 10-m-long glass-insulated single-crystal tin-doped bismuth microwire ( d = 4 μm). Crucial for this experiment is the ability to grow the microwire as a single-crystal using a technique of recrystallization with laser heating and under a strong electric field. The sample was wound as a spiral, bonded to a copper disk, and used in various experiments. The sensitivity of the sample to heat flow is as high as 10-2 V/W with a time constant τ of about 0.5 s.

Anisotropic Thermoelectric Devices Made from Single-Crystal Semimetal Microwires in Glass Coating

NASA Astrophysics Data System (ADS)

Konopko, L. A.; Nikolaeva, A. A.; Kobylianskaya, A. K.; Huber, T. E.

2018-04-01

Thermoelectric heat conversion based on the Seebeck and Peltier effects generated at the junction between two materials of type-n and type-p is well known. Here, we present a demonstration of an unconventional thermoelectric energy conversion that is based on a single element made of an anisotropic material. In such materials, a heat flow generates a transverse thermoelectric electric field lying across the heat flow. Potentially, in applications involving miniature devices, the anisotropic thermoelectric (AT) effect has the advantage over traditional thermoelectrics that it simplifies the thermoelectric generator architecture. This is because the generator can be made of a single thermoelectric material without the complexity of a series of contacts forming a pile. A feature of anisotropic thermoelectrics is that the thermoelectric voltage is proportional to the element length and inversely proportional to the effective thickness. The AT effect has been demonstrated with artificial anisotropic thin film consisting of layers of alternating thermoelectric type, but there has been no demonstration of this effect in a long single-crystal. Electronic transport measurements have shown that the semimetal bismuth is highly anisotropic. We have prepared an experimental sample consisting of a 10-m-long glass-insulated single-crystal tin-doped bismuth microwire (d = 4 μm). Crucial for this experiment is the ability to grow the microwire as a single-crystal using a technique of recrystallization with laser heating and under a strong electric field. The sample was wound as a spiral, bonded to a copper disk, and used in various experiments. The sensitivity of the sample to heat flow is as high as 10-2 V/W with a time constant τ of about 0.5 s.

Combining EPR spectroscopy and X-ray crystallography to elucidate the structure and dynamics of conformationally constrained spin labels in T4 lysozyme single crystals.

PubMed

Consentius, Philipp; Gohlke, Ulrich; Loll, Bernhard; Alings, Claudia; Heinemann, Udo; Wahl, Markus C; Risse, Thomas

2017-08-09

Electron paramagnetic resonance (EPR) spectroscopy in combination with site-directed spin labeling is used to investigate the structure and dynamics of conformationally constrained spin labels in T4 lysozyme single crystals. Within a single crystal, the oriented ensemble of spin bearing moieties results in a strong angle dependence of the EPR spectra. A quantitative description of the EPR spectra requires the determination of the unit cell orientation with respect to the sample tube and the orientation of the spin bearing moieties within the crystal lattice. Angle dependent EPR spectra were analyzed by line shape simulations using the stochastic Liouville equation approach developed by Freed and co-workers and an effective Hamiltonian approach. The gain in spectral information obtained from the EPR spectra of single crystalline samples taken at different frequencies, namely the X-band and Q-band, allows us to discriminate between motional models describing the spectra of isotropic solutions similarly well. In addition, it is shown that the angle dependent single crystal spectra allow us to identify two spin label rotamers with very similar side chain dynamics. These results demonstrate the utility of single crystal EPR spectroscopy in combination with spectral line shape simulation techniques to extract valuable dynamic information not readily available from the analysis of isotropic systems. In addition, it will be shown that the loss of electron density in high resolution diffraction experiments at room temperature does not allow us to conclude that there is significant structural disorder in the system.

A micromechanical constitutive model for anisotropic cyclic deformation of super-elastic NiTi shape memory alloy single crystals

NASA Astrophysics Data System (ADS)

Yu, Chao; Kang, Guozheng; Kan, Qianhua

2015-09-01

Based on the experimental observations on the anisotropic cyclic deformation of super-elastic NiTi shape memory alloy single crystals done by Gall and Maier (2002), a crystal plasticity based micromechanical constitutive model is constructed to describe such anisotropic cyclic deformation. To model the internal stress caused by the unmatched inelastic deformation between the austenite and martensite phases on the plastic deformation of austenite phase, 24 induced martensite variants are assumed to be ellipsoidal inclusions with anisotropic elasticity and embedded in the austenite matrix. The homogeneous stress fields in the austenite matrix and each induced martensite variant are obtained by using the Mori-Tanaka homogenization method. Two different inelastic mechanisms, i.e., martensite transformation and transformation-induced plasticity, and their interactions are considered in the proposed model. Following the assumption of instantaneous domain growth (Cherkaoui et al., 1998), the Helmholtz free energy of a representative volume element of a NiTi shape memory single crystal is established and the thermodynamic driving forces of the internal variables are obtained from the dissipative inequalities. The capability of the proposed model to describe the anisotropic cyclic deformation of super-elastic NiTi single crystals is first verified by comparing the predicted results with the experimental ones. It is concluded that the proposed model can capture the main quantitative features observed in the experiments. And then, the proposed model is further used to predict the uniaxial and multiaxial transformation ratchetting of a NiTi single crystal.

Performance of A Compact Multi-crystal High-purity Germanium Detector Array for Measuring Coincident Gamma-ray Emissions

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

Howard, Chris; Daigle, Stephen; Buckner, Matt

2015-02-18

The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ) 15O* reaction for several transition energies at an effective center of mass energy of 163 keV. Owing to the segmented nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within the uncertainties with the past measurements. Details of the analysis and detector performance will be presented.

Polymorphism of Alprazolam (Xanax): a review of its crystalline phases and identification, crystallographic characterization, and crystal structure of a new polymorph (form III).

PubMed

de Armas, Héctor Novoa; Peeters, Oswald M; Van den Mooter, Guy; Blaton, Norbert

2007-05-01

A new polymorphic form of Alprazolam (Xanax), 8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo-[4,3-alpha][1,4]benzodiazepine, C(17)H(13)ClN(4), has been investigated by means of X-ray powder diffraction (XRPD), single crystal X-ray diffraction, and differential scanning calorimetry (DSC). This polymorphic form (form III) was obtained during DSC experiments after the exothermic recrystallization of the melt of form I. The crystal unit cell dimensions for form III were determined from diffractometer methods. The monoclinic unit cell found for this polymorph using XRPD after indexing the powder diffractogram was confirmed by the cell parameters obtained from single crystal X-ray diffractometry on a crystal isolated from the DSC pans. The single crystal unit cell parameters are: a = 28.929(9), b = 13.844(8), c = 7.361(3) angstroms, beta = 92.82(3) degrees , V = 2944(2) angstroms(3), Z = 8, space group P2(1) (No.4), Dx = 1.393 Mg/m(3). The structure obtained from single crystal X-ray diffraction was used as initial model for Rietveld refinement on the powder diffraction data of form III. The temperature phase transformations of alprazolam were also studied using high temperature XRPD. A review of the different phases available in the Powder Diffraction File (PDF) database for this drug is described bringing some clarification and corrections. (c) 2007 Wiley-Liss, Inc. and the American Pharmacists Association.

Anomalous domain inversion in LiNbO3 single crystals investigated by scanning probe microscopy

NASA Astrophysics Data System (ADS)

Lilienblum, M.; Soergel, E.

2011-09-01

Ferroelectric domains were written in lithium niobate (LiNbO3) single crystals by applying voltage pulses to the tip of a scanning force microscope. The generated domains are subsequently imaged by piezoresponse force microscopy. As it has been previously observed not only full domains but also doughnut-shaped ones arise from tip-based domain formation. In this contribution, we present our experiments which were carried out with 10-20 μm thin LiNbO3 single crystals. We show that by choosing appropriate writing parameters, domains of predetermined shape (full or doughnut) can be reliably generated. In addition to the duration and the amplitude of the voltage pulse the moment of the retraction of the tip from the sample surface was found to be a crucial parameter for reproducible domain formation.

Crystal structures of carbonates up to Mbar pressures determined by single crystal synchrotron radiation diffraction

NASA Astrophysics Data System (ADS)

Merlini, M.

2013-12-01

The recent improvements at synchrotron beamlines, currently allow single crystal diffraction experiments at extreme pressures and temperatures [1,2] on very small single crystal domains. We successfully applied such technique to determine the crystal structure adopted by carbonates at mantle pressures. The knowledge of carbon-bearing phases is in fact fundamental for any quantitative modelling of global carbon cycle. The major technical difficulty arises after first order transitions or decomposition reactions, since original crystal (apx. 10x10x5 μm3) is transformed in much smaller crystalline domains often with random orientation. The use of 3D reciprocal space visualization software and the improved resolution of new generation flat panel detectors, however, allow both identification and integration of each single crystal domain, with suitable accuracy for ab-initio structure solution, performed with direct and charge-flipping methods and successive structure refinements. The results obtained on carbonates, indicate two major crystal-chemistry trends established at high pressures. The CO32- units, planar and parallel in ambient pressure calcite and dolomite structures, becomes non parallel in calcite- and dolomite-II and III phases, allowing more flexibility in the structures with possibility to accommodate strain arising from different cation sizes (Ca and Mg in particular). Dolomite-III is therefore also observed to be thermodynamically stable at lower mantle pressures and temperatures, differently from dolomite, which undergoes decomposition into pure end-members in upper mantle. At higher pressure, towards Mbar (lowermost mantle and D'' region) in agreement with theoretical calculations [3,4] and other experimental results [5], carbon coordination transform into 4-fold CO4 units, with different polymerisation in the structure depending on carbonate composition. The second important crystal chemistry feature detected is related to Fe2+ in Fe-bearing magnesite, which spontaneously oxidises at HP/HT, forming Fe3+ carbonates, Fe3+ oxides and reduced carbon (diamonds). Single crystal diffraction approach allowed full structure determination of these phases, yielding to the discovery of few unpredicted structures, such as Mg2Fe2C4O13 and Fe13O19, which can be well reproduced in different experiments. Mg2Fe2C4O13 carbonate present truncated chain C4O13 groups, and Fe13O19 oxide, whose stoichiometry is intermediate between magnetite and hematite, is a one-layer structure, with features encountered in superconducting materials. The results fully support the ideas of unexpected complexities in the mineralogy of the lowermost mantle, and single crystal technique, once properly optimized in ad-hoc synchrotron beamlines, is fundamental for extracting accurate structural information, otherwise rarely accessible with other experimental techniques. References: [1] Merlini M., Hanfland M. (2013). Single crystal diffraction at Mbar conditions by synchrotron radiation. High Pressure Research, in press. [2] Dubrovinsky et al., (2010). High Pressure Research, 30, 620-633. [3] Arapan et al. (1997). Phys. Rev. Lett., 98, 268501. [4] Oganov et al. (2008) EPSL, 273, 38-47. [5] Boulard et al. (2011) PNAS, 108, 5184-5187.

Growth of tourmaline single crystals containing transition metal elements in hydrothermal solutions

NASA Astrophysics Data System (ADS)

Setkova, Tatiana; Shapovalov, Yury; Balitsky, Vladimir

2011-03-01

Interest in the growth of tourmaline single crystals is based on the promising piezoelectric and pyroelectric properties of this material compared to quartz crystals currently in use. Moreover, synthetic tourmaline can be used as a substitute for the natural stone in the jewelry industry similar to other synthetic analogues of gemstones. Single crystals of colored Co-, Ni-, Fe-, (Ni,Cr)-, (Ni,Fe)-, and (Co,Ni,Cr)-containing tourmalines with concentration of transition metal elements up to 16 wt% on a seed have been grown from complex boron-containing hydrothermal solutions at a range of temperatures 400-750 °C and pressures 100 MPa. Experiments were conducted under conditions of a thermal gradient in titanium and chromium-nickel autoclaves. Tourmaline growth on a seed crystal occurs only if separate tourmaline-forming components (monocrystalline corundum and quartz bars) are used as charge. All tourmalines specified above grow in analogous (+) direction of the optical axis with a speed of 0.05 mm/day by faces of the trigonal pyramid, except tourmalines containing chromium. They grow in analogous (+0001) direction with a speed 0.05 mm/day, and in antilogous (-0001) direction with a speed of 0.01 mm/day by faces of the trigonal pyramid and in prism direction with a speed of 0.001 mm/day. Along with the large single crystals, a great amount of finest (30-150 μm in size) tourmaline crystals was formed during the runs by spontaneous nucleation both on the surface of the seed crystals and in the charge.

Astronaut Joseph R. Tanner works with PCG experiment on middeck

NASA Image and Video Library

1994-11-14

On the Space Shuttle Atlantis' mid-deck, astronaut Joseph R. Tanner, mission specialist, works at area amidst several lockers onboard the Shuttle which support the Protein Crystal Growth (PCG) experiment. This particular section is called the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES). Together with the Vapor Diffusion Apparatus (VDA), housed in a Single Locker Thermal Enclosure (SLTES) which is out of frame, the Cos/TES represents the continuing research into the structures of proteins and other macromolecules such as viruses.

Astronauts Brent Jett and Koichi Wakata work with Protein Crystal Growth experiment

NASA Image and Video Library

1996-01-20

STS072-310-007 (11-20 Jan. 1996) --- Astronauts Brent W. Jett Jr. (left) and Koichi Wakata work with the Protein Crystal Growth (PCG) experiment at the Single Locker Thermal Enclosure System (STES) on the Space Shuttle Endeavour’s mid-deck. Jett, making his first flight in space, served as the crew’s pilot, while Wakata served as a mission specialist. Wakata, also a first time Shuttle crew member, represents Japan’s National Space Development Agency (NASDA).

Detection of single nano-defects in photonic crystals between crossed polarizers.

PubMed

Grepstad, Jon Olav; Kaspar, Peter; Johansen, Ib-Rune; Solgaard, Olav; Sudbø, Aasmund

2013-12-16

We investigate, by simulations and experiments, the light scattering of small particles trapped in photonic crystal membranes supporting guided resonance modes. Our results show that, due to amplified Rayleigh small particle scattering, such membranes can be utilized to make a sensor that can detect single nano-particles. We have designed a biomolecule sensor that uses cross-polarized excitation and detection for increased sensitivity. Estimated using Rayleigh scattering theory and simulation results, the current fabricated sensor has a detection limit of 26 nm, corresponding to the size of a single virus. The sensor can potentially be made both cheap and compact, to facilitate use at point-of-care.

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Pauli structures arising from confined particles interacting via a statistical potential

NASA Astrophysics Data System (ADS)

Batle, Josep; Ciftja, Orion; Farouk, Ahmed; Alkhambashi, Majid; Abdalla, Soliman

2017-09-01

There have been suggestions that the Pauli exclusion principle alone can lead a non-interacting (free) system of identical fermions to form crystalline structures dubbed Pauli crystals. Single-shot imaging experiments for the case of ultra-cold systems of free spin-polarized fermionic atoms in a two-dimensional harmonic trap appear to show geometric arrangements that cannot be characterized as Wigner crystals. This work explores this idea and considers a well-known approach that enables one to treat a quantum system of free fermions as a system of classical particles interacting with a statistical interaction potential. The model under consideration, though classical in nature, incorporates the quantum statistics by endowing the classical particles with an effective interaction potential. The reasonable expectation is that possible Pauli crystal features seen in experiments may manifest in this model that captures the correct quantum statistics as a first order correction. We use the Monte Carlo simulated annealing method to obtain the most stable configurations of finite two-dimensional systems of confined particles that interact with an appropriate statistical repulsion potential. We consider both an isotropic harmonic and a hard-wall confinement potential. Despite minor differences, the most stable configurations observed in our model correspond to the reported Pauli crystals in single-shot imaging experiments of free spin-polarized fermions in a harmonic trap. The crystalline configurations observed appear to be different from the expected classical Wigner crystal structures that would emerge should the confined classical particles had interacted with a pair-wise Coulomb repulsion.

Experimental Deformation of Enstatite Single Crystals at Mantle Pressure and Temperature

NASA Astrophysics Data System (ADS)

Raterron, P. C.; Holyoke, C. W.; Girard, J.

2012-12-01

Orthopyroxenes (OPx) is the second most abundant constituent of the upper mantle, thus may significantly influence mantle plasticity. However, little is known on OPx rheology at high pressure; this is because apparatuses allowing controlled deformation experiments at asthenospheric pressures (P > 3 GPa) are available since only a decade (see Raterron and Merkel, 2009, J. Synch. Rad., 16, 748-756). Mackwell (1991, GRL, 18, 2027-2030) reports a preliminary study of the high-temperature rheology of enstatite single crystals, but these experiments were carried out at room pressure, i.e. in the protoenstatite stability field, and the results cannot directly apply to mantle phases. In order to quantify the effect of pressure on OPx rheology, deformation experiments were carried out in compression on natural enstatite (En90) single crystals in the Deformation-DIA apparatus (D-DIA), at P > 5 GPa and high temperature (T > 1200°C) within the orthoenstatite stability field. The applied stress and specimen strain rates were measured in situ using X-ray diffraction and imaging techniques at the X17B2 beamline of the National Synchrotron Light Source (NSLS, NY, USA). The cylindrical specimens were oriented with their axis - the compression direction - along [101]c crystallographic direction which forms a 45° angle with both [100] and [001] directions. This geometry imposes during compression a maximum shear stress in (001) plane along [001] direction, which results in the activation of [001](001) dislocation slip system known as the weakest slip in OPx. Specimens were deformed together with other crystals or aggregates - two by two, one atop the other in the compression column - in order to compare [101]c crystal plasticity with that of either [011]c enstatite crystals - within which [001](010) slip system is activated - or enstatite aggregates, or again orientated San Carlos olivine crystals of known rheology. Run products microstructures were investigated by electron microscopy. We will present these results which bring new light on the activity of orthoenstatite dislocation slips at mantle P and T conditions.

Inverse Slip Accompanying Twinning and Detwinning during Cyclic Loading of Magnesium Single Crystal

DOE PAGES

Yu, Qin; Wang, Jian; Jiang, Yanyao

2013-01-01

In situ , observation of twinning and detwinning in magnesium single crystals during tension-compression cyclic loading was made using optical microscopy. A quantitative analysis of plastic strain indicates that twinning and detwinning experience two stages, low and high work hardening de-twinning, and pure re-twinning and fresh twinning combined with retwinning. Slip is always activated. For the first time, inverse slip accompanying with pure retwinning and high work hardening detwinning was experimentally identified, which provides insights in better understanding of the activity of twining, detwinning, and slips.

Helium diffusion experiments on synthetic apatite crystals and single-grain fragments: can we retrieve the He diffusion profiles?

NASA Astrophysics Data System (ADS)

Kasanzu, C.; Beucher, R.; Brown, R. W.; Persano, C.; Stuart, F.

2011-12-01

Apatite (U-Th)/he thermochronometry is one of the most widely used methods of quantifying thermal histories of rocks within the vicinity of the surface. Theoretical and practical development carried out during the last decade, among which was the release of affordable LASERs, have led to standard practice of analyzing single grain rather than multigrain aliquots. The standard theoretical basis for interpreting these ages assumes that the technique is used on full grains. However, the natural weak cleavage of apatite leads to fragmentation of these individual prismatic crystals during the rock crushing and mineral separation process. Apatites are most often broken along a weak cleavage perpendicular to the c-axis. It is therefore common practice to analyze fragments of whole grains, not complete crystals. It is also well known that dating often leads to single ages being more dispersed than expected whatever the efforts to avoid perturbations on the He system. Using a theoretical numerical model and considering both axial and radial diffusion, we demonstrate thata largepart (most?) of the dispersion is due to analyses of single apatite fragments. This effect is larger for older grains which have exprienced a slow cooling history and have well rounded diffusive profiles. Ages are a strongfunction of the fragment size (length specifically), we show that ages from apatite fragments with 1 prismatic termination (1T) can be used to retrieve the helium diffusion profile, provided a sufficient number of single fragment analyses are carried out. The shape of the helium diffusion profile provides a strong constraint on the style of the thermal history and so we propose to use single crystal fragment analyses to extract a mean diffusion profile, and deduce the thermal history of the sample. In order to test these ideas, we performed a set of experiments with natural samples and semi-synthetic grains of apatite. Synthetic grains are obtained by drilling cores of various length/width ratios within standard Durango crystals while natural grains are separated from a deep borehole in south-Africa (BK1) and from the Australian craton. Several experiences are presented: 1) (U-Th)/He dating of about 100 1T single-fragment aliquots of different shape ratio from the BK1 borehole; 2) (U-Th)/He dating of 20 2T single-fragment aliquot from an Australian sample previously dated following standard procedure. 3) (U-Th)/He dating of synthetic fragmentsfrom synthetic grains previously degassed by a known percentageusing a thermo-regulated furnace. The results of the experiments lead to important new insight into the natural dispersion of (U-Th)/He single-grain ages. They show that far from being problematic, highly dispersed data may indeed contain first-order information on the thermal history of rocks. We discuss all the details of the standard (U-Th)/He approach such as the effects of temporally variable diffusivity (e.g. radiation damage models), zonation of U and Th and arbitrary grain size variations.

Effect of guest-host interaction on Raman spectrum of a CO2 clathrate hydrate single crystal

NASA Astrophysics Data System (ADS)

Ikeda, Tomoko; Mae, Shinji; Uchida, Tsutomu

1998-01-01

The polarized Raman spectra of an artificial CO2 clathrate hydrate single crystal have been measured in order to examine the crystal-orientation dependence of the Raman spectra. Since the crystal had crystallographic facets, the orientation of the crystal was determined by using the Miller indices of the facets. When the angle θ between the polarization plane of the incident laser beam and the direction of one of the <110> axes of the single crystal varied, it was observed that the intensities of the peaks, which were caused by the Fermi resonance of the symmetric stretching mode and the overtone of the bending mode of CO2, and the O-H symmetric stretching vibration mode, varied with θ. Since the tetrakaidecahedron cage in the CO2 clathrate hydrate is distorted along the <100> axis, the variations of the scattering intensities of the CO2 have been calculated by using a simple model that assumes that the CO2 rotates on the {100} plane in the tetrakaidecahedron cage. The results obtained from the experiments are consistent with the calculations made by using this model. It has been concluded that the anisotropy of the peak intensities of the CO2 show the influence of the cage geometry on the motion of the guest molecule. The anisotropy of the O-H symmetric stretching vibration mode was interpreted with a five-body structure model. As the calculation with the model was consistent with the result obtained from the experiment, it was found that the anisotropy of the peak intensity of the O-H symmetric stretching vibration mode was related to the arrangement of the water molecules. We consider that the result indicates the influence of the motion of the guest molecule on the surrounding hydrogen-bonded network.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador).

PubMed

Chevrel, Magdalena Oryaëlle; Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B

2015-03-01

Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt-sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time-Temperature-Transformation) diagram illustrating the crystallization "nose" for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear-thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador)

PubMed Central

Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B.; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B.

2015-01-01

Abstract Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt‐sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time‐Temperature‐Transformation) diagram illustrating the crystallization “nose” for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear‐thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity. PMID:27656114

Finite Element Analysis of a Copper Single Crystal Shape Memory Alloy-Based Endodontic Instruments

NASA Astrophysics Data System (ADS)

Vincent, Marin; Thiebaud, Frédéric; Bel Haj Khalifa, Saifeddine; Engels-Deutsch, Marc; Ben Zineb, Tarak

2015-10-01

The aim of the present paper is the development of endodontic Cu-based single crystal Shape Memory Alloy (SMA) instruments in order to eliminate the antimicrobial and mechanical deficiencies observed with the conventional Nickel-Titane (NiTi) SMA files. A thermomechanical constitutive law, already developed and implemented in a finite element code by our research group, is adopted for the simulation of the single crystal SMA behavior. The corresponding material parameters were identified starting from experimental results for a tensile test at room temperature. A computer-aided design geometry has been achieved and considered for a finite element structural analysis of the endodontic Cu-based single crystal SMA files. They are meshed with tetrahedral continuum elements to improve the computation time and the accuracy of results. The geometric parameters tested in this study are the length of the active blade, the rod length, the pitch, the taper, the tip diameter, and the rod diameter. For each set of adopted parameters, a finite element model is built and tested in a combined bending-torsion loading in accordance with ISO 3630-1 norm. The numerical analysis based on finite element procedure allowed purposing an optimal geometry suitable for Cu-based single crystal SMA endodontic files. The same analysis was carried out for the classical NiTi SMA files and a comparison was made between the two kinds of files. It showed that Cu-based single crystal SMA files are less stiff than the NiTi files. The Cu-based endodontic files could be used to improve the root canal treatments. However, the finite element analysis brought out the need for further investigation based on experiments.

Comparing olivine single crystal and polycrystal rheology: evidence for supplementary accommodation mechanisms at grain boundaries

NASA Astrophysics Data System (ADS)

Bollinger, C.; Merkel, S.; Raterron, P.; Castelnau, O.; Detrez, F.

2013-12-01

Rheology in the Earth's upper-mantle is mostly constrained by the plastic properties of olivine. Over recent years, several groups have been carrying out deformation experiments on single crystals and polycrystals of olivine at upper mantle pressure (P) and temperature (T). Yet, the rheology of olivine at mantle conditions is still not well constrained. We carried out deformation experiments on San Carlos olivine polycrystals, at P and T ranging from 3 to 8 GPa and 1373 to 1673 K, respectively, and at strain rates ranging from 10-6 to 10-4 s-1, using the D-DIA apparatus installed at the NSLS X17B2 beamline (NY, USA). The deformation rates of the polycrystals are compared to those of single crystals oriented along the soft orientations [110]c, [011]c, [101]c which activate the easiest slip systems (Raterron et al., 2012). This comparison suggests that, in olivine polycrystals deforming in the dislocation creep regime, other relaxation mechanisms need to be considered to account for the observed polycrystal strain rates. This highlights the importance of supplementary mechanisms, such as those occurring at grain boundaries, to properly model olivine aggregates plasticity.

Deformation mechanisms, defects, heat treatment, and thermal conductivity in large grain niobium

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

Bieler, Thomas R., E-mail: bieler@egr.msu.edu; Kang, Di, E-mail: kangdi@msu.edu; Baars, Derek C., E-mail: baarsder@gmail.com

2015-12-04

The physical and mechanical metallurgy underlying fabrication of large grain cavities for superconducting radio frequency accelerators is summarized, based on research of 1) grain orientations in ingots, 2) a metallurgical assessment of processing a large grain single cell cavity and a tube, 3) assessment of slip behavior of single crystal tensile samples extracted from a high purity ingot slice before and after annealing at 800 °C / 2 h, 4) development of crystal plasticity models based upon the single crystal experiments, and 5) assessment of how thermal conductivity is affected by strain, heat treatment, and exposure to hydrogen. Because of themore » large grains, the plastic anisotropy of deformation is exaggerated, and heterogeneous strains and localized defects are present to a much greater degree than expected in polycrystalline material, making it highly desirable to computationally anticipate potential forming problems before manufacturing cavities.« less

Spall behaviour of single crystal aluminium at three principal orientations

NASA Astrophysics Data System (ADS)

Owen, G. D.; Chapman, D. J.; Whiteman, G.; Stirk, S. M.; Millett, J. C. F.; Johnson, S.

2017-10-01

A series of plate impact experiments have been conducted to study the spall strength of the three principal crystallographic orientations of single crystal aluminium ([100], [110] and, [111]) and ultra-pure polycrystalline aluminium. The samples have been shock loaded at two impact stresses (4 GPa and 10 GPa). Significant differences have been observed in the elastic behaviour, the pullback velocities, and the general shape of the wave profiles, which can be accounted for by considerations of the microscale homogeneity, the dislocation density, and the absence of grain boundaries in the single crystal materials. The data have shown that there is a consistent order of spall strength measured for the four sample materials. The [111] orientation has the largest spall strength and elastic limit, followed closely by [110], [100], and then the polycrystalline material. This order is consistent with both quasi-static data and geometrical consideration of Schmid factors.

Plastic Deformation of Aluminum Single Crystals at Elevated Temperatures

NASA Technical Reports Server (NTRS)

Johnson, R D; Young, A P; Schwope, A D

1956-01-01

This report describes the results of a comprehensive study of plastic deformation of aluminum single crystals over a wide range of temperatures. The results of constant-stress creep tests have been reported for the temperature range from 400 degrees to 900 degrees F. For these tests, a new capacitance-type extensometer was designed. This unit has a range of 0.30 inch over which the sensitivity is very nearly linear and can be varied from as low a sensitivity as is desired to a maximum of 20 microinches per millivolt with good stability. Experiments were carried out to investigate the effect of small amounts of prestraining, by two different methods, on the creep and tensile properties of these aluminum single crystals. From observations it has been concluded that plastic deformation takes place predominantly by slip which is accompanied by the mechanisms of kinking and polygonization.

Two-dimensional single crystal diamond refractive x-ray lens

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

Antipov, S., E-mail: s.antipov@euclidtechlabs.com; Baryshev, S. V.; Butler, J. E.

2016-07-27

The next generation light sources such as diffraction-limited storage rings and high repetition rate x-ray free-electron lasers will generate x-ray beams with significantly increased brilliance. These future machines will require X-ray optical components that are capable of handling higher instantaneous and average power densities while tailoring the properties of the x-ray beams for a variety of scientific experiments. Single crystal diamond is one of the best bulk materials for this application, because it is radiation hard, has a suitable uniform index of refraction and the best available thermal properties. In this paper we report on fabrication and experimental testing ofmore » a two-dimensional (2D) single crystal diamond compound refractive X-ray lenses (CRL). These lenses were manufactured using femto-second laser cutting and tested at the Advanced Photon Source of Argonne National Laboratory.« less

GROWTH AND CHARACTERIZATION OF SINGLE CRYSTALS OF RARE EARTH COMPOUNDS.

DTIC Science & Technology

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

Effect of Surface Preparation on the 815°C Oxidation of Single-Crystal Nickel-Based Superalloys

NASA Astrophysics Data System (ADS)

Sudbrack, Chantal K.; Beckett, Devon L.; MacKay, Rebecca A.

2015-11-01

A primary application for single-crystal superalloys has been jet engine turbine blades, where operation temperatures reach well above 1000°C. The NASA Glenn Research Center is considering use of single-crystal alloys for future, lower temperature application in the rims of jet engine turbine disks. Mechanical and environmental properties required for potential disk rim operation at 815°C are being examined, including the oxidation and corrosion behavior, where there is little documentation at intermediate temperatures. In this study, single-crystal superalloys, LDS-1101+Hf and CMSX-4+Y, were prepared with different surface finishes and compared after isothermal and cyclic oxidation exposures. Surface finish has a clear effect on oxide formation at 815°C. Machined low-stress ground surfaces after exposure for 440 h produce thin Al2O3 external scales, which is consistent with higher temperature oxidation, whereas polished surfaces with a mirror finish yield much thicker NiO external scales with subscale of Cr2O3-spinel-Al2O3, which may offer less reliable oxidation resistance. Additional experiments separate the roles of cold-work, localized deformation, and the extent of polishing and surface roughness on oxide formation.

Auger electron spectroscopy analysis for growth interface of cubic boron nitride single crystals synthesized under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Lv, Meizhe; Xu, Bin; Cai, Lichao; Guo, Xiaofei; Yuan, Xingdong

2018-05-01

After rapid cooling, cubic boron nitride (c-BN) single crystals synthesized under high pressure and high temperature (HPHT) are wrapped in the white film powders which are defined as growth interface. In order to make clear that the transition mechanism of c-BN single crystals, the variation of B and N atomic hybrid states in the growth interface is analyzed with the help of auger electron spectroscopy in the Li-based system. It is found that the sp2 fractions of B and N atoms decreases, and their sp3 fractions increases from the outer to the inner in the growth interface. In addition, Lithium nitride (Li3N) are not found in the growth interface by X-ray diffraction (XRD) experiment. It is suggested that lithium boron nitride (Li3BN2) is produced by the reaction of hexagonal boron nitride (h-BN) and Li3N at the first step, and then B and N atoms transform from sp2 into sp3 state with the catalysis of Li3BN2 in c-BN single crystals synthesis process.

Structural and magnetic investigations of single-crystalline neodymium zirconate pyrochlore Nd2Zr2O7

NASA Astrophysics Data System (ADS)

Hatnean, M. Ciomaga; Lees, M. R.; Petrenko, O. A.; Keeble, D. S.; Balakrishnan, G.; Gutmann, M. J.; Klekovkina, V. V.; Malkin, B. Z.

2015-05-01

We report structural and magnetic properties studies of large high-quality single crystals of the frustrated magnet Nd2Zr2O7 . Powder x-ray diffraction analysis confirms that Nd2Zr2O7 adopts the pyrochlore structure. Room-temperature x-ray diffraction and time-of-flight neutron-scattering experiments show that the crystals are stoichiometric in composition with no measurable site disorder. The temperature dependence of the magnetic susceptibility shows no magnetic ordering at temperatures down to 0.5 K. Fits to the magnetic susceptibility data using a Curie-Weiss law reveal a ferromagnetic coupling between the Nd moments. Magnetization versus field measurements show a local Ising anisotropy along the <111 > axes of the Nd3 + ions in the ground state. Specific heat versus temperature measurements in zero applied magnetic field indicate the presence of a thermal anomaly below T ˜7 K, but no evidence of magnetic ordering is observed down to 0.5 K. The experimental temperature dependence of the single-crystal bulk dc susceptibility and isothermal magnetization are analyzed using crystal field theory and the crystal field parameters and exchange coupling constants determined.

Magnetic and crystal structures of the honeycomb lattice Na2IrO3 and single layer Sr2IrO4

NASA Astrophysics Data System (ADS)

Ye, Feng

2013-03-01

5 d based iridates have recently attracted great attention due to the large spin-orbit coupling (SOC). It is now recognized that the SOC that competes with other relevant energies, particularly the on-site Coulomb interaction U, and have driven novel electronic and magnetic phases. Combining single crystal neutron and x-ray diffractions, we have investigated the magnetic and crystal structures of the honeycomb lattice Na2IrO3. The system orders magnetically below 18.1 K with Ir4+ ions forming zigzag spin chains within the layered honeycomb network with ordered moment of 0.22 μB /Ir site. Such a configuration sharply contrasts the Neel or stripe states proposed in the Kitaev-Heisenberg model. The structure refinement reveals that the Ir atoms form nearly ideal 2D honeycomb lattice while the IrO6 octahedra experience a trigonal distortion that is critical to the ground state. The results of this study provide much-needed experimental insights into the magnetic and crystal structure crucial to the understanding of the exotic magnetic order and possible topological characteristics in the 5 d-electron based honeycomb lattice. Neutron diffraction experiments are also performed to investigate the magnetic and crystal structure of the single layer iridate Sr2IrO4, where new structural information and spin order are obtained that is not available from previous neutron powder diffraction measurement. This work was sponsored in part by the Scientific User Facilities Division, Office of Basic Energy Sciences, US Department of Energy.

Force measurements in stiff, 3D, opaque granular materials

NASA Astrophysics Data System (ADS)

Hurley, Ryan C.; Hall, Stephen A.; Andrade, José E.; Wright, Jonathan

2017-06-01

We present results from two experiments that provide the first quantification of inter-particle force networks in stiff, 3D, opaque granular materials. Force vectors between all grains were determined using a mathematical optimization technique that seeks to satisfy grain equilibrium and strain measurements. Quantities needed in the optimization - the spatial location of the inter-particle contact network and tensor grain strains - were found using 3D X-ray diffraction and X-ray computed tomography. The statistics of the force networks are consistent with those found in past simulations and 2D experiments. In particular, we observe an exponential decay of normal forces above the mean and a partition of forces into strong and weak networks. In the first experiment, involving 77 single-crystal quartz grains, we also report on the temporal correlation of the force network across two sequential load cycles. In the second experiment, involving 1099 single-crystal ruby grains, we characterize force network statistics at low levels of compression.

Serial snapshot crystallography for materials science with SwissFEL

DOE PAGES

Dejoie, Catherine; Smeets, Stef; Baerlocher, Christian; ...

2015-04-21

New opportunities for studying (sub)microcrystalline materials with small unit cells, both organic and inorganic, will open up when the X-ray free electron laser (XFEL) presently being constructed in Switzerland (SwissFEL) comes online in 2017. Our synchrotron-based experiments mimicking the 4%-energy-bandpass mode of the SwissFEL beam show that it will be possible to record a diffraction pattern of up to 10 randomly oriented crystals in a single snapshot, to index the resulting reflections, and to extract their intensities reliably. The crystals are destroyed with each XFEL pulse, but by combining snapshots from several sets of crystals, a complete set of datamore » can be assembled, and crystal structures of materials that are difficult to analyze otherwise will become accessible. Even with a single shot, at least a partial analysis of the crystal structure will be possible, and with 10–50 femtosecond pulses, this offers tantalizing possibilities for time-resolved studies.« less

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Identification of Zn-vacancy-hydrogen complexes in ZnO single crystals: A challenge to positron annihilation spectroscopy

NASA Astrophysics Data System (ADS)

Brauer, G.; Anwand, W.; Grambole, D.; Grenzer, J.; Skorupa, W.; Čížek, J.; Kuriplach, J.; Procházka, I.; Ling, C. C.; So, C. K.; Schulz, D.; Klimm, D.

2009-03-01

A systematic study of various, nominally undoped ZnO single crystals, either hydrothermally grown (HTG) or melt grown (MG), has been performed. The crystal quality has been assessed by x-ray diffraction, and a comprehensive estimation of the detailed impurity and hydrogen contents by inductively coupled plasma mass spectrometry and nuclear reaction analysis, respectively, has been made also. High precision positron lifetime experiments show that a single positron lifetime is observed in all crystals investigated, which clusters at 180-182 ps and 165-167 ps for HTG and MG crystals, respectively. Furthermore, hydrogen is detected in all crystals in a bound state with a high concentration (at least 0.3at.% ), whereas the concentrations of other impurities are very small. From ab initio calculations it is suggested that the existence of Zn-vacancy-hydrogen complexes is the most natural explanation for the given experimental facts at present. Furthermore, the distribution of H at a metal/ZnO interface of a MG crystal, and the H content of a HTG crystal upon annealing and time afterward has been monitored, as this is most probably related to the properties of electrical contacts made at ZnO and the instability in p -type conductivity observed at ZnO nanorods in literature. All experimental findings and presented theoretical considerations support the conclusion that various types of Zn-vacancy-hydrogen complexes exist in ZnO and need to be taken into account in future studies, especially for HTG materials.

Accurate determination of chemical shift tensor orientations of single-crystals by solid-state magic angle spinning NMR

NASA Astrophysics Data System (ADS)

Avadhut, Yamini S.; Weber, Johannes; Schmedt auf der Günne, Jörn

2017-09-01

An improved implementation of single-crystal magic-angle-spinning (MAS) NMR is presented which gives access to chemical shift tensors both in orientation (relative to the crystal axis system) and principal axis values. For mounting arbitrary crystals inside ordinary MAS rotors, a mounting tool is described which allows to relate the crystal orientation determined by diffraction techniques to the rotor coordinate system. The crystal is finally mounted into a MAS rotor equipped with a special insert which allows a defined reorientation of the single-crystal by 90°. The approach is based on the idea that the dispersive spectra, which are obtained when applying read-pulses at specific rotor-phases, not only yield the size of the eigenvalues but also encode the orientation of the different chemical shift (rank-2) tensors. For this purpose two 2D-data sets with orthogonal crystal orientation are fitted simultaneously. The presented analysis for chemical shift tensors is supported by an analytical formula which allows fast calculation of phase and amplitude of individual spinning side-bands and by a protocol which solves the problem of finding the correct reference phase of the spectrum. Different rotor-synchronized pulse-sequences are introduced for the same reason. Experiments are performed on L-alanine and O-phosphorylethanolamine and the observed errors are analyzed in detail. The experimental data are opposed to DFT-computed chemical shift tensors which have been obtained by the extended embedded ion method.

Apparatus for single ice crystal growth from the melt.

PubMed

Zepeda, Salvador; Nakatsubo, Shunichi; Furukawa, Yoshinori

2009-11-01

A crystal growth apparatus was designed and built to study the effect of growth modifiers, antifreeze proteins and antifreeze glycoproteins (AFGPs), on ice crystal growth kinetics and morphology. We used a capillary growth technique to obtain a single ice crystal with well-defined crystallographic orientation grown in AFGP solution. The basal plane was readily observed by rotation of the capillary. The main growth chamber is approximately a 0.8 ml cylindrical volume. A triple window arrangement was used to minimize temperature gradients and allow for up to 10 mm working distance objective lens. Temperature could be established to within +/-10 mK in as little as 3.5 min and controlled to within +/-2 mK after 15 min for at least 10 h. The small volume growth chamber and fast equilibration times were necessary for parabolic flight microgravity experiments. The apparatus was designed for use with inverted and side mount configurations.

Controlled vapor crystal growth of N a4I r3O8 : A three-dimensional quantum spin liquid candidate

NASA Astrophysics Data System (ADS)

Zheng, Hong; Zhang, Junjie; Stoumpos, Constantinos C.; Ren, Yang; Chen, Yu-Sheng; Dally, Rebecca; Wilson, Stephen D.; Islam, Zahirul; Mitchell, J. F.

2018-04-01

We report the successful bulk single-crystal growth of the hyperkagome lattice iridate N a4I r3O8 (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 ions at the notionally disordered Na sites as a plausible origin for the observed superlattice.

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

Imaging photonic crystals using hemispherical digital condensers and phase-recovery techniques.

PubMed

Alotaibi, Maged; Skinner-Ramos, Sueli; Farooq, Hira; Alharbi, Nouf; Alghasham, Hawra; de Peralta, Luis Grave

2018-05-10

We describe experiments where Fourier ptychographic microscopy (FPM) and dual-space microscopy (DSM) are implemented for imaging photonic crystals using a hemispherical digital condenser (HDC). Phase-recovery imaging simulations show that both techniques should be able to image photonic crystals with a period below the Rayleigh resolution limit. However, after processing the experimental images using both phase-recovery algorithms, we found that DSM can, but FPM cannot, image periodic structures with a period below the diffraction limit. We studied the origin of this apparent contradiction between simulations and experiments, and we concluded that the occurrence of unwanted reflections in the HDC is the source of the apparent failure of FPM. We thereafter solved the problem of reflections by using a single-directional illumination source and showed that FPM can image photonic crystals with a period below the Rayleigh resolution limit.

Processing of mercurous chloride in reduced gravity

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

Watson, C.; Singh, N.; Thomas, A.

1996-12-31

In a joint experiment between the Northrop-Grumman Science and Technology Center and the University of Alabama in Huntsville, Consortium for Materials Development in Space (UAH/CMDS), single crystals of mercurous chloride (Hg{sub 2}Cl{sub 2}) were grown in the Space Experiment Facility (SEF) transparent furnace that was flown on Spacelab 4 (STS-77) in May 1996. Single crystals of this material can be readily grown in normal gravity by closed-tube physical vapor transport, but the crystals generally contain structural inhomogeneities which degrade the optical performance. The nature and cause of these defects are not completely understood, but their degree appears to correlate withmore » the Rayleigh number that characterizes the convective transport during their growth; hence, it is suspected that uncontrolled convection may play a role in the defect structure. The objective of the flight experiment was to reduce the convective flows by several orders of magnitude to see if the structural inhomogeneities can be reduced or eliminated. This paper will describe the physical and thermal properties of the SEF furnace, the ampoule design and loading procedure, and the ground testing, and will also present the preliminary flight results.« less

Microstructurally-sensitive fatigue crack nucleation in Ni-based single and oligo crystals

NASA Astrophysics Data System (ADS)

Chen, Bo; Jiang, Jun; Dunne, Fionn P. E.

2017-09-01

An integrated experimental, characterisation and computational crystal plasticity study of cyclic plastic beam loading has been carried out for nickel single crystal (CMSX4) and oligocrystal (MAR002) alloys in order to assess quantitatively the mechanistic drivers for fatigue crack nucleation. The experimentally validated modelling provides knowledge of key microstructural quantities (accumulated slip, stress and GND density) at experimentally observed fatigue crack nucleation sites and it is shown that while each of these quantities is potentially important in crack nucleation, none of them in its own right is sufficient to be predictive. However, the local (elastic) stored energy density, measured over a length scale determined by the density of SSDs and GNDs, has been shown to predict crack nucleation sites in the single and oligocrystals tests. In addition, once primary nucleated cracks develop and are represented in the crystal model using XFEM, the stored energy correctly identifies where secondary fatigue cracks are observed to nucleate in experiments. This (Griffith-Stroh type) quantity also correctly differentiates and explains intergranular and transgranular fatigue crack nucleation.

Morphology and solubility of multiple crystal forms of Taka-amylase A

NASA Astrophysics Data System (ADS)

Ninomiya, Kumiko; Yamamoto, Tenyu; Oheda, Tadashi; Sato, Kiyotaka; Sazaki, Gen; Matsuura, Yoshiki

2001-01-01

An α-amylase originating from a mold Aspergillus oryzae, Taka-amylase A (Mr of 52 kDa, pI of 3.8), has been purified to an electrophoretically single band grade. Crystallization behaviors were investigated using ammonium sulfate and polyethleneglycol 8000 as precipitants. The variations in the morphology of the crystals obtained with changing crystallization parameters are described. Five apparently different crystal forms were obtained, and their morphology and crystallographic data have been determined. Solubility values of four typical forms were measured using a Michelson-type two-beam interferometer. The results of these experiments showed that this protein can be a potentially interesting and useful model for crystal growth study with a gram-amount availability of pure protein sample.

Integrated double-clad photonic crystal fiber amplifier

NASA Astrophysics Data System (ADS)

Liu, Jun; Gu, Yanran; Chen, Zilun

2017-10-01

This paper studies and fabricates an integrated double-clad photonic crystal fiber amplifier, which overcomes the shortcomings of space application and makes full use of excellent property of double-clad photonic crystal fiber. In the experiment, the (6 + 1) × 1 end-pump coupler with DC-PCF is fabricated. The six pump fibers are fabricated with 105 / 125μm (NA = 0.22) multi-mode fiber. The signal fiber is made of ordinary single-mode fiber SMF-28. Then we spliced the tapered fiber bundle to photonic crystal fiber. At last, we produce double-clad photonic crystal fiber with an end-cap that are able to withstand high average power and protect the system. We have fabricated an integrated Yb-double-clad photonic crystal fiber amplifier.

Subsurface Growth Of Silicide Structures In Silicon

NASA Technical Reports Server (NTRS)

Fathauer, Robert W.; George, Thomas; Pike, William T.; Schowalter, Leo

1993-01-01

Technique shows promise for fabrication of novel electronic, optoelectronic, and electro-optical devices. Experiments demonstrated feasibility of growing microscopic single-crystal CoSi2 structures beneath surfaces of Si substrates.

Growth of CdZnTe Crystals for Radiation Detector Applications by Directional Solidification

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2014-01-01

Advances in Cadmium Zinc Telluride (Cd(sub 1-x)Zn(sub x)Te) growth techniques are needed for the production of large-scale arrays of gamma and x-ray astronomy. The research objective is to develop crystal growth recipes and techniques to obtain large, high quality CdZnTe single crystal with reduced defects, such as charge trapping, twinning, and tellurium precipitates, which degrade the performance of CdZnTe and, at the same time, to increase the yield of usable material from the CdZnTe ingot. A low gravity material experiment, "Crystal Growth of Ternary Compound Semiconductors in Low Gravity Environment", will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). One section of the flight experiment is the melt growth of CdZnTe ternary compounds. This talk will focus on the ground-based studies on the growth of Cd(sub 0.80)Zn(sub 0.20)Te crystals for radiation detector applications by directional solidification. In this investigation, we have improved the properties that are most critical for the detector applications (electrical properties and crystalline quality): a) Electrical resistivity: use high purity starting materials (with reproducible impurity levels) and controlled Cd over pressure during growth to reproducibly balance the impurity levels and Cd vacancy concentration b) Crystalline quality: use ultra-clean growth ampoule (no wetting after growth), optimized thermal profile and ampoule design, as well as a technique for supercool reduction to growth large single crystal with high crystalline quality

Hematite-Ilmenite with Magnetite from the Ecstall Pluton, British Columbia: Single Crystal Magnetic Experiments

NASA Astrophysics Data System (ADS)

Scott, G. R.; Brownlee, S. J.; Feinberg, J. M.; Renne, P. R.

2008-12-01

Rocks provide a compound paleomagnetic signal from mixtures of various iron minerals with different grain sizes and magnetic stabilities. To unravel this complex signal, specific mineral phases with stable remanence can be individually examined as single crystals. In the case of the Ecstall Pluton (~91 Ma), intra-pluton discordance of paleomagnetic directions may be the result of post-crystallization deformation, or mineralogical changes caused by re-heating from the adjacent Quottoon Pluton (~52 Ma). In order to distinguish between these two hypotheses we conducted rock magnetic experiments on single crystals of finely-exsolved hematite-ilmenite along a transect approaching the Quottoon Pluton. Reflected light, and SEM observations show grains of hematite and ilmenite as the dominant Fe-oxide throughout the Ecstall. Nearest the Quottoon Pluton, the hematite-ilmenite grains exhibit the classic rutile blitz texture. The lamellar microstructure observed in the hematite-ilmenite grains, as well as the rutile blitz texture are linked to the thermal history of the Ecstall Pluton, and have important effects on the magnetic properties of these grains (i.e. lamellar magnetism). Our results include the magnetic unmixing of isothermal remanence magnetization (IRM) acquisition, First Order Reversal Curve (FORC) diagrams, temperature vs. remanence experiments (MPMS), and TEM studies. These data provide a spatially resolved record of rock magnetic variations across the Ecstall Pluton, showing evidence of thermally activated reduction of hematite to magnetite in samples within 13 km of the Quottoon Pluton. TEM analysis shows the magnetite is present as 20-50 nm-sized particles within hematite. This mineralogic change may be responsible for the variations in paleomagnetic directions across the Ecstall Pluton, and clear evidence for this reaction cannot be found by traditional rock characterization techniques, illustrating the need to couple detailed rock magnetic, paleomagnetic, and mineralogic analyses.

Effect of water on olivine single crystal plasticity, deformed under upper mantle condition

NASA Astrophysics Data System (ADS)

Girard, J.; Chen, J.; Raterron, P. C.; Holyoke, C. W.

2011-12-01

The earth upper mantle, mainly composed of olivine, is seismically anisotropic. Seismic anisotropy attenuation has been observed at 200km depth. Karato et al. (1992) attributed this attenuation to a transition between two deformation mechanisms, from dislocation creep above 200km to diffusion creep bellow 200km. This transition occurs because of hydroxyl concentration. Mainprice et al.(2005) predicted a change in LPO induced by a change of slip system, from [100] slip to [001] slip, though theoritical modeling. According to his study, pressure is the parameter inducing the slip system transition, which is responsible for the seismic anisotropy attenuation. Raterron et al. (2007) performed single crystal deformation experiment under anhydrous conditions and observe that slip system transition occurring around 8 GPa. However this pressure would correspond to 300km depth which doesn't match the seismic anisotropy attenuation depth, observed by seismologist. In this study, experiments have been performed to quantify the effects of water on olivine single crystals deformed using Deformation DIA press and synchrotron beam. Deformation was carried out in uniaxial compression along the so-called [110]c and [011]c crystallographic direction in order to activate [100](010) and [001](010) dislocation slip system respectively, at P ranging from 4 to 8GPa and T=1200°C. Both single crystals were loaded in the cell to directly compare their deformation in same condition of stress temperature and pressure. We used a sleeve (talc = enstatite + coesite + H2O) about the annulus of the single crystals as source of water in the assembly. Stress and specimen strain rates were calculated by in-situ X-ray diffraction and time resolved imaging, respectively. By direct comparison of single crystals strain rates, we observed that [110]c deform faster than [011]c bellow 5GPa. However above 6GPa [011]c deform faster. This revealed that [100](010) is the dominant slip system bellow 5GPa, and [001](010) becomes dominant above 6GPa. Thus, we observe a slip system switch over at about 5-6GPa in wet condition. This slip system switch over will result in change of lattice preferred orientation in olivine, from [100] slip to [001] slip, and therefore reduce seismic anisotropy attenuation down to 1.9% (Mainprice et al.,2005). According to our results, the slip system transition is induced by pressure, and water influences the pressure where the switch over occurs. These results not only can explain the depth where the seismic anisotropy attenuation (i.e. 200 km, corresponding to 6GPa) but also can help to understand the regional variation of the depth, as local hydroxyl contents in the mantle may varies significantly. TEM investigation and water content measurement of recovered specimens from the deformation experiments will also be discussed.

Crystallization of the collagen-like polypeptide (PPG)10 aboard the International Space Station. 1. Video observation.

PubMed

Vergara, Alessandro; Corvino, Ermanno; Sorrentino, Giosué; Piccolo, Chiara; Tortora, Alessandra; Carotenuto, Luigi; Mazzarella, Lelio; Zagari, Adriana

2002-10-01

Single chains of the collagen model polypeptide with sequence (Pro-Pro-Gly)(10), hereafter referred to as (PPG)(10), aggregate to form rod-shaped triple helices. Crystals of (PPG)(10) were grown in the Advanced Protein Crystallization Facility (APCF) both onboard the International Space Station (ISS) and on Earth. The experiments allow the direct comparison of four different crystallization environments for the first time: solution in microgravity ((g), agarose gel in (g, solution on earth, and gel on earth. Both on board and on ground, the crystal growth was monitored by a CCD video camera. The image analysis provided information on the spatial distribution of the crystals, their movement and their growth rate. The analysis of the distribution of crystals reveals that the crystallization process occurs as it does in batch conditions. Slow motions have been observed onboard the ISS. Different to Space-Shuttle experiment, the crystals onboard the ISS moved coherently and followed parallel trajectories. Growth rate and induction time are very similar both in gel and in solution, suggesting that the crystal growth rate is controlled by the kinetics at the interface under the used experimental conditions. These results provide the first data in the crystallogenesis of (PPG)(10), which is a representative member of non-globular, rod-like proteins.

Towards establishing a combined rate law of nucleation and crystal growth - The case study of gypsum precipitation

NASA Astrophysics Data System (ADS)

Rendel, Pedro M.; Gavrieli, Ittai; Wolff-Boenisch, Domenik; Ganor, Jiwchar

2018-03-01

The main obstacle in the formulation of a quantitative rate-model for mineral precipitation is the absence of a rigorous method for coupling nucleation and growth processes. In order to link both processes, we conducted a series of batch experiments in which gypsum nucleation was followed by crystal growth. Experiments were carried out using various stirring methods in several batch vessels made of different materials. In the experiments, the initial degree of supersaturation of the solution with respect to gypsum (Ωgyp) was set between 1.58 and 1.82. Under these conditions, heterogeneous nucleation is the dominant nucleation mode. Based on changes in SO42- concentration with time, the induction time of gypsum nucleation and the following rate of crystal growth were calculated for each experiment. The induction time (6-104 h) was found to be a function of the vessel material, while the rates of crystal growth, which varied over three orders of magnitude, were strongly affected by the stirring speed and its mode (i.e. rocking, shaking, magnetic stirrer, and magnetic impeller). The SO42- concentration data were then used to formulate a forward model that couples the simple rate laws for nucleation and crystal growth of gypsum into a single kinetic model. Accordingly, the obtained rate law is based on classical nucleation theory and heterogeneous crystal growth.

Three-Dimensional Stress Fields and Slip Systems for Single Crystal Superalloy Notched Specimens

NASA Technical Reports Server (NTRS)

Magnan, Shannon M.; Throckmorton, David (Technical Monitor)

2002-01-01

Single crystal superalloys have become increasingly popular for turbine blade and vane applications due to their high strength, and creep and fatigue resistance at elevated temperatures. The crystallographic orientation of a single crystal material greatly affects its material properties, including elastic modulus, shear modulus, and ductility. These directional properties, along with the type of loading and temperature, dictate an anisotropic response in the yield strength, creep resistance, creep rupture ductility, fatigue resistance, etc. A significant amount of research has been conducted to determine the material properties in the <001> orientation, yet the material properties deviating from the <001> orientation have not been assessed for all cases. Based on the desired application and design criteria, a crystal orientation is selected to yield the maximum properties. Currently, single crystal manufacturing is able to control the primary crystallographic orientation within 15 of the target orientation, which is an acceptable deviation to meet both performance and cost guidelines; the secondary orientation is rarely specified. A common experiment is the standard load-controlled tensile test, in which specimens with different orientations can be loaded to observe the material response. The deformation behavior of single-crystal materials under tension and compression is known to be a function of not only material orientation, but also of varying microdeformation (i.e. dislocation) mechanisms. The underlying dislocation motion causes deformation via slip, and affects the activation of specific slip systems based on load and orientation. The slip can be analyzed by observing the visible traces left on the surface of the specimen from the slip activity within the single crystal material. The goal of this thesis was to predict the slip systems activated in three-dimensional stress fields of a notched tensile specimen, as a function of crystal orientation, using finite element analysis without addressing microstructural deformation mechanisms that govern their activation. Out of three orientations tested, the specimen with a [110] load orientation and a [001] growth direction had the lowest maximum resolved shear stress; this specimen orientation appears to be the best design candidate for a tensile application.

Structural study of quasi-one-dimensional vanadium pyroxene LiVSi{sub 2}O{sub 6} single crystals

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

Ishii, Yuto; Matsushita, Yoshitaka; Oda, Migaku

Single crystals of quasi-one-dimensional vanadium pyroxene LiVSi{sub 2}O{sub 6} were synthesized and the crystal structures at 293 K and 113 K were studied using X-ray diffraction experiments. We found a structural phase transition from the room-temperature crystal structure with space group C2/c to a low-temperature structure with space group P2{sub 1}/c, resulting from a rotational displacement of SiO{sub 4} tetrahedra. The temperature dependence of magnetic susceptibility shows a broad maximum around 116 K, suggesting an opening of the Haldane gap expected for one-dimensional antiferromagnets with S=1. However, an antiferromagnetic long-range order was developed below 24 K, probably caused by amore » weak inter-chain magnetic coupling in the compound. - Graphical abstract: Low temperature crystal structure of LiVSi{sub 2}O{sub 6} and an orbital arrangement within the V-O zig-zag chain along the c-axis. - Highlights: • A low temperature structure of LiVSi{sub 2}O{sub 6} was determined by single crystal X-ray diffraction measurements. • The origin of the structural transition is a rotational displacement of SiO{sub 4} tetrahedra. • The uniform orbital overlap in the V-O zigzag chain makes the system a quasi one-dimensional antiferromagnet.« less

Mercury-cadmium-telluride - Technical significance and microgravity relevance related to crystal growth

NASA Astrophysics Data System (ADS)

Walcher, H.; Diehl, R.; Baars, J.

The technical importance of the mixed-crystal system Hg(1-x)Cd(x)Te (MCT) is related to a growing interest in detector devices for the infrared spectral ranges of the two atmospheric 'windows'. Applications are not restricted to the military sector, but are also related to astronomy, archeology, medicine, construction engineering, fire fighting, and the determination of pollutants in the atmosphere. It is found that MCT is uniquely qualified for the considered applications, because no other material combines, in the same way, all the required characteristics. However, problems arise in connection with the need for pure, homogeneous, single crystals of adequate size, which are free of any defects. The best results in attempts to grow such crystals have been obtained in experiments utilizing the traveling heater method (THM). Remaining difficulties are caused by effects of gravity. It is, therefore, expected that the crystals needed can be produced under conditions of microgravity. Suitable experiments for exploring this possibility are discussed.

III-V semiconductor solid solution single crystal growth

NASA Technical Reports Server (NTRS)

Gertner, E. R.

1982-01-01

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

High pressure phase transitions in lawsonite at simultaneous high pressure and temperature: A single crystal study

NASA Astrophysics Data System (ADS)

O'Bannon, E. F., III; Vennari, C.; Beavers, C. C. G.; Williams, Q. C.

2015-12-01

Lawsonite (CaAl2Si2O7(OH)2.H2O) is a hydrous mineral with a high overall water content of ~11.5 wt.%. It is a significant carrier of water in subduction zones to depths greater than ~150 km. The structure of lawsonite has been extensively studied under room temperature, high-pressure conditions. However, simultaneous high-pressure and high-temperature experiments are scarce. We have conducted synchrotron-based simultaneous high-pressure and temperature single crystal experiments on lawsonite up to a maximum pressure of 8.4 GPa at ambient and high temperatures. We used a natural sample of lawsonite from Valley Ford, California (Sonoma County). At room pressure and temperature lawsonite crystallizes in the orthorhombic system with Cmcm symmetry. Room temperature compression indicates that lawsonite remains in the orthorhombic Cmcm space group up to ~9.0 GPa. Our 5.0 GPa crystal structure is similar to the room pressure structure, and shows almost isotropic compression of the crystallographic axes. Unit cell parameters at 5.0 GPa are a- 5.7835(10), b- 8.694(2), and c- 13.009(3). Single-crystal measurements at simultaneous high-pressure and temperature (e.g., >8.0 GPa and ~100 oC) can be indexed to a monoclinic P-centered unit cell. Interestingly, a modest temperature increase of ~100 oC appears to initiate the orthorhombic to monoclinic phase transition at ~0.6-2.4 GPa lower than room temperature compression studies have shown. There is no evidence of dehydration or H atom disorder under these conditions. This suggests that the orthorhombic to monoclinic transition could be kinetically impeded at 298 K, and that monoclinic lawsonite could be the dominant water carrier through much of the depth range of upper mantle subduction processes.

Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto.

PubMed

Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

2010-12-01

Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27,724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a=74.3, b=49.9, c=56.3 Å, β=95.2°. Diffraction images were processed to a resolution of 1.74 Å with an Rmerge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase.

Purification, crystallization and preliminary X-ray diffraction experiment of nattokinase from Bacillus subtilis natto

PubMed Central

Yanagisawa, Yasuhide; Chatake, Toshiyuki; Chiba-Kamoshida, Kaori; Naito, Sawa; Ohsugi, Tadanori; Sumi, Hiroyuki; Yasuda, Ichiro; Morimoto, Yukio

2010-01-01

Nattokinase is a single polypeptide chain composed of 275 amino acids (molecular weight 27 724) which displays strong fibrinolytic activity. Moreover, it can activate other fibrinolytic enzymes such as pro-urokinase and tissue plasminogen activator. In the present study, native nattokinase from Bacillus subtilis natto was purified using gel-filtration chromatography and crystallized to give needle-like crystals which could be used for X-ray diffraction experiments. The crystals belonged to space group C2, with unit-cell parameters a = 74.3, b = 49.9, c = 56.3 Å, β = 95.2°. Diffraction images were processed to a resolution of 1.74 Å with an R merge of 5.2% (15.3% in the highest resolution shell) and a completeness of 69.8% (30.0% in the highest resolution shell). This study reports the first X-ray diffraction analysis of nattokinase. PMID:21139221

OZSPEC-2: an improved broadband high-resolution elliptical crystal x-ray spectrometer for high-energy density physics experiments (invited).

PubMed

Heeter, R F; Anderson, S G; Booth, R; Brown, G V; Emig, J; Fulkerson, S; McCarville, T; Norman, D; Schneider, M B; Young, B K F

2008-10-01

A novel time, space, and energy-resolved x-ray spectrometer has been developed which produces, in a single snapshot, a broadband and relatively calibrated spectrum of the x-ray emission from a high-energy density laboratory plasma. The opacity zipper spectrometer (OZSPEC-1) records a nearly continuous spectrum for x-ray energies from 240 to 5800 eV in a single shot. The second-generation OZSPEC-2, detailed in this work, records fully continuous spectra on a single shot from any two of these three bands: 270-650, 660-1580, and 1960-4720 eV. These instruments thus record thermal and line radiation from a wide range of plasmas. These instruments' single-shot bandwidth is unmatched in a time-gated spectrometer; conversely, other broadband instruments are either time-integrated (using crystals or gratings), lack spectral resolution (diode arrays), or cover a lower energy band (gratings). The OZSPECs are based on the zipper detector, a large-format (100x35 mm) gated microchannel plate detector, with spectra dispersed along the 100 mm dimension. OZSPEC-1 and -2 both use elliptically bent crystals of OHM, RAP, and/or PET. Individual spectra are gated in 100 ps. OZSPEC-2 provides one-dimensional spatial imaging with 30-50 microm resolution over a 1500 microm field of view at the source. The elliptical crystal design yields broad spectral coverage with resolution E/DeltaE>500, strong rejection of hard x-ray backgrounds, and negligible source broadening for extended sources. Near-term applications include plasma opacity measurements, detailed spectra of inertial fusion Hohlraums, and laboratory astrophysics experiments.

Temperature dependent evolution of wrinkled single-crystal silicon ribbons on shape memory polymers.

PubMed

Wang, Yu; Yu, Kai; Qi, H Jerry; Xiao, Jianliang

2017-10-25

Shape memory polymers (SMPs) can remember two or more distinct shapes, and thus can have a lot of potential applications. This paper presents combined experimental and theoretical studies on the wrinkling of single-crystal Si ribbons on SMPs and the temperature dependent evolution. Using the shape memory effect of heat responsive SMPs, this study provides a method to build wavy forms of single-crystal silicon thin films on top of SMP substrates. Silicon ribbons obtained from a Si-on-insulator (SOI) wafer are released and transferred onto the surface of programmed SMPs. Then such bilayer systems are recovered at different temperatures, yielding well-defined, wavy profiles of Si ribbons. The wavy profiles are shown to evolve with time, and the evolution behavior strongly depends on the recovery temperature. At relatively low recovery temperatures, both wrinkle wavelength and amplitude increase with time as evolution progresses. Finite element analysis (FEA) accounting for the thermomechanical behavior of SMPs is conducted to study the wrinkling of Si ribbons on SMPs, which shows good agreement with experiment. Merging of wrinkles is observed in FEA, which could explain the increase of wrinkle wavelength observed in the experiment. This study can have important implications for smart stretchable electronics, wrinkling mechanics, stimuli-responsive surface engineering, and advanced manufacturing.

The effect of surface conditions on the work function of insulators and semiconductors

NASA Technical Reports Server (NTRS)

George, A.

1973-01-01

Ionization energies of organic semiconductors were determined using single crystals of the material. The theory of the method is essentially that of Millikan's oil drop experiment. The technique employed in the experiment is based on the electrostatic method of balancing a charged particle in an electric field against the force of gravity for different excitation energies above the threshold value, and from an estimate of the balancing voltages, read off the ionization energy from the intercept of the energy axis in a plot wavelength corresponding to the balancing potential for the incident radiation of wavelength. In the modified technique which is adopted in the present experimental investigation, a small single crystal is suspended by a fine quartz fiber between two vertical capacitor plates to which a suitable high voltage is applied.

Adhesion and friction of iron and gold in contact with elemental semiconductors

NASA Technical Reports Server (NTRS)

Buckley, D. H.; Brainard, W. A.

1977-01-01

Adhesion and friction experiments were conducted with single crystals of iron and gold in contact with single crystals of germanium and silicon. Surfaces were examined in the sputter cleaned state and in the presence of oxygen and a lubricant. All experiments were conducted at room temperature with loads of 1 to 50 grams, and sliding friction was at a sliding velocity of 0.7 mm/min. Results indicate that the friction nature of metals in contact with semiconductors is sensitive to orientation, that strong adhesion of metals to both germanium and silicon occurs, and that friction is lower with silicon than with germanium for the same orientation. Surface effects are highly sensitive to environment. Silicon, for example, behaves in an entirely brittle manner in the clean state, but in the presence of a lubricant the surface deforms plastically.

Beryllium, zinc and lead single crystals as a thermal neutron monochromators

NASA Astrophysics Data System (ADS)

Adib, M.; Habib, N.; Bashter, I. I.; Morcos, H. N.; El-Mesiry, M. S.; Mansy, M. S.

2015-03-01

The monochromatic features of Be, Zn and Pb single crystals are discussed in terms of orientation, mosaic spread, and thickness within the wavelength band from 0.04 up to 0.5 nm. A computer program MONO written in "FORTRAN-77", has been adapted to carry out the required calculations. Calculations show that a 5 mm thick of beryllium (HCP structure) single crystal cut along its (0 0 2) plane having 0.6° FWHM are the optimum parameters when it is used as a monochromator with high reflected neutron intensity from a thermal neutron flux. Furthermore, at wavelengths shorter than 0.16 nm it is free from the accompanying higher order ones. Zinc (HCP structure) has the same parameters, with intensity much less than the latter. The same features are seen with lead (FCC structure) cut along its (3 1 1) plane with less reflectivity than the former. However, Pb (3 1 1) is more preferable than others at neutron wavelengths ⩽ 0.1 nm, since the glancing angle (θ ∼ 20°) is more suitable to carry out diffraction experiments. For a cold neutron flux, the first-order neutrons reflected from beryllium is free from the higher orders up to 0.36 nm. While for Zn single crystal is up to 0.5 nm.

Pink-beam serial crystallography

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

Meents, A.; Wiedorn, M. O.; Srajer, V.

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Pink-beam serial crystallography

DOE PAGES

Meents, A.; Wiedorn, M. O.; Srajer, V.; ...

2017-11-03

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized formore » very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.« less

Analysis of Shock Compression of Strong Single Crystals With Logarithmic Thermoelastic-Plastic Theory

DTIC Science & Technology

2014-05-01

Royal Society of London Series A, 465, 307–334. Clayton, J. (2010a). Modeling nonlinear electromechanical behavior of shocked silicon carbide . Journal...and fourth-order longitudinal elastic constants by shock compression techniques–application to sapphire and fused quartz. Journal of the Acoustical...Vogler, T., & Clayton, J. (2008). Heterogeneous deformation and spall of an extruded tungsten alloy: Plate impact experiments and crystal plasticity

OSL studies of alkali fluoroperovskite single crystals for radiation dosimetry

NASA Astrophysics Data System (ADS)

Daniel, D. Joseph; Raja, A.; Madhusoodanan, U.; Annalakshmi, O.; Ramasamy, P.

2016-08-01

This paper presents a preliminary investigation of the optically stimulated luminescence (OSL) of alkali fluoroperovskite single crystals for radiation dosimetry. The perovskite-like KMgF3, NaMgF3 and LiBaF3 polycrystalline compounds doped with rare earths (Eu2+ and Ce3+) were synthesized by standard solid state reaction technique. Phase purity of the synthesized compounds was analyzed by powder X-ray diffraction technique. Single crystals of these compounds have been grown from melt by using vertical Bridgman-Stockbarger method. The Linearly Modulated OSL and Continuous Wave OSL measurements were performed in these alkali fluorides using blue light stimulation. Thermal bleaching experiments have shown that OSL signals originate from traps which are unstable near 200 °C, thus proving the suitability of the signals for dosimetric purposes. Optical bleaching measurements were also performed for these fluoride samples. OSL dose response was studied as a function of dose which was found to increase with beta dose.

MHz rate and efficient synchronous heralding of single photons at telecom wavelengths.

PubMed

Pomarico, Enrico; Sanguinetti, Bruno; Guerreiro, Thiago; Thew, Rob; Zbinden, Hugo

2012-10-08

We report on the realization of a synchronous source of heralded single photons at telecom wavelengths with MHz heralding rates and high heralding efficiency. This source is based on the generation of photon pairs at 810 and 1550 nm via Spontaneous Parametric Down Conversion (SPDC) in a 1 cm periodically poled lithium niobate (PPLN) crystal pumped by a 532 nm pulsed laser. As high rates are fundamental for multi-photon experiments, we show that single telecom photons can be announced at 4.4 MHz rate with 45% heralding efficiency. When we focus only on the optimization of the coupling of the heralded photon, the heralding efficiency can be increased up to 80%. Furthermore, we experimentally observe that group velocity mismatch inside long crystals pumped in a pulsed mode affects the spectrum of the emitted photons and their fibre coupling efficiency. The length of the crystal in this source has been chosen as a trade off between high brightness and high coupling efficiency.

Deformation and fracture of single-crystal and sintered polycrystalline silicon carbide produced by cavitation

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Hattori, Shuji; Okada, Tsunenori; Buckley, Donald H.

1987-01-01

An investigation was conducted to examine the deformation and fracture behavior of single-crystal and sintered polycrystalline SiC surfaces exposed to cavitation. Cavitation erosion experiments were conducted in distilled water at 25 C by using a magnetostrictive oscillator in close proximity (1 mm) to the surface of SiC. The horn frequency was 20 kHz, and the double amplitude of the vibrating disk was 50 microns. The results of the investigation indicate that the SiC (0001) surface could be deformed in a plastic manner during cavitation. Dislocation etch pits were formed when the surface was chemically etched. The number of defects, including dislocations in the SiC (0001) surface, increased with increasing exposure time to cavitation. The presence of intrinsic defects such as voids in the surficial layers of the sintered polycrystalline SiC determined the zones at which fractured grains and fracture pits (pores) were generated. Single-crystal SiC had superior erosion resistance to that of sintered polycrystalline SiC.

Deformation and fracture of single-crystal and sintered polycrystalline silicon carbide produced by cavitation

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa; Hattori, Shuji; Okada, Tsunenori; Buckley, Donald H.

1989-01-01

An investigation was conducted to examine the deformation and fracture behavior of single-crystal and sintered polycrystalline SiC surfaces exposed to cavitation. Cavitation erosion experiments were conducted in distilled water at 25 C by using a magnetostrictive oscillator in close proximity (1 mm) to the surface of SiC. The horn frequency was 20 kHz, and the double amplitude of the vibrating disk was 50 microns. The results of the investigation indicate that the SiC (0001) surface could be deformed in a plastic manner during cavitation. Dislocation etch pits were formed when the surface was chemically etched. The number of defects, including dislocations in SiC (0001) surface, increased with increasing exposure time to cavitation. The presence of intrinsic defects such as voids in the surficial layers of the sintered polycrystalline SiC determined the zones at which fractured grains and fracture pits (pores) were generated. Single-crystal SiC had superior erosion resistance to that of sintered polycrystalline SiC.

Experiment and density functional theory analyses of GdTaO4 single crystal

NASA Astrophysics Data System (ADS)

Ding, Shoujun; Kinross, Ashlie; Wang, Xiaofei; Yang, Huajun; Zhang, Qingli; Liu, Wenpeng; Sun, Dunlu

2018-05-01

GdTaO4 is a type of excellent materials that can be used as scintillation, laser matrix as well as self-activated phosphor has generated significant interest. Whereas its band structure, electronic structure and optical properties are still need elucidation. To solve this intriguing problem, high-quality GdTaO4 single crystal (M-type) was grown successfully using Czochralski method. Its structure as well as optical properties was determined in experiment. Moreover, a systematic theoretical calculation based on the density function theory methods were performed on M-type and M‧-type GdTaO4 and their band structure, density of state as well as optical properties were obtained. Combine with the performed experiment results, the calculated results were proved with high reliability. Hence, the calculated results obtained in this work could provide a deep understanding of GdTaO4 material, which also useful for the further investigation on GdTaO4 material.

Study of temperature-dependent Raman spectroscopy and electrical properties in [001]-oriented 0.35Pb(In1/2Nb1/2)O3-0.35Pb(Mg1/3Nb2/3)O3-0.30PbTiO3-Mn single crystals

NASA Astrophysics Data System (ADS)

Liu, Xing; Fang, Bijun; Deng, Ji; Yan, Hong; Deng, Hao; Yue, Qingwen; Ding, Jianning; Zhao, Xiangyong; Luo, Haosu

2016-01-01

In this work, the temperature-dependent Raman spectra and electrical properties of the [001]-oriented 0.5 mol. % Mn-doped 0.35Pb(In1/2Nb1/2)O3-0.35Pb(Mg1/3Nb2/3)O3-0.30PbTiO3-Mn (PIMNT-Mn) single crystals were investigated. All the unpoled and poled PIMNT-Mn single crystals experience a ferroelectric tetragonal phase to paraelectric cubic phase transition (FET-PC) around 183 °C (TC), which exhibits a second-order transition behavior. Whereas, the poled PIMNT-Mn single crystals exhibit another two dielectric anomalies around 130 °C (TRM) and 148 °C (TMT), in which the ferroelectric rhombohedral phase to ferroelectric monoclinic phase (FER-FEM) and the ferroelectric monoclinic phase to ferroelectric tetragonal phase (FEM-FET) transitions take place, respectively. Both the two ferroelectric phase transitions exhibit a first-order transition behavior. The discontinuous change of the phase degree (θ) and frequencies (fr and fa) around TRM suggest the occurrence of the FER-FEM phase transition in the poled PIMNT-Mn single crystals. The narrowing of the 510 cm-1 and 582 cm-1 Raman modes around the TRM, TMT, and TC temperatures shown in the temperature-dependent Raman spectra suggests their increased ordering of the local structure. The intensity ratio of I272 cm-1/I801 cm-1 increases obviously around the phase transition temperatures (TRM, TMT, and TC), indicating the reduction of the long-range order. The anomalous broadening of the 272 cm-1 Raman mode around the TRM, TMT, and TC temperatures indicates the occurrence of the successive ferroelectric phase transitions (FER-FEM, FEM-FET, and FET-PC) with increasing temperature in the poled PIMNT-Mn single crystals.

Sponge-like nanoporous single crystals of gold

PubMed Central

Khristosov, Maria Koifman; Bloch, Leonid; Burghammer, Manfred; Kauffmann, Yaron; Katsman, Alex; Pokroy, Boaz

2015-01-01

Single crystals in nature often demonstrate fascinating intricate porous morphologies rather than classical faceted surfaces. We attempt to grow such crystals, drawing inspiration from biogenic porous single crystals. Here we show that nanoporous single crystals of gold can be grown with no need for any elaborate fabrication steps. These crystals are found to grow following solidification of a eutectic composition melt that forms as a result of the dewetting of nanometric thin films. We also present a kinetic model that shows how this nano-porous single-crystalline structure can be obtained, and which allows the potential size of the porous single crystal to be predicted. Retaining their single-crystalline nature is due to the fact that the full crystallization process is faster than the average period between two subsequent nucleation events. Our findings clearly demonstrate that it is possible to form single-crystalline nano porous metal crystals in a controlled manner. PMID:26554856

High-pressure crystallography of periodic and aperiodic crystals

PubMed Central

Hejny, Clivia; Minkov, Vasily S.

2015-01-01

More than five decades have passed since the first single-crystal X-ray diffraction experiments at high pressure were performed. These studies were applied historically to geochemical processes occurring in the Earth and other planets, but high-pressure crystallography has spread across different fields of science including chemistry, physics, biology, materials science and pharmacy. With each passing year, high-pressure studies have become more precise and comprehensive because of the development of instrumentation and software, and the systems investigated have also become more complicated. Starting with crystals of simple minerals and inorganic compounds, the interests of researchers have shifted to complicated metal–organic frameworks, aperiodic crystals and quasicrystals, molecular crystals, and even proteins and viruses. Inspired by contributions to the microsymposium ‘High-Pressure Crystallography of Periodic and Aperiodic Crystals’ presented at the 23rd IUCr Congress and General Assembly, the authors have tried to summarize certain recent results of single-crystal studies of molecular and aperiodic structures under high pressure. While the selected contributions do not cover the whole spectrum of high-pressure research, they demonstrate the broad diversity of novel and fascinating results and may awaken the reader’s interest in this topic. PMID:25866659

7 Å resolution in protein two-dimensional-crystal X-ray diffraction at Linac Coherent Light Source

PubMed Central

Pedrini, Bill; Tsai, Ching-Ju; Capitani, Guido; Padeste, Celestino; Hunter, Mark S.; Zatsepin, Nadia A.; Barty, Anton; Benner, W. Henry; Boutet, Sébastien; Feld, Geoffrey K.; Hau-Riege, Stefan P.; Kirian, Richard A.; Kupitz, Christopher; Messerschmitt, Marc; Ogren, John I.; Pardini, Tommaso; Segelke, Brent; Williams, Garth J.; Spence, John C. H.; Abela, Rafael; Coleman, Matthew; Evans, James E.; Schertler, Gebhard F. X.; Frank, Matthias; Li, Xiao-Dan

2014-01-01

Membrane proteins arranged as two-dimensional crystals in the lipid environment provide close-to-physiological structural information, which is essential for understanding the molecular mechanisms of protein function. Previously, X-ray diffraction from individual two-dimensional crystals did not represent a suitable investigational tool because of radiation damage. The recent availability of ultrashort pulses from X-ray free-electron lasers (XFELs) has now provided a means to outrun the damage. Here, we report on measurements performed at the Linac Coherent Light Source XFEL on bacteriorhodopsin two-dimensional crystals mounted on a solid support and kept at room temperature. By merging data from about a dozen single crystal diffraction images, we unambiguously identified the diffraction peaks to a resolution of 7 Å, thus improving the observable resolution with respect to that achievable from a single pattern alone. This indicates that a larger dataset will allow for reliable quantification of peak intensities, and in turn a corresponding increase in the resolution. The presented results pave the way for further XFEL studies on two-dimensional crystals, which may include pump–probe experiments at subpicosecond time resolution. PMID:24914166

Frictional properties of single crystals HMX, RDX and PETN explosives.

PubMed

Wu, Y Q; Huang, F L

2010-11-15

The frictional properties of single crystals of cyclotetramethylene tetranitramine (HMX), cyclotrimethylene trinitramine (RDX) and pentaerythritol tetranitrate (PETN) secondary explosives are examined using a sensitive friction machine. The explosive crystals used for the measurements are at least 3.5 mm wide. The friction coefficients between crystals of the same explosive (i.e., HMX on HMX, etc.), crystals of different explosives (i.e., HMX on RDX, etc.), and each explosive and a well-polished gauge steel surface are determined. The frictional surfaces are also studied under an environmental scanning electron microscope (ESEM) to analyze surface microstructural changes under increasing loading forces. The friction coefficients vary considerably with increasing normal loading forces and are particularly sensitive to slider shapes, crystal roughness and the mechanical properties of both the slider and the sample. With increasing loading forces, most friction experiments show surface damage, consisting of grooves, debris, and nano-particles, on both the slider and sample. In some cases, a strong evidence of a localized molten state is found in the central region of the friction track. Possible mechanisms that affect the friction coefficient are discussed based on microscopic observations. Copyright © 2010 Elsevier B.V. All rights reserved.

Assessment of In Situ Time Resolved Shock Experiments at Synchrotron Light Sources*

NASA Astrophysics Data System (ADS)

Belak, J.; Ilavsky, J.; Hessler, J. P.

2005-07-01

Prior to fielding in situ time resolved experiments of shock wave loading at the Advanced Photon Source, we have performed feasibility experiments assessing a single photon bunch. Using single and poly-crystal Al, Ti, V and Cu shock to incipient spallation on the gas gun, samples were prepared from slices normal to the spall plane of thickness 100-500 microns. In addition, single crystal Al of thickness 500 microns was shocked to incipient spallation and soft recovered using the LLNL e-gun mini-flyer system. The e-gun mini-flyer impacts the sample target producing a 10's ns flat-top shock transient. Here, we present results for imaging, small-angle scattering (SAS), and diffraction. In particular, there is little SAS away from the spall plane and significant SAS at the spall plane, demonstrating the presence of sub-micron voids. * Use of the Advanced Photon Source was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. W-31-109-Eng-38 and work performed under the auspices of the U.S. Department of Energy by University of California, Lawrence Livermore National Laboratory under Contract W-7405-Eng-48.

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

NASA Technical Reports Server (NTRS)

Gertner, E. R.

1980-01-01

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

Strain Coupling of a Nitrogen-Vacancy Center Spin to a Diamond Mechanical Oscillator

NASA Astrophysics Data System (ADS)

Teissier, J.; Barfuss, A.; Appel, P.; Neu, E.; Maletinsky, P.

2014-07-01

We report on single electronic spins coupled to the motion of mechanical resonators by a novel mechanism based on crystal strain. Our device consists of single-crystal diamond cantilevers with embedded nitrogen-vacancy center spins. Using optically detected electron spin resonance, we determine the unknown spin-strain coupling constants and demonstrate that our system resides well within the resolved sideband regime. We realize coupling strengths exceeding 10 MHz under mechanical driving and show that our system has the potential to reach strong coupling. Our novel hybrid system forms a resource for future experiments on spin-based cantilever cooling and coherent spin-oscillator coupling.

Dynamic creation and evolution of gradient nanostructure in single-crystal metallic microcubes

NASA Astrophysics Data System (ADS)

Thevamaran, Ramathasan; Lawal, Olawale; Yazdi, Sadegh; Jeon, Seog-Jin; Lee, Jae-Hwang; Thomas, Edwin L.

2016-10-01

We demonstrate the dynamic creation and subsequent static evolution of extreme gradient nanograined structures in initially near-defect-free single-crystal silver microcubes. Extreme nanostructural transformations are imposed by high strain rates, strain gradients, and recrystallization in high-velocity impacts of the microcubes against an impenetrable substrate. We synthesized the silver microcubes in a bottom-up seed-growth process and use an advanced laser-induced projectile impact testing apparatus to selectively launch them at supersonic velocities (~400 meters per second). Our study provides new insights into the fundamental deformation mechanisms and the effects of crystal and sample-shape symmetries resulting from high-velocity impacts. The nanostructural transformations produced in our experiments show promising pathways to developing gradient nanograined metals for engineering applications requiring both high strength and high toughness—for example, in structural components of aircraft and spacecraft.

Spectroscopic study of shock-induced decomposition in ammonium perchlorate single crystals.

PubMed

Gruzdkov, Y A; Winey, J M; Gupta, Y M

2008-05-01

Time-resolved Raman scattering measurements were performed on ammonium perchlorate (AP) single crystals under stepwise shock loading. For particular temperature and pressure conditions, the intensity of the Raman spectra in shocked AP decayed exponentially with time. This decay is attributed to shock-induced chemical decomposition in AP. A series of shock experiments, reaching peak stresses from 10-18 GPa, demonstrated that higher stresses inhibit decomposition while higher temperatures promote it. No orientation dependence was found when AP crystals were shocked normal to the (210) and (001) crystallographic planes. VISAR (velocity interferometer system for any reflector) particle velocity measurements and time-resolved optical extinction measurements carried out to verify these observations are consistent with the Raman data. The combined kinetic and spectroscopic results are consistent with a proton-transfer reaction as the first decomposition step in shocked AP.

Protein crystal structure from non-oriented, single-axis sparse X-ray data

DOE PAGES

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.; ...

2016-01-01

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

Protein crystal structure from non-oriented, single-axis sparse X-ray data

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

Wierman, Jennifer L.; Lan, Ti-Yen; Tate, Mark W.

X-ray free-electron lasers (XFELs) have inspired the development of serial femtosecond crystallography (SFX) as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR) sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that aremore » kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using theEMCalgorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL) crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ~200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using theEMCalgorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. In conclusion, this suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of theEMCalgorithm even in cases where the data are sparse.« less

A combined crystallographic, thermal, Raman and computational study on polymorphism and phase transition in 1-(4-hexyloxy-3-hydroxyphenyl)ethanone.

PubMed

Suárez, Sebastián; Manzano, Veronica E; Fantoni, Adolfo C; Halac, Emilia; Baggio, Ricardo; Cukiernik, Fabio D

2017-12-01

The crystal structure of the triclinic polymorph of 1-(4-hexyloxy-3-hydroxyphenyl)ethanone, C 14 H 20 O 3 , differs markedly from that of the orthorhombic polymorph [Manzano et al. (2015). Acta Cryst. C71, 1022-1027]. The two molecular structures are alike with respect to their bond lengths and angles, but differ in their spatial arrangement. This gives rise to quite different packing schemes, even if built up by similar chains having the hydroxy-ethanone O-H...O hydrogen-bond synthon in common. Both phases were found to be related by a first-order thermally driven phase transformation at 338-340 K, which is discussed in detail. The relative stabilities of both polymorphs are explained on the basis of both the noncovalent interactions operating in each structure and quantum chemical calculations. The polymorphic phase transition has also been studied experimentally by means of differential scanning calorimetry (DSC) experiments, conducted on individual single crystals, Raman spectroscopy and controlled heating under a microscope of individual single crystals, which were further characterized by powder and single-crystal X-ray diffraction.

Growth of single crystals of BaFe12O19 by solid state crystal growth

NASA Astrophysics Data System (ADS)

Fisher, John G.; Sun, Hengyang; Kook, Young-Geun; Kim, Joon-Seong; Le, Phan Gia

2016-10-01

Single crystals of BaFe12O19 are grown for the first time by solid state crystal growth. Seed crystals of BaFe12O19 are buried in BaFe12O19+1 wt% BaCO3 powder, which are then pressed into pellets containing the seed crystals. During sintering, single crystals of BaFe12O19 up to ∼130 μm thick in the c-axis direction grow on the seed crystals by consuming grains from the surrounding polycrystalline matrix. Scanning electron microscopy-energy dispersive spectroscopy analysis shows that the single crystal and the surrounding polycrystalline matrix have the same chemical composition. Micro-Raman scattering shows the single crystal to have the BaFe12O19 structure. The optimum growth temperature is found to be 1200 °C. The single crystal growth behavior is explained using the mixed control theory of grain growth.

Research on subsurface defects of potassium dihydrogen phosphate crystals fabricated by single point diamond turning technique

NASA Astrophysics Data System (ADS)

Tie, Guipeng; Dai, Yifan; Guan, Chaoliang; Chen, Shaoshan; Song, Bing

2013-03-01

Potassium dihydrogen phosphate (KDP) crystals, which are widely used in high-power laser systems, are required to be free of defects on fabricated subsurfaces. The depth of subsurface defects (SSD) of KDP crystals is significantly influenced by the parameters used in the single point diamond turning technique. In this paper, based on the deliquescent magnetorheological finishing technique, the SSD of KDP crystals is observed and the depths under various cutting parameters are detected and discussed. The results indicate that no SSD is generated under small parameters and with the increase of cutting parameters, SSD appears and the depth rises almost linearly. Although the ascending trends of SSD depths caused by cutting depth and feed rate are much alike, the two parameters make different contributions. Taking the same material removal efficiency as a criterion, a large cutting depth generates shallower SSD depth than a large feed rate. Based on the experiment results, an optimized cutting procedure is obtained to generate defect-free surfaces.

Understanding the Earth's Mantle Through Advanced Elasticity Measurements

NASA Astrophysics Data System (ADS)

Marquardt, Hauke; Schulze, Kirsten; Kurnosov, Alexander; Buchen, Johannes; Frost, Daniel; Boffa Ballaran, Tiziana; Marquardt, Katharina; Kawazoe, Takaaki

2017-04-01

Constraints on the inner structure, chemical and mineralogical composition as well as dynamics of Earth's mantle can be derived through comparison of laboratory elasticity data to seismological observables. A quantitative knowledge of the elastic properties of mantle minerals, and their variations with chemical composition, at pressure and temperature conditions of Earth's mantle is key to construct reliable synthetic mineral physics-based seismic velocity models to be compared to seismic observables. We will discuss results of single-crystal elasticity measurements on Earth mantle minerals that have been conducted using the combined Brillouin scattering and x-ray diffraction (XRD) system at BGI Bayreuth in combination with advanced sample preparation using the focused ion beam (FIB) technique [1] that allows for tailoring sizes and shapes of tiny single-crystals. In our experiments, multiple FIB-prepared single-crystals were loaded in a single sample chamber of a resistively-heated diamond-anvil cell (DAC). The possiblity to measure simultaneously acoustic wave velocities and density (unit-cell parameters) in the DAC in combination with the multi-sample approach facilitates direct quantification of the effects of chemical substitution on the elasticity and seismic wave velocities at non-ambient conditions. Our experimental approach eliminates uncertainties arising from the combination of data collected under (potentially) different conditions in several DAC runs, in different laboratories and/or from using different pressure-temperature sensors. We will present our recent experiments on the elasticity of single-crystal Fe-Al-bearing bridgmanite in the lower mantle and discuss implications for the composition and oxidation state of Earth's lower mantle. We will further discuss our laboratory data on the effects of 'water' and iron on the seismic wave velocities of ringwoodite in Earth's transition zone and outline implications for mapping 'water' in the transition zone using geophysical observables. [1] Marquardt, H. and K. Marquardt, 2012. American Mineralogist 97, 299-304.

Quantitative determination of zero-gravity effects on electronic materials processing germanium crystal growth with simultaneous interface demarcation. Experiment MA-060

NASA Technical Reports Server (NTRS)

Gatos, H. C.; Witt, A. F.

1977-01-01

Experiment MA-060 was designed to establish the crystal growth and segregation characteristics of a melt in a directional solidification configuration under near zero-g conditions. The interface demarcation technique was incorporated into the experiment since it constitutes a unique tool for recording the morphology of the growth rate throughout solidification, and for establishing an absolute time reference framework for all stages of the solidification process. An extensive study was performed of the germanium crystals grown during the Apollo-Soyuz Test Project mission. It was found that single crystal growth was achieved and that the interface demarcation functioned successfully. There was no indication that convection driven by thermal or surface tension gradients was present in the melt. The gallium segregation, in the absence of gravity, was found to be fundamentally different in its initial and its subsequent stages from that of the ground-based tests. None of the existing theoretical models for growth and segregation can account for the observed segregation behavior in the absence of gravity.

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

Effect of water on olivine single crystals plasticity, deformed under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Girard, Jennifer

The Earth's upper mantle, mainly composed of olivine, is seismically anisotropic. Seismic anisotropy attenuation has been observed at 220km depth. Karato et al. (1992) attributed this attenuation to a transition between two deformation mechanisms, from dislocation creep above 220km to diffusion creep below 220km, induced by a change in water content. Couvy (2005) and Mainprice et al. (2005) predicted a change in Lattice Preferred Orientation induced by pressure, which comes from a change of slip system, from [100] slip to [001] slip, and is responsible for the seismic anisotropy attenuation. Raterron et al. (2007) ran single crystal deformation experiments under anhydrous conditions and observed that the slip system transition occurs around 8GPa, which corresponds to a depth of 260Km. Experiments were done to quantify the effects of water on olivine single crystals deformed using D-DIA press and synchrotron beam. Deformations were carried out in uniaxial compression along [110]c, [011]c, and [101]c, crystallographic directions, at pressure ranging from 4 to 8GPa and temperature between 1373 and 1473K. Talc sleeves about the annulus of the single crystals were used as source of water in the assembly. Stress and specimen strain rates were calculated by in-situ X-ray diffraction and time resolved imaging, respectively. By direct comparison of single crystals strain rates, we observed that [110]c deforms faster than [011]c below 5GPa. However above 6GPa [011]c deforms faster than [110]c. This revealed that [100](010) is the dominant slip system below 5GPa, and above 6GPa [001](010) becomes dominant. According to our results, the slip system transition, which is induced by pressure, occurs at 6GPa. Water influences the pressure where the switch over occurs, by lowering the transition pressure. The pressure effect on the slip systems activity has been quantified and the hydrolytic weakening has also been estimated for both orientations. Data also shows that temperature affects the slip system activity. The regional variation of the depth for the seismic anisotropy attenuation, which would depend on local hydroxyl content and temperature variations and explains the seismic anisotropy attenuation occurring at about 220Km depth in the mantle, where the pressure is about 6GPa. Deformation of MgO single crystal oriented [100], [110] and [111] were also performed. The results predict a change in the slip system activity at 23GPa, again induced by pressure. This explains the seismic anisotropy observed in the lower mantle.

Microgravity

NASA Image and Video Library

2000-11-03

On the Space Shuttle Orbiter Atlantis' middeck, Astronaut Joseph R. Tarner, mission specialist, works at an area amidst several lockers which support the Protein Crystal Growth (PCG) experiment during the STS-66 mission. This particular section is called the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES). Together with the Vapor Diffusion Apparatus (VDA), housed in Single Locker Thermal Enclosure (SLTES), the COS/TES represents the continuing research into the structure of proteins and other macromolecules such as viruses.

Single shot ultrafast dynamic ellipsometry (UDE) of laser-driven shocks in single crystal explosives

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

Whitley, Von H; Mcgrane, Shawn D; Moore, David S

2009-01-01

We report on the first experiments to measure states in shocked energetic single crystals with dynamic ellipsometry. We demonstrate that these ellipsometric techniques can produce reasonable Hugoniot values using small amounts of crystalline RDX and PETN. Pressures, particle velocities and shock velocities obtained using shocked ellipsometry are comparable to those found using gas-gun flyer plates and molecular dynamics calculations. The adaptation of the technique from uniform thin films of polymers to thick non-perfect crystalline materials was a significant achievement. Correct sample preparation proved to be a crucial component. Through trial and error, we were able to resolve polishing issues, samplemore » quality problems, birefringence effects and mounting difficulties that were not encountered using thin polymer films.« less

What determines the interfacial configuration of Nb/Al2O3 and Nb/MgO interface

PubMed Central

Du, J. L.; Fang, Y.; Fu, E. G.; Ding, X.; Yu, K. Y.; Wang, Y. G.; Wang, Y. Q.; Baldwin, J. K.; Wang, P. P.; Bai, Q.

2016-01-01

Nb films are deposited on single crystal Al2O3 (110) and MgO(111) substrates by e-beam evaporation technique. Structure of Nb films and orientation relationships (ORs) of Nb/Al2O3 and Nb/MgO interface are studied and compared by the combination of experiments and simulations. The experiments show that the Nb films obtain strong (110) texture, and the Nb film on Al2O3(110) substrate shows a higher crystalline quality than that on MgO(111) substrate. First principle calculations show that both the lattice mismatch and the strength of interface bonding play major roles in determining the crystalline perfection of Nb films and ORs between Nb films and single crystal ceramic substrates. The fundamental mechanisms for forming the interfacial configuration in terms of the lattice mismatch and the strength of interface bonding are discussed. PMID:27698458

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.

Crucibleless crystal growth and Radioluminescence study of calcium tungstate single crystal fiber

NASA Astrophysics Data System (ADS)

Silva, M. S.; Jesus, L. M.; Barbosa, L. B.; Ardila, D. R.; Andreeta, J. P.; Silva, R. S.

2014-11-01

In this article, single phase and high optical quality scheelite calcium tungstate single crystal fibers were grown by using the crucibleless laser heated pedestal growth technique. The as-synthesized calcium tungstate powders used for shaping seed and feed rods were investigated by X-ray diffraction technique. As-grown crystals were studied by Raman spectroscopy and Radioluminescence measurements. The results indicate that in both two cases, calcined powder and single crystal fiber, only the expected scheelite CaWO4 phase was observed. It was verified large homogeneity in the crystal composition, without the presence of secondary phases. The Radioluminescence spectra of the as-grown single crystal fibers are in agreement with that present in Literature for bulk single crystals, presented a single emission band centered at 420 nm when irradiated with β-rays.

Single crystalline growth of a soluble organic semiconductor in a parallel aligned liquid crystal solvent using rubbing-treated polyimide films

NASA Astrophysics Data System (ADS)

Matsuzaki, Tomoya; Shibata, Yosei; Takeda, Risa; Ishinabe, Takahiro; Fujikake, Hideo

2017-01-01

For directional control of organic single crystals, we propose a crystal growth method using liquid crystal as the solvent. In this study, we examined the formation of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) single crystals using a parallel aligned liquid crystal (LC) cell and rubbing-treated polyimide films in order to clarify the effects of LC alignment on anisotropic C8-BTBT crystal growth. Based on the results, we found that the crystal growth direction of C8-BTBT single crystals was related to the direction of the aligned LC molecules because of rubbing treatment. Moreover, by optical evaluation, we found that the C8-BTBT single crystals have a aligned molecular structure.

An Experiment on the Particle-Wave Nature of Electrons

ERIC Educational Resources Information Center

Matteucci, Giorgio; Migliori, Andrea; Medina, Francisco; Castaneda, Roman

2009-01-01

A primary electron beam of a transmission electron microscope is scattered into secondary beams by the planes of atoms of a single crystal. These secondary beams are focused to form a diffraction pattern on the final screen. This experiment is similar to the Thompson one which, independently by Davisson and Germer, demonstrated the de Broglie…

The application and use of chemical space mapping to interpret crystallization screening results

PubMed Central

Snell, Edward H.; Nagel, Ray M.; Wojtaszcyk, Ann; O’Neill, Hugh; Wolfley, Jennifer L.; Luft, Joseph R.

2008-01-01

Macromolecular crystallization screening is an empirical process. It often begins by setting up experiments with a number of chemically diverse cocktails designed to sample chemical space known to promote crystallization. Where a potential crystal is seen a refined screen is set up, optimizing around that condition. By using an incomplete factorial sampling of chemical space to formulate the cocktails and presenting the results graphically, it is possible to readily identify trends relevant to crystallization, coarsely sample the phase diagram and help guide the optimization process. In this paper, chemical space mapping is applied to both single macromolecules and to a diverse set of macromolecules in order to illustrate how visual information is more readily understood and assimilated than the same information presented textually. PMID:19018100

The application and use of chemical space mapping to interpret crystallization screening results.

PubMed

Snell, Edward H; Nagel, Ray M; Wojtaszcyk, Ann; O'Neill, Hugh; Wolfley, Jennifer L; Luft, Joseph R

2008-12-01

Macromolecular crystallization screening is an empirical process. It often begins by setting up experiments with a number of chemically diverse cocktails designed to sample chemical space known to promote crystallization. Where a potential crystal is seen a refined screen is set up, optimizing around that condition. By using an incomplete factorial sampling of chemical space to formulate the cocktails and presenting the results graphically, it is possible to readily identify trends relevant to crystallization, coarsely sample the phase diagram and help guide the optimization process. In this paper, chemical space mapping is applied to both single macromolecules and to a diverse set of macromolecules in order to illustrate how visual information is more readily understood and assimilated than the same information presented textually.

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.

A new generation of 99.999% enriched 28Si single crystals for the determination of Avogadro’s constant

NASA Astrophysics Data System (ADS)

Abrosimov, N. V.; Aref'ev, D. G.; Becker, P.; Bettin, H.; Bulanov, A. D.; Churbanov, M. F.; Filimonov, S. V.; Gavva, V. A.; Godisov, O. N.; Gusev, A. V.; Kotereva, T. V.; Nietzold, D.; Peters, M.; Potapov, A. M.; Pohl, H.-J.; Pramann, A.; Riemann, H.; Scheel, P.-T.; Stosch, R.; Wundrack, S.; Zakel, S.

2017-08-01

A metrological challenge is currently underway to replace the present definition of the kilogram. One prerequisite for this is that the Avogadro constant, N A, which defines the number of atoms in a mole, needs to be determined with a relative uncertainty of better than 2  ×  10-8. The method applied in this case is based on the x-ray crystal density experiment using silicon crystals. The first attempt, in which silicon of natural isotopic composition was used, failed. The solution chosen subsequently was the usage of silicon highly enriched in 28Si from Russia. First, this paper reviews previous efforts from the very first beginnings to an international collaboration with the goal of producing a 28Si single crystal with a mass of 5 kg, an enrichment greater than 0.9999 and of sufficient chemical purity. Then the paper describes the activities of a follow-up project, conducted by PTB, to produce a new generation of highly enriched silicon in order to demonstrate the quasi-industrial and reliable production of more than 12 kg of the 28Si material with enrichments of five nines. The intention of this project is also to show the availability of 28Si single crystals as a guarantee for the future realisation of the redefined kilogram.

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography.

PubMed

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

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals (Helliwell, 1984). Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to the diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. A possible mechanism to account for these observations is proposed.

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

DOE PAGES

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

2017-01-01

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

Bragg coherent diffraction imaging and metrics for radiation damage in protein micro-crystallography

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

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

The proliferation of extremely intense synchrotron sources has enabled ever higher-resolution structures to be obtained using data collected from smaller and often more imperfect biological crystals. Synchrotron beamlines now exist that are capable of measuring data from single crystals that are just a few micrometres in size. This provides renewed motivation to study and understand the radiation damage behaviour of small protein crystals. Reciprocal-space mapping and Bragg coherent diffractive imaging experiments have been performed on cryo-cooled microcrystals of hen egg-white lysozyme as they undergo radiation damage. Several well established metrics, such as intensity-loss and lattice expansion, are applied to themore » diffraction data and the results are compared with several new metrics that can be extracted from the coherent imaging experiments. Individually some of these metrics are inconclusive. However, combining metrics, the results suggest that radiation damage behaviour in protein micro-crystals differs from that of larger protein crystals and may allow them to continue to diffract for longer. As a result, a possible mechanism to account for these observations is proposed.« less

Spacelab

NASA Image and Video Library

1985-04-01

The primary purpose of the Spacelab-3 mission was to conduct materials science experiments in a stable low-gravity environment. In addition, the crew performed research in life sciences, fluid mechanics, atmospheric science, and astronomy. Spacelab-3 was equipped with several new minilabs, special facilities that would be used repeatedly on future flights. Two elaborate crystal growth furnaces, a life support and housing facility for small animals, and two types of apparatus for the study of fluids were evaluated on their inaugural flight. In this photograph, astronaut Don Lind observes the mercuric iodide growth experiment through a microscope at the vapor crystal growth furnace. The goals of this investigation were to grow near-perfect single crystals of mercuric iodide and to gain improved understanding of crystal growth by a vapor process. Mercuric iodide crystals have practical use as sensitive x-ray and gamma-ray detectors, and in portable detector devices for nuclear power plant monitoring, natural resource prospecting, biomedical applications in diagnosis and therapy, and in astronomical instruments. Managed by the Marshall Space Flight Center, Spacelab-3 (STS-51B) was launched aboard the Space Shuttle Orbiter Challenger on April 29, 1985.

Spacelab-3 (STS-51B) Onboard Photograph

NASA Technical Reports Server (NTRS)

1985-01-01

The primary purpose of the Spacelab-3 mission was to conduct materials science experiments in a stable low-gravity environment. In addition, the crew performed research in life sciences, fluid mechanics, atmospheric science, and astronomy. Spacelab-3 was equipped with several new minilabs, special facilities that would be used repeatedly on future flights. Two elaborate crystal growth furnaces, a life support and housing facility for small animals, and two types of apparatus for the study of fluids were evaluated on their inaugural flight. In this photograph, astronaut Don Lind observes the mercuric iodide growth experiment through a microscope at the vapor crystal growth furnace. The goals of this investigation were to grow near-perfect single crystals of mercuric iodide and to gain improved understanding of crystal growth by a vapor process. Mercuric iodide crystals have practical use as sensitive x-ray and gamma-ray detectors, and in portable detector devices for nuclear power plant monitoring, natural resource prospecting, biomedical applications in diagnosis and therapy, and in astronomical instruments. Managed by the Marshall Space Flight Center, Spacelab-3 (STS-51B) was launched aboard the Space Shuttle Orbiter Challenger on April 29, 1985.

Secondary orientation effects in a single crystal superalloy under mechanical and thermal loads

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

1991-01-01

The nickel-base single crystal superalloy PWA 1480 is a candidate blading material for the advanced turbopump development program of the SSME. In order to improve thermal fatigue resistance of the turbine blades, the single crystal superalloy PWA 1480 is grown along the low modulus zone axes (001) crystal orientation by a directional solidification process. Since cubic single crystal materials such as PWA 1480 exhibit anisotropic elastic behavior, the stresses developed within the single crystal superalloy due to mechanical and thermal loads are likely to be affected by the exact orientation of the secondary crystallographic direction with respect to the geometry of the turbine blade. The effects of secondary crystal orientation on the elastic response of single crystal PWA 1480 superalloy were investigated.

Piezoelectric single crystals for ultrasonic transducers in biomedical applications

PubMed Central

Zhou, Qifa; Lam, Kwok Ho; Zheng, Hairong; Qiu, Weibao; Shung, K. Kirk

2014-01-01

Piezoelectric single crystals, which have excellent piezoelectric properties, have extensively been employed for various sensors and actuators applications. In this paper, the state–of–art in piezoelectric single crystals for ultrasonic transducer applications is reviewed. Firstly, the basic principles and design considerations of piezoelectric ultrasonic transducers will be addressed. Then, the popular piezoelectric single crystals used for ultrasonic transducer applications, including LiNbO3 (LN), PMN–PT and PIN–PMN–PT, will be introduced. After describing the preparation and performance of the single crystals, the recent development of both the single–element and array transducers fabricated using the single crystals will be presented. Finally, various biomedical applications including eye imaging, intravascular imaging, blood flow measurement, photoacoustic imaging, and microbeam applications of the single crystal transducers will be discussed. PMID:25386032

A Fiber Optic Probe for Monitoring Protein Aggregation, Nucleation, and Crystallization

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.; Arabshahi, Alireza; Wilson, William W.; Bray, Terry L.; DeLucas, Lawrence J.

1996-01-01

Protein crystals are experimentally grown in hanging drops in microgravity experiments on-board the Space Shuttle orbiter. The technique of dynamic light scattering (DLS) can be used to monitor crystal growth process in hanging droplets (approx. 30 (L)) in microgravity experiments, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. In this paper we demonstrate that such experiments are now feasible. We apply a newly developed fiber optic probe to various earth and space (micro- gravity) bound protein crystallization system configurations to test its capability. These include conventional batch (cuvette or capillary) systems, hanging drop method in a six-pack hanging drop vapor diffusion apparatus (HDVDA), a modified HDVDA for temperature- induced nucleation and aggregation studies, and a newly envisioned dynamically controlled vapor diffusion system (DCVDS) configuration. Our compact system exploits the principles of DLS and offers a fast (within a few seconds) means of quantitatively and non-invasively monitoring the various growth stages of protein crystallization. In addition to DLS capability, the probe can also be used for performing single-angle static light scattering measurements. It utilizes extremely low levels of laser power (approx. few (W)) without a need of having any optical alignment and vibration isolation. The compact probe is also equipped with a miniaturized microscope for visualization of macroscopic protein crystals. This new optical diagnostic system opens up enormous opportunity for exploring new ways to grow good quality crystals suitable for x-ray crystallographic analysis and may help develop a concrete scientific basis for understanding the process of crystallization.

Correlation between the conformational states of F1-ATPase as determined from its crystal structure and single-molecule rotation

PubMed Central

Okuno, Daichi; Fujisawa, Ryo; Iino, Ryota; Hirono-Hara, Yoko; Imamura, Hiromi; Noji, Hiroyuki

2008-01-01

F1-ATPase is a rotary molecular motor driven by ATP hydrolysis that rotates the γ-subunit against the α3β3 ring. The crystal structures of F1, which provide the structural basis for the catalysis mechanism, have shown essentially 1 stable conformational state. In contrast, single-molecule studies have revealed that F1 has 2 stable conformational states: ATP-binding dwell state and catalytic dwell state. Although structural and single-molecule studies are crucial for the understanding of the molecular mechanism of F1, it remains unclear as to which catalytic state the crystal structure represents. To address this issue, we introduced cysteine residues at βE391 and γR84 of F1 from thermophilic Bacillus PS3. In the crystal structures of the mitochondrial F1, the corresponding residues in the ADP-bound β (βDP) and γ were in direct contact. The βE190D mutation was additionally introduced into the β to slow ATP hydrolysis. By incorporating a single copy of the mutant β-subunit, the chimera F1, α3β2β(E190D/E391C)γ(R84C), was prepared. In single-molecule rotation assay, chimera F1 showed a catalytic dwell pause in every turn because of the slowed ATP hydrolysis of β(E190D/E391C). When the mutant β and γ were cross-linked through a disulfide bond between βE391C and γR84C, F1 paused the rotation at the catalytic dwell angle of β(E190D/E391C), indicating that the crystal structure represents the catalytic dwell state and that βDP is the catalytically active form. The former point was again confirmed in experiments where F1 rotation was inhibited by adenosine-5′-(β,γ-imino)-triphosphate and/or azide, the most commonly used inhibitors for the crystallization of F1. PMID:19075235

Dynamic creation and evolution of gradient nanostructure in single-crystal metallic microcubes.

PubMed

Thevamaran, Ramathasan; Lawal, Olawale; Yazdi, Sadegh; Jeon, Seog-Jin; Lee, Jae-Hwang; Thomas, Edwin L

2016-10-21

We demonstrate the dynamic creation and subsequent static evolution of extreme gradient nanograined structures in initially near-defect-free single-crystal silver microcubes. Extreme nanostructural transformations are imposed by high strain rates, strain gradients, and recrystallization in high-velocity impacts of the microcubes against an impenetrable substrate. We synthesized the silver microcubes in a bottom-up seed-growth process and use an advanced laser-induced projectile impact testing apparatus to selectively launch them at supersonic velocities (~400 meters per second). Our study provides new insights into the fundamental deformation mechanisms and the effects of crystal and sample-shape symmetries resulting from high-velocity impacts. The nanostructural transformations produced in our experiments show promising pathways to developing gradient nanograined metals for engineering applications requiring both high strength and high toughness-for example, in structural components of aircraft and spacecraft. Copyright © 2016, American Association for the Advancement of Science.

Techniques for determining thermal conductivity and heat capacity under hydrostatic pressure

NASA Astrophysics Data System (ADS)

Andersson, S.; Bäckström, G.

1986-08-01

The paper describes a method for measuring the pressure dependence of the thermal conductivity and the heat capacity of hard materials and single crystals. Two parallel metal strips are evaporated onto a flat surface of the specimen, one being used as a heater, the other as a resistance thermometer. The appropriate theoretical expression for a specimen in a liquid medium is fitted to the temperature, sampled at constant time intervals. The thermophysical properties of the liquid high-pressure medium are taken from hot-wire experiments. The procedure has been thoroughly tested at atmospheric pressure using an MgO crystal and glass as specimens and liquids of different characteristics in lieu of high-pressure medium. The accuracy attainable was found to be 3% or better, the standard deviation of the measurements being about 0.3%. The potential of the system was demonstrated by measurements on single-crystal MgO under pressures up to 1 GPa.

Optical spectra and band structure of Ag(x)Ga(x)Ge(1-x)Se2 (x = 0.333, 0.250, 0.200, 0.167) single crystals: experiment and theory.

PubMed

Reshak, A H; Parasyuk, O V; Fedorchuk, A O; Kamarudin, H; Auluck, S; Chyský, J

2013-12-05

Theoretical and experimental studies of the Ag(x)Ga(x)Ge(1-x)Se2 (x = 0.333, 0.250, 0.200, 0.167) single crystals are performed. These crystals possess a lot of intrinsic defects which are responsible for their optoelectronic features. The theoretical investigations were performed by means of DFT calculations using different exchange-correlation potentials. The experimental studies were carried out using the modulated VUV ellipsometry for dielectric constants and birefringence studies. The comparison of the structure obtained from X-ray with the theoretically optimized structure is presented. The crucial role of the intrinsic defect states is manifested in the choice of the exchange correlation potential used. The data may be applicable for a large number of the ternary chalcogenides which are sensitive to the presence of the local disordered states near the band edges.

Preparation of a Non-Polar ZnO Film on a Single-Crystal NdGaO3 Substrate by the RF Sputtering Method

NASA Astrophysics Data System (ADS)

Kashiwaba, Y.; Tanaka, Y.; Sakuma, M.; Abe, T.; Imai, Y.; Kawasaki, K.; Nakagawa, A.; Niikura, I.; Kashiwaba, Y.; Osada, H.

2018-04-01

Preparation of non-polar ZnO ( 11\\overline{2} 0 ) films on single-crystal NdGaO3 (NGO) (001) substrates was successfully achieved by the radio frequency (RF) sputtering method. Orientation, deposition rate, and surface roughness of ZnO films strongly depend on the working pressure. Characteristics of ZnO films deposited on single-crystal NGO (001) substrates were compared with those of ZnO films deposited on single-crystal sapphire ( 01\\overline{1} 2 ) substrates. An x-ray diffraction peak of the ZnO ( 11\\overline{2} 0 ) plane was observed on ZnO films deposited on single-crystal NGO (001) substrates under working pressure of less than 0.5 Pa. On the other hand, uniaxially oriented ZnO ( 11\\overline{2} 0 ) films on single-crystal sapphire ( 01\\overline{1} 2 ) substrates were observed under working pressure of 0.1 Pa. The mechanism by which the diffraction angle of the ZnO ( 11\\overline{2} 0 ) plane on single-crystal NGO (001) substrates was shifted is discussed on the basis of anisotropic stress of lattice mismatch. The deposition rate of ZnO films decreased with an increase in working pressure, and the deposition rate on single-crystal NGO (001) substrates was larger than that on single-crystal sapphire ( 01\\overline{1} 2 ) substrates. Root mean square (RMS) roughness of ZnO films increased with an increase in working pressure, and RMS roughness of ZnO films on single-crystal NGO (001) substrates was smaller than that of ZnO films on single-crystal sapphire ( 01\\overline{1} 2 ) substrates even though the film thickness on single-crystal NGO (001) substrates was greater than that on sapphire substrates. It is thought that a single-crystal NGO (001) substrate is useful for deposition of non-polar ZnO ( 11\\overline{2} 0 ) films.

Electrical characteristics of organic perylene single-crystal-based field-effect transistors

NASA Astrophysics Data System (ADS)

Lee, Jin-Woo; Kang, Han-Saem; Kim, Min-Ki; Kim, Kihyun; Cho, Mi-Yeon; Kwon, Young-Wan; Joo, Jinsoo; Kim, Jae-Il; Hong, Chang-Seop

2007-12-01

We report on the fabrication of organic field-effect transistors (OFETs) using perylene single crystal as the active material and their electrical characteristics. Perylene single crystals were directly grown from perylene powder in a furnace using a relatively short growth time of 1-3 h. The crystalline structure of the perylene single crystals was characterized by means of a single-crystal x-ray diffractometer. In order to place the perylene single crystal onto the Au electrodes of the field-effect transistor, a polymethlymethacrylate thin layer was spin-coated on top of the crystal surface. The OFETs fabricated using the perylene single crystal showed a typical p-type operating mode. The field-effect mobility of the perylene crystal based OFETs was measured to be ˜9.62×10-4 cm2/V s at room temperature. The anisotropy of the mobility implying the existence of different mobilities when applying currents in different directions was observed for the OFETs, and the existence of traps in the perylene crystal was found through the measurements of the temperature-dependent mobility at various operating drain voltages.

Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

NASA Astrophysics Data System (ADS)

Lunt, A. J. G.; Xie, M. Y.; Baimpas, N.; Zhang, S. Y.; Kabra, S.; Kelleher, J.; Neo, T. K.; Korsunsky, A. M.

2014-08-01

Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals. Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.

A loophole-free Bell's inequality experiment

NASA Astrophysics Data System (ADS)

Kwiat, Paul G.; Steinberg, Aephraim M.; Chiao, Raymond Y.; Eberhard, Philippe H.

1994-05-01

The proof of Nature's nonlocality through Bell-type experiments is a topic of longstanding interest. Nevertheless, no experiments performed thus far have avoided the so-called 'detection loophole,' arising from low detector efficiencies and angular-correlation difficulties. In fact, most, if not all, of the systems employed to date can never close this loophole, even with perfect detectors. In addition, another loophole involving the non-rapid, non-random switching of various parameter settings exists in all past experiments. We discuss a proposal for a potentially loophole-free Bell's inequality experiment. The source of the EPR-correlated pairs consists of two simultaneously-pumped type-2 phase-matched nonlinear crystals and a polarizing beam splitter. The feasibility of such a scheme with current detector technology seems high, and will be discussed. We also present a single-crystal version, motivated by other work presented at this conference. In a separate experiment, we have measured the absolute detection efficiency and time response of four single-photon detectors. The highest observed efficiencies were 70.7 plus or minus 1.9 percent (at 633 nm, with a device from Rockwell International) and 76.4 plus or minus 2.3 percent (at 702 nm, with an EG&G counting module). Possible efficiencies as high as 90 percent were implied. The EG&G devices displayed sub-nanosecond time resolution.

A loophole-free Bell's inequality experiment

NASA Technical Reports Server (NTRS)

Kwiat, Paul G.; Steinberg, Aephraim M.; Chiao, Raymond Y.; Eberhard, Philippe H.

1994-01-01

The proof of Nature's nonlocality through Bell-type experiments is a topic of longstanding interest. Nevertheless, no experiments performed thus far have avoided the so-called 'detection loophole,' arising from low detector efficiencies and angular-correlation difficulties. In fact, most, if not all, of the systems employed to date can never close this loophole, even with perfect detectors. In addition, another loophole involving the non-rapid, non-random switching of various parameter settings exists in all past experiments. We discuss a proposal for a potentially loophole-free Bell's inequality experiment. The source of the EPR-correlated pairs consists of two simultaneously-pumped type-2 phase-matched nonlinear crystals and a polarizing beam splitter. The feasibility of such a scheme with current detector technology seems high, and will be discussed. We also present a single-crystal version, motivated by other work presented at this conference. In a separate experiment, we have measured the absolute detection efficiency and time response of four single-photon detectors. The highest observed efficiencies were 70.7 plus or minus 1.9 percent (at 633 nm, with a device from Rockwell International) and 76.4 plus or minus 2.3 percent (at 702 nm, with an EG&G counting module). Possible efficiencies as high as 90 percent were implied. The EG&G devices displayed sub-nanosecond time resolution.

Reproducible Crystal Growth Experiments in Microgravity Science Glovebox at the International Space Station (SUBSA Investigation)

NASA Technical Reports Server (NTRS)

Ostrogorsky, A.; Marin, C.; Volz, M. P.; Bonner, W. A.

2005-01-01

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is the first investigation conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. 8 single crystals of InSb, doped with Te and Zn, were directionally solidified in microgravity. The experiments were conducted in a furnace with a transparent gradient section, and a video camera, sending images to the earth. The real time images (i) helped seeding, (ii) allowed a direct measurement of the solidification rate. The post-flight characterization of the crystals includes: computed x-ray tomography, Secondary Ion Mass Spectroscopy (SIMS), Hall measurements, Atomic Absorption (AA), and 4 point probe analysis. For the first time in microgravity, several crystals having nearly identical initial transients were grown. Reproducible initial transients were obtained with Te-doped InSb. Furthermore, the diffusion controlled end-transient was demonstrated experimentally (SUBSA 02). From the initial transients, the diffusivity of Te and Zn in InSb was determined.

First Principle and Experimental Study for Site Preferences of Formability Improved Alloying Elements in Mg Crystal

NASA Astrophysics Data System (ADS)

Zeng, Ying; Jiang, Bin; Shi, Ouling; Quan, Gaofen; Al-Ezzi, Salih; Pan, FuSheng

2018-07-01

Some alloying elements (Al, Er, Gd, Li, Mn, Sn, Y, Zn) were proved recently by calculations or experiments to improve the formability of Mg alloys, but ignoring their site preference in Mg crystals during the calculated process. A crystallographic model was built via first principle calculations to predict the site preferences of these elements. Regularities between doping elements and site preferences were summarized. Meanwhile, in the basis of the crystallographic model, a series of formulas were deduced combining the diffraction law. It predicted that a crystal plane with abnormal XRD peak intensity of the Mg-based solid solutions, compared to that of the pure Mg, prefers to possess solute atoms. Thus, three single-phase solid solution alloys were then prepared through an original In-situ Solution Treatment, and their XRD patterns were compared. Finally, the experiment further described the site preferences of these solute atoms in Mg crystal, verifying the calculation results.

First Principle and Experimental Study for Site Preferences of Formability Improved Alloying Elements in Mg Crystal

NASA Astrophysics Data System (ADS)

Zeng, Ying; Jiang, Bin; Shi, Ouling; Quan, Gaofen; Al-Ezzi, Salih; Pan, FuSheng

2018-03-01

Some alloying elements (Al, Er, Gd, Li, Mn, Sn, Y, Zn) were proved recently by calculations or experiments to improve the formability of Mg alloys, but ignoring their site preference in Mg crystals during the calculated process. A crystallographic model was built via first principle calculations to predict the site preferences of these elements. Regularities between doping elements and site preferences were summarized. Meanwhile, in the basis of the crystallographic model, a series of formulas were deduced combining the diffraction law. It predicted that a crystal plane with abnormal XRD peak intensity of the Mg-based solid solutions, compared to that of the pure Mg, prefers to possess solute atoms. Thus, three single-phase solid solution alloys were then prepared through an original In-situ Solution Treatment, and their XRD patterns were compared. Finally, the experiment further described the site preferences of these solute atoms in Mg crystal, verifying the calculation results.

Observation of a commensurate array of flux chains in tilted flux lattices in Bi-Sr-Ca-Cu-O single crystals

NASA Astrophysics Data System (ADS)

Bolle, C. A.; Gammel, P. L.; Grier, D. G.; Murray, C. A.; Bishop, D. J.; Mitzi, D. B.; Kapitulnik, A.

1991-01-01

We report the observation of a novel flux-lattice structure, a commensurate array of flux-line chains. Our experiments consist of the magnetic decoration of the flux lattices in single crystals of Ba-Sr-Ca-Cu-O where the magnetic field is applied at an angle with respect to the conducting planes. For a narrow range of angles, the equilibrium structure is one with uniformly spaced chains with a higher line density of vortices than the background lattice. Our observations are in qualitative agreement with theories which suggest that, in strongly anisotropic materials the vortices develop an attractive interaction in tilted magnetic fields.

40-Tesla pulsed-field cryomagnet for single crystal neutron diffraction

NASA Astrophysics Data System (ADS)

Duc, F.; Tonon, X.; Billette, J.; Rollet, B.; Knafo, W.; Bourdarot, F.; Béard, J.; Mantegazza, F.; Longuet, B.; Lorenzo, J. E.; Lelièvre-Berna, E.; Frings, P.; Regnault, L.-P.

2018-05-01

We present the first long-duration and high duty cycle 40-T pulsed-field cryomagnet addressed to single crystal neutron diffraction experiments at temperatures down to 2 K. The magnet produces a horizontal field in a bi-conical geometry, ±15° and ±30° upstream and downstream of the sample, respectively. Using a 1.15 MJ mobile generator, magnetic field pulses of 100 ms length are generated in the magnet, with a rise time of 23 ms and a repetition rate of 6-7 pulses per hour at 40 T. The setup was validated for neutron diffraction on the CEA-CRG three-axis spectrometer IN22 at the Institut Laue Langevin.

Enhanced electrocaloric cooling in ferroelectric single crystals by electric field reversal

NASA Astrophysics Data System (ADS)

Ma, Yang-Bin; Novak, Nikola; Koruza, Jurij; Yang, Tongqing; Albe, Karsten; Xu, Bai-Xiang

2016-09-01

An improved thermodynamic cycle is validated in ferroelectric single crystals, where the cooling effect of an electrocaloric refrigerant is enhanced by applying a reversed electric field. In contrast to the conventional adiabatic heating or cooling by on-off cycles of the external electric field, applying a reversed field is significantly improving the cooling efficiency, since the variation in configurational entropy is increased. By comparing results from computer simulations using Monte Carlo algorithms and experiments using direct electrocaloric measurements, we show that the electrocaloric cooling efficiency can be enhanced by more than 20% in standard ferroelectrics and also relaxor ferroelectrics, like Pb (Mg1 /3 /Nb2 /3)0.71Ti0.29O3 .

Single crystal diamond detector measurements of deuterium-deuterium and deuterium-tritium neutrons in Joint European Torus fusion plasmas.

PubMed

Cazzaniga, C; Sundén, E Andersson; Binda, F; Croci, G; Ericsson, G; Giacomelli, L; Gorini, G; Griesmayer, E; Grosso, G; Kaveney, G; Nocente, M; Perelli Cippo, E; Rebai, M; Syme, B; Tardocchi, M

2014-04-01

First simultaneous measurements of deuterium-deuterium (DD) and deuterium-tritium neutrons from deuterium plasmas using a Single crystal Diamond Detector are presented in this paper. The measurements were performed at JET with a dedicated electronic chain that combined high count rate capabilities and high energy resolution. The deposited energy spectrum from DD neutrons was successfully reproduced by means of Monte Carlo calculations of the detector response function and simulations of neutron emission from the plasma, including background contributions. The reported results are of relevance for the development of compact neutron detectors with spectroscopy capabilities for installation in camera systems of present and future high power fusion experiments.

Exploring the folding pattern of a polymer chain in a single crystal by combining single-molecule force spectroscopy and steered molecular dynamics simulations.

PubMed

Song, Yu; Feng, Wei; Liu, Kai; Yang, Peng; Zhang, Wenke; Zhang, Xi

2013-03-26

Understanding the folding pattern of a single polymer chain within its single crystal will shed light on the mechanism of crystallization. Here, we use the combined techniques of atomic force microscopy (AFM)-based single-molecule force spectroscopy (SMFS) and steered molecular dynamics (SMD) simulations to study the folding pattern of a polyethylene oxide (PEO) chain in its single crystal. Our results show that the folding pattern of a PEO chain in the crystal formed in dilute solution follows the adjacent re-entry folding model. While in the crystal obtained from the melt, the nonadjacent folding with large and irregular loops contributes to big force fluctuations in the force-extension curves. The method established here can offer a novel strategy to directly unravel the chain-folding pattern of polymer single crystals at single-molecule level.

Prediction of Fretting Crack Location and Orientation in a Single Crystal Nickel Alloy

NASA Technical Reports Server (NTRS)

Matlik, J. F.; Farris, T. N.; Haynes, J.; Swanson, G. R.; Ham-Battista, G.

2005-01-01

Fretting is a structural damage mechanism arising between two nominally clamped surfaces subjected to an oscillatory loading. A critical location for fretting induced damage has been identified at the blade/disk and blade/damper interfaces of gas turbine engine turbomachinery and space propulsion components. The high- temperature, high-frequency loading environment seen by these components lead to severe stress gradients at the edge-of-contact that could potentially foster crack growth leading to component failure. These contact stresses drive crack nucleation in fretting and are very sensitive to the geometry of the contacting bodies, the contact loads, materials, temperature, and contact surface tribology (friction). Recently, a high-frequency, high-temperature load frame has been designed for experimentally investigating fretting damage of single crystal nickel materials employed in aircraft and spacecraft turbomachinery. A modeling method for characterizing the fretting stresses of the spherical fretting contact stress behavior in this experiment is developed and described. The calculated fretting stresses for a series of experiments are then correlated to the observed fretting damage. Results show that knowledge of the normal stresses and resolved shear stresses on each crystal plane can aid in predicting crack locations and orientations.

Effect of amaranth dye on the growth and properties of conventional and SR method grown KAP single crystals

NASA Astrophysics Data System (ADS)

Babu Rao, G.; P., Rajesh; Ramasamy, P.

2018-04-01

The 0.1 mol% amaranth added KAP single crystals were grown from aqueous solutions by both slow evaporation solution technique and Sankaranarayanan-Ramasamy method. The single crystal having dimension of 45 mm length and 12 mm diameter was grown with growth rate of 1.5 mm/day using SR method. 87 % transmittance is obtained for SR method grown amaranth added KAP single crystal. The high intense luminescence at 661 nm is obtained from amaranth added conventional and SR method grown KAP single crystal. The amaranth added KAP single crystal possesses good mechanical and laser damage threshold stability.

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

NASA Technical Reports Server (NTRS)

Malkin, Alexander J.

1998-01-01

During the past year we have focused on application of in situ Atomic Force Microscopy (AFM) for studies of the growth mechanisms and kinetics of crystallization for different macromolecular systems. Mechanisms of macrostep formation and their decay, which are important in understanding of defect formation, were studied on the surfaces of thaumatin, catalase, canavalin and lysozyme crystals. Experiments revealed that step bunching on crystalline surfaces occurred either due to two- or three-dimensional nucleation on the terraces of vicinal slopes or as a result of uneven step generation by complex dislocation sources. No step bunching arising from interaction of individual steps in the course of the experiment was observed. The molecular structure of the growth steps for thaumatin and lipase crystals were deduced. It was further shown that growth step advance occurs by incorporation of single protein molecules. In singular directions growth steps move by one-dimensional nucleation on step edges followed by lateral growth. One-dimensional nuclei have different sizes, less then a single unit cell, varying for different directions of step movement. There is no roughness due to thermal fluctuations, and each protein molecule which incorporated into the step remained. Growth kinetics for catalase crystals was investigated over wide supersaturation ranges. Strong directional kinetic anisotropy in the tangential step growth rates in different directions was seen. The influence of impurities on growth kinetics and cessation of macromolecular crystals was studied. Thus, for catalase, in addition to pronounced impurity effects on the kinetics of crystallization, we were also able to directly observe adsorption of some impurities. At low supersaturation we repeatedly observed filaments which formed from impurity molecules sedimenting on the surfaces. Similar filaments were observed on the surfaces of thaumatin, canavalin and STMV crystals as well, but the frequency was low compared with catalase crystallization. Cessation of growth of xylanase and lysozyme crystals was also observed and appeared to be a consequence of the formation of dense impurity adsorption layers. Attachment: "An in situ AFM investigation of catalase crystallization", "Atomic force microscopy studies of living cells: visualization of motility, division, aggregation, transformation, and apoptosis", AFM studies on mechanisms of nucleation and growth of macromolecular crystals", and "In situ atomic force microscopy studies of surface morphology, growth kinetics, defect structure and dissolution in macromolecular crystallization".

Comparison study of morphology and crystallization behavior of polyethylene and poly(ethylene oxide) on single-walled carbon nanotubes.

PubMed

Zheng, Xiaoli; Xu, Qun

2010-07-29

In this work, we provided a comparison study of morphology and crystallization behavior of polyethylene (PE) and poly(ethylene oxide) (PEO) on single-walled carbon nanotubes (SWNTs) with assistance of supercritical CO(2). The resulting polymer/SWNT nanohybrids were characterized by transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, Raman spectra, wide-angle X-ray diffraction, and differential scanning calorimetry. SWNT small bundles were decorated by PE lamellar crystals, forming nanohybrid "shish-kebab" (NHSK) structure, whereas SWNTs were only wrapped by a thin amorphous polymer coating in the case of PEO. The varying morphologies of the nanohybrids were found to depend on the molecular conformation and the interactions between polymer chains and SWNTs. Nonisothermal experiments showed that SWNTs provided heterogeneous nucleation sites for PE crystallization, while the NHSK structure hindered polymer chain diffusion and crystal growth. Also, SWNTs played antinucleation effect on PEO. In addition, the formation mechanism analysis indicated that PE chains preferred to form a homogeneous coating along the tube axis before proceeding to kebab crystal growth. The purpose of this work is to enlarge the area of theoretical understanding of introducing precisely hierarchical structures on carbon nanotubes, which are important for functional design in nanodevice applications.

Control of Orientation and Morphology of Crystals Grown Under Organic Templates

NASA Astrophysics Data System (ADS)

Stripe, Benjamin

Living creatures demonstrate an extraordinary ability to both grow and control the growth of inorganic crystals. These biominerals are found almost everywhere in nature from simple plants and plankton to our own teeth and bones. A great deal of research has been focused on how living creatures are able to achieve such control over the shape, size, orientation, and arrangement of these biominerals. Many studies have been done demonstrating the effects the presence of organic molecules can have on the morphology of nucleating inorganic crystals. These studies have led to the use of ordered arrays of biological molecules as templates to select the orientation of the crystals. Such experiments have had amazing success cataloging monolayers, orientations and morphologies of crystals grown beneath them. However, despite several decades of work, the exact mechanisms by which the orientation and morphology of crystals is selected by organic templates are still not known. The present study attempts to explain the complex interactions that take place at the template surface and decide the orientations and morphologies of the crystals that nucleate there. To do this, scanning electron microscopy (SEM), grazing incidence x-ray diffraction (GID), and x-ray reflectivity have been used to probe the templates and nucleating crystals in situ. The experiments described here seek to move beyond the well-studied two-component systems. In many of these two-component systems a single template and a single type of crystal are grown, and often many claims and comparisons are made about monolayer charge, crystal surface energies, stereochemical recognition, and lattice matches. However, almost all of the claims and comparisons are between systems that are different enough that assumptions about relative charge, strain, recognition, and lattice dynamics are either unfounded or poorly supported. To bridge this gap in the comparison of these different two-component systems the studies presented here are tunable three-component systems. These experiments allow for either continuously adjusting the template by means of two miscible monolayers or adjusting the growing crystals by incorporation of secondary ions. In either case, the idea is the same: we can more accurately compare two-component systems and isolate the controlling factor in the selection of orientation and morphology of the nucleating crystals. The results of these studies have shown that there is a complex interplay of charge, lattice parameters and kinetics. Despite this, we have been able to show that well-oriented growth of single non-dendritic crystals is limited to a fairly small range of surface charges and relative growth kinetics. Within this range, variations in the growing crystals can be seen based on changes in the average lattice parameters despite there being no evidence of direct epitaxy. Theories have evolved around the idea of stereochemical matching between the template and nucleating surface. These theories correlate the template molecular tilt to the orientation relative to the nucleation plane. However, these theories are not supported by the results presented in this manuscript. The data presented in this manuscript are suggestive of far more complex interfacial interactions involving an intermediary amorphous precursor, or possible networks of hydrated or hydrogen bonded ions than has been suggested in previous studies. Excitingly, it appears to be possible to control the selection of orientation using these multicomponent systems despite the complex interactions at the surface.

Ultrastructural studies of synthetic apatite crystals.

PubMed

Arends, J; Jongebloed, W L

1979-03-01

In this paper a survey is given of some ultrastructural properties of synthetic hydroxyapatite. The preparation method by which single crystals with a length in the range of 0.1-3.0mm and a defined purity and stoïchiometry can be produced is given. Two groups of materials are considered in detail: carbonate-rich (greater than 0.1% CO3) and low-carbonate hydroxyapatites. The experiments on carbonate-rich material, being the most interesting from a biological point of view, show that acids attack at an active site in the hexagonal basal-plane of the crystals. Later on the crystals dissolve in the center of the crystal parallel to the c-axis forming tube-like structures. The active site can be protected from dissolution if the crystals are pretreated by EHDP or MFP. A comparison with lattice defect theory shows that most likely dislocations of the "hollow-core" type are responsible for the preferential dissolution.

7 Å Resolution in Protein 2-Dimentional-Crystal X-Ray Diffraction at Linac Coherent Light Source

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

Pedrini, Bill; Tsai, Ching-Ju; Capitani, Guido

2014-06-09

Membrane proteins arranged as two-dimensional (2D) crystals in the lipid en- vironment provide close-to-physiological structural information, which is essential for understanding the molecular mechanisms of protein function. X-ray diffraction from individual 2D crystals did not represent a suitable investigation tool because of radiation damage. The recent availability of ultrashort pulses from X-ray Free Electron Lasers (X-FELs) has now provided a mean to outrun the damage. Here we report on measurements performed at the LCLS X-FEL on bacteriorhodopsin 2D crystals mounted on a solid support and kept at room temperature. By merg- ing data from about a dozen of single crystalmore » diffraction images, we unambiguously identified the diffraction peaks to a resolution of 7 °A, thus improving the observable resolution with respect to that achievable from a single pattern alone. This indicates that a larger dataset will allow for reliable quantification of peak intensities, and in turn a corresponding increase of resolution. The presented results pave the way to further X-FEL studies on 2D crystals, which may include pump-probe experiments at subpicosecond time resolution.« less

Synthesis, crystal structure, Hirshfeld surfaces analysis and anti-ischemic activity of cinnamide derivatives

NASA Astrophysics Data System (ADS)

Zhong, Jian-gang; Han, Jia-pei; Li, Xiao-feng; Xu, Yi; Zhong, Yan; Wu, Bin

2018-02-01

Two cinnamide derivatives, namely, (E)-1-(4-(bis(4-methylphenyl)- methyl)piperazin-1-yl)-3-(3,4-diethoxyphenyl)prop-2-en-1-one (5) and (E)-1-(4-(bis- (4-fluorophenyl)methyl)piperazin-1-yl)-3-(4-methoxyphenyl)prop-2-en-1-one (6), have been synthesized and characterized by IR spectra, High resolution mass spectra, 1H NMR spectra, 13C NMR spectra. The compound 5 is a novel compound and has never been reported in the literature. Their crystal structures were studied by single-crystal X-ray diffraction. They all crystallize in the monoclinic system. The single-crystal X-ray revealed that compound 5 has infinite X-shaped 1-D polymeric chains structure and compound 6 has a layered 3-D structure by intermolecular interactions. Hirshfeld surface analysis demonstrated the presence of H⋯H, O⋯H, C⋯H, F⋯H, Csbnd H⋯π and π⋯π intermolecular interactions. In addition, the MTT assay results indicated that the compounds 5 and 6 display effective activities against neurotoxicity which is induced by glutamine in PC12 cells. The in vivo experiment indicated that the compound 6 has a good protective effect on cerebral infarction.

Models of Mass Transport During Microgravity Crystal Growth of Alloyed Semiconductors in a Magnetic Field

NASA Technical Reports Server (NTRS)

Ma, Nancy

2003-01-01

Alloyed semiconductor crystals, such as germanium-silicon (GeSi) and various II-VI alloyed crystals, are extremely important for optoelectronic devices. Currently, high-quality crystals of GeSi and of II-VI alloys can be grown by epitaxial processes, but the time required to grow a certain amount of single crystal is roughly 1,000 times longer than the time required for Bridgman growth from a melt. Recent rapid advances in optoelectronics have led to a great demand for more and larger crystals with fewer dislocations and other microdefects and with more uniform and controllable compositions. Currently, alloyed crystals grown by bulk methods have unacceptable levels of segregation in the composition of the crystal. Alloyed crystals are being grown by the Bridgman process in space in order to develop successful bulk-growth methods, with the hope that the technology will be equally successful on earth. Unfortunately some crystals grown in space still have unacceptable segregation, for example, due to residual accelerations. The application of a weak magnetic field during crystal growth in space may eliminate the undesirable segregation. Understanding and improving the bulk growth of alloyed semiconductors in microgravity is critically important. The purpose of this grant to to develop models of the unsteady species transport during the bulk growth of alloyed semiconductor crystals in the presence of a magnetic field in microgravity. The research supports experiments being conducted in the High Magnetic Field Solidification Facility at Marshall Space Flight Center (MSFC) and future experiments on the International Space Station.

Translation effects on vertical Bridgman growth and optical, mechanical and surface analysis of 2-phenylphenol single crystal

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

Sadhasivam, S., E-mail: sadha.phy1@gmail.com; Perumal, Rajesh Narayana

2-phenylphenol optical crystals were grown in cone ampoules using vertical Bridgman technique. Single crystal of 2-phenylphenol with 150 mm length has been grown. The inclination on the conical part of the ampoule reduces the growth defects in the 2-phenylphenol single crystal. The lattice parameters and structure studied using single crystal X-ray diffraction method. 2-phenylphenol single crystal belongs to orthorhombic space group Fdd2. The micro translation rate affects crystal growth of 2-phenylphenol crystal was studied. The translation rate dependent defects present in the crystal were investigated by transmittance, indentation and etching characterizations. The dislocation induced indentation crack lengths variations were studied. Etchmore » pits and striations observed for the selective etchants furnish significant information on growth aspects and degree of defect present in the crystal.« less

Polarized neutron imaging and three-dimensional calculation of magnetic flux trapping in bulk of superconductors

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

Treimer, Wolfgang; Ebrahimi, Omid; Karakas, Nursel

Polarized neutron radiography was used to study the three-dimensional magnetic flux distribution inside of single-crystal and polycrystalline Pb cylinders with large (cm3) volume and virtually zero demagnetization. Experiments with single crystals being in the Meissner phase (T

All-fiber mode-locked laser via short single-wall carbon nanotubes interacting with evanescent wave in photonic crystal fiber.

PubMed

Li, Yujia; Gao, Lei; Huang, Wei; Gao, Cong; Liu, Min; Zhu, Tao

2016-10-03

We report an all-fiber passively mode-locked laser based on a saturable absorber fabricated by filling short single-wall carbon nanotubes into cladding holes of grapefruit-type photonic crystal fiber. The single-wall carbon nanotube is insensitive to polarization of light for its one-dimensional structure, which suppresses the polarization dependence loss. Carbon nanotubes interact with photonic crystal fiber with ultra-weak evanescent field, which enhances the damage threshold of the saturable absorber and improves the operating stability. In our experiment, conventional soliton with a pulse duration of 1.003 ps and center wavelength of 1566.36 nm under a pump power of 240 mW is generated in a compact erbium-doped fiber laser cavity with net anomalous dispersion of -0.4102 ps². The signal to noise ratio of the fundamental frequency component is ~80 dB. The maximum average output power of the mode-locked laser reaches 9.56 mW under a pump power of 360 mW. The output power can be further improved by a higher pump power.

Silicon on-chip bandpass filters for the multiplexing of high sensitivity photonic crystal microcavity biosensors

PubMed Central

Chakravarty, Swapnajit; Yang, Chun-Ju; Wang, Zheng; Tang, Naimei; Fan, Donglei; Chen, Ray T.

2015-01-01

A method for the dense integration of high sensitivity photonic crystal (PC) waveguide based biosensors is proposed and experimentally demonstrated on a silicon platform. By connecting an additional PC waveguide filter to a PC microcavity sensor in series, a transmission passband is created, containing the resonances of the PC microcavity for sensing purpose. With proper engineering of the passband, multiple high sensitivity PC microcavity sensors can be integrated into microarrays and be interrogated simultaneously between a single input and a single output port. The concept was demonstrated with a 2-channel L55 PC biosensor array containing PC waveguide filters. The experiment showed that the sensors on both channels can be monitored simultaneously from a single output spectrum. Less than 3 dB extra loss for the additional PC waveguide filter is observed. PMID:25829549

Lessons from high-throughput protein crystallization screening: 10 years of practical experience

PubMed Central

JR, Luft; EH, Snell; GT, DeTitta

2011-01-01

Introduction X-ray crystallography provides the majority of our structural biological knowledge at a molecular level and in terms of pharmaceutical design is a valuable tool to accelerate discovery. It is the premier technique in the field, but its usefulness is significantly limited by the need to grow well-diffracting crystals. It is for this reason that high-throughput crystallization has become a key technology that has matured over the past 10 years through the field of structural genomics. Areas covered The authors describe their experiences in high-throughput crystallization screening in the context of structural genomics and the general biomedical community. They focus on the lessons learnt from the operation of a high-throughput crystallization screening laboratory, which to date has screened over 12,500 biological macromolecules. They also describe the approaches taken to maximize the success while minimizing the effort. Through this, the authors hope that the reader will gain an insight into the efficient design of a laboratory and protocols to accomplish high-throughput crystallization on a single-, multiuser-laboratory or industrial scale. Expert Opinion High-throughput crystallization screening is readily available but, despite the power of the crystallographic technique, getting crystals is still not a solved problem. High-throughput approaches can help when used skillfully; however, they still require human input in the detailed analysis and interpretation of results to be more successful. PMID:22646073

Ultratough CVD single crystal diamond and three dimensional growth thereof

DOEpatents

Hemley, Russell J [Washington, DC; Mao, Ho-kwang [Washington, DC; Yan, Chih-shiue [Washington, DC

2009-09-29

The invention relates to a single-crystal diamond grown by microwave plasma chemical vapor deposition that has a toughness of at least about 30 MPa m.sup.1/2. The invention also relates to a method of producing a single-crystal diamond with a toughness of at least about 30 MPa m.sup.1/2. The invention further relates to a process for producing a single crystal CVD diamond in three dimensions on a single crystal diamond substrate.

Development of n- and p-type Doped Perovskite Single Crystals Using Solid-State Single Crystal Growth (SSCG) Technique

DTIC Science & Technology

2017-10-09

doped BaTiO3 single crystal) could be also fabricated by using a BaTiO3 ceramics with the same compositional gradient (Fig. 8). This result has...piezoelectric applications. Compositionally PZT ceramics lie near the MPB between the tetragonal and rhombohedral phases and MPB compositions ...single crystal growth) technique are suitable to grow a variety of “n- and p-type doped” perovskite single crystals of complicated compositions . The

Crystal Growth and Characterization of the Narrow-Band-Gap Semiconductors OsPn 2 (Pn = P, As, Sb)

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

Bugaris, Daniel E.; Malliakas, Christos D.; Shoemaker, Daniel P.

2014-09-15

Using metal fluxes, crystals of the binary osmium dipnictides OsPn(2) (Pn = P, As, Sb) have been grown for the first time. Single-crystal X-ray diffraction confirms that these compounds crystallize in the marcasite structure type with orthorhombic space group Pnnm. The structure is a three-dimensional framework of corner- and edge-sharing OsPn(6) octahedra, as well as [Pn(2)(-4)] anions. Raman spectroscopy shows the presence of PP single bonds, consistent with the presence of [Pn(2)(-4)] anions and formally Os4+ cations. Optical-band-gap and high-temperature electrical resistivity measurements indicate that these materials are narrow-band-gap semiconductors. The experimentally determined Seebeck coefficients reveal that nominally undoped OsP2more » and OsSb2 are n-type semiconductors, whereas OsAs2 is p-type. Electronic band structure using density functional theory calculations shows that these compounds are indirect narrow-band-gap semiconductors. The bonding p orbitals associated with the Pn(2) dimer are below the Fermi energy, and the corresponding antibonding states are above, consistent with a PnPn single bond. Thermopower calculations using Boltzmann transport theory and constant relaxation time approximation show that these materials are potentially good thermoelectrics, in agreement with experiment.« less

Crystal growth and DFT insight on sodium para-nitrophenolate para-nitrophenol dihydrate single crystal for NLO applications

NASA Astrophysics Data System (ADS)

Selvakumar, S.; Boobalan, Maria Susai; Anthuvan Babu, S.; Ramalingam, S.; Leo Rajesh, A.

2016-12-01

Single crystals of sodium para-nitrophenolate para-nitrophenol dihydrate (SPPD) were grown by slow evaporation technique and its structure has been studied by FT-IR, FT-Raman and single crystal X-ray diffraction techniques. The optical and electrical properties were characterized by UV-Vis spectrum, and dielectric studies respectively. SPPD was thermally stable up to 128 °C as determined by TG-DTA curves. Using the Kurtz-Perry powder method, the second-harmonic generation efficiency was found to be five times to that of KDP. Third-order nonlinear response was studied using Z-scan technique with a He-Ne laser (632.8 nm) and NLO parameters such as intensity dependent refractive index, nonlinear absorption coefficient and third-order susceptibility were also estimated. The molecular geometry from X-ray experiment in the ground state has been compared using density functional theory (DFT) with appropriate basis set. The first-order hyperpolarizability also calculated using DFT approaches. Stability of the molecule arising from hyperconjugative interactions leading to its nonlinear optical activity and charge delocalization were analyzed using natural bond orbital technique. HOMO-LUMO energy gap value suggests the possibility of charge transfer within the molecule. Based on optimized ground state geometries, Natural bond orbital (NBO) analysis was performed to study donor-acceptor interactions.

Growth of high quality bulk size single crystals of inverted solubility lithium sulphate monohydrate

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

Silambarasan, A.; Rajesh, P., E-mail: rajeshp@ssn.edu.in; Ramasamy, P.

2015-06-24

The paper summarizes the processes of growing large lithium sulfate monohydrate (LSMH) single crystals. We have established a procedure to grow high quality bulk size single crystals of inverted solubility LSMH by a newly developed unidirectional crystallization technique called the Sankeranarayenan - Ramasamy (SR) method. The convective flow of crystal growth processes from solution and the conditions of growing crystals of various aspects were discussed. Good quality LSMH single crystal is grown of the size 20 mmX80 mm without cracks, localized-defects and inclusions. The as-grown crystals are suitable for piezoelectric and nonlinear optical applications.

A new method to evaluate the quality of single crystal Cu by an X-ray diffraction butterfly pattern method

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

Xu Zhenming; Guo Zhenqi; Li Jianguo

2004-12-15

A new method for the evaluation of the quality of an Ohno continuous cast (OCC) Cu single crystal by X-ray diffraction (XRD) butterfly pattern was brought forward. Experimental results show that the growth direction of single crystal Cu is inclined from both sides of the single crystal Cu rod to the axis and is axially symmetric. The degree of deviation from the [100] orientation from the crystal axis is less than 5 deg. with a casting speed 10-40 mm/min. The orientation of single crystal Cu does not have a fixed direction but is in a regular range. Moreover, the orientationmore » of stray grains in the single crystal Cu is random from continuous casting.« less

Spray printing of organic semiconducting single crystals

NASA Astrophysics Data System (ADS)

Rigas, Grigorios-Panagiotis; Payne, Marcia M.; Anthony, John E.; Horton, Peter N.; Castro, Fernando A.; Shkunov, Maxim

2016-11-01

Single-crystal semiconductors have been at the forefront of scientific interest for more than 70 years, serving as the backbone of electronic devices. Inorganic single crystals are typically grown from a melt using time-consuming and energy-intensive processes. Organic semiconductor single crystals, however, can be grown using solution-based methods at room temperature in air, opening up the possibility of large-scale production of inexpensive electronics targeting applications ranging from field-effect transistors and light-emitting diodes to medical X-ray detectors. Here we demonstrate a low-cost, scalable spray-printing process to fabricate high-quality organic single crystals, based on various semiconducting small molecules on virtually any substrate by combining the advantages of antisolvent crystallization and solution shearing. The crystals' size, shape and orientation are controlled by the sheer force generated by the spray droplets' impact onto the antisolvent's surface. This method demonstrates the feasibility of a spray-on single-crystal organic electronics.

Gallium arsenide single crystal solar cell structure and method of making

NASA Technical Reports Server (NTRS)

Stirn, Richard J. (Inventor)

1983-01-01

A production method and structure for a thin-film GaAs crystal for a solar cell on a single-crystal silicon substrate (10) comprising the steps of growing a single-crystal interlayer (12) of material having a closer match in lattice and thermal expansion with single-crystal GaAs than the single-crystal silicon of the substrate, and epitaxially growing a single-crystal film (14) on the interlayer. The material of the interlayer may be germanium or graded germanium-silicon alloy, with low germanium content at the silicon substrate interface, and high germanium content at the upper surface. The surface of the interface layer (12) is annealed for recrystallization by a pulsed beam of energy (laser or electron) prior to growing the interlayer. The solar cell structure may be grown as a single-crystal n.sup.+ /p shallow homojunction film or as a p/n or n/p junction film. A Ga(Al)AS heteroface film may be grown over the GaAs film.

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

NASA Astrophysics Data System (ADS)

Yamaki, Kazuhiro; Bamba, Yoshihiro; Irie, Akinobu

2018-03-01

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

Demonstration of single crystal growth via solid-solid transformation of a glass

DOE PAGES

Savytskii, Dmytro; Knorr, Brian; Dierolf, Volkmar; ...

2016-03-18

Many advanced technologies have relied on the availability of single crystals of appropriate material such as silicon for microelectronics or superalloys for turbine blades. Similarly, many promising materials could unleash their full potential if they were available in a single crystal form. However, the current methods are unsuitable for growing single crystals of these oftentimes incongruently melting, unstable or metastable materials. Here we demonstrate a strategy to overcome this hurdle by avoiding the gaseous or liquid phase, and directly converting glass into a single crystal. Specifically, Sb 2S 3 single crystals are grown in Sb-S-I glasses as an example ofmore » this approach. In this first unambiguous demonstration of an all-solid-state glass → crystal transformation, extraneous nucleation is avoided relative to crystal growth via spatially localized laser heating and inclusion of a suitable glass former in the composition. Lastly, the ability to fabricate patterned single-crystal architecture on a glass surface is demonstrated, providing a new class of micro-structured substrate for low cost epitaxial growth, active planar devices, etc.« less

Hydrolytic weakening in olivine single crystals

NASA Astrophysics Data System (ADS)

Tielke, Jacob A.; Zimmerman, Mark E.; Kohlstedt, David L.

2017-05-01

Deformation experiments on single crystals of San Carlos olivine under hydrous conditions were performed to investigate the microphysical processes responsible for hydrolytic weakening during dislocation creep. Hydrogen was supplied to the crystals using either talc or brucite sealed in nickel capsules with the crystal. Deformation experiments were carried out using a gas medium apparatus at temperatures of 1050° to 1250°C, a confining pressure of 300 MPa, differential stresses of 45 to 294 MPa, and resultant strain rates of 1.5 × 10-6 to 4.4 × 10-4 s-1. For talc-buffered (i.e., water and orthopyroxene-buffered) samples at high temperatures, the dependence of strain rate on stress follows a power law relationship with a stress exponent (n) of ˜2.5 and an activation energy of ˜490 kJ/mol. Brucite-buffered samples deformed faster than talc-buffered samples but contained similar hydrogen concentrations, demonstrating that strain rate is influenced by orthopyroxene activity under hydrous conditions. The values of n and dependence of strain rate on orthopyroxene activity are consistent with hydrolytic weakening occurring in the climb-controlled dislocation creep regime that is associated with deformation controlled by lattice diffusion under hydrous conditions and by pipe diffusion under anhydrous conditions. Analyses of postdeformation electron-backscatter diffraction data demonstrate that dislocations with [100] Burgers vectors are dominant in the climb-controlled regime and dislocations with [001] are dominant in the glide-controlled regime. Comparison of the experimentally determined constitutive equations demonstrates that under hydrous conditions crystals deform 1 to 2 orders of magnitude faster than under anhydrous conditions.

Nanostructure and elastic modulus of single trabecula in bovine cancellous bone.

PubMed

Yamada, Satoshi; Tadano, Shigeru; Fukuda, Sakurako

2014-11-07

We aimed to investigate the elastic modulus of trabeculae using tensile tests and assess the effects of nanostructure at the hydroxyapatite (HAp) crystal scale on the elastic modulus. In the experiments, 18 trabeculae that were at least 3mm in length in the proximal epiphysis of three adult bovine femurs were used. Tensile tests were conducted using a small tensile testing device coupled with microscopy under air-dried condition. The c-axis orientation of HAp crystals and the degree of orientation were measured by X-ray diffraction. To observe the deformation behavior of HAp crystals under tensile loading, the same tensile tests were conducted in X-ray diffraction measurements. The mineral content of specimens was evaluated using energy dispersive X-ray spectrometry. The elastic modulus of a single trabecula varied from 4.5 to 23.6 GPa, and the average was 11.5 ± 5.0 GPa. The c-axis of HAp crystals was aligned with the trabecular axis and the crystals were lineally deformed under tensile loading. The ratio of the HAp crystal strain to the tissue strain (strain ratio) had a significant correlation with the elastic modulus (r=0.79; P<0.001). However, the mineral content and the degree of orientation did not vary widely and did not correlate with the elastic modulus in this study. It suggests that the strain ratio may represent the nanostructure of a single trabecula and would determine the elastic modulus as well as mineral content and orientation. Copyright © 2014 Elsevier Ltd. All rights reserved.

Crystal growth and scintillation properties of Pr-doped SrI2 single crystals

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Ito, Tomoki; Yoshino, Masao; Yamaji, Akihiro; Ohashi, Yuji; Kurosawa, Shunsuke; Kamada, Kei; Yoshikawa, Akira

2018-04-01

Pr-doped SrI2 (Pr:SrI2) single crystals with various Pr concentrations were grown by the halide-micro-pulling-down (H-μ-PD) method, and the scintillation properties were investigated. Pr1%:SrI2 single crystal with high transparency could be grown by the H-μ-PD method while Pr2, 3 and 5%:SrI2 single crystals included some cracks and opaque parts. In the photoluminescence spectrum of the Pr1%:SrI2 single crystal, an emission peak originated from the Pr3+ ion was observed around 435 nm while the radioluminescence spectra showed an emission peak around 535 nm for the undoped SrI2 and Pr:SrI2 single crystals. Light yields of Pr1, 2, 3 and 5%:SrI2 single crystals under γ-ray irradiation were 7700, 8700, 7200 and 6700 photons/MeV, respectively. Decay times of Pr1 and 2%:SrI2 single crystals under γ-ray irradiation were 55.9 and 35.0 ns of the fast decay component, and 435 and 408 ns of the slow decay component, respectively.

Acoustic methods for high-throughput protein crystal mounting at next-generation macromolecular crystallographic beamlines.

PubMed

Roessler, Christian G; Kuczewski, Anthony; Stearns, Richard; Ellson, Richard; Olechno, Joseph; Orville, Allen M; Allaire, Marc; Soares, Alexei S; Héroux, Annie

2013-09-01

To take full advantage of advanced data collection techniques and high beam flux at next-generation macromolecular crystallography beamlines, rapid and reliable methods will be needed to mount and align many samples per second. One approach is to use an acoustic ejector to eject crystal-containing droplets onto a solid X-ray transparent surface, which can then be positioned and rotated for data collection. Proof-of-concept experiments were conducted at the National Synchrotron Light Source on thermolysin crystals acoustically ejected onto a polyimide `conveyor belt'. Small wedges of data were collected on each crystal, and a complete dataset was assembled from a well diffracting subset of these crystals. Future developments and implementation will focus on achieving ejection and translation of single droplets at a rate of over one hundred per second.

UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

PubMed

Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

2016-01-01

This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

Acoustic methods for high-throughput protein crystal mounting at next-generation macromolecular crystallographic beamlines

PubMed Central

Roessler, Christian G.; Kuczewski, Anthony; Stearns, Richard; Ellson, Richard; Olechno, Joseph; Orville, Allen M.; Allaire, Marc; Soares, Alexei S.; Héroux, Annie

2013-01-01

To take full advantage of advanced data collection techniques and high beam flux at next-generation macromolecular crystallography beamlines, rapid and reliable methods will be needed to mount and align many samples per second. One approach is to use an acoustic ejector to eject crystal-containing droplets onto a solid X-ray transparent surface, which can then be positioned and rotated for data collection. Proof-of-concept experiments were conducted at the National Synchrotron Light Source on thermolysin crystals acoustically ejected onto a polyimide ‘conveyor belt’. Small wedges of data were collected on each crystal, and a complete dataset was assembled from a well diffracting subset of these crystals. Future developments and implementation will focus on achieving ejection and translation of single droplets at a rate of over one hundred per second. PMID:23955046

Plastic deformation in nanoscale gold single crystals and open-celled nanoporous gold

NASA Astrophysics Data System (ADS)

Lee, Dongyun; Wei, Xiaoding; Zhao, Manhong; Chen, Xi; Jun, Seong C.; Hone, James; Kysar, Jeffrey W.

2007-01-01

The results of two sets of experiments to measure the elastic-plastic behaviour of gold at the nanometre length scale are reported. One set of experiments was on free-standing nanoscale single crystals of gold, and the other was on free-standing nanoscale specimens of open-celled nanoporous gold. Both types of specimens were fabricated from commercially available leaf which was either pure Au or a Au/Ag alloy following by dealloying of the Ag. Mechanical testing specimens of a 'dog-bone' shape were fabricated from the leaf using standard lithographic procedures after the leaf had been glued onto a silicon wafer. The thickness of the gauge portion of the specimens was about 100 nm, the width between 250 nm and 300 nm and the length 7 µm. The specimens were mechanically loaded with a nanoindenter (MTS) at the approximate midpoint of the gauge length. The resulting force-displacement curve of the single crystal gold was serrated and it was evident that slip localization occurred on individual slip systems; however, the early stages of the plastic deformation occurred in a non-localized manner. The results of detailed finite element analyses of the specimen suggest that the critical resolved shear stress of the gold single crystal was as high as 135 MPa which would lead to a maximum uniaxial stress of about 500 MPa after several per cent strain. The behaviour of the nanoporous gold was substantially different. It exhibited an apparent elastic behaviour until the point where it failed in an apparently brittle manner, although it is assumed that plastic deformation occurred in the ligaments prior to failure. The average elastic stiffness of three specimens was measured to be Enp = 8.8 GPa and the stress at ultimate failure averaged 190 MPa for the three specimens tested. Scaling arguments suggest that the stress in the individual ligaments could approach the theoretical shear strength. Presented at the IUTAM Symposium on Plasticity at the Micron Scale, Technical University of Denmark, Copenhagen, Denmark.

Spectroscopic investigations using density functional theory on 2-methoxy- 4(phenyliminomethyl)phenol: A non linear optical material

NASA Astrophysics Data System (ADS)

Hijas, K. M.; Madan Kumar, S.; Byrappa, K.; Geethakrishnan, T.; Jeyaram, S.; Nagalakshmi, R.

2018-03-01

Single crystals of 2-methoxy-4(phenyliminomethyl)phenol were grown from ethanol by slow evaporation solution growth technique. Single crystal X-ray diffraction experiment reveals the crystallization in orthorhombic system having non-centrosymmetric space group C2221. Geometrical optimization by density functional theory method was carried out using Gaussian program and compared with experimental results. Detailed experimental and theoretical vibrational analyses were carried out and the results were correlated to find close agreement. Thermal analyses show the material is thermally stable with a melting point of 159 °C. Natural bond orbital analysis was carried out to explain charge transfer interactions through hydrogen bonding. Relatively smaller HOMO-LUMO band gap favors the non linear optical activity of the molecule. Natural population analysis and molecular electrostatic potential calculations visualize the charge distribution in an isolated molecule. Calculated first-order molecular hyperpolarizability and preliminary second harmonic generation test carried out using Kurtz-Perry technique establish 2-methoxy-4(phenyliminomethyl)phenol crystal as a good non linear optical material. Z-scan proposes the material for reverse saturable absorption.

Growth of zinc selenide single crystals by physical vapor transport in microgravity

NASA Technical Reports Server (NTRS)

Rosenberger, Franz

1993-01-01

The goals of this research were the optimization of growth parameters for large (20 mm diameter and length) zinc selenide single crystals with low structural defect density, and the development of a 3-D numerical model for the transport rates to be expected in physical vapor transport under a given set of thermal and geometrical boundary conditions, in order to provide guidance for an advantageous conduct of the growth experiments. In the crystal growth studies, it was decided to exclusively apply the Effusive Ampoule PVT technique (EAPVT) to the growth of ZnSe. In this technique, the accumulation of transport-limiting gaseous components at the growing crystal is suppressed by continuous effusion to vacuum of part of the vapor contents. This is achieved through calibrated leaks in one of the ground joints of the ampoule. Regarding the PVT transport rates, a 3-D spectral code was modified. After introduction of the proper boundary conditions and subroutines for the composition-dependent transport properties, the code reproduced the experimentally determined transport rates for the two cases with strongest convective flux contributions to within the experimental and numerical error.

From Modeling of Plasticity in Single-Crystal Superalloys to High-Resolution X-rays Three-Crystal Diffractometer Peaks Simulation

NASA Astrophysics Data System (ADS)

Jacques, Alain

2016-12-01

The dislocation-based modeling of the high-temperature creep of two-phased single-crystal superalloys requires input data beyond strain vs time curves. This may be obtained by use of in situ experiments combining high-temperature creep tests with high-resolution synchrotron three-crystal diffractometry. Such tests give access to changes in phase volume fractions and to the average components of the stress tensor in each phase as well as the plastic strain of each phase. Further progress may be obtained by a new method making intensive use of the Fast Fourier Transform, and first modeling the behavior of a representative volume of material (stress fields, plastic strain, dislocation densities…), then simulating directly the corresponding diffraction peaks, taking into account the displacement field within the material, chemical variations, and beam coherence. Initial tests indicate that the simulated peak shapes are close to the experimental ones and are quite sensitive to the details of the microstructure and to dislocation densities at interfaces and within the soft γ phase.

Numerical study of slip system activity and crystal lattice rotation under wedge nanoindents in tungsten single crystals

NASA Astrophysics Data System (ADS)

Volz, T.; Schwaiger, R.; Wang, J.; Weygand, S. M.

2018-05-01

Tungsten is a promising material for plasma facing components in future nuclear fusion reactors. In the present work, we numerically investigate the deformation behavior of unirradiated tungsten (a body-centered cubic (bcc) single crystal) underneath nanoindents. A finite element (FE) model is presented to simulate wedge indentation. Crystal plasticity finite element (CPFE) simulations were performed for face-centered and body-centered single crystals accounting for the slip system family {110} <111> in the bcc crystal system and the {111} <110> slip family in the fcc system. The 90° wedge indenter was aligned parallel to the [1 ¯01 ]-direction and indented the crystal in the [0 1 ¯0 ]-direction up to a maximum indentation depth of 2 µm. In both, the fcc and bcc single crystals, the activity of slip systems was investigated and compared. Good agreement with the results from former investigations on fcc single crystals was observed. Furthermore, the in-plane lattice rotation in the material underneath an indent was determined and compared for the fcc and bcc single crystals.

Channeling, Volume Reection and Gamma Emission Using 14GeV Electrons in Bent Silicon Crystals

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

Benson, Brandon

2015-08-14

High energy electrons can be deflected with very tight bending radius using a bent silicon crystal. This produces gamma radiation. As these crystals can be thin, a series of bent silicon crystals with alternating direction has the potential to produce coherent gamma radiation with reasonable energy of the driving electron beam. Such an electron crystal undulator offers the prospect for higher energy radiation at lower cost than current methods. Permanent magnetic undulators like LCLS at SLAC National Accelerator Laboratory are expensive and very large (about 100 m in case of the LCLS undulator). Silicon crystals are inexpensive and compact whenmore » compared to the large magnetic undulators. Additionally, such a high energy coherent light source could be used for probing through materials currently impenetrable by x-rays. In this work we present the experimental data and analysis of experiment T523 conducted at SLAC National Accelerator Laboratory. We collected the spectrum of gamma ray emission from 14 GeV electrons on a bent silicon crystal counting single photons. We also investigated the dynamics of electron motion in the crystal i.e. processes of channeling and volume reflection at 14 GeV, extending and building off previous work. Our single photon spectrum for the amorphous crystal orientation is consistent with bremsstrahlung radiation and the volume reflection crystal orientation shows a trend consistent with synchrotron radiation at a critical energy of 740 MeV. We observe that in these two cases the data are consistent, but we make no further claims because of statistical limitations. We also extended the known energy range of electron crystal dechanneling length and channeling efficiency to 14 GeV.« less

Feasibilty analyses of electroepitaxial research and development accomodations. Volume 1: Accommodations assessment

NASA Technical Reports Server (NTRS)

1983-01-01

A preliminary assessment of the feasibility of accommodating the on-orbit R&D requirements for electroepitaxial crystal growth using the Orbiter middeck, the Materials Experiment Assembly or the Get-Away Special cans was performed. The study is based on the proposed electroepitaxial growth of single crystals of gallium arsenide (GaAs). Baseline R&D requirements, synthesizing furnace and facility conceptual design requirements, accommodation requirements, preliminary compatibility assessments are established. The systems engineering approach employed for the individual assessments is outlined.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Astrophysics Data System (ADS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-09-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

A preliminary review of organic materials single crystal growth by the Czochralski technique

NASA Technical Reports Server (NTRS)

Penn, B. G.; Shields, A. W.; Frazier, D. O.

1988-01-01

The growth of single crystals of organic compounds by the Czochralski method is reviewed. From the literature it is found that single crystals of benzil, a nonlinear optical material with a d sub 11 value of 11.2 + or - 1.5 x d sub 11 value of alpha quartz, has fewer dislocations than generally contained in Bridgman crystals. More perfect crystals were grown by repeated Czochralski growth. This consists of etching away the defect-containing portion of a Czochralski grown crystal and using it as a seed for further growth. Other compounds used to grow single crystals are benzophenone, 12-tricosanone (laurone), and salol. The physical properties, growth apparatus, and processing conditions presented in the literature are discussed. Moreover, some of the possible advantages of growing single crystals of organic compounds in microgravity to obtain more perfect crystals than on Earth are reviewed.

Mechanochemical Synthesis of Carbon Nanothread Single Crystals.

PubMed

Li, Xiang; Baldini, Maria; Wang, Tao; Chen, Bo; Xu, En-Shi; Vermilyea, Brian; Crespi, Vincent H; Hoffmann, Roald; Molaison, Jamie J; Tulk, Christopher A; Guthrie, Malcolm; Sinogeikin, Stanislav; Badding, John V

2017-11-15

Synthesis of well-ordered reduced dimensional carbon solids with extended bonding remains a challenge. For example, few single-crystal organic monomers react under topochemical control to produce single-crystal extended solids. We report a mechanochemical synthesis in which slow compression at room temperature under uniaxial stress can convert polycrystalline or single-crystal benzene monomer into single-crystalline packings of carbon nanothreads, a one-dimensional sp 3 carbon nanomaterial. The long-range order over hundreds of microns of these crystals allows them to readily exfoliate into fibers. The mechanochemical reaction produces macroscopic single crystals despite large dimensional changes caused by the formation of multiple strong, covalent C-C bonds to each monomer and a lack of reactant single-crystal order. Therefore, it appears not to follow a topochemical pathway, but rather one guided by uniaxial stress, to which the nanothreads consistently align. Slow-compression room-temperature synthesis may allow diverse molecular monomers to form single-crystalline packings of polymers, threads, and higher dimensional carbon networks.

ANTIFERROMAGNETIC SPIN RESONANCE OF COBR2.6H20,

DTIC Science & Technology

Electron spin resonance experiments were carried out on single crystals of CoBr2.6H20 at temperatures from 1.2 to 4.2K, using a microwave transmission spectrometer over a range of frequencies from 29 to 59 kMc .

Study of FES/CAST/HGS

NASA Technical Reports Server (NTRS)

Workman, Gary L.; Cummings, Rick; Jones, Brian

1992-01-01

The microgravity materials processing program has been instrumental in providing the crystal growth community with an experimental environment to better understand the phenomena associated with the growing of crystals. In many applications one may pursue the growth of large single crystals which cannot be grown on earth due to convective driven flows. A microgravity environment is characterized by neither convection of buoyancy. Consequently superior crystals are able to be grown in space. On the other hand, since neither convection nor buoyancy dominates the fluid flow in a microgravity environment, then lesser dominating phenomena can affect crystal growth, such as surface driven flows or diffusion limited solidification. In the case of experiments that are to be flown in space using the Fluid Experiments System (FES), diffusion limited growth should be the dominating phenomenon. The use of holographic and Schlieren optical techniques for studying the concentration gradients in solidification processes has been used by several investigators over the years. The Holographic Ground System (HGS) facility at MSFC has been a primary resource in researching this capability. Consequently scientific personnel have been able to utilize these techniques in both ground based research and in space experiments. An important event in the scientific utilization of the HGS facilities was the TGS (triglycine sulfate) Crystal Growth and the Casting and Solidification Technology (CAST) experiments that were flown on the International Microgravity Lab (IML) mission in March of this year. The preparation and processing of these space observations are the primary experiments reported in this work. This project provides some ground-based studies to optimize on the holographic techniques used to acquire information about the crystal growth processes flown on IML. Since the ground-based studies will be compared with the space-based experimental results, it is necessary to conduct sufficient ground based studies to best determine how the experiment in space worked. The current capabilities in computer based systems for image processing and numerical computation have certainly assisted in those efforts. As anticipated, this study has certainly shown that these advanced computing capabilities are helpful in the data analysis of such experiments.

Hitting the target: fragment screening with acoustic in situ co-crystallization of proteins plus fragment libraries on pin-mounted data-collection micromeshes.

PubMed

Yin, Xingyu; Scalia, Alexander; Leroy, Ludmila; Cuttitta, Christina M; Polizzo, Gina M; Ericson, Daniel L; Roessler, Christian G; Campos, Olven; Ma, Millie Y; Agarwal, Rakhi; Jackimowicz, Rick; Allaire, Marc; Orville, Allen M; Sweet, Robert M; Soares, Alexei S

2014-05-01

Acoustic droplet ejection (ADE) is a powerful technology that supports crystallographic applications such as growing, improving and manipulating protein crystals. A fragment-screening strategy is described that uses ADE to co-crystallize proteins with fragment libraries directly on MiTeGen MicroMeshes. Co-crystallization trials can be prepared rapidly and economically. The high speed of specimen preparation and the low consumption of fragment and protein allow the use of individual rather than pooled fragments. The Echo 550 liquid-handling instrument (Labcyte Inc., Sunnyvale, California, USA) generates droplets with accurate trajectories, which allows multiple co-crystallization experiments to be discretely positioned on a single data-collection micromesh. This accuracy also allows all components to be transferred through small apertures. Consequently, the crystallization tray is in equilibrium with the reservoir before, during and after the transfer of protein, precipitant and fragment to the micromesh on which crystallization will occur. This strict control of the specimen environment means that the crystallography experiments remain identical as the working volumes are decreased from the few microlitres level to the few nanolitres level. Using this system, lysozyme, thermolysin, trypsin and stachydrine demethylase crystals were co-crystallized with a small 33-compound mini-library to search for fragment hits. This technology pushes towards a much faster, more automated and more flexible strategy for structure-based drug discovery using as little as 2.5 nl of each major component.

Hitting the target: fragment screening with acoustic in situ co-crystallization of proteins plus fragment libraries on pin-mounted data-collection micromeshes

PubMed Central

Yin, Xingyu; Scalia, Alexander; Leroy, Ludmila; Cuttitta, Christina M.; Polizzo, Gina M.; Ericson, Daniel L.; Roessler, Christian G.; Campos, Olven; Ma, Millie Y.; Agarwal, Rakhi; Jackimowicz, Rick; Allaire, Marc; Orville, Allen M.; Sweet, Robert M.; Soares, Alexei S.

2014-01-01

Acoustic droplet ejection (ADE) is a powerful technology that supports crystallographic applications such as growing, improving and manipulating protein crystals. A fragment-screening strategy is described that uses ADE to co-crystallize proteins with fragment libraries directly on MiTeGen MicroMeshes. Co-crystallization trials can be prepared rapidly and economically. The high speed of specimen preparation and the low consumption of fragment and protein allow the use of individual rather than pooled fragments. The Echo 550 liquid-handling instrument (Labcyte Inc., Sunnyvale, California, USA) generates droplets with accurate trajectories, which allows multiple co-crystallization experiments to be discretely positioned on a single data-collection micromesh. This accuracy also allows all components to be transferred through small apertures. Consequently, the crystallization tray is in equilibrium with the reservoir before, during and after the transfer of protein, precipitant and fragment to the micromesh on which crystallization will occur. This strict control of the specimen environment means that the crystallography experiments remain identical as the working volumes are decreased from the few microlitres level to the few nanolitres level. Using this system, lysozyme, thermolysin, trypsin and stachydrine demethylase crystals were co-crystallized with a small 33-compound mini-library to search for fragment hits. This technology pushes towards a much faster, more automated and more flexible strategy for structure-based drug discovery using as little as 2.5 nl of each major component. PMID:24816088

Microstructure and pinning properties of hexagonal-disc shaped single crystalline MgB2

NASA Astrophysics Data System (ADS)

Jung, C. U.; Kim, J. Y.; Chowdhury, P.; Kim, Kijoon H.; Lee, Sung-Ik; Koh, D. S.; Tamura, N.; Caldwell, W. A.; Patel, J. R.

2002-11-01

We synthesized hexagonal-disc-shaped MgB2 single crystals under high-pressure conditions and analyzed the microstructure and pinning properties. The lattice constants and the Laue pattern of the crystals from x-ray micro-diffraction showed the crystal symmetry of MgB2. A thorough crystallographic mapping within a single crystal showed that the edge and c axis of hexagonal-disc shape exactly matched the [101¯0] and the [0001] directions of the MgB2 phase. Thus, these well-shaped single crystals may be the best candidates for studying the direction dependences of the physical properties. The magnetization curve and the magnetic hysteresis curve for these single crystals showed the existence of a wide reversible region and weak pinning properties, which supported our single crystals being very clean.

Growth and microtopographic study of CuInSe{sub 2} single crystals

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

Chauhan, Sanjaysinh M.; Chaki, Sunil, E-mail: sunilchaki@yahoo.co.in; Deshpande, M. P.

2016-05-23

The CuInSe{sub 2} single crystals were grown by chemical vapour transport (CVT) technique using iodine as transporting agent. The elemental composition of the as-grown CuInSe{sub 2} single crystals was determined by energy dispersive analysis of X-ray (EDAX). The unit cell crystal structure and lattice parameters were determined by X-ray diffraction (XRD) technique. The surface microtopographic study of the as-grown CuInSe{sub 2} single crystals surfaces were done to study the defects, growth mechanism, etc. of the CVT grown crystals.

Method for the preparation of inorganic single crystal and polycrystalline electronic materials

NASA Technical Reports Server (NTRS)

Groves, W. O. (Inventor)

1969-01-01

Large area, semiconductor crystals selected from group 3-5 compounds and alloys are provided for semiconductor device fabrication by the use of a selective etching operation which completely removes the substrate on which the desired crystal was deposited. The substrate, selected from the same group as the single crystal, has a higher solution rate than the epitaxial single crystal which is essentially unaffected by the etching solution. The preparation of gallium phosphide single crystals using a gallium arsenide substrate and a concentrated nitric acid etching solution is described.

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, fromSphingobiumsp. SYK-6 was crystallized by the hanging-drop vapour-diffusion method. However, the obtainedP3 121 orP3 221 crystals, which diffracted to 2.5–3.3 Å resolution, were hemihedrally twinned. To overcome the twinning problem, microseeding usingP3 121/P3 221 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 groupP2 12 12, with unit-cell parametersa= 102.0,b= 117.3,c= 128.1 Å. TheP2 12 12 crystals diffracted to better than 2.0 Å resolution after optimizing the cryoconditions. Phasing using the single anomalous diffractionmore » 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

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

Porosity Evolution in a Creeping Single Crystal (Preprint)

DTIC Science & Technology

2012-08-01

1] indicated that the growth of initially present processing induced voids in a nickel based single crystal superalloy played a significant role in...processing induced voids in a nickel based single crystal superalloy played a significant role in limiting creep life. Also, creep tests on single...experimental observations of creep deformation and failure of a nickel based single crystal superalloy, [1, 2]. Metallographic observations have shown that Ni

Lattice Rotation Patterns and Strain Gradient Effects in Face-Centered-Cubic Single Crystals Under Spherical Indentation

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

Gao, Y. F.; Larson, B. C.; Lee, J. H.

Strain gradient effects are commonly modeled as the origin of the size dependence of material strength, such as the dependence of indentation hardness on contact depth and spherical indenter radius. However, studies on the microstructural comparisons of experiments and theories are limited. First, we have extended a strain gradient Mises-plasticity model to its crystal plasticity version and implemented a finite element method to simulate the load-displacement response and the lattice rotation field of Cu single crystals under spherical indentation. The strain gradient simulations demonstrate that the forming of distinct sectors of positive and negative angles in the lattice rotation fieldmore » is governed primarily by the slip geometry and crystallographic orientations, depending only weakly on strain gradient effects, although hardness depends strongly on strain gradients. Second, the lattice rotation simulations are compared quantitatively with micron resolution, three-dimensional X-ray microscopy (3DXM) measurements of the lattice rotation fields under 100mN force, 100 mu m radius spherical indentations in < 111 >, < 110 >, and < 001 > oriented Cu single crystals. Third, noting the limitation of continuum strain gradient crystal plasticity models, two-dimensional discrete dislocation simulation results suggest that the hardness in the nanocontact regime is governed synergistically by a combination of strain gradients and source-limited plasticity. However, the lattice rotation field in the discrete dislocation simulations is found to be insensitive to these two factors but to depend critically on dislocation obstacle densities and strengths.« less

Splitting Fermi Surfaces and Heavy Electronic States in Non-Centrosymmetric U3Ni3Sn4

NASA Astrophysics Data System (ADS)

Maurya, Arvind; Harima, Hisatomo; Nakamura, Ai; Shimizu, Yusei; Homma, Yoshiya; Li, DeXin; Honda, Fuminori; Sato, Yoshiki J.; Aoki, Dai

2018-04-01

We report the single-crystal growth of the non-centrosymmetric paramagnet U3Ni3Sn4 by the Bridgman method and the Fermi surface properties detected by de Haas-van Alphen (dHvA) experiments. We have also investigated single-crystal U3Ni3Sn4 by single-crystal X-ray diffraction, magnetization, electrical resistivity, and heat capacity measurements. The angular dependence of the dHvA frequencies reveals many closed Fermi surfaces, which are nearly spherical in topology. The experimental results are in good agreement with local density approximation (LDA) band structure calculations based on the 5f-itinerant model. The band structure calculation predicts many Fermi surfaces, mostly with spherical shape, derived from 12 bands crossing the Fermi energy. To our knowledge, the splitting of Fermi surfaces due to the non-centrosymmetric crystal in 5f-electron systems is experimentally detected for the first time. The temperature dependence of the dHvA amplitude reveals a large cyclotron effective mass of up to 35 m0, indicating the heavy electronic state of U3Ni3Sn4 due to the proximity of the quantum critical point. From the field dependence of the dHvA amplitude, a mean free path of conduction electrons of up to 1950 Å is detected, reflecting the good quality of the grown crystal. The small splitting energy related to the antisymmetric spin-orbit interaction is most likely due to the large cyclotron effective mass.

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

Lumpkin, A. H.; Macrander, A. T.

Using the 1-BM-C beamline at the Advanced Photon Source (APS), we have performed the initial indirect x - ray imaging point-spread-function (PSF) test of a unique 88-mm diameter YAG:Ce single crystal of only 100 - micron thickness. The crystal was bonded to a fiber optic plat e (FOP) for mechanical support and to allow the option for FO coupling to a large format camera. This configuration resolution was compared to that of self - supported 25-mm diameter crystals, with and without an Al reflective coating. An upstream monochromator was used to select 17-keV x-rays from the broadband APS bending magnetmore » source of synchrotron radiation. The upstream , adjustable Mo collimators were then used to provide a series of x-ray source transverse sizes from 200 microns down to about 15-20 microns (FWHM) at the crystal surface. The emitted scintillator radiation was in this case lens coupled to the ANDOR Neo sCMOS camera, and the indirect x-ray images were processed offline by a MATLAB - based image processing program. Based on single Gaussian peak fits to the x-ray image projected profiles, we observed a 10.5 micron PSF. This sample thus exhibited superior spatial resolution to standard P43 polycrystalline phosphors of the same thickness which would have about a 100-micron PSF. Lastly, this single crystal resolution combined with the 88-mm diameter makes it a candidate to support future x-ray diffraction or wafer topography experiments.« less

Nuclear Resonance Scattering of Circularly Polarized SR

NASA Astrophysics Data System (ADS)

Szymanski, K.; Satula, D.; Dobrzynski, L.; Kalska, B.

2004-09-01

Results of the experiments with nuclear resonance scattering of synchrotron radiation aiming at construction of the circularly polarized beam suitable for nuclear hyperfine studies are reported. Si(4 0 0) single crystal slab, 100 μ m thick, was used as a quarter wave plate. Observed twofold reduction of the intensity in proposed geometry is due to the Si crystal itself. Hyperfine interactions are used to probe polarization state of the synchrotron beam. Too large angular beam divergence did not allow for achieving full circular polarization of photons. Consequently, further experiments are proposed to overcame beam divergence problems. A number of calculations presented in the paper show that cheap and easily available Si plate can serve as an effective desired polarizer.

HYSPEC : A CRYSTAL TIME OF FLIGHT HYBRID SPECTROMETER FOR THE SPALLATION NEUTRON SOURCE.

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

SHAPIRO,S.M.; ZALIZNYAK,I.A.

2002-12-30

This document lays out a proposal by the Instrument Development Team (IDT) composed of scientists from leading Universities and National Laboratories to design and build a conceptually new high-flux inelastic neutron spectrometer at the pulsed Spallation Neutron Source (SNS) at Oak Ridge. This instrument is intended to supply users of the SNS and scientific community, of which the IDT is an integral part, with a platform for ground-breaking investigations of the low-energy atomic-scale dynamical properties of crystalline solids. It is also planned that the proposed instrument will be equipped with a polarization analysis capability, therefore becoming the first polarized beammore » inelastic spectrometer in the SNS instrument suite, and the first successful polarized beam inelastic instrument at a pulsed spallation source worldwide. The proposed instrument is designed primarily for inelastic and elastic neutron spectroscopy of single crystals. In fact, the most informative neutron scattering studies of the dynamical properties of solids nearly always require single crystal samples, and they are almost invariably flux-limited. In addition, in measurements with polarization analysis the available flux is reduced through selection of the particular neutron polarization, which puts even more stringent limits on the feasibility of a particular experiment. To date, these investigations have mostly been carried out on crystal spectrometers at high-flux reactors, which usually employ focusing Bragg optics to concentrate the neutron beam on a typically small sample. Construction at Oak Ridge of the high-luminosity spallation neutron source, which will provide intense pulsed neutron beams with time-averaged fluxes equal to those at medium-flux reactors, opens entirely new opportunities for single crystal neutron spectroscopy. Drawing upon experience acquired during decades of studies with both crystal and time-of-flight (TOF) spectrometers, the IDT has developed a conceptual design for a focused-beam, hybrid time-of-flight instrument with a crystal monochromator for the SNS called HYSPEC (an acronym for hybrid spectrometer). The proposed instrument has a potential to collect data more than an order of magnitude faster than existing steady-source spectrometers over a wide range of energy transfer ({h_bar}{omega}) and momentum transfer (Q) space, and will transform the way that data in elastic and inelastic single-crystal spectroscopy are collected. HYSPEC is optimized to provide the highest neutron flux on sample in the thermal and epithermal neutron energy ranges at a good-to-moderate energy resolution. By providing a flux on sample several times higher than other inelastic instruments currently planned for the SNS, the proposed instrument will indeed allow unique ground-breaking measurements, and will ultimately make polarized beam studies at a pulsed spallation source a realistic possibility.« less

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

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

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

2016-05-06

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

Crystallography of the NiHfSi Phase in a NiAl (0.5 Hf) Single-Crystal Alloy

NASA Technical Reports Server (NTRS)

Garg, A.; Noebe, R. D.; Darolia, R.

1996-01-01

Small additions of Hf to conventionally processed NiAl single crystals result in the precipitation of a high density of cuboidal G-phase along with a newly identified silicide phase. Both of these phases form in the presence of Si which is not an intentional alloying addition but is a contaminant resulting from contact with the ceramic shell molds during directional solidification of the single-crystal ingots. The morphology, crystal structure and Orientation Relationship (OR) of the silicide phase in a NiAl (0.5 at.%Hf) single-crystal alloy have been determined using transmission electron microscopy, electron microdiffraction and energy dispersive X-ray spectroscopy. Qualitative elemental analysis and indexing of the electron microdiffraction patterns from the new phase indicate that it is an orthorhombic NiHfSi phase with unit cell parameters, a = 0.639 nm, b = 0.389 nm and c = 0.72 nm, and space group Pnma. The NiHfSi phase forms as thin rectangular plates on NiAl/111/ planes with an OR that is given by NiHfSi(100))(parallel) NiAl(111) and NiHfSi zone axes(010) (parallel) NiAl zone axes (101). Twelve variants of the NiHfSi phase were observed in the alloy and the number of variants and rectangular morphology of NiHfSi plates are consistent with symmetry requirements. Quenching experiments indicate that nucleation of the NiHfSi phase in NiAI(Hf) alloys is aided by the formation of NiAl group of zone axes (111) vacancy loops that form on the NiAl /111/ planes.

Calculations of single crystal elastic constants for yttria partially stabilised zirconia from powder diffraction data

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

Lunt, A. J. G., E-mail: alexander.lunt@eng.ox.ac.uk; Xie, M. Y.; Baimpas, N.

2014-08-07

Yttria Stabilised Zirconia (YSZ) is a tough, phase-transforming ceramic that finds use in a wide range of commercial applications from dental prostheses to thermal barrier coatings. Micromechanical modelling of phase transformation can deliver reliable predictions in terms of the influence of temperature and stress. However, models must rely on the accurate knowledge of single crystal elastic stiffness constants. Some techniques for elastic stiffness determination are well-established. The most popular of these involve exploiting frequency shifts and phase velocities of acoustic waves. However, the application of these techniques to YSZ can be problematic due to the micro-twinning observed in larger crystals.more » Here, we propose an alternative approach based on selective elastic strain sampling (e.g., by diffraction) of grain ensembles sharing certain orientation, and the prediction of the same quantities by polycrystalline modelling, for example, the Reuss or Voigt average. The inverse problem arises consisting of adjusting the single crystal stiffness matrix to match the polycrystal predictions to observations. In the present model-matching study, we sought to determine the single crystal stiffness matrix of tetragonal YSZ using the results of time-of-flight neutron diffraction obtained from an in situ compression experiment and Finite Element modelling of the deformation of polycrystalline tetragonal YSZ. The best match between the model predictions and observations was obtained for the optimized stiffness values of C11 = 451, C33 = 302, C44 = 39, C66 = 82, C12 = 240, and C13 = 50 (units: GPa). Considering the significant amount of scatter in the published literature data, our result appears reasonably consistent.« less

Ultrathin solution-processed single crystals of thiophene-phenylene co-oligomers for organic field-effect devices

NASA Astrophysics Data System (ADS)

Glushkova, Anastasia V.; Poimanova, Elena Yu.; Bruevich, Vladimir V.; Luponosov, Yuriy N.; Ponomarenko, Sergei A.; Paraschuk, Dmitry Yu.

2017-08-01

Thiophene-phenylene co-oligomers (TPCO) single crystals are promising materials for organic light-emitting devices, e.g., light-emitting transistors (OLETs), due to their ability to combine high luminescence and efficient charge transport. However, optical confinement in platy single crystals strongly decreases light emission from their top surface degrading the device performance. To avoid optical waveguiding, single crystals thinner than 100 nm would be beneficial. Herein, we report on solution-processed ultrathin single crystals of TPCO and study their charge transport properties. As materials we used 1,4-bis(5'-hexyl-2,2'-bithiophene-5-yl)benzene (DH-TTPTT) and 1,4-bis(5'-decyl-2,2'-bithiophene-5-yl)benzene (DD-TTPTT). The ultrathin single crystals were studied by optical polarization, atomic-force, and transmission electron microscopies, and as active layers in organic field effect transistors (OFET). The OFET hole mobility was increased tenfold for the oligomer with longer alkyl substituents (DD-TTPTT) reaching 0.2 cm2/Vs. Our studies of crystal growth indicate that if the substrate is wetted, it has no significant effect on the crystal growth. We conclude that solution-processed ultrathin TPCO single crystals are a promising platform for organic optoelectronic field-effect devices.

Nanoparticles Incorporated inside Single-Crystals: Enhanced Fluorescent Properties

DOE PAGES

Liu, Yujing; Zang, Huidong; Wang, Ling; ...

2016-09-25

Incorporation of guest materials inside single-crystalline hosts leads to single-crystal composites that have become more and more frequently seen in both biogenic and synthetic crystals. The unique composite structure together with long-range ordering promises special properties that are, however, less often demonstrated. In this study, we examine the fluorescent properties of quantum dots (QDs) and polymer dots (Pdots) encapsulated inside the hosts of calcite single-crystals. Two CdTe QDs and two Pdots are incorporated into growing calcite crystals, as the QDs and Pdots are dispersed in the crystallization media of agarose gels. As a result, enhanced fluorescent properties are obtained frommore » the QDs and Pdots inside calcite single-crystals with greatly improved photostability and significantly prolonged fluorescence lifetime, compared to those in solutions and gels. Particularly, the fluorescence lifetime increases by 0.5-1.6 times after the QDs or Pdots are incorporated. The enhanced fluorescent properties indicate the advantages of encapsulation by single-crystal hosts that provide dense shells to isolate the fluorescent nanoparticles from atmosphere. As such, this work has implications for advancing the research of single-crystal composites toward their functional design.« less

Solar cell structure incorporating a novel single crystal silicon material

DOEpatents

Pankove, Jacques I.; Wu, Chung P.

1983-01-01

A novel hydrogen rich single crystal silicon material having a band gap energy greater than 1.1 eV can be fabricated by forming an amorphous region of graded crystallinity in a body of single crystalline silicon and thereafter contacting the region with atomic hydrogen followed by pulsed laser annealing at a sufficient power and for a sufficient duration to recrystallize the region into single crystal silicon without out-gassing the hydrogen. The new material can be used to fabricate semiconductor devices such as single crystal silicon solar cells with surface window regions having a greater band gap energy than that of single crystal silicon without hydrogen.

Crystal growth, structural, thermal and mechanical behavior of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) single crystals.

PubMed

Mahadevan, M; Ramachandran, K; Anandan, P; Arivanandhan, M; Bhagavannarayana, G; Hayakawa, Y

2014-12-10

Single crystals of l-arginine 4-nitrophenolate 4-nitrophenol dihydrate (LAPP) have been grown successfully from the solution of l-arginine and 4-nitrophenol. Slow evaporation of solvent technique was adopted to grow the bulk single crystals. Single crystal X-ray diffraction analysis confirms the grown crystal has monoclinic crystal system with space group of P21. Powder X-ray diffraction analysis shows the good crystalline nature. The crystalline perfection of the grown single crystals was analyzed by HRXRD by employing a multicrystal X-ray diffractometer. The functional groups were identified from proton NMR spectroscopic analysis. Linear and nonlinear optical properties were determined by UV-Vis spectrophotometer and Kurtz powder technique respectively. It is found that the grown crystal has no absorption in the green wavelength region and the SHG efficiency was found to be 2.66 times that of the standard KDP. The Thermal stability of the crystal was found by obtaining TG/DTA curve. The mechanical behavior of the grown crystal has been studied by Vicker's microhardness method. Copyright © 2014 Elsevier B.V. All rights reserved.

Friction and wear of metals with a single-crystal abrasive grit of silicon carbide: Effect of shear strength of metal

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1978-01-01

Sliding friction experiments were conducted with spherical, single-crystal silicon carbide riders in contact with various metals and with metal riders in contact with silicon carbide flats. Results indicate that: (1) the friction force in the plowing of metal and (2) the groove height (corresponding to the volume of the groove) are related to the shear strength of the metal. That is, they decrease linearly as the shear strength of the bulk metal increases. Grooves are formed in metals primarily from plastic deformation, with occasional metal removal. The relation between the groove width D and the load W can be expressed by W = kD, superscript n which satisfies Meyer's law.

Lightweight and High-Resolution Single Crystal Silicon Optics for X-ray Astronomy

NASA Technical Reports Server (NTRS)

Zhang, William W.; Biskach, Michael P.; Chan, Kai-Wing; Mazzarella, James R.; McClelland, Ryan S.; Riveros, Raul E.; Saha, Timo T.; Solly, Peter M.

2016-01-01

We describe an approach to building mirror assemblies for next generation X-ray telescopes. It incorporates knowledge and lessons learned from building existing telescopes, including Chandra, XMM-Newton, Suzaku, and NuSTAR, as well as from our direct experience of the last 15 years developing mirror technology for the Constellation-X and International X-ray Observatory mission concepts. This approach combines single crystal silicon and precision polishing, thus has the potential of achieving the highest possible angular resolution with the least possible mass. Moreover, it is simple, consisting of several technical elements that can be developed independently in parallel. Lastly, it is highly amenable to mass production, therefore enabling the making of telescopes of very large photon collecting areas.

Friction and wear of single-crystal manganese-zinc ferrite

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1979-01-01

Sliding friction experiments were conducted with single crystal manganese-zinc ferrite in contact with itself and with transition metals. Results indicate mating highest atomic density directions (110) on matched crystallographic planes exhibit the lowest coefficient of friction, indicating that direction is important in the friction behavior of ferrite. Matched parallel high atomic density planes and crystallographic directions at the interface exhibit low coefficients of friction. The coefficients of friction for ferrite in contact with various metals are related to the relative chemical activity of these metals. The more active the metal, the higher the coefficient of friction. Cracking and the formation of hexagon- and rectangular-shaped platelet wear debris due to cleavages of (110) planes are observed on the ferrite surfaces as a result of sliding.

Thermally Assisted Macroscopic Quantum Resonance on a Single-Crystal of Mn12-ac

NASA Astrophysics Data System (ADS)

Lionti, F.; Thomas, L.; Ballou, R.; Wernsdorfer, W.; Barbara, B.; Sulpice, A.; Sessoli, R.; Gatteschi, D.

1997-03-01

Magnetization measurements have been performed on a single mono-crystal of the molecule Mn12-acetate (L. Thomas, F. Lionti, R. Ballou, R. Sessoli, D. Gatteschi and B. Barbara, Nature, 383, 145 (1996).). Steps were observed in the hysteresis loop for values of the applied field at which level crossings of the collective spin states of each manganese clusters take place. The influence of quartic terms is taken into account. At these fields, the magnetization relaxes at short time scales, being otherwise essentially blocked. This novel behavior is interpreted in terms of resonant quantum tunneling of the magnetization from thermally activated energy levels. Hysteresis loop measurements performed for different field orientations and ac-susceptibility experiments, confirm general trends of this picture.

Effect of a High Magnetic Field on γ' Phase for Ni-Based Single Crystal Superalloy During Directional Solidification

NASA Astrophysics Data System (ADS)

Xuan, Weidong; Lan, Jian; Zhao, Dengke; Li, Chuanjun; Shang, Xingfu; Zhong, Yunbo; Li, Xi; Ren, Zhongming

2018-05-01

The effect of a high magnetic field on the γ' phase of Ni-based single crystal superalloy during directional solidification is investigated experimentally. The results clearly indicate that the magnetic field significantly reduces the γ' phase size. Further, the quenching experiment is carried out, and the results found that the length of mushy zone is obviously decreased under a high magnetic field. Based on both experimental results and nucleation mechanism, it is found that the decrease of γ' phase size should be attributed to the fact that a high magnetic field causes the increase of temperature gradient in front of solid/liquid interface and leads to the increase of undercooling of γ' phase.

Microtube-Czochralski technique (μT-CZ):. a novel way of seeding the melt to grow bulk single crystal

NASA Astrophysics Data System (ADS)

Sankaranarayanan, K.; Ramasamy, P.

1998-09-01

A novel microtube seeding has been proposed in the conventional Czochralski pulling technique to grow a bulk single crystal. The versatility of the technique has been shown by adopting this method for the growth of benzil. Benzil single crystals having hexagonal facets are grown by this technique called the microtube-Czochralski technique (μT-CZ). Due to capillary rise, a fine column of melt was crystallized inside the microtube, which leads to the formation of the single crystal nucleation and ends up with hexagonal morphology. The reproducibility for getting single crystal is about 80%. It is evident that this technique is more viable to grow a bulk single crystal from the melt without a pregrown-seed. Further, the proposed μT-CZ technique can also be extended to other newer materials with the proper choice of the microtube.

Effect of Chain Conformation on the Single-Molecule Melting Force in Polymer Single Crystals: Steered Molecular Dynamics Simulations Study.

PubMed

Feng, Wei; Wang, Zhigang; Zhang, Wenke

2017-02-28

Understanding the relationship between polymer chain conformation as well as the chain composition within the single crystal and the mechanical properties of the corresponding single polymer chain will facilitate the rational design of high performance polymer materials. Here three model systems of polymer single crystals, namely poly(ethylene oxide) (PEO), polyethylene (PE), and nylon-66 (PA66) have been chosen to study the effects of chain conformation, helical (PEO) versus planar zigzag conformation (PE, PA66), and chain composition (PE versus PA66) on the mechanical properties of a single polymer chain. To do that, steered molecular dynamics simulations were performed on those polymer single crystals by pulling individual polymer chains out of the crystals. Our results show that the patterns of force-extension curve as well as the chain moving mode are closely related to the conformation of the polymer chain in the single crystal. In addition, hydrogen bonds can enhance greatly the force required to stretch the polymer chain out of the single crystal. The dynamic breaking and reformation of multivalent hydrogen bonds have been observed for the first time in PA66 at the single molecule level.

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

Patel, J. R.

We synthesized hexagonal-disc-shaped MgB{sub 2} single crystals under high-pressure conditions and analyzed the microstructure and pinning properties. The lattice constants and the Laue pattern of the crystals from X-ray micro-diffraction showed the crystal symmetry of MgB{sub 2}. A thorough crystallographic mapping within a single crystal showed that the edge and c-axis of hexagonal-disc shape exactly matched the (10-10) and the (0001) directions of the MgB{sub 2} phase. Thus, these well-shaped single crystals may be the best candidates for studying the direction dependences of the physical properties. The magnetization curve and the magnetic hysteresis for these single crystals showed the existencemore » of a wide reversible region and weak pinning properties, which supported our single crystals being very clean.« less

Characterization of high energy Xe ion irradiation effects in single crystal molybdenum with depth-resolved synchrotron microbeam diffraction

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

Yun, Di; Miao, Yinbin; Xu, Ruqing

2016-04-01

Microbeam X-ray diffraction experiments were conducted at beam line 34-ID of the Advanced Photon Source (APS) on fission fragment energy Xe heavy ion irradiated single crystal Molybdenum (Mo). Lattice strain measurements were obtained with a depth resolution of 0.7 mu m, which is critical in resolving the peculiar heterogeneity of irradiation damage associated with heavy ion irradiation. Q-space diffraction peak shift measurements were correlated with lattice strain induced by the ion irradiations. Transmission electron microscopy (TEM) characterizations were performed on the as-irradiated materials as well. Nanometer sized Xe bubble microstructures were observed via TEM. Molecular Dynamics (MD) simulations were performedmore » to help interpret the lattice strain measurement results from the experiment. This study showed that the irradiation effects by fission fragment energy Xe ion irradiations can be collaboratively understood with the depth resolved X-ray diffraction and TEM measurements under the assistance of MD simulations. (c) 2015 Elsevier B.V. All rights reserved.« less

Crossover from Commensurate to Incommensurate Antiferromagnetism in Stoichiometric NaFeAs Revealed by Single-Crystal 23Na,75As-NMR Experiments

NASA Astrophysics Data System (ADS)

Kitagawa, Kentaro; Mezaki, Yuji; Matsubayashi, Kazuyuki; Uwatoko, Yoshiya; Takigawa, Masashi

2011-03-01

We report the results of 23Na and 75As nuclear magnetic resonance (NMR) experiments on a self-flux grown high-quality single crystal of stoichiometric NaFeAs. The NMR spectra reveal a tetragonal to twinned-orthorhombic structural phase transition at TO = 57 K and an antiferromagnetic (AF) transition at TAF = 45 K. The divergent behavior of nuclear relaxation rate near TAF shows significant anisotropy, indicating that the critical slowing down of stripe-type AF fluctuations are strongly anisotropic in spin space. The NMR spectra at sufficiently low temperatures consist of sharp peaks showing a commensurate stripe AF order with a small moment of ˜0.3 μB. However, the spectra just below TAF exhibit a highly asymmetric broadening pointing to an incommensurate modulation. The commensurate-incommensurate crossover in NaFeAs shows a certain similarity to the behavior of SrFe2As2 under high pressure.

Single-crystal silicon optical fiber by direct laser crystallization

DOE PAGES

Ji, Xiaoyu; Lei, Shiming; Yu, Shih -Ying; ...

2016-12-05

Semiconductor core optical fibers with a silica cladding are of great interest in nonlinear photonics and optoelectronics applications. Laser crystallization has been recently demonstrated for crystallizing amorphous silicon fibers into crystalline form. Here we explore the underlying mechanism by which long single-crystal silicon fibers, which are novel platforms for silicon photonics, can be achieved by this process. Using finite element modeling, we construct a laser processing diagram that reveals a parameter space within which single crystals can be grown. Utilizing this diagram, we illustrate the creation of single-crystal silicon core fibers by laser crystallizing amorphous silicon deposited inside silica capillarymore » fibers by high-pressure chemical vapor deposition. The single-crystal fibers, up to 5.1 mm long, have a very welldefined core/cladding interface and a chemically pure silicon core that leads to very low optical losses down to ~0.47-1dB/cm at the standard telecommunication wavelength (1550 nm). Furthermore, tt also exhibits a photosensitivity that is comparable to bulk silicon. Creating such laser processing diagrams can provide a general framework for developing single-crystal fibers in other materials of technological importance.« less

Elasticity, strength, and toughness of single crystal silicon carbide, ultrananocrystalline diamond, and hydrogen-free tetrahedral amorphous carbon

NASA Astrophysics Data System (ADS)

Espinosa, H. D.; Peng, B.; Moldovan, N.; Friedmann, T. A.; Xiao, X.; Mancini, D. C.; Auciello, O.; Carlisle, J.; Zorman, C. A.; Merhegany, M.

2006-08-01

In this work, the authors report the mechanical properties of three emerging materials in thin film form: single crystal silicon carbide (3C-SiC), ultrananocrystalline diamond, and hydrogen-free tetrahedral amorphous carbon. The materials are being employed in micro- and nanoelectromechanical systems. Several reports addressed some of the mechanical properties of these materials but they are based in different experimental approaches. Here, they use a single testing method, the membrane deflection experiment, to compare these materials' Young's moduli, characteristic strengths, fracture toughnesses, and theoretical strengths. Furthermore, they analyze the applicability of Weibull theory [Proc. Royal Swedish Inst. Eng. Res. 153, 1 (1939); ASME J. Appl. Mech. 18, 293 (1951)] in the prediction of these materials' failure and document the volume- or surface-initiated failure modes by fractographic analysis. The findings are of particular relevance to the selection of micro- and nanoelectromechanical systems materials for various applications of interest.

Toward a compact fibered squeezing parametric source.

PubMed

Brieussel, Alexandre; Ott, Konstantin; Joos, Maxime; Treps, Nicolas; Fabre, Claude

2018-03-15

In this work, we investigate three different compact fibered systems generating vacuum squeezing that involve optical cavities limited by the end surface of a fiber and by a curved mirror and containing a thin parametric crystal. These systems have the advantage to couple squeezed states directly to a fiber, allowing the user to benefit from the flexibility of fibers in the use of squeezing. Three types of fibers are investigated: standard single-mode fibers, photonic-crystal large-mode-area single-mode fibers, and short multimode fibers taped to a single-mode fiber. The observed squeezing is modest (-0.56  dB, -0.9  dB, -1  dB), but these experiments open the way for miniaturized squeezing devices that could be a very interesting advantage in scaling up quantum systems for quantum processing, opening new perspectives in the domain of integrated quantum optics.

Vibration energy harvester with sustainable power based on a single-crystal piezoelectric cantilever array.

PubMed

Kim, Moonkeun; Lee, Sang-Kyun; Ham, Yong-Hyun; Yang, Yil Suk; Kwon, Jong-Kee; Kwon, Kwang-Ho

2012-08-01

We designed and fabricated a bimorph cantilever array for sustainable power with an integrated Cu proof mass to obtain additional power and current. We fabricated a cantilever system using single-crystal piezoelectric material and compared the calculations for single and arrayed cantilevers to those obtained experimentally. The vibration energy harvester had resonant frequencies of 60.4 and 63.2 Hz for short and open circuits, respectively. The damping ratio and quality factor of the cantilever device were 0.012 and 41.66, respectively. The resonant frequency at maximum average power was 60.8 Hz. The current and highest average power of the harvester array were found to be 0.728 mA and 1.61 mW, respectively. The sustainable maximum power was obtained after slightly shifting the short-circuit frequency. In order to improve the current and power using an array of cantilevers, we also performed energy conversion experiments.

Formation of curved micrometer-sized single crystals.

PubMed

Koifman Khristosov, Maria; Kabalah-Amitai, Lee; Burghammer, Manfred; Katsman, Alex; Pokroy, Boaz

2014-05-27

Crystals in nature often demonstrate curved morphologies rather than classical faceted surfaces. Inspired by biogenic curved single crystals, we demonstrate that gold single crystals exhibiting curved surfaces can be grown with no need of any fabrication steps. These single crystals grow from the confined volume of a droplet of a eutectic composition melt that forms via the dewetting of nanometric thin films. We can control their curvature by controlling the environment in which the process is carried out, including several parameters, such as the contact angle and the curvature of the drops, by changing the surface tension of the liquid drop during crystal growth. Here we present an energetic model that explains this phenomenon and predicts why and under what conditions crystals will be forced to grow with the curvature of the microdroplet even though the energetic state of a curved single crystal is very high.

Gradient Plasticity Model and its Implementation into MARMOT

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

Barker, Erin I.; Li, Dongsheng; Zbib, Hussein M.

2013-08-01

The influence of strain gradient on deformation behavior of nuclear structural materials, such as boby centered cubic (bcc) iron alloys has been investigated. We have developed and implemented a dislocation based strain gradient crystal plasticity material model. A mesoscale crystal plasticity model for inelastic deformation of metallic material, bcc steel, has been developed and implemented numerically. Continuum Dislocation Dynamics (CDD) with a novel constitutive law based on dislocation density evolution mechanisms was developed to investigate the deformation behaviors of single crystals, as well as polycrystalline materials by coupling CDD and crystal plasticity (CP). The dislocation density evolution law in thismore » model is mechanism-based, with parameters measured from experiments or simulated with lower-length scale models, not an empirical law with parameters back-fitted from the flow curves.« less

Synthesis, Characterization, and Crystallization of Syndiotactic Alternating Ethylene-Propylene Crystalline Copolymer and its Blends.

NASA Astrophysics Data System (ADS)

Chien, Haoyang

A syndiotactic alternating ethylene-propylene (SYN-ALT-EP) crystalline copolymer was synthesized by complete hydrogenation, using a diimide reduction, of syndiotactic cis-1,4-poly(pentadiene-1,3) (CIS-PPD). The microstructure was studied by both high resolution nuclear magnetic resonance (NMR) spectroscopy and also fourier transform infra-red (FTIR) spectroscopy. The number average length of syndiotactic sequences is about 69 which indicates a high degree of syndiotacticity (97%) in the microstructure of this copolymer. The single FTIR absorbance at 733 cm^{ -1} without any splitting suggests an alternating arrangement of ethylene and propylene units. The solution state characterization of SYN-ALT -EP was studied by gel permeation chromatography using on -line measurements of multi-angle laser light scattering (MALLS), single capillary viscosities (VISC), and concentrations by differential refractive index (DRI) detectors. The Mark-Houwink-Sakurada parameters of "K" and "a" in THF at 30^circC are determined to be 8.99 times 10^ {-5} and 0.8, respectively. The universal GPC calibration curve can be applied to this copolymer in THF at 30^circC. Two different molecular relaxation processes ( alpha and beta relaxations) were found via dynamic mechanical (DM) analysis below room temperature: an alpha relaxation (around -60^ circC) and a beta relaxation (around -125^circ C). The apparent activation energy of the alpha relaxation is 285 kJ/mol, and the activation energy of the beta relaxation is 43 kJ/mol based on the Arrhenius equation. Molecular motion in SYN-ALT-EP copolymer was probed by solid state ^{13}C NMR experiments. At temperatures above T_{rm g} there are two major molecular motions in this copolymer: a backbone motion (the rotational motion about single bonds) and a methyl side group rotation. The backbone motion is frozen below T_{rm g}, but the methyl rotation still occurs. As the temperature is further decreased to about -175 ^circC, well below the beta -transition observed in DM analysis, the methyl side group rotation slows down, suggesting that the methyl rotation may be associated with the observed beta relaxation process. The equilibrium melting temperature is 55 +/- 1^circC; the equilibrium heat of fusion is 8.8 +/- 0.3 kJ/mol. The overall crystallization kinetics show an Avrami exponent (n) that qualitatively increases with crystallization temperature during primary crystallization. The transition from Regime II to Regime III is observed near T_{rm c} = 26 ^circC based on linear crystal growth rate experiments. The fold surface free energy ( sigma_{rm e}) is determined to be 33 erg/cm^2. A monoclinic crystal unit cell was determined (a = 11.19A b = 11.82A c = 9.00A gamma = 67.03^circ) from the fiber pattern via wide angle x-ray diffraction experiments (WAXD). A banded spherulitic morphology was observed by polarized light microscopy (PLM) and transmission electron microscopy (TEM). Such texture is characteristic of the co-twisting of growing lamellae. The morphology changes from regularly banded spherulites to non-regularly banded spherulites and may be correlated with the Regime III to Regime II transition. A plate-like single crystal morphology was also observed by polarized light microscopy after a melt crystallization at small supercooling conditions. Blends of SYN-ALT-EP/IPP, SYN-ALT-EP/HDPE, and SYN-ALT-EP/LDPE were made and examined. Neither T _{rm g} shifting nor co-crystallization using different blending compositions were observed. Therefore, only limited, if any, miscibility exists in these blends.

Capillarity creates single-crystal calcite nanowires from amorphous calcium carbonate.

PubMed

Kim, Yi-Yeoun; Hetherington, Nicola B J; Noel, Elizabeth H; Kröger, Roland; Charnock, John M; Christenson, Hugo K; Meldrum, Fiona C

2011-12-23

Single-crystal calcite nanowires are formed by crystallization of morphologically equivalent amorphous calcium carbonate (ACC) particles within the pores of track etch membranes. The polyaspartic acid stabilized ACC is drawn into the membrane pores by capillary action, and the single-crystal nature of the nanowires is attributed to the limited contact of the intramembrane ACC particle with the bulk solution. The reaction environment then supports transformation to a single-crystal product. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Laser radiation frequency doubling in a single-crystal fibre based on a stoichiometric LiNbO3 crystal

NASA Astrophysics Data System (ADS)

Kashin, V. V.; Nikolaev, D. A.; Rusanov, S. Ya; Tsvetkov, V. B.

2015-01-01

We demonstrate the employment of single-crystal optical fibres based on lithium niobate for doubling the laser radiation frequency. The measured characteristics of the fibre confirm its high quality and spatial homogeneity. Parameters of the frequency doublers for neodymium laser radiation (λ = 1 mm) based on fibre and bulk single crystals are compared. Single crystals are grown by the method of laser-heated pedestal growing with heating by radiation of a CO2 laser (LHPG-method).

Effect of L-Valine on the growth and characterization of Sodium Acid Phthalate (SAP) single crystals.

PubMed

Nirmala, L Ruby; Thomas Joseph Prakash, J

2013-06-01

Undoped and amino acid doped good quality single crystals of Sodium Acid Phthalate crystals (SAP) were grown by slow evaporation solution growth technique which are semiorganic in nature. The effect of amino acid (L-Valine) dopant on the growth and the properties of SAP single crystal was investigated. The single crystal X-ray diffraction studies and FT-IR studies were carried out to identify the crystal structure and the presence of functional groups in undoped and L-Valine doped SAP crystals. The transparent nature of the grown crystal was observed using UV-Visible spectrum. The thermal decomposition of the doped SAP crystals was investigated by thermo gravimetric analysis (TGA) and differential thermal analysis (DTA). The enhancement in the NLO property of the undoped and L-Valine doped SAP crystals using KDP crystal as a reference was studied using SHG measurements. Vickers micro hardness measurements are used for the study of mechanical strength of the grown crystals. Copyright © 2013 Elsevier B.V. All rights reserved.

Positioning and joining of organic single-crystalline wires

PubMed Central

Wu, Yuchen; Feng, Jiangang; Jiang, Xiangyu; Zhang, Zhen; Wang, Xuedong; Su, Bin; Jiang, Lei

2015-01-01

Organic single-crystal, one-dimensional materials can effectively carry charges and/or excitons due to their highly ordered molecule packing, minimized defects and eliminated grain boundaries. Controlling the alignment/position of organic single-crystal one-dimensional architectures would allow on-demand photon/electron transport, which is a prerequisite in waveguides and other optoelectronic applications. Here we report a guided physical vapour transport technique to control the growth, alignment and positioning of organic single-crystal wires with the guidance of pillar-structured substrates. Submicrometre-wide, hundreds of micrometres long, highly aligned, organic single-crystal wire arrays are generated. Furthermore, these organic single-crystal wires can be joined within controlled angles by varying the pillar geometries. Owing to the controllable growth of organic single-crystal one-dimensional architectures, we can present proof-of-principle demonstrations utilizing joined wires to allow optical waveguide through small radii of curvature (internal angles of ~90–120°). Our methodology may open a route to control the growth of organic single-crystal one-dimensional materials with potential applications in optoelectronics. PMID:25814032

Antioxidative succinobucol-sterol conjugates: Crystal structures and pseudosymmetry in the crystals

NASA Astrophysics Data System (ADS)

Ikonen, Satu; Jurček, Ondřej; Wimmer, Zdeněk; Drašar, Pavel; Kolehmainen, Erkki

2012-03-01

An extensive study to attach succinobucol to sterols has provided conjugates which comprise two pharmaceutically important compounds into one entity where the components are expected to have a synergistic effect. The motivation to design these novel conjugates was the need to broaden the armamentarium of current agents used in the treatment of atherosclerotic diseases and type 2 diabetes. In desire for detailed information of these compounds in solid state, which also have an influence to their physiological activity, systematic crystallization experiments were performed and as a result, X-ray quality single crystals were obtained from four succinobucol-sterol conjugates. All of these compounds crystallized in space group P1 with two or four molecules in an asymmetric unit and the crystallographically independent molecules were found to be related by pseudosymmetry (i.e. by pseudoinversion in 1-3 and by pseudoinversion plus pseudotranslation in 4).

3D coherent X-ray diffractive imaging of an Individual colloidal crystal grain

NASA Astrophysics Data System (ADS)

Shabalin, A.; Meijer, J.-M.; Sprung, M.; Petukhov, A. V.; Vartanyants, I. A.

Self-assembled colloidal crystals represent an important model system to study nucleation phenomena and solid-solid phase transitions. They are attractive for applications in photonics and sensorics. We present results of a coherent x-ray diffractive imaging experiment performed on a single colloidal crystal grain. The full three-dimensional (3D) reciprocal space map measured by an azimuthal rotational scan contained several orders of Bragg reflections together with the coherent interference signal between them. Applying the iterative phase retrieval approach, the 3D structure of the crystal grain was reconstructed and positions of individual colloidal particles were resolved. We identified an exact stacking sequence of hexagonal close-packed layers including planar and linear defects. Our results open up a breakthrough in applications of coherent x-ray diffraction for visualization of the inner 3D structure of different mesoscopic materials, such as photonic crystals. Present address: University of California - San Diego, USA.

Eye-Safe Polycrystalline Lasers

DTIC Science & Technology

2013-03-01

developed novel ceramic and single crystal laser gain media as a platform for power scaling to +100 kW class levels. Hydrothermal techniques were used...order of magnitude improvement in purity. Bulk single crystal growth was demonstrated for scandia and lutetia single crystals , as well as several...exhibited equivalent transparency to that of the single crystal in the near-infrared spectral region and initial lasing results have been successful

Single crystalline hollow metal-organic frameworks: a metal-organic polyhedron single crystal as a sacrificial template.

PubMed

Kim, Hyehyun; Oh, Minhak; Kim, Dongwook; Park, Jeongin; Seong, Junmo; Kwak, Sang Kyu; Lah, Myoung Soo

2015-02-28

Single crystalline hollow metal-organic frameworks (MOFs) with cavity dimensions on the order of several micrometers and hundreds of micrometers were prepared using a metal-organic polyhedron single crystal as a sacrificial hard template. The hollow nature of the MOF crystal was confirmed by scanning electron microscopy of the crystal sliced using a focused ion beam.

Crystal growth, structure analysis and characterisation of 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid single crystal

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

Sankari, R. Siva, E-mail: sivasankari.sh@act.edu.in; Perumal, Rajesh Narayana

2014-04-24

Single crystal of dielectric material 2 - (1, 3 - dioxoisoindolin - 2 - yl) acetic acid has been grown by slow evaporation solution growth method. The grown crystal was harvested in 25 days. The crystal structure was analyzed by Single crystal X - ray diffraction. UV-vis-NIR analysis was performed to examine the optical property of the grown crystal. The thermal property of the grown crystal was studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The dielectric measurements were carried out and the dielectric constant was calculated and plotted at all frequencies.

Wafer-scale single-crystal perovskite patterned thin films based on geometrically-confined lateral crystal growth

PubMed Central

Lee, Lynn; Baek, Jangmi; Park, Kyung Sun; Lee, Yong-EunKoo; Shrestha, Nabeen K.; Sung, Myung M.

2017-01-01

We report a facile roll-printing method, geometrically confined lateral crystal growth, for the fabrication of large-scale, single-crystal CH3NH3PbI3 perovskite thin films. Geometrically confined lateral crystal growth is based on transfer of a perovskite ink solution via a patterned rolling mould to a heated substrate, where the solution crystallizes instantly with the immediate evaporation of the solvent. The striking feature of this method is that the instant crystallization of the feeding solution under geometrical confinement leads to the unidirectional lateral growth of single-crystal perovskites. Here, we fabricated single-crystal perovskites in the form of a patterned thin film (3 × 3 inch) with a high carrier mobility of 45.64 cm2 V−1 s−1. We also used these single-crystal perovskite thin films to construct solar cells with a lateral configuration. Their active-area power conversion efficiency shows a highest value of 4.83%, which exceeds the literature efficiency values of lateral perovskite solar cells. PMID:28691697

Structural evolution of gypsum under high pressure: single-crystal X-ray experiments revisited

NASA Astrophysics Data System (ADS)

Li, Tsung-Lung; Lee, Pei-Lun

2018-05-01

The structures of gypsum at pressures up to approximately 4 GPa are studied with density functional theory (DFT) and thoroughly compared with single-crystal X-ray diffraction experiments reported in the literature [Comodi et al. in (Am Miner 93:1530-1537, 2008)]. It is found that the exchange-correlation density functional revPBE (revised Perdew-Burke-Ernzerhof) in conjunction with a nonlocal van der Waals (vdW) correction is capable of modeling the lattice constants, axial compressibility, and bulk modulus with good accuracy, suggesting that the inclusion of the vdW functional is crucially important for understanding the structure of hydrous minerals. To gain further physical insights, the geometric parameters associated with the constituting components of gypsum (water molecules, SO4 tetrahedra, and CaO8 polyhedra) are analyzed and compared with the experimental values. DFT simulations show that, under pressure, the polyhedral layers remain as nearly planar sheets of interconnecting SO4 tetrahedra and CaO8 polyhedra without further crinkling. DFT analysis on the layer compressibility along the major crystal axis reveals that, in contrast to experimental reports, the hydrous interlayer is less compressible than the polyhedral layer. Squeezed by the lateral pressure, the water molecules in the hydrous interlayer become better affixed along the major axis, making the interlayer harder to compress along this axis.

Observations on the crystallization of spodumene from aqueous solutions in a hydrothermal diamond-anvil cell

USGS Publications Warehouse

Li, Jianking; Chou, I-Ming; Yuan, Shunda; Burruss, Robert A.

2013-01-01

Crystallization experiments were conducted in a new type of hydrothermal diamond-anvil cell (HDAC; type V) using LiAlSi2O6 (S) gel and H2O (W) as starting materials. A total of 21 experiments were performed at temperatures up to 950°C and pressures up to 788 MPa. In the samples with relatively low W/S ratios, many small crystals formed in the melt phase during cooling. In those with high W/S ratios, only a few crystals with smooth surfaces crystallized from the aqueous fluid in the presence of melt droplets, which were gradually consumed during crystal growth, indicating rapid transfer of material from the melt to the crystals through the aqueous fluid. The nucleation of crystals started at 710 (±70)°C and 520 (±80) MPa, and crystal growth ended at 570 (±40)°C and 320 (±90) MPa, with the cooling P-T path within the stability field of spodumene + quartz in the S-W system. The observed linear crystal growth rates in the aqueous phase, calculated by dividing the maximum length of a single crystal by the duration of the entire growth step, were 4.7 × 10−6 and 5.7 × 10−6 cm s−1 for the cooling rates of 0.5 and 1°C min−1, respectively. However, a rapid crystal growth rate of 3.6 × 10−5 cm s−1 in the aqueous fluid was observed when the components were supplied by nearby melt droplets. Our results show that when crystals nucleate in the aqueous fluid instead of the melt phase, there are fewer nuclei formed, and they grow much faster due to the low viscosity of the aqueous fluid, which accelerates diffusion of components for the growth of crystals. Therefore, the large crystals in granitic pegmatite can crystallize directly from aqueous fluids rather than hydrosilicate melt.

Mosaic anisotropy model for magnetic interactions in mesostructured crystals

NASA Astrophysics Data System (ADS)

Goldman, Abby R.; Asenath-Smith, Emily; Estroff, Lara A.

2017-10-01

We propose a new model for interpreting the magnetic interactions in crystals with mosaic texture called the mosaic anisotropy (MA) model. We test the MA model using hematite as a model system, comparing mosaic crystals to polycrystals, single crystal nanoparticles, and bulk single crystals. Vibrating sample magnetometry confirms the hypothesis of the MA model that mosaic crystals have larger remanence (Mr/Ms) and coercivity (Hc) compared to polycrystalline or bulk single crystals. By exploring the magnetic properties of mesostructured crystalline materials, we may be able to develop new routes to engineering harder magnets.

The use of a mini-κ goniometer head in macromolecular crystallography diffraction experiments

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

Brockhauser, Sandor; UJF–EMBL–CNRS UMI 3265, 6 Rue Jules Horowitz, 38043 Grenoble; Ravelli, Raimond B. G.

2013-07-01

Hardware and software solutions for MX data-collection strategies using the EMBL/ESRF miniaturized multi-axis goniometer head are presented. Most macromolecular crystallography (MX) diffraction experiments at synchrotrons use a single-axis goniometer. This markedly contrasts with small-molecule crystallography, in which the majority of the diffraction data are collected using multi-axis goniometers. A novel miniaturized κ-goniometer head, the MK3, has been developed to allow macromolecular crystals to be aligned. It is available on the majority of the structural biology beamlines at the ESRF, as well as elsewhere. In addition, the Strategy for the Alignment of Crystals (STAC) software package has been developed to facilitatemore » the use of the MK3 and other similar devices. Use of the MK3 and STAC is streamlined by their incorporation into online analysis tools such as EDNA. The current use of STAC and MK3 on the MX beamlines at the ESRF is discussed. It is shown that the alignment of macromolecular crystals can result in improved diffraction data quality compared with data obtained from randomly aligned crystals.« less

Proposal for Research on High-Brightness Cathodes for High-Power Free-Electron Lasers (FEL)

DTIC Science & Technology

2013-05-09

recent experiments involving single crystal diamond amplifier cathodes (DAC) at Brookhaven National Laboratory ( BNL ). While the emission surface of our...diamond grain in the entire structure, both surface and interior, is passivated with hydrogen. The aforementioned studies at BNL found that

Patterned solid state growth of barium titanate crystals

NASA Astrophysics Data System (ADS)

Ugorek, Michael Stephen

An understanding of microstructure evolution in ceramic materials, including single crystal development and abnormal/enhanced grain growth should enable more controlled final ceramic element structures. In this study, two different approaches were used to control single crystal development in a patterned array. These two methods are: (1) patterned solid state growth in BaTiO 3 ceramics, and (2) metal-mediated single crystal growth in BaTiO 3. With the patterned solid state growth technique, optical photolithography was used to pattern dopants as well as [001] and [110] BaTiO3 single crystal template arrays with a 1000 microm line pattern array with 1000 microm spacings. These patterns were subsequently used to control the matrix grain growth evolution and single crystal development in BaTiO3. It was shown that the growth kinetics can be controlled by a small initial grain size, atmosphere conditions, and the introduction of a dopant at selective areas/interfaces. By using a PO2 of 1x10-5 atm during high temperature heat treatment, the matrix coarsening has been limited (to roughly 2 times the initial grain size), while retaining single crystal boundary motion up to 0.5 mm during growth for dwell times up to 9 h at 1300°C. The longitudinal and lateral growth rates were optimized at 10--15 microm/h at 1300°C in a PO2 of 1x10 -5 atm for single crystal growth with limited matrix coarsening. Using these conditions, a patterned microstructure in BaTiO3 was obtained. With the metal-mediated single crystal growth technique, a novel approach for fabricating 2-2 single crystal/polymer composites with a kerf < 5 microns was demonstrated. Surface templated grain growth was used to propagate a single crystal interface into a polycrystalline BaTiO3 or Ba(Zr0.05 Ti0.95)O3 matrix with lamellar nickel layers. The grain growth evolution and texture development were studied using both [001] and [110] BaTiO3 single crystals templates. By using a PO 2 of 1x10-11 atm during high temperature heat treatment, matrix coarsening was limited while enabling single crystal boundary motion up to 0.35 mm during growth between 1250°C and 1300°C with growth rates ˜ 3--4 microm/h for both single crystal orientations. By removing the inner electrodes, 2-2 single crystal (or ceramic) composites were prepared. The piezoelectric and dielectric properties of the composites of the two compositions were measured. The d33 and d31 of the composites were similar to the polycrystalline ceramic of the same composition.

The evolution of machining-induced surface of single-crystal FCC copper via nanoindentation

NASA Astrophysics Data System (ADS)

Zhang, Lin; Huang, Hu; Zhao, Hongwei; Ma, Zhichao; Yang, Yihan; Hu, Xiaoli

2013-05-01

The physical properties of the machining-induced new surface depend on the performance of the initial defect surface and deformed layer in the subsurface of the bulk material. In this paper, three-dimensional molecular dynamics simulations of nanoindentation are preformed on the single-point diamond turning surface of single-crystal copper comparing with that of pristine single-crystal face-centered cubic copper. The simulation results indicate that the nucleation of dislocations in the nanoindentation test on the machining-induced surface and pristine single-crystal copper is different. The dislocation embryos are gradually developed from the sites of homogeneous random nucleation around the indenter in the pristine single-crystal specimen, while the dislocation embryos derived from the vacancy-related defects are distributed in the damage layer of the subsurface beneath the machining-induced surface. The results show that the hardness of the machining-induced surface is softer than that of pristine single-crystal copper. Then, the nanocutting simulations are performed along different crystal orientations on the same crystal surface. It is shown that the crystal orientation directly influences the dislocation formation and distribution of the machining-induced surface. The crystal orientation of nanocutting is further verified to affect both residual defect generations and their propagation directions which are important in assessing the change of mechanical properties, such as hardness and Young's modulus, after nanocutting process.

Dual crystal x-ray spectrometer at 1.8 keV for high repetition-rate single-photon counting spectroscopy experiments

DOE PAGES

Gamboa, E. J.; Bachmann, B.; Kraus, D.; ...

2016-08-01

The recent development of high-repetition rate x-ray free electron lasers (FEL), makes it possible to perform x-ray scattering and emission spectroscopy measurements from thin foils or gasses heated to high-energy density conditions by integrating over many experimental shots. Since the expected signal may be weaker than the typical CCD readout noise over the region-of-interest, it is critical to the success of this approach to use a detector with high-energy resolution so that single x-ray photons may be isolated. We describe a dual channel x-ray spectrometer developed for the Atomic and Molecular Optics endstation at the Linac Coherent Light Source (LCLS)more » for x-ray spectroscopy near the K-edge of aluminum. The spectrometer is based on a pair of curved PET (002) crystals coupled to a single pnCCD detector which simultaneously measures x-ray scattering and emission in the forward and backward directions. Furthermore, the signals from single x-ray photons are accumulated permitting continuous single-shot acquisition at 120 Hz.« less

Left-right correlation in coupled F-center defects.

PubMed

Janesko, Benjamin G

2016-08-07

This work explores how left-right correlation, a textbook problem in electronic structure theory, manifests in a textbook example of electrons trapped in crystal defects. I show that adjacent F-center defects in lithium fluoride display symptoms of "strong" left-right correlation, symptoms similar to those seen in stretched H2. Simulations of UV/visible absorption spectra qualitatively fail to reproduce experiment unless left-right correlation is taken into account. This is of interest to both the electronic structure theory and crystal-defect communities. Theorists have a new well-behaved system to test their methods. Crystal-defect groups are cautioned that the approximations that successfully model single F-centers may fail for adjacent F-centers.

Three-Dimensional Large Screen Display Using Polymer-Dispersed Liquid-Crystal Light Valves and a Schlieren Optical System: Proposal and Basic Experiments

NASA Astrophysics Data System (ADS)

Takizawa, Kuniharu

A novel three-dimensional (3-D) projection display used with polarized eyeglasses is proposed. It consists of polymer-dispersed liquid crystal-light valves that modulate the illuminated light based on light scattering, a polarization beam splitter, and a Schlieren projection system. The features of the proposed display include a 3-D image display with a single projector, half size and half power consumption compared with a conventional 3-D projector with polarized glasses. Measured electro-optic characteristics of a polymer-dispersed liquid-crystal cell inserted between crossed polarizers suggests that the proposed display achieves small cross talk and high-extinction ratio.

Electron paramagnetic resonance study of radiation-induced paramagnetic centers in succinic anhydride single crystal

NASA Astrophysics Data System (ADS)

Caliskan, Betul; Caliskan, Ali Cengiz; Er, Emine

2017-09-01

Succinic anhydride single crystals were exposed to 60Co-gamma irradiation at room temperature. The irradiated single crystals were investigated at 125 K by Electron Paramagnetic Resonance (EPR) Spectroscopy. The investigation of EPR spectra of irradiated single crystals of succinic anhydride showed the presence of two succinic anhydride anion radicals. The anion radicals observed in gamma-irradiated succinic anhydride single crystal were created by the scission of the carbon-oxygen double bond. The structure of EPR spectra demonstrated that the hyperfine splittings arise from the same radical species. The reduction of succinic anhydride was identified which is formed by the addition of an electron to oxygen of the Csbnd O bond. The g values, the hyperfine structure constants and direction cosines of the radiation damage centers observed in succinic anhydride single crystal were obtained.

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

EPR and optical investigation of Mn2+ doped L-histidine-4-nitrophenolate 4-nitrophenol single crystal

NASA Astrophysics Data System (ADS)

Prabakaran, R.; Subramanian, P.

2018-04-01

Single crystals of L-histidine-4-nitrophenolate 4-nitrophenol[LHFNP] complex doped with Mn2+ were grown by the slow evaporation method at room temperature. The EPR spectrum reveals the entry of one Mn2+ ion in the lattice. The angular variation plot was drawn between the angles and the magnetic field position. The spin Hamiltonian parameters were obtained by EPR-NMR program. The D and E values show the rhombic field around the ion and is an interstitial one. The g value obtained here suggests that the Mn2+ ion experiences a strong field and there is a transfer of electron from the metal ion to the ligand atom. The optical absorption study shows various bands and are assigned to the transition from the ground state 6A1g(S). The Racah and crystal field parameters have also been evaluated and fitted to the experimental values. The Racah parameter shows the covalent bonding between the metal ion to the ligand.

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

Light Hydrocarbon Adsorption Mechanisms in Two Calcium-Based Microporous Metal Organic Frameworks

DOE PAGES

Plonka, Anna M.; Chen, Xianyin; Wang, Hao; ...

2016-01-25

The adsorption mechanism of ethane, ethylene, and acetylene (C 2H n; n = 2, 4, 6) on two microporous metal organic frameworks (MOFs) is described here that is consistent with observations from single crystal and powder X-ray diffraction, calorimetric measurements, and gas adsorption isotherm measurements. Two calcium-based MOFs, designated as SBMOF-1 and SBMOF-2 (SB: Stony Brook), form three-dimensional frameworks with one-dimensional open channels. As determined from single crystal diffraction experiments, channel geometries of both SBMOF-1 and SBMOF-2 provide multiple adsorption sites for hydrocarbon molecules through C–H···π and C–H···O interactions, similarly to interactions in the molecular and protein crystals. In conclusion,more » both materials selectively adsorb C 2 hydrocarbon gases over methane as determined with IAST and breakthrough calculations as well as experimental breakthrough measurements, with C 2H 6/CH 4 selectivity as high as 74 in SBMOF-1.« less

Structural, optical, mechanical and dielectric studies of pure and doped L-Prolinium trichloroacetate single crystals.

PubMed

Renuka, N; Ramesh Babu, R; Vijayan, N; Vasanthakumar, Geetha; Krishna, Anuj; Ramamurthi, K

2015-02-25

In the present work, pure and metal substituted L-Prolinium trichloroacetate (LPTCA) single crystals were grown by slow evaporation method. The grown crystals were subjected to single crystal X-ray diffraction (XRD), powder X-ray diffraction, FTIR, UV-Visible-NIR, hardness, photoluminescence and dielectric studies. The dopant concentration in the crystals was measured by inductively coupled plasma (ICP) analysis. Single crystal X-ray diffraction studies of the pure and metal substituted LPTCA revealed that the grown crystals belong to the trigonal system. Ni(2+) and Co(2+) doping slightly altered the lattice parameters of LPTCA without affecting the basic structure of the crystal. FTIR spectral analysis confirms the presence of various functional groups in the grown crystals. The mechanical behavior of pure and doped crystals was analyzed by Vickers's microhardness test. The optical transmittance, dielectric and photoluminescence properties of the pure and doped crystals were analyzed. Copyright © 2014 Elsevier B.V. All rights reserved.

Channeling experiments at planar diamond and silicon single crystals with electrons from the Mainz Microtron MAMI

NASA Astrophysics Data System (ADS)

Backe, H.; Lauth, W.; Tran Thi, T. N.

2018-04-01

Line structures were observed for (110) planar channeling of electrons in a diamond single crystal even at a beam energy of 180 MeV . This observation motivated us to initiate dechanneling length measurements as function of the beam energy since the occupation of quantum states in the channeling potential is expected to enhance the dechanneling length. High energy loss signals, generated as a result of emission of a bremsstrahlung photon with about half the beam energy at channeling of 450 and 855 MeV electrons, were measured as function of the crystal thickness. The analysis required additional assumptions which were extracted from the numerical solution of the Fokker-Planck equation. Preliminary results for diamond are presented. In addition, we reanalyzed dechanneling length measurements at silicon single crystals performed previously at the Mainz Microtron MAMI at beam energies between 195 and 855 MeV from which we conclude that the quality of our experimental data set is not sufficient to derive definite conclusions on the dechanneling length. Our experimental results are below the predictions of the Fokker-Planck equation and somewhat above the results of simulation calculations of A. V. Korol and A. V. Solov'yov et al. on the basis of the MBN Explorer simulation package. We somehow conservatively conclude that the prediction of the asymptotic dechanneling length on the basis of the Fokker-Planck equation represents an upper limit.

Single crystals of selected titanates and tungstates

NASA Technical Reports Server (NTRS)

Loiacono, G. M.

1972-01-01

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

Interface Character of Aluminum-Graphite Metal Matrix Composites.

DTIC Science & Technology

1983-01-27

studied included the commer- cial A/graphite composites; layered model systems on single crystal and poly- crystalline graphite substrates as well as...composition and thickness of the composite interface, and graphite crystal orientation. 3 For the model systems in this study , single crystal graphite...been reviewed by Kingcry. Segregation at surfaces in single- crystal MgO of Fe, Cr and Sc, which were Dresent in concentrations within the single- 3phase

Crystal structure and spectral properties of vitamin K3 based nitrobenzo[a]phenoxazines

NASA Astrophysics Data System (ADS)

Chadar, Dattatray; Chakravarty, Debamitra; Lande, Dipali N.; Gejji, Shridhar P.; Sahoo, Suprabha; Salunke-Gawali, Sunita

2017-12-01

Benzo[a]phenoxazines are the planar polycyclic fluorescent compounds, find a variety of applications in biological sciences and are of growing interest. In the present work we synthesized heterocyclic aromatic fluorescent benzo[a]phenoxazines namely, 6-methyl-9-nitro-5H-benzo[a]phenoxazin-5-one (1) and 6-methyl-10-nitro-5H-benzo[a]phenoxazin-5-one (2) which are characterized in terms of the 1H and 13C chemical shifts from 2D gHSQCAD NMR experiments. Single crystal X-ray experiments revealed both 1 and 2 possess the Csbnd H⋯O interactions. Moreover the π•••π stacking interactions between planar polycycles have been noticed only in 1. The structural and vibrational spectral inferences obtained from experiments are corroborated through the ωB97xD based density functional theory.

Magnetic and magnetostrictive behavior of Dy 3+ doped CoFe 2O 4 single crystals grown by flux method

NASA Astrophysics Data System (ADS)

Kambale, Rahul C.; Song, K. M.; Won, C. J.; Lee, K. D.; Hur, N.

2012-02-01

We studied the effect of Dy 3+ content on the magnetic properties of cobalt ferrite single crystal. The single crystals of CoFe 1.9Dy 0.1O 4 were grown by the flux method using Na 2B 4O 7.10 H 2O (Borax) as a solvent (flux). The black and shiny single crystals were obtained as a product. The X-ray diffraction analysis at room temperature confirmed the spinel cubic structure with lattice constant a=8.42 Å of the single crystals. The compositional analysis endorses the presence of constituents Co, Fe and Dy elements after sintering at 1300 °C within the final structure. The magnetic hysteresis measurements at various temperatures viz. 10 K, 100 K, 200 K and 300 K reveal the soft ferrimagnetic nature of the single crystal than that of for pure CoFe 2O 4. The observed saturation magnetization ( Ms) and coercivity ( Hc) are found to be lower than that of pure CoFe 2O 4 single crystal. The magnetostriction ( λ) measurement was carried out along the [001] direction. The magnetic measurements lead to conclude that the present single crystals can be used for magneto-optic recording media.

Magnetic spherical cores partly coated with periodic mesoporous organosilica single crystals.

PubMed

Li, Jing; Wei, Yong; Li, Wei; Deng, Yonghui; Zhao, Dongyuan

2012-03-07

Core-shell structured materials are of special significance in various applications. Until now, most reported core-shell structures have polycrystalline or amorphous coatings as their shell layers, with popular morphologies of microspheres or quasi-spheres. However, the single crystals, either mesoscale or atomic ones, are still rarely reported as shell layers. If single crystals can be coated on core materials, it would result in a range of new type core-shell structures with various morphologies, and probably more potential applications. In this work, we demonstrate that periodic mesoporous organosilica (PMO) single crystals can partly grow on magnetic microspheres to form incomplete Fe(3)O(4)@nSiO(2)@PMO core-shell materials in aqueous solution, which indeed is the first illustration that mesoporous single-crystal materials can be used as shell layers for preparation of core-shell materials. The achieved materials have advantages of high specific surface areas, good magnetic responses, embedded functional groups and cubic mesopore channels, which might provide them with various application conveniences. We suppose the partial growth is largely decided by the competition between growing tendency of single crystals and the resistances to this tendency. In principle, other single crystals, including a range of atomic single crystals, such as zeolites, are able to be developed into such core-shell structures.

Athermal Mechanisms of Size-Dependent Crystal Flow Gleaned from Three-Dimensional Discrete Dislocation Simulations

DTIC Science & Technology

2008-01-01

Sevillano, et. al . directly developed a definition of the single-slip glide-resistance correlation length, 10//5.8 o  , from 2d simulations of single...dislocation percolation through point-obstacle fields [35, 36]. Subsequently, predictions for the size- dependence of * from Gil Sevillano, et. al ...Sevillano, et. al ., and microcrystal deformation experiments was perhaps fortuitous, significant merit remains within their treatment. The more general

Time-resolved spectroscopic measurements of shock-wave induced decomposition in cyclotrimethylene trinitramine (RDX) crystals: anisotropic response.

PubMed

Dang, Nhan C; Dreger, Zbigniew A; Gupta, Yogendra M; Hooks, Daniel E

2010-11-04

Plate impact experiments on the (210), (100), and (111) planes were performed to examine the role of crystalline anisotropy on the shock-induced decomposition of cyclotrimethylenetrinitramine (RDX) crystals. Time-resolved emission spectroscopy was used to probe the decomposition of single crystals shocked to peak stresses ranging between 7 and 20 GPa. Emission produced by decomposition intermediates was analyzed in terms of induction time to emission, emission intensity, and the emission spectra shapes as a function of stress and time. Utilizing these features, we found that the shock-induced decomposition of RDX crystals exhibits considerable anisotropy. Crystals shocked on the (210) and (100) planes were more sensitive to decomposition than crystals shocked on the (111) plane. The possible sources of the observed anisotropy are discussed with regard to the inelastic deformation mechanisms of shocked RDX. Our results suggest that, despite the anisotropy observed for shock initiation, decomposition pathways for all three orientations are similar.

Flux growth of high-quality CoFe 2O 4 single crystals and their characterization

NASA Astrophysics Data System (ADS)

Wang, W. H.; Ren, X.

2006-04-01

We report the growth of high-quality CoFe 2O 4 single crystals using a borax flux method. The crystals were characterized by powder X-ray diffraction, electron probe microanalysis and Raman spectroscopy. We found the crystals are flux-free and highly homogeneous in composition. X-ray rocking curves of the CoFe 2O 4 single crystals showed a full-width at half-maximum of 0.15°. The saturation magnetization of the CoFe 2O 4 single crystals was measured to be 90 emu/g or equivalently 3.65 μ B/f.u. at 5 K.

EPR study of free radical in gamma-irradiated bis(cyclopentadienyl)zirconium dichloride single crystal

NASA Astrophysics Data System (ADS)

Caliskan, Betul; Caliskan, Ali Cengiz

2017-06-01

Bis(cyclopentadienyl)zirconium dichloride (BCZD; zirconocene dichloride) single crystals were exposed to 60Co-γ irradiation at room temperature. The irradiated single crystals were investigated between 125 and 470 K by electron paramagnetic resonance spectroscopy. The spectra of the crystals were found to be temperature independent. The paramagnetic center was attributed to the cyclopentadienyl radical. The g values of the radiation damage center observed in BCZD single crystal and the hyperfine structure constants of the free electron with nearby protons were obtained.

Tribochemical wear of single crystal aluminum in NaCl solution studied by atomic force microscopy

NASA Astrophysics Data System (ADS)

Cai, M.; Langford, S. C.; Dickinson, J. T.

2011-09-01

We report a systematic study of chemically enhanced wear of single crystal aluminum surfaces in aqueous solutions using an environmentally equipped atomic force microscope (AFM). The experiments were conducted by using a standard Si3N4 AFM tip to apply a localized force on a polished, single crystal aluminum (110) surface. Most measurements were performed in 0.5 M NaCl solution. We show the effect of applied force, number of scans, chemical solution, and temperature on the chemical-mechanical wear of aluminum on the nanometer scale. Aggressive chemical environments significantly enhance the wear of aluminum relative to scanning in dry air. Quantitative measurements show that the wear volume increases in proportion to the square root of force and the number of scans (or time). Arrhenius plots of wear volume versus temperature are consistent with an activation energy of 31 kJ/mol for scanning in 0.5 M NaCl. The wear of the AFM tip and the aluminum substrate is explained in terms of the synergistic surface chemical reactions and mechanical action of the tip. We compare these results to previous studies of AFM wear of silicate glass.

Magnon drag thermopower and thermomagnetic properties of single-crystal iron

NASA Astrophysics Data System (ADS)

Watzman, Sarah; Jin, Hyungyu; Heremans, Joseph

2015-03-01

Lucassen et al. demonstrate that magnon drag involves a spin-transfer mechanism closely related to the recently discovered spin-Seebeck effect. This talk will first present results of experiments mapping out the thermopower and magnetothermopower of single-crystal iron and prove that its thermopower is indeed dominated by magnon drag, as suggested by Blatt et al. in 1967. Measurements will then be presented on the magnetic field and temperature dependence of the full thermomagnetic tensor of iron's thermopower in the xxx, xyx, and xyz geometries (the first index gives the direction of the heat flux, the second the measured electric field, the third the applied magnetic field). Results of magneto-thermopower and Nernst coefficients will be reported for single-crystal samples oriented with x =[100]. The Nernst coefficients of elemental iron contain a contribution of a direct spin-transfer mechanism, which should be present in the absence of an interface between a ferromagnet and a normal metal. This mechanism could be put to use in high temperature ferromagnetic metallic thermoelectric alloys. This work is supported by the NSF GRFP under Grant No. DGE-0822215 and the ARO MURI under Grant No. W911NF-14-1-0016.

Ultrafast dynamic response of single crystal β-HMX

NASA Astrophysics Data System (ADS)

Zaug, Joseph M.; Armstrong, Michael R.; Crowhurst, Jonathan C.; Radousky, Harry B.; Ferranti, Louis; Swan, Raymond; Gross, Rick; Teslich, Nick E.; Wall, Mark A.; Austin, Ryan A.; Fried, Laurence E.

2017-01-01

We report results from ultrafast compression experiments conducted on β-HMX single crystals. Results consist of nominally 12 picosecond time-resolved wave profile data, (ultrafast time domain interferometry -TDI measurements), that were analyzed to determine high-velocity wave speeds as a function of piston velocity. TDI results are used to validate calculations of anisotropic stress-strain behavior of shocked loaded energetic materials. Our previous results derived using a 350 ps duration compression drive revealed anisotropic elastic wave response in single crystal β-HMX from (110) and (010) impact planes. Here we present results using a 1.05 ns duration compression drive with a 950 ps interferometry window to extend knowledge of the anisotropic dynamic response of β-HMX within eight microns of the initial impact plane. We observe two distinct wave profiles from (010) and three wave profiles from (010) impact planes. The (110) impact plane wave speeds typically exceed (010) impact plane wave speeds at the same piston velocities. The development of multiple hydrodynamic wave profiles begins at 20 GPa for the (110) impact plane and 28 GPa for the (10) impact plane. We compare our ultrafast TDI results with previous gun and plate impact results on β-HMX and PBX9501.

Studies of Second Order Optical Nonlinearities of 4-Aminobenzophenone (ABP) Single Crystal Films

NASA Astrophysics Data System (ADS)

Bhowmik, Achintya; Thakur, Mrinal

1998-03-01

Specific organic materials exhibit very high second order optical susceptibilities. Growth of single crystal films of these materials and characterization of nonlinear optical properties are necessary for implementation of device applications. We have grown large-area films ( 1 cm^2 area, 4 μm thick) of ABP by a modification of the shear method. Single crystal nature of the films was confirmed by polarized optical microscopy. X-ray diffraction analysis showed a [100] surface orientation. The absorption spectra revealed transparency from 390 nm to 1940 nm. Significant elements of the second order optical susceptibility tensor were measured by detailed SHG experiments using a Nd:YAG laser (1064 nm, 100 ps, 82 MHz). Second-harmonic power was measured using lock-in detection with carefully selected polarization conditions while the film was rotated about the propagation direction. Using LiNbØas the reference, d-coefficients of ABP were found to be d_23=7.2 pm/V and d_22=0.7 pm/V. Type-I and type-II phase-matching directions were identified on the film by analyzing the optical indicatrix surfaces at fundamental and second-harmonic frequencies.

Growth and characterization of CaCu3Ti4O12 single crystals

NASA Astrophysics Data System (ADS)

Kim, Hui Eun; Yang, Sang-don; Lee, Jung-Woo; Park, Hyun Min; Yoo, Sang-Im

2014-12-01

The CaCu3Ti4O12 (CCTO) single crystals could be grown from the melt with the nominal composition of Ca:Cu:Ti=1:59:20 in a platinum (Pt) crucible using a self-flux method. The flux-grown CCTO single crystals have well-developed {100} habit planes, and their compositions are close to the ratio of Ca:Cu:Ti=1:3:4. Interestingly, flux-grown CCTO single crystals exhibited two different back reflection Laue patterns; one exhibited only [100] cubic Laue patterns, and the other showed not only [100] cubic Laue patterns but also the satellite spots related to the twin boundary, implying that twin-free CCTO single crystals can be grown by the self-flux method. Both the dielectric constants and losses of twinned CCTO single crystal are significantly higher than those of untwined CCTO crystal at relatively low frequency regime (<10 kHz), suggesting that the dielectric property is sensitive to the twin boundary.

A multistep single-crystal-to-single-crystal bromodiacetylene dimerization

NASA Astrophysics Data System (ADS)

Hoheisel, Tobias N.; Schrettl, Stephen; Marty, Roman; Todorova, Tanya K.; Corminboeuf, Clémence; Sienkiewicz, Andrzej; Scopelliti, Rosario; Schweizer, W. Bernd; Frauenrath, Holger

2013-04-01

Packing constraints and precise placement of functional groups are the reason that organic molecules in the crystalline state often display unusual physical or chemical properties not observed in solution. Here we report a single-crystal-to-single-crystal dimerization of a bromodiacetylene that involves unusually large atom displacements as well as the cleavage and formation of several bonds. Density functional theory computations support a mechanism in which the dimerization is initiated by a [2 + 1] photocycloaddition favoured by the nature of carbon-carbon short contacts in the crystal structure. The reaction proceeded up to the theoretical degree of conversion without loss of crystallinity, and it was also performed on a preparative scale with good yield. Moreover, it represents the first synthetic pathway to (E)-1,2-dibromo-1,2-diethynylethenes, which could serve as synthetic intermediates for the preparation of molecular carbon scaffolds. Our findings both extend the scope of single-crystal-to-single-crystal reactions and highlight their potential as a synthetic tool for complex transformations.

Preparation of Gd(OH){sub 3} large single crystals by solid KOH assisted hydrothermal method and their luminescent and magnetic properties

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

Wu, Hai; Zhang, Youjin, E-mail: zyj@ustc.edu.cn; Zhou, Maozhong

Highlights: • Gd(OH){sub 3} large single crystals were prepared by solid KOH assisted hydrothermal method. • The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. • The Gd(OH){sub 3} samples emitted a strong narrow-band ultraviolet B (NB-UVB) light. • The Gd(OH){sub 3} samples showed good paramagnetic properties. - Abstract: Large single crystals of gadolinium hydroxide [Gd(OH){sub 3}] in the length of several millimeters were successfully prepared by using solid KOH assisted hydrothermal method. Gd(OH){sub 3} samples were characterized by X-ray diffraction (XRD), 4-circle single-crystal diffraction, Fourier transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS). FESEM imagemore » shows hexagonal prism morphology for the Gd(OH){sub 3} large crystals. The possible growth mechanism of Gd(OH){sub 3} large single crystals was proposed. The photoluminescence and magnetic properties of Gd(OH){sub 3} species were investigated.« less

Method for the growth of large low-defect single crystals

NASA Technical Reports Server (NTRS)

Powell, J. Anthony (Inventor); Neudeck, Philip G. (Inventor); Trunek, Andrew J. (Inventor); Spry, David J. (Inventor)

2008-01-01

A method and the benefits resulting from the product thereof are disclosed for the growth of large, low-defect single-crystals of tetrahedrally-bonded crystal materials. The process utilizes a uniquely designed crystal shape whereby the direction of rapid growth is parallel to a preferred crystal direction. By establishing several regions of growth, a large single crystal that is largely defect-free can be grown at high growth rates. This process is particularly suitable for producing products for wide-bandgap semiconductors, such as SiC, GaN, AlN, and diamond. Large low-defect single crystals of these semiconductors enable greatly enhanced performance and reliability for applications involving high power, high voltage, and/or high temperature operating conditions.

Crystalline perfection and optical studies of L-Histidinium dihydrogen phosphate orthophosphoric acid (LHDP) single crystals

NASA Astrophysics Data System (ADS)

Ittyachan, Reena; Arunkumar, A.; Bhagavannarayana, G.

2015-10-01

Single crystals of L-Histidinium dihydrogenphosphate orthophosphoric acid (LHDP) were grown by slow evaporation solution growth technique. The grown crystals were confirmed by single crystal X-ray diffraction techniques. The HRXRD rocking curve measurements revealed the crystalline perfection of grown crystal and the absence of structural grain boundaries. The lower optical cut-off wavelength for this crystal was observed at 240 nm. The third order nonlinear refractive index (n2), nonlinear absorption coefficient (β) and susceptibility (χ(3)) were calculated by Z-scan studies using Nd: YAG laser as a source. The single shot laser damage threshold of grown crystal was measured to be 6.286 GW/cm2 using Nd: YAG laser.

Kinetics of Nucleation and Crystal Growth in Glass Forming Melts in Microgravity

NASA Technical Reports Server (NTRS)

Day, Delbert E.; Ray, Chandra S.

2001-01-01

This flight definition project has the specific objective of investigating the kinetics of nucleation and crystal growth in high temperature inorganic oxide, glass forming melts in microgravity. It is related to one of our previous NASA projects that was concerned with glass formation for high temperature containerless melts in microgravity. The previous work culminated in two experiments which were conducted aboard the space shuttle in 1983 and 1985 and which consisted of melting (at 1500 C) and cooling levitated 6 to 8 mm diameter spherical samples in a Single Axis Acoustic Levitator (SAAL) furnace. Compared to other types of materials, there have been relatively few experiments, 6 to 8, conducted on inorganic glasses in space. These experiments have been concerned with mass transport (alkali diffusion), containerless melting, critical cooling rate for glass formation, chemical homogeneity, fiber pulling, and crystallization of glass forming melts. One of the most important and consistent findings in all of these experiments has been that the glasses prepared in microgravity are more resistant to crystallization (better glass former) and more chemically homogeneous than equivalent glasses made on Earth (1 g). The chemical composition of the melt appears relatively unimportant since the same general results have been reported for oxide, fluoride and chalcogenide melts. These results for space-processed glasses have important implications, since glasses with a higher resistance to crystallization or higher chemical homogeneity than those attainable on Earth can significantly advance applications in areas such as fiber optics communications, high power laser glasses, and other photonic devices where glasses are the key functional materials.

Synthesis, crystal structure, thermal and nonlinear optical properties of new metal-organic single crystal: Tetrabromo (piperazinium) zincate (II) (TBPZ)

NASA Astrophysics Data System (ADS)

Boopathi, K.; Babu, S. Moorthy; Ramasamy, P.

2018-04-01

Tetrabromo (piperazinium) zincate, a new metal-organic crystal has been synthesized and its single crystal grown by slow evaporation method. The grown crystal has characterized by structural, spectral, thermal, linear and nonlinear optical properties. Single crystal X-ray diffractions study reveals that grown crystal belongs to orthorhombic crystal system with space group P212121. The presence of functional groups is identified by FT-IR spectral analysis. Thermal stability of the crystal was ascertained by TG-DTA measurement. The second order harmonic generation efficiency was measured using Kurtz and Perry technique and it was found to be 1.5 times that of KDP.

Cloud chamber experiments on the origin of ice crystal complexity in cirrus clouds

NASA Astrophysics Data System (ADS)

Schnaiter, Martin; Järvinen, Emma; Vochezer, Paul; Abdelmonem, Ahmed; Wagner, Robert; Jourdan, Olivier; Mioche, Guillaume; Shcherbakov, Valery N.; Schmitt, Carl G.; Tricoli, Ugo; Ulanowski, Zbigniew; Heymsfield, Andrew J.

2016-04-01

This study reports on the origin of small-scale ice crystal complexity and its influence on the angular light scattering properties of cirrus clouds. Cloud simulation experiments were conducted at the AIDA (Aerosol Interactions and Dynamics in the Atmosphere) cloud chamber of the Karlsruhe Institute of Technology (KIT). A new experimental procedure was applied to grow and sublimate ice particles at defined super- and subsaturated ice conditions and for temperatures in the -40 to -60 °C range. The experiments were performed for ice clouds generated via homogeneous and heterogeneous initial nucleation. Small-scale ice crystal complexity was deduced from measurements of spatially resolved single particle light scattering patterns by the latest version of the Small Ice Detector (SID-3). It was found that a high crystal complexity dominates the microphysics of the simulated clouds and the degree of this complexity is dependent on the available water vapor during the crystal growth. Indications were found that the small-scale crystal complexity is influenced by unfrozen H2SO4 / H2O residuals in the case of homogeneous initial ice nucleation. Angular light scattering functions of the simulated ice clouds were measured by the two currently available airborne polar nephelometers: the polar nephelometer (PN) probe of Laboratoire de Métérologie et Physique (LaMP) and the Particle Habit Imaging and Polar Scattering (PHIPS-HALO) probe of KIT. The measured scattering functions are featureless and flat in the side and backward scattering directions. It was found that these functions have a rather low sensitivity to the small-scale crystal complexity for ice clouds that were grown under typical atmospheric conditions. These results have implications for the microphysical properties of cirrus clouds and for the radiative transfer through these clouds.

Hyperthermal atomic oxygen generator

NASA Technical Reports Server (NTRS)

Khandelwal, Govind S.; Wu, Dongchuan

1990-01-01

Characterization of the transport properties of oxygen through silver was continued. Specifically, experiments measuring the transport through Ag(111), Ag(110), Ag(100) single crystals and through Ag0.05 Zr alloy were completed. In addition, experiments using glow discharge excitation of oxygen to assist in the transport were completed. It was found that the permeability through the different orientations of single crystal Ag was the same, but significant differences existed in the diffusivity. The experimental ratio of diffusivities, however, was in reasonable agreement with theoretical estimates. Since the solubilities of orientations must be the same, this suggests some problems with the assumption K = DS. The glow discharge experiments show that there is a substantial increase in transport (factor of six) when the upstream pressure is dissociated to some fraction of atoms (which have a much higher sticking coefficient). These results indicate that there is a significant surface limitation because of dissociative adsorption of the molecules. Experiments with the Ag0.05 Zr alloy and its high-grain boundary and defect density show a permeability of greater than a factor of two over ordinary polycrystalline Ag, but it is unclear as to whether this is because of enhanced transport through these defects or whether the Zr and defects on the surface increased the sticking coefficient and therefore the transport.

(1)H-(13)C Hetero-nuclear dipole-dipole couplings of methyl groups in stationary and magic angle spinning solid-state NMR experiments of peptides and proteins.

PubMed

Wu, Chin H; Das, Bibhuti B; Opella, Stanley J

2010-02-01

(13)C NMR of isotopically labeled methyl groups has the potential to combine spectroscopic simplicity with ease of labeling for protein NMR studies. However, in most high resolution separated local field experiments, such as polarization inversion spin exchange at the magic angle (PISEMA), that are used to measure (1)H-(13)C hetero-nuclear dipolar couplings, the four-spin system of the methyl group presents complications. In this study, the properties of the (1)H-(13)C hetero-nuclear dipolar interactions of (13)C-labeled methyl groups are revealed through solid-state NMR experiments on a range of samples, including single crystals, stationary powders, and magic angle spinning of powders, of (13)C(3) labeled alanine alone and incorporated into a protein. The spectral simplifications resulting from proton detected local field (PDLF) experiments are shown to enhance resolution and simplify the interpretation of results on single crystals, magnetically aligned samples, and powders. The complementarity of stationary sample and magic angle spinning (MAS) measurements of dipolar couplings is demonstrated by applying polarization inversion spin exchange at the magic angle and magic angle spinning (PISEMAMAS) to unoriented samples. Copyright 2009 Elsevier Inc. All rights reserved.

How far could energy transport within a single crystal

NASA Astrophysics Data System (ADS)

Zhang, Yifan; Che, Yanke; Zhao, Jincai; Steve, Granick

Efficient transport of excitation energy over long distance is a vital process in light-harvesting systems and molecular electronics. The energy transfer distance is largely restricted by the probability decay of the exciton when hopping within a single crystal. Here, we fabricated an organic single crystal within which the energy could transfer more than 100 μm, a distance only limited by its crystal size. Our system could be regarded as a ``Sprint relay game'' performing on different surface of tracks. Photoinduced ``athletes'' (excitons) triggered intermolecular ``domino'' reaction to propagate energy for a long distance. In addition, athletes with the same ability runs much farther on smooth ideal track (single crystal assembled from merely van der Waals interaction) than bumpy mud track (crystal assembled from combination of pi-stacking, hydrogen bond and van der Waals interactions). Our finding presents new physics on enhancing energy transfer length within a single crystal. Current Affiliation: Institute for Basic Science, South Korea.

Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

NASA Technical Reports Server (NTRS)

Arakere, N. K.; Swanson, G.

2002-01-01

High cycle fatigue (HCF) induced failures in aircraft gas turbine and rocket engine turbopump blades is a pervasive problem. Single crystal nickel turbine blades are being utilized in rocket engine turbopumps and jet engines throughout industry because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities over polycrystalline alloys. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493, PWA 1484, RENE' N-5 and CMSX-4. These alloys play an important role in commercial, military and space propulsion systems. Single crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant factor in the overall analysis. The failure modes of single crystal turbine blades are complicated to predict due to the material orthotropy and variations in crystal orientations. Fatigue life estimation of single crystal turbine blades represents an important aspect of durability assessment. It is therefore of practical interest to develop effective fatigue failure criteria for single crystal nickel alloys and to investigate the effects of variation of primary and secondary crystal orientation on fatigue life. A fatigue failure criterion based on the maximum shear stress amplitude /Delta(sub tau)(sub max))] on the 24 octahedral and 6 cube slip systems, is presented for single crystal nickel superalloys (FCC crystal). This criterion reduces the scatter in uniaxial LCF test data considerably for PWA 1493 at 1200 F in air. Additionally, single crystal turbine blades used in the alternate advanced high-pressure fuel turbopump (AHPFTP/AT) are modeled using a large-scale three-dimensional finite element model. This finite element model is capable of accounting for material orthotrophy and variation in primary and secondary crystal orientation. Effects of variation in crystal orientation on blade stress response are studied based on 297 finite element model runs. Fatigue lives at critical points in the blade are computed using finite element stress results and the failure criterion developed. Stress analysis results in the blade attachment region are also presented. Results presented demonstrates that control of secondary and primary crystallographic orientation has the potential to significantly increase a component S resistance to fatigue crack growth with- out adding additional weight or cost. [DOI: 10.1115/1.1413767

Infrared and Raman spectroscopy and DFT calculations of DL amino acids: Valine and lysine hydrochloride

NASA Astrophysics Data System (ADS)

Paiva, F. M.; Batista, J. C.; Rêgo, F. S. C.; Lima, J. A.; Freire, P. T. C.; Melo, F. E. A.; Mendes Filho, J.; de Menezes, A. S.; Nogueira, C. E. S.

2017-01-01

Single crystals of DL-valine and DL-lysine hydrochloride were grown by slow evaporation method and the crystallographic structure were confirmed by X-ray diffraction experiment and Rietveld method. These two crystals have been studied by Raman spectroscopy in the 25-3600 cm-1 spectral range and by infrared spectroscopy through the interval 375-4000 cm-1 at room temperature. Experimental and theoretical vibrational spectra were compared and a complete analysis of the modes was done in terms of the Potential Energy Distribution (PED).

Optimal fusion offset in splicing photonic crystal fibers

NASA Astrophysics Data System (ADS)

Jin, Wa; Bi, Weihong; Fu, Guangwei

2013-08-01

Heat transfer is very complicate in fusion splicing process of photonic crystal fibers (PCFs) due to different structures and sizes of air hole, which requires different fusion splicing power and offsets of heat source. Based on the heat transfer characteristics, this paper focus on the optimal splicing offset splicing the single mode fiber and PCFs with a CO2 laser irradiation. The theory and experiments both show that the research results can effectively calculate the optimal fusion splicing offset and guide the practical splicing between PCFs and SMFs.

Preparation and guest-uptake protocol for a porous complex useful for 'crystal-free' crystallography.

PubMed

Inokuma, Yasuhide; Yoshioka, Shota; Ariyoshi, Junko; Arai, Tatsuhiko; Fujita, Makoto

2014-02-01

We recently reported a new method for single-crystal X-ray diffraction (SCD) analysis that does not require the crystallization of the target compound. In this 'crystal-free' crystallography, a tiny crystal of a porous complex is soaked in the solution of the target guest. The guest molecules are absorbed and oriented in the crystal pores and can be analyzed by X-ray diffraction. We describe here a detailed synthetic protocol for the preparation of uniform single crystals of the porous host complex and for the subsequent guest uptake. The protocol describes our most versatile porous complex, which is prepared from commercially available ZnI2 and 2,4,6-tri(4-pyridyl)-1,3,5-triazine. The host complex has large pores with a cross-section of 8 × 5 Å(2). Single crystals of the complex are grown from layered solutions of the two components. The pores of the as-synthesized complex are filled with nitrobenzene, which is replaced with the inert solvent cyclohexane. This solvent exchange is essential for the rapid and effective inclusion of target compounds. The most crucial and delicate step is the selection of high-quality single crystals from the mixture of crystals of various shapes and sizes. We suggest using the facial indices of the single crystals as a criterion for crystal selection. Single-crystal samples for X-ray analysis can be prepared by immersing the selected crystals in a cyclohexane/dichloromethane solution of target compound. After a very slow evaporation of the solvent, typically over 2 d, the final crystal can be picked and directly subjected to SCD analysis. The protocol can be completed within ∼16 d.

Space Processing Applications Rocket project SPAR III

NASA Technical Reports Server (NTRS)

Reeves, F.

1978-01-01

This document presented the engineering report and science payload III test report and summarized the experiment objectives, design/operational concepts, and final results of each of five scientific experiments conducted during the third Space Processing Applications Rocket (SPAR) flight flown by NASA in December 1976. The five individual SPAR experiments, covering a wide and varied range of scientific materials processing objectives, were entitled: Liquid Mixing, Interaction of Bubbles with Solidification Interfaces, Epitaxial Growth of Single Crystal Film, Containerless Processing of Beryllium, and Contact and Coalescence of Viscous Bodies.

Characterizing new compositions of [001]C relaxor ferroelectric single crystals using a work-energy model

NASA Astrophysics Data System (ADS)

Gallagher, John A.

2016-04-01

The desired operating range of ferroelectric materials with compositions near the morphotropic phase boundary is limited by field induced phase transformations. In [001]C cut and poled relaxor ferroelectric single crystals the mechanically driven ferroelectric rhombohedral to ferroelectric orthorhombic phase transformation is hindered by antagonistic electrical loading. Instability around the phase transformation makes the current experimental technique for characterization of the large field behavior very time consuming. Characterization requires specialized equipment and involves an extensive set of measurements under combined electrical, mechanical, and thermal loads. In this work a mechanism-based model is combined with a more limited set of experiments to obtain the same results. The model utilizes a work-energy criterion that calculates the mechanical work required to induce the transformation and the required electrical work that is removed to reverse the transformation. This is done by defining energy barriers to the transformation. The results of the combined experiment and modeling approach are compared to the fully experimental approach and error is discussed. The model shows excellent predictive capability and is used to substantially reduce the total number of experiments required for characterization. This decreases the time and resources required for characterization of new compositions.

Mechanical properties and negative thermal expansion of a dense rare earth formate framework

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

Zhang, Zhanrui; Jiang, Xingxing; Feng, Guoqiang

The fundamental mechanical properties of a dense metal–organic framework material, [NH{sub 2}CHNH{sub 2}][Er(HCOO){sub 4}] (1), have been studied using nanoindentation technique. The results demonstrate that the elastic moduli, hardnesses, and yield stresses on the (021)/(02−1) facets are 29.8/30.2, 1.80/1.83 and 0.93/1.01 GPa, respectively. Moreover, variable-temperature powder and single-crystal X-ray diffraction experiments reveal that framework 1 shows significant negative thermal expansion along its b axis, which can be explained by using a hinge–strut structural motif. - Graphical abstract: The structure of framework, [NH{sub 2}CHNH{sub 2}][Er(HCOO){sub 4}], and its indicatrix of thermal expansion. - Highlights: • The elastic modulus, hardness, and yieldmore » stress properties of a rare earth metal–organic framework material were studied via nanoindentation technique. • Variable-temperature powder X-ray diffraction experiments reveal that this framework shows significant negative thermal expansion along its b axis. • Based on variable-temperature single-crystal X-ray diffraction experiments, the mechanism of negative thermal expansion can be explained by a hinge–strut structural motif.« less

Linear electro-optic properties of relaxor-based ferroelectric 0.24Pb(In1/2Nb1/2)O3-(0.76 − x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 single crystals

PubMed Central

Wu, Fengmin; Yang, Bin; Sun, Enwei; Liu, Gang; Tian, Hao; Cao, Wenwu

2013-01-01

Linear electro-optic properties of 0.24Pb(In1/2Nb1/2)O3-(0.76 − x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 single crystals, with compositions in the rhombohedral, morphotropic phase boundary (MPB) and tetragonal phases, have been investigated. Very large effective electro-optic coefficient γc (204 pm/V) was observed in a crystal with the MPB composition when it is poled along [001]. The rhombohedral phase (x = 0.27 and 0.30) single crystals poled along [111] direction and tetragonal phase (x = 0.39) single crystal poled along [001] direction are in single domain, and their electro-optic coefficients (γc = 76, 94, and 43 pm/V for the crystals with x = 0.27, 0.30, and 0.39, respectively) were found to be much higher than that of traditional electro-optic single crystal LiNbO3 (γc = 19.9 pm/V). The electro-optic coefficients of the single crystal in the rhombohedral phase have excellent temperature stability in the experimental temperature range of 10–40 °C. The half-wave voltage Vπ was calculated to be much lower (less than 1000 V) than that of LiNbO3 single crystal (2800 V). These superior properties make the ternary relaxor-PT single crystals very promising for electro-optic modulation applications. PMID:23922449

Single crystal and optical ceramic multicomponent garnet scintillators: A comparative study

NASA Astrophysics Data System (ADS)

Wu, Yuntao; Luo, Zhaohua; Jiang, Haochuan; Meng, Fang; Koschan, Merry; Melcher, Charles L.

2015-04-01

Multicomponent garnet materials can be made in optical ceramic as well as single crystal form due to their cubic crystal structure. In this work, high-quality Gd3Ga3Al2O12:0.2 at% Ce (GGAG:Ce) single crystal and (Gd,Lu)3Ga3Al2O12:1 at% Ce (GLuGAG:Ce) optical ceramics were fabricated by the Czochralski method and a combination of hot isostatic pressing (HIPing) and annealing treatment, respectively. Under optical and X-ray excitation, the GLuGAG:Ce optical ceramic exhibits a broad Ce3+ transition emission centered at 550 nm, while the emission peak of the GGAG:Ce single crystal is centered at 540 nm. A self-absorption effect in GLuGAG:Ce optical ceramic results in this red-shift of the Ce3+ emission peak compared to that in the GGAG:Ce single crystal. The light yield under 662 keV γ-ray excitation was 45,000±2500 photons/MeV and 48,200±2410 photons/MeV for the GGAG:Ce single crystal and GLuGAG:Ce optical ceramic, respectively. An energy resolution of 7.1% for 662 keV γ-rays was achieved in the GLuGAG:Ce optical ceramic with a Hamamatsu R6231 PMT, which is superior to the value of 7.6% for a GGAG:Ce single crystal. Scintillation decay time measurements under 137Cs irradiation show two exponential decay components of 58 ns (47%) and 504 ns (53%) for the GGAG:Ce single crystal, and 84 ns (76%) and 148 ns (24%) for the GLuGAG:Ce optical ceramic. The afterglow level after X-ray cutoff in the GLuGAG:Ce optical ceramic is at least one order of magnitude lower than in the GGAG:Ce single crystal.

Structural analysis of benzothienobenzothiophene-based soluble organic semiconducting crystals grown by liquid crystal solvent

NASA Astrophysics Data System (ADS)

Shibata, Yosei; Matsuzaki, Tomoya; Ishinabe, Takahiro; Fujikake, Hideo

2018-06-01

In this study, we analyzed organic semiconducting single crystals composed of benzothienobenzothiophene derivatives (2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene, C8-BTBT) grown by nematic-phase liquid crystal (LC) solvent. As a result, we clarified that the crystal b-axis direction of the C8-BTBT single crystals was consistent with the LC alignment direction. By optical evaluation and simulation based on density functional theory, we found that the C8-BTBT single crystals in LC solvent exhibited a novel molecular conformation having alkyl chains oriented toward the b-axis.

Elastic response of (001)-oriented PWA 1480 single crystal - The influence of secondary orientation

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Azis, Ali; Mcgaw, Michael

1991-01-01

The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

Ultrasound Flow Mapping for the Investigation of Crystal Growth.

PubMed

Thieme, Norman; Bonisch, Paul; Meier, Dagmar; Nauber, Richard; Buttner, Lars; Dadzis, Kaspars; Patzold, Olf; Sylla, Lamine; Czarske, Jurgen

2017-04-01

A high energy conversion and cost efficiency are keys for the transition to renewable energy sources, e.g., solar cells. The efficiency of multicrystalline solar cells can be improved by enhancing the understanding of its crystallization process, especially the directional solidification. In this paper, a novel measurement system for the characterization of flow phenomena and solidification processes in low-temperature model experiments on the basis of ultrasound (US) Doppler velocimetry is described. It captures turbulent flow phenomena in two planes with a frame rate of 3.5 Hz and tracks the shape of the solid-liquid interface during multihour experiments. Time-resolved flow mapping is performed using four linear US arrays with a total of 168 transducer elements. Long duration measurements are enabled through an online, field-programmable gate array (FPGA)-based signal processing. Nine single US transducers allow for in situ tracking of a solid-liquid interface. Results of flow and solidification experiments in the model experiment are presented and compared with numerical simulation. The potential of the developed US system for measuring turbulent flows and for tracking the solidification front during a directional crystallization process is demonstrated. The results of the model experiments are in good agreement with numerical calculations and can be used for the validation of numerical models, especially the selection of the turbulence model.

Method of making single crystal fibers

NASA Technical Reports Server (NTRS)

Westfall, Leonard J. (Inventor)

1990-01-01

Single crystal fibers are made from miniature extruded ceramic feed rods. A decomposable binder is mixed with powders to inform a slurry which is extruded into a small rod which may be sintered, either in air or in vacuum, or it may be used in the extruded and dried condition. A pair of laser beams focuses onto the tip of the rod to melt it thereby forming a liquid portion. A single crystal seed fiber of the same material as the feed rod contacts this liquid portion to establish a zone of liquid material between the feed rod and the single crystal seed fiber. The feed rod and the single crystal feed fiber are moved at a predetermined speed to solidify the molten zone onto the seed fiber while simultaneously melting additional feed rod. In this manner a single crystal fiber is formed from the liquid portion.

Effect of grain boundary on the field-effect mobility of microrod single crystal organic transistors.

PubMed

Kim, Jaekyun; Kang, Jingu; Cho, Sangho; Yoo, Byungwook; Kim, Yong-Hoon; Park, Sung Kyu

2014-11-01

High-performance microrod single crystal organic transistors based on a p-type 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) semiconductor are fabricated and the effects of grain boundaries on the carrier transport have been investigated. The spin-coating of C8-BTBT and subsequent solvent vapor annealing process enabled the formation of organic single crystals with high aspect ratio in the range of 10 - 20. It was found that the organic field-effect transistors (OFETs) based on these single crystals yield a field-effect mobility and an on/off current ratio of 8.04 cm2/Vs and > 10(5), respectively. However, single crystal OFETs with a kink, in which two single crystals are fused together, exhibited a noticeable drop of field-effect mobility, and we claim that this phenomenon results from the carrier scattering at the grain boundary.

Single crystal diamond membranes for nanoelectronics.

PubMed

Bray, Kerem; Kato, Hiromitsu; Previdi, Rodolfo; Sandstrom, Russell; Ganesan, Kumaravelu; Ogura, Masahiko; Makino, Toshiharu; Yamasaki, Satoshi; Magyar, Andrew P; Toth, Milos; Aharonovich, Igor

2018-02-22

Single crystal, nanoscale diamond membranes are highly sought after for a variety of applications including nanophotonics, nanoelectronics and quantum information science. However, so far, the availability of conductive diamond membranes has remained an unreachable goal. In this work we present a complete nanofabrication methodology for engineering high aspect ratio, electrically active single crystal diamond membranes. The membranes have large lateral directions, exceeding ∼500 × 500 μm 2 and are only several hundreds of nanometers thick. We further realize vertical single crystal p-n junctions made from the diamond membranes that exhibit onset voltages of ∼10 V and a current of several mA. Moreover, we deterministically introduce optically active color centers into the membranes, and demonstrate for the first time a single crystal nanoscale diamond LED. The robust and scalable approach to engineer the electrically active single crystal diamond membranes offers new pathways for advanced nanophotonic, nanoelectronic and optomechanical devices employing diamond.

The effect of Fe 3+ doping in Potassium Hydrogen Phthalate single crystals on structural and optical properties

NASA Astrophysics Data System (ADS)

Kumar, R. Ashok; Sivakumar, N.; Vizhi, R. Ezhil; Babu, D. Rajan

2011-02-01

This work investigates the influence of iron doping on Potassium Hydrogen Phthalate (KHP) single crystals by the slow evaporation solution growth technique. Factors such as evaporation rate, solution pH, solute concentration, super saturation limit, etc. are very important in order to have optically transparent single crystals. As part of the work, the effects of metallic salt FeCl 3 in different concentrations were analyzed with pure KHP. Powder X-ray diffraction suggests that the grown crystals are crystallized in the orthorhombic structure. The functional groups and the effect of moisture on the doped crystals can be analyzed with the help of a FTIR spectrum. The pure and doped KHP single crystal shows good transparency in the entire visible region, which is suitable for optical device applications. The refractive indices along b axis of pure and doped KHP single crystals were analyzed by the prism coupling technique. The emission of green light with the use of a Nd:YAG laser ( λ=1064 nm) confirmed the second harmonic generation properties of the grown crystals.

Photoconductive and electro-optic effects in (Cd,Mg)Te single crystals measured in an experiment-on-chip configuration

NASA Astrophysics Data System (ADS)

Serafini, John; Hossain, A.; James, R. B.; Guziewicz, M.; Kruszka, R.; Słysz, W.; Kochanowska, D.; Domagala, J. Z.; Mycielski, A.; Sobolewski, Roman

2017-07-01

We present our studies on both photoconductive (PC) and electro-optic (EO) responses of (Cd,Mg)Te single crystals. In an In-doped Cd0.92Mg0.08Te single crystal, subpicosecond electrical pulses were optically generated via a PC effect, coupled into a transmission line, and, subsequently, detected using an internal EO sampling scheme, all in the same (Cd,Mg)Te material. For photo-excitation and EO sampling, we used femtosecond optical pulses generated by the same Ti:sapphire laser with the wavelengths of 410 and 820 nm, respectively. The shortest transmission line distance between the optical excitation and EO sampling points was 75 μm. By measuring the transient waveforms at different distances from the excitation point, we calculated the transmission-line complex propagation factor, as well as the THz frequency attenuation factor and the propagation velocity, all of which allowed us to reconstruct the electromagnetic transient generated directly at the excitation point, showing that the original PC transient was subpicosecond in duration with a fall time of ˜500 fs. Finally, the measured EO retardation, together with the amount of the electric-field penetration, allowed us to determine the magnitude of the internal EO effect in our (Cd,Mg)Te crystal. The obtained THz-frequency EO coefficient was equal to 0.4 pm/V, which is at the lower end among the values reported for CdTe-based ternaries, apparently, due to the disorientation of the tested crystal that resulted in the non-optimal EO measurement condition.

Photoconductive and electro-optic effects in (Cd,Mg)Te single crystals measured in an experiment-on-chip configuration

DOE PAGES

Serafini, John; Hossain, A.; James, R. B.; ...

2017-07-03

We present our studies on both photoconductive (PC) and electro-optic (EO) responses of (Cd,Mg)Te single crystals. In an In-doped Cd 0.92Mg 0.08Te single crystal, subpicosecond electrical pulses were optically generated via a PC effect, coupled into a transmission line, and, subsequently, detected using an internal EO sampling scheme, all in the same (Cd,Mg)Te material. For photo-excitation and EO sampling, we used femtosecond optical pulses generated by the same Ti:sapphire laser with the wavelength 410 and 820 nm, respectively. The shortest transmission line distance between the optical excitation and EO sampling points was 75 μm. By measuring the transient waveforms atmore » different distances from the excitation point, we calculated the transmission-line complex propagation factor, as well as the THz frequency attenuation factor and the propagation velocity, all of which allowed us to reconstruct the electromagnetic transient generated directly at the excitation point, showing that the original PC transient was subpicosecond in duration with a fall time of ~500 fs. Finally, the measured EO retardation, together with the amount of the electric-field penetration, allowed us to determine the magnitude of the internal EO effect in our (Cd,Mg)Te crystal. The obtained THz-frequency EO coefficient was equal to 0.4 pm/V, which is at the lower end among the values reported for CdTe-based ternaries, due to a twinned structure and misalignment of the tested (Cd,Mg)Te crystal.« less

First- and second-order Raman scattering from MoTe2 single crystal

NASA Astrophysics Data System (ADS)

Caramazza, Simone; Collina, Arianna; Stellino, Elena; Ripanti, Francesca; Dore, Paolo; Postorino, Paolo

2018-02-01

We report on Raman experiments performed on a MoTe2 single crystal. The system belongs to the wide family of transition metal dichalcogenides which includes several of the most interesting two-dimensional materials for both basic and applied physics. Measurements were performed in the standard basal plane configuration, by placing the ab plane of the crystal perpendicular to the wave vector k i of the incident beam to explore the in-plane vibrational modes, and in the edge plane configuration with k i perpendicular to the crystal c axis, thus mainly exciting out-of-plane modes. For both configurations we performed a polarization-dependent study of the first-order Raman components and detailed computation of the corresponding selection rules. We were thus able to provide a complete assignment of the observed first-order Raman peaks, in agreement with previous literature results. A thorough analysis of the second-order Raman bands, as observed in both basal and edge plane configurations, provides new information and allows a precise assignment of these spectral structures. In particular, we have observed and assigned Raman active modes of the M point of the Brillouin zone previously predicted by ab initio calculations but never previously measured.

Reduction of oxygen concentration by heater design during Czochralski Si growth

NASA Astrophysics Data System (ADS)

Zhou, Bing; Chen, Wenliang; Li, Zhihui; Yue, Ruicun; Liu, Guowei; Huang, Xinming

2018-02-01

Oxygen is one of the highest-concentration impurities in single crystals grown by the Czochralski (CZ) process, and seriously impairs the quality of the Si wafer. In this study, computer simulations were applied to design a new CZ system. A more appropriate thermal field was acquired by optimization of the heater structure. The simulation results showed that, compared with the conventional system, the oxygen concentration in the newly designed CZ system was reduced significantly throughout the entire CZ process because of the lower crucible wall temperature and optimized convection. To verify the simulation results, experiments were conducted on an industrial single-crystal furnace. The experimental results showed that the oxygen concentration was reduced significantly, especially at the top of the CZ-Si ingot. Specifically, the oxygen concentration was 6.19 × 1017 atom/cm3 at the top of the CZ-Si ingot with the newly designed CZ system, compared with 9.22 × 1017 atom/cm3 with the conventional system. Corresponding light-induced degradation of solar cells based on the top of crystals from the newly designed CZ system was 1.62%, a reduction of 0.64% compared with crystals from the conventional system (2.26%).

Effects of wear on structure-sensitive magnetic properties of ceramic ferrite in contact with magnetic tape

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.; Tanaka, K.

1985-01-01

Wear experiments and electron microscopy and diffraction studies were conducted to examine the wear and deformed layers in single-crystal Mn-Zn (ceramic) ferrite magnetic head material in contact with magnetic tape and the effects of that contact on magnetic properties. The crystalline state of the single-crystal magnetic head was changed drastically during the sliding process. A nearly amorphous structure was produced on its wear surface. Deformation in the surficial layer of the magnetic head was a critical factor in readback signal loss above 2.5 dB. The signal output level was reduced as applied normal load was increased. Considerable plastic flow occurred on the magnetic tape surface with sliding, and the signal loss due to the tape wear was approximately 1 dB.

Multigap superconductivity and strong electron-boson coupling in Fe-based superconductors: a point-contact Andreev-reflection study of Ba(Fe(1-x)Co(x))2As2 single crystals.

PubMed

Tortello, M; Daghero, D; Ummarino, G A; Stepanov, V A; Jiang, J; Weiss, J D; Hellstrom, E E; Gonnelli, R S

2010-12-03

Directional point-contact Andreev-reflection measurements in Ba(Fe(1-x)Co(x))2As2 single crystals (T(c) = 24.5 K) indicate the presence of two superconducting gaps with no line nodes on the Fermi surface. The point-contact Andreev-reflection spectra also feature additional structures related to the electron-boson interaction, from which the characteristic boson energy Ω(b)(T) is obtained, very similar to the spin-resonance energy observed in neutron scattering experiments. Both the gaps and the additional structures can be reproduced within a three-band s ± Eliashberg model by using an electron-boson spectral function peaked at Ω(0) = 12 meV ≃ Ω(b)(0).

Friction and wear of single-crystal and polycrystalline maganese-zinc ferrite in contact with various metals

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1977-01-01

Sliding friction experiments were conducted with single-crystal (SCF) and hot-pressed polycrystalline (HPF) manganese-zinc ferrite in contact with various metals. Results indicate that the coefficients of friction for SCF and HPF are related to the relative chemical activity of those metals in high vacuum. The more active the metal, the higher the coefficient of friction. The coefficients of friction for both SCF and HPF were the same and much higher in vacuum than in argon at atmospheric pressure. All the metals tested transferred to the surface of both SCF and HPF in sliding. Both SCF and HPF exhibited cracking and fracture with sliding. Cracking in SCF is dependent on crystallographic characteristics. In HPF, cracking depends on the orientation of the individual crystallites.

Sensitivity of Cirrus Bidirectional Reflectance at MODIS Bands to Vertical Inhomogeneity of Ice Crystal Habits and Size Distribution

NASA Technical Reports Server (NTRS)

Yang, P.; Gao, B.-C.; Baum, B. A.; Wiscombe, W.; Hu, Y.; Nasiri, S. L.; Soulen, P. F.; Heymsfield, A. J.; McFarquhar, G. M.; Miloshevich, L. M.

2000-01-01

A common assumption in satellite imager-based cirrus retrieval algorithms is that the radiative properties of a cirrus cloud may be represented by those associated with a specific ice crystal shape (or habit) and a single particle size distribution. However, observations of cirrus clouds have shown that the shapes and sizes of ice crystals may vary substantially with height within the clouds. In this study we investigate the sensitivity of the top-of-atmosphere bidirectional reflectances at two MODIS bands centered at 0.65 micron and 2.11 micron to the cirrus models assumed to be either a single homogeneous layer or three distinct but contiguous, layers. First, we define the single- and three-layer cirrus cloud models with respect to ice crystal habit and size distribution on the basis of in situ replicator data acquired during the First ISCCP Regional Experiment (FIRE-II), held in Kansas during the fall of 1991. Subsequently, fundamental light scattering and radiative transfer theory is employed to determine the single scattering and the bulk radiative properties of the cirrus cloud. Regarding the radiative transfer computations, we present a discrete form of the adding/doubling principle by introducing a direct transmission function, which is computationally straightforward and efficient an improvement over previous methods. For the 0.65 micron band, at which absorption by ice is negligible, there is little difference between the bidirectional reflectances calculated for the one- and three-layer cirrus models, suggesting that the vertical inhomogeneity effect is relatively unimportant. At the 2.11 micron band, the bidirectional reflectances computed for both optically thin (tau = 1) and thick (tau = 10) cirrus clouds show significant differences between the results for the one- and three-layer models. The reflectances computed for the three-layer cirrus model are substantially larger than those computed for the single-layer cirrus. Finally, we find that cloud reflectance is very sensitive to the optical properties of the small crystals that predominate in the top layer of the three-layer cirrus model. It is critical to define the most realistic geometric shape for the small "quasi-spherical" ice crystals in the top layer for obtaining reliable single-scattering parameters and bulk radiative properties of cirrus.

Strain coupling between nitrogen vacancy centers and the mechanical motion of a diamond optomechanical crystal resonator

NASA Astrophysics Data System (ADS)

Cady, J. V.; Lee, K. W.; Ovartchaiyapong, P.; Bleszynski Jayich, A. C.

Several experiments have recently demonstrated coupling between nitrogen vacancy (NV) centers in diamond and mechanical resonators via crystal strain. In the strong coupling regime, such devices could realize applications critical to emerging quantum technologies, including phonon-mediated spin-spin interactions and mechanical cooling with the NV center1. An outstanding challenge for these devices is generating higher strain coupling in high frequency devices while maintaining the excellent coherence properties of the NV center and high mechanical quality factors. As a step toward these objectives, we demonstrate single-crystal diamond optomechanical crystal resonators with embedded NV centers. These devices host highly-confined GHz-scale mechanical modes that are isolated from mechanical clamping losses and generate strain profiles that allow for large strain coupling to NV centers far from noise-inducing surfaces.

Applications of Classical and Quantum Mechanical Channeling in Condensed Matter Physics

NASA Astrophysics Data System (ADS)

Haakenaasen, Randi

1995-01-01

The first part of this work involves ion channeling measurements on the high temperature superconductor rm YBa_{2}Cu_{3}O _{7-delta}(YBCO). The experiments were motivated by several previous reports of anomalous behavior in the displacements of the Cu and O atoms in the vicinity of the critical temperature rm(T _{c}) in several high temperature superconductors. Our measurements were complimentary to previous experiments in that we used thin film YBCO (as opposed to bulk single crystals) and focused on a small region around rm T_{c}. We mapped out the channeling parameters chi _{min} and Psi_ {1/2} in a 30 K region around rm T_{c} in 1-2 K steps in thin film YBCO(001) on MgO. Neither of our measurements showed any discontinuities in chi _{min} or Psi_ {1/2} near the superconducting phase transition, and we therefore have no reason to expect anything but a smooth increase in atomic vibrations in this region. We conclude that any anomalous behavior in atomic displacements deduced from previous channeling experiments is not essential to superconductivity. In the second part of the work positrons were used to study quantum mechanical channeling effects. We clearly observed and quantitatively accounted for quantum interference effects, including Bragg diffraction, in the forward transmission of channeled MeV positrons through a single crystal. Experimental scans across the (100), (110), and (111) planes in Si showed excellent agreement with theoretical dynamical diffraction calculations, giving us confidence that we can accurately predict the spatial and momentum distributions of channeled positrons. New experiments are envisioned in which the channeling effect is combined with 2 quantum annihilation in flight measurements to determine valence electron and magnetic spin distributions in a crystal. Since the channeling effect focuses the positrons to the interstices of the crystal, the annihilation rate will reflect the valence electron density. Furthermore, the annihilation rate is sensitive to electron spin polarization, opening up the possibility of making measurements on magnetic materials. Detailed estimates for the count rates of such experiments are presented, indicating the feasibility of developing positron channeling into a new tool in solid state physics.

Crystal-field analysis of U3+ ions in K2LaX5 (X=Cl, Br or I) single crystals

NASA Astrophysics Data System (ADS)

Karbowiak, M.; Edelstein, N.; Gajek, Z.; Drożdżyński, J.

1998-11-01

An analysis of low temperature absorption spectra of U3+ ions doped in K2LaX5 (X=Cl, Br or I) single crystals is reported. The energy levels of the U3+ ion in the single crystals were assigned and fitted to a semiempirical Hamiltonian representing the combined atomic and crystal-field interactions at the Cs symmetry site. An analysis of the nephelauxetic effect and crystal-field splittings in the series of compounds is also reported.

Averaging of elastic constants for polycrystals

DOE PAGES

Blaschke, Daniel N.

2017-10-13

Many materials of interest are polycrystals, i.e., aggregates of single crystals. Randomly distributed orientations of single crystals lead to macroscopically isotropic properties. Here in this paper, we briefly review strategies of calculating effective isotropic second and third order elastic constants from the single crystal ones. Our main emphasis is on single crystals of cubic symmetry. Specifically, the averaging of third order elastic constants has not been particularly successful in the past, and discrepancies have often been attributed to texturing of polycrystals as well as to uncertainties in the measurement of elastic constants of both poly and single crystals. While thismore » may well be true, we also point out here shortcomings in the theoretical averaging framework.« less

Development of a Single-Crystal Fifth-Generation Nickel Superalloy

NASA Astrophysics Data System (ADS)

Petrushin, N. V.; Elyutin, E. S.; Visik, E. M.; Golynets, S. A.

2017-11-01

The chemical and phase compositions of a rhenium-ruthenium-containing fifth-generation VZhM8 nickel superalloy, which is intended for single-crystal turbine blades of an aviation engine, are calculated using computer simulation. VZhM8 alloy <001>, <011>, and <111> single crystals are fabricated. The microstructure, the γ/γ' misfit, the segregation coefficients of alloying elements, the dissolution temperature of the γ' phase, and the solidus and liquidus temperatures of the VZhM8 alloy single crystals in the as-cast state and after heat treatment are studied. The temperature-time dependences of the static elastic modulus, the short-term mechanical properties, and the long-term strength of the alloy single crystals are determined

Growth and studies of cyclohexylammonium 4-methoxy benzoate single crystal for nonlinear optical applications

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

Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@annauniv.edu

2015-06-24

Cyclohexylammonium 4-Methoxy Benzoate (C4MB) was synthesised and the functional groups were confirmed by FTIR analysis. The purified C4MB (by repeated recrystallisation) was used for single crystal growth. Single crystal of cyclohexylammonium 4-methoxy benzoate was successfully grown by slow evaporation solution growth method at ambient temperature. Structural orientations were determined from single crystal X-ray diffractometer. Optical absorption and cut off wavelength were identified by UV-Visible spectroscopy. Thermal stability of the crystal was studied from thermogravimetric and differential thermal analyses curves. Mechanical stability of the grown crystal was analysed by Vicker’s microhardness tester. The Second Harmonic Generation (SHG) study revealed that themore » C4MB compound exhibits the SHG efficiency 3.3 times greater than KDP crystal.« less

Synthesis, structural, thermal and Hirshfeld surface analysis of novel [1,2,4]triazolo[3,4-b][1,3,4] thiadiazine carrying 1,4-benzothiazine-3-one moiety

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped single crystal of the title compound was grown by slow evaporation solution growth technique using ethanol as solvent. The grown single crystal was characterized using FT-IR, Single crystal XRD and Thermal analysis. The FT-IR spectrum confirms the molecular structure and identifies the different functional groups present in the compound. Single crystal XRD study reveals that the crystallized compound belongs to the monoclinic crystal system with P21/c space group and the corresponding cell parameters were identified. The thermal stability of the material was determined using both TGA and DTA analysis. The intermolecular interaction of each individual atom in the crystal lattice was estimated using Hirshfeld surface and finger print analysis.

Influence of solvents on the habit modification of alpha lactose monohydrate single crystals

NASA Astrophysics Data System (ADS)

Parimaladevi, P.; Srinivasan, K.

2013-02-01

Restricted evaporation of solvent method was adopted for the growth of alpha lactose monohydrate single crystals from different solvents. The crystal habits of grown crystals were analysed. The form of crystallization was confirmed by powder x-ray diffraction analysis. Thermal behaviour of the grown crystals was studied by using differential scanning calorimetry.

Analytical studies on the crystal melt interface shape in the Czochralski process for oxide single crystals

NASA Astrophysics Data System (ADS)

Jeong, Ja Hoon; Kang, In Seok

2000-09-01

Effects of the operating conditions on the crystal-melt interface shape are analytically investigated for the Czochralski process of the oxide single crystals. The ideas, which were used for the silicon single-crystal growth by Jeong et al. (J. Crystal Growth 177 (1997) 157), are extended to the oxide single-crystal growth problem by considering the internal radiation in the crystal phase and the melt phase heat transfer with the high Prandtl number. The interface shape is approximated in the simplest form as a quadratic function of radial position and an expression for the deviation from the flat interface shape is derived as a function of operating conditions. The radiative heat transfer rate between the interface and the ambient is computed by calculating the view factors for the curved interface shape with the assumption that the crystal phase is completely transparent. For the melt phase, the well-known results from the thermal boundary layer analysis are applied for the asymptotic case of high Prandtl number based on the idea that the flow field near the crystal-melt interface can be modeled as either a uniaxial or a biaxial flow. Through this work, essential information on the interface shape deformation and the effects of operating conditions are brought out for the oxide single-crystal growth.

Crystal structure, spectral, thermal and dielectric studies of a new zinc benzoate single crystal

NASA Astrophysics Data System (ADS)

Bijini, B. R.; Prasanna, S.; Deepa, M.; Nair, C. M. K.; Rajendra Babu, K.

2012-11-01

Single crystals of zinc benzoate with a novel structure were grown in gel media. Sodium metasilicate of gel density 1.04 g/cc at pH 6 was employed to yield transparent single crystals. The crystal structure of the compound was ascertained by single crystal X-ray diffractometry. It was noted that the crystal belongs to monoclinic system with space group P21/c with unit cell parameters a = 10.669(1) Å, b = 12.995(5) Å, c = 19.119(3) Å, and β = 94.926(3)°. The crystal was seen to possess a linear polymeric structure along b-axis; with no presence of coordinated or lattice water. CHN analysis established the stoichiometric composition of the crystal. The existence of functional groups present in the single crystal system was confirmed by FT-IR studies. The thermal characteristic of the sample was analysed by TGA-DTA techniques, and the sample was found to be thermally stable up to 280 °C. The kinetic and thermodynamic parameters were also determined. UV-Vis spectroscopy corroborated the transparency of the crystal and revealed the optical band gap to be 4 eV. Dielectric studies showed decrease in the dielectric constant of the sample with increase in frequency.

Reliability Studies of Ceramic Capacitors.

DTIC Science & Technology

1983-07-01

increases. This case has been found to be a good approximation for single crystals with high chemical and structural purity. Shallow traps may arise as a...theory, this sudden increase may be otherwise explained. Single crystals of ZnS have been found to exhibit this vertical increase in the current...Smith and Rose observed SCLC behavior in CdS single crystals . Branwood and Tredgold 2 8 and Branwood et al. 2 9 measured BaTiO 3 single crystals and

Reversible conversion of valence-tautomeric copper metal-organic frameworks dependent single-crystal-to-single-crystal oxidation/reduction: a redox-switchable catalyst for C-H bonds activation reaction.

PubMed

Huang, Chao; Wu, Jie; Song, Chuanjun; Ding, Ran; Qiao, Yan; Hou, Hongwei; Chang, Junbiao; Fan, Yaoting

2015-06-28

Upon single-crystal-to-single-crystal (SCSC) oxidation/reduction, reversible structural transformations take place between the anionic porous zeolite-like Cu(I) framework and a topologically equivalent neutral Cu(I)Cu(II) mixed-valent framework. The unique conversion behavior of the Cu(I) framework endowed it as a redox-switchable catalyst for the direct arylation of heterocycle C-H bonds.

Solution-grown organic single-crystalline p-n junctions with ambipolar charge transport.

PubMed

Fan, Congcheng; Zoombelt, Arjan P; Jiang, Hao; Fu, Weifei; Wu, Jiake; Yuan, Wentao; Wang, Yong; Li, Hanying; Chen, Hongzheng; Bao, Zhenan

2013-10-25

Organic single-crystalline p-n junctions are grown from mixed solutions. First, C60 crystals (n-type) form and, subsequently, C8-BTBT crystals (p-type) nucleate heterogeneously on the C60 crystals. Both crystals continue to grow simultaneously into single-crystalline p-n junctions that exhibit ambipolar charge transport characteristics. This work provides a platform to study organic single-crystalline p-n junctions. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Growth and nonlinear optical characterization of organic single crystal films

NASA Astrophysics Data System (ADS)

Zhou, Ligui

1997-12-01

Organic single crystal films are important for various future applications in photonics and integrated optics. The conventional method for inorganic crystal growth is not suitable for organic materials, and the high temperature melting method is not good for most organic materials due to decomposition problems. We developed a new method-modified shear method-to grow large area organic single crystal thin films which have exceptional nonlinear optical properties and high quality surfaces. Several organic materials (NPP, PNP and DAST) were synthesized and purified before the thin film crystal growth. Organic single crystal thin films were grown from saturated organic solutions using modified shear method. The area of single crystal films were about 1.5 cm2 for PNP, 1 cm2 for NPP and 5 mm2 for DAST. The thickness of the thin films which could be controlled by the applied pressure ranged from 1μm to 10 μm. The single crystal thin films of organic materials were characterized by polarized microscopy, x-ray diffraction, polarized UV-Visible and polarized micro-FTIR spectroscopy. Polarized microscopy showed uniform birefringence and complete extinction with the rotation of the single crystal thin films under crossed- polarization, which indicated high quality single crystals with no scattering. The surface orientation of single crystal thin films was characterized by x-ray diffraction. The molecular orientation within the crystal was further studied by the polarized UV-Visible and Polarized micro-FTIR techniques combined with the x-ray and polarized microscopy results. A Nd:YAG laser with 35 picosecond pulses at 1064nm wavelength was employed to perform the nonlinear optical characterization of the organic single crystal thin films. Two measurement techniques were used to study the crystal films: second harmonic generation (SHG) and electro-optic (EO) effect. SHG results showed that the nonlinear optical coefficient of NPP was 18 times that of LiNbO3, a standard inorganic crystal material, and the nonlinear optical coefficient of PNP was 11 times that of LiNbO3. Electro-optic measurements showed that r11 = 65 pm/V for NPP and r12 = 350 pm/V for DAST. EO modulation effect was also observed using Fabry-Perot interferometry. Waveguide devices are very important for integrated optics. But the fabrication of waveguide devices on the organic single crystal thin films was difficult due to the solubility of the film in common organic solvents. A modified photolithographic technique was employed to make channel waveguides and poly(vinyl alcohol) (PVA) was used as a protective layer in the fabrication of the waveguides. Waveguides with dimensions about 7/mum x 1μm x 1mm were obtained.

Synthesis, growth, structural and optical studies of a novel organic Piperazine (bis) p-toluenesulfonate single crystal.

PubMed

Rekha, P; Peramaiyan, G; NizamMohideen, M; Kumar, R Mohan; Kanagadurai, R

2015-03-15

A novel organic single crystal of Piperazinium (bis) p-toluenesulfonate (PPTS) was grown by a slow evaporation solution growth technique. The structure of the grown crystal was determined using single crystal X-ray diffraction analysis. The PPTS crystal belongs to the triclinic crystal system with space group of P1¯. The presence of functional groups was confirmed by FTIR spectral analysis. The optical transmittance range and cut-off wavelength were identified by UV-vis-NIR spectral studies. The luminescent properties of PPTS crystal were investigated. The thermal behavior of PPTS crystal was studied by TG-DT analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Structure and Growth Control of Organic-Inorganic Halide Perovskites for Optoelectronics: From Polycrystalline Films to Single Crystals.

PubMed

Chen, Yani; He, Minhong; Peng, Jiajun; Sun, Yong; Liang, Ziqi

2016-04-01

Recently, organic-inorganic halide perovskites have sparked tremendous research interest because of their ground-breaking photovoltaic performance. The crystallization process and crystal shape of perovskites have striking impacts on their optoelectronic properties. Polycrystalline films and single crystals are two main forms of perovskites. Currently, perovskite thin films have been under intensive investigation while studies of perovskite single crystals are just in their infancy. This review article is concentrated upon the control of perovskite structures and growth, which are intimately correlated for improvements of not only solar cells but also light-emitting diodes, lasers, and photodetectors. We begin with the survey of the film formation process of perovskites including deposition methods and morphological optimization avenues. Strategies such as the use of additives, thermal annealing, solvent annealing, atmospheric control, and solvent engineering have been successfully employed to yield high-quality perovskite films. Next, we turn to summarize the shape evolution of perovskites single crystals from three-dimensional large sized single crystals, two-dimensional nanoplates, one-dimensional nanowires, to zero-dimensional quantum dots. Siginificant functions of perovskites single crystals are highlighted, which benefit fundamental studies of intrinsic photophysics. Then, the growth mechanisms of the previously mentioned perovskite crystals are unveiled. Lastly, perspectives for structure and growth control of perovskites are outlined towards high-performance (opto)electronic devices.

Ames Lab 101: Single Crystal Growth

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

Schlagel, Deborah

2013-09-27

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

Ames Lab 101: Single Crystal Growth

ScienceCinema

Schlagel, Deborah

2018-01-16

Ames Laboratory scientist Deborah Schlagel talks about the Lab's research in growing single crystals of various metals and alloys. The single crystal samples are vital to researchers' understanding of the characteristics of a materials and what gives these materials their particular properties.

Elastic response of zone axis (001)-oriented PWA 1480 single crystal: The influence of secondary orientation

NASA Technical Reports Server (NTRS)

Kalluri, Sreeramesh; Abdul-Aziz, Ali; Mcgaw, Michael A.

1991-01-01

The influence of secondary orientation on the elastic response of a zone axis (001)-oriented nickel-base single-crystal superalloy, PWA 1480, was investigated under mechanical loading conditions by applying finite element techniques. Elastic stress analyses were performed with a commercially available finite element code. Secondary orientation of the single-crystal superalloy was offset with respect to the global coordinate system in increments from 0 to 90 deg and stresses developed within the single crystal were determined for each loading condition. The results indicated that the stresses were strongly influenced by the angular offset between the secondary crystal orientation and the global coordinate system. The degree of influence was found to vary with the type of loading condition (mechanical, thermal, or combined) imposed on the single-crystal superalloy.

Study on structural, morphological, optical and thermal properties of guanidine carbonate doped nickel sulfate hexahydrate crystal.

PubMed

Silambarasan, A; Rajesh, P; Ramasamy, P

2015-01-05

The single crystal of guanidine carbonate doped nickel sulfate hexahydrate was grown from solution for ultraviolet filters. The single crystal XRD confirms that the grown single crystal belongs to the tetragonal system with the space group of P4₁2₁2. The crystallinity of the grown crystal was estimated by powder X-ray diffraction studies. The optical transmission and thermal stability of as-grown guanidine carbonate doped nickel sulfate single crystals have been studied. The optical transmission spectrum demonstrates the characteristics of ultraviolet filters. The TG/DTA studies confirm the thermal properties of grown crystals. Thermo-gravimetric analysis showed that the dehydration temperature of the guanidine carbonate doped nickel sulfate crystal is about 100 °C, which is much higher than that of pure nickel sulfate hexahydrate (NSH) crystals which is 72 °C. The growth behaviors and dislocation density were detected under the high resolution XRD and etching studies respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Room temperature aluminum antimonide radiation detector and methods thereof

DOEpatents

Lordi, Vincenzo; Wu, Kuang Jen J.; Aberg, Daniel; Erhart, Paul; Coombs, III, Arthur W; Sturm, Benjamin W

2015-03-03

In one embodiment, a method for producing a high-purity single crystal of aluminum antimonide (AlSb) includes providing a growing environment with which to grow a crystal, growing a single crystal of AlSb in the growing environment which comprises hydrogen (H.sub.2) gas to reduce oxide formation and subsequent incorporation of oxygen impurities in the crystal, and adding a controlled amount of at least one impurity to the growing environment to effectively incorporate at least one dopant into the crystal. In another embodiment, a high energy radiation detector includes a single high-purity crystal of AlSb, a supporting structure for the crystal, and logic for interpreting signals obtained from the crystal which is operable as a radiation detector at a temperature of about 25.degree. C. In one embodiment, a high-purity single crystal of AlSb includes AlSb and at least one dopant selected from a group consisting of selenium (Se), tellurium (Te), and tin (Sn).

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB6 Single Crystals

PubMed Central

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; Tutmaher, J. A.; Leiner, J. C.; Lumsden, M. D.; Lavelle, C. M.; Wang, X. P.; Hoffmann, C.; Siegler, M. A.; Haldolaarachchige, N.; Young, D. P.; McQueen, T. M.

2016-01-01

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-ray computed tomography experiments we observe that natural isotope containing (SmB6) and doubly isotope enriched (154Sm11B6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB6. These results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported. PMID:26892648

Insight into Flufenamic Acid Cocrystal Dissolution in the Presence of a Polymer in Solution: from Single Crystal to Powder Dissolution.

PubMed

Guo, Minshan; Wang, Ke; Qiao, Ning; Fábián, László; Sadiq, Ghazala; Li, Mingzhong

2017-12-04

Effects of three polymers, polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), and copolymer of vinylpyrrolidone/vinyl acetate (PVP-VA), on the dissolution behavior of the cocrystals of flufenamic acid with theophylline (FFA-TP CO) and nicotinamide (FFA-NIC CO) were investigated at multiple length scales. At the molecular level, the interactions of crystal surfaces with a polymer were analyzed by observing etching pattern changes using atomic force microscopy. At the macroscopic scale, dissolution rates of particular faces of a single crystal were determined by measurement of the physical retreat velocities of the faces using optical light microscopy. In the bulk experiments, the FFA concentration in a dissolution medium in the absence or presence of a polymer was measured under both sink and nonsink conditions. It has been found that the dissolution mechanisms of FFA-TP CO are controlled by the defect sites of the crystal surface and by precipitation of the parent drug FFA as individual crystals in the bulk fluid. In contrast, the dissolution mechanisms of FFA-NIC CO are controlled by surface layer removal and by a surface precipitation mechanism, where the parent drug FFA precipitates directly onto the surface of the dissolving cocrystals. Through controlling the dissolution environment by predissolving a polymer, PVP or PVP-VA, which can interact with the crystal surface to alter its dissolution properties, improved solubility, and dissolution rates of FFA-TP CO and FFA-NIC CO have been demonstrated.

On the Chemistry and Physical Properties of Flux and Floating Zone Grown SmB 6 Single Crystals

DOE PAGES

Phelan, W. A.; Koohpayeh, S. M.; Cottingham, P.; ...

2016-02-19

Recent theoretical and experimental findings suggest the long-known but not well understood low temperature resistance plateau of SmB 6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet others have ascribed this feature to impurities, vacancies, and surface reconstructions. Given the typical methods used to prepare SmB 6 single crystals, flux and floating-zone procedures, such ascriptions should not be taken lightly. We demonstrate how compositional variations and/or observable amounts of impurities in SmB 6 crystals grown using both procedures affect the physical properties. From X-ray diffraction, neutron diffraction, and X-raymore » computed tomography experiments we observe that natural isotope containing (SmB 6) and doubly isotope enriched ( 154Sm 11B 6) crystals prepared using aluminum flux contain co-crystallized, epitaxial aluminum. Further, a large, nearly stoichiometric crystal of SmB 6 was successfully grown using the float-zone technique; upon continuing the zone melting, samarium vacancies were introduced. These samarium vacancies drastically alter the resistance and plateauing magnitude of the low temperature resistance compared to stoichiometric SmB 6. Finally, these results highlight that impurities and compositional variations, even at low concentrations, must be considered when collecting/analyzing physical property data of SmB 6. Finally, a more accurate samarium-154 coherent neutron scattering length, 8.9(1) fm, is reported.« less

Low Leakage Superconducting Tunnel Junctions with a Single Crystal Al2O3 Barrier

DTIC Science & Technology

2016-03-30

have recently implemented Josephson junction superconducting devices into qubits [1-6]. Before a multi -qubit quantum computer is realized, however...Low-Leakage Superconducting Tunnel Junctions with a Single-Crystal Al2O3 Barrier* S Oh1,2, K Cicak1, R McDermott3, K B Cooper3, K D Osborn1, R W...growth scheme for single-crystal Al2O3 tunnel barriers. The barriers are epitaxially grown on single-crystal rhenium (Re) base electrodes that are

Direct detection of light dark matter and solar neutrinos via color center production in crystals

NASA Astrophysics Data System (ADS)

Budnik, Ranny; Cheshnovsky, Ori; Slone, Oren; Volansky, Tomer

2018-07-01

We propose a new low-threshold direct-detection concept for dark matter and for coherent nuclear scattering of solar neutrinos, based on the dissociation of atoms and subsequent creation of color center type defects within a lattice. The novelty in our approach lies in its ability to detect single defects in a macroscopic bulk of material. This class of experiments features ultra-low energy thresholds which allows for the probing of dark matter as light as O (10) MeV through nuclear scattering. Another feature of defect creation in crystals is directional information, which presents as a spectacular signal and a handle on background reduction in the form of daily modulation of the interaction rate. We discuss the envisioned setup and detection technique, as well as background reduction. We further calculate the expected rates for dark matter and solar neutrinos in two example crystals for which available data exists, demonstrating the prospective sensitivity of such experiments.

Can the propensity of protein crystallization be increased by using systematic screening with metals?

PubMed

Hegde, Raghurama P; Pavithra, Gowribidanur C; Dey, Debayan; Almo, Steven C; Ramakumar, S; Ramagopal, Udupi A

2017-09-01

Protein crystallization is one of the major bottlenecks in protein structure elucidation with new strategies being constantly developed to improve the chances of crystallization. Generally, well-ordered epitopes possessing complementary surface and capable of producing stable inter-protein interactions generate a regular three-dimensional arrangement of protein molecules which eventually results in a crystal lattice. Metals, when used for crystallization, with their various coordination numbers and geometries, can generate such epitopes mediating protein oligomerization and/or establish crystal contacts. Some examples of metal-mediated oligomerization and crystallization together with our experience on metal-mediated crystallization of a putative rRNA methyltransferase from Sinorhizobium meliloti are presented. Analysis of crystal structures from protein data bank (PDB) using a non-redundant data set with a 90% identity cutoff, reveals that around 67% of proteins contain at least one metal ion, with ∼14% containing combination of metal ions. Interestingly, metal containing conditions in most commercially available and popular crystallization kits generally contain only a single metal ion, with combinations of metals only in a very few conditions. Based on the results presented in this review, it appears that the crystallization screens need expansion with systematic screening of metal ions that could be crucial for stabilizing the protein structure or for establishing crystal contact and thereby aiding protein crystallization. © 2017 The Protein Society.

Studies of the crystallization of amorphous trehalose using simultaneous gravimetric vapor sorption/near IR (GVS/NIR) and "modulated" GVS/NIR.

PubMed

Moran, Abigail; Buckton, Graham

2009-01-01

The purpose of this research was to investigate the influence of changes in the amorphous state on the crystallization of trehalose. Amorphous trehalose is known to stabilize biomaterials; hence, an understanding of crystallization is vital. Amorphous trehalose, prepared by spray-drying, was exposed to either a single step (0-75%) in relative humidity (RH) or to modulated 0-75-0% RH to cause crystallization. For the single-step experiment, two samples crystallized in a predictable manner to form the dihydrate. One sample, while notionally identical, did not crystallize in the same way and showed a mass loss throughout the time at 75% RH, with a final mass less than that expected for the dihydrate. The idiosyncratic sample was seen to have a starting near infrared (NIR) spectra similar to that exhibited by anhydrous crystalline trehalose, implying that short-range order in the amorphous material (or a small amount of crystalline seed, not detectable using powder X-ray diffraction) caused the sample to fail to form the dihydrate fully when exposed to high RH. The modulated RH study showed that the amorphous material interacted strongly with water; the intensity of the NIR traces was not proportional to mass of water but rather the extent of hydrogen bonding. Subsequent crystallization of this sample clearly was a partial formation of the dihydrate, but with the bulk of the sample then shielded such that it was unable to show significant sorption when exposed to elevated RH. It has been shown that the nature of the amorphous form will alter the way in which samples crystallize. With oscillation in RH, it was possible to further understand the interactions between water and amorphous trehalose.

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

NASA Technical Reports Server (NTRS)

Chen, Po-Shou; Wilcox, Roy C.

1990-01-01

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

Attenuation of thermal neutrons by an imperfect single crystal

NASA Astrophysics Data System (ADS)

Naguib, K.; Adib, M.

1996-06-01

A semi-empirical formula is given which allows one to calculate the total thermal cross section of an imperfect single crystal as a function of crystal constants, temperature and neutron energy E, in the energy range between 3 meV and 10 eV. The formula also includes the contribution of the parasitic Bragg scattering to the total cross section that takes into account the crystal mosaic spread value and its orientation with respect to the neutron beam direction. A computer program (ISCANF) was developed to calculate the total attenuation of neutrons using the proposed formula. The ISCANF program was applied to investigate the neutron attenuation through a copper single crystal. The calculated values of the neutron transmission through the imperfect copper single crystal were fitted to the measured ones in the energy range 3 - 40 meV at different crystal orientations. The result of fitting shows that use of the computer program ISCANF allows one to predict the behaviour of the total cross section of an imperfect copper single crystal for the whole energy range.

Seeded growth of boron arsenide single crystals with high thermal conductivity

NASA Astrophysics Data System (ADS)

Tian, Fei; Song, Bai; Lv, Bing; Sun, Jingying; Huyan, Shuyuan; Wu, Qi; Mao, Jun; Ni, Yizhou; Ding, Zhiwei; Huberman, Samuel; Liu, Te-Huan; Chen, Gang; Chen, Shuo; Chu, Ching-Wu; Ren, Zhifeng

2018-01-01

Materials with high thermal conductivities are crucial to effectively cooling high-power-density electronic and optoelectronic devices. Recently, zinc-blende boron arsenide (BAs) has been predicted to have a very high thermal conductivity of over 2000 W m-1 K-1 at room temperature by first-principles calculations, rendering it a close competitor for diamond which holds the highest thermal conductivity among bulk materials. Experimental demonstration, however, has proved extremely challenging, especially in the preparation of large high quality single crystals. Although BAs crystals have been previously grown by chemical vapor transport (CVT), the growth process relies on spontaneous nucleation and results in small crystals with multiple grains and various defects. Here, we report a controllable CVT synthesis of large single BAs crystals (400-600 μm) by using carefully selected tiny BAs single crystals as seeds. We have obtained BAs single crystals with a thermal conductivity of 351 ± 21 W m-1 K-1 at room temperature, which is almost twice as conductive as previously reported BAs crystals. Further improvement along this direction is very likely.

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

Ji, Xiaoyu; Lei, Shiming; Yu, Shih -Ying

Semiconductor core optical fibers with a silica cladding are of great interest in nonlinear photonics and optoelectronics applications. Laser crystallization has been recently demonstrated for crystallizing amorphous silicon fibers into crystalline form. Here we explore the underlying mechanism by which long single-crystal silicon fibers, which are novel platforms for silicon photonics, can be achieved by this process. Using finite element modeling, we construct a laser processing diagram that reveals a parameter space within which single crystals can be grown. Utilizing this diagram, we illustrate the creation of single-crystal silicon core fibers by laser crystallizing amorphous silicon deposited inside silica capillarymore » fibers by high-pressure chemical vapor deposition. The single-crystal fibers, up to 5.1 mm long, have a very welldefined core/cladding interface and a chemically pure silicon core that leads to very low optical losses down to ~0.47-1dB/cm at the standard telecommunication wavelength (1550 nm). Furthermore, tt also exhibits a photosensitivity that is comparable to bulk silicon. Creating such laser processing diagrams can provide a general framework for developing single-crystal fibers in other materials of technological importance.« less

Mid-IR supercontinuum generation and applications: a review

NASA Astrophysics Data System (ADS)

Yin, Shizhuo; Ruffin, Paul; Brantley, Christina; Edwards, Eugene; Luo, Claire

2014-09-01

In this paper, a review on mid-IR supercontinuum generation (SCG) and its applications is presented. First, the physical mechanism of the supercontinuum generation in IR crystal fiber is introduced. Second, the recent progress on IR single crystal fiber, in particular ultrathin core double cladding IR single crystal fiber is described. Third, the transmission characteristics of mid-IR crystal fiber is illustrated. Fourth, the mid-IR supercontinuum generation in IR single crystal fiber is presented. Finally, the application of IR supercontinuum for smart target recognition is illustrated

Size dependence of nanoscale wear of silicon carbide

Treesearch

Chaiyapat Tangpatjaroen; David Grierson; Steve Shannon; Joseph E. Jakes; Izabela Szlufarska

2017-01-01

Nanoscale, single-asperity wear of single-crystal silicon carbide (sc- SiC) and nanocrystalline silicon carbide (nc-SiC) is investigated using single-crystal diamond nanoindenter tips and nanocrystalline diamond atomic force microscopy (AFM) tips under dry conditions, and the wear behavior is compared to that of single-crystal silicon with both thin and thick native...

Anisotropic Laminar Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

2006-01-01

The design, fabrication, and testing of a flexible, laminar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d33 piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d33 estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

Anisotropic Piezocomposite Actuator Incorporating Machined PMN-PT Single Crystal Fibers

NASA Technical Reports Server (NTRS)

Wilkie, W. Keats; Inman, Daniel J.; Lloyd, Justin M.; High, James W.

2004-01-01

The design, fabrication, and testing of a flexible, planar, anisotropic piezoelectric composite actuator utilizing machined PMN-32%PT single crystal fibers is presented. The device consists of a layer of rectangular single crystal piezoelectric fibers in an epoxy matrix, packaged between interdigitated electrode polyimide films. Quasistatic free-strain measurements of the single crystal device are compared with measurements from geometrically identical specimens incorporating polycrystalline PZT-5A and PZT-5H piezoceramic fibers. Free-strain actuation of the single crystal actuator at low bipolar electric fields (+/- 250 V/mm) is approximately 400% greater than that of the baseline PZT-5A piezoceramic device, and 200% greater than that of the PZT-5H device. Free-strain actuation under high unipolar electric fields (0-4kV/mm) is approximately 200% of the PZT-5A baseline device, and 150% of the PZT-5H alternate piezoceramic device. Performance increases at low field are qualitatively consistent with predicted increases based on scaling the low-field d(sub 33) piezoelectric constants of the respective piezoelectric materials. High-field increases are much less than scaled d(sub 33) estimates, but appear consistent with high-field freestrain measurements reported for similar bulk single-crystal and piezoceramic compositions. Measurements of single crystal actuator capacitance and coupling coefficient are also provided. These properties were poorly predicted using scaled bulk material dielectric and coupling coefficient data. Rules-of-mixtures calculations of the effective elastic properties of the single crystal device and estimated actuation work energy densities are also presented. Results indicate longitudinal stiffnesses significantly lower (50% less) than either piezoceramic device. This suggests that single-crystal piezocomposite actuators will be best suited to low induced-stress, high strain and deflection applications.

Three-Dimensional Conformation of Folded Polymers in Single Crystals

NASA Astrophysics Data System (ADS)

Hong, You-lee; Yuan, Shichen; Li, Zhen; Ke, Yutian; Nozaki, Koji; Miyoshi, Toshikazu

2015-10-01

The chain-folding mechanism and structure of semicrystalline polymers have long been controversial. Solid-state NMR was applied to determine the chain trajectory of 13C CH3 -labeled isotactic poly(1-butene) (i PB 1 ) in form III chiral single crystals blended with nonlabeled i PB 1 crystallized in dilute solutions under low supercooling. An advanced 13C - 13C double-quantum NMR technique probing the spatial proximity pattern of labeled 13C nuclei revealed that the chains adopt a three-dimensional (3D) conformation in single crystals. The determined results indicate a two-step crystallization process of (i) cluster formation via self-folding in the precrystallization stage and (ii) deposition of the nanoclusters as a building block at the growth front in single crystals.

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

DOE PAGES

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

2017-04-07

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

Left-right correlation in coupled F-center defects

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

Janesko, Benjamin G., E-mail: b.janesko@tcu.edu

This work explores how left-right correlation, a textbook problem in electronic structure theory, manifests in a textbook example of electrons trapped in crystal defects. I show that adjacent F-center defects in lithium fluoride display symptoms of “strong” left-right correlation, symptoms similar to those seen in stretched H{sub 2}. Simulations of UV/visible absorption spectra qualitatively fail to reproduce experiment unless left-right correlation is taken into account. This is of interest to both the electronic structure theory and crystal-defect communities. Theorists have a new well-behaved system to test their methods. Crystal-defect groups are cautioned that the approximations that successfully model single F-centersmore » may fail for adjacent F-centers.« less

Position sensitive detection of nuclear radiation mediated by non equilibrium phonons at low temperatures

NASA Astrophysics Data System (ADS)

Pröbst, F.; Peterreins, Th.; Feilitzsch, F. v.; Kraus, H.

1990-03-01

Many experiments in nuclear and particle physics would benefit from the development of a device capable of detecting non-ionizing events with a low energy threshold. In this context, we report on experimental tests of a detector based on the registration of nonequilibrium phonons. The device is composed of a silicon single crystal (size: 20×10×3 mm 3) and of an array of superconducting tunnel junctions evaporated onto the surface of the crystal. The junctions serve as sensors for phonons created by absorption of nuclear radiation in the crystal. We show how pulse height analysis and the investigation of time differences between correlated pulses in different junctions can be used to obtain information about the point of absorption.

Highly mobile type II twin boundary in Ni-Mn-Ga five-layered martensite

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

Sozinov, A.; Lanska, N.; Soroka, A.

2011-09-19

Twin relationships and stress-induced reorientation were studied in Ni{sub 2}Mn{sub 1.14}Ga{sub 0.86} single crystal with five-layered modulated martensite crystal structure. Very low twinning stress of about 0.1 MPa was found for twin boundaries which deviated a few degrees from the (011) crystallographic plane. However, twin boundaries oriented exactly parallel to the (011) plane exhibited considerably higher level of twinning stress, above 1 MPa. X-ray diffraction experiments and calculations based on approximation of the martensite crystal lattice as a tetragonal lattice with a slight monoclinic distortion identified the two different kinds of twin interfaces as type II and type I twinmore » boundaries.« less

Solution-processed, Self-organized Organic Single Crystal Arrays with Controlled Crystal Orientation

PubMed Central

Kumatani, Akichika; Liu, Chuan; Li, Yun; Darmawan, Peter; Takimiya, Kazuo; Minari, Takeo; Tsukagoshi, Kazuhito

2012-01-01

A facile solution process for the fabrication of organic single crystal semiconductor devices which meets the demand for low-cost and large-area fabrication of high performance electronic devices is demonstrated. In this paper, we develop a bottom-up method which enables direct formation of organic semiconductor single crystals at selected locations with desired orientations. Here oriented growth of one-dimensional organic crystals is achieved by using self-assembly of organic molecules as the driving force to align these crystals in patterned regions. Based upon the self-organized organic single crystals, we fabricate organic field effect transistor arrays which exhibit an average field-effect mobility of 1.1 cm2V−1s−1. This method can be carried out under ambient atmosphere at room temperature, thus particularly promising for production of future plastic electronics. PMID:22563523

Effect of Crystal Orientation on Analysis of Single-Crystal, Nickel-Based Turbine Blade Superalloys

NASA Technical Reports Server (NTRS)

Swanson, G. R.; Arakere, N. K.

2000-01-01

High-cycle fatigue-induced failures in turbine and turbopump blades is a pervasive problem. Single-crystal nickel turbine blades are used because of their superior creep, stress rupture, melt resistance, and thermomechanical fatigue capabilities. Single-crystal materials have highly orthotropic properties making the position of the crystal lattice relative to the part geometry a significant and complicating factor. A fatigue failure criterion based on the maximum shear stress amplitude on the 24 octahedral and 6 cube slip systems is presented for single-crystal nickel superalloys (FCC crystal). This criterion greatly reduces the scatter in uniaxial fatigue data for PWA 1493 at 1,200 F in air. Additionally, single-crystal turbine blades used in the Space Shuttle main engine high pressure fuel turbopump/alternate turbopump are modeled using a three-dimensional finite element (FE) model. This model accounts for material orthotrophy and crystal orientation. Fatigue life of the blade tip is computed using FE stress results and the failure criterion that was developed. Stress analysis results in the blade attachment region are also presented. Results demonstrate that control of crystallographic orientation has the potential to significantly increase a component's resistance to fatigue crack growth without adding additional weight or cost.

Structural, mechanical, electrical and optical properties of a new lithium boro phthalate NLO crystal synthesized by a slow evaporation method

NASA Astrophysics Data System (ADS)

Mohanraj, K.; Balasubramanian, D.; Jhansi, N.

2017-11-01

A new non-linear optical (NLO) single crystal of lithium boro phthalate (LiBP) was grown by slow solvent evaporation technique. The powder sample was subjected to powder X-ray diffraction (PXRD) to find its crystalline nature and the crystal structure of the grown crystal was determined using single crystal X-ray (SXRD) diffraction analysis. The Fourier Transform Infrared (FTIR) spectrum was recorded for grown crystal to identify the various functional groups present in the compound. The mechanical property of the LiBP single crystal was studied using Vickers microhardness tester. The dielectric constant and dielectric loss measurements were carried out for the grown crystal at various temperatures. The grown crystal was subjected to UV-Visible Spectral Studies to analyze the linear optical behavior of the grown crystal. The Kurtz-Perry Powder technique was employed to measure the Second Harmonic Generation efficiency of the grown crystal.

Synthesis, crystal structure, NLO and Hirshfeld surface analysis of 1,2,3-triazolyl chalcone single crystal

NASA Astrophysics Data System (ADS)

Shruthi, C.; Ravindrachary, V.; Guruswamy, B.; Lokanath, N. K.; Kumara, Karthik; Goveas, Janet

2018-05-01

Needle shaped brown coloured single crystal of the title compound was grown by slow evaporation technique using methanol as solvent. The grown crystal was characterized using FT-IR, Single crystal XRD, UV-visible and NLO studies. Crystal structure was confirmed by FT-IR study and the functional groups were identified. XRD study reveals that the crystal belongs to orthorhombic crystal system with pnaa space group and the corresponding cell parameters were calculated. UV-visible spectrum shows that the crystal is transparent in the entire visible region and absorption takes place in the UV-range. NLO efficiency of the crystal obtained 0.66 times that of urea was determined by SHG test. The intermolecular interaction and percentage contribution of each individual atom in the crystal lattice was quantized using Hirshfeld surface and 2D finger print analysis.

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.

Growth and characterization of hexamethylenetetramine crystals grown from solution

NASA Astrophysics Data System (ADS)

Babu, B.; Chandrasekaran, J.; Balaprabhakaran, S.

2014-06-01

Organic nonlinear optical single crystals of hexamethylenetetramine (HMT; 10 × 10 × 5 mm3) were prepared by crystallization from methanol solution. The grown crystals were subjected to various characterization techniques such as single crystal XRD, powder XRD, UV-Vis and electrical studies. Single crystal XRD analysis confirmed the crystalline structure of the grown crystals. Their crystalline nature was also confirmed by powder XRD technique. The optical transmittance property was identified from UV-Vis spectrum. Dielectric measurements were performed as a function of frequency at different temperatures. DC conductivity and photoconductivity studies were also carried out for the crystal. The powder second harmonic generation efficiency (SHG) of the crystal was measured using Nd:YAG laser and the efficiency was found to be two times greater than that of potassium dihydrogen phosphate (KDP).

Growth of propyl-p-hydroxybenzoate single crystals and its characterizations

NASA Astrophysics Data System (ADS)

Karunagaran, N.; Ramasamy, P.

2012-06-01

Single crystals of Propyl-p-hydroxybenzoate (PHB) crystals have been grown by slow evaporation solution technique (SEST) using methanol as a solvent. The PHB single crystal of dimension up to 27×16×8 mm3 has been grown in a period of 18 days at room temperature. The optical transparency of the grown PHB crystal has been measured on (212) plane by UV-Vis-NIR spectrophotometer. The crystal has 60% of transparency in the entire visible region. The thermo gravimetric analysis (TG) and differential thermal analysis (DTA) studies reveal that the crystal is thermally stable up to 99°C. The mechanical strength of the grown PHB crystal is measured using Vickers microhardness tester. The chemical etching studies were carried out on (212) plane using methanol etchant. The laser damage threshold of PHB crystal is 1.3 GW/cm2. The dielectric properties have been investigated. The birefringence value is found to be 0.10148 at the wavelength of 504 nm. The refractive index of grown PHB single crystal is 1.6753.

A STUDY OF DISLOCATION STRUCTURE OF SUBBOUNDARIES IN MOLYBDENUM SINGLE CRYSTALS,

DTIC Science & Technology

MOLYBDENUM, *DISLOCATIONS), GRAIN STRUCTURES(METALLURGY), SINGLE CRYSTALS, ZONE MELTING, ELECTRON BEAM MELTING, GRAIN BOUNDARIES, MATHEMATICAL ANALYSIS, ETCHED CRYSTALS, ETCHING, ELECTROEROSIVE MACHINING, CHINA

Growth of single crystals from solutions using semi-permeable membranes

NASA Astrophysics Data System (ADS)

Varkey, A. J.; Okeke, C. E.

1983-05-01

A technique suitable for growth of single crystals from solutions using semi-preamble membranes is described. Using this technique single crystals of copper sulphate, potassium bromide and ammonium dihydrogen phosphate have been successfully grown. Advantages of this technique over other methods are discussed.

Crystal growth and characterization of semi organic nonlinear optical (NLO) piperazinium tetrachlorozincate monohydrate (PTCZ) single crystal

NASA Astrophysics Data System (ADS)

Karuppasamy, P.; Pandian, Muthu Senthil; Ramasamy, P.

2018-04-01

The semi-organic single crystal of piperazinium tetrachlorozincate monohydrate (PTCZ) was successfully grown by slow evaporation solution technique (SEST). The grown crystal was subjected to the single crystal XRD studies for confirming the unit cell parameters. The optical quality of the grown crystal was identified by the UV-Vis NIR spectrum analysis and the optical band gap energy was calculated. The photoconductivity study reveals that the grown crystal has positive photoconductive nature. The mechanical stability of the grown crystal was analyzed using Vickers microhardness analyzer. The third-order nonlinear optical properties such as nonlinear refractive index (n2), absorption co-efficient (β) and susceptibility (χ(3)) were studied by Z-scan technique at 640 nm using solid state laser.

On the development of two characteristically different crystal morphology in SiO(2)-MgO-Al (2)O (3)-K (2)O-B (2)O (3)-F glass-ceramic system.

PubMed

Roy, Shibayan; Basu, Bikramjit

2009-01-01

The present work demonstrates how crystals with two different characteristic morphologies can be formed in SiO(2)-MgO-Al(2)O(3)-K(2)O-B(2)O(3)-F glass-ceramic system by adopting two sets of heat treatment experiments. In our study, single stage heat treatment experiments were performed at 1,000 degrees C for varying holding time of 8-24 h with 4 h time interval and as a function of temperature in the range of 1,000-1,120 degrees C with 40 degrees C temperature interval. The constant heating rate of 10 degrees C/min was employed for both sets of experiments. The microstructural changes were investigated using Fourier transformed infrared spectroscopy (FT-IR), SEM-EDS and XRD. For temperature variation batches, the microstructure is characterized by interlocked, randomly oriented mica plates ('house-of-cards' morphology). An important and new observation of complex crystal morphology is made in the samples heat treated at 1,000 degrees C for varying holding times. Such morphology appears to be the results of composite spherulitic-dendritic like growth of mica rods radiating from a central nucleus. The possible mechanism for such characteristic crystal growth morphology is discussed with reference to a nucleation-growth kinetics based model. The activation energy for crystal nucleation and Avrami index are computed to be 388 kJ/mol and 1.3 respectively, assuming Johnson-Mehl-Avrami model of crystallization. Another important result is that a maximum of around 70% of spherulitic-dendritic like crystal morphology can be obtained after heat treatment at 1,000 degrees C for 24 h, while a lower amount (approximately 58%) of interlocked plate like mica crystals is formed after heat treatment at 1,040 degrees C for 4 h.

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

Yin, Xingyu; Stony Brook University, NY 11794-5215; Nanjing University, Nanjing, Jiangsu

A method is presented for screening fragment libraries using acoustic droplet ejection to co-crystallize proteins and chemicals directly on micromeshes with as little as 2.5 nl of each component. This method was used to identify previously unreported fragments that bind to lysozyme, thermolysin, and trypsin. Acoustic droplet ejection (ADE) is a powerful technology that supports crystallographic applications such as growing, improving and manipulating protein crystals. A fragment-screening strategy is described that uses ADE to co-crystallize proteins with fragment libraries directly on MiTeGen MicroMeshes. Co-crystallization trials can be prepared rapidly and economically. The high speed of specimen preparation and the lowmore » consumption of fragment and protein allow the use of individual rather than pooled fragments. The Echo 550 liquid-handling instrument (Labcyte Inc., Sunnyvale, California, USA) generates droplets with accurate trajectories, which allows multiple co-crystallization experiments to be discretely positioned on a single data-collection micromesh. This accuracy also allows all components to be transferred through small apertures. Consequently, the crystallization tray is in equilibrium with the reservoir before, during and after the transfer of protein, precipitant and fragment to the micromesh on which crystallization will occur. This strict control of the specimen environment means that the crystallography experiments remain identical as the working volumes are decreased from the few microlitres level to the few nanolitres level. Using this system, lysozyme, thermolysin, trypsin and stachydrine demethylase crystals were co-crystallized with a small 33-compound mini-library to search for fragment hits. This technology pushes towards a much faster, more automated and more flexible strategy for structure-based drug discovery using as little as 2.5 nl of each major component.« less

The effect of protein–precipitant interfaces and applied shear on the nucleation and growth of lysozyme crystals

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

Reis, Nuno M.; Chirgadze, Dimitri Y.; Blundell, Tom L.

The nucleation of lysozyme in microbatch experiments was linked to the formation of protein–precipitant interfaces. The use of oscillatory shear allowed decreasing the nucleation rate and extending the growth period for lysozyme crystals, presumably through the control of the number of interfaces and removal of impurities or defects. This paper is concerned with the effect of protein–precipitant interfaces and externally applied shear on the nucleation and growth kinetics of hen egg-white lysozyme crystals. The early stages of microbatch crystallization of lysozyme were explored using both optical and confocal fluorescence microscopy imaging. Initially, an antisolvent (precipitant) was added to a proteinmore » drop and the optical development of the protein–precipitant interface was followed with time. In the presence of the water-soluble polymer poly(ethylene glycol) (PEG) a sharp interface was observed to form immediately within the drop, giving an initial clear separation between the lighter protein solution and the heavier precipitant. This interface subsequently became unstable and quickly developed within a few seconds into several unstable ‘fingers’ that represented regions of high concentration-gradient interfaces. Confocal microscopy demonstrated that the subsequent nucleation of protein crystals occurred preferentially in the region of these interfaces. Additional experiments using an optical shearing system demonstrated that oscillatory shear significantly decreased nucleation rates whilst extending the growth period of the lysozyme crystals. The experimental observations relating to both nucleation and growth have relevance in developing efficient and reliable protocols for general crystallization procedures and the controlled crystallization of single large high-quality protein crystals for use in X-ray crystallography.« less

Effects of Ca/Sr ratio control on optical and scintillation properties of Eu-doped Li(Ca,Sr)AlF6 single crystals

NASA Astrophysics Data System (ADS)

Yokota, Yuui; Tanaka, Chieko; Kurosawa, Shunsuke; Yamaji, Akihiro; Ohashi, Yuji; Kamada, Kei; Nikl, Martin; Yoshikawa, Akira

2018-05-01

Eu-doped Li(Ca,Sr)AlF6 [Eu:LiCSAF] single crystals with various Ca/Sr ratios were grown by the micro-pulling-down method, and their optical and scintillation properties were investigated to reveal the effects of Ca/Sr ratio on optical and scintillation properties of the Eu:LiCSAF single crystals. The Li(Ca1-x-ySrxEuy)AlF6 single crystals could be grown in 0 ≤ x ≤ 0.1, 0.5 ≤ x ≤ 1.0 and y = 0.02 while the Eu:LiCSAF crystals with x = 0.2, 0.25 and 0.4 included two colquiriite-type phases with different lattice parameters. The Li(Ca1-x-ySrxEuy)AlF6 single crystal with x = 0.25 and y = 0.02 showed the highest light yield under neutron irradiation.

Ag-ligand modified tungstovandates and their efficient catalysis degradation properties for methylene blue

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

Zheng, Ran; Zhang, Huixia; Liu, Yunping

Two polytungstovandates [Ag(mbpy){sub 2}][Ag{sub 2}(mbpy){sub 3}][VW{sub 5}O{sub 19}]·H{sub 2}O (1) and [Ag(mbpy)]{sub 2}[Ag(mbpy){sub 2}]{sub 4}[VW{sub 12}O{sub 40}] (2) (mbpy =4,4′-dimethyl-2,2′-bipyridyl), had been hydrothermally synthesized and characterized by IR, TG, and single-crystal X-ray diffraction techniques. Single-crystal structural analysis revealed that the polyanionic clusters in two compounds are different: Lindqvist-type in 1 and α-Keggin-type in 2, respectively, while the cationic moieties in them are Ag-mbpy units. The experiments showed that this kind of hybrid crystal materials possesses more efficiently catalytic performance for the degradation of organic dye methylene blue (MB) in water solution under the UV irradiation. The significant degradation rate ofmore » MB can reach 89.9%, 94.9% by crystals 1 and 2 (40 mg) in the course of about 5 min. - Graphical abstract: Two Ag-ligand modified polytungstovandates had been synthesized and characterized, which were active in the catalytic degradation of organic dye methylene blue under the UV irradiation. - Highlights: • Two Ag-ligand modified tungstovandates were synthesized and characterized. • Weak interactions play important roles in constructing crystal frameworks. • Compounds are active to catalyze the degradation of methylene blue.« less

Highly reproducible alkali metal doping system for organic crystals through enhanced diffusion of alkali metal by secondary thermal activation.

PubMed

Lee, Jinho; Park, Chibeom; Song, Intek; Koo, Jin Young; Yoon, Taekyung; Kim, Jun Sung; Choi, Hee Cheul

2018-05-16

In this paper, we report an efficient alkali metal doping system for organic single crystals. Our system employs an enhanced diffusion method for the introduction of alkali metal into organic single crystals by controlling the sample temperature to induce secondary thermal activation. Using this system, we achieved intercalation of potassium into picene single crystals with closed packed crystal structures. Using optical microscopy and Raman spectroscopy, we confirmed that the resulting samples were uniformly doped and became K 2 picene single crystal, while only parts of the crystal are doped and transformed into K 2 picene without secondary thermal activation. Moreover, using a customized electrical measurement system, the insulator-to-semiconductor transition of picene single crystals upon doping was confirmed by in situ electrical conductivity and ex situ temperature-dependent resistivity measurements. X-ray diffraction studies showed that potassium atoms were intercalated between molecular layers of picene, and doped samples did not show any KH- nor KOH-related peaks, indicating that picene molecules are retained without structural decomposition. During recent decades, tremendous efforts have been exerted to develop high-performance organic semiconductors and superconductors, whereas as little attention has been devoted to doped organic crystals. Our method will enable efficient alkali metal doping of organic crystals and will be a resource for future systematic studies on the electrical property changes of these organic crystals upon doping.

Fe-Al alloy single-crystal thin film preparation for basic magnetic measurements

NASA Astrophysics Data System (ADS)

Abe, Tatsuya; Kawai, Tetsuroh; Futamoto, Masaaki; Ohtake, Mitsuru; Inaba, Nobuyuki

2018-04-01

Fe100-xAlx (x = 0, 4, 10, 20, 30 at. %) alloy films of 40 nm thickness are prepared on MgO(001) single-crystal substrates by varying substrate temperature from room temperature to 600 °C. Single-crystal films of (001) orientation with bcc-based disordered A2 structure are obtained for the Al content range of x = 0 - 20 at. %. An ordered phase of DO3 structure is observed in Fe70Al30 films prepared at temperatures higher than 200 °C, whereas (001) oriented single-crystal films of A2 structure are obtained when prepared at room temperature. The film surface profile does not depend much on the film composition, while the surface roughness increases with increasing substrate temperature. Island-like crystals are observed for films prepared at 600°C for all compositions. Difference in lattice spacing measured parallel and perpendicular to the substrate is noted for the single-crystal thin films and it increases with increasing Al content. The lattice strain in single-crystal film is caused possibly to accommodate the lattice mismatch with the MgO substrate. The (001)-oriented single-crystal films with A2 structure show four-fold symmetries in in-plane magnetic anisotropy with the easy magnetization axis A2[100] and the hard magnetization axis A2[110], whereas the films with DO3 ordered structure show almost isotropic magnetic properties.

The origin of transverse anisotropy in axially symmetric single molecule magnets.

PubMed

Barra, Anne-Laure; Caneschi, Andrea; Cornia, Andrea; Gatteschi, Dante; Gorini, Lapo; Heiniger, Leo-Philipp; Sessoli, Roberta; Sorace, Lorenzo

2007-09-05

Single-crystal high-frequency electron paramagnetic resonance spectroscopy has been employed on a truly axial single molecule magnet of formula [Mn(12)O(12)(tBu-CH(2)CO(2))16(CH(3)OH)4].CH(3)OH to investigate the origin of the transverse magnetic anisotropy, a crucial parameter that rules the quantum tunneling of the magnetization. The crystal structure, including the absolute structure of the crystal used for EPR experiments, has been fully determined and found to belong to I4 tetragonal space group. The angular dependence of the resonance fields in the crystallographic ab plane shows the presence of high-order tetragonal anisotropy and strong dependence on the MS sublevels with the second-highest-field transition being angular independent. This was rationalized including competing fourth- and sixth-order transverse parameters in a giant spin Hamiltonian which describes the magnetic anisotropy in the ground S = 10 spin state of the cluster. To establish the origin of these anisotropy terms, the experimental results have been further analyzed using a simplified multispin Hamiltonian which takes into account the exchange interactions and the single ion magnetic anisotropy of the Mn(III) centers. It has been possible to establish magnetostructural correlations with spin Hamiltonian parameters up to the sixth order. Transverse anisotropy in axial single molecule magnets was found to originate from the multispin nature of the system and from the breakdown of the strong exchange approximation. The tilting of the single-ion easy axes of magnetization with respect to the 4-fold molecular axis of the cluster plays the major role in determining the transverse anisotropy. Counterintuitively, the projections of the single ion easy axes on the ab plane correspond to hard axes of magnetization.

High field electron paramagnetic resonance spectroscopy under ultrahigh vacuum conditions—A multipurpose machine to study paramagnetic species on well defined single crystal surfaces

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

Rocker, J.; Cornu, D.; Kieseritzky, E.

2014-08-01

A new ultrahigh vacuum (UHV) electron paramagnetic resonance (EPR) spectrometer operating at 94 GHz to investigate paramagnetic centers on single crystal surfaces is described. It is particularly designed to study paramagnetic centers on well-defined model catalysts using epitaxial thin oxide films grown on metal single crystals. The EPR setup is based on a commercial Bruker E600 spectrometer, which is adapted to ultrahigh vacuum conditions using a home made Fabry Perot resonator. The key idea of the resonator is to use the planar metal single crystal required to grow the single crystalline oxide films as one of the mirrors of themore » resonator. EPR spectroscopy is solely sensitive to paramagnetic species, which are typically minority species in such a system. Hence, additional experimental characterization tools are required to allow for a comprehensive investigation of the surface. The apparatus includes a preparation chamber hosting equipment, which is required to prepare supported model catalysts. In addition, surface characterization tools such as low energy electron diffraction (LEED)/Auger spectroscopy, temperature programmed desorption (TPD), and infrared reflection absorption spectroscopy (IRAS) are available to characterize the surfaces. A second chamber used to perform EPR spectroscopy at 94 GHz has a room temperature scanning tunneling microscope attached to it, which allows for real space structural characterization. The heart of the UHV adaptation of the EPR experiment is the sealing of the Fabry-Perot resonator against atmosphere. To this end it is possible to use a thin sapphire window glued to the backside of the coupling orifice of the Fabry Perot resonator. With the help of a variety of stabilization measures reducing vibrations as well as thermal drift it is possible to accumulate data for a time span, which is for low temperature measurements only limited by the amount of liquid helium. Test measurements show that the system can detect paramagnetic species with a density of approximately 5 × 10{sup 11} spins/cm{sup 2}, which is comparable to the limit obtained for the presently available UHV-EPR spectrometer operating at 10 GHz (X-band). Investigation of electron trapped centers in MgO(001) films shows that the increased resolution offered by the experiments at W-band allows to identify new paramagnetic species, that cannot be differentiated with the currently available methodology.« less

Spatiotemporal dynamics of the spin transition in [Fe (HB(tz)3) 2] single crystals

NASA Astrophysics Data System (ADS)

Ridier, Karl; Rat, Sylvain; Shepherd, Helena J.; Salmon, Lionel; Nicolazzi, William; Molnár, Gábor; Bousseksou, Azzedine

2017-10-01

The spatiotemporal dynamics of the spin transition have been thoroughly investigated in single crystals of the mononuclear spin-crossover (SCO) complex [Fe (HB (tz )3)2] (tz = 1 ,2 ,4-triazol-1-yl) by optical microscopy. This compound exhibits an abrupt spin transition centered at 334 K with a narrow thermal hysteresis loop of ˜1 K (first-order transition). Most single crystals of this compound reveal exceptional resilience upon repeated switching (several hundred cycles), which allowed repeatable and quantitative measurements of the spatiotemporal dynamics of the nucleation and growth processes to be carried out. These experiments revealed remarkable properties of the thermally induced spin transition: high stability of the thermal hysteresis loop, unprecedented large velocities of the macroscopic low-spin/high-spin phase boundaries up to 500 µm/s, and no visible dependency on the temperature scan rate. We have also studied the dynamics of the low-spin → high-spin transition induced by a local photothermal excitation generated by a spatially localized (Ø = 2 μ m ) continuous laser beam. Interesting phenomena have been evidenced both in quasistatic and dynamic conditions (e.g., threshold effects and long incubation periods, thermal activation of the phase boundary propagation, stabilization of the crystal in a stationary biphasic state, and thermal cutoff frequency). These measurements demonstrated the importance of thermal effects in the transition dynamics, and they enabled an accurate determination of the thermal properties of the SCO compound in the framework of a simple theoretical model.

Thermal Mechanical Stability of Single-Crystal-Oxide Refractive Concentrators Evaluated for High-Temperature Solar-Thermal Propulsion

NASA Technical Reports Server (NTRS)

Jacobson, Nathan S.; Jacobson, Nathan S.; Miller, Robert A.

1999-01-01

Recently, refractive secondary solar concentrator systems were developed for solar thermal power and propulsion (ref. 1). Single-crystal oxides-such as yttria-stabilized zirconia (Y2O3-ZrO2), yttrium aluminum garnet (Y3Al5O12, or YAG), magnesium oxide (MgO), and sapphire (Al2O3)-are candidate refractive secondary concentrator materials. However, the refractive concentrator system will experience high-temperature thermal cycling in the solar thermal engine during the sun/shade transition of a space mission. The thermal mechanical reliability of these components in severe thermal environments is of great concern. Simulated mission tests are important for evaluating these candidate oxide materials under a variety of transient and steady-state heat flux conditions. In this research at the NASA Lewis Research Center, a controlled heat flux test approach was developed for investigating the thermal mechanical stability of the candidate oxide. This approach used a 3.0-kW continuous-wave (wavelength, 10.6 mm) carbon dioxide (CO2) laser (ref. 2). The CO2 laser is especially well-suited for single-crystal thermal shock tests because it can directly deliver well-characterized heat energy to the oxide surfaces. Since the oxides are opaque at the 10.6-mm wavelength of the laser beam, the light energy is absorbed at the surfaces rather than transmitting into the crystals, and thus generates the required temperature gradients within the specimens. The following figure is a schematic diagram of the test rig.

Temperature dependence of single-crystal elastic constants of flux-grown alpha-GaPO(4).

PubMed

Armand, P; Beaurain, M; Rufflé, B; Menaert, B; Papet, P

2009-06-01

The lattice parameter change with respect to temperature (T) has been measured using high-temperature powder X-ray diffraction techniques for high-temperature flux-grown GaPO(4) single crystals with the alpha-quartz structure. The lattice and the volume linear thermal expansion coefficients in the temperature range 303-1173 K were computed from the X-ray data. The percentage linear thermal expansions along the a and c axes at 1173 K are 1.5 and 0.51, respectively. The temperature dependence of the mass density rho of flux-grown GaPO(4) single crystals was evaluated using the volume thermal expansion coefficient alpha(V)(T) = 3.291 x 10(-5) - 2.786 x 10(-8) [T] + 4.598 x 10(-11)[T](2). Single-crystal high-resolution Brillouin spectroscopy measurements have been carried out at ambient pressure from 303 to 1123 K to determine the elastic constants C(IJ) of high-temperature flux-grown GaPO(4) material. The single-crystal elastic moduli were calculated using the sound velocities via the measured Brillouin frequency shifts Deltanu(B). These are, to our knowledge, the highest temperatures at which single-crystal elastic constants of alpha-GaPO(4) have been measured. Most of the room-temperature elastic constant values measured on flux-grown GaPO(4) material are higher than the ones found for hydrothermally grown GaPO(4) single crystals. The fourth-order temperature coefficients of both the Brillouin frequency shifts T(nuB)((n)) and the single-crystal elastic moduli T(C(IJ))((n)) were obtained. The first-order temperature coefficients of the C(IJ) are in excellent agreement with previous reports on low-temperature hydrothermally grown alpha-GaPO(4) single crystals, while small discrepancies in the higher-order temperature coefficients are observed. This is explained in terms of the OH content in the GaPO(4) network, which is an important parameter in the crystal thermal behavior.

Structure and Growth Control of Organic–Inorganic Halide Perovskites for Optoelectronics: From Polycrystalline Films to Single Crystals

PubMed Central

Chen, Yani; He, Minhong; Peng, Jiajun; Sun, Yong

2016-01-01

Recently, organic–inorganic halide perovskites have sparked tremendous research interest because of their ground‐breaking photovoltaic performance. The crystallization process and crystal shape of perovskites have striking impacts on their optoelectronic properties. Polycrystalline films and single crystals are two main forms of perovskites. Currently, perovskite thin films have been under intensive investigation while studies of perovskite single crystals are just in their infancy. This review article is concentrated upon the control of perovskite structures and growth, which are intimately correlated for improvements of not only solar cells but also light‐emitting diodes, lasers, and photodetectors. We begin with the survey of the film formation process of perovskites including deposition methods and morphological optimization avenues. Strategies such as the use of additives, thermal annealing, solvent annealing, atmospheric control, and solvent engineering have been successfully employed to yield high‐quality perovskite films. Next, we turn to summarize the shape evolution of perovskites single crystals from three‐dimensional large sized single crystals, two‐dimensional nanoplates, one‐dimensional nanowires, to zero‐dimensional quantum dots. Siginificant functions of perovskites single crystals are highlighted, which benefit fundamental studies of intrinsic photophysics. Then, the growth mechanisms of the previously mentioned perovskite crystals are unveiled. Lastly, perspectives for structure and growth control of perovskites are outlined towards high‐performance (opto)electronic devices. PMID:27812463

A Quick Method for Determining the Density of Single Crystals.

ERIC Educational Resources Information Center

Roman, Pascual; Gutierrez-Zorrilla, Juan M.

1985-01-01

Shows how the Archimedes method is used to determine the density of a single crystal of ammonium oxalate monohydrate. Also shows how to calculate the density of other chemicals when they are available as single crystals. Experimental procedures and materials needed are included. (JN)

Crystal growth, structural, optical, mechanical and thermal properties of a new nonlinear optical single crystal: L-Ornithine monohydrochloride.

PubMed

Balakrishnan, T; Ramamurthi, K

2009-03-01

Amino acid family crystals exhibit excellent nonlinear optical and electro optical properties. l-Ornithine monohydrochloride single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystals were characterized by single crystal and powder X-ray diffraction analysis, Fourier transform infrared (FTIR) spectroscopy, TGA, DTA and DSC analyses. UV-vis-NIR spectrum shows excellent transmission in the UV, visible and NIR region (300-1600nm). The mechanical properties of grown crystals were studied using Vickers microhardness tester. Its second harmonic generation efficiency was tested using Nd:YAG laser and is 1.25 times that of KDP.

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

High-pressure crystal structures of an insensitive energetic crystal: 1,1-diamino-2,2-dinitroethene

DOE PAGES

Dreger, Zbigniew A.; Stash, Adam I.; Yu, Zhi -Gang; ...

2015-12-03

Understanding the insensitivity/stability of insensitive high explosive crystals requires detailed structural information at high pressures and high temperatures of interest. Synchrotron single crystal x-ray diffraction experiments were used to determine the high-pressure structures of 1,1-diamino-2,2-dinitroethene (FOX-7), a prototypical insensitive high explosive. The phase transition around 4.5 GPa was investigated and the structures were determined at 4.27 GPa (α’-phase) and 5.9 GPa (ε-phase). The α’-phase (monoclinic, P2 1/ n), structurally indistinguishable from the ambient α-phase, transforms to the new ε-phase (triclinic, P1). The most notable features of the ε-phase, compared to the α’-phase, are: formation of planar layers and flattening ofmore » molecules. Density functional theory (DFT-D2) calculations complemented the experimental results. Furthermore, the results presented here are important for understanding the molecular and crystalline attributes governing the high-pressure insensitivity/stability of insensitive high explosive crystals.« less

High-pressure crystal structures of an insensitive energetic crystal: 1,1-diamino-2,2-dinitroethene

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

Dreger, Zbigniew A.; Stash, Adam I.; Yu, Zhi -Gang

Understanding the insensitivity/stability of insensitive high explosive crystals requires detailed structural information at high pressures and high temperatures of interest. Synchrotron single crystal x-ray diffraction experiments were used to determine the high-pressure structures of 1,1-diamino-2,2-dinitroethene (FOX-7), a prototypical insensitive high explosive. The phase transition around 4.5 GPa was investigated and the structures were determined at 4.27 GPa (α’-phase) and 5.9 GPa (ε-phase). The α’-phase (monoclinic, P2 1/ n), structurally indistinguishable from the ambient α-phase, transforms to the new ε-phase (triclinic, P1). The most notable features of the ε-phase, compared to the α’-phase, are: formation of planar layers and flattening ofmore » molecules. Density functional theory (DFT-D2) calculations complemented the experimental results. Furthermore, the results presented here are important for understanding the molecular and crystalline attributes governing the high-pressure insensitivity/stability of insensitive high explosive crystals.« less

Nonuniform carrier density in Cd 3 As 2 evidenced by optical spectroscopy

DOE PAGES

Crassee, I.; Martino, E.; Homes, C. C.; ...

2018-03-22

In this paper, we report the detailed optical properties of Cd 3As 2 crystals in a wide parameter space: temperature, magnetic field, carrier concentration, and crystal orientation. We investigate high-quality crystals synthesized by three different techniques. In all the studied samples, independently of how they were prepared and how they were treated before the optical experiments, our data indicate conspicuous fluctuations in the carrier density (up to 30%). These charge puddles have a characteristic scale of 100 μm, they become more pronounced at low temperatures, and possibly, they become enhanced by the presence of crystal twinning. The Drude response ismore » characterized by very small scattering rates (~1 meV) for as-grown samples. Mechanical treatment, such as cutting or polishing, influences the optical properties of single crystals, by increasing the Drude scattering rate and also modifying the high-frequency optical response. Finally, magnetoreflectivity and Kerr rotation are consistent with electronlike charge carriers and a spatially nonuniform carrier density.« less

Nonuniform carrier density in Cd3As2 evidenced by optical spectroscopy

NASA Astrophysics Data System (ADS)

Crassee, I.; Martino, E.; Homes, C. C.; Caha, O.; Novák, J.; Tückmantel, P.; Hakl, M.; Nateprov, A.; Arushanov, E.; Gibson, Q. D.; Cava, R. J.; Koohpayeh, S. M.; Arpino, K. E.; McQueen, T. M.; Orlita, M.; Akrap, Ana

2018-03-01

We report the detailed optical properties of Cd3As2 crystals in a wide parameter space: temperature, magnetic field, carrier concentration, and crystal orientation. We investigate high-quality crystals synthesized by three different techniques. In all the studied samples, independently of how they were prepared and how they were treated before the optical experiments, our data indicate conspicuous fluctuations in the carrier density (up to 30%). These charge puddles have a characteristic scale of 100 μ m , they become more pronounced at low temperatures, and possibly, they become enhanced by the presence of crystal twinning. The Drude response is characterized by very small scattering rates (˜1 meV) for as-grown samples. Mechanical treatment, such as cutting or polishing, influences the optical properties of single crystals, by increasing the Drude scattering rate and also modifying the high-frequency optical response. Magnetoreflectivity and Kerr rotation are consistent with electronlike charge carriers and a spatially nonuniform carrier density.

Nonuniform carrier density in Cd 3 As 2 evidenced by optical spectroscopy

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

Crassee, I.; Martino, E.; Homes, C. C.

In this paper, we report the detailed optical properties of Cd 3As 2 crystals in a wide parameter space: temperature, magnetic field, carrier concentration, and crystal orientation. We investigate high-quality crystals synthesized by three different techniques. In all the studied samples, independently of how they were prepared and how they were treated before the optical experiments, our data indicate conspicuous fluctuations in the carrier density (up to 30%). These charge puddles have a characteristic scale of 100 μm, they become more pronounced at low temperatures, and possibly, they become enhanced by the presence of crystal twinning. The Drude response ismore » characterized by very small scattering rates (~1 meV) for as-grown samples. Mechanical treatment, such as cutting or polishing, influences the optical properties of single crystals, by increasing the Drude scattering rate and also modifying the high-frequency optical response. Finally, magnetoreflectivity and Kerr rotation are consistent with electronlike charge carriers and a spatially nonuniform carrier density.« less

Single-frequency Nd:YAG ring lasers with corner cube prism

NASA Astrophysics Data System (ADS)

Wu, Ke Ying; Yang, Su Hui; Zhao, Chang Ming; Wei, Guang Hui

2000-04-01

Kane and Byer reported the first monolithic non-planar miniature ring lasers in 1985. An intrinsic optical diode enforces unidirectional and hence single-frequency oscillation of this device. It has the advantages of compactness, reliability and high efficiency. We put forward another form of the non-planar ring lasers, in which the corner cube prism is the key element and the Nd:YAG crystal is used as a Porro prism to enclose the ring resonator. The phase shift due to the total internal reflections of the three differently orientated reflection planes of the corner cube prism, Faraday rotation in the Nd:YAG crystal placed in a magnetic field and the different output coupling in S and P polarization form an optical diode and enforce the single- frequency generating. A round trip analysis of the polarization properties of the resonator is made by the evaluation of Jones matrix. The results of our initial experiment are given in the paper.

Magnetic and Structural Characterization of Fe-Ga Using Kerr Microscopy and Neutron Scattering

DTIC Science & Technology

2010-01-01

117 4.6 Schematic of triple axes single crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right...Therefore, USANS data is one-dimensional. 4.3.3 Single Crystal Neutron Diffraction The single crystal neutron diffractometer, TriCS at Paul Scherrer...crystal neutron diffractometer (left). TriCS intrument at Paul Scherrer Institut, Switzerland (right) [106] 4.4 Unpolarized SANS In this section, SANS

A possibility of parallel and anti-parallel diffraction measurements on neu- tron diffractometer employing bent perfect crystal monochromator at the monochromatic focusing condition

NASA Astrophysics Data System (ADS)

Choi, Yong Nam; Kim, Shin Ae; Kim, Sung Kyu; Kim, Sung Baek; Lee, Chang-Hee; Mikula, Pavel

2004-07-01

In a conventional diffractometer having single monochromator, only one position, parallel position, is used for the diffraction experiment (i.e. detection) because the resolution property of the other one, anti-parallel position, is very poor. However, a bent perfect crystal (BPC) monochromator at monochromatic focusing condition can provide a quite flat and equal resolution property at both parallel and anti-parallel positions and thus one can have a chance to use both sides for the diffraction experiment. From the data of the FWHM and the Delta d/d measured on three diffraction geometries (symmetric, asymmetric compression and asymmetric expansion), we can conclude that the simultaneous diffraction measurement in both parallel and anti-parallel positions can be achieved.

High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization

NASA Astrophysics Data System (ADS)

Saidaminov, Makhsud I.; Abdelhady, Ahmed L.; Murali, Banavoth; Alarousu, Erkki; Burlakov, Victor M.; Peng, Wei; Dursun, Ibrahim; Wang, Lingfei; He, Yao; Maculan, Giacomo; Goriely, Alain; Wu, Tom; Mohammed, Omar F.; Bakr, Osman M.

2015-07-01

Single crystals of methylammonium lead trihalide perovskites (MAPbX3; MA=CH3NH3+, X=Br- or I-) have shown remarkably low trap density and charge transport properties; however, growth of such high-quality semiconductors is a time-consuming process. Here we present a rapid crystal growth process to obtain MAPbX3 single crystals, an order of magnitude faster than previous reports. The process is based on our observation of the substantial decrease of MAPbX3 solubility, in certain solvents, at elevated temperatures. The crystals can be both size- and shape-controlled by manipulating the different crystallization parameters. Despite the rapidity of the method, the grown crystals exhibit transport properties and trap densities comparable to the highest quality MAPbX3 reported to date. The phenomenon of inverse or retrograde solubility and its correlated inverse temperature crystallization strategy present a major step forward for advancing the field on perovskite crystallization.

Growth of PBI 2 single crystals from stoichiometric and Pb excess melts

NASA Astrophysics Data System (ADS)

Hayashi, T.; Kinpara, M.; Wang, J. F.; Mimura, K.; Isshiki, M.

2008-01-01

We have successfully grown high-purity and -quality PbI 2 single crystals by the vertical Bridgman method. The rocking curves of four-crystal X-ray diffraction (XRD) show 120 arcsec in full-width at half-maximum (FWHM). The photoluminescence (PL) spectra at 7.8 K show the resolved intensive exciton emission line and the weak DAP emission band. The deep-level emissions are not observed. The measurement of the electrical and radiographic properties show that Leadiodide (PbI 2) single crystal has a resistivity of 5×10 10 Ω cm and imager lag is 8 s, respectively. In order to improve the controllability of crystal growth, PbI 2 single crystals were also grown from a lead (Pb) excess PbI 2 source. The experimental results show very good reproducibility. In addition, the growth models of crystal are proposed, and the growth mechanism is discussed.

Solid state parameters, structure elucidation, High Resolution X-Ray Diffraction (HRXRD), phase matching, thermal and impedance analysis on L-Proline trichloroacetate (L-PTCA) NLO single crystals.

PubMed

Kalaiselvi, P; Raj, S Alfred Cecil; Jagannathan, K; Vijayan, N; Bhagavannarayana, G; Kalainathan, S

2014-11-11

Nonlinear optical single crystal of L-Proline trichloroacetate (L-PTCA) was successfully grown by Slow Evaporation Solution Technique (SEST). The grown crystals were subjected to single crystal X-ray diffraction analysis to confirm the structure. From the single crystal XRD data, solid state parameters were determined for the grown crystal. The crystalline perfection has been evaluated using high resolution X-ray diffractometer. The frequencies of various functional groups were identified from FTIR spectral analysis. The percentage of transmittance was obtained from UV Visible spectral analysis. TGA-DSC measurements indicate the thermal stability of the crystal. The dielectric constant, dielectric loss and ac conductivity were measured by the impedance analyzer. The DC conductivity was calculated by the cole-cole plot method. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Ben Yahia, Hamdi, E-mail: benyahia.hamdi@voila.fr; Rodewald, Ute Ch.; Boulahya, Khalid

Graphical abstract: The new compounds RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) were synthesised by solid state reaction via a salt flux route and investigated by HRTEM, SAED, and single crystal X-ray diffraction. - Highlights: • We discovered the series of RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) compounds. • The RE{sub 4}O{sub 4}[AsO{sub 4}]Cl single crystals were grown using NaCl/KCl flux. • The RE{sub 4}O{sub 4}[AsO{sub 4}]Cl structures were solved using single crystal X-ray diffraction data. • The layered RE{sub 4}O{sub 4}[AsO{sub 4}]Cl compounds were further characterized using HRTEMmore » and SAED. • We observed an alternation of ordered-[RE{sub 4}O{sub 4}]{sup 4+} and disordered-[ClAsO{sub 4}]{sup 4–} layers. - Abstract: The new compounds RE{sub 4}O{sub 4}[AsO{sub 4}]Cl (RE = La, Pr, Nd, Sm, Eu, Gd) were synthesised by solid state reaction via a salt flux route and investigated by HRTEM, SAED, and single crystal X-ray diffraction. The samples crystallise with a tetragonal cell, space group P4{sub 2}/mnm and Z = 2. Their crystal structure consists of an alternation of [RE{sub 4}O{sub 4}]{sup 4+} and [ClAsO{sub 4}]{sup 4–} layers. The [RE{sub 4}O{sub 4}]{sup 4+} layer contains ORE{sub 4/4} tetrahedra which share common edges. The anions AsO{sub 4}{sup 3–} and Cl{sup –} are located between these layers in disordered manner. SAED and HRTEM experiments confirmed this structural model and enabled us to propose an ordered model for the [ClAsO{sub 4}]{sup 4–} layers.« less

Continuum Excitation and Pseudospin Wave in Quantum Spin-Liquid and Quadrupole Ordered States of Tb2+xTi2-xO7+y

NASA Astrophysics Data System (ADS)

Kadowaki, Hiroaki; Wakita, Mika; Fåk, Björn; Ollivier, Jacques; Ohira-Kawamura, Seiko; Nakajima, Kenji; Takatsu, Hiroshi; Tamai, Mototake

2018-06-01

The ground states of the frustrated pyrochlore oxide Tb2+xTi2-xO7+y have been studied by inelastic neutron scattering experiments. Three single-crystal samples are investigated; one shows no phase transition (x = -0.007 < xc ˜ -0.0025), being a putative quantum spin-liquid (QSL), and the other two (x = 0.000,0.003) show electric quadrupole ordering (QO) below Tc ˜ 0.5 K. The QSL sample shows continuum excitation spectra with an energy scale 0.1 meV as well as energy-resolution-limited (nominally) elastic scattering. As x is increased, pseudospin wave of the QO state emerges from this continuum excitation, which agrees with that of powder samples and consequently verifies good x control for the present single crystal samples.

Interplay of magnetism and superconductivity in EuFe2(As1-xPx)2 single crystals probed by muon spin rotation and 57Fe Mössbauer spectroscopy

NASA Astrophysics Data System (ADS)

Goltz, T.; Kamusella, S.; Jeevan, H. S.; Gegenwart, P.; Luetkens, H.; Materne, P.; Spehling, J.; Sarkar, R.; Klauss, H.-H.

2014-12-01

We present our results of a local probe study on EuFe2(As1-xPx)2 single crystals with x=0.13, 0.19 and 0.28 by means of muon spin rotation and 57Fe Mössbauer spectroscopy. We focus our discussion on the sample with x=0.19 viz. at the optimal substitution level, where bulk superconductivity (TSC = 28 K) sets in above static europium order (TEu = 20 K) but well below the onset of the iron antiferromagnetic (AFM) transition (~100 K). We find enhanced spin dynamics in the Fe sublattice closely above TSC and propose that these are related to enhanced Eu fluctuations due to the evident coupling of both sublattices observed in our experiments.

Friction and wear behavior of single-crystal silicon carbide in sliding contact with various metals

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1978-01-01

Sliding friction experiments were conducted with single-crystal silicon carbide in contact with various metals. Results indicate the coefficient of friction is related to the relative chemical activity of the metals. The more active the metal, the higher the coefficient of friction. All the metals examined transferred to silicon carbide. The chemical activity of the metal and its shear modulus may play important roles in metal transfer, the form of the wear debris and the surface roughness of the metal wear scar. The more active the metal, and the less resistance to shear, the greater the transfer to silicon carbide and the rougher the wear scar on the surface of the metal. Hexagon shaped cracking and fracturing formed by cleavage of both prismatic and basal planes is observed on the silicon carbide surface.

Electronic structure of single crystalline Bi 2(Sr,Ca,La) 3Cu 2O 8

NASA Astrophysics Data System (ADS)

Lindberg, P. A. P.; Shen, Z.-X.; Dessau, D. S.; Wells, B. O.; Borg, A.; Mitzi, D. B.; Lindau, I.; Spicer, W. E.; Kapitulnik, A.

1989-12-01

Angle-resolved photoemission experiments on single crystals of Bi 2(Sr,Ca,La) 3Cu 2O 8 are reported. The data show a dispersionless behaviour of the valence band states as a function of the perpendicular component of the wave vector (along the c-axis), while as a function of the parallel component (in the a-b plane) clear dispersion occurs. Furthermore, polarization-dependent excitations reveal information on the symmetry of the unoccupied states.

Electrochemical deposition of silver crystals aboard Skylab 4

NASA Technical Reports Server (NTRS)

Grodzka, P. G.; Facemire, B. R.; Johnston, M. H.; Gates, D. W.

1976-01-01

Silver crystals were grown aboard Skylab 4 by an electro-chemical reaction and subsequently returned to earth for comparison with crystals grown at 1- and 5-g. Both the Skylab and earth-grown crystals show a variety of structures. Certain tendencies in structure dependency on gravity level, however, can be discerned. In addition, downward growing dendrite streamers; upward growing chunky crystal streamers; growth along an air/liquid interface; and ribbon, film, and fiber crystal habits were observed in experiments conducted on the ground with solutions of varying concentrations. It was also observed that the crystal structures of space and ground electro-deposited silver crystals were very similar to the structures of germanium selenide and germanium telluride crystals grown in space and on the ground by a vapor transport technique. Consideration of the data leads to the conclusions that: (1) the rate of electrochemical displacement of silver ions from a 5 percent aqueous solution by copper is predominantly diffussion controlled in space and kinetically controlled in 1- and higher-g because of augmentation of mass transport by convection; (2) downward and upward crystal streamers are the result of gravity-driven convection, the flow patterns of which can be delineated. Lateral growths along an air/liquid interface are the result of surface-tension-driven convection, the pattern of which also can be delineated; (3) electrolysis in space or low-g environments can produce either dendritic crystals with more perfect microcrystalline structures or massive, single crystals with fewer defects than those grown on ground or at higher g-levels. Ribbons or films of space-grown silicon crystals would find a ready market for electronic substrate and photocell applications. Space-grown dendritic, metal crystals present the possibility of unique catalysts. Large perfect crystals of various materials are desired for a number of electronic and optical applications; and (4) vapor transport growth of germanium selenide and germanium telluride is affected by convection mechanisms similar to the mechanisms hypothesized for the electrochemical deposition of silver crystals. Evidence and considerations leading to the preceding summaries and conclusions are presented. The implications of the findings and conclusions for technological applications are discussed, and recommendations for further experiments are presented.

Selective Metal Cation Capture by Soft Anionic Metal-Organic Frameworks via Drastic Single-Crystal-to-Single-Crystal Transformations

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

Tian, Jian; Saraf, Laxmikant V.; Schwenzer, Birgit

2012-05-25

Flexible anionic metal-organic frameworks transform to neutral heterobimetallic systems via single-crystal-to-single-crystal processes invoked by cation insertion. These transformations are directed by cooperative bond breakage and formation, resulting in expansion or contraction of the 3D framework by up to 33% due to the flexible nature of the organic linker. These MOFs displays highly selective uptake of divalent transition metal cations (Co2+ and Ni2+ for example) over alkali metal cations (Li+ and Na+).

Erbium Distribution in Single Crystal YAG Fibers Grown by Laser-Heated Pedestal Growth Technique

DTIC Science & Technology

2015-08-28

single crystal YAG fibers grown by laser - heated pedestal growth technique Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host...inserted into a SC YAG tube. This rod-in-tube was used as a preform in our laser -heated pedestal growth (LHPG) apparatus to grow a fiber with a radial...fibers grown by laser -heated pedestal growth technique Report Title Single crystal (SC) yttrium aluminum garnet (YAG, Y3Al5O12) as a host material has

Alloy Design Challenge: Development of Low Density Superalloys for Turbine Blade Applications

NASA Technical Reports Server (NTRS)

MacKay, Rebecca A.; Gabb, Timothy P.; Smialek, James L.; Nathal, Michael V.

2009-01-01

New low density single crystal (LDS) alloys have been developed for turbine blade applications, which have the potential for significant improvements in the thrust to weight ratio over current production alloys. An innovative alloying strategy was identified to achieve high temperature creep resistance, alloy density reductions, microstructural stability, and cyclic oxidation resistance. The approach relies on the use of molybdenum (Mo) as a potent solid solution strengthener for the nickel (Ni)-base superalloy; Mo has a density much closer to Ni than other refractory elements, such as rhenium (Re) or tungsten (W). A host of testing and microstructural examinations was conducted on the superalloy single crystals, including creep rupture testing, microstructural stability, cyclic oxidation, and hot corrosion. The paper will provide an overview of the single crystal properties that were generated in this new superalloy design space. The paper will also demonstrate the feasibility of this innovative approach of low density single crystal superalloy design. It will be shown that the best LDS alloy possesses the best attributes of three generations of single crystal alloys: the low density of first-generation single crystal alloys, the excellent oxidation resistance of second-generation single crystal alloys, and a creep strength which exceeds that of second and third generation alloys.

van der Waals epitaxy of SnS film on single crystal graphene buffer layer on amorphous SiO2/Si

NASA Astrophysics Data System (ADS)

Xiang, Yu; Yang, Yunbo; Guo, Fawen; Sun, Xin; Lu, Zonghuan; Mohanty, Dibyajyoti; Bhat, Ishwara; Washington, Morris; Lu, Toh-Ming; Wang, Gwo-Ching

2018-03-01

Conventional hetero-epitaxial films are typically grown on lattice and symmetry matched single crystal substrates. We demonstrated the epitaxial growth of orthorhombic SnS film (∼500 nm thick) on single crystal, monolayer graphene that was transferred on the amorphous SiO2/Si substrate. Using X-ray pole figure analysis we examined the structure, quality and epitaxy relationship of the SnS film grown on the single crystal graphene and compared it with the SnS film grown on commercial polycrystalline graphene. We showed that the SnS films grown on both single crystal and polycrystalline graphene have two sets of orientation domains. However, the crystallinity and grain size of the SnS film improve when grown on the single crystal graphene. Reflection high-energy electron diffraction measurements show that the near surface texture has more phases as compared with that of the entire film. The surface texture of a film will influence the growth and quality of film grown on top of it as well as the interface formed. Our result offers an alternative approach to grow a hetero-epitaxial film on an amorphous substrate through a single crystal graphene buffer layer. This strategy of growing high quality epitaxial thin film has potential applications in optoelectronics.

Molecular-dynamic simulations of the thermophysical properties of hexanitrohexaazaisowurtzitane single crystal at high pressures and temperatures

NASA Astrophysics Data System (ADS)

Kozlova, S. A.; Gubin, S. A.; Maklashova, I. V.; Selezenev, A. A.

2017-11-01

Molecular dynamic simulations of isothermal compression parameters are performed for a hexanitrohexaazaisowurtzitane single crystal (C6H6O12N12) using a modified ReaxFF-log reactive force field. It is shown that the pressure-compression ratio curve for a single C6H6O12N12 crystal at constant temperature T = 300 K in pressure range P = 0.05-40 GPa is in satisfactory agreement with experimental compression isotherms obtained for a single C6H6O12N12 crystal. Hugoniot molecular-dynamic simulations of the shock-wave hydrostatic compression of a single C6H6O12N12 crystal are performed. Along with Hugoniot temperature-pressure curves, calculated shock-wave pressure-compression ratios for a single C6H6O12N12 crystal are obtained for a wide pressure range of P = 1-40 GPa. It is established that the percussive adiabat obtained for a single C6H6O12N12 crystal is in a good agreement with the experimental data. All calculations are performed using a LAMMPS molecular dynamics simulation software package that provides a ReaxFF-lg reactive force field to support the approach.

Compaction of Chromite Cumulates applying a Centrifuging Piston-Cylinder

NASA Astrophysics Data System (ADS)

Manoochehri, S.; Schmidt, M. W.

2012-12-01

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

Thermal conductivity investigation of adhesive-free bond laser components

NASA Astrophysics Data System (ADS)

Li, Da; Hong, Pengda; Vedula, MahaLakshmi; Meissner, Helmuth E.

2017-02-01

An interferometric method has been developed and employed at Onyx Optics, Inc. to accurately measure the thermal conductivity of laser-active crystals as function of dopant concentration or inactive materials such as single crystals, optical ceramics and glasses relative to a standard of assumed to be known thermal conductivity [1]. This technique can also provide information on heat transfer resistance at the interface between two materials in close thermal contact. While the technique appears generally applicable to composites between optically homogeneous materials, we report on thermal conductivities and heat transfer coefficients of selected adhesive-free bond (AFB®) laser composites. Single crystal bars and AFB bonded crystal doublets with the combinations of various rare-earth (Nd3+, Yb3+, Er3+, and Tm3+ trivalent ion doped YAG, and un-doped YAG have been fabricated with the AFB technique. By loading the test sample in a vacuum cryostat, with a precisely controlled heat load at one end of the doublets, the temperature distribution inside the single crystal or the composite samples can been precisely mapped by measuring the optical path difference interferometrically, given the material's thermal-optical properties. No measurable heat transfer resistance can be identified for the AFB interfaces between low-concentration doped YAG and un-doped YAG. For the heavily doped RE3+:YAG, for example, 10% Yb:YAG, the thermal conductivity measured in our experiment is 8.3 W/m•K, using the thermal conductivity of undoped YAG reported in [1] as basis. The thermal transfer resistance of the AFB interface with un-doped YAG, if there is any at the AFB interface, could be less than 1.29×10-6 m2•K/W.

A High-Rate, Single-Crystal Model for Cyclotrimethylene Trinitramine including Phase Transformations and Plastic Slip

DOE PAGES

Addessio, Francis L.; Luscher, Darby Jon; Cawkwell, Marc Jon; ...

2017-05-14

A continuum model for the high-rate, thermo-mechanical deformation of single-crystal cyclotrimethylene trinitramine (RDX) is developed. The model includes the effects of anisotropy, large deformations, nonlinear thermo-elasticity, phase transformations, and plastic slip. A multiplicative decomposition of the deformation gradient is used. The volumetric elastic component of the deformation is accounted for through a free-energy based equation of state for the low- (α) and high-pressure (γ) polymorphs of RDX. Crystal plasticity is addressed using a phenomenological thermal activation model. The deformation gradient for the phase transformation is based on an approach that has been applied to martensitic transformations. Simulations were conducted andmore » compared to high-rate, impact loading of oriented RDX single crystals. The simulations considered multiple orientations of the crystal relative to the direction of shock loading and multiple sample thicknesses. Thirteen slip systems, which were inferred from indentation and x-ray topography, were used to model the α-polymorph. It is shown that by increasing the number of slip systems from the previously considered number of six (6) to thirteen (13) in the α-polymorph, better comparisons with data may be obtained. Simulations of impact conditions in the vicinity of the α- to γ-polymorph transformation (3.8 GPa) are considered. Eleven of the simulations, which were at pressures below the transformation value (3.0 GPa), were compared to experimental data. Comparison of the model was also made with available data for one experiment above the transformation pressure (4.4 GPa). Also, simulations are provided for a nominal pressure of 7.5 GPa to demonstrate the effect of the transformation kinetics on the deformation of a high-rate plate impact problem.« less

A High-Rate, Single-Crystal Model for Cyclotrimethylene Trinitramine including Phase Transformations and Plastic Slip

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

Addessio, Francis L.; Luscher, Darby Jon; Cawkwell, Marc Jon

A continuum model for the high-rate, thermo-mechanical deformation of single-crystal cyclotrimethylene trinitramine (RDX) is developed. The model includes the effects of anisotropy, large deformations, nonlinear thermo-elasticity, phase transformations, and plastic slip. A multiplicative decomposition of the deformation gradient is used. The volumetric elastic component of the deformation is accounted for through a free-energy based equation of state for the low- (α) and high-pressure (γ) polymorphs of RDX. Crystal plasticity is addressed using a phenomenological thermal activation model. The deformation gradient for the phase transformation is based on an approach that has been applied to martensitic transformations. Simulations were conducted andmore » compared to high-rate, impact loading of oriented RDX single crystals. The simulations considered multiple orientations of the crystal relative to the direction of shock loading and multiple sample thicknesses. Thirteen slip systems, which were inferred from indentation and x-ray topography, were used to model the α-polymorph. It is shown that by increasing the number of slip systems from the previously considered number of six (6) to thirteen (13) in the α-polymorph, better comparisons with data may be obtained. Simulations of impact conditions in the vicinity of the α- to γ-polymorph transformation (3.8 GPa) are considered. Eleven of the simulations, which were at pressures below the transformation value (3.0 GPa), were compared to experimental data. Comparison of the model was also made with available data for one experiment above the transformation pressure (4.4 GPa). Also, simulations are provided for a nominal pressure of 7.5 GPa to demonstrate the effect of the transformation kinetics on the deformation of a high-rate plate impact problem.« less

Two-Oxide Disequilibrium: A New Geospeedometer Based on Diffusion in Ilmenite

NASA Astrophysics Data System (ADS)

Williams, K. B.; Krawczynski, M. J.; Van Orman, J. A.

2016-12-01

Diffusion-annealing experiments were conducted in a 0.5" piston cylinder apparatus to investigate diffusivity of Fe2+, Mg2+, and Mn2+ in ilmenite solid solutions between 800ºC and 1000ºC. Polycrystalline ilmenite (FeTiO3) was juxtaposed against either an oriented geikielite (MgTiO3) single crystal or polycrystalline Mn-bearing (5 mol% Mn) ilmenite, in a "diffusion-couple" geometry. Geikielite single crystals were synthesized at Los Alamos National Laboratory, cut into 1 mm edge-length cubes, and polished either perpendicular or parallel to the c-axis. Polycrystalline ilmenite starting materials were synthesized by mixing high purity reagent-grade oxides (FeO, MnO, and TiO2) and sintering in a piston cylinder apparatus, then cut into wafers and polished. Experimental run products were analyzed by electron microprobe at Washington University in St. Louis. Microprobe analyses were obtained perpendicularly across the diffusion interface for each experiment. Experimental diffusion profiles create smooth curves that, when fit with an error function, define Fe-Mg and Fe-Mn interdiffusion coefficients in ilmenite. The diffusion coefficients do not appear compositionally dependent, but do show significant anisotropy. Preliminary results suggest diffusion activation energies are lower in ilmenite than in titanomagnetite [1]. Ilmenite-titanomagnetite equilibria define pre-eruptive temperatures and oxygen fugacities. However, oxides often exist out of equilibrium [2]. We use the cation diffusion data for ilmenite and existing data on titanomagnetite to establish two-oxide disequilibrium as a geospeedometer. Our data constrain oxide-oxide re-equilibration timescales at Mt. Unzen to months, consistent with estimates from zoned, single crystals of magnetite [3,4]. Future experiments will examine the effect of oxygen fugacity on diffusivity in ilmenite solid solutions. References:[1] Van Orman & Crispin (2010) RiMG 72, 757-825.[2] Bacon & Hirschmann (1988) Am. Min. 73, 57-61.[3] Nakamura (1995) Geology 23, 807-810.[4] Venezky & Rutherford (1999) J. Volc. Geo. Res. 89, 213-230.

The Curious Case of 2-Propyl-1H-benzimidazole in the Solid State: An Experimental and Theoretical Study.

PubMed

Quesada-Moreno, María Mar; Cruz-Cabeza, Aurora J; Avilés-Moreno, Juan Ramón; Cabildo, Pilar; Claramunt, Rosa M; Alkorta, Ibon; Elguero, José; Zúñiga, Francisco J; López-González, Juan Jesús

2017-08-03

2-Propyl-1H-benzimidazole (2PrBzIm) is a small molecule, commercially available, which displays a curious behavior in the solid state. 2PrBzIm, although devoid of chirality by fast rotation about a single bond of the propyl group in solution, crystallizes as a conglomerate showing chiroptical properties. An exhaustive analysis of its crystal structure and a wide range of experiments monitored by vibrational circular dichroism spectroscopy eliminated all possibilities of an artifact. What remains is a new example of the unexplained phenomenon of persistent supramolecular chirality.

In-line microfluidic refractometer based on C-shaped fiber assisted photonic crystal fiber Sagnac interferometer.

PubMed

Wu, Chuang; Tse, Ming-Leung Vincent; Liu, Zhengyong; Guan, Bai-Ou; Lu, Chao; Tam, Hwa-Yaw

2013-09-01

We propose and demonstrate a highly sensitive in-line photonic crystal fiber (PCF) microfluidic refractometer. Ultrathin C-shaped fibers are spliced in-between the PCF and standard single-mode fibers. The C-shaped fibers provide openings for liquid to flow in and out of the PCF. Based on a Sagnac interferometer, the refractive index (RI) response of the device is investigated theoretically and experimentally. A high sensitivity of 6621 nm/RIU for liquid RI from 1.330 to 1.333 is achieved in the experiment, which agrees well with the theoretical analysis.

Fermi Surface Studies and Temperature Dependence of the Electron-Positron Momentum Density in the High Critical Temperature Superconducting Yttrium BARIUM(2) COPPER(3) OXYGEN(7-X) System by Two-Dimensional Acar

NASA Astrophysics Data System (ADS)

von Stetten, Eric Carl

The electron-positron momentum density has been measured by the two dimensional angular correlation of annihilation radiation (2D ACAR) technique for single crystal and polycrystalline (sintered powder) YBa_2 Cu_3O_{7-x} samples. For sintered superconducting and nonsuperconducting samples, the shape and temperature variation of the momentum density was investigated using the high sensitivity 2D ACAR technique. The possible existence of Fermi surfaces (FS's) in the YBa_2Cu _3O_{7-x} system was investigated in high precision 2D ACAR experiments on an oriented (twinned) single crystal superconducting YBa_2Cu _3O_{7-x} (x ~ 0.1) sample, at temperatures above and below the superconducting transition temperature (~85 K). These experiments were performed in the c-axis projection, in order to observe the theoretically predicted cylindrical FS's (if they exist) in a single experiment, without a full reconstruction of the three dimensional momentum density. Large differences were observed between the room temperature 2D ACAR spectra for superconducting and nonsuperconducting sintered powder samples, and smaller differences were observed between the spectra for similarly prepared superconducting samples. For sintered superconducting samples, complex sample dependent temperature variations of the momentum density were observed, in contrast to the small linear temperature variation observed for a sintered powder nonsuperconducting sample. These results are interpreted as manifestations of the theoretically predicted preferential sampling of the linear Cu-O chain region by the positron in the YBa _2Cu_3O _{7-x} system. High precision experiments on the single crystal superconducting sample revealed a nearly isotropic 2D ACAR spectrum, with only four small (~3% of the height at p_{x} = p _{y} = 0) peaks centered along the (110) symmetry lines. A small narrowing of the 2D ACAR spectrum was observed above T_{c}. The Brillouin-zone-reduced momentum density was formed using the "Lock-Crisp-West folding" technique, in order to identify possible FS signatures; several small features were observed that could possibly be due to FS's. A computer study of statistical noise propagation in 2D ACAR data, however, found that the possible FS signatures in the experimental data are similar in shape and magnitude to noise produced features.

Crystal growth, piezoelectric, non-linear optical and mechanical properties of lithium hydrogen oxalate monohydrate single crystal

NASA Astrophysics Data System (ADS)

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

2017-05-01

Semi-organic lithium hydrogen oxalate monohydrate non-linear optical single crystals have been grown by slow evaporation solution growth technique at 35 °C. Single crystal X-ray diffraction study showed that the grown crystal belongs to the triclinic system with space group P1. The mechanical strength decreases with increasing load. The piezoelectric coefficient is found to be 1.41 pC/N. The nonlinear optical property was measured using Kurtz Perry powder technique and SHG efficiency was almost equal to that of KDP.

ACTIVE MEDIA: BaY2F8 single crystals doped with rare-earth ions as promising up-conversion media for UV and VUV lasers

NASA Astrophysics Data System (ADS)

Pushkar', A. A.; Uvarova, T. V.; Molchanov, V. N.

2008-04-01

BaY2F8 crystals are studied as promising active media for UV and VUV lasers. The up-conversion pumping of rare-earth activators is proposed to solve problems related to the solarisation of the medium and the selection of pump sources. The technology of growing oriented BaY2F8 single crystals is developed and the influence of the crystal orientation on the growth rate and quality of single crystals is determined.

The Crystal Hotel: A Microfluidic Approach to Biomimetic Crystallization.

PubMed

Gong, Xiuqing; Wang, Yun-Wei; Ihli, Johannes; Kim, Yi-Yeoun; Li, Shunbo; Walshaw, Richard; Chen, Li; Meldrum, Fiona C

2015-12-02

A "crystal hotel" microfluidic device that allows crystal growth in confined volumes to be studied in situ is used to produce large calcite single crystals with predefined crystallographic orientation, microstructure, and shape by control of the detailed physical environment, flow, and surface chemistry. This general approach can be extended to form technologically important, nanopatterned single crystals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Channeling technique to make nanoscale ion beams

NASA Astrophysics Data System (ADS)

Biryukov, V. M.; Bellucci, S.; Guidi, V.

2005-04-01

Particle channeling in a bent crystal lattice has led to an efficient instrument for beam steering at accelerators [Biryukov et al., Crystal Channeling and its Application at High Energy Accelerators, Springer, Berlin, 1997], demonstrated from MeV to TeV energies. In particular, crystal focusing of high-energy protons to micron size has been demonstrated at IHEP with the results well in match with Lindhard (critical angle) prediction. Channeling in crystal microstructures has been proposed as a unique source of a microbeam of high-energy particles [Bellucci et al., Phys. Rev. ST Accel. Beams 6 (2003) 033502]. Channeling in nanostructures (single-wall and multi-wall nanotubes) offers the opportunities to produce ion beams on nanoscale. Particles channeled in a nanotube (with typical diameter of about 1 nm) are trapped in two dimensions and can be steered (deflected, focused) with the efficiency similar to that of crystal channeling or better. This technique has been a subject of computer simulations, with experimental efforts under way in several high-energy labs, including IHEP. We present the theoretical outlook for making channeling-based nanoscale ion beams and report the experience with crystal-focused microscale proton beams.

The tensile effect on crack formation in single crystal silicon irradiated by intense pulsed ion beam

NASA Astrophysics Data System (ADS)

Liang, Guoying; Shen, Jie; Zhang, Jie; Zhong, Haowen; Cui, Xiaojun; Yan, Sha; Zhang, Xiaofu; Yu, Xiao; Le, Xiaoyun

2017-10-01

Improving antifatigue performance of silicon substrate is very important for the development of semiconductor industry. The cracking behavior of silicon under intense pulsed ion beam irradiation was studied by numerical simulation in order to understand the mechanism of induced surface peeling observed by experimental means. Using molecular dynamics simulation based on Stillinger Weber potential, tensile effect on crack growth and propagation in single crystal silicon was investigated. Simulation results reveal that stress-strain curves of single crystal silicon at a constant strain rate can be divided into three stages, which are not similar to metal stress-strain curves; different tensile load velocities induce difference of single silicon crack formation speed; the layered stress results in crack formation in single crystal silicon. It is concluded that the crack growth and propagation is more sensitive to strain rate, tensile load velocity, stress distribution in single crystal silicon.

Crystal growth of triphenylphosphine oxide 4-nitrophenol (TP4N) for nonlinear optical (NLO) applications

NASA Astrophysics Data System (ADS)

Pandian, Muthu Senthil; Karuppasamy, P.; Kamalesh, T.; Ramasamy, P.; Verma, Sunil

2018-04-01

The optically good quality organic single crystals of triphenylphosphine oxide 4-nitrophenol (TP4N) were successfully grown by slow evaporation solution technique (SEST) using methanol as solvent. The lattice parameters of the grown crystal were confirmed by single crystal X-ray diffraction analysis. The optical transmittance, cut-off wavelength and band gap of the TP4N crystal were obtained by UV-Vis NIR spectrum analysis. The photoluminescence studies were carried out to find out the luminesce properties of TP4N single crystal. The photoconductivity studies reveal that the TP4N crystal has negative photoconductive nature. The third order nonlinear susceptibility (χ(3)) of TP4N crystal was evaluated using the Z-scan technique at 640 nm.

Growth, optical, ICP and thermal studies of nonlinear optical single crystal: Sodium acid phthalate (NaAP)

NASA Astrophysics Data System (ADS)

Mahadevan, M.; Arivanandhan, M.; Elangovan, K.; Anandan, P.; Ramachandran, K.

2017-07-01

Good quality single crystals of sodium acid phthalate (NaAP) were grown by slow evaporation technique. Single crystal X-ray diffraction study of the grown crystal reveals that the crystal belongs to orthorhombic system with space group B2ab. Fourier transform infrared spectrum confirms the presence of the functional groups of the grown material. Inductively coupled plasma emission spectroscopy analysis is used to confirm the presence of Na element in the sample. Thermal analysis of the NaAP crystal shows that the crystal is stable up to 140°C. Optical transmittance of the grown crystal was recorded in the wavelength range from 200 and 800 nm using UV-Vis-NIR spectrophotometer. The second harmonic generation of NaAP was analysed using Kurtz powder technique.

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.

Direct Observation of Halide Migration and its Effect on the Photoluminescence of Methylammonium Lead Bromide Perovskite Single Crystals.

PubMed

Luo, Yanqi; Khoram, Parisa; Brittman, Sarah; Zhu, Zhuoying; Lai, Barry; Ong, Shyue Ping; Garnett, Erik C; Fenning, David P

2017-11-01

Optoelectronic devices based on hybrid perovskites have demonstrated outstanding performance within a few years of intense study. However, commercialization of these devices requires barriers to their development to be overcome, such as their chemical instability under operating conditions. To investigate this instability and its consequences, the electric field applied to single crystals of methylammonium lead bromide (CH 3 NH 3 PbBr 3 ) is varied, and changes are mapped in both their elemental composition and photoluminescence. Synchrotron-based nanoprobe X-ray fluorescence (nano-XRF) with 250 nm resolution reveals quasi-reversible field-assisted halide migration, with corresponding changes in photoluminescence. It is observed that higher local bromide concentration is correlated to superior optoelectronic performance in CH 3 NH 3 PbBr 3 . A lower limit on the electromigration rate is calculated from these experiments and the motion is interpreted as vacancy-mediated migration based on nudged elastic band density functional theory (DFT) simulations. The XRF mapping data provide direct evidence of field-assisted ionic migration in a model hybrid-perovskite thin single crystal, while the link with photoluminescence proves that the halide stoichiometry plays a key role in the optoelectronic properties of the perovskite. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Positronium hydride in hydrogen-laden thermochemically reduced MgO single crystals

NASA Astrophysics Data System (ADS)

Pareja, R.; de La Cruz, R. M.; Pedrosa, M. A.; González, R.; Chen, Y.

1990-04-01

Thermochemical reduction of hydrogen-laden MgO single crystals at T~2400 K results in a large concentration of both hydride (H-) ions and anion vacancies (>1024 m-3). Positron-lifetime experiments of these crystals provide evidence for bound positronium hydride states also referred to as [e+-H-] or PsH states. The presence of the anion vacancies was found to inhibit the formation of these states. After thermally annealing out these vacancies, such that H- concentration remains intact, two long-lived components appear in the lifetime spectrum. Furthermore, these two components correlate with the presence of the H-ions. These results suggest the existence of bound [e+-H-] states when positrons are trapped by the H- ions, and the subsequent formation of positronium (Ps) states by the dissociation of the [e+-H-] states. From the values of the intermediate lifetime component, a value of (570+/-50) ps is obtained for the lifetime of the PsH state located in an anion vacancy in MgO. The longest lifetime component ~(1-3) ns is attributed to pick-off annihilation of ortho-Ps states.